Process for producing a sintered layered body by controlling the particle size distribution and specific surface area of a powder employed, and associated layered body and assembly

Abstract

A method for producing a laminated body includes the following steps: a. introducing a first powder into an internal volume to obtain a first powder layer in the internal volume, wherein i. the internal volume A. has a cross-sectional width W of at least 200 mm, and B. is at least partially defined by an internal surface of a mold, wherein the mold has at least one wall, and wherein the wall comprises carbon; ii. the first powder is a mixture comprising a first component powder and another component powder, wherein the first component powder and the other component powder have different chemical properties. a. The first powder layer is subjected to heat and pressure to obtain the laminate, wherein i. the heat is generated by a voltage applied across the mold, the internal volume, or both, and ii. the laminate comprises the first layer; wherein the other component powder of the first powder has a particle size distribution D = q(χ) with respect to particle size χ, such that ID has a global maximum value α with respect to particle size χα and volume density qα, and II. if D has a local maximum value β with respect to particle size χβ and volume density qβ, then qα / qβ is at least 10.

Description

[Technical Field]

[0001] This invention generally relates to sintering under pressure and using an electric current, commonly known as spark plasma sintering (SPS). A specific embodiment of the invention relates to a spark plasma sintering process for obtaining a laminated body, wherein the laminated body is obtained using a first powder comprising a mixture of a first component powder and another component powder, wherein the other component powder has a unimodal particle size distribution. Another embodiment of the invention relates to a spark plasma sintering process for obtaining a laminated body, wherein the laminated body is obtained using a first powder comprising a mixture of a first component powder and another component powder, wherein the other component powder has a specific surface area of ​​less than 12 m² / g. Yet another embodiment of the invention relates to a spark plasma sintering process for obtaining a laminated body, wherein the laminated body is obtained using a first powder comprising a mixture of a first component powder and another component powder, wherein the other component powder has a unimodal particle size distribution and a specific surface area of ​​less than 12 m² / g. Another aspect of the present invention relates to a laminate obtained by a spark plasma sintering process, and the use of a first powder comprising a mixture of a first component powder and a second component powder, wherein the second component powder has a unimodal particle size distribution and / or a selected value for specific surface area. [Previous Technology]

[0002] Sintering methods provide a way to form a bulk from powder by applying heat and pressure. In one method commonly known as spark plasma sintering (SPS), electric current is used to achieve heating. State-of-the-art spark plasma sintering methods have been applied to a variety of materials. Existing literature focuses on small-scale systems, providing portions with a bulk extension of up to about 150 mm. The problems of using SPS to prepare larger portions are theoretically assessed by Eugene A. Olevsky et al. in the following: "Fundamental Aspects of Spark Plasma Sintering: I. Experimental Analysis of Scalability" (J. Am. Ceram. Soc., 95 [8], 2406 to 2413 (2012)) and "Fundamental Aspects of Spark Plasma Sintering: II. Experimental Analysis of Scalability" (J. Am. Ceram. Soc., 95 [8], 2414 to 2422 (2012)). Several challenges and complexities associated with large-scale systems were identified. The produced multilayers can be used in plasma processing chambers in the semiconductor manufacturing industry. Use of the substrate in such industries requires high-quality substrates, specifically etch-resistant, robust, and with very high purity. The use of the substrate in such industries also requires the multilayer to have a diameter of at least 200 mm. WO2022072703 A1 and WO2022133180 A1 disclose the use of spark plasma sintering to produce multilayers. [Summary of the Invention]

[0003] The object of the present invention is to overcome at least one of the disadvantages encountered in the present best technology.

[0004] A further object of the present invention is to provide a process for producing a laminate, wherein the laminate has a diameter of at least 200 mm.

[0005] A further object of the present invention is to provide a process for producing laminates, wherein the laminates have improved properties.

[0006] A further object of the present invention is to provide a process for producing laminates, wherein the laminates have increased strength.

[0007] A further object of the present invention is to provide a process for producing laminates, wherein the laminates have increased scratch resistance.

[0008] A further object of the present invention is to provide a process for producing a laminate, wherein the laminate has a reduced density variation in the laminate.

[0009] A further object of the present invention is to provide a process for producing laminates, wherein the laminates have a reduced defect rate.

[0010] A further object of the present invention is to provide a process for producing a laminate, wherein the laminate has increased etch resistance.

[0011] A further object of the present invention is to provide a process for producing laminates, wherein the laminates have reduced color variations.

[0012] A further object of the present invention is to provide a process for producing a laminate, wherein the laminate has reduced porosity.

[0013] A further object of the present invention is to provide a process for producing a laminate, wherein the laminate has a small amount of unreacted starting powder.

[0014] A further object of the present invention is to provide a laminate having a diameter of at least 200 mm.

[0015] A further object of the present invention is to provide a laminate having improved properties (such as increased strength, increased scratch resistance, reduced density variation, reduced defect rate, increased etch resistance, reduced color variation, reduced porosity, and less unreacted starting powder).

[0016] Any embodiment of the present invention contributes to at least partially achieving at least one of the objectives mentioned above.

[0017] An embodiment of the present invention is a process for producing a laminate, comprising the following steps: a. introducing a first powder into an internal volume to obtain a first powder layer in the internal volume, wherein i. the internal volume A. has a cross-sectional width W of at least 200 mm, preferably at least 300 mm, more preferably at least 400 mm, and further preferably at least 500 mm, and B. is at least partially delimited by an internal surface of a mold, wherein the mold has at least one wall, and wherein the wall comprises carbon; ii. the first powder is a mixture comprising a first component powder and another component powder, wherein the first component powder and the other component powder have different chemical compositions; b. subjecting the first powder layer to heat and pressure to obtain the laminate, wherein i. the heat is generated by a voltage applied across the mold, the internal volume, or both, and ii. the laminate comprises a first layer.

[0018] This independent embodiment is a first embodiment of a process for producing the laminate. In a preferred embodiment of this process, the internal volume has a cross-sectional width W in the range of 200 mm to 650 mm, more preferably 300 mm to 650 mm, even more preferably 400 mm to 650 mm, and further preferably 500 mm to 650 mm. In a preferred embodiment of this process, the first powder is obtained by mixing the first component powder and the other component powder. In this embodiment, it is preferable that the mixing is performed before the first powder is introduced into the internal volume. In a preferred embodiment of this process, the first component powder is zirconium oxide. In another preferred embodiment of this process, the other component powder is alumina.

[0019] In the following preferred embodiments, when "process" is mentioned, it should be understood to refer to the process used to produce the laminate.

[0020] In a preferred embodiment of the procedure, the first powder comprises at least one or all of the following: yttrium, aluminum, zirconium, magnesium, or a combination of at least two of them.

[0021] This preferred embodiment of the present invention is a second embodiment of the procedure, which is preferably based on the first embodiment of the procedure. A preferred combination of at least two of the chemical elements in the second embodiment of the procedure includes yttrium aluminum garnet, zirconium oxide-toughened alumina, and combinations thereof. In a particularly preferred embodiment of the second embodiment of the procedure, the first powder comprises yttrium oxide and alumina.

[0022] In a preferred embodiment of the procedure, the first powder comprises at least one oxide, preferably at least one oxide selected from the group consisting of: yttrium oxide, aluminum oxide, zirconium oxide, magnesium oxide, and combinations of at least two thereof.

[0023] This preferred embodiment of the present invention is the third embodiment of the procedure, which is preferably based on any of the first to second embodiments of the procedure. In a particularly preferred embodiment of the third embodiment of the procedure, the first powder comprises yttrium oxide and aluminum oxide. In a preferred embodiment of the third embodiment of the procedure, if the at least one oxide comprises and / or is zirconium oxide, then the zirconium oxide is preferably partially stabilized zirconium oxide, stabilized zirconium oxide, or a combination thereof. In this embodiment, partially stabilized zirconium oxide is preferred over stabilized zirconium oxide.

[0024] In a preferred embodiment of the procedure, the first powder is a mixture of two component powders.

[0025] This preferred embodiment of the present invention is the fourth embodiment of the procedure, which is preferably based on any one of the first to third embodiments of the procedure. In the preferred embodiment of the fourth embodiment of the procedure, the two component powders are yttrium oxide powder and aluminum oxide powder.

[0026] In a preferred embodiment of the procedure, at least one or all of the following are applicable to the first powder: a. containing at least 25 mol-%, preferably at least 30 mol-%, and even more preferably at least 35 mol-%, of yttrium oxide; b. containing at least 50 mol-%, more preferably at least 55 mol-%, and even more preferably at least 60 mol-%, of aluminum oxide.

[0027] This preferred embodiment of the present invention is the fifth embodiment of the procedure, which is preferably dependent on any of the first to fourth embodiments of the procedure. In the fifth embodiment of the procedure, all feasible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In one preferred embodiment of the fifth embodiment of the procedure, feature a., the first powder contains yttrium oxide in the range of 28 mol-% to 48 mol-%, more preferably 32 mol-% to 44 mol-%, and even more preferably 36 mol-% to 40 mol-%. In one preferred embodiment of the fifth embodiment of the procedure, feature b., the first powder contains alumina in the range of 52 mol-% to 72 mol-%, more preferably 56 mol-% to 68 mol-%, and even more preferably 60 mol-% to 64 mol-%. In one of the fifth embodiments of the procedure, a particularly preferred embodiment, the first powder comprises yttrium oxide and aluminum oxide.

[0028] In one preferred embodiment of the procedure, at least one or all of the following are applicable to the first powder: a. Yttrium oxide contained in the range of 35.5 mol-% to 39.5 mol-%, preferably 36.5 mol-% to 38.5 mol-%, and more preferably 37.4 mol-% to 37.6 mol-%. b. Aluminum oxide contained in the range of 60.5 mol-% to 64.5 mol-%, preferably 61.5 mol-% to 63.5 mol-%, and more preferably 62.4 mol-% to 62.6 mol-%.

[0029] This preferred embodiment of the invention is the sixth embodiment of the procedure, which is preferably based on any of the first to fifth embodiments of the procedure. In the sixth embodiment of the procedure, all possible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In one preferred embodiment of the sixth embodiment of the procedure, the first powder is a stoichiometric powder mixture of 37.4 mol-% to 37.6 mol-% yttrium oxide and 62.4% mol-% to 62.6% mol-% alumina. The following ratio is particularly preferred: 37.5 mol-% yttrium oxide and 62.5 mol-% alumina. In the sixth embodiment of the procedure, the combination of features a+b does not necessarily have to add up to 100 mol-%.

[0030] In a preferred embodiment of the procedure, the first component powder of the first powder has at least one or all of the following properties: a. a d10 particle size in the range of 1 µm to 7 µm, preferably 1.5 µm to 6 µm, more preferably 2 µm to 5.4 µm, even more preferably 2.5 µm to 4.7 µm, and further preferably 2.9 µm to 4.3 µm; b. a d50 particle size in the range of 2 µm to 14 µm, preferably 3 µm to 12 µm, more preferably 4 µm to 10 µm, even more preferably 4.7 µm to 8 µm, and further preferably 5.1 µm to 7.5 µm; c. a d50 particle size in the range of 3 µm to 20 µm, preferably 5 µm to 18 µm, more preferably 7 µm to 16 µm, and even more preferably 7.5 µm to 14 µm. μm, and more preferably d90 particle size in the range of 8 µm to 12 µm.

[0031] This preferred embodiment of the invention is the seventh embodiment of the procedure, which is preferably dependent on any of the first to sixth embodiments of the procedure. In the seventh embodiment of the procedure, all feasible combinations of features a. to c. are preferred embodiments of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c. The values ​​given in at least one or all of features a. to c. in the seventh embodiment of the procedure are preferably applicable after the first powder has been heat-treated (e.g., calcined). In the preferred embodiment of the seventh embodiment of the procedure, the first component powder of the first powder is yttrium oxide.

[0032] In a preferred embodiment of the procedure, the other component powder of the first powder has at least one or all of the following properties: a. a d10 particle size in the range of 0.005 µm to 0.4 µm, preferably 0.01 µm to 0.3 µm, more preferably 0.04 µm to 0.26 µm, even more preferably 0.06 µm to 0.21 µm, and further preferably 0.1 µm to 0.17 µm; b. a d50 particle size in the range of 0.01 µm to 0.8 µm, preferably 0.05 µm to 0.65 µm, more preferably 0.1 µm to 0.5 µm, even more preferably 0.13 µm to 0.4 µm, and further preferably 0.17 µm to 0.34 µm; c. a d50 particle size in the range of 0.05 µm to 0.7 µm. The d90 particle size is in the range of µm, preferably from 0.1 µm to 5 µm, more preferably from 0.2 µm to 3 µm, even more preferably from 0.3 µm to 2.5 µm, and even more preferably from 0.5 µm to 1.7 µm.

[0033] This preferred embodiment of the invention is the eighth embodiment of the procedure, which is preferably dependent on any of the first to seventh embodiments of the procedure. In the eighth embodiment of the procedure, all feasible combinations of features a. to c. are preferred embodiments of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c. The values ​​given in at least one or all of features a. to c. in the eighth embodiment of the procedure are preferably applicable before the first powder has been heat-treated (e.g., calcined). In the preferred embodiment of the eighth embodiment of the procedure, the other component powder of the first powder is alumina.

[0034] In a preferred embodiment of the procedure, the first powder layer has a thickness such that the first layer formed from the first powder layer has a thickness in the range of 0.5 mm to 12 mm, preferably 2 mm to 8 mm, and even more preferably 4 mm to 5 mm.

[0035] This preferred embodiment of the present invention is the ninth embodiment of the program, which is preferably any of the first to eighth embodiments of the program.

[0036] In a preferred embodiment of the procedure, the procedure further includes the step of introducing another powder into the internal volume to obtain another powder layer.

[0037] This preferred embodiment of the present invention is the tenth embodiment of the procedure, which is preferably dependent on any of the first to ninth embodiments of the procedure. In one preferred embodiment of the tenth embodiment of the procedure, the first powder layer and the other powder layer are in physical contact with each other (e.g., in contact with each other). In one preferred embodiment of the tenth embodiment of the procedure, the other powder is introduced into the internal volume before subjecting the first powder layer to the heat and pressure. In this embodiment, it is preferable that both the first powder layer and the other powder layer are subject to the heat and pressure, thereby resulting in the laminate containing the first layer and the other layer. In one preferred embodiment of the tenth embodiment of the procedure, the other powder is introduced into the internal volume before or after the first powder layer has been obtained. In this embodiment, more preferably, the other powder is introduced into the internal volume after the first powder layer has been obtained. In an alternative preferred embodiment of the procedure, after the first powder layer has been subjected to heat and pressure, the other powder is introduced into the internal volume. In this alternative preferred embodiment, the other powder layer is subjected to further heat and pressure. In this alternative preferred embodiment, the laminate is obtained, wherein the laminate comprises the first layer and the other layer.

[0038] In a preferred embodiment of the procedure, the other powder comprises aluminum, zirconium, or a combination thereof.

[0039] This preferred embodiment of the invention is the 11th embodiment of the procedure, which is more preferably based on the 10th embodiment of the procedure. In the 11th embodiment of the procedure, the preferred combination of aluminum and zirconium is zirconium oxide toughened alumina. Here, the zirconium oxide is preferably partially stable, stable, or a combination thereof, wherein partially stable zirconium oxide is particularly preferred.

[0040] In a preferred embodiment of the procedure, the other powder comprises at least one oxide, preferably at least one oxide selected from the group consisting of: aluminum oxide, zirconium oxide, and combinations thereof.

[0041] This preferred embodiment of the present invention is the 12th embodiment of the procedure, which is preferably based on any of the 10th to 11th embodiments of the procedure. In the preferred embodiment of the 12th embodiment of the procedure, if the at least one oxide comprises and / or is zirconium oxide, then the zirconium oxide is partially stable, stable, or a combination of at least both. In this embodiment, partially stable zirconium oxide is preferred over stable zirconium oxide.

[0042] In a preferred embodiment of the procedure, the other powder is a mixture of at least two component powders, preferably alumina powder and zirconium oxide powder.

[0043] This preferred embodiment of the present invention is the 13th embodiment of the program, which is preferably any of the 10th to 12th embodiments of the program.

[0044] In a preferred embodiment of the procedure, at least one or all of the following are applicable to the other powder: a. Containing alumina, preferably in the range of 60 wt% to 92.5 wt%, more preferably in the range of 66 wt% to 89 wt%, even more preferably in the range of 71 wt% to 84 wt%, and further preferably in the range of 75 wt% to 79 wt% based on the total weight of the other powder; b. Containing zirconium oxide, preferably in the range of 7.5 wt% to 40 wt%, more preferably in the range of 11 wt% to 35 wt%, even more preferably in the range of 16 wt% to 29 wt%, and further preferably in the range of 21 wt% to 25 wt%.

[0045] This preferred embodiment of the invention is the 14th embodiment of the procedure, which is preferably dependent on any of the 10th to 13th embodiments of the procedure. In the 14th embodiment of the procedure, all possible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In one particularly preferred embodiment of the 14th embodiment of the procedure, the other powder comprises a mixture of alumina powder and zirconium oxide powder. In the 14th embodiment of the procedure, the zirconium oxide is preferably at least one of partially stabilized zirconium oxide and stabilized zirconium oxide, wherein partially stabilized zirconium oxide is particularly preferred.

[0046] In a preferred embodiment of the procedure, the other powder comprises a mixture of a first component powder and another component powder, wherein the first component powder of the other powder has at least one or all of the following properties: a. a d10 particle size in the range of 0.01 µm to 0.4 µm, preferably 0.04 µm to 0.35 µm, more preferably 0.06 µm to 0.27 µm, even more preferably 0.09 µm to 0.22 µm, and further preferably 0.11 µm to 0.18 µm; b. a d50 particle size in the range of 0.01 µm to 3 µm, preferably 0.1 µm to 1.5 µm, more preferably 0.2 µm to 1 µm, even more preferably 0.26 µm to 0.6 µm, and further preferably 0.3 µm to 0.36 µm; c. a d50 particle size in the range of 0.3 µm to 0.4 µm, preferably 0.04 µm to 0.35 µm, more preferably 0.26 µm to 0.27 µm, and even more preferably 0.26 µm to 0.6 µm, and even more preferably 0.3 µm to 0.36 µm; The d90 particle size is in the range of µm to 10 µm, more preferably in the range of 0.4 µm to 7 µm, more preferably in the range of 0.47 µm to 6 µm, even more preferably in the range of 0.53 µm to 3 µm, and even more preferably in the range of 0.57 µm to 1 µm.

[0047] This preferred embodiment of the invention is the 15th embodiment of the procedure, which is preferably based on any of the 10th to 14th embodiments of the procedure. In the 15th embodiment of the procedure, all feasible combinations of features a. to c. are preferred embodiments of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c. The values ​​given in at least one or all of features a. to c. in the 15th embodiment of the procedure are preferably applicable after the other powder has been heat-treated (e.g., calcined). In the preferred embodiment of the 15th embodiment of the procedure, the first component powder of the other powder is zirconium oxide.

[0048] In a preferred embodiment of the procedure, the other powder comprises a mixture of a first component powder and another component powder, wherein the other component powder of the other powder has at least one or all of the following properties: a. a d10 particle size in the range of 0.01 µm to 0.3 µm, more preferably 0.03 µm to 0.2 µm, and even more preferably 0.05 µm to 0.15 µm; b. a d50 particle size in the range of 0.01 µm to 1.5 µm, more preferably 0.05 µm to 1.0 µm, and even more preferably 0.1 µm to 0.8 µm; c. a d90 particle size in the range of 0.01 µm to 6.0 µm, more preferably 0.05 µm to 3.5 µm, and even more preferably 0.1 µm to 3.0 µm.

[0049] This preferred embodiment of the invention is the 16th embodiment of the procedure, which is preferably dependent on any of the 10th to 15th embodiments of the procedure. In the 16th embodiment of the procedure, all feasible combinations of features a. to c. are preferred embodiments of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c. The values ​​given in at least one or all of features a. to c. in the 16th embodiment of the procedure are preferably applicable before the other powder has been heat-treated (e.g., calcined). In the preferred embodiment of the 16th embodiment of the procedure, the other component powder of the other powder is alumina.

[0050] In a preferred embodiment of the procedure, the other powder layer has a thickness such that the other layer formed from the other powder layer has a thickness in the range of 5 mm to 50 mm, preferably 15 mm to 40 mm, further preferably 20 mm to 35 mm, and even more preferably 25 mm to 30 mm.

[0051] This preferred embodiment of the present invention is the 17th embodiment of the program, which is preferably any of the 10th to 16th embodiments of the program.

[0052] In a preferred embodiment of the procedure, one of the following is applicable: a. The first powder is capable of forming a first oxide under applied heat and pressure, preferably oxide A; b. The first powder is capable of forming another oxide under applied heat and pressure, preferably oxide B.

[0053] This preferred embodiment of the present invention is the 18th embodiment of the program, which is preferably based on any one of the 1st to 17th embodiments of the program. In the 18th embodiment of the program, feature a is particularly preferred.

[0054] In a preferred embodiment of the procedure, one of the following is applicable: a. The other powder is capable of forming the first oxide under applied heat and pressure; b. The other powder is capable of forming the other oxide under applied heat and pressure; c. The first powder and the other powder are capable of forming the first oxide under applied heat and pressure; d. The first powder and the other powder are capable of forming the other oxide under applied heat and pressure; e. The first powder is capable of forming the first oxide under applied heat and pressure, and the other powder is capable of forming the other oxide under applied heat and pressure; f. The first powder is capable of forming the other oxide under applied heat and pressure, and the other powder is capable of forming the first oxide under applied heat and pressure.

[0055] This preferred embodiment of the present invention is the 19th embodiment of the program, which is preferably based on any one of the 10th to 18th embodiments of the program. In the 19th embodiment of the program, features e. and f. are particularly preferred, with feature e. being the most preferred. The first oxide and the other oxide are the same as those described in the aforementioned 18th embodiment of the program. In the preferred embodiment of the 19th embodiment of the program, the first oxide is oxide A. In another preferred embodiment of the 19th embodiment of the program, the other oxide is oxide B.

[0056] In a preferred embodiment of the procedure, the first oxide is one of the following: a. a cubic phase, preferably a cubic phase containing yttrium, more preferably a cubic phase of yttrium aluminum oxide, and even more preferably YAG, preferably a composition having a ratio of yttrium oxide and aluminum oxide of 3:5; b. an oxide containing magnesium, more preferably an oxide containing magnesium and aluminum, such as magnesium aluminate spinel (MgAl2O4); c. a combination of yttrium oxide and zirconium oxide, wherein the zirconium oxide is present in amounts within the following ranges: preferably 10 mol-% to 25 mol-%, more preferably 15 mol-% to 25 mol-%, and even more preferably 18 mol-% to 25 mol-%; preferably 10 mol-% to 23 mol-%, more preferably 10 mol-% to 20 mol-%; preferably 15 mol-% to 23 mol-%. mol-%; the balance preferably includes yttrium oxide; particularly preferably, the combination of yttrium oxide and zirconium oxide is in the form of a crystalline solid solution; d. YAG and at least one of the following: at least one perovskite, monoclinic, alumina, yttrium oxide, a combination thereof, preferably YAG, and at least one of the following crystal phases: YAP (yttrium aluminum perovskite), YAM (yttrium aluminum monoclinic), yttrium oxide, alumina, or at least two of the above; at least one or all of YAP, YAM, yttrium oxide, and alumina preferably exist in an amount of less than 5% by volume; preferably, at least one or all of the crystal phases of YAG, YAP, and YAM are polycrystalline.

[0057] This preferred embodiment of the present invention is the 20th embodiment of the procedure, which is preferably based on any of the 18th to 19th embodiments of the procedure. Feature a of the 20th embodiment of the procedure is particularly preferred. In this embodiment, it is preferable that the first oxide contains less than 0.01 mol-% of at least one, preferably all of the following: YAP, YAM, and yttrium oxide.

[0058] In a preferred embodiment of the procedure, the other oxide comprises at least one or all of the following: a. aluminum oxide; b. zirconium oxide, preferably stabilized zirconium oxide and / or partially stabilized zirconium oxide, wherein partially stabilized zirconium oxide is particularly preferred.

[0059] This preferred embodiment of the invention is the 21st embodiment of the procedure, which is preferably based on any of the 18th to 20th embodiments of the procedure. In the 21st embodiment of the procedure, all possible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In a particularly preferred embodiment of the 21st embodiment of the procedure, the other oxide comprises alumina and zirconium oxide. In this embodiment, it is preferable that the other oxide comprises at least two separate crystalline phases of zirconium oxide and alumina, referred herein as a composite oxide or particulate composite or zirconium oxide dispersed toughened alumina (ZTA).

[0060] In a preferred embodiment of the procedure, during the step of subjecting the first powder layer and, preferably, the other powder layer (if present), to the heat and the pressure, the temperature in the internal volume is within the following ranges: 900°C to 2000°C, preferably 950°C to 1900°C, more preferably 1000°C to 1800°C, and even more preferably 1050°C to 1700°C; preferably 1000°C to 1700°C, more preferably 1100°C to 1700°C, even more preferably 1200°C to 1700°C, even more preferably 1300°C to 1700°C, and even even more preferably 1400°C to 1700°C.

[0061] This preferred embodiment of the present invention is the 22nd embodiment of the program, which is preferably any of the 1st to 21st embodiments of the program.

[0062] In a preferred embodiment of the procedure, during the step of subjecting the first powder layer and, preferably, the other powder layer (if present), to the heat and the pressure, the first powder layer and, preferably, the other powder layer (if present), are subjected to the following pressures: at least 1 MPa, preferably at least 5 MPa, more preferably at least 10 MPa, further preferably at least 15 MPa; preferably 1 MPa to 100 MPa, more preferably 5 MPa to 60 MPa, even more preferably 5 MPa to 45 MPa, further preferably 5 MPa to 30 MPa, and even more preferably 5 MPa to 15 MPa; preferably 10 MPa to 60 MPa, more preferably 10 MPa to 45 MPa, even more preferably 10 MPa to 30 MPa, and even more preferably 10 MPa to 15 MPa; preferably 15 MPa to 60 MPa, more preferably 15 MPa to 45 MPa. MPa, or even better, 15 MPa to 30 MPa, and even more preferably 15 MPa to 20 MPa.

[0063] This preferred embodiment of the present invention is the 23rd embodiment of the program, which is preferably any of the 1st to 22nd embodiments of the program.

[0064] In a preferred embodiment of the procedure, the voltage (applied across the mold, the internal volume, or both) is in the range of 0.5 V to 10 V, more preferably 1 V to 8 V, more preferably 1.5 V to 7 V, and even more preferably 2 V to 6 V.

[0065] This preferred embodiment of the present invention is the 24th embodiment of the program, which is preferably any of the 1st to 23rd embodiments of the program.

[0066] In a preferred embodiment of the procedure, the voltage (applied across the mold, the internal volume, or both) is obtained by providing current to a device containing the internal volume, wherein the current is in the range of 1 kA to 100 kA, preferably 5 kA to 90 kA, more preferably 10 kA to 80 kA, even more preferably 15 kA to 70 kA, and further preferably in the range of 20 kA to 60 kA; alternatively, the current may be greater than 100 kA.

[0067] This preferred embodiment of the present invention is the 25th embodiment of the program, which is preferably based on any one of the 1st to 24th embodiments of the program. In the 25th embodiment of the program, the current is preferably provided by a power supply connected to the device.

[0068] In a preferred embodiment of the procedure, the laminate has a diameter of at least 200 mm, more preferably at least 300 mm, and more preferably at least 500 mm; the diameter can reach up to 2000 mm or more; the diameter is preferably no greater than 1500 mm, more preferably no greater than 900 mm, even more preferably no greater than 800 mm, further preferably no greater than 700 mm, and even more preferably no greater than 650 mm; the diameter is preferably in the following range: greater than 200 mm to 625 mm; more preferably 300 mm to 625 mm, even more preferably 400 mm to 625 mm, and even more preferably 500 mm to 625 mm.

[0069] This preferred embodiment of the present invention is the 26th embodiment of the program, which is preferably any of the 1st to 25th embodiments of the program.

[0070] In a preferred embodiment of the procedure, the applied electrical power flux is in the range of 0.05 W / mm² to 1.6 W / mm², more preferably in the range of 0.1 W / mm² to 1.3 W / mm², and even more preferably in the range of 0.3 W / mm² to 1 W / mm², wherein the power flux is applicable to at least one or all of the following: the mold, the internal volume, the first powder layer, the other powder layer (if present), at least one punch (if present), or at least both of the following.

[0071] This preferred embodiment of the present invention is the 27th embodiment of the procedure, which is preferably based on any one of the 1st to 26th embodiments of the procedure. In the preferred embodiment of the 27th embodiment of the procedure, when the laminate to be prepared has a diameter in the range of >500 mm to 650 mm, the power flux is in the range of 0.05 W / mm² to 1 W / mm², more preferably in the range of 0.1 W / mm² to 0.7 W / mm², and even more preferably in the range of 0.3 W / mm² to 0.5 W / mm². In a preferred embodiment of the 27th embodiment of the procedure, when the laminate to be prepared has a diameter in the range of 300 mm to 500 mm, the electrical power flux is in the range of >0.1 W / mm² to 1.6 W / mm², more preferably >0.3 W / mm² to 1.3 W / mm², and even more preferably >0.5 W / mm² to 1.0 W / mm².

[0072] In a preferred embodiment of the procedure, the internal volume is defined by: a. the inner surface of the first punch of the first punch; b. the inner surface of the second punch of the second punch; and c. the inner surface of the mold, wherein I. the first punch and the second punch are adapted and configured to apply pressure to the first powder layer and preferably the other powder layer (if present) in the internal volume during the step of subjecting the first powder layer and preferably the other powder layer (if present) to the heat and the pressure, II. the pressure is applied along the compression axis, and III. the angle between the compression axis and the cross-sectional width W of the internal volume is in the range of 88° to 92°, preferably 89° to 91°, and further preferably 89.5° to 90.5°.

[0073] This preferred embodiment of the present invention is the 28th embodiment of the program, which is preferably any of the 1st to 27th embodiments of the program.

[0074] In a preferred embodiment of the procedure, the first powder is capable of forming at least one or all of the following under applied heat and pressure: a. Oxide A, comprising at least 1 mol-% of a Group 3 (formerly Group IIIB) element (preferably yttrium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is expressed as oxygen in oxide A; preferably, oxide A is a cubic phase of yttrium aluminum oxide, more preferably YAG; b. Oxide B, comprising at least 1 mol-% of a Group 4 (formerly Group IVB) element (preferably zirconium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is expressed as oxygen in oxide B; preferably, oxide B is ZTA.

[0075] This preferred embodiment of the present invention is the 29th embodiment of the procedure, which is preferably dependent on any of the 1st to 28th embodiments of the procedure. In the 29th embodiment of the procedure, all feasible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In the 29th embodiment of the procedure, the groups refer to groups of the periodic table. Feature a. in the 29th embodiment of the procedure is particularly preferred. In the preferred embodiment of the 29th embodiment of the procedure, oxide A is an inorganic oxide. In the preferred embodiment of the 29th embodiment of the procedure, oxide B is an inorganic oxide. In the preferred embodiment of the 29th embodiment of the procedure, feature a., oxide A contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 3 (formerly Group IIIB) element. In the preferred embodiment of the 29th example of the procedure, feature a., the oxide A contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 13 (formerly Group IIIA) element. In the preferred embodiment of the 29th example of the procedure, feature b., the oxide B contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 4 (formerly Group IVB) element. In the preferred embodiment of the 29th example of the procedure, feature b., the oxide B contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 13 (formerly Group IIIA) element.

[0076] In a preferred embodiment of the procedure, the other powder is capable of forming at least one or all of the following under applied heat and pressure: a. Oxide A, comprising at least 1 mol-% of a Group 3 (formerly Group IIIB) element (preferably yttrium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is expressed as oxygen in oxide A; preferably, oxide A is a cubic phase of yttrium aluminum oxide, more preferably YAG; b. Oxide B, comprising at least 1 mol-% of a Group 4 (formerly Group IVB) element (preferably zirconium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is expressed as oxygen in oxide B; preferably, oxide B is ZTA.

[0077] This preferred embodiment of the present invention is the 30th embodiment of the procedure, which is preferably dependent on any of the 10th to 29th embodiments of the procedure. In the 30th embodiment of the procedure, all feasible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In the 30th embodiment of the procedure, the groups refer to groups of the periodic table. Feature b. in the 30th embodiment of the procedure is particularly preferred. In the preferred embodiment of the 30th embodiment of the procedure, oxide A is an inorganic oxide. In the preferred embodiment of the 30th embodiment of the procedure, oxide B is an inorganic oxide. In the preferred embodiment of the 30th embodiment of the procedure, feature a., oxide A contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 3 (formerly Group IIIB) element. In the preferred embodiment of the 30th example of the procedure, feature a., the oxide A contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 13 (formerly Group IIIA) element. In the preferred embodiment of the 30th example of the procedure, feature b., the oxide B contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 4 (formerly Group IVB) element. In the preferred embodiment of the 30th example of the procedure, feature b., the oxide B contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 13 (formerly Group IIIA) element.

[0078] In a preferred embodiment of the procedure, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to particle size q, such that a. D has a global maximum value α with respect to particle size χα and volume density qα, and b. if D has a local maximum value β with respect to particle size χβ and volume density qβ, then qα / qβ is at least 10, preferably at least 20, more preferably at least 30, even more preferably at least 50, and further preferably at least 100.

[0079] This preferred embodiment of the present invention is the 31st embodiment of the program, which is preferably based on any one of the 1st to 30th embodiments of the program. In the preferred embodiment of the 31st embodiment of the program, D is unimodal (e.g., D has a global maximum value but does not have one or more local maximum values ​​β).

[0080] In a preferred embodiment of the procedure, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to volume density q, such that a. D has a global maximum value α with particle size χα and volume density qα, and b. if D has a local maximum value β with particle size χβ and volume density qβ, then qβ is less than 1.00 x 10-3, preferably less than 0.50 x 10-3, more preferably less than 0.10 x 10-3, and even more preferably less than 0.01 x 10-3.

[0081] This preferred embodiment of the present invention is the 32nd embodiment of the program, which is preferably any of the 1st to 31st embodiments of the program.

[0082] In a preferred embodiment of the procedure, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to volume density q, wherein D is unimodal.

[0083] This preferred embodiment of the present invention is the 33rd embodiment of the program, which is preferably any of the 1st to 32nd embodiments of the program.

[0084] In a preferred embodiment of the procedure, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to volume density q, wherein D has a global maximum value α with respect to particle size χα and volume density qα, and wherein χα is in the range of 2.7 µm to 7 µm, preferably 3.2 µm to 6 µm, more preferably 3.7 µm to 5.3 µm, and even more preferably 4.2 µm to 4.8 µm.

[0085] This preferred embodiment of the present invention is the 34th embodiment of the program, which is preferably any of the 1st to 33rd embodiments of the program.

[0086] In a preferred embodiment of the procedure, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to volume density q, wherein D has a global maximum value α for particle size χα and volume density qα, and wherein qα is in the range of 6.8 to 12, preferably 7.5 to 10.5, more preferably 8.2 to 10, and even more preferably 8.8 to 9.4.

[0087] This preferred embodiment of the present invention is the 35th embodiment of the program, which is preferably any of the 1st to 34th embodiments of the program.

[0088] In a preferred embodiment of any of the 31st to 35th embodiments of the procedure, the particle size distribution D = q(χ) of the other component powder is the particle size distribution of the other component powder before the first component powder and the other component powder are mixed to obtain the first powder.

[0089] In a preferred embodiment of the procedure, the other component powder of the first powder has a specific surface area of ​​less than or equal to 12 m2 / g, more preferably less than or equal to 10 m2 / g, more preferably less than or equal to 9 m2 / g, and even more preferably less than or equal to 8.5 m2 / g.

[0090] This preferred embodiment of the present invention is the 36th embodiment of the program, which is preferably any of the 1st to 35th embodiments of the program.

[0091] In a preferred embodiment of the procedure, the specific surface area of ​​the other component powder of the first powder is in the range of 2.5 m2 / g to 12 m2 / g, more preferably 3 m2 / g to 10 m2 / g, more preferably 3.5 m2 / g to 9 m2 / g, and even more preferably 4 m2 / g to 8.5 m2 / g.

[0092] This preferred embodiment of the present invention is the 37th embodiment of the procedure, which is preferably based on any one of the 1st to 36th embodiments of the procedure. In one particularly preferred embodiment of the 37th embodiment of the procedure, the specific surface area of ​​the other component powder of the first powder is in the range of 4.2 to 8.3 m2 / g, more preferably 4.5 to 8 m2 / g.

[0093] In one preferred embodiment of the procedure, the first layer has a thickness of at least 2 mm, preferably at least 4 mm, more preferably at least 5 mm, and even more preferably at least 8 mm.

[0094] This preferred embodiment of the present invention is the 38th embodiment of the program, which is preferably any of the 1st to 37th embodiments of the program.

[0095] In one preferred embodiment of the procedure, the first layer has a thickness of at least 10 mm, more preferably at least 14 mm, more preferably at least 17 mm, and even more preferably at least 20 mm.

[0096] This preferred embodiment of the present invention is the 39th embodiment of the procedure, which is preferably attached to any of the 1st to 38th embodiments of the procedure. In one preferred embodiment of the 39th embodiment of the procedure, the first layer has a thickness in the range of 10 to 70 mm, more preferably 14 to 50 mm, even more preferably 17 to 40 mm, and further preferably 20 to 30 mm. In one preferred embodiment of the 39th embodiment of the procedure, the first layer has a thickness in the range of 15 to 70 mm, more preferably 15 to 50 mm, even more preferably 15 to 40 mm, and further preferably 15 to 30 mm. In one preferred embodiment of the 39th embodiment of the procedure, the first layer has a thickness in the range of 20 to 70 mm, more preferably 20 to 50 mm, even more preferably 20 to 40 mm, and further preferably 20 to 30 mm.

[0097] In a preferred embodiment of the procedure, the other component powder of the first powder is an oxide of a Group 13 (formerly Group 3A) element (preferably aluminum).

[0098] This preferred embodiment of the present invention is the 40th embodiment of the program, which is preferably any of the 1st to 39th embodiments of the program.

[0099] In a preferred embodiment of the procedure, the first component powder of the first powder is an oxide selected from elements of Group 3 (formerly IIIB) (preferably yttrium) or elements of Group 4 (formerly IVB) (preferably zirconium).

[0100] This preferred embodiment of the present invention is the 41st embodiment of the procedure, which is preferably any one of the 1st to 40th embodiments of the procedure. In one particularly preferred embodiment of the 41st embodiment of the procedure, the first component powder is an oxide selected from elements of Group 3 (formerly IIIB) (more preferably yttrium).

[0101] In a preferred embodiment of the procedure, at least one or all of the following applies: a. The first component powder of the first powder has a purity of at least 95%, preferably at least 97%, more preferably at least 99%, even more preferably at least 99.99%, further preferably at least 99.999%, and even more preferably at least 99.9999%; b. The other component powder of the first powder has a purity of at least 95%, preferably at least 97%, more preferably at least 99%, even more preferably at least 99.99%, further preferably at least 99.999%, and even more preferably at least 99.9999%; c. The first powder has a purity of at least 95%, preferably at least 97%, more preferably at least 99%, even more preferably at least 99.99%, further preferably at least 99.999%, and even more preferably at least 99.9999%.

[0102] This preferred embodiment of the present invention is the 42nd embodiment of the program, which is preferably based on any of the 1st to 41st embodiments of the program. In one embodiment of the 42nd embodiment of the program, all feasible combinations of features a. to c. are preferred embodiments of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c.

[0103] In one preferred embodiment of the procedure, the first component powder of the first powder has a particle size distribution E = r(χ) of bulk density r versus particle size χ, wherein E has a global maximum value δ for particle size χδ and bulk density rδ, and wherein at least one or all of the following applies: a. χδ is in the range of 3 to 9 µm, preferably 4.5 to 7.5 µm, more preferably 5 to 6.8 µm, and even more preferably 5.5 to 6.3 µm; b. rδ is in the range of 0.05 to 0.22, preferably 0.08 to 0.18, and more preferably 0.11 to 0.15; c. E is unimodal.

[0104] This preferred embodiment of the present invention is the 43rd embodiment of the procedure, which is preferably dependent on any of the 1st to 42nd embodiments of the procedure. In one embodiment of the 43rd embodiment of the procedure, all feasible combinations of features a. to c. are preferred embodiments of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c. In one preferred embodiment of the 43rd embodiment of the procedure, the first powder is obtained by mixing the first component powder and the other component powder. In this embodiment, it is preferable that the mixing is performed before the first powder is introduced into the internal volume. In one preferred embodiment of the 43rd embodiment of the procedure, at least one or all of features a. to c. are applied before mixing the first component powder with the other component powder to obtain the first powder.

[0105] In one preferred embodiment of the procedure, before introducing the first powder into the internal volume, the procedure includes the step of mixing the first component powder with the other component powder to obtain the first powder.

[0106] This preferred embodiment of the present invention is the 44th embodiment of the program, which is preferably any of the 1st to 43rd embodiments of the program.

[0107] In one preferred embodiment of the procedure, before mixing the first component powder and the other component powder to obtain the first powder, the other component powder is subjected to heat treatment, wherein the heat treatment preferably reduces the number of peaks in the particle size distribution D.

[0108] This preferred embodiment of the present invention is the 45th embodiment of the procedure, which is preferably based on any one of the 1st to 44th embodiments of the procedure. In one preferred embodiment of the 45th embodiment of the procedure, the heat treatment of the other component powder of the first powder is performed before the first powder is introduced into the internal volume.

[0109] In one preferred embodiment of the procedure, the temperature at which the other component powder of the first powder undergoes the heat treatment is in the range of 850 to 1100°C, more preferably 900 to 1030°C, and even more preferably 930 to 980°C.

[0110] This preferred embodiment of the present invention is the 46th embodiment of the program, which is more preferably based on the 45th embodiment of the program.

[0111] In a preferred embodiment of the procedure, the first powder is subjected to heat treatment before being introduced into the internal volume.

[0112] This preferred embodiment of the present invention is the 47th embodiment of the procedure, which is preferably based on any one of the 1st to 46th embodiments of the procedure. In one preferred embodiment of the 47th embodiment of the procedure, the heat treatment is performed after the first component powder and the other component powder are mixed to obtain the first powder.

[0113] In a preferred embodiment of the procedure, one of the following applies: a. The temperature at which the first powder undergoes the heat treatment is in the range of 680 to 1100°C, preferably 740 to 950°C, and even more preferably 780 to 870°C; b. The temperature at which the first powder undergoes the heat treatment is in the range of 950 to 1200°C, preferably 990 to 1140°C, and even more preferably 1030 to 1080°C.

[0114] This preferred embodiment of the invention is the 48th embodiment of the procedure, which is preferably based on the 47th embodiment of the procedure. In one preferred embodiment of the 48th embodiment of the procedure, the heat treatment of the first powder is performed after the first component powder and the other component powder are mixed to obtain the first powder. In the 48th embodiment of the procedure, feature a is preferred over feature b. In the 48th embodiment of the procedure, feature a is preferred over feature b in the following case: the other component powder is subjected to heat treatment before mixing the first component powder and the other component powder to obtain the first powder (see, for example, the 45th embodiment of the procedure).

[0115] In one preferred embodiment of the procedure, the first powder has a specific surface area in the range of 1.6 to 7 m2 / g, more preferably 2 to 6.6 m2 / g, more preferably 2.4 to 6.2 m2 / g, even more preferably 2.7 to 5.8 m2 / g, and even more preferably 3 to 5.5 m2 / g.

[0116] This preferred embodiment of the present invention is the 49th embodiment of the procedure, which is preferably based on any one of the 1st to 48th embodiments of the procedure. In one preferred embodiment of the 49th embodiment of the procedure, the first powder has the specific surface area after being heat-treated.

[0117] The preferred embodiments and preferred forms of the procedure for the first powder are also preferably applicable to the first powder layer. The preferred embodiments and preferred forms of the procedure for the first powder layer are also preferably applicable to the first powder. The preferred embodiments and preferred forms of the procedure for the other powder are also preferably applicable to the other powder layer. The preferred embodiments and preferred forms of the procedure for the other powder layer are also preferably applicable to the other powder.

[0118] An embodiment of the present invention comprises a stack containing a first layer, preferably a stack obtainable by means of a procedure for obtaining a stack according to the present invention, and more preferably a stack obtainable by means of a procedure according to any one of the first to 49 embodiments of the procedure. This embodiment is the first embodiment of the stack.

[0119] In a preferred embodiment of the laminate, the first layer comprises yttrium, aluminum, zirconium, magnesium, or a combination of at least two of them.

[0120] This preferred embodiment of the present invention is a second embodiment of the laminate, which is preferably attached to the first embodiment of the laminate. A preferred combination of at least two of the chemical elements in the second embodiment of the laminate includes yttrium aluminum garnet, zirconium oxide-toughened alumina, and combinations thereof. In a particularly preferred embodiment of the second embodiment of the laminate, the first layer comprises yttrium oxide and alumina.

[0121] In a preferred embodiment of the laminate, the first layer comprises at least one oxide, preferably at least one oxide selected from the group consisting of: yttrium oxide, aluminum oxide, zirconium oxide, magnesium oxide, and combinations of at least two thereof.

[0122] This preferred embodiment of the present invention is a third embodiment of the laminate, which is preferably attached to any of the first to second embodiments of the laminate. In a particularly preferred embodiment of the third embodiment of the laminate, the first layer comprises yttrium oxide and aluminum oxide. In a preferred embodiment of the third embodiment of the laminate, if the at least one oxide comprises and / or is zirconium oxide, then the zirconium oxide is preferably partially stabilized zirconium oxide, stabilized zirconium oxide, or a combination thereof. In this embodiment, partially stabilized zirconium oxide is preferred over stabilized zirconium oxide.

[0123] In a preferred embodiment of the laminate, at least one or all of the following are applicable to the first layer: a. containing at least 25 mol-%, preferably at least 30 mol-%, and even more preferably at least 35 mol-%, of yttrium oxide; b. containing at least 50 mol-%, more preferably at least 55 mol-%, and even more preferably at least 60 mol-%, of aluminum oxide.

[0124] This preferred embodiment of the present invention is the fourth embodiment of the laminate, which is preferably attached to any of the first to third embodiments of the laminate. In the fourth embodiment of the laminate, all possible combinations of features a. and b. are preferred embodiments of the embodiment. These combinations are, for example, a; b; a+b. In the preferred embodiment of the fourth embodiment of the laminate, feature a., the first layer contains yttrium oxide in the range of 28 mol-% to 48 mol-%, more preferably 32 mol-% to 44 mol-%, and even more preferably 36 mol-% to 40 mol-%. In a preferred embodiment of the fourth embodiment of the laminate, feature b. indicates that the first layer comprises alumina in the range of 52 mol-% to 72 mol-%, more preferably 56 mol-% to 68 mol-%, and even more preferably 60 mol-% to 64 mol-%. In a particularly preferred embodiment of the fourth embodiment of the laminate, the first layer comprises yttrium oxide and alumina.

[0125] In a preferred embodiment of the laminate, at least one or all of the following are applicable to the first layer: a. Yttrium oxide contained in the range of 35.5 mol-% to 39.5 mol-%, preferably 36.5 mol-% to 38.5 mol-%, and even more preferably 37.4 mol-% to 37.6 mol-%. b. Aluminum oxide contained in the range of 60.5 mol-% to 64.5 mol-%, preferably 61.5 mol-% to 63.5 mol-%, and even more preferably 62.4 mol-% to 62.6 mol-%.

[0126] This preferred embodiment of the present invention is the fifth embodiment of the laminate, which is preferably attached to any of the first to fourth embodiments of the laminate. In the fifth embodiment of the laminate, all feasible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In the preferred embodiment of the fifth embodiment of the laminate, the first layer contains yttrium oxide in the range of 37.4 mol-% to 37.6 mol-% and aluminum oxide in the range of 62.4 mol-% and 62.6 mol-%. The following ratio is particularly preferred: 37.5 mol-% yttrium oxide and 62.5 mol-% aluminum oxide. In the fifth embodiment of the laminate, the combination of features a+b does not necessarily have to add up to 100 mol-%.

[0127] In a preferred embodiment of the laminate, the first layer comprises at least one or all of the following: a. Oxide A, comprising at least 1 mol-% of a Group 3 (formerly Group IIIB) element (preferably yttrium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is expressed as oxygen in oxide A; preferably, oxide A is a cubic phase of yttrium aluminum oxide, more preferably YAG; b. Oxide B, comprising at least 1 mol-% of a Group 4 (formerly Group IVB) element (preferably zirconium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is expressed as oxygen in oxide B; preferably, oxide B is ZTA.

[0128] This preferred embodiment of the present invention is the sixth embodiment of the laminate, which is preferably attached to any of the first to fifth embodiments of the laminate. In the state of the sixth embodiment of the laminate, all feasible combinations of features a. and b. are the preferred state of this embodiment. These combinations are, for example, a; b; a+b. In the sixth embodiment of the laminate, the groups refer to the groups of the periodic table. Feature a. in the sixth embodiment of the laminate is particularly preferred. In the preferred state of the sixth embodiment of the process, oxide A is an inorganic oxide. In the preferred state of the sixth embodiment of the process, oxide B is an inorganic oxide. In the preferred state of the sixth embodiment of the laminate, feature a., oxide A contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 3 (formerly Group IIIB) element. In the preferred sample of the sixth embodiment of the laminate, feature a. the oxide A contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 13 (formerly Group IIIA) element. In the preferred sample of the sixth embodiment of the laminate, feature b. the oxide B contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 4 (formerly Group IVB) element. In the preferred sample of the sixth embodiment of the laminate, feature b. the oxide B contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 13 (formerly Group IIIA) element.

[0129] In a preferred embodiment of the laminate, the thickness of the first layer is in the range of 0.5 mm to 12 mm, more preferably in the range of 2 mm to 8 mm, and even more preferably in the range of 4 mm to 5 mm.

[0130] This preferred embodiment of the present invention is the seventh embodiment of the laminate, which is preferably attached to any one of the first to sixth embodiments of the laminate.

[0131] In a preferred embodiment of the laminate, the laminate includes another layer.

[0132] This preferred embodiment of the present invention is the eighth embodiment of the laminate, which is preferably attached to any one of the first to seventh embodiments of the laminate.

[0133] In a preferred embodiment of the laminate, the other layer comprises aluminum, zirconium, or a combination thereof.

[0134] This preferred embodiment of the present invention is the ninth embodiment of the laminate, which is more preferably attached to the eighth embodiment of the laminate. In the ninth embodiment of the laminate, the preferred combination of aluminum and zirconium is zirconium oxide toughened alumina. Here, the zirconium oxide is preferably partially stable, stable, or a combination of at least two of them, wherein partially stable zirconium oxide is particularly preferred.

[0135] In a preferred embodiment of the laminate, the other layer comprises at least one oxide, preferably at least one oxide selected from the group consisting of: aluminum oxide, zirconium oxide, and combinations thereof.

[0136] This preferred embodiment of the present invention is the tenth embodiment of the laminate, which is preferably attached to any of the eighth to ninth embodiments of the laminate. In the preferred embodiment of the tenth embodiment of the laminate, if the at least one oxide comprises and / or is zirconium oxide, then the zirconium oxide is partially stable, stable, or a combination of at least two of the above. In this embodiment, partially stable zirconium oxide is preferred over stable zirconium oxide.

[0137] In a preferred embodiment of the laminate, at least one or all of the following are applicable to the other layer: a. Alumina comprising: 70 vol-% to 97 vol-%, preferably 75 vol-% to 95 vol-%, and more preferably 80 vol-% to 92 vol-%; preferably 70 vol-% to 90 vol-%, more preferably 75 vol-% to 95 vol-%, even more preferably 80 vol-% to 90 vol-%; preferably 75 vol-% to 86 vol-%, more preferably 80 vol-% to 86 vol-%, all based on the total volume of the other layer; b. Zirconia comprising: 3 vol-% to 30 vol-%, preferably 5 vol-% to 25 vol-%, and more preferably 8 vol-% to 20 vol-%. vol-% to 30 vol-%, more preferably 10 vol-% to 25 vol-%, even more preferably 10 vol-% to 20 vol-%, and more preferably 14 vol-% to 25 vol-%, even more preferably 20 vol-% to 25 vol-%, and more preferably 14 vol-% to 20 vol-%, all based on the total volume of the other layer.

[0138] This preferred embodiment of the present invention is the 11th embodiment of the laminate, which is preferably attached to any of the 8th to 10th embodiments of the laminate. In the 11th embodiment of the laminate, all possible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In the 11th embodiment of the laminate, it is preferable that the other layer comprises both alumina and zirconium oxide. In this embodiment, it is preferable that the other layer comprises alumina in the range of 80 vol-% to 92 vol-% and zirconium oxide in the range of 8 vol-% to 20 vol-%.

[0139] In a preferred embodiment of the laminate, the other layer comprises at least one or all of the following: a. Oxide A, comprising at least 1 mol-% of a Group 3 (formerly Group IIIB) element (preferably yttrium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is expressed as oxygen in oxide A; preferably, oxide A is a cubic phase of yttrium aluminum oxide, more preferably YAG; b. Oxide B, comprising at least 1 mol-% of a Group 4 (formerly Group IVB) element (preferably zirconium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is expressed as oxygen in oxide B; preferably, oxide B is ZTA.

[0140] This preferred embodiment of the present invention is the 12th embodiment of the laminate, which is preferably attached to any of the 8th to 11th embodiments of the laminate. In the 12th embodiment of the laminate, all possible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In the 12th embodiment of the laminate, the groups refer to the groups of the periodic table. Feature b. in the 12th embodiment of the laminate is particularly preferred. In the preferred embodiment of the 12th embodiment of the process, oxide A is an inorganic oxide. In the preferred embodiment of the 12th embodiment of the process, oxide B is an inorganic oxide. In the preferred embodiment of the 12th embodiment of the laminate, feature a., oxide A contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 3 (formerly Group IIIB) element. In the preferred sample of the 12th embodiment of the laminate, feature a. the oxide A contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 13 (formerly Group IIIA) element. In the preferred sample of the 12th embodiment of the laminate, feature b. the oxide B contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 4 (formerly Group IVB) element. In the preferred sample of the 12th embodiment of the laminate, feature b. the oxide B contains at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-%, of a Group 13 (formerly Group IIIA) element.

[0141] In a preferred embodiment of the laminate, at least one or all of the following applies: a. The thickness of the other layer is 1.5 to 15 times greater than the thickness of the first layer, preferably 2 to 10 times greater, and more preferably 3.5 to 8 times greater; b. The thickness of the other layer is in the range of 5 mm to 50 mm, preferably in the range of 15 mm to 35 mm, and even more preferably in the range of 20 mm to 30 mm;

[0142] This preferred embodiment of the present invention is the 13th embodiment of the laminate, which is preferably attached to any of the 8th to 12th embodiments of the laminate. In the 13th embodiment of the laminate, all feasible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b.

[0143] In a preferred embodiment of the laminate, one of the following applies: a. The first layer comprises the first oxide, wherein the first oxide is preferably oxide A; b. The first layer comprises the other oxide, wherein the other oxide is preferably oxide B.

[0144] This preferred embodiment of the present invention is the 14th embodiment of the laminate, which is preferably attached to any one of the 1st to 13th embodiments of the laminate. In the 14th embodiment of the procedure, feature a is particularly preferred.

[0145] In a preferred embodiment of the laminate, one of the following is applicable: a. The other layer comprises the first oxide; b. The other layer comprises the other oxide; c. The first layer and the other layer comprise the first oxide; d. The first layer and the other layer comprise the other oxide; e. The first layer comprises the first oxide and the other layer comprises the other oxide; f. The first layer comprises the other oxide and the other layer comprises the first oxide.

[0146] This preferred embodiment of the present invention is the 15th embodiment of the laminate, which is preferably attached to any one of the 8th to 14th embodiments of the laminate. In the preferred embodiment of the 15th embodiment of the laminate, features e. and f. are particularly preferred, wherein feature e. is the most preferred. The first oxide and the other oxide are the same as those described in the aforementioned 14th embodiment of the laminate. In the preferred embodiment of the 15th embodiment of the laminate, the first oxide is oxide A. In another preferred embodiment of the 15th embodiment of the laminate, the other oxide is oxide B.

[0147] In a preferred embodiment of the laminate, the first oxide is one of the following: a. a cubic phase, preferably a cubic phase containing yttrium, more preferably a cubic phase of yttrium aluminum oxide, and even more preferably YAG, preferably a composition having a yttrium oxide and aluminum oxide composition in a ratio of 3:5; b. an oxide containing magnesium, more preferably an oxide containing magnesium and aluminum, such as magnesium aluminate spinel (MgAl2O4); c. a combination of yttrium oxide and zirconium oxide, wherein the zirconium oxide is present in amounts within the following ranges: preferably 10 mol-% to 25 mol-%, more preferably 15 mol-% to 25 mol-%, and even more preferably 18 mol-% to 25 mol-%; preferably 10 mol-% to 23 mol-%, more preferably 10 mol-% to 20 mol-%; preferably 15 mol-% to 23 mol-%. mol-%; the balance preferably includes yttrium oxide; particularly preferably, the combination of yttrium oxide and zirconium oxide is in the form of a crystalline solid solution. d. YAG and at least one of the following: at least one perovskite, monoclinic, alumina, yttrium oxide, a combination thereof, preferably YAG, and at least one of the following crystal phases: YAP (yttrium aluminum perovskite), YAM (yttrium aluminum monoclinic), yttrium oxide, alumina, or at least two of the above; at least one or all of YAP, YAM, yttrium oxide, and alumina preferably exist in an amount of less than 5% by volume; preferably, at least one or all of the crystal phases of YAG, YAP, and YAM are polycrystalline.

[0148] This preferred embodiment of the present invention is the 16th embodiment of the laminate, which is preferably based on any of the 14th to 15th embodiments of the laminate. Feature a. of the 16th embodiment of the laminate is particularly preferred. In this embodiment, it is preferable that the first oxide contains at least one, preferably all, of the following at less than 0.01 mol-%: YAP, YAM, and yttrium oxide.

[0149] In a preferred embodiment of the laminate, the other oxide comprises at least one or all of the following: a. aluminum oxide; b. zirconium oxide, preferably stabilized zirconium oxide and / or partially stabilized zirconium oxide, wherein partially stabilized zirconium oxide is particularly preferred.

[0150] This preferred embodiment of the present invention is the 17th embodiment of the laminate, which is preferably attached to any of the 14th to 16th embodiments of the laminate. In the 17th embodiment of the laminate, all possible combinations of features a. and b. are preferred embodiments of this embodiment. These combinations are, for example, a; b; a+b. In a particularly preferred embodiment of the 17th embodiment of the laminate, the other oxide comprises alumina and zirconium oxide. In this embodiment, it is preferable that the other oxide comprises at least two separate crystalline phases of zirconium oxide and alumina, referred herein as a composite oxide or particulate composite or zirconium oxide dispersed toughened alumina (ZTA).

[0151] In a preferred embodiment of the laminate, the first layer has at least one or all of the following properties: a. The value of density divided by theoretical density is in the range of 0.95 to 1, preferably in the range of 97 to 1, more preferably in the range of 98 to 1, and even more preferably in the range of 0.99 to 1; a value less than 1.0 is even more preferred; b. The average grain size is in the range of 0.4 µm to 10 µm, preferably in the range of 0.6 µm to 8 µm, more preferably in the range of 0.8 µm to 6.5 µm, even more preferably in the range of 1 µm to 4 µm, even more preferably in the range of 1.1 µm to 3 µm, even more preferably in the range of 1.2 µm to 3 µm, even more preferably in the range of 1.3 µm to 2.5 µm, and even even more preferably in the range of 1.4 µm to 2.2 µm; c. The standard deviation of the average grain size distribution is in the range of 1.2 µm to 2.8 µm. d. A density in the range of 3.9 g / cm³ to 5 g / cm³, more preferably in the range of 4.1 g / cm³ to 4.8 g / cm³, and even more preferably in the range of 4.3 g / cm³ to 4.6 g / cm³.

[0152] This preferred embodiment of the present invention is the 18th embodiment of the laminate, which is preferably attached to any of the 1st to 17th embodiments of the laminate. In the 18th embodiment of the laminate, all possible combinations of features a. to d. are preferred embodiments of this embodiment. These combinations are, for example, a; b; c; d; a+b; a+c; a+d; b+c; b+d; c+d; a+b+c; a+b+d; a+c+d; b+c+d; a+b+c+d; a+b+c+d; a+b+c+d; a+b+c+d.

[0153] In a preferred embodiment of the laminate, the other layer has at least one of the following properties: a. The value of density divided by theoretical density is in the range of 0.95 to 1, preferably in the range of 97 to 1, more preferably in the range of 98 to 1, and even more preferably in the range of 0.99 to 1; a value less than 1.0 is even more preferred; b. An average grain size of 5 µm or less, preferably 4.5 µm or less, more preferably 4 µm or less, even more preferably 3.5 µm or less, even more preferably 3 µm or less, even more preferably 2.5 µm or less, even more preferably 2 µm or less, even more preferably 1.5 µm or less, and even even more preferably 1 µm or less; c. The standard deviation of the average grain size distribution is in the range of 1.2 µm to 2.8 µm, preferably in the range of 1.6 µm to 2.4 µm, and even more preferably in the range of 1.8 µm. d. A density in the range of µm to 2.2 µm; e. A density in the range of 3.9 g / cm3 to 4.8 g / cm3, preferably 4.1 g / cm3 to 4.6 g / cm3, and even more preferably 4.19 g / cm3 to 4.46 g / cm3; f. A density in the range of 3.9 g / cm3 to 4.8 g / cm3, more preferably 4.1 g / cm3 to 4.6 g / cm3, and even more preferably 4.19 g / cm3 to 4.46 g / cm3; g. A density in the range of 3.9 g / cm3 to 4.8 g / cm3, more preferably 4.1 g / cm3 to 4.6 g / cm3, and even more preferably 4.19 g / cm3 to 4.46 g / cm3;

[0154] This preferred embodiment of the present invention is the 19th embodiment of the laminate, which is preferably attached to any of the 8th to 18th embodiments of the laminate. In the 19th embodiment of the laminate, all possible combinations of features a. to e. are preferred embodiments of this embodiment. These combinations are, for example, a; b; c; d; e; a+b; a+c; a+d; a+e; b+c; b+d; b+e; c+d; c+e; d+e; a+b+c; a+b+d; a+b+e; a+c+d; a+c+e; a+d+e; b+c+d; b+c+e; b+d+e; c+d+e; a+b+c+d; a+b+c+e; a+b+d+e; a+c+d+e; b+c+d+e; a+b+c+d+e. In the 19th embodiment of the laminate, the variation of the "density divided by the theoretical density" is preferably applicable to the maximum size of the laminate. In the 19th embodiment of the laminate, feature b., preferably, the average grain size is in the range of 1 µm to 3 µm.

[0155] In a preferred embodiment of the laminate, the laminate has a diameter of at least 200 mm, more preferably at least 300 mm, and more preferably at least 500 mm; the diameter can reach up to 2000 mm or more; the diameter is preferably no greater than 1500 mm, more preferably no greater than 900 mm, even more preferably no greater than 800 mm, further preferably no greater than 700 mm, and even more preferably no greater than 650 mm; the diameter is preferably in the following range: greater than 200 mm to 625 mm; more preferably 300 mm to 625 mm, even more preferably 400 mm to 625 mm, and even more preferably 500 mm to 625 mm.

[0156] This preferred embodiment of the present invention is the 20th embodiment of the laminate, which is preferably attached to any one of the 1st to 19th embodiments of the laminate.

[0157] In a preferred embodiment of the laminate, the first layer and the other layer are in contact with each other and are preferably connected.

[0158] This preferred embodiment of the present invention is the 21st embodiment of the laminate, which is preferably attached to any one of the 1st to 20th embodiments of the laminate.

[0159] In one preferred embodiment of the laminate, the first layer has a thickness of at least 2 mm, more preferably at least 4 mm, more preferably at least 5 mm, and even more preferably at least 8 mm.

[0160] This preferred embodiment of the present invention is the 22nd embodiment of the laminate, which is preferably attached to any one of the 1st to 21st embodiments of the laminate.

[0161] In one preferred embodiment of the laminate, the first layer has a thickness of at least 10 mm, more preferably at least 14 mm, more preferably at least 17 mm, and even more preferably at least 20 mm.

[0162] This preferred embodiment of the present invention is the 23rd embodiment of the laminate, which is preferably attached to any of the 1st to 22nd embodiments of the laminate. In one preferred embodiment of the 23rd embodiment of the laminate, the first layer has a thickness in the range of 10 to 70 mm, more preferably 14 to 50 mm, even more preferably 17 to 40 mm, and further preferably 20 to 30 mm. In one preferred embodiment of the 23rd embodiment of the laminate, the first layer has a thickness in the range of 15 to 70 mm, more preferably 15 to 50 mm, even more preferably 15 to 40 mm, and further preferably 15 to 30 mm. In one preferred embodiment of the 23rd embodiment of the laminate, the first layer has a thickness in the range of 20 to 70 mm, more preferably 20 to 50 mm, even more preferably 20 to 40 mm, and further preferably 20 to 30 mm.

[0163] One embodiment of the present invention comprises an assembly of a multilayer (which in turn comprises a first layer), preferably an assembly of a multilayer according to the present invention, and more preferably an assembly of a multilayer according to any one of the first to 23 embodiments of the multilayer. This embodiment is the first embodiment of the assembly. In a preferred embodiment of the first embodiment of the assembly, the assembly is adapted and configured for the production of components and / or wafers in the semiconductor industry.

[0164] In one preferred embodiment of the assembly, the assembly is selected from the group consisting of: a plasma etcher, a plasma processing chamber (etching or deposition process), a wear-resistant liner for a bearing, a mill liner for a grinder, a dielectric window, an RF window, a focusing ring, a process ring, a deposition ring, a nozzle or gas injector, a spray head, a gas distribution plate, an etching chamber liner, a plasma source adapter, a gas inlet connector, a diffuser, an electrostatic wafer chuck (ESC), a chuck, a wafer, an ion suppressor element, a panel, an isolator, a spacer, a protective ring in the plasma processing chamber, or a combination of at least two of these.

[0165] This preferred embodiment of the present invention is a second embodiment of the assembly, which is preferably attached to the first embodiment of the assembly. In a preferred embodiment of the second embodiment of the assembly, the assembly is a window, cover, chamber top, or combination thereof of a plasma etcher. In this embodiment, it is further preferred that the laminate includes a ZTA layer and a YAG layer.

[0166] An embodiment of the present invention comprises an apparatus having an internal volume defined by the following apparatus portions: i. the inner surface of a first punch of a first punch; ii. the inner surface of a second punch of a second punch; and iii. the inner surface of a die; wherein: a. the first punch and the second punch are adapted and configured to apply a pressure of at least 1 MPa, preferably at least 5 MPa, more preferably at least 10 MPa, and even more preferably at least 15 MPa along a compression axis to a target material in the internal volume, preferably wherein the target material is at least one powder layer, such as the first powder layer; b. the first punch and the second punch are connected to a power source; c. the first punch and the second punch contain at least 50 wt% carbon by total weight of the punches; d. the internal volume has at least 200 mm, preferably at least 300 mm, more preferably at least 400 mm, and even more preferably at least 500 mm. A cross-sectional width W of mm, wherein the cross-sectional width W is perpendicular to the compression axis; wherein the internal volume contains a first powder, wherein the first powder is a mixture of a first component powder and another component powder, wherein the first component powder and the other component powder have different chemical compositions.

[0167] This embodiment is the first embodiment of the device.

[0168] In a preferred embodiment of the device, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to particle size q, such that a. D has a global maximum value α with particle size χα and volume density qα, and b. if D has a local maximum value β with particle size χβ and volume density qβ, then qα / qβ is at least 10, preferably at least 20, more preferably at least 30, and even more preferably at least 50.

[0169] This preferred embodiment of the present invention is a second embodiment of the device, which is more preferably based on the first embodiment of the device.

[0170] In a preferred embodiment of the device, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to volume density q, such that a. D has a global maximum value α with respect to particle size χα and volume density qα, and b. if D has a local maximum value β with respect to particle size χβ and volume density qβ, then qβ is less than 1.00 x 10-3, preferably less than 0.50 x 10-3, more preferably less than 0.10 x 10-3, and even more preferably less than 0.01 x 10-3.

[0171] This preferred embodiment of the present invention is the third embodiment of the device, which is preferably attached to any of the first to second embodiments of the device.

[0172] In a preferred embodiment of the device, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to volume density q, wherein D is unimodal.

[0173] This preferred embodiment of the present invention is the fourth embodiment of the device, which is preferably attached to any one of the first to third embodiments of the device.

[0174] In a preferred embodiment of the device, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to volume density q, wherein D has a global maximum value α with respect to particle size χα and volume density qα, and wherein χα is in the range of 2.7 µm to 7 µm, preferably 3.2 µm to 6 µm, more preferably 3.7 µm to 5.3 µm, and even more preferably 4.2 µm to 4.8 µm.

[0175] This preferred embodiment of the present invention is the fifth embodiment of the device, which is preferably attached to any one of the first to fourth embodiments of the device.

[0176] In a preferred embodiment of the device, the other component powder of the first powder has a particle size distribution D = q(χ) with respect to volume density q, wherein D has a global maximum value α with respect to particle size χα and volume density qα, and wherein qα is in the range of 6.8 to 12, preferably 7.5 to 10.5, more preferably 8.2 to 10, and even more preferably 8.8 to 9.4.

[0177] This preferred embodiment of the present invention is the sixth embodiment of the device, which is preferably attached to any one of the first to fifth embodiments of the device.

[0178] In any of the preferred embodiments of the first to the sixth embodiment of the device, the particle size distribution D = q(χ) of the other component powder is the particle size distribution of the other component powder before the first component powder is mixed with the other component powder to obtain the first powder.

[0179] In a preferred embodiment of the device, the other component powder of the first powder has a specific surface area of ​​less than or equal to 12 m2 / g, more preferably less than or equal to 10 m2 / g, more preferably less than or equal to 9 m2 / g, and even more preferably less than or equal to 8.5 m2 / g.

[0180] This preferred embodiment of the present invention is the seventh embodiment of the device, which is preferably attached to any one of the first to sixth embodiments of the device.

[0181] In a preferred embodiment of the device, the specific surface area of ​​the other component powder of the first powder is in the range of 2.5 m2 / g to 12 m2 / g, more preferably 3 m2 / g to 10 m2 / g, more preferably 3.5 m2 / g to 9 m2 / g, and even more preferably 4 m2 / g to 8.5 m2 / g.

[0182] This preferred embodiment of the present invention is the eighth embodiment of the device, which is preferably attached to any of the first to seventh embodiments of the device. In one particularly preferred embodiment of the eighth embodiment of the device, the specific surface area of ​​the other component powder of the first powder is in the range of 4.2 to 8.3 m2 / g, more preferably 4.5 to 8 m2 / g.

[0183] In a preferred embodiment of the apparatus, the first component powder of the first powder has a particle size distribution E = r(χ) of bulk density r versus particle size χ, wherein E has a global maximum value δ for particle size χδ and bulk density rδ, and wherein at least one or all of the following applies: a. χδ is in the range of 3 to 9 µm, preferably 4.5 to 7.5 µm, more preferably 5 to 6.8 µm, and even more preferably 5.5 to 6.3 µm; b. rδ is in the range of 0.05 to 0.22, preferably 0.08 to 0.18, and more preferably 0.11 to 0.15; c. E is unimodal.

[0184] This preferred embodiment of the invention is the ninth embodiment of the device, which is preferably attached to any of the first to eighth embodiments of the device. In one embodiment of the ninth embodiment of the device, all feasible combinations of features a. to c. are preferred embodiments of this embodiment. These combinations are, for example, a; b; c; a+b; a+c; b+c; a+b+c.

[0185] In one preferred embodiment of the present invention, at least one of the steps of the procedure according to any one of the first to 49 embodiments of the present invention is performed using the apparatus according to any one of the first to 9 embodiments of the present invention.

[0186] One embodiment of the present invention relates to the use of a powder for producing a laminate containing a first layer, the powder being a mixture comprising a first component powder and another component powder, wherein a. the first component powder and the other component powder have different chemical compositions, b. the other component powder has a particle size distribution D = q(χ) of bulk density q to particle size χ, wherein D is unimodal, c. the other component powder has a specific surface area of ​​less than or equal to 12 m² / g, preferably less than or equal to 10 m² / g, more preferably less than or equal to 9 m² / g, and even more preferably less than or equal to 8.5 m² / g.

[0187] This embodiment is a first embodiment of the use of the present invention. In a preferred embodiment of this use, the powder is a first powder. In a preferred embodiment of this use, the laminated system is produced by sintering, more preferably by spark plasma sintering. In a preferred embodiment of this use, the laminate has a diameter of at least 200 mm, more preferably at least 300 mm, even more preferably at least 400 mm, and further preferably at least 500 mm. In this embodiment, the laminate preferably has a diameter in the range of 200 to 650 mm, more preferably 300 to 650 mm, even more preferably 400 to 650 mm, and further preferably 500 to 650 mm. In one preferred embodiment of the first application, the first layer has a thickness ranging from 10 mm to 70 mm, more preferably 14 to 50 mm, even more preferably 17 to 40 mm, and further preferably 20 to 30 mm. In another preferred embodiment of the first application, the first layer has a thickness ranging from 15 to 70 mm, more preferably 15 to 50 mm, even more preferably 15 to 40 mm, and further preferably 15 to 30 mm. In yet another preferred embodiment of the first application, the first layer has a thickness ranging from 20 to 70 mm, more preferably 20 to 50 mm, even more preferably 20 to 40 mm, and further preferably 20 to 30 mm. In a preferred embodiment of the first use, the specific surface area of ​​the other component powder of the first powder is in the range of 2.5 to 12 m² / g, more preferably 3 to 10 m² / g, more preferably 3.5 to 9 m² / g, and even more preferably 4 to 8.5 m² / g. Preferred embodiments and examples of the procedure, as given in, for example, any of embodiments 1 to 49, are also preferred embodiments and examples of the above-described use. For example, a preferred embodiment regarding the particle size distribution D of the other component powder (of the first powder) is also a preferred embodiment of the powder in the first embodiment of the use.

Implementation Method

[0189] Features described as preferred in one category of the invention (e.g., a process) are similarly preferred in embodiments of other categories of the invention (e.g., an apparatus). Preferred embodiments of the invention are: preferred embodiments of a process for producing a laminate, preferred embodiments of a laminate, preferred embodiments of an assembly, preferred embodiments of an application, and preferred embodiments of an apparatus.

[0190] In this document, the disclosure of a scope is preferably understood to include both endpoints of the scope. Furthermore, each disclosure of a scope in the document is preferably understood to also disclose a preferred sub-scope that excludes one endpoint or both endpoints. For example, the disclosure of a scope from X1 to X2 should be understood to disclose a scope that includes both endpoints X1 and X2. Furthermore, it should also be understood to disclose a scope that includes endpoint X1 but excludes endpoint X2, a scope that excludes endpoint X1 but includes endpoint X2, and a scope that excludes both endpoints X1 and X2.

[0191] Some preferred embodiments and preferred models have various combinations of features as alternatives. Where these various combinations are disclosed, such combinations are separated by semicolons (";"). For example, the list of combinations of features for "a; a+b; a+c+d" for preferred embodiments discloses preferred embodiments including feature "a", preferred embodiments including features "a" and "b", and preferred embodiments including features "a", "c", and "d".

[0192] The following abbreviations are used in the description: AC (alternating current), DC (direct current), SPS (spark plasma sintering), RPM (revolutions per minute), YAG (yttrium aluminum garnet), ZTA (zirconia toughened alumina).

[0193] "Spark plasma sintering" is also known as "field-assisted sintering technology" (FAST) and "direct current sintering" (DCS).

[0194] The term "powder" should be understood to refer collectively to both the first powder and the other powder (i.e., the first powder and the other powder are examples of powder). Therefore, the embodiments, preferred embodiments, and preferred states of the powder are respectively embodiments, preferred embodiments, and preferred states of the first powder. Therefore, the embodiments, preferred embodiments, and preferred states of the powder are respectively embodiments, preferred embodiments, and preferred states of the other powder.

[0195] The term "purity" refers to the absence of various impurities in a) starting materials that can form powder (e.g., component powder), b) powder, and c) laminates as disclosed herein. The higher the purity, the closer it is to 100%, the more it indicates that the material is essentially free of impurities and contains only the intended material composition. Preferred intended material compositions include Y, Al, and O.

[0196] The term "impurity" refers to compounds / contaminants present in a) starting materials that can form powders (e.g., component powders), b) powders, and c) laminates as disclosed herein, other than the intended compounds themselves (e.g., component powders, powders, and laminates formed therefrom of magnesium oxide, aluminum oxide, yttrium oxide, and zirconium oxide). Impurities may be present in the starting materials or may be generated by processing (e.g., processing of component powders or powders) or during sintering.

[0197] The term "dopant" refers to a substance added to and / or to a component powder. An impurity differs from a dopant in that, as defined herein, a dopant is a substance intentionally added to a component powder and / or to achieve, for example, certain electrical, mechanical, optical, or other properties (such as grain size modification) in a laminate. As used herein, the term "dopant" does not include powder, provided it can remain in the laminate.

[0198] The term "stabilizing compound" means a substance that is intentionally added to a component powder and / or powder. As defined herein, a stable compound should not be construed as an impurity.

[0199] The term "alumina" should be understood as referring to aluminum oxide, which has the chemical formula Al₂O₃. The term "yttrium oxide" should be understood as referring to yttrium oxide, which has the chemical formula Y₂O₃. The term "zirconia" should be understood as referring to zirconium dioxide, which has the chemical formula ZrO₂.

[0200] The term “calcination” should be understood as referring to the heat treatment of component powders and / or powders in air, which is used to remove moisture and / or impurities, increase crystallinity, and in some cases modify the specific surface area of ​​the powder.

[0201] The term "yttrium aluminum oxide" should be understood to refer to at least one of the crystal phases of yttrium aluminum oxide, including Y3Al5O12 (YAG; yttrium aluminum garnet / cubic phase), YAlO3 (YAP; yttrium aluminum perovskite phase), and Y4Al2O9 (YAM; yttrium aluminum monoclinic phase), and combinations thereof. Preferably, YAG is polycrystalline. Zirconia-toughened alumina (ZTA) should be understood to include at least two separate crystal phases of zirconium oxide and alumina.

[0202] The term “phase” should be understood as referring to the phase, crystal region, part or layer of a laminate with a specific crystal structure.

[0203] The term "layer" should be understood as referring to the thickness of a material, preferably one of several. The material can be, for example, powder or a region in a laminate.

[0204] An example of "target material in internal volume" is one or more powder layers in internal volume. An example of powder layers is a first powder layer and another powder layer.

[0205] The term "layered body" is preferably understood as an integral article formed by applying heat and pressure to one or more powder layers to create a monolithic body. Preferably, the layered body is formed by co-compacting at least two powder layers to create a monolithic body. The term "co-compacting" refers to the process of introducing at least two loose powders into an internal volume to form at least two powder layers, wherein the at least two powder layers are subsequently subjected to heat and pressure. The layered body according to the invention is preferably free of binders, dispersants, and other similar organic substances, as commonly found in the art for forming green bodies or shaped bodies, or with desired features. The layered body can be machined into components that can be used as chamber components in plasma processing applications.

[0206] The term "unitary" should be understood as meaning a single workpiece or a single integrated component that is complete in itself without any additional workpieces; that is, the component is a single workpiece formed as a unit. A unitary component may have more than one layer.

[0207] The term "layered component" refers to a stacked body after a machining step, preferably a machining step that produces the form or shape of a specific component for use in a semiconductor processing chamber.

[0208] The term “annealing” should be understood as the heat treatment of a laminate in air, used for example to reduce stress and / or to standardize stoichiometry.

[0209] The term "ambient temperature" refers to the temperature in the range of 22°C to 25°C. The term "ambient pressure" is better understood as atmospheric pressure.

[0210] As used herein, the term “substantially” is a descriptive term that indicates an approximation and means “considerable in extent” or “largely but not wholly that which is specified”, and is intended to avoid strict numerical boundaries for the specified parameter.

[0211] The terms "approximately" and "about" are allowed a variation of plus or minus 10% when used in conjunction with numbers. Equipment

[0212] The apparatus according to the invention is adapted and configured for producing a laminate from at least one powder layer, preferably by sintering the at least one powder layer, and more preferably by spark plasma sintering. The apparatus according to the invention includes a mold, and preferably includes a first punch and a second punch.

[0213] The device according to the invention is preferably connected to a power source, wherein the power source is preferably a DC power source, and more preferably a rectified DC power source.

[0214] The apparatus according to the invention preferably comprises at least one or all of the following components: a housing, a vacuum device, a hydraulic piston, a foil liner on the inner surface of the mold, and a cooling system adapted and configured to cool the apparatus, preferably during the step of subjecting at least one powder layer to heat and pressure. The apparatus according to the invention preferably comprises a sintering chamber adapted and configured to accommodate an internal volume (i.e., the sintering chamber is adapted and configured to accommodate the mold, the first punch, and the second punch).

[0215] The apparatus according to the invention is preferably adapted and configured to apply an electrical power flux in the range of 0.05 to 1.6 W / mm², more preferably 0.1 to 1.3 W / mm², and even more preferably 0.3 to 1 W / mm² to at least one or all of the following: the mold, the internal volume, the target material in the internal volume, and at least one punch. The electrical power flux is defined as the electrical power input Pw, which is calculated using the formula Pw=Iw*Vw / Aw, where Iw is the current supplied by the power source, Vw is the voltage applied across the mold, the internal volume, or both, and Aw is the surface area on which the voltage is applied.

[0216] The device according to the invention is adapted and configured to apply pressure to a target material in an internal volume, wherein the pressure is preferably applied along a compression axis. Preferably, the angle between the compression axis and the cross-sectional width W of the internal volume is in the range of 88° to 92°, more preferably 89° to 91°, and even more preferably in the range of 89.5° to 90.5°. Internal volume

[0217] The device according to the invention includes an internal volume, wherein the internal volume is at least partially defined by the internal surface of the mold (i.e., the device according to the invention includes a mold). Preferably, the internal volume is defined by the internal surface of the first punch of the first punch, the internal surface of the second punch of the second punch, and the internal surface of the mold (i.e., the device includes a mold and preferably the first punch and the second punch). The internal volume may be defined only by the internal surfaces of the first punch, the second punch, and the mold, or it may be additionally defined by one or more other surfaces. However, more preferably, the internal volume is defined only by the internal surfaces of the first punch, the second punch, and the mold.

[0218] In a preferred embodiment of the invention, the mold is adapted and configured to be removable from the device (i.e., the internal volume is removable from the device). In this embodiment, preferably, the first punch and / or the second punch are also adapted and configured to be removable from the device.

[0219] The internal volume of the present invention is adapted and configured to accommodate at least one powder and / or at least one powder layer. Preferably, the internal volume is cylindrical. In a preferred embodiment of the invention, the cross-sectional width W of the internal volume is at least 300 mm, and more preferably at least 500 mm. The cross-sectional width W can reach a height of 2000 mm or greater. In a preferred embodiment of the invention, the cross-sectional width of the internal volume is not greater than 1500 mm, more preferably not greater than 900 mm, even more preferably not greater than 800 mm, further preferably not greater than 700 mm, and even more preferably not greater than 650 mm. In a preferred embodiment of the invention, the cross-sectional width W of the internal volume is preferably in the range of 200 mm to 650 mm, more preferably in the range of 300 mm to 650 mm, even more preferably in the range of 400 mm to 650 mm, and even more preferably in the range of 500 mm to 650 mm. In a preferred embodiment of the invention, the cross-sectional width is in the range of 550 mm to 625 mm. Mold

[0220] The device according to the invention includes a mold having an internal surface. Preferably, the mold is conductive. If the mold is conductive, it is preferable that the mold has isotropic conductivity.

[0221] The preferred mold contains one or more elements selected from Group 14 of the periodic table. Group 14 elements are sometimes also referred to as Group IVA elements or Group 4A elements. The mold preferably contains one or more elements selected from the group consisting of: C, Si, Ge, Sn, and Pb, more preferably selected from C, Si, Ge, and Sn, and even more preferably selected from C and Si. C-series elements are preferred Group 14 elements. By total weight of the mold, the preferred mold contains at least 50 wt-%, more preferably at least 60 wt-%, even more preferably at least 70 wt-%, even more preferably at least 80 wt-%, even more preferably at least 90 wt-%, and even more preferably at least 95 wt-% of Group 14 elements.

[0222] The preferred mold contains at least 50 wt%, more preferably at least 60 wt%, even more preferably at least 70 wt%, further preferably at least 80 wt%, further preferably at least 90 wt%, further preferably at least 95 wt%, and even more preferably at least 99 wt% carbon, wherein the wt% is based on the total weight of the mold. The preferred mold contains carbon in the form of graphite. The mold is preferably made of carbon material, most preferably graphite.

[0223] The preferred mold has at least one wall, wherein the wall contains at least 50 wt-%, preferably at least 60 wt-%, even more preferably at least 70 wt-%, further preferably at least 80 wt-%, further preferably at least 90 wt-%, further preferably at least 95 wt-%, and even more preferably at least 99 wt-% carbon by the total weight of the mold.

[0224] If the mold contains carbon, it may additionally contain one or more other Group 14 elements, preferably selected from Si, Ge, Sn, and Pb, even more preferably selected from Si, Ge, and Sn, further preferably selected from Si and Ge, and even more preferably Si. In addition to carbon, the other Group 14 elements are also preferably present in the mold, with a total content of at least 0.1 wt% by the total weight of the mold, more preferably at least 1 wt% and even more preferably at least 2 wt%. Elements other than C, Si, Ge, Sn, and Pb may be present in the mold. If elements other than C, Si, Ge, Sn, and Pb are present in the mold, then, by the total weight of the mold, these other elements are preferably present in a total content of no more than 1 wt%, more preferably no more than 0.5 wt%, and even more preferably no more than 0.1 wt%.

[0225] The mold can be a single piece or multiple pieces, preferably a single piece. More preferably, the mold is a single connected body, and even more preferably a single cylindrical body. If the mold has multiple pieces, it is preferable to have 2 to 10 pieces, more preferably 2 to 5 pieces, even more preferably 2 to 3 pieces, and further preferably 2 pieces. Punch

[0226] The apparatus according to the present invention preferably includes a first punch and a second punch. The first punch preferably has an inner surface. The inner surface of the first punch is preferably substantially perpendicular to the inner surface of the mold. The inner surface of the first punch is preferably the lower surface of the first punch. The inner surface of the first punch is preferably substantially horizontal. The inner surface of the first punch is preferably substantially flat. The second punch preferably has an inner surface. The inner surface of the second punch is preferably substantially perpendicular to the inner surface of the mold. The inner surface of the second punch is preferably the upper surface of the second punch. The inner surface of the second punch is preferably substantially horizontal. The inner surface of the second punch is preferably substantially flat. The first punch is preferably disposed above the second punch. The first punch and the second punch are preferably vertically positioned above and below the internal volume, respectively.

[0227] The first and second punches are preferably adapted and configured to apply pressure to the target within the internal volume, and more preferably to generate increased pressure within the internal volume. The first and second punches are preferably adapted and configured to apply pressure along a compression axis. Preferably, the compression axis is substantially perpendicular to the inner surface of the first punch and / or the inner surface of the second punch. The first and / or second punches are preferably adapted and configured to be movable along the compression axis.

[0228] The first and second punches are preferably adapted and configured to apply a pressure of at least 1 MPa, more preferably at least 5 MPa, even more preferably at least 10 MPa, and even more preferably at least 15 MPa to the target in the internal volume. The first and second punches can be adapted and configured to apply a pressure of up to 80 MPa, or even greater. The first and second punches are preferably adapted and configured to apply pressure to the target material in the internal volume, wherein the pressure is in the range of 1 MPa to 100 MPa, more preferably 5 MPa to 60 MPa, even more preferably 5 MPa to 45 MPa, further preferably 5 MPa to 30 MPa, and even more preferably in the range of 5 MPa to 15 MPa; preferably 10 MPa to 60 MPa, more preferably 10 MPa to 45 MPa, even more preferably 10 MPa to 30 MPa, and even more preferably in the range of 10 MPa to 15 MPa; preferably 15 MPa to 60 MPa, more preferably 15 MPa to 45 MPa, even more preferably 15 MPa to 30 MPa, and even more preferably in the range of 15 MPa to 20 MPa.

[0229] The first and second punches are preferably conductive. The first and second punches are preferably adapted and configured to allow a current of at least 5 kA, more preferably at least 10 kA, even more preferably at least 50 kA, and further preferably at least 60 kA across the internal volume. The first and second punches can be adapted and configured to allow a current of up to 100 kA, or even greater.

[0230] The first and second punches are preferably made of carbon material, and most preferably of graphite. By total weight of the punches, the first and second punches preferably contain at least 50 wt%, more preferably at least 60 wt%, even more preferably at least 70 wt%, further preferably at least 80 wt%, further preferably at least 90 wt%, further preferably at least 95 wt%, further preferably at least 99 wt%, and even more preferably at least 99.5 wt% carbon.

[0231] Preferably, the first punch and the other punch have a cross-sectional width equal to or less than the cross-sectional width W of the internal volume. More preferably, the first punch and the other punch have a cross-sectional width smaller than the cross-sectional width W of the internal volume in the range of 10 mm to 200 µm, even more preferably in the range of 30 mm to 150 µm, and even more preferably in the range of 50 mm to 100 µm. Power supply

[0232] The power supply is preferably adapted and configured to generate Joule heating in the powder layer present in the internal volume. The power supply can be adapted and configured to generate alternating current, pulsed direct current, or continuous direct current. Continuous direct current is preferred.

[0233] In a preferred embodiment of the invention, the power supply is a rectified DC power supply. A rectified DC power supply is preferably understood to mean a power source adapted and configured to convert alternating current into direct current. Examples of rectified DC power supplies are those adapted and configured to perform divided-wave rectification, full-wave rectification (e.g., bridge rectifier), or both. Preferred rectified DC power supplies include silicon controlled rectifiers (SCRs), inverters based on insulated-gate bipolar transistors (IGBTs), or both. Here, the IGBT transistor system is preferred over the SCR rectifier.

[0234] In one preferred embodiment of the present invention, the power supply is adapted and configured to be used for one or more of the following: to rectify three-phase AC power into DC power; to rectify single-phase AC power into DC power.

[0235] The power supply is preferably adjusted and configured to provide a current of at least 5 kA, more preferably at least 10 kA, even more preferably at least 50 kA, further preferably at least 60 kA, and even more preferably at least 100 kA. The power supply is preferably adjusted and configured to provide a current in the range of 1 kA to 100 kA, more preferably 5 kA to 90 kA, more preferably 10 kA to 80 kA, even more preferably 15 kA to 70 kA, and even more preferably 20 kA to 60 kA; the power supply can be adjusted and configured to provide a current greater than 100 kA. Type of contact

[0236] If two components of the device are in electrical contact, this should preferably be understood as meaning that current can flow between the two components. If two elements are in physical contact, this should preferably be understood as meaning that the two elements touch each other. Examples of two elements include two components of the device, two powder layers (e.g., the first powder layer and another powder layer) within the internal volume of the device, and two layers of the laminate (e.g., the first layer and another layer). Powder

[0237] If the powder is composed of or contains multiple component powders (e.g., one or two), it is preferable not to mean that the (one or more) component powders contain / do not contain, for example, impurities, stabilizing compounds, sintering aids, and dopants.

[0238] If the powder is a mixture of at least two component powders, it is preferable to mix the component powders before subjecting the powder to heat and pressure in the internal volume. If the powder is a mixture of at least one component powder, it is preferable to understand that at least one of the at least two component powders has a different property. Examples of the at least one property include average particle size, specific surface area, and chemical composition. In one particularly preferred embodiment of the invention, the at least two component powders have different chemical compositions.

[0239] In this invention, the terms "first component powder" and "other component powder" are used to distinguish two component powders from each other in the context of a mixture constituting a particular powder. For example, the first component powder of the first powder and the first component powder of the other powder may or may not have the same chemical composition. For example, the first component powder of the first powder and the other component powder of the other powder may or may not have the same chemical composition. For example, the other component powder of the first powder and the other component powder of the other powder may or may not have the same chemical composition. For example, the other component powder of the first powder and the first component powder of the other powder may or may not have the same chemical composition. The foregoing should also be preferably understood to apply to any powder, including mixtures of another powder and at least two component powders.

[0240] The other powder may consist of a single-component powder. However, more preferably, the other powder is a mixture of at least two component powders.

[0241] In a preferred embodiment of the present invention, the first powder is polycrystalline or crystalline. In a preferred embodiment of the present invention, the other powder is polycrystalline or crystalline. Crystalline powder should preferably be understood as having a single-crystal structure.

[0242] Another powder may be composed of a single-component powder. However, more preferably, the other powder is a mixture of at least three component powders. In a preferred embodiment of the invention, the other powder is a mixture of yttrium oxide powder, alumina powder, and at least one of partially stabilized and stabilized zirconium oxide (preferably partially stabilized zirconium oxide). In this embodiment, relative to the weight of the other powder, it is preferred that the other powder contains 1% to 57% by weight, more preferably 3% to 57% by weight, and even more preferably 5% to 57% by weight of yttrium oxide. In this embodiment, relative to the weight of the other powder, it is preferred that the other powder contains 1% to 40% by weight, more preferably 1% to 30% by weight, even more preferably 3% to 30% by weight, even more preferably 5% to 30% by weight, and even more preferably 5% to 15% by weight of yttrium oxide. In this sample, relative to the weight of the other powder, it is preferable that the other powder contains 43% to 92.5% by weight, and more preferably 65% ​​to 75% by weight of alumina. In this sample, relative to the weight of the other powder, it is preferable that the other powder contains 0.4% to 40% by weight, more preferably 4% to 40% by weight, even more preferably 15% to 40% by weight, and further preferably 15% to 25% by weight of zirconium oxide. For example, relative to the weight of the other powder, the other powder contains 6% by weight of yttrium oxide, 73% by weight of alumina, and 21% by weight of zirconium oxide.

[0243] The preferred zirconia powder may contain a stabilizing compound comprising at least one selected from the group consisting of: yttrium oxide, lanthanum oxide (La₂O₃), cerium oxide, magnesium oxide, samarium oxide (Sm₂O₃), calcium oxide, and combinations thereof. To form partially stabilized zirconia, these stabilizing compounds may each be present in an amount of 0.5 mol-% to 50 mol-%, preferably 0.5 mol-% to 30 mol-%, preferably 0.5 mol-% to 15 mol-%, preferably 0.5 mol-% to 10 mol-%, preferably 1 mol-% to 50 mol-%, preferably 1 mol-% to 30 mol-%, preferably 1 mol-% to 10 mol-%, preferably 1 mol-% to 5 mol-%, and most preferably about 3 mol-%. In order to form stable zirconium oxide, these stabilizing compounds may each be present in an amount greater than 6 mol-% to 45 mol-%, preferably greater than 10 mol-% to 45 mol-%, preferably greater than 25 mol-% to 45 mol-%, preferably greater than 6 mol-% to 30 mol-%, preferably greater than 6 mol-% to about 15 mol-%, preferably greater than 8 mol-% to 15 mol-%.

[0244] Preferably, zirconia is partially or completely stabilized using yttrium oxide. Preferably, the zirconia is partially or completely stabilized by yttrium oxide. The partially stabilized yttrium oxide zirconia may be formed from a powder mixture containing 1 mol-% to 10 mol-% yttrium oxide, preferably 1 mol-% to 8 mol-% yttrium oxide, preferably 1 mol-% to 5 mol-% yttrium oxide, preferably 2 mol-% to 4 mol-% yttrium oxide, and most preferably about 3 mol-% yttrium oxide.

[0245] In a preferred embodiment of the present invention, the first powder and / or the other powder has a specific surface area (SSA) in the range of 1 m² / g to 18 m² / g, more preferably 1 m² / g to 14 m² / g, more preferably 1 m² / g to 10 m² / g, more preferably 1 m² / g to 8 m² / g, more preferably 2 m² / g to 18 m² / g, more preferably 2 m² / g to 14 m² / g, more preferably 2 m² / g to 10 m² / g, more preferably 3 m² / g to 9 m² / g, more preferably 3 m² / g to 6 m² / g.

[0246] The powder may contain at least one metal oxide. The powder may be a metal oxide. Here, the metallic element forming the oxide may be selected from one or more of the following: metalloids, such as boron (B), silicon (Si), germanium (Ge), antimony (Sb), and bismuth (Bi); representative elements, such as magnesium (Mg), calcium (Ca), strontium (Sr), barium (Ba), zinc (Zn), aluminum (Al), indium (In), and tin (Sn); transition metal elements, such as scandium (Sc), yttrium (Y), titanium (Ti), zirconium (Zr), hafnium (Hf), vanadium (M), niobium (Nb), tantalum (Ta), chromium (Cr), molybdenum (Mo), tungsten (W), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), silver (Ag), and gold (Au); and lanthanides, such as lanthanum (La), cerium (Ce), pium (Pr), neodymium (Nd), samarium (Sm), europium (Er), and ilium (Lu). Preferably, the metallic element is selected from one or more of the following elements: Mg, Y, Ti, Zr, Cr, Mn, Fe, Zn, Al, and Er, and more preferably from Y, Al, and Zr.

[0247] In a preferred embodiment of the invention, the powder has a d10 particle size in the range of 0.1 µm to 4 µm, more preferably 0.2 µm to 4 µm, even more preferably 0.3 µm to 4 µm, and further preferably 0.4 µm to 4 µm. In another preferred embodiment of the invention, the powder has a d10 particle size in the range of 0.1 µm to 3 µm, more preferably 0.1 µm to 2 µm, even more preferably 0.1 µm to 3 µm, further preferably 0.1 µm to 2 µm, and even further preferably 0.1 µm to 1 µm. In the preferred embodiment of the invention, at least one or all of the d10 particle sizes mentioned above are applicable after the powder has been heat-treated (e.g., calcined).

[0248] In a preferred embodiment of the present invention, the powder has a d50 particle size in the range of 3 µm to 50 µm, more preferably 3 µm to 40 µm, more preferably 3 µm to 30 µm, even more preferably 3 µm to 20 µm, further preferably 3 µm to 10 µm, and even more preferably 3 µm to 8 µm. In another preferred embodiment of the present invention, the powder has a d50 particle size in the range of 5 µm to 50 µm, more preferably 10 µm to 50 µm, even more preferably 20 µm to 50 µm, and even more preferably 30 µm to 50 µm. In yet another preferred embodiment of the present invention, the powder has a d50 particle size in the range of 5 µm to 10 µm. In a further preferred embodiment of the present invention, the powder has a d50 particle size in the range of 6 µm to 15 µm. In a preferred embodiment of the present invention, at least one or all of the d50 particle sizes mentioned above are used after the powder has been heat-treated (e.g., calcined).

[0249] In a preferred embodiment of the present invention, the powder has a d90 particle size in the range of 10 µm to 350 µm, more preferably 10 µm to 300 µm, more preferably 10 µm to 250 µm, even more preferably 10 µm to 200 µm, further preferably 10 µm to 175 µm, further preferably 10 µm to 150 µm, further preferably 10 µm to 100 µm, further preferably 10 µm to 75 µm, further preferably 10 µm to 50 µm, further preferably 10 µm to 40 µm, and even more preferably 10 µm to 25 µm. In another preferred embodiment of the invention, the powder has a d90 particle size in the range of 20 µm to 350 µm, more preferably 40 µm to 350 µm, even more preferably 60 µm to 350 µm, further preferably 100 µm to 350 µm, even more preferably 150 µm to 350 µm, and even more preferably 200 µm to 350 µm. In yet another preferred embodiment of the invention, the powder has a d90 particle size in the range of 12 µm to 330 µm, more preferably 100 µm to 330 µm, and even more preferably 100 µm to 250 µm. In the preferred embodiment of the invention, at least one or all of the d90 particle sizes mentioned above are applicable after the powder has been heat-treated (e.g., calcined).

[0250] In a preferred embodiment of the present invention, the first powder has a purity of at least 95%, preferably at least 97%, more preferably at least 99%, even more preferably at least 99.99%, further preferably at least 99.999%, and even further preferably at least 99.9999%.

[0251] Any powder that a person skilled in the art would consider suitable for the present invention may be used. Suitable powders are well known and are available from multiple suppliers. Composition of the first powder

[0252] In one embodiment of the present invention, the first powder is a mixture comprising at least two component powders. In a preferred embodiment of the present invention, the first powder is a mixture of yttrium oxide powder and alumina powder. In this embodiment, preferably, the first powder is a stoichiometric mixture of 37.4 mol-% to 37.6 mol-% yttrium oxide and 62.6% mol-% to 62.4% mol-% alumina, and more preferably, 37.5 mol-% yttrium oxide and 62.5 mol-% alumina. By weight, the first powder may be formed from a mixture of 42.9% to 43.4% alumina and 56.6% to 57.1% yttrium oxide. In this embodiment, the first component powder of the first powder is preferably yttrium oxide powder. In this embodiment, the other component powder of the first powder is preferably alumina powder.

[0253] In one preferred embodiment of the present invention, the first component powder of the first powder (e.g., yttrium oxide) has a specific surface area in the range of 0.1 to 8 m2 / g, more preferably 0.5 to 7 m2 / g, even more preferably 1 to 6 m2 / g, and further preferably 1.5 to 4 m2 / g.

[0254] In another preferred embodiment of the present invention, the first powder and / or component powder is YAG powder. In this embodiment, it is preferable that the YAG powder has a d50 particle size in the range of 3 µm to 10 µm, more preferably 4 µm to 9 µm, and even more preferably 5 µm to 8 µm.

[0255] In one preferred embodiment of the present invention, the first component powder of the first powder has a purity of at least 95%, preferably at least 97%, more preferably at least 99%, even more preferably at least 99.99%, further preferably at least 99.999%, and even more preferably at least 99.9999%. In another preferred embodiment of the present invention, the other component powder of the first powder has a purity of at least 95%, preferably at least 97%, more preferably at least 99%, even more preferably at least 99.99%, further preferably at least 99.999%, and even more preferably at least 99.9999%.

[0256] Any component powder deemed suitable for the first powder by those skilled in the art can be used. Suitable component powders are well known and are available from several suppliers. The component powder of the other powder...

[0257] In one preferred embodiment of the present invention, the other powder is a mixture comprising at least two component powders. In one preferred embodiment of the present invention, the other powder is a mixture of alumina powder and at least one of partially stabilized and stabilized zirconia (preferably partially stabilized zirconia). In this embodiment, preferably, the other powder comprises alumina in an amount (by weight) of 60% to 92.5%, and more preferably 75% to 85% relative to the other powder. In this embodiment, preferably, the other powder comprises zirconia in an amount (by weight) of 7.5% to 40%, and more preferably 15% to 25% relative to the other powder. For example, the other powder is a mixture of 77% alumina and 23% zirconia. In this embodiment, the first component powder of the other powder is preferably zirconia powder, and more preferably comprises at least one or all of the following: partially stabilized zirconia and stabilized zirconia, wherein partially stabilized zirconia is more preferred. In this sample, the other component powder of the other powder is preferably alumina powder.

[0258] In one preferred embodiment of the present invention, the first component powder of the other powder (e.g., zirconium oxide) has a specific surface area in the range of 1 to 16 m2 / g, more preferably 2 to 14 m2 / g, even more preferably 4 to 12 m2 / g, and further preferably 6 to 10 m2 / g.

[0259] In one preferred embodiment of the present invention, another component powder of another powder (e.g., alumina) has a specific surface area in the range of 1 to 16 m2 / g, more preferably 2 to 14 m2 / g, even more preferably 4 to 12 m2 / g, and further preferably 6 to 10 m2 / g.

[0260] If the other powder contains at least two component powders, any component powder that a person skilled in the art would consider suitable for the present invention may be used. Suitable component powders are well known and are available from several suppliers. Particle size distribution of component powders

[0261] According to one embodiment of the present invention, another component powder of the first powder has a particle size distribution D = q(χ) with respect to bulk density q. Here, bulk density q should be understood as the fractional volume (expressed as a percentage) of the total cumulative volume of the other component powder containing particles with particle size χ. Therefore, integrating with respect to all particle sizes χ with respect to q yields the total cumulative volume of the other component powder (i.e., 100%). As provided above, the definition of q also applies to the particle size distribution of the powder and any other component powder.

[0262] Preferably, the global maximum and local maximum of the particle size distribution (PSD) should not be interpreted as noise in the PSD. In this invention, the global maximum should not be interpreted as an instance of a local maximum.

[0263] The local maximum value of PSD should preferably be understood as the peak value of the particle size distribution. A unimodal PSD should preferably be understood as having a single peak value. A multimodal PSD should preferably be understood as having more than one peak value. Examples of multimodal PSD include bimodal PSD and trimodal PSD. A bimodal PSD should preferably be understood as having two peak values. A trimodal PSD should preferably be understood as having three peak values. The peak values ​​of a multimodal PSD do not need to have the same q value. Heat treatment of powder

[0264] In one embodiment of the invention, it is preferable to subject at least one powder and / or at least one component powder used in the process for producing the laminate to heat treatment (here, the at least one powder is, for example, a first powder and another powder; here, the at least one component powder is, for example, a first component powder of a first powder, another component powder of a first powder, a first component powder of another powder, and another component powder of another powder). In this embodiment, it is preferable to subject the at least one powder to heat and pressure within the internal volume of the apparatus. In this embodiment, it is preferable to subject the at least one powder to heat treatment before introducing it into the internal volume of the apparatus. In a preferred embodiment of the invention, the at least one component powder is heat treated before mixing the component powder to form a powder.

[0265] The preferred heat treatment of the powder is calcination of the powder. The preferred heat treatment of the component powder is calcination of the component powder.

[0266] Heat treatment of powders and / or component powders is preferably performed in an oxygen-containing environment at ambient pressure, although other pressures and calcination environments may be used. The preferred oxygen-containing environment is an ambient atmosphere.

[0267] The heat treatment of powders and / or component powders is preferably performed at a temperature in the range of 600°C to 1100°C, more preferably at 600°C to 1000°C, and even more preferably at a temperature in the range of 600°C to 900°C. The heat treatment of powders and / or component powders is preferably performed at a temperature in the range of 700°C to 1100°C, more preferably at 800°C to 1100°C, even more preferably at 800°C to 1000°C, and even more preferably at a temperature in the range of 850°C to 950°C.

[0268] The heat treatment of powders and / or component powders preferably has a duration of 4 to 12 hours, more preferably 4 to 10 hours, even more preferably 4 to 8 hours, and further preferably 4 to 6 hours. Alternatively, the heat treatment of powders and / or component powders preferably has a duration of 6 to 12 hours.

[0269] Heat treatment of powders and / or component powders is preferably performed in a container (e.g., a crucible and a kiln) containing a first cavity. Any container that a person skilled in the art would consider suitable may be used for heat treatment of powders and / or component powders. Such containers are well known to those skilled in the art. An example of a suitable container is the VIK283 kiln, which is available from Paragon Industries, LP (Mesquite, Texas, USA). Mixing and grinding

[0270] If the powder (e.g., a first powder and another powder) is a mixture of at least two component powders (e.g., a first component powder and another component powder), the mixing of the at least two component powders can be performed using at least one or all of the following: wet ball milling, dry ball milling, wet tumbling mixing, dry tumbling mixing, jet milling, or a combination of at least two thereof. Preferred ball milling uses rotation about an axis to mix the at least two component powders. Preferred tumbling mixing uses tumbling rotation or vertical rotation to mix the at least two component powders. The at least two component powders are mixed in a volumetric section (such as a container or barrel).

[0271] Ball milling (dry ball milling, wet ball milling) and / or rotary mixing (dry rotary mixing, wet rotary mixing) preferably uses high-purity (>99.99%) alumina media (the media are also referred to as stirring elements herein). In other cases where agglomeration may be a concern, harder media, such as zirconium oxide, are preferred. The media loading for ball milling and / or rotary mixing may vary from a large-size (about 30 mm) media element to about 50% (by powder weight) of the media loading.

[0272] Dry ball milling and / or dry rolling mixing is preferably performed for a duration ranging from 12 hours to 48 hours, more preferably from 16 hours to 48 hours, and even more preferably from 24 hours to 48 hours. Dry ball milling and / or dry rolling mixing is preferably performed in a volumetric section that rotates at a rate ranging from 50 RPM to 200 RPM, more preferably from 75 RPM to 150 RPM, and even more preferably from 100 RPM to 125 RPM.

[0273] Wet ball milling and / or wet rotary mixing are preferably performed by suspending the powders of at least two components in at least one solvent and / or water to form a slurry. Preferred solvents are alcohols, such as ethanol and methanol. Ethanol is particularly preferred. The slurry can be formed to have a powder loading of preferably 5% to 50% by weight of the powder, more preferably 10% to 40% by weight of the powder, and even more preferably 20% to 40% by weight of the powder during milling and / or mixing. When wet ball milling and / or wet rotary mixing are used, any amount of commercially available dispersants (such as polymethyl methacrylate (PMMA) and polyvinylpyrrolidone (PVP)) can optionally be added to the slurry. Optionally, a dispersant amount from zero (no dispersant) to 0.2% by weight of the powder, and optionally from 0 to 0.1% by weight of the powder, can be added. The media loading can vary from no media used during wet ball milling to 50% by weight of powder and higher, more preferably from 40% by weight to 90% by weight of powder, and even more preferably from 50% by weight to 80% by weight of powder. Wet ball milling and / or wet rolling mixing are preferably performed for a duration of 8 to 48 hours, more preferably 12 to 48 hours, and even more preferably 16 to 48 hours. Wet ball milling and / or wet rolling mixing are preferably performed for a duration of 8 to 36 hours, more preferably 8 to 24 hours, and even more preferably 8 to 12 hours. Wet ball milling is preferably performed in a volumetric section that rotates at a rate ranging from 50 to 200 RPM, more preferably from 75 to 150 RPM, and even more preferably from 100 to 125 RPM. RPM values ​​are preferably used for volume sections with a diameter of up to 200 mm. Wet rolling mixing is preferably performed at RPMs of 10 to 30, and more preferably 15 to 25.

[0274] Jet milling processes known to those skilled in the art can also be used to mix the at least two component powders to form a powder. Jet milling uses a high-speed jet of inert gas and / or air to collide with the particles of the at least two component powders without the use of grinding or mixing media. The volume section can be designed so that larger particles can preferentially reduce their size, which can provide a narrow particle size distribution in the powder. Preferably, the powder leaves the volume section when it reaches the desired particle size determined at the time of setting the jet mill before mixing.

[0275] The at least two component powders and / or powders may be subjected to jet milling at a pressure of about 100 psi, whether alone or in combination with any or all of the powder milling and / or mixing procedures disclosed herein. After jet milling, the powders may optionally be sieved using any number of sieves (which may have openings of, for example, 45 μm to 400 μm) and / or blended, without limitation on repetition or sequence.

[0276] Any apparatus deemed suitable for mixing and / or grinding by those skilled in the art may be used. Such apparatus is well known. One example is a wet rotary mixer, such as the Model 309-E3, 55-gallon drum mixer from Morse Manufacturing Company, Inc. (Syracuse, New York, USA). Powder is introduced into the internal volume.

[0277] In a preferred embodiment of the invention, when powder is introduced into the internal volume, the powder is introduced simultaneously with the removal of the internal volume from the apparatus (i.e., removal of the mold, the first punch, and the second punch from the apparatus). Here, "removed" is preferably understood to mean that the internal volume is located outside the apparatus, for example, outside the sintering chamber of the apparatus. In one preferred embodiment of the invention, after the powder is introduced into the internal volume, the powder is spread to form a powder layer. In another preferred embodiment of the invention, when one or more, more preferably all, powder layers are present in the internal volume, the internal volume is placed in the apparatus, and more preferably in the sintering chamber of the apparatus (i.e., the mold, the first punch, and the second punch are placed in the sintering chamber of the apparatus). Powder layer

[0278] In one preferred embodiment of the present invention, the first powder and the first powder layer preferably have the same chemical composition. In one preferred embodiment of the present invention, the first powder layer comprises at least 75 wt-%, more preferably at least 85 wt-%, even more preferably at least 95 wt-%, and further preferably at least 99 wt-%, of the first powder, wherein wt-% is based on the total weight of the first powder layer. In one preferred embodiment of the present invention, the first powder layer is composed of the first powder.

[0279] In one preferred embodiment of the present invention, the other powder and the other powder layer preferably have the same chemical composition. In one preferred embodiment of the present invention, the other powder layer comprises at least 75 wt-%, more preferably at least 85 wt-%, even more preferably at least 95 wt-%, and further preferably at least 99 wt-%, of the other powder, wherein wt-% is based on the total weight of the other powder layer. In one preferred embodiment of the present invention, the other powder layer is composed of another powder, oxide A and oxide B.

[0280] The terms "oxide A" and "oxide B" are used to distinguish these oxides from each other and to indicate an oxide having one or more of the properties described below.

[0281] Oxide A comprises at least 1 mol-% of a Group 3 (formerly Group IIIB) element (preferably yttrium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is based on oxygen in oxide A. Preferably, oxide A is the cubic phase of yttrium aluminum oxide, more preferably YAG. In one preferred embodiment of the invention, oxide A comprises at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-% of a Group 3 (formerly Group IIIB) element. In one preferred embodiment of the invention, oxide A comprises at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-% of a Group 13 (formerly Group IIIA) element. Particularly preferred is that, as used herein, the first oxide is oxide A.

[0282] Oxide B comprises at least 1 mol-% of a Group 4 (formerly Group IVB) element (preferably zirconium) and at least 1 mol-% of a Group 13 (formerly Group IIIA) element (preferably aluminum), wherein the mol-% is based on oxygen in oxide B. Preferably, oxide B is ZTA. In one preferred embodiment of the invention, oxide B comprises at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-% of a Group 4 (formerly Group IVB) element. In one preferred embodiment of the invention, oxide B comprises at least 3 mol-%, more preferably at least 5 mol-%, and even more preferably at least 7 mol-% of a Group 13 (formerly Group IIIA) element. Particularly preferred is another oxide system, as used herein, oxide B. Procedure for producing laminates.

[0283] This invention relates to a process for producing laminates. In this embodiment, a preferred process is a sintering process, more preferably a spark plasma sintering process. The preferred spark plasma sintering process produces laminates by applying heat and pressure to at least one powder layer. The heat is preferably obtained by using an electric current.

[0284] A preferred process for producing laminates increases the density of the at least one powder layer to produce laminates.

[0285] A preferred process for producing multilayers may employ dopants. As used herein, the term "dopant" refers to a substance added to powders and / or multilayers to produce desired properties (e.g., altered electrical properties) in the multilayers. If one or more dopants are used, it is preferred that the powders and / or multilayers contain the one or more dopants in amounts ranging from 0.002 wt% to < 0.05 wt%, more preferably from 0.0035 wt% to 0.02 wt%, and even more preferably from 0.0075 wt% to 0.01 wt%. Examples of dopants include Sc, La, Er, Ce, Cr, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Tm, Yb, Lu, Zr, and oxides and combinations thereof.

[0286] A preferred process for producing laminates does not employ sintering aids. As used herein, the term "sintering aid" refers to compounds such as silicon dioxide (SiO2), lithium oxide (Li2O), lithium fluoride (LiF), magnesium oxide (MgO), and / or calcium oxide (CaO), which are added to the powder during the process for producing laminates to enhance densification and thereby reduce porosity. If sintering aids are used, it is preferable that the powder contains 5 ppm or less, and more preferably 2 ppm or less of the sintering aid. Application of heat and pressure

[0287] In this embodiment of the invention, the step of subjecting the first powder layer in the internal volume and / or any other powder layer present in the internal volume to heat and pressure results in a laminated body. Preferably, it should be understood that the laminated body typically begins to form before the step of subjecting the first powder layer to heat and pressure is completed (e.g., a partially formed or formed laminated body may be present in the internal volume during the step of subjecting the first powder layer to heat and pressure). Therefore, the step of subjecting the first powder layer to heat and pressure preferably further includes subjecting at least one or all of the following to heat and pressure: a partially formed laminated body (in the internal volume), a formed laminated body (in the internal volume). The step of subjecting the first powder layer to heat and pressure is preferably terminated by removing the voltage applied across the mold, the internal volume, or both.

[0288] During the step of applying heat and pressure to the first powder layer and / or any other powder layer present in the internal volume, the order of applying heat and pressure may vary to obtain the desired pressure and temperature for producing the laminate, as disclosed herein. In one embodiment of the invention, it is preferred that pressure is applied to obtain the desired pressure for producing the laminate, and then heat is applied to obtain the desired temperature for producing the laminate. In another embodiment of the invention, it is preferred that heat is applied to obtain the desired temperature for producing the laminate, and then pressure is applied to obtain the desired pressure for producing the laminate. In yet another embodiment of the invention, it is preferred that heat and pressure are applied at least partially simultaneously, and more preferably simultaneously, to obtain the desired temperature and pressure for producing the laminate. In yet another preferred embodiment of the invention, the step of applying heat and pressure may comprise at least two sub-steps, wherein the at least two sub-steps are distinguished from each other by a change in the temperature of the applied heat and / or pressure.

[0289] In one embodiment of the present invention, it is preferred that the first powder layer in the internal volume and any other powder layers present in the internal volume are heated by means of a mold, or a punch, or both. In this embodiment, it is preferred that the heating is performed by means of a mold and a punch.

[0290] Applying heat and pressure to the powder layer results in the formation of a laminate. For example, applying heat and pressure to a first powder layer and another powder layer results in the formation of a first layer and another layer of the laminate, respectively.

[0291] In a preferred embodiment of the present invention, the step of applying heat and pressure is performed for a duration of 4 to 20 hours, more preferably 6 to 16 hours, more preferably 8 to 14 hours, and even more preferably 10 to 12 hours.

[0292] In one preferred embodiment of the present invention, during the step of applying heat and pressure, the maximum temperature and pressure are applied for a duration of 0.5 minutes to 180 minutes, more preferably 0.5 minutes to 120 minutes, even more preferably 0.5 minutes to 100 minutes, further preferably 0.5 minutes to 80 minutes, further preferably 0.5 minutes to 60 minutes, further preferably 0.5 minutes to 40 minutes, further preferably 0.5 minutes to 20 minutes, further preferably 0.5 minutes to 10 minutes, and even more preferably 0.5 minutes to 5 minutes. In one preferred embodiment of the invention, during the step of applying heat and pressure, the maximum temperature and pressure are applied for a duration of 5 minutes to 120 minutes, more preferably 10 minutes to 120 minutes, even more preferably 20 minutes to 120 minutes, further preferably 40 minutes to 120 minutes, even more preferably 60 minutes to 120 minutes, and even more preferably 100 minutes to 120 minutes. In another preferred embodiment of the invention, during the step of applying heat and pressure, the maximum temperature and pressure are applied for a duration of 30 minutes to 90 minutes.

[0293] In a preferred embodiment of the present invention, during the step of subjecting the first powder layer and / or any other powder layer present in the internal volume to heat and pressure, the maximum temperature in the internal volume is between 900°C and 2000°C, preferably between 950°C and 1900°C, more preferably between 1000°C and 1800°C, and even more preferably between 1050°C and 1700°C; preferably between 1000°C and 1700°C, more preferably between 1100°C and 1700°C, even more preferably between 1200°C and 1700°C, even more preferably between 1300°C and 1700°C, and even even more preferably between 1400°C and 1700°C.

[0294] In the preferred embodiment S1 of the present invention, the step of applying heat and temperature to the first powder layer and / or any other powder layer present in the internal volume comprises a first sub-step SRAMP and another sub-step SSINT. In this embodiment S1, preferably, during the first sub-step SRAMP, the temperature in the internal volume increases at a rate in the range of 1°C / min to 100°C / min, more preferably 2°C / min to 50°C / min, even more preferably 3°C / min to 25°C / min, further preferably 3°C / min to 10°C / min, and even more preferably 5°C / min to 10°C / min. In this embodiment S1, preferably, the maximum temperature during the first sub-step SRAMP is in the range of 900°C to 1300°C. In this sample S1, preferably, during the other sub-step SSINT, the temperature in the internal volume increases at a rate ranging from 0.5°C / min to 5°C / min, more preferably from 1°C / min to 4°C / min, and even more preferably from 1.5°C / min to 3°C / min. In this sample S1, preferably, during the other sub-step SSINT, the maximum temperature in the internal volume is in the range of 1100°C to 2000°C, more preferably from 1300°C to 1850°C, more preferably from 1450°C to 1750°C, and even more preferably from 1575°C to 1675°C. In this state S1, preferably, during the other sub-step SSINT, the pressure in the internal volume increases at a rate ranging from 0.5 MPa / min to 30 MPa / min, more preferably from 0.75 MPa / min to 10 MPa / min, and even more preferably from 1 MPa / min to 5 MPa / min. Cooling of the laminate.

[0295] In a preferred embodiment C1, the process for producing the laminate includes the following steps: once the laminate has been obtained, the temperature of the laminate is reduced. In one preferred embodiment C1, the laminate system is passively cooled by removing a heat source (e.g., by removing the application of voltage across the mold, internal volume, or both; by removing the power applied to the apparatus used to produce the laminate). In another embodiment C1, the laminate is cooled under inert gas convection (e.g., under argon or nitrogen at 1 bar). Other gas pressures greater than or less than 1 bar may also be used. In another embodiment C1, the laminate is cooled under forced convection conditions in an oxygen environment.

[0296] In a preferred embodiment of Example C1, the pressure applied to the internal volume is also reduced during the step of reducing the temperature of the laminate (e.g., the pressure applied by the first and second punches is removed). In a preferred embodiment of Example C1, the temperature of the laminate can be reduced under vacuum conditions.

[0297] The temperature of the laminate can be decreased at a rate within the following ranges: preferably 0.5 °C / min to 20 °C / min, more preferably 1 °C / min to 10 °C / min, even more preferably 1 °C / min to 8 °C / min, further preferably 1 °C / min to 5 °C / min; preferably 2 °C / min to 10 °C / min, more preferably 2 °C / min to 8 °C / min, and further preferably 2 °C / min to 5 °C / min. Further variations of this process...

[0298] In one preferred embodiment V1 of the present invention, the process for producing the laminate further includes a step of reducing the gas pressure in the internal volume, wherein the reducing step is preferably performed after the first powder is introduced into the internal volume and / or after any other existing powder layer is introduced into the internal volume.

[0299] In state V1, preferably, the gas pressure is reduced before subjecting the first powder layer and / or any other powder layer present in the internal volume to heat and pressure. In state V1, preferably, the gas pressure is reduced to 10 mPa or less, more preferably to 5 mPa or less, and even more preferably to 1 mPa or less. Preferably, the gas pressure is reduced to the range of 1 mPa to 10 mPa.

[0300] In a preferred embodiment V1 of the present invention, the process for producing the laminate is performed in at least one or all of the following: a non-oxidizing atmosphere; an inert atmosphere; and more preferably an atmosphere containing argon. Laminated body

[0301] The laminate according to the present invention comprises at least a first layer. This should not be construed as meaning that the laminate must comprise more than one layer, that is, it should not be construed as meaning that the laminate comprises one or more other layers besides the first layer. The laminate may consist of only the first layer. However, more preferably, the laminate has at least a first layer and another layer. If the laminate comprises a first layer and another layer, it is more preferably that the first layer and the other layer are in contact with each other.

[0302] According to the procedure of the present invention, a laminate is produced, wherein the laminate system is obtained by heating and pressurizing at least one powder layer within the internal volume of the apparatus. For example, the first layer of the laminate is obtained by heating and pressurizing a first powder layer within the internal volume of the apparatus. Preferably, the first layer of the laminate is obtained from the first powder layer. If the laminate has another layer, it is preferable that the other layer is obtained from another powder layer.

[0303] The preferred laminate has a higher density than the at least one powder layer. The preferred laminate has at least 95% of its theoretical density, more preferably at least 99%, and even more preferably at least 99.9%. The preferred laminate system is associated with the following items.

[0304] The preferred laminate comprises at least one element selected from the group consisting of: oxygen, nitrogen, carbon, yttrium, zirconium, aluminum, titanium, silicon, boron, phosphorus, and beryllium. These elements may be components of oxides, nitrides, or carbides.

[0305] If the laminate contains oxygen, the content of the simple oxides required to prepare it is often quantified. Some preferred oxide compositions are silicon dioxide, boron oxide, beryllium oxide, yttrium oxide, aluminum oxide, zirconium oxide, titanium oxide, silica, quartz, calcium oxide, cerium oxide, nickel oxide, copper oxide, strontium oxide, scandium oxide, samarium oxide, hafnium oxide, vanadium oxide, niobium oxide, tungsten oxide, manganese oxide, tantalum oxide, tantalum oxide, thallium oxide, europium oxide, neodymium oxide, yttrium aluminate oxide, zirconium aluminate oxide, lanthanum oxide, diurnal oxide, and erbium oxide.

[0306] If the laminate contains nitrogen, the content of the simple nitride required to prepare it is usually quantified. Some preferred nitride components are selected from one or more of the following groups: silicon nitride, titanium nitride, yttrium nitride, aluminum nitride, boron nitride, beryllium nitride, and tungsten nitride.

[0307] If the laminate contains carbon, the content of the simple carbide required to prepare it is often quantified. Some preferred carbide compositions are silicon carbide, tungsten carbide, chromium carbide, vanadium carbide, niobium carbide, molybdenum carbide, tantalum carbide, titanium carbide, zirconium carbide, hafnium carbide, and boron carbide.

[0308] The laminate may contain one or more borides. Some preferred boride compositions of the laminate are selected from one or more of the following groups: molybdenum boride, chromium boride, hafnium boride, zirconium boride, tantalum boride, titanium boride, and titanium diboride.

[0309] The preferred stacked body comprises one or more species selected from the group consisting of: sapphire, aluminum oxide, yttrium aluminum monoclinic (YAM) (preferably Y4Al2O9), yttrium aluminum garnet (YAG) (preferably Y3Al5O12), yttrium aluminum perovskite (YAP) (preferably YAlO3), lapis lazuli, aluminum-rich andalusite, magnesium aluminate spinel, zirconium oxide, erbium aluminum garnet (EAG), yttrium oxynitride, silicon oxynitride, magnesium silicate, aluminum nitride, and silicon carbide.

[0310] In one preferred embodiment A1 of the present invention, the first layer of the laminate contains YAG, more preferably at least 90 vol-%, even more preferably at least 95 vol-%, and even more preferably at least 99 vol-%, of YAG, wherein the vol-% is based on the volume of the first layer. In this sample A1, it is preferable that the first layer contains an amount of YAG in the range of 90 vol-% to 99.9 vol-%, more preferably 90 vol-% to 99.8 vol-%, even more preferably 90 vol-% to 99.8 vol-%, further preferably 90 vol-% to 99.8 vol-%, further preferably 93 vol-% to 99.8 vol-%, further preferably 93 vol-% to 99.7 vol-%, and even more preferably 93 vol-% to 99.6 vol-%, wherein the vol-% is based on the volume of the first layer.

[0311] In one preferred embodiment A2 of the present invention, the laminate comprises a first layer and another layer. In this embodiment A2, preferably, the first layer comprises YAG, more preferably as described in the aforementioned embodiment A1. In embodiment A2, preferably, the other layer comprises at least 90 vol-%, even more preferably at least 95 vol-%, and even more preferably at least 99 vol-%, of ZTA, wherein the vol-% is based on the volume of the other layer.

[0312] In another preferred embodiment A3 of the present invention, the first layer comprises aluminum nitride. In yet another preferred embodiment A4 of the present invention, the first layer comprises silicon carbide. In one or both of embodiments A3 and A4, preferably, the laminate comprises a first layer and another layer, wherein the other layer comprises ZTA, more preferably as described in embodiment A2 above.

[0313] Preferred laminated ceramic bodies. Preferred ceramic inorganic materials. Preferred ceramic nonmetals. Some preferred ceramic oxides, nitrides, carbides, or combinations thereof. Preferred ceramic refractory materials.

[0314] Preferred oxide ceramics may be single-element oxides or mixed oxides of more than one element. Oxide ceramics may contain some nitride or carbide contents, or both. Oxide ceramics may be free of nitrides or carbides, or both. Preferred oxide ceramics may be stoichiometric or non-stoichiometric. Stoichiometric oxides preferably have an integer ratio between the atomic numbers of their component elements. Oxide ceramics may contain two or more elemental groups, each element being stoichiometric with other elements in its own group, but non-stoichiometric with members of other groups.

[0315] Some preferred mixed oxide systems are selected from one or more of the following groups: zirconium silicate oxide, hafnium aluminate oxide, hafnium silicate oxide, titanium silicate oxide, lanthanum silicate oxide, lanthanum aluminate oxide (LAO), yttrium silicate oxide, titanium silicate oxide, tantalum silicate oxide, nitrogen oxides, barium titanate, lead titanate, and lead zirconate titanate.

[0316] Nitrogen-containing ceramics are often quantified by the content of the simple nitrides required for their preparation. Some preferred nitride compositions are selected from one or more of the following groups: silicon nitride, titanium nitride, yttrium nitride, aluminum nitride, boron nitride, beryllium nitride, and tungsten nitride.

[0317] Preferred nitride ceramics may be single-element nitrides or mixed nitrides of more than one element. Nitride ceramics may contain some oxide or carbide content, or both. Nitride ceramics may be free of oxides or carbides, or both. Preferred nitride ceramics may be stoichiometric or non-stoichiometric. Stoichiometric nitrides preferably have an integer ratio between the atomic numbers of their component elements. Nitride ceramics may contain two or more elemental groups, each element being stoichiometric to other elements in its own group, but non-stoichiometric to members of other groups.

[0318] Preferred carbide ceramics may be single-element carbides or mixed carbides of more than one element. Carbide ceramics may contain some oxide or nitride contents, or both. Carbide ceramics may be free of oxides or nitrides, or both. Preferred carbide ceramics may be stoichiometric or non-stoichiometric. Stoichiometric carbides preferably have an integer ratio between the atomic numbers of their component elements. Carbide ceramics may contain two or more elemental groups, each element being stoichiometric with other elements in its own group, but non-stoichiometric with members of other groups.

[0319] Preferably, the laminate has a size of at least 200 mm, more preferably at least 300 mm, and even more preferably at least 500 mm. The size of the laminate may reach up to 2000 mm or more. In one preferred embodiment of the invention, the size of the laminate is no greater than 1500 mm, more preferably no greater than 900 mm, even more preferably no greater than 800 mm, even more preferably no greater than 700 mm, and even even more preferably no greater than 650 mm. In one preferred embodiment of the invention, the size of the laminate is preferably in the range of 200 mm to 650 mm, more preferably in the range of 300 mm to 650 mm, even more preferably in the range of 400 mm to 650 mm, and even more preferably in the range of 500 mm to 650 mm. In one preferred embodiment of the invention, the size of the laminate is in the range of 550 mm to 625 mm. In the above preferred embodiment, the size of the laminate should be understood as the maximum size of the laminate (e.g., diameter).

[0320] In one preferred embodiment of the present invention, the first layer is polycrystalline or crystalline. In another preferred embodiment of the present invention, if the laminate includes another layer, it is preferably that the other layer is polycrystalline or crystalline. A crystalline layer is preferably understood to have a single-crystal structure.

[0321] The laminate according to the present invention is preferably used in a plasma processing chamber. Heat treatment of the laminate.

[0322] In this embodiment of the invention, it is preferable to subject the laminate to heat treatment. A preferred heat treatment of the laminate is annealing. A laminate that has undergone heat treatment may be referred to as a treated laminate. A laminate that has undergone annealing may be referred to as an annealed laminate.

[0323] In a preferred embodiment of the present invention, the heat treatment of the laminate is performed at a temperature in the range of 900°C to 1800°C, more preferably 1000°C to 1700°C, more preferably 1100°C to 1600°C, even more preferably 1200°C to 1500°C, further preferably 1300°C to 1475°C, and even more preferably 1350°C to 1450°C.

[0324] In a preferred embodiment of the present invention, the heat treatment of the laminate is performed at a heating and / or cooling rate in the range of 0.05°C / min to 50°C / min, more preferably 0.1°C / min to 25°C / min, even more preferably 0.3°C / min to 10°C / min, and further preferably 0.5°C / min to 5°C / min. In a preferred embodiment of the present invention, the heat treatment of the laminate is performed at a cooling rate in the range of 1°C / min to 50°C / min, more preferably 3°C / min to 50°C / min, even more preferably 5°C / min to 50°C / min, and further preferably 25°C / min to 50°C / min. In a preferred embodiment of the present invention, the heat treatment of the laminate is performed at a heating rate in the range of 0.05°C / min to 10°C / min, more preferably 0.1°C / min to 5°C / min, even more preferably 0.3°C / min to 2°C / min, and even more preferably 0.5°C / min to 1°C / min.

[0325] In a preferred embodiment of the present invention, the heat treatment of the laminate is performed for a duration of 1 hour to 24 hours, more preferably 1 hour to 18 hours, even more preferably 1 hour to 16 hours, and further preferably 1 hour to 8 hours. The heat treatment of the laminate is performed for a duration of 4 hours to 24 hours, more preferably 8 hours to 24 hours, and even more preferably 12 hours to 24 hours. The heat treatment of the laminate is performed for a duration of 4 hours to 12 hours, and more preferably 6 hours to 10 hours.

[0326] The heat treatment of the laminated body is preferably performed under conditions such as forced convection or oxidation in air. The heat treatment of the laminated body is preferably performed under ambient pressure.

[0327] The heat treatment of the laminate can be performed while it is within the internal volume of the device. Alternatively, the heat treatment of the laminate can be performed outside the internal volume of the device. For example, the laminate can be removed from the internal volume of the device and placed in another cavity, where the laminate is subjected to heat treatment in the other cavity.

[0328] Another example of a cavity is a furnace cavity. Any furnace that a person skilled in the art deems suitable for the heat treatment of laminates can be used. Such furnaces are well known to those skilled in the art. One example is the STD-1200-17 industrial box furnace, which is available from JinYu Electric Material Co., Ltd. (Dengfeng City, China). Applications of Laminated Bodies

[0329] In a preferred embodiment, the laminate disclosed herein can be machined into a process ring. Examples of process rings include insertion rings, focusing rings, venting rings, capping rings, deposition rings, etching rings, shielding rings, carrier rings, or substrate picking rings, which are components of a plasma vacuum processing chamber. Each process ring comprises: an annular body, wherein the body preferably comprises 90% to 99.8% by volume of polycrystalline yttrium aluminum garnet, wherein the annular body has at least one surface having a surface area; and an opening surrounded by the annular body. Preferably, the polycrystalline yttrium aluminum garnet comprises pores on the at least one surface having a pore size of no more than 5 µm, and preferably having a maximum pore size of 1.5 µm for at least 95% of the pores.

[0330] In another preferred embodiment, the laminate disclosed herein can be machined into a "spray head" gas flow manifold, also known as a spray head assembly or gas distribution assembly. This device is generally used to distribute process gases across the surface of a wafer. The process gases can flow out from the spray head and be distributed across the wafer; the wafer can be supported by a base assembly within a processing chamber housing the spray head. The distribution of process gases across the wafer can be achieved through a pattern of gas distribution holes that guide the gas flow from inside the spray head assembly to the wafer.

[0331] The spray head assembly generally includes: a back plate portion having at least one gas inlet; a front plate portion opposite to the back plate portion, wherein the front plate portion includes a plurality of gas distribution holes; and an internal volume communicating with the gas distribution holes and the gas inlet. Preferably, the back plate portion and the front plate portion each contain 90% to 99.8% by volume of polycrystalline yttrium aluminum garnet and have at least one surface, wherein the polycrystalline yttrium aluminum garnet preferably contains pores on the at least one surface, and wherein such pores preferably have a pore size of not more than 5 µm and preferably have a maximum pore size of 1.5 µm for at least 95% of the pores.

[0332] In a preferred embodiment, the laminate disclosed herein can be machined into a gas distribution nozzle, comprising: a body having at least one gas injection channel and at least one surface having a surface area, wherein the body preferably comprises 90 vol% to 99.8 vol% polycrystalline yttrium aluminum garnet, wherein the polycrystalline yttrium aluminum garnet preferably comprises pores on the at least one surface, and wherein the pores preferably have a pore size of no more than 5 µm and preferably have a maximum pore size of 1.5 µm for at least 95% of the pores.

[0333] In yet another embodiment, the laminate disclosed herein can be machined into a dielectric window, preferably through which RF or microwave energy can pass when the dielectric window is used in a plasma processing chamber. The dielectric window comprises: a body having at least one surface having a surface area, wherein the body preferably comprises 90 vol% to 99.8 vol% polycrystalline yttrium aluminum garnet, wherein the polycrystalline yttrium aluminum garnet preferably comprises pores on the at least one surface, and wherein the pores preferably have a pore size of no more than 5 µm and preferably have a maximum pore size of 1.5 µm for at least 95% of the pores.

[0334] The dielectric window disclosed herein may be a single layer, or may have more than one layer (i.e., a multilayer dielectric window), as long as it allows the transmission of radiation / energy. If the dielectric window is multilayered, it may contain at least one layer containing a material other than YAG. Exemplary materials include alumina or quartz. The dielectric window may have any shape, such as a disc or a circle, and be large enough to form the ceiling of the processing chamber. (Diagram illustration)

[0335] FIG1A shows a cross-sectional side view of the device 100 according to the present invention. The device has a first punch 003 and a second punch 008, the first punch having a first punch inner surface 004 and the second punch having a second punch inner surface 007. Punches 003 and 008 are made of solid graphite. The punch inner surfaces 004 and 007 are therefore also graphite. The first punch 003 is positioned above the second punch 008. The first punch 003 is horizontal and downward oriented with the first punch inner surface 004 as its orientation. The first punch 003 can be moved in the vertical direction by a first pushing member 001 connected via a first piston 002. The second punch 008 is horizontal and upward oriented with the second punch inner surface 007 as its orientation. The second punch 008 can be moved in the vertical direction by a second pushing member 010 connected via a second piston 009. The inner surfaces 004 of the first punch and 007 of the second punch can therefore move toward each other along the direction of the compression shaft 011.

[0336] The device has a mold 006, which is shaped as a hollow graphite cylinder with walls 015 and an inner surface 005. The device has a power supply 012, which is adjusted and configured to supply direct current (DC). The power supply 012 is electrically connected to a first punch 003 and a second punch 008. The internal volume 013 is defined (or delimited) by the inner surface 004 of the first punch from above, the inner surface 007 of the second punch from below, and the inner surface 005 of the mold 006. In the case of FIG1A, both the inner surfaces 004 and 007 of the punches are circular, while the inner surface 005 is cylindrical. Therefore, the internal volume 013 is also cylindrical.

[0337] Figure 1B shows a cross-sectional side view of the apparatus of Figure 1A, wherein the internal volume 013 is loaded and ready for sintering. The internal volume 013 is filled with a first powder for sintering, wherein the first powder is configured to form a first powder layer 014. Prior to sintering, the inner surfaces 004 and 007 of the punches move inward to abut against the first powder layer 014. The inner surfaces 004 and 007 of the punches move inward along the compression axis 011 as indicated by the arrows. During sintering, the inner surfaces 004 and 007 of the punches apply force to the first powder layer 014, thus generating pressure in the internal volume 013. During sintering, a voltage is also applied across the internal volume 013 (between the first inner surface 004 of the punches and the second inner surface 007 of the punches) and / or the die 006. The voltage is obtained using a power supply 012. Heat is generated in the internal volume 013 due to the applied voltage. The first powder layer 014 is sintered by being subjected to heat and pressure, thereby obtaining a laminate. When the sintering process is complete, the laminate is allowed to cool. During cooling, punches 003 and 008 retract (i.e., the punches do not apply pressure to the laminate). Voltage is also removed during cooling.

[0338] Although only the first powder layer 014 is shown in Figure 1B, one or more additional powders may be introduced into the internal volume 013 prior to sintering. For example, once the first powder layer 014 has been obtained, another powder is introduced into the internal volume 013 to obtain another powder layer. The other powder layer is above and in contact with the first powder layer 014. During sintering, pressure is applied to both the first powder layer 014 and the other powder layer in the internal volume 013. The other powder layer is also heated together with the first powder layer. By subjecting the first powder layer 014 and the other powder layer to heat and pressure, the first powder layer 014 and the other powder layer are sintered, thereby obtaining a laminate. The laminate comprises a first layer and another layer. The first layer is obtained from the first powder layer, and the other layer is obtained from the other powder layer.

[0339] Figure 2 is a flowchart showing the steps of a first embodiment of a process 200 for producing a laminate according to the present invention. In step 201, a first powder is introduced into the internal volume of the apparatus to obtain a first powder layer in the internal volume. The internal volume is defined by the internal surface of a mold, the internal surface of a first punch of a first punch, and the internal surface of a second punch of a second punch. The internal volume has a cross-sectional width of at least 200 mm. The mold, the first punch, and the second punch are made of graphite. The apparatus is adapted and configured for spark plasma sintering. The first powder is a mixture comprising a first component powder and another component powder, wherein the first component powder and the other component powder have different chemical compositions. Furthermore, the other component powder of the first powder has a unimodal particle size distribution. Preferably, the other component powder of the first powder has a specific surface area in the range of 3 to 10 m² / g, more preferably 3.5 to 9 m² / g. In step 202, the first powder layer is subjected to heat and pressure to obtain a laminate. Heat is generated by voltage applied across the mold, the internal volume, or both. The laminate contains a first layer.

[0340] Figures 3A and 3B show the core test 300 used herein. Figure 3A shows a perspective view before the test begins. The core removal tool 301 is positioned above the first flat surface 302 of the stack 306. In Figure 3A, the stack 306 is a flat stack and is in the form of a cylindrical disk. The tool 301 is oriented along an axis perpendicular to the first flat surface 302. Arrow 308 shows the direction of travel of the tool 301 along the axis toward the stack 306. Once in contact with the stack 306, the core removal tool 301 moves in a circular motion within a core removal region 307, which has a diameter larger than the diameter of the tip 309 of the core removal tool 301. The circular motion is parallel to the first flat surface 302 and results in the removal of the cylindrical region (or core) from the stack 306. Furthermore, the geometric center 305 of the first flat surface 302 is also the geometric center 305 of the core removal region 307. Figure 3B shows a cross-sectional view from the side during the core test. Tool 301 has advanced a distance 303 into the laminate 306 having a sample thickness 304. Figure 3B shows the core removal tool 301 removing the cylindrical segment 310 from the laminate 306. The distance 303 is determined between the first flat surface 302 and the end of tool 301. The test is completed when a crack is first observed in the laminate 306. The success level is determined as the ratio of the core removal distance 303 at the end of the test to the total thickness of the laminate 306, expressed as a percentage.

[0341] Figure 4 shows how to measure the angle of repose of the powder. A coarse filter 401 is fixed at a distance 402 above the working surface 403. The coarse filter 401 is positioned such that its center 404 is above the center of the working surface 403. Powder 405 is added to the coarse filter 401 and allowed to flow through it (as indicated by the arrow in Figure 4). As a result, the powder collects on the working surface 403 in a cone-shaped form 406. Once the coarse filter 401 has been emptied, a tangent 407 is fitted to one side of the cone-shaped form 406, and a protractor is used to measure the angle 408 formed between the tangent 407 and the working surface 403. This angle 408 is the angle of repose of the powder.

[0342] Figure 5 shows how the temperature of the side and top of the laminate is measured. Figure 5 shows the mold 006, the first punch 003, and the second punch 008 that form the internal volume 013. The laminate 501 exists in and occupies the internal volume 013. In Figure 5, the internal volume 013 is located in the sintering apparatus. The pyrometer 502 is also located in the sintering apparatus. A quartz observation window 503 is connected between the pyrometer 502 and the internal volume 013. Figure 5 also shows a recess 504 on one side of the mold 006 (i.e., the side facing the pyrometer 502). The pyrometer 502 is used to measure the temperature in the recess 504. The temperature of the recess 504 is defined as the temperature of the side 505 of the laminate 501. A thermocouple 507 is used to measure the temperature at the top 506 of the laminate 501. Thermocouple 507 is located at the center of the first punch 003 (at the position of compression shaft 011 - see Figure 1).

[0343] Figure 6 shows the particle size distribution (PSD) of the first component powder and the other component powder of the first powder. The first component powder (in this case, yttrium oxide) has a single peak PSD 601. The other component powder (in this case, alumina) also has a single peak PSD 602. The single peak PSD 602 ​​has a global maximum value of 603 (the global maximum value α for particle size χα and bulk density qα). The global maximum value 603 is also referred to as the peak value of PSD 602.

[0344] Figure 7 is a flowchart showing the steps of a second embodiment of a process 700 for producing a laminate according to the present invention. In step 701, another component powder (alumina) is heat-treated (calcined). Preferably, after heat treatment, the other component powder has a unimodal particle size distribution. Preferably, after heat treatment, the other component powder has a specific surface area in the range of 3 to 10 m² / g, more preferably 3.5 to 9 m² / g. In step 702, a first component powder (yttrium oxide) and another component powder are mixed to obtain a first powder. In an optional step 703, the first powder is heat-treated (calcined). In step 704, the first powder is introduced into the internal volume of the apparatus to obtain a first powder layer in the internal volume. The internal volume is defined by the internal surface of the mold, the internal surface of the first punch of the first punch, and the internal surface of the second punch of the second punch. The internal volume has a cross-sectional width of at least 200 mm. The mold, as well as the first and second punches, are made of graphite. The apparatus is adapted and configured for spark plasma sintering. In step 705, the first powder layer is subjected to heat and pressure to obtain a laminate. Heat is generated by a voltage applied across the mold, its internal volume, or both. The laminate comprises the first layer. Testing Method

[0345] The following test methods were used within the context of this invention. Unless otherwise stated, measurements were taken at an ambient temperature of 23°C and an ambient pressure of 100 kPa (0.986 atm). Carbon content and other elemental contents.

[0346] The carbon content of the powder is expressed in ppm (by weight), based on the total weight of the powder. The carbon content was measured using an EMIA series carbon / sulfur analyzer (model EMIA-Expert, available from Horiba Instruments Inc. (USA)). Carbon content was analyzed by placing 0.5 g of powder in a crucible and then placing the crucible in the carbon / sulfur analyzer. Before placing the powder in the crucible, the crucible was heated to at least 1000°C in a muffle furnace for 60 minutes. Afterward, the crucible was removed from the furnace and placed in a desiccator. The crucible was allowed to return to room temperature before placing the powder sample in it.

[0347] Regarding the content of other elements in the powder: The sulfur content of the powder is expressed in ppm (by weight) based on the total weight of the powder. The same carbon / sulfur analyzer and measurement method used for carbon are also used to measure the sulfur content of the powder. The chlorine content of the powder is expressed in ppm (by weight) based on the total weight of the powder. The chlorine content of the powder is measured using inductively coupled plasma mass spectrometry (ICP-MS), as described below. For this measurement, an Agilent 7900 ICP-MS (model G8403) is used, which is available from Agilent Technologies, Inc. (USA).

[0348] Place the powder sample in a 15 ml vial. Then dissolve the powder using one or more acids and by adding heat via microwave radiation. The amount of powder used is shown in the table below. Select an amount of acid sufficient to dissolve the powder and obtain a solution. The solution in the vial should not exceed 10 ml. For the application of heat, an ultraWave single-chamber microwave was used. Heat was applied for 50 minutes, during which the temperature of the solution should be 240 ± 10 °C for at least 25 minutes. Table: Amounts of powder and acid used for measurement powder acid Yttrium oxide (Y2O3): 36 mg HNO3 Aluminum oxide (Al2O3): 40 mg HNO3 Al2O3-Y2O3 mixture: 40 mg HNO3 + H2SO4 + H3PO4 + HF YAG (Y3Al5O 12 40 mg HNO3 + H2SO4 + H3PO4 + HF Zirconium oxide (ZrO2): 36 mg HNO3 + H2SO4 + H3PO4 + HF ZrO2-Y2O3 mixture: 36 mg HNO3 + H2SO4 + H3PO4 + HF Magnesium oxide (MgO): 36 mg HNO3

[0349] For powders not indicated in the table above, use the amount of powder and acid as shown for zirconium oxide.

[0350] Once the powder has dissolved, vortex the vial for 10 seconds and place it in an Agilent 7900 ICP-MS for chlorine content measurement. The ICP-MS removes the sample from the vial, nebulizes it to form an aerosol, and then subjectes the aerosol to plasma. The resulting ions are then counted using a mass spectrometer.

[0351] For this measurement, the argon regulator in the Agilent 7900 ICP-MS is set to 100 psi, the helium regulator to 10 psi, and the nitrogen regulator to 10 psi. Additionally, the plasma used for the measurement is allowed to preheat for 30 minutes before the measurement. The Agilent 7900 ICP-MS also features a cooler set to 55 psi and 15°C. Powder water content

[0352] The water content of the powder was measured using an i-Thermo G163L moisture analyzer (available from BEL Engineering srl (Monza, Italy)). Purity of the powder and component powders.

[0353] Inductively coupled plasma mass spectrometry (ICP-MS) was used to measure the purity of powders and component powders (e.g., alumina, yttrium oxide). Purity is reported herein as a percentage relative to 100% purity, indicating that the material contains only the desired component and is free of impurities, dopants, sintering aids, and the like. (Station angle)

[0354] The angle of repose of the powder was measured as shown in Figure 4. The distance between the coarse filter and the working surface was between 17.78 and 20.32 cm (7 to 8 inches). The working surface was a circle with a diameter of 20.32 cm (8 inches). The angle of repose was measured at 10 evenly spaced locations around the circumference of the working surface. The average of these 10 measurements was defined as the angle of repose of the powder, as asserted herein. Specific surface area

[0355] The specific surface area of ​​the powder was measured according to standard ASTM C1274. This measurement was performed using a Horiba BET surface area analyzer (model SA-9601), which is capable of measuring specific surface areas from 0.01 to 2000 m² / g. Particle size

[0356] The particle size distribution of powders, component powders, and powder layers was measured using a Horiba LA-960 laser scattering particle size analyzer, which is capable of measuring particle sizes from 10 nm to 5 mm. Particle size measurements were performed by adding a 1 g sample of powder along with a drop of Na4P2O7 (removed by pipette) to deionized water in the Horiba LA-960 analyzer. During the measurement, circulation, stirring, and ultrasound were activated in the analyzer. For this measurement, both circulation and stirring were set to level 5, and ultrasound was used at power level 6 for 12 minutes.

[0357] Particle size measurement is also used to obtain the particle size distribution of powders and component powders. Particle size and particle size distribution are based on volume; for example, the values ​​of d10, d50, and d90 are based on volume. Core Testing

[0358] Core removal is performed on the laminate to determine the presence of excessive internal stress. The laminate is a planar laminate having a first flat surface and a thickness perpendicular to the first flat surface. A 10 mm diamond core removal tool is used, which is available, for example, from Schott Diamantwerkzeuge GmbH of Stadtoldendorf, Germany. The core removal tool is used in a commercially available CNC machine to remove the core from the laminate under test. The hole formed in the laminate by removing the core is from 56 mm to 60 mm and has a nominal diameter of 58 mm. The core is removed by drilling a hole in the laminate by passing the tool in a helical pattern over the surface of the laminate. Suitable CNC machines for this test are available, for example, from DMG Mori Company Limited of Los Angeles, California, USA (such as its Ultrasonic 60 eVo linear model). Another supplier of suitable CNC machines is Fair Friend Ent.Co. Ltd. of Taiwan (such as the Feeler HV-1650 model). The test ends when the core extends through the laminate or when a crack is observed in the laminate, whichever occurs first. The success score is given as a percentage of the thickness of the core cut from the tested laminate. A 100% success rating indicates low internal stress (if any); a success rating above 75% but below 100% indicates low internal stress; a success rating between 25% and 75% indicates moderate stress; and a success rating below 25% indicates high internal stress. The above test method is further illustrated in Figures 3A and 3B. Volumetric porosity

[0359] If the volumetric porosity is 2% or higher, calculate the volumetric porosity of the laminate and the layers of the laminate from the density measurement performed according to ASTM B962-17. If the volumetric porosity is less than 2%, perform the measurement according to standard ASTM B311-17. Grain size

[0360] The average grain size is measured using the Heyn linear intercept procedure as described in ASTM standard E112-2010. The color of the laminate...

[0361] The CIELAB color coordinates of the laminate were determined using a WR-18 colorimeter available from FRU (China). Etching resistance

[0362] To determine the etch resistance of a layer (e.g., the first layer) in a multilayer stack, 100 samples of that layer were selected. Each sample had a width and length of 6 mm x 6 mm and a thickness of 2 mm. Each sample was mounted onto a c-plane sapphire wafer using a silicon-based thermal compound. Areas of the sample were protected from the etching process by bonding 5 mm x 5 mm square sapphire ceramic to the sample surface.

[0363] A dry etching process was then performed for each sample using a Versaline DESC PDC Deep Silicon Etch (available from Plasma-Therm (USA)). The etching process was performed using a pressure of 10 ml, a bias of 600 volts, and an ICP power of 2000 watts. Furthermore, a two-step etching process was used, with a total duration of 6 hours. The first etching step had a CF4 flow rate of 90 standard cubic centimeters per minute (sccm), an oxygen flow rate of 30 sccm per minute (sccm), and an argon flow rate of 20 sccm per minute (sccm). The second etching step had an oxygen flow rate of 100 sccm per minute (sccm) and an argon flow rate of 20 sccm per minute (sccm). Both the first and second etching steps were performed for 300 seconds each and were repeated for a combined duration of 6 hours. After the etching process was completed, the surface roughness parameters Sa, Sz, and Sdr were measured using the procedure disclosed herein. Surface Roughness

[0364] Surface roughness parameters Sa, Sz, and Sdr are measured according to standard ISO 25178-2:2012, section 4.1.7. Density and theoretical density of the laminate.

[0365] The density of the laminate is measured according to standard ASTM B962–17. The theoretical density is calculated from X-ray diffraction (XRD) data. Unit parameters a, b, and c are obtained from the XRD data. The unit volume is calculated using the unit parameters. The number of molecular units present in each unit is determined based on the crystal structure of the material. Since the chemical structure is known, the molecular weight of the laminate is known. Using the aforementioned data, the theoretical density is calculated as follows: Theoretical density = (Molecular weight x Number of molecules per unit) / (Volume of unit x Number of Avogadro molecules). Fracture toughness

[0366] Rupture toughness is determined according to standard ASTM E1820-18. Flexural strength

[0367] Flexural strength is determined according to standard ASTM C1161-18. Temperature

[0368] The temperature of the side surface of the laminate is determined as shown in Figure 5.

[0369] The temperature in the recess of the mold was measured using a model E2MH-R08-V-0-0 pyrometer (available from Fluke Process Instruments). The diameter of the recess was 1.27 cm (0.5 inches). The recess extended to a depth of 13.46 cm (5.3 inches) into the mold wall. The wall thickness measured at the location of the recess was approximately 15.24 cm (6 inches). The pyrometer was positioned at a distance of 30.48 cm (12 inches) from the recess.

[0370] The temperature at the top of the laminate was measured as shown in Figure 5. For this measurement, a thermocouple of model A14A-N51700-1, which is available from Nanmac Corporation (USA), was used. The thermocouple was positioned at a distance between 15.24 cm and 20.32 cm (6 inches to 8 inches) from the top of the laminate.

[0371] The temperature in the internal volume is measured using the same thermocouple used to measure the temperature at the top of the laminate. That is, the temperature of the internal volume and the temperature at the top of the laminate (once the laminate has been formed) are the same measured values.

[0372] The temperature for calcining the (component) powder is obtained by reading the digital readings on the kiln used in the calcination process.

[0373] EXTECH visual particle counters (0.3, 0.5, 1.0, 2.5, and 10 µm) were used to measure the temperature of the environment (i.e., the exterior of an internal volume) (such as a storage room). Pressure

[0374] A load cell (available from Interface Force Measurement Solutions (USA)) was used to measure the force in the internal volume. The load cell used was model 1290CHG-2000K with a capacity of 2000 Klbf. The pressure in the internal volume was then calculated by dividing the force by the area of ​​the internal volume. The area of ​​the internal volume was given by π(DINT / 2)², where DINT is the diameter of the internal volume. Example

[0375] The invention is further illustrated by examples. The invention is not limited to these embodiments. In the table of embodiments, the magnitude of the effect is indicated by one or more "+" or "-". The following ratios are used: "-----", "----", "---", "-", "-", "+", "++", "+++", "++++", "+++++". The reference value is indicated by "Ref". No change relative to the reference value is indicated by "0". Basic settings

[0376] Unless otherwise stated, the basic settings described below apply to all instances.

[0377] Two component powders are provided, wherein the first component powder is yttrium oxide powder and the other component powder is alumina powder. The yttrium oxide has a d10 particle size in the range of 2 µm to 4 µm, a d50 particle size in the range of 6 µm to 8 µm, and a d90 particle size in the range of 11 µm to 13 µm. The yttrium oxide also has a unimodal particle distribution.

[0378] Alumina and yttrium oxide were mixed using wet ball milling to obtain a first powder. Wet ball milling was performed using a high-purity (>99.9%) alumina medium, wherein the weight of the alumina medium was approximately 90% to approximately the same as the weight of the powder, i.e., approximately 50% loading. A slurry was formed by adding ethanol to the alumina and yttrium oxide, wherein the ethanol constituted approximately 40 wt% to 50 wt% of the total slurry weight (the weight of ethanol and the first powder together). The slurry was mixed at 150 RPM for approximately 15 to 20 hours. After milling, ethanol was extracted from the slurry using a rotary evaporator. The dried powder was then tumbled and sieved according to methods known to those skilled in the art to obtain the first powder. The first powder was then calcined (heat-treated) at 800°C to 1050°C for 7 hours, depending on the container size (larger containers require longer calcination times). After calcination, the first powder has a d50 particle size in the range of 9 µm to 13 µm, and by total weight, the first powder contains alumina in the range of 42.9 wt-% to 43.4 wt-% and yttrium oxide in the range of 56.6 wt-% to 57.1 wt-%

[0379] Two additional component powders are provided, wherein the first component powder is a partially stabilized zirconia powder, and the other component powder is an alumina powder. The alumina has a d10 particle size in the range of 0.05 µm to 0.15 µm, a d50 particle size in the range of 0.2 µm to 0.5 µm, and a d90 particle size in the range of 0.4 µm to 1 µm. The zirconia has a d10 particle size in the range of 0.08 µm to 0.2 µm, a d50 particle size in the range of 0.2 µm to 0.5 µm, and a d90 particle size in the range of 0.5 µm to 1.2 µm.

[0380] Alumina and zirconium oxide were mixed using wet ball milling to obtain another powder. The wet ball milling was performed using a high-purity (>99.9%) alumina medium at a loading of approximately 80% of the powder weight. A slurry was formed by adding ethanol to the alumina and yttrium oxide, wherein the ethanol constituted approximately 50 wt% of the total slurry weight. The slurry was mixed at 20 RPM for approximately 20 hours. After milling, ethanol was extracted from the slurry using a rotary evaporator. The dried powder was then tumbled and sieved according to methods known to those skilled in the art to obtain another powder. This other powder was subsequently calcined (heat-treated) at 900°C for 7 hours, depending on the container size (smaller containers require a shorter time). After calcination, the other powder has a d50 particle size in the range of 90 µm to 110 µm, and the first powder further comprises, by total weight, alumina in the range of 77.1 wt% to 78.3 wt% and zirconium oxide in the range of 21.7 wt% to 22.9 wt%. Alternatively, the alumina and zirconium oxide can be jet-milled instead of wet ball milling.

[0381] A first powder is introduced into the internal volume of the apparatus (spark plasma sintering apparatus) shown in FIG. 1. The first powder is spread evenly to obtain a first powder layer. Then, another powder is introduced into the internal volume by placing another powder on the first powder layer. The other powder is spread evenly to obtain another powder layer on the first powder layer. The first powder and the other powder are introduced while the internal volume is removed from the apparatus. The internal volume is then placed in the sintering chamber of the apparatus and the internal volume is evacuated to obtain a pressure in the internal volume in the range of 10⁻³ Torr to 10⁻² Torr.

[0382] The first powder layer and the other powder layer are subjected to heat and pressure. During this step of subjecting the first powder layer and the other powder layer to heat and pressure, the temperature and pressure in the internal volume are increased to 1625°C and 15 MPa, respectively. The first powder layer and the other powder layer are subjected to a temperature of 1625°C and a pressure of 15 MPa for 60 to 75 minutes. Thereafter, the sintering chamber is filled with an inert gas, preferably nitrogen, and cooling is allowed for several hours. The resulting laminate has a first layer and another layer adjacent to each other (i.e., in contact with each other). The first layer is made of YAG, and the other layer is made of ZTA. Applying heat and pressure to the first powder layer causes alumina and yttrium oxide to react to form the YAG layer of the laminate. Similarly, applying heat and pressure to the other powder layer causes alumina and zirconium oxide to form the ZTA layer of the laminate.

[0383] Once the laminate reaches a temperature of approximately 25°C, it is removed and placed in a furnace under normal atmospheric pressure and oxygen conditions. The laminate is then heat-treated at 1400°C for 8 hours. Example 1

[0384] Example 1 was repeated for different values ​​of the specific surface area of ​​the other component powder (alumina) of the first powder. The specific surface area values ​​are shown in Table 1. The other component powder of the first powder has a unimodal particle size distribution and a d50 in the range of 0.04 µm to 0.26 µm.

[0385] In Example 1, the internal volume of the apparatus has a cross-sectional width of 600 mm. Therefore, the produced laminate also has a diameter of 600 mm. Furthermore, the first layer of the laminate is made of YAG and has a thickness of 5 mm. Table 1 Example 1.1 1.2 1.3 1.4 1.5 1.6 1.7 settings Specific surface area [m 2 / g] 2 3 4 6 8 10 14 Produced laminates strength -- - + + + - -- Core test success rate -- - + + + - -- Etch resistance -- - + + + - -- Porosity ++ + - - - + ++ Unreacted component powder ++ + - - - + ++

[0386] The technical effects in Table 1 are as follows: - Strength: The external force or stress required to permanently deform or fracture the laminate (especially the first layer) when an external force or stress is applied to it. "+" indicates a higher strength, and "-" indicates a lower strength. Increased strength is desired. - Core Test Success Rate: The percentage of laminates that pass the core test. If a laminate cracks or fractures during the core test, it fails the core test. "+" indicates a higher core test success rate, and "-" indicates a lower success rate. A higher core test success rate is desired. - Etching Resistance: The resistance of the laminate, specifically the first layer made of YAG, to chemical etchants. "+" indicates a higher resistance, and "-" indicates a lower resistance. Higher resistance is desired. - Porosity: The volumetric porosity of the laminate, specifically the first layer. "+" indicates a higher volumetric porosity, and "-" indicates a lower volumetric porosity. The desired outcome is a smaller volumetric porosity. - Unreacted component powder: The amount of alumina and yttrium oxide present in the first layer of the laminate. "+" indicates a larger amount of component powder alumina and yttrium oxide present in the first layer, and "-" indicates a smaller amount of component powder alumina and yttrium oxide present. The desired outcome is to reduce the amount of component powder in the first layer of the laminate.

[0387] In a variation of Example 1, the example was repeated for a configuration with only a first powder layer (i.e., without introducing another powder layer into the internal volume). Therefore, the resulting laminate had only a single YAG layer. Similar results as shown in Table 1 were also obtained for the monolayer. Example 2

[0388] Example 2 was repeated using different particle size distributions (PSDs) of the other component powder (alumina) of the first powder. The results are shown in Table 2. In Example 2, the specific surface area of ​​the other component powder of the first powder was in the range of 7.5 to 8.5 m² / g. In Example 2, the trimodal PSD had a global maximum and two local minimums. The local minimum corresponds to a particle size smaller than the particle size corresponding to the global maximum. In Example 2, the internal volume of the apparatus had a cross-sectional width of 600 mm. Therefore, the produced laminate also had a diameter of 600 mm. Table 2 Example 2.1 2.2 2.3 2.4 settings Particle size distribution Three Peaks Three Peaks Single peak Single peak Produced laminates Thickness of YAG layer [mm] 5 20 5 20 strength - --- + + Scratch resistance - --- + + density change + +++ - - Core test success rate - --- + + Etch resistance - --- + + The volume of the first layer having the desired color [%] - --- + + Porosity + +++ - - Unreacted component powder + +++ - -

[0389] The technical effects in Table 2 are as described with respect to Table 1. Furthermore, Table 2 has the following technical effects: - Scratch resistance: The scratch resistance of the laminate, and specifically the first layer. "+" indicates greater scratch resistance, and "-" indicates less scratch resistance. The desired effect is increased scratch resistance. - Density variation: The density variation of the laminate, and specifically the first layer. "+" indicates greater density variation, and "-" indicates less density variation. The desired effect is reduced density variation. - Volume of the first layer with the desired color: The desired effect is that the first layer has white. The first layer is considered to have white when its color coordinates (represented in the 1976 CIELAB color space) have the following coordinates: absolute values ​​of L* greater than 65, and a* and b* less than 5. "+" indicates a larger volume, and "-" indicates a smaller volume. The desired effect is increased volume of the first layer with the desired color. Example 3

[0390] The settings for Example 3.1 are the same as those described in the "Basic Settings". The settings for Example 3.2 are the same as those described in the "Basic Settings", but with the following differences. Before mixing yttrium oxide and alumina (which are the first component powder and the other component powder, respectively) to obtain the first powder, the alumina is calcined separately (subjected to heat treatment). This separate calcination of the alumina is carried out at a temperature of 900 to 1000°C for 7 hours. Before any processing step (e.g., calcination, mixing), the particle size distribution (PSD) of the alumina in Examples 3.1 and 3.2 both have a trimodal PSD. After calcination in Example 3.2, the PSD of the alumina is unimodal. Table 3 Example 3.1 3.2 settings The separate calcination of the other component powder (alumina) of the first powder. no yes Produced laminates strength - + Scratch resistance - + density change + - Core test success rate - + Etch resistance - + The volume of the first layer having the desired color [%] - + Porosity + - Unreacted component powder + -

[0391] The technical effects in Table 3 are as described with reference to Tables 1 and 2. Example 4

[0392] Example 4 was repeated for different d50 values ​​of the other component powder (alumina) of the first powder. The d50 values ​​are shown in Table 4. The other component powder of the first powder has a unimodal particle size distribution. In Example 4, the internal volume of the apparatus has a cross-sectional width of 600 mm. Therefore, the produced laminate also has a diameter of 600 mm. Furthermore, the first layer of the laminate is made of YAG and has a thickness of 5 mm. Table 4 Example 4.1 4.2 4.3 4.4 4.5 4.6 settings (of the first powder) another component powder d 50 [µm] 0.005 0.01 0.1 0.2 0.5 1 Produced laminates Thickness of YAG layer [mm] 5 5 5 5 5 5 strength -- - + + - -- Scratch resistance -- - + + - -- density change -- - + + - -- Core test success rate - + ++ ++ + - Etch resistance -- - + + - -- The volume of the first layer having the desired color [%] -- - + + - -- Porosity -- - + + - -- Unreacted component powder -- - + + - --

[0393] The technical effects in Table 4 are as described with reference to Tables 1 and 2. Component Symbols 100 Device according to the present invention 001 First propulsion component 002 First piston 003 First punch 004 The inner surface of the first punch 005 The inner surface of the mold 006 mold 007 The inner surface of the second punch 008 Second punch 009 Second piston 010 Second propulsion component 011 compression shaft 012 power supply 013 Internal volume 014 First powder layer 015 mold wall 200 First embodiment of a process for producing laminates 201 A first powder is introduced into an internal volume to obtain a first powder layer, wherein the first powder is a mixture of a first component powder and another component powder, wherein the other component powder has a unimodal PSD. 202 The first powder layer is subjected to heat and pressure to obtain a laminate. 300 Core test settings 301 Core extraction tools 302 First flat surface 303 Drilling depth 304 Sample thickness 305 Geometric center 306 Flat-form lamination 307 Take the core area 308 The direction of movement perpendicular to the flat lamination body 309 Take the tip of the core tool 310 Cylindrical segments removed from flat-form laminations 400 Stationary angle measurement 401 coarse filter 402 Distance between the funnel and the working surface 403 working surface 404 Funnel outlet 405 Powder added to the funnel 406 Powder collected in a cone-shaped form 407 Tangent 408 Angle of rest 500 Temperature measurement of the sides and top of the laminate 501 laminated body 502 pyrometer 503 Observation window 504 Concave part in the mold 505 Side of the laminate 506 Top of the stacked body 507 thermocouple 600 First, the composition of the powder and its particle size distribution. 601 Particle size distribution of the first component powder 602 Particle size distribution of the other component powder 603 Global maximum value 700 Second embodiment of a process for producing laminates 701 The other component powder is subjected to heat treatment 702 Mix the first component powder and the other component powder to obtain the first powder. 703 The first powder is subjected to heat treatment 704 A first powder is introduced into the internal volume to obtain a first powder layer. 705 The first powder layer is subjected to heat and pressure to obtain a laminate. [Simplified Explanation of the Diagram]

[0188] Together with some illustrative figures, the following schematic diagrams show the forms of the invention used to enhance understanding of the invention. Therefore, these figures should not be considered as limiting the invention. The figures are not drawn to scale. [Figure 1A] shows a cross-sectional side view of the device according to the invention. [Figure 1B] shows a cross-sectional side view of the device of Figure 1A, wherein the internal volume is loaded and ready for sintering. [Figure 2] is a flowchart showing the steps of a first embodiment of the procedure for producing a laminate according to the invention. [Figure 3A] and [Figure 3B] show the core tests used herein. [Figure 4] shows how to measure the stationary angle of the powder. [Figure 5] shows how to measure the temperature of the side and top of the laminate. [Figure 6] shows the particle size distribution of the first component powder and the other component powder of the first powder. [Figure 7] is a flowchart showing the steps of a second embodiment of the procedure for producing a laminate according to the invention.

Claims

1. A method for producing a laminate, comprising the following steps: a. introducing a first powder into an internal volume to obtain a first powder layer in the internal volume, wherein i. the internal volume A. has a cross-sectional width W of at least 200 mm, and B. is at least partially delimited by an internal surface of a mold, wherein the mold has at least one wall, and wherein the wall comprises carbon; ii. the first powder is a mixture comprising a first component powder and another component powder, wherein the first component powder and the other component powder have different chemical compositions; b. subjecting the first powder layer to heat and pressure to obtain the laminate, wherein i. the heat is generated by a voltage applied across the mold, the internal volume, or both, and ii. the laminate comprises a first layer; wherein the other component powder of the first powder has a particle size distribution D = q(χ) of bulk density q to particle size χ, such that I. D has a global maximum value α for particle size χα and bulk density qα, and II. If D has a local maximum value β for particle size χβ and bulk density qβ, then qα / qβ is at least 10.

2. The method of claim 1, wherein the other component powder of the first powder has at least one of the following properties: a. a d10 particle size in the range of 0.005 µm to 0.4 µm; b. a d50 particle size in the range of 0.01 µm to 0.8 µm; c. a d90 particle size in the range of 0.05 µm to 7 µm.

3. The method of claim 1 or 2, wherein the other component powder of the first powder has a particle size distribution D = q(χ) with respect to bulk density q, wherein D is unimodal.

4. The method of claim 1 or 2, wherein the other component powder of the first powder has a specific surface area of ​​less than or equal to 12 m² / g.

5. The method of claim 1 or 2, wherein the specific surface area of ​​the other component powder of the first powder is in the range of 2.5 m2 / g to 12 m2 / g.

6. The method of claim 1 or 2, wherein the other component powder is subjected to heat treatment before mixing the first component powder and the other component powder to obtain the first powder.

7. The method of claim 1 or 2, wherein the first layer has a thickness of at least 10 mm.

8. The method of claim 1 or 2, wherein the other component powder of the first powder has a particle size distribution D = q(χ) with respect to volume density q, wherein D has a global maximum value α with respect to particle size χα and volume density qα, and wherein χα is in the range of 2.7 µm to 7 µm.

9. The method of claim 1 or 2, wherein the other component powder of the first powder is an oxide of a group 13 (formerly group 3A) element.

10. The method of claim 1 or 2, wherein the first powder comprises: yttrium, aluminum, zirconium, magnesium, or a combination of at least two thereof.

11. The method of claim 1 or 2, wherein the first powder is capable of forming at least one of the following under applied heat and pressure: a. oxide A, comprising at least 1 mol-% of a Group 3 (formerly Group IIIB) element and at least 1 mol-% of a Group 13 (formerly Group IIIA) element, wherein the mol-% is expressed as oxygen in oxide A; b. oxide B, comprising at least 1 mol-% of a Group 4 (formerly Group IVB) element and at least 1 mol-% of a Group 13 (formerly Group IIIA) element, wherein the mol-% is expressed as oxygen in oxide B.

12. A stacked volume obtained by any one of claims 1 to 11.

13. An assembly comprising a stack as claimed in claim 12.

14. Use of a powder for producing a laminate comprising a first layer, the powder being a mixture comprising a first component powder and another component powder, wherein a. the first component powder and the other component powder have different chemical compositions, b. the other component powder has a particle size distribution D = q(χ) of bulk density q versus particle size χ, wherein D is unimodal, and c. the other component powder has a specific surface area of ​​less than or equal to 12 m² / g.

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