Silicon-molybdenum alloy tubular target material and preparation method and application thereof

Through wet ball mill mixing and hot isostatic sintering processes, the problem of insufficient density and molding performance of silicon-molybdenum tubular targets in the prior art is solved, and a high density and uniform silicon-molybdenum tubular target is prepared, which meets the high performance requirements.

CN119736586AActive Publication Date: 2025-04-01KONFOONG MATERIALS INTERNATIONAL CO LTD
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Patent Information

Application Number
CN202411862385.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-17
Publication Date
2025-04-01
Estimated Expiration
2044-12-17

AI Technical Summary

Technical Problem

It is difficult to prepare large-size silicon-molybdenum tubular targets with high density and high silicon content in the prior art, and the powder mixing uniformity of silicon-molybdenum materials and poor molding performance.

Method used

Wet ball milling is used to mix silicon powder, molybdenum powder and binder, and a high density large-size silicon-molybdenum tubular target is prepared through cold isostatic treatment and hot isostatic sintering process.

Benefits of technology

The high density and internal uniformity of silicon-molybdenum tubular targets are achieved, the mechanical processing performance of green bodies is improved, and the requirements of high-performance tubular targets are met.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of target material preparation, in particular to a silicon-molybdenum alloy tubular target material and a preparation method and application thereof, through the technology of mixing silicon powder and molybdenum powder through wet ball milling, the powder mixing uniformity is improved; according to the silicon-molybdenum alloy tubular target material, the forming performance of the silicon-molybdenum alloy tubular target material is improved by adding the binder, so that forming of the large-size tubular target material is achieved, the machining performance of a green body is improved, finally, densification is conducted through the hot isostatic pressing treatment process, and the prepared silicon-molybdenum alloy tubular target material is high in density and good in internal uniformity and can meet the high-performance requirement of the tubular target material.
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Description

Technical Field

[0001] The invention relates to the technical field of target material preparation, and in particular to a silicon-molybdenum alloy tubular target material and a preparation method and application thereof. Background Art

[0002] Silicon-molybdenum target is a commonly used target in the vacuum sputtering process. Since the oxide gate formed by sputtering of silicon-molybdenum target has stable contact performance with polysilicon, this silicide can withstand high temperature treatment without decomposing into oxides, and has excellent anti-oxidation and chemical corrosion resistance, silicon-molybdenum target is widely used in the field of electronic gate materials and electronic thin films.

[0003] In recent years, the industry's demand for high-purity silicon-molybdenum targets has increased significantly. However, most of the silicon-molybdenum targets produced in the prior art have low density and cannot meet the requirements of the high-end electronics industry for target quality, and are only partially used in low-end products. Common preparation methods for silicon-molybdenum materials include mechanical alloying, pressureless sintering, reaction sintering, hot pressing sintering, etc. Among them, the maximum density of pressureless sintered silicon-molybdenum materials is only 90% of the theoretical density. Reaction sintering undergoes a thermochemical reaction between the element powders. The effect of the reaction depends on the initial and final chemical composition, the microstructure of the reaction pressed block, the reaction process atmosphere, and the thermal boundary conditions. Due to expansion and the presence of oxide film on the particle surface, reaction sintering cannot guarantee very high density. Pressure sintering can significantly improve the densification process and obtain nearly fully dense materials.

[0004] CN 104513953A discloses a method for making a molybdenum-silicon target, comprising: providing molybdenum powder and silicon powder, mixing the molybdenum powder and the silicon powder to form a molybdenum-silicon mixed powder; and sintering the molybdenum-silicon mixed powder by a hot pressing process to form a molybdenum-silicon target. The density of the molybdenum-silicon target formed by the method of the invention is very high, but the method is mainly suitable for silicon-molybdenum alloy targets with a high molybdenum content.

[0005] CN 105483624A discloses a method for manufacturing a molybdenum-silicon target material and a combination thereof, wherein the method for manufacturing the molybdenum-silicon target material comprises: providing molybdenum powder and silicon powder; mixing the molybdenum powder and the silicon powder using a mixing process to form a mixed powder; using a cold pressing process to make the mixed powder into a molybdenum-silicon target material blank; using a vacuum hot pressing sintering process to make the molybdenum-silicon target material blank into a molybdenum-silicon target material. The manufacturing method using this scheme can obtain a molybdenum-silicon target material with a higher density, but it is only applicable to molybdenum-silicon flat circular targets, and has certain limitations for preparing large-sized molybdenum-silicon tubular targets.

[0006] In addition, there are some difficulties in the preparation of silicon-molybdenum alloy: the density of silicon and molybdenum is quite different, and silicon powder is very easy to agglomerate, which makes it difficult to mix the powder evenly; the cold pressing forming performance of silicon is poor, and the green body after cold pressing has low strength and high brittleness, making it difficult to machine.

[0007] Therefore, in view of the shortcomings of the prior art, it is necessary to provide a method for preparing a large-sized tubular silicon-molybdenum target material with good molding effect and high density. Summary of the invention

[0008] The purpose of the present invention is to provide a silicon-molybdenum alloy tubular target material and a preparation method and application thereof, so as to realize the preparation of a silicon-molybdenum alloy tubular target material with high silicon content, high density and large size.

[0009] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0010] In a first aspect, the present invention provides a method for preparing a silicon-molybdenum alloy tubular target, the preparation method comprising the following steps:

[0011] (1) mixing silicon powder, molybdenum powder and a binder by wet ball milling, and subjecting the obtained mixture to cold isostatic pressing to obtain a silicon-molybdenum alloy billet;

[0012] (2) The silicon-molybdenum alloy blank obtained in step (1) is subjected to degreasing treatment and hot isostatic pressing sintering in sequence to obtain the silicon-molybdenum alloy tubular target.

[0013] The preparation method of the silicon-molybdenum alloy tubular target provided by the present invention adopts the process of wet ball milling to mix silicon powder and molybdenum powder to improve the uniformity of the mixed powder; improves its forming performance by adding a binder, thereby realizing the forming of large-size tubular targets and improving the mechanical processing performance of green blanks; finally, densification is carried out by hot isostatic pressing, and the prepared silicon-molybdenum alloy tubular target has a high density.

[0014] Preferably, the particle size of the silicon powder in step (1) is 5-8 μm, for example, 5 μm, 5.5 μm, 6 μm, 7 μm or 8 μm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0015] Preferably, the purity of the silicon powder in step (1) is 5N.

[0016] Preferably, the particle size of the molybdenum powder in step (1) is 3-5 μm, for example, 3 μm, 3.5 μm, 4 μm, 4.5 μm or 5 μm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0017] Preferably, the purity of the molybdenum powder in step (1) is 3N5.

[0018] Preferably, based on the total mass fraction of 100wt%, in the silicon powder and molybdenum powder in step (1), the mass fraction of molybdenum powder is 10-50wt%, and the remainder is silicon powder.

[0019] The mass percentage of the molybdenum powder is 10-50wt%, for example, it can be 10wt%, 20wt%, 30wt%, 40wt% or 50wt%, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0020] Preferably, the binder in step (1) comprises any one of epoxy resin, acrylic resin or polyimide resin or a combination of at least two thereof. Typical but non-limiting combinations include a combination of epoxy resin and acrylic resin, a combination of acrylic resin and polyimide resin, or a combination of epoxy resin, acrylic resin and polyimide resin.

[0021] Preferably, the mass of the binder in step (1) is 0.2-1wt% of the total amount of silicon powder and molybdenum powder, for example, it can be 0.2wt%, 0.4wt%, 0.6wt%, 0.8wt% or 1wt%, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0022] The amount of the binder needs to be controlled within a reasonable range. If the amount is too large or too small, the ball-milling mixing uniformity of silicon powder and molybdenum powder cannot be effectively improved.

[0023] Preferably, the ball milling medium used in the wet ball milling mixing in step (1) comprises anhydrous ethanol.

[0024] The anhydrous ethanol is of analytical grade.

[0025] Preferably, the mass of the anhydrous ethanol is 20-50wt% of the total amount of silicon powder, molybdenum powder and anhydrous ethanol, for example, it can be 20wt%, 25wt%, 30wt%, 40wt% or 50wt%, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0026] Preferably, the ball milling balls used for the wet ball milling mixing in step (1) include zirconia balls with diameters of 5 mm, 10 mm and 15 mm, respectively, and the mass ratio is 1:(9-11):(9-11), for example, it can be 1:9:9, 1:10:10 or 1:11:11, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0027] In the present invention, by selecting zirconia balls of different diameters for wet ball milling, the mixing effect of silicon powder and molybdenum powder can be increased and the mixing uniformity can be improved.

[0028] Preferably, the ratio of the mass of the ball milling balls used for the wet ball milling mixing in step (1) to the total mass of the silicon powder and the molybdenum powder is 1:(1.5-2.5), for example, it can be 1:1.5, 1:1.8, 1:2, 1:2.2 or 1:2.5, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0029] Preferably, the rotation speed of the wet ball milling mixing in step (1) is 10-15 r / min, for example, it can be 10 r / min, 12 r / min, 13 r / min, 14 r / min or 15 r / min, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0030] Preferably, the wet ball milling mixing time in step (1) is 23-25 ​​h, for example, 23 h, 23.5 h, 24 h, 24.5 h or 25 h, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0031] Preferably, the mixed material in step (1) is dried before cold isostatic pressing.

[0032] Preferably, the pressure of the cold isostatic pressing treatment in step (1) is 150-250 MPa, for example, 150 MPa, 180 MPa, 200 MPa, 220 MPa or 250 MPa, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0033] Preferably, the holding time of the cold isostatic pressing treatment in step (1) is 15-30 min, for example, 15 min, 20 min, 25 min, 28 min or 30 min, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0034] Preferably, the silicon-molybdenum alloy blank is processed before the degreasing treatment in step (2).

[0035] The degreasing treatment is to use a degreasing agent to degrease the processed silicon-molybdenum alloy blank to remove the binder added during powder mixing.

[0036] Preferably, the temperature of the hot isostatic pressing sintering in step (2) is 600-900°C, for example, 600°C, 650°C, 700°C, 800°C or 900°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0037] Preferably, the pressure of the hot isostatic pressing sintering in step (2) is 100-150 MPa, for example, 100 MPa, 120 MPa, 130 MPa, 140 MPa or 150 MPa, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0038] Preferably, the hot isostatic pressing sintering time in step (2) is 2-4 hours, for example, 2 hours, 2.5 hours, 3 hours, 3.5 hours or 4 hours, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0039] Preferably, the hot isostatic pressing sintering in step (2) is carried out in a stainless steel jacket.

[0040] As a preferred technical solution of the preparation method of the present invention, the preparation method comprises the following steps:

[0041] (1) Wet ball milling silicon powder, molybdenum powder and a binder for 23-25 ​​hours at a rotation speed of 10-15 r / min, and drying the resulting mixture and cold isostatic pressing it at 150-250 MPa for 15-30 min to obtain a silicon-molybdenum alloy billet; the particle size of the silicon powder is 5-8 μm and the purity is 5N; the particle size of the molybdenum powder is 3-5 μm and the purity is 3N5; based on the total mass fraction of 100wt%, the mass of the molybdenum powder in the silicon powder and the molybdenum powder accounts for 10-50wt%, and the remainder is silicon powder; the mass of the binder is 0.2-1wt% of the total amount of the silicon powder and the molybdenum powder;

[0042] The ball milling medium used in the wet ball milling mixing includes anhydrous ethanol, and the mass of the anhydrous ethanol is 20-50wt% of the total amount of silicon powder, molybdenum powder and anhydrous ethanol; the ball milling balls used in the wet ball milling mixing include zirconium oxide balls with diameters of 5mm, 10mm and 15mm, respectively, and the mass ratio is 1:(9-11):(9-11); the ratio of the mass of the ball milling balls to the total mass of silicon powder and molybdenum powder is 1:(1.5-2.5);

[0043] (2) The silicon-molybdenum alloy blank obtained in step (1) is degreased after processing, and then hot isostatically pressed in a stainless steel sheath at a temperature of 600-900° C., a pressure of 100-150 MPa, and a time of 2-4 h to obtain the silicon-molybdenum alloy tubular target.

[0044] In a second aspect, the present invention provides a silicon-molybdenum alloy tubular target material, which is prepared by the method for preparing the silicon-molybdenum alloy tubular target material described in the first aspect.

[0045] The silicon-molybdenum alloy tubular target material provided by the present invention has good internal uniformity and high density, can be made into a large-sized tube, and meets the high performance requirements of the tubular target material.

[0046] In a third aspect, the present invention provides an application of the silicon-molybdenum alloy tubular target material as described in the second aspect, wherein the silicon-molybdenum alloy tubular target material is used for preparing electronic gate materials or electronic thin films.

[0047] The silicon-molybdenum alloy tubular target material is used as a raw material for preparing an electronic gate material or an electronic film, which can ensure a higher comprehensive performance.

[0048] Compared with the prior art, the present invention has the following beneficial effects:

[0049] The preparation method of the silicon-molybdenum alloy tubular target provided by the present invention adopts the process of mixing silicon powder and molybdenum powder by wet ball milling to improve the uniformity of the mixed powder; improves its forming performance by adding a binder, thereby realizing the forming of large-size tubular targets and improving the mechanical processing performance of green billets; finally, densification is carried out by a hot isostatic pressing process; the prepared silicon-molybdenum alloy tubular target has high density and good internal uniformity, and can meet the high performance requirements of the tubular target. DETAILED DESCRIPTION

[0050] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0051] Example 1

[0052] This embodiment provides a silicon-molybdenum alloy tubular target material, and the preparation method of the silicon-molybdenum alloy tubular target material comprises the following steps:

[0053] (1) Wet ball milling is performed at a rotation speed of 13 r / min for 24 hours to mix silicon powder, molybdenum powder and epoxy resin, and the obtained mixture is dried and then cold isostatically pressed at 200 MPa for 25 minutes to obtain a silicon-molybdenum alloy billet; the particle size of the silicon powder is 6 μm and the purity is 5N; the particle size of the molybdenum powder is 4 μm and the purity is 3N5; based on the total mass fraction of 100wt%, the mass of the molybdenum powder in the silicon powder and the molybdenum powder accounts for 30wt%, and the remainder is silicon powder; the mass of the epoxy resin is 0.6wt% of the total amount of the silicon powder and the molybdenum powder;

[0054] The ball milling medium used in the wet ball milling is anhydrous ethanol, and the mass of the anhydrous ethanol is 30wt% of the total amount of silicon powder, molybdenum powder and anhydrous ethanol; the ball milling balls used in the wet ball milling include zirconium oxide balls with diameters of 5mm, 10mm and 15mm, respectively, and the mass ratio is 1:10:10; the ratio of the mass of the ball milling balls to the total mass of silicon powder and molybdenum powder is 1:2;

[0055] (2) The silicon-molybdenum alloy blank obtained in step (1) is processed and then degreased, and then hot isostatically pressed in a stainless steel sheath at a temperature of 700° C., a pressure of 130 MPa, and a time of 3 h to obtain the silicon-molybdenum alloy tubular target.

[0056] Example 2

[0057] This embodiment provides a silicon-molybdenum alloy tubular target material, and the preparation method of the silicon-molybdenum alloy tubular target material comprises the following steps:

[0058] (1) Wet ball milling silicon powder, molybdenum powder and acrylic resin at a rotation speed of 10 r / min for 25 hours, and the obtained mixture is dried and then cold isostatically pressed at 150 MPa for 30 minutes to obtain a silicon-molybdenum alloy billet; the particle size of the silicon powder is 5 μm and the purity is 5N; the particle size of the molybdenum powder is 5 μm and the purity is 3N5; based on the total mass fraction of 100wt%, the mass of the molybdenum powder in the silicon powder and the molybdenum powder accounts for 10wt%, and the remainder is silicon powder; the mass of the acrylic resin is 0.2wt% of the total amount of the silicon powder and the molybdenum powder;

[0059] The ball milling medium used in the wet ball milling is anhydrous ethanol, and the mass of the anhydrous ethanol is 20wt% of the total amount of silicon powder, molybdenum powder and anhydrous ethanol; the ball milling balls used in the wet ball milling include zirconium oxide balls with diameters of 5mm, 10mm and 15mm, respectively, and the mass ratio is 1:9:9; the ratio of the mass of the ball milling balls to the total mass of silicon powder and molybdenum powder is 1:1.5;

[0060] (2) The silicon-molybdenum alloy blank obtained in step (1) is processed and then degreased, and then hot isostatically pressed in a stainless steel sheath at a temperature of 600° C., a pressure of 150 MPa, and a time of 4 h to obtain the silicon-molybdenum alloy tubular target.

[0061] Example 3

[0062] This embodiment provides a silicon-molybdenum alloy tubular target material, and the preparation method of the silicon-molybdenum alloy tubular target material comprises the following steps:

[0063] (1) Wet ball milling is performed at a rotation speed of 15 r / min for 23 hours to mix silicon powder, molybdenum powder and polyimide resin, and the obtained mixture is dried and then cold isostatically pressed at 250 MPa for 15 minutes to obtain a silicon-molybdenum alloy billet; the particle size of the silicon powder is 8 μm and the purity is 5N; the particle size of the molybdenum powder is 3 μm and the purity is 3N5; based on the total mass fraction of 100wt%, the mass of the molybdenum powder in the silicon powder and the molybdenum powder accounts for 50wt%, and the remainder is silicon powder; the mass of the polyimide resin is 1wt% of the total amount of the silicon powder and the molybdenum powder;

[0064] The ball milling medium used in the wet ball milling is anhydrous ethanol, and the mass of the anhydrous ethanol is 50wt% of the total amount of silicon powder, molybdenum powder and anhydrous ethanol; the ball milling balls used in the wet ball milling include zirconium oxide balls with diameters of 5mm, 10mm and 15mm, respectively, and the mass ratio is 1:11:11; the ratio of the mass of the ball milling balls to the total mass of silicon powder and molybdenum powder is 1:2.5;

[0065] (2) The silicon-molybdenum alloy blank obtained in step (1) is processed and then degreased, and then hot isostatically pressed in a stainless steel sheath at a temperature of 900° C., a pressure of 100 MPa, and a time of 2 h to obtain the silicon-molybdenum alloy tubular target.

[0066] Example 4

[0067] This embodiment provides a silicon-molybdenum alloy tubular target. The difference between the preparation method of the silicon-molybdenum alloy tubular target and that of Example 1 is that, except for adjusting the mass of the epoxy resin in step (1) to 0.1wt% of the total amount of silicon powder and molybdenum powder, the rest is the same as that of Example 1.

[0068] Example 5

[0069] This embodiment provides a silicon-molybdenum alloy tubular target. The difference between the preparation method of the silicon-molybdenum alloy tubular target and that of Example 1 is that, except for adjusting the mass of the epoxy resin in step (1) to 1.5wt% of the total amount of silicon powder and molybdenum powder, the rest is the same as that of Example 1.

[0070] Example 6

[0071] This embodiment provides a silicon-molybdenum alloy tubular target. The difference between the preparation method of the silicon-molybdenum alloy tubular target and that of Example 1 is that, except that the ball milling balls used for the wet ball milling mixing in step (1) are replaced with a single 10 mm diameter zirconia ball, the rest is the same as that of Example 1.

[0072] Example 7

[0073] This embodiment provides a silicon-molybdenum alloy tubular target material. The difference between the preparation method of the silicon-molybdenum alloy tubular target material and that of Embodiment 1 is that, except for adjusting the pressure of the cold isostatic pressing treatment in step (2) to 130 MPa, the rest is the same as that of Embodiment 1.

[0074] Example 8

[0075] This embodiment provides a silicon-molybdenum alloy tubular target material. The difference between the preparation method of the silicon-molybdenum alloy tubular target material and that of Embodiment 1 is that, except for adjusting the pressure of the cold isostatic pressing treatment in step (2) to 270 MPa, the rest is the same as that of Embodiment 1.

[0076] Example 9

[0077] This embodiment provides a silicon-molybdenum alloy tubular target. The difference between the preparation method of the silicon-molybdenum alloy tubular target and that of Embodiment 1 is that, except for adjusting the temperature of the hot isostatic pressing sintering in step (2) to 550° C., the rest is the same as that of Embodiment 1.

[0078] Example 10

[0079] This embodiment provides a silicon-molybdenum alloy tubular target. The difference between the preparation method of the silicon-molybdenum alloy tubular target and that of Embodiment 1 is that, except for adjusting the temperature of the hot isostatic pressing sintering in step (2) to 950° C., the rest is the same as that of Embodiment 1.

[0080] Comparative Example 1

[0081] This comparative example provides a silicon-molybdenum alloy tubular target material. The difference between the preparation method of the silicon-molybdenum alloy tubular target material and that of Example 1 is that epoxy resin is not added in step (1), and the degreasing treatment is adaptively deleted in step (2). The rest is the same as that of Example 1.

[0082] Comparative Example 2

[0083] This comparative example provides a silicon-molybdenum alloy tubular target material. The preparation method of the silicon-molybdenum alloy tubular target material is different from that of Example 1 in that the wet ball milling mixing in step (1) is adjusted to dry milling, and anhydrous ethanol is adaptively removed. The rest is the same as Example 1.

[0084] The silicon-molybdenum alloy tubular targets provided in Examples 1-10 and Comparative Examples 1 and 2 were subjected to a SEM test for structural uniformity, and the results obtained were classified as "uniform", "relatively uniform", and "uneven". The density was measured by the Archimedean drainage method and the average value was taken to calculate the density. The results are shown in Table 1.

[0085] Table 1

[0086]

[0087]

[0088] It can be seen from Table 1 that the silicon-molybdenum alloy tubular target material prepared by the preparation method provided by the present invention has good internal uniformity and density, high blank strength, easy processing and forming, and can prepare a large-sized silicon-molybdenum alloy tubular target material with a high silicon content;

[0089] By comparing Example 1 with Examples 4 and 5, it can be seen that if the amount of binder is too low, the strength of the blank cannot be improved, and if the amount is too high, the ball milling mixing uniformity of silicon powder and molybdenum powder cannot be effectively improved; by comparing Example 1 with Example 6, it can be seen that the use of ball milling balls with a single diameter reduces the powder mixing effect, which in turn leads to a decrease in the internal uniformity of the prepared silicon-molybdenum alloy tubular target; by comparing Example 1 with Examples 7-10, it can be seen that the selection of cold isostatic pressing pressure and hot isostatic pressing temperature needs to be within a reasonable range. Exceeding the limited range will reduce the internal uniformity and density of the silicon-molybdenum alloy tubular target.

[0090] By comparing Example 1 with Comparative Example 1, it can be seen that without adding a binder, the strength of the blank will be significantly reduced, resulting in poor processing performance and inability to achieve the forming of large-sized tubular targets; by comparing Example 1 with Comparative Example 2, it can be seen that the powder mixing effect is significantly reduced by dry grinding compared to wet ball milling, thereby reducing the internal uniformity and density of the silicon-molybdenum alloy tubular target.

[0091] In summary, the preparation method of the silicon-molybdenum alloy tubular target provided by the present invention adopts the process of wet ball milling to mix silicon powder and molybdenum powder to improve the uniformity of the mixed powder; by adding a binder to improve its forming performance, thereby realizing the forming of large-size tubular targets and improving the mechanical processing performance of green billets; finally, hot isostatic pressing is used for densification. The prepared silicon-molybdenum alloy tubular target has high density and good internal uniformity, and can meet the high performance requirements as a tubular target.

[0092] The above description is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention are within the protection scope and disclosure scope of the present invention.

Claims

1. A method for preparing a silicon-molybdenum alloy tubular target, characterized in that: The preparation method comprises the following steps: (1) mixing silicon powder, molybdenum powder and a binder by wet ball milling, and subjecting the obtained mixture to cold isostatic pressing to obtain a silicon-molybdenum alloy billet; (2) The silicon-molybdenum alloy blank obtained in step (1) is subjected to degreasing treatment and hot isostatic pressing sintering in sequence to obtain the silicon-molybdenum alloy tubular target.

2. The preparation method according to claim 1, characterized in that: The particle size of the silicon powder in step (1) is 5-8 μm; Preferably, the purity of the silicon powder in step (1) is 5N; Preferably, the particle size of the molybdenum powder in step (1) is 3-5 μm; Preferably, the purity of the molybdenum powder in step (1) is 3N5; Preferably, based on the total mass fraction of 100wt%, in the silicon powder and molybdenum powder in step (1), the mass fraction of molybdenum powder is 10-50wt%, and the remainder is silicon powder.

3. The preparation method according to claim 1 or 2, characterized in that: The adhesive in step (1) comprises any one of epoxy resin, acrylic resin or polyimide resin or a combination of at least two thereof; Preferably, the mass of the binder in step (1) is 0.2-1wt% of the total amount of silicon powder and molybdenum powder.

4. The preparation method according to any one of claims 1 to 3, characterized in that The ball milling medium used in the wet ball milling mixing in step (1) includes anhydrous ethanol; Preferably, the mass of the anhydrous ethanol is 20-50wt% of the total amount of silicon powder, molybdenum powder and anhydrous ethanol; Preferably, the ball milling balls used for the wet ball milling in step (1) include zirconium oxide balls with diameters of 5 mm, 10 mm and 15 mm, respectively, with a mass ratio of 1:(9-11):(9-11); Preferably, the ratio of the mass of the ball milling balls used in the wet ball milling mixing in step (1) to the total mass of the silicon powder and the molybdenum powder is 1:(1.5-2.5); Preferably, the rotation speed of the wet ball milling mixing in step (1) is 10-15 r / min; Preferably, the wet ball milling mixing time in step (1) is 23-25 ​​hours.

5. The preparation method according to any one of claims 1 to 4, characterized in that: The mixed material in step (1) is dried before cold isostatic pressing; Preferably, the pressure of the cold isostatic pressing treatment in step (1) is 150-250 MPa; Preferably, the holding time of the cold isostatic pressing treatment in step (1) is 15-30 minutes.

6. The preparation method according to any one of claims 1 to 5, characterized in that: The silicon-molybdenum alloy blank is processed before the degreasing treatment in step (2).

7. The preparation method according to any one of claims 1 to 6, characterized in that: The temperature of the hot isostatic pressing sintering in step (2) is 600-900° C. Preferably, the hot isostatic pressing sintering pressure in step (2) is 100-150 MPa; Preferably, the hot isostatic pressing sintering time in step (2) is 2-4 hours; Preferably, the hot isostatic pressing sintering in step (2) is carried out in a stainless steel jacket.

8. The preparation method according to claim 1, characterized in that: The preparation method comprises the following steps: (1) Wet ball milling silicon powder, molybdenum powder and a binder for 23-25 ​​hours at a rotation speed of 10-15 r / min, and drying the resulting mixture and cold isostatic pressing it at 150-250 MPa for 15-30 min to obtain a silicon-molybdenum alloy billet; the particle size of the silicon powder is 5-8 μm and the purity is 5N; the particle size of the molybdenum powder is 3-5 μm and the purity is 3N5; based on the total mass fraction of 100wt%, the mass of the molybdenum powder in the silicon powder and the molybdenum powder accounts for 10-50wt%, and the remainder is silicon powder; the mass of the binder is 0.2-1wt% of the total amount of the silicon powder and the molybdenum powder; The ball milling medium used in the wet ball milling mixing includes anhydrous ethanol, and the mass of the anhydrous ethanol is 20-50wt% of the total amount of silicon powder, molybdenum powder and anhydrous ethanol; the ball milling balls used in the wet ball milling mixing include zirconium oxide balls with diameters of 5mm, 10mm and 15mm, respectively, and the mass ratio is 1:(9-11):(9-11); the ratio of the mass of the ball milling balls to the total mass of silicon powder and molybdenum powder is 1:(1.5-2.5); (2) The silicon-molybdenum alloy blank obtained in step (1) is degreased after processing, and then hot isostatically pressed in a stainless steel sheath at a temperature of 600-900° C., a pressure of 100-150 MPa, and a time of 2-4 h to obtain the silicon-molybdenum alloy tubular target.

9. A silicon-molybdenum alloy tubular target, characterized in that: The silicon-molybdenum alloy tubular target is prepared by the method for preparing the silicon-molybdenum alloy tubular target according to any one of claims 1 to 8.

10. An application of the silicon-molybdenum alloy tubular target as claimed in claim 9, characterized in that: The silicon-molybdenum alloy tubular target is used for preparing electronic gate materials or electronic thin films.

Citation Information

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