Metal-Si powder, method for producing the same, and method for producing a metal-Si sintered body, a sputtering target, and a metal-Si thin film.

The use of a gas atomization method to create a metal-Si powder with crystalline phase particles addresses the strength and cracking issues of silicide-based sputtering targets, enhancing the productivity and yield of thin film manufacturing by producing a high-strength, low-oxygen sputtering target and film.

JP7831285B2Active Publication Date: 2026-03-17TOSOH CORP
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Patent Information

Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Filing Date
2021-05-24
Publication Date
2026-03-17

AI Technical Summary

Technical Problem

Existing sputtering targets containing silicides like CrSi2 have low strength and are prone to cracking during processing and discharge, making them difficult to use effectively in industrial thin film manufacturing.

Method used

A metal-Si powder is produced using a gas atomization method that incorporates multiple crystalline phase particles, resulting in a sintered body with low oxygen content and high strength, which is then used to create a sputtering target and thin film.

Benefits of technology

The method produces a sputtering target and thin film with improved strength and reduced oxygen content, reducing cracking and particle generation, thereby increasing productivity and yield in thin film manufacturing.

✦ Generated by Eureka AI based on patent content.

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Abstract

This metal-Si based powder contains metal-Si based particles including multiple crystal phase particles. The crystal phase particles include a crystal phase containing a compound of a metal and Si. The crystal phase particles have an average particle diameter of, for example, 20 μm or less. The metal-Si based particles have an average particle diameter of, for example, 5-100 μm.
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Description

[Technical Field]

[0001] The present invention relates to metal-Si powder, a method for producing the same, and a method for producing a metal-Si sintered body, a sputtering target, and a metal-Si thin film. [Background technology]

[0002] In recent years, silicides such as CrSi2 have been used as thin films in many technological fields, including semiconductors and solar cells, due to their high resistivity (unit: Ω·cm) which is less susceptible to temperature changes. In industrial thin film manufacturing, sputtering using sputtering targets is widely used. However, compositions containing silicides such as CrSi2 generally have low strength and may crack during processing on the sputtering target and during discharge during film deposition. For this reason, compositions containing silicides are known to be difficult to use as sputtering targets.

[0003] Patent Document 1 below discloses a method for manufacturing a sputtering target containing a Cr phase, a Si phase, and a silicide compound in the target material by thermal spraying in order to improve the strength of the sputtering target.

[0004] Patent Document 2 below discloses a method for producing a composition having a eutectic aggregate containing Si and silicide by melting.

[0005] Patent documents 3 and 4 below also disclose sputtering targets containing Si and silicide. [Prior art documents] [Patent Documents]

[0006] [Patent Document 1] Japanese Patent Application Publication No. 2017-82314 [Patent Document 2] Japan Special Publication No. 2013-502368 [Patent Document 3] Japanese Patent Publication No. 2002-173765 [Patent Document 4] Japanese Patent Publication No. 2003-167324 [Overview of the project] [Problems that the invention aims to solve]

[0007] However, the compositions or sputtering targets described in the above-mentioned Patent Documents 1 to 4 had room for improvement in terms of achieving both low oxygen content and high strength.

[0008] The object of the present invention is to provide a metal-Si powder capable of producing a sintered body having low oxygen content and high strength, a method for producing the same, and a method for producing a metal-Si sintered body, a sputtering target, and a metal-Si thin film. [Means for solving the problem]

[0009] The inventors of the present invention conducted thorough research on silicide-based powders and found that, for example, by using a gas atomization method, it is possible to incorporate multiple crystalline phase particles into the metal-Si particles contained in the metal-Si powder, resulting in a sintered body obtained by firing the metal-Si powder that has a low oxygen content and high strength. This led to the completion of the present invention.

[0010] In other words, the first aspect of the present invention is as follows: A first aspect of the present invention is a metal-Si powder containing metal-Si particles comprising a plurality of crystalline phase particles, wherein the crystalline phase particles include a crystalline phase comprising a compound of metal and Si. The above-mentioned metal-Si powder can be used to produce sintered bodies with low oxygen content and high strength.

[0011] In the above-mentioned metal-Si powder, it is preferable that the crystalline phase particles have an average particle size of 20 μm or less. In this case, a sintered body with higher strength can be manufactured compared to the case where the average particle size of the crystalline phase exceeds 20 μm.

[0012] In the above metal-Si based powder, it is preferable that the metal-Si based particles have an average particle size of 5 to 100 μm. In this case, compared with the case where the average particle size of the metal-Si based particles is less than 5 μm, the specific surface area of the metal-Si based particles becomes smaller, and the amount of oxygen in the sintered body can be made smaller. On the other hand, compared with the case where the average particle size of the metal-Si based particles is greater than 100 μm, the quenching effect by the gas atomization method becomes larger, and the crystal phase particles are less likely to coarsen, so the strength of the sintered body can be made greater.

[0013] In the above metal-Si based powder, it is preferable that the metal-Si based particles further contain a substance that fills the gaps between the plurality of crystal phase particles, and the substance is composed of a crystal phase. In this case, the plurality of crystal phase particles are less likely to be separated by the substance, and the strength of the metal-Si based powder is further improved.

[0014] In the above metal-Si based powder, it is preferable that the metal-Si based particles contain two types of crystal phases. In this case, compared with the case where the metal-Si based particles are composed of a single crystal phase, the grain growth of the crystal phase particles is suppressed, and the crystal phase particles become fine particles. Therefore, the metal-Si based powder becomes higher in strength.

[0015] In the above metal-Si based powder, it is preferable that the two types of crystal phases are composed of a first crystal phase made of silicide and a second crystal phase made of Si. In this case, since the crystal phase particles are composed of two different crystal phases, the grain growth of the crystal phase particles is suppressed and becomes fine particles. Therefore, the metal-Si based powder becomes higher in strength.

[0016] [[ID=第26]]In the above metal-Si based powder, it is preferable that the content of the first crystal phase is greater than the content of the second crystal phase. In this case, compared to the case where the content of the first crystalline phase is less than or equal to the content of the second crystalline phase, the proportion of high-strength crystalline phase particles increases, resulting in a higher strength for the metal-Si based powder.

[0017] In the above-mentioned metal-Si powder, the metal is preferably Cr. In this case, the metal-Si powder makes it possible to manufacture thin films that are less susceptible to temperature changes and have high resistivity.

[0018] The above metal-Si powder preferably contains 0.5 wt% or less of oxygen. In this case, it is possible to suppress the generation of particles when manufacturing films (thin films) using a sputtering target obtained using a sintered body of metal-Si powder, and to improve the yield of the film product.

[0019] In the above-mentioned metal-Si powder, it is preferable that the relative density of the lightly loaded material to the true density is 50% or more. In this case, compared to the case where the relative density of the lightly loaded material to the true density is less than 50%, the shrinkage of the metal-Si powder during firing is reduced, making it possible to produce a near-net sintered body. Furthermore, the usefulness of the metal-Si powder as a powder for additive manufacturing can be enhanced.

[0020] A second aspect of the present invention is a method for producing the above-described metal-Si powder, comprising the steps of: heating and melting a mixture of metal and Si to form a melt; and injecting gas into the melt. According to the above manufacturing method, a metal-Si powder can be produced that can create a sintered body with low oxygen content and high strength.

[0021] A third aspect of the present invention is a metal-Si sintered body obtained by firing the metal-Si powder described above. The above metal-Si sintered body can have low oxygen content and high strength.

[0022] The above metal-Si sintered body preferably contains sintered particles having an average particle size of 40 μm or less. In this case, the strength of the sintered body increases dramatically compared to the case where the average particle size of the sintered particles is larger than 40 μm.

[0023] The above metal-Si sintered body preferably contains 0.5 wt% or less of oxygen and has a flexural strength of 100 MPa or more. In this case, the generation of particles when manufacturing films (thin films) using a sputtering target obtained by firing a sintered body of metal-Si powder can be suppressed, and the yield of films (film products) can be improved. Furthermore, if the strength of the sintered body is high, cracking is less likely to occur during grinding and bonding processes when joining the sintered body to a substrate. As a result, the yield of film products is increased, and the productivity of film products is improved. Moreover, even when high power is applied to the sintered body during sputtering, cracking problems are less likely to occur.

[0024] A fourth aspect of the present invention is a sputtering target comprising the metal-Si sintered body described above. The above-described sputtering target can have low oxygen content and high strength. Therefore, the sputtering target is less likely to crack even when the output of the sputtering equipment is high, which makes it possible to increase the productivity of manufacturing thin films, and because it has a low oxygen content, it is possible to suppress the generation of particles due to abnormal discharge during sputtering.

[0025] A fifth aspect of the present invention is a method for manufacturing a thin film, which includes the step of performing sputtering using the above-described sputtering target to form a thin film on the surface of a substrate. The above method for manufacturing thin films makes it possible to increase the productivity of manufacturing thin films because the sputtering target is less likely to crack even when the output of the sputtering apparatus is high. Furthermore, because the sputtering target has a low oxygen content, it is possible to suppress the generation of particles due to abnormal discharge during sputtering.

[0026] Furthermore, the aspects of the present invention may be as follows. (1) A metal-Si powder characterized in that each powder contains two or more crystalline phase particles measuring 1 to 20 μm, and the average particle size is 5 to 100 μm. (2) The metal-Si powder described in (1), wherein the metal is Cr (chromium). (3) The metal-Si powder described in (1) or (2), wherein the oxygen content is 0.5 wt% or less. (4) A metal-Si powder according to any one of (1) to (3), characterized in that the relative density of the lightly packed powder is 50% or more. (5) A method for producing a metal-Si powder according to any one of (1) to (4), characterized by mixing metal flakes and silicon (Si) flakes, heating and melting them, and spraying a high-pressure gas onto the melted liquid that has been dropped. (6) A metal-Si sintered body made from any of the powders described in (1) to (4). (7) A metal-Si sintered body as described in (6), wherein the average particle size is 40 μm or less, the oxygen content is 0.5 wt% or less, and the flexural strength is 100 MPa or more. (8) The metal-Si sintered body according to (6) or (7), wherein the metal is Cr (chromium). A sputtering target characterized by being made of a metal-Si sintered body as described in any of (9), (6) to (8). A method for manufacturing a thin film, characterized by sputtering using the sputtering target described in (10)(9). [Effects of the Invention]

[0027] The present invention provides a metal-Si-based powder capable of producing a sintered body having low oxygen content and high strength, a method for producing the same, and a method for producing a metal-Si-based sintered body, a sputtering target, and a metal-Si-based thin film. [Brief explanation of the drawing]

[0028] [Figure 1]This is a schematic cross-sectional view showing an example of a metal-Si-based powder representing the first aspect of the present invention. [Figure 2] This is a cross-sectional view showing a metal-Si sintered body, representing a third aspect of the present invention. [Figure 3] This is a cross-sectional view showing a thin film formed by the fifth method for forming a thin film according to the present invention. [Figure 4] This figure shows an SEM image of the cross-section of the powder obtained in Example 1. [Figure 5] This figure shows an SEM image of the powder obtained in Comparative Example 2. [Modes for carrying out the invention]

[0029] The present invention will be described in detail below.

[0030] <Metal-Si powder> First, the first aspect of the present invention, the metal-Si powder, will be described with reference to Figure 1. Figure 1 is a schematic cross-sectional view showing an example of the metal-Si powder of the first aspect of the present invention. As shown in Figure 1, the metal-Si powder 10 of the first aspect of the present invention contains metal-Si particles 10A, which include a plurality of crystalline phase particles 11, and the crystalline phase particles 11 include a crystalline phase containing a compound of metal and Si.

[0031] According to the above metal-Si powder 10, a sintered body with low oxygen content and high strength can be manufactured.

[0032] Although the reason for obtaining the above effects is not clear, the inventors of this invention surmise that the above effects are obtained for the following reasons. Specifically, the inclusion of multiple crystalline phase particles 11 in the metal-Si particles 10A reduces the specific surface area, thereby reducing the amount of oxygen adsorbed on the crystalline phase particles 11 (adsorbed oxygen amount). Thus, the metal-Si particles 10A can reduce the amount of oxygen in the sintered body. Furthermore, the inclusion of multiple crystalline phase particles 11 in the metal-Si particles 10A results in fine crystalline phase particles 11, and when stress is applied to the metal-Si particles 10A, that stress is dispersed among the multiple crystalline phase particles 11, making it possible to manufacture a high-strength sintered body.

[0033] The metal-Si powder 10 may consist of only one metal-Si particle 10A, or it may consist of an aggregate of metal-Si particles 10A.

[0034] The number of crystalline phase particles 11 in the metal-Si-based particles 10A may be several, but is preferably 10 or more, more preferably 40 or more, and particularly preferably 100 or more. However, it is preferable that the number of crystalline phase particles 11 in the metal-Si-based particles 10A be 500 or less. In this case, the surface irregularities of the aggregate of crystalline phase particles 11 are reduced, and the amount of adsorbed oxygen can be further reduced. Here, the crystalline phase particles 11 contain a crystalline phase. The presence of a crystalline phase in the crystalline phase particles 11 can be confirmed by the EBSD (Electron Back Scatter Diffraction) method. Specifically, a cross-section of the metal-Si-based powder 10 (the surface exposed after cutting the metal-Si-based powder 10) is tilted by 70° in a scanning electron microscope, and an electron beam is irradiated onto the crystalline phase particles 11 in that cross-section. The diffraction pattern from the crystalline phase particles 11 is obtained, and the presence or absence of a crystalline phase can be confirmed based on the image of this diffraction pattern.

[0035] The average particle size of the crystalline phase particles 11 is not particularly limited, but is preferably 20 μm or less, more preferably 10 μm or less, and especially preferably 5 μm or less.

[0036] When the average particle size of the crystalline phase particles 11 is 20 μm or less, a sintered body with higher strength can be manufactured compared to when the average particle size of the crystalline phase particles 11 exceeds 20 μm. From the viewpoint of increasing the strength of the sintered body, it is preferable that the average particle size of the crystalline phase particles 11 be 1 μm or more.

[0037] The average particle size of the metal-Si particles 10A is not particularly limited as long as it is larger than the average particle size of the crystalline phase particles 11, and is preferably 5 to 100 μm. In this case, compared to the case where the average particle size is smaller than 5 μm, the specific surface area of ​​the metal-Si particles 10A becomes smaller, and the amount of oxygen in the sintered body can be reduced. On the other hand, compared to the case where the average particle size is larger than 100 μm, the rapid cooling effect by the gas atomization method is greater, and the crystalline phase particles 11 are less likely to coarseen, so the strength of the sintered body can be increased. The average particle size of the metal-Si particles 10A is more preferably 10 to 70 μm, and even more preferably 15 to 40 μm.

[0038] The metal-Si particles 10A may consist only of a plurality of crystalline phase particles 11, but as shown in Figure 1, they may also contain a substance 12 that fills the gaps between the plurality of crystalline phase particles 11. In this case, the substance 12 is composed of a crystalline phase. By further including the substance 12 in the metal-Si particles 10A, the plurality of crystalline phase particles 11 become less likely to separate due to the substance 12, and the strength of the metal-Si powder 10 is further improved.

[0039] The metal-Si particles 10A in the metal-Si powder 10 can have different structures depending on the number of crystalline phases. In the case of a single-phase powder with one crystalline phase, only the crystalline phase particles 11 made up of that crystalline phase aggregate to form a particle (a single metal-Si particle 10A). In the case of a two-phase powder with two crystalline phases, the larger proportion of the crystalline phase forms crystalline phase particles 11, while the smaller proportion of the crystalline phase does not form crystalline phase particles 11 but instead fills the spaces between the crystalline phase particles 11 and exists within the substance 12. The substance 12 is composed of two types of crystalline phases and is finer than the crystalline phase particles 11. The substance 12 may also have, for example, a layered structure. In this case, particles (metal-Si particles 10A) are formed by the aggregation of these crystalline phase particles 11 and the layered substance 12.

[0040] The metal-Si particles 10A may contain two types of crystalline phases or be composed of a single crystalline phase, but it is preferable that they contain two types of crystalline phases. In this case, compared to when the metal-Si particles 10A are composed of a single crystalline phase, grain growth of the crystalline phase particles is suppressed, and the crystalline phase particles become finer. As a result, the metal-Si powder 10 becomes stronger.

[0041] When the metal-Si-based particles 10A contain two types of crystalline phases, it is preferable that the two crystalline phases consist of a first crystalline phase made of silicide and a second crystalline phase made of Si. In this case, since the crystalline phase particles are composed of two different crystalline phases (crystalline structures), grain growth of the crystalline phase particles is suppressed, resulting in a finer structure. Therefore, the metal-Si-based powder 10 becomes stronger.

[0042] The content of the first crystalline phase may be greater than or less than the content of the second crystalline phase, but it is preferable that it be greater than the content of the second crystalline phase. In this case, the proportion of high-strength crystalline phase particles is higher compared to the case where the content of the first crystalline phase is less than or equal to the content of the second crystalline phase, so the metal-Si powder 10 becomes stronger.

[0043] The content of the first crystalline phase in the metal-Si particles 10A is not particularly limited, but is preferably 30 wt% or more, more preferably 40 wt% or more, and particularly preferably 50 wt% or more. In this case, compared to the case where the content of the first crystalline phase in the metal-Si particles 10A is less than 30 wt%, the proportion of high-strength crystalline phase particles increases, resulting in higher strength for the metal-Si powder 10. However, the content of the first crystalline phase in the metal-Si particles 10A is preferably 95 wt% or less, and more preferably 90 wt% or less.

[0044] Examples of metals in the metal-Si compound contained in the crystalline phase particles 11 include chromium (Cr), molybdenum (Mo), tungsten (W), barium (Ba), calcium (Ca), magnesium (Mg), strontium (Sr), iron (Fe), titanium (Ti), tantalum (Ta), and cobalt (Co). Among these, chromium (Cr), molybdenum (Mo), and tungsten (W) are preferred metals, with chromium (Cr) being particularly preferred. In this case, the metal-Si powder 10 can be used to produce a thin film that is less susceptible to temperature changes and has high resistivity.

[0045] The oxygen content of the metal-Si powder 10 is preferably 0.5 wt% or less, more preferably 0.1 wt% or less, even more preferably 0.05 wt% or less, and particularly preferably 0.03 wt% or less. When the oxygen content of the metal-Si powder 10 is 0.5 wt% or less, the generation of particles when manufacturing a film (thin film) using a sputtering target obtained using a sintered body of the metal-Si powder 10 can be suppressed, and the yield of the film product can be improved.

[0046] The relative density of the lightly loaded powder 10 to the true density is not particularly limited, but is preferably 50% or more. In this case, compared to the case where the relative density of the lightly loaded powder 10 to the true density is less than 50%, the amount of shrinkage of the metal-Si powder 10 during firing is reduced, making it possible to produce a near-net sintered body. Furthermore, the usefulness of the metal-Si powder 10 as a powder for additive manufacturing can be increased. The relative density of the lightly loaded powder 10 to the true density is more preferably 55% or more, and even more preferably 60% or more.

[0047] The metal-Si powder 10 preferably has a total amount of metal impurities of 300 ppm by mass or less, and particularly preferably 200 ppm by mass or less. Here, metal impurities refer to metals other than the metals that make up the metal-Si powder 10, and whose concentration is 1000 ppm by mass or less.

[0048] In particular, when the metal constituting the metal-Si powder 10 is a metal other than Fe, Mn, Mg, Ca, Sr, and Ba, the total amount of Fe and Mn is preferably 100 ppm by mass or less, and especially preferably 50 ppm by mass or less. Compared to the case where the total amount of Fe and Mn exceeds 100 ppm by mass, the metal-Si powder 10 makes it possible to produce a thin film that is less susceptible to temperature changes and has high resistivity.

[0049] Furthermore, when the metal constituting the metal-Si powder 10 is a metal other than Fe, Mn, Mg, Ca, Sr, and Ba, the total amount of Mg, Ca, Sr, and Ba is preferably 3 ppm by mass or less, and particularly preferably 2 ppm by mass or less. Compared to the case where the total amount of Mg, Ca, Sr, and Ba exceeds 3 ppm by mass, the metal-Si powder 10 makes it possible to produce a thin film that is less susceptible to temperature changes and has high resistivity.

[0050] <Method for producing metal-Si powder> Next, a method for producing metal-Si-based powder, which is a second aspect of the present invention, will be described.

[0051] The present invention provides a method for producing metal-Si powder, which includes the steps of heating and melting a mixture of metal and silicon (Si) as raw materials to form a molten material, and injecting gas into the molten material.

[0052] The purity of the raw materials, metal and silicon (Si), is not particularly limited, but is preferably 99.9% or higher, and more preferably 99.99% or higher. When the purity is 99.9% or higher, the metal-Si powder 10 is less likely to cause abnormal grain growth during the firing process to form a sintered body by firing the metal-Si powder 10, and less likely to be a source of particles during film formation, compared to when the purity is less than 99.9%. Furthermore, it is preferable that the oxygen content in the raw materials is low. When the oxygen content in the raw materials is low, the oxygen content in the final sputtering target is also low, making the metal-Si powder 10 less likely to cause particle generation.

[0053] The shape of the metal and silicon is not particularly limited, but flake form is preferred. In this case, the specific surface area of ​​the raw materials is reduced, and the amount of oxygen in the resulting metal-Si powder and sintered body can be further reduced. The above mixture can be obtained by mixing the metal and silicon.

[0054] In the process of injecting gas into the molten liquid, the molten liquid may or may not be dispensed by dripping.

[0055] In the process of injecting gas into a molten liquid, "injecting" can also be expressed as "spraying."

[0056] As a method for producing the metal-Si-based powder described above, gas atomization is preferred.

[0057] Gas compositing is a technique for producing powder by mixing raw materials, heating and melting them to form a molten liquid, and then rapidly cooling the resulting particles by injecting or spraying a gas such as high-pressure gas into the molten liquid that has been dropped onto the mixture.

[0058] In particular, the metal-Si powder 10 produced by the gas atomization method is preferably a powder with an average particle size (50% particle size) of 5 to 100 μm, more preferably 10 to 70 μm, and especially preferably 15 to 40 μm.

[0059] A characteristic of powders obtained by the gas atomization method is that they contain fine crystalline phase particles within the metal-Si particles. Because the crystalline phase particles have a small surface area and are fine-grained, the sintered body obtained by firing the powder can be made with low oxygen content and high strength. On the other hand, it is possible to produce a sintered body with high strength even with a mixture of fine powders that do not contain crystalline phase particles within the metal-Si particles, but the oxygen content in the sintered body will be high. Furthermore, it is possible to obtain a sintered body with low oxygen content even with a mixture of coarse-grained powders that do not contain crystalline phase particles within the metal-Si particles, but the strength will be lower due to the large particle size of the coarse-grained powder.

[0060] In the heating and melting conditions, the heating temperature is preferably higher than the melting temperature, and the difference between the heating temperature and the melting temperature (ΔT) is preferably 50 to 300°C. More preferably, ΔT is 100 to 250°C. Here, the melting temperature represents the temperature at which the raw material powder melts. If ΔT is small, the phase with the higher melting point of the two crystalline phases precipitates first, making it difficult to refine the powder. On the other hand, if ΔT is large, the powders sinter together after gas atomization and adhere to the wall surface, resulting in poor powder recovery.

[0061] Inert gases such as argon (Ar), nitrogen (N2), and helium (He) can be used as the gas to be injected or sprayed.

[0062] The gas pressure is preferably 1 MPa or higher, more preferably 4 MPa or higher, and particularly preferably 7 MPa or higher. A gas pressure of 1 MPa or higher enhances the rapid cooling effect. Furthermore, a gas pressure of 10 MPa or lower is preferable. In this case, it is possible to prevent the equipment for producing metal-Si powder from becoming larger or the productivity of metal-Si powder from decreasing.

[0063] Gas atomization can be performed using either a crucible or an electrode method. When using the crucible method, a crucible is used. The material that can be used to construct the crucible is, for example, carbon, alumina, magnesia, silicon nitride, zirconia, or boron nitride. Furthermore, crucibles made of carbon, alumina, magnesia, or zirconia with a coating of boron nitride or silicon carbide can also be used.

[0064] Furthermore, it is preferable to manage the powder after gas atomization in a vacuum or in an inert atmosphere such as nitrogen or argon. In this case, oxidation is less likely to occur from the surface compared to leaving the powder in the atmosphere, and the amount of oxygen in the powder can be reduced.

[0065] <Metal-Si sintered body> Next, the third aspect of the present invention, the metal-Si sintered body, will be described with reference to Figure 2. Figure 2 is a cross-sectional view showing the third aspect of the present invention, the metal-Si sintered body.

[0066] As shown in Figure 2, the third aspect of the present invention, the metal-Si sintered body 20, is a sintered body obtained by sintering metal-Si powder 10 and contains sintered particles 21. The metal-Si sintered body 20 can have a low oxygen content and high strength.

[0067] The average particle size of the sintered particles 21 contained in the metal-Si sintered body 20 is not particularly limited, but is preferably 40 μm or less. In this case, the strength of the metal-Si sintered body 20 increases more rapidly compared to when the average particle size of the sintered particles 21 is larger than 40 μm. In order to stably increase the strength of the metal-Si sintered body 20, the average particle size is more preferably 20 μm or less, and particularly preferably 10 μm or less. The average particle size of the sintered particles 21 is preferably 1 μm or more. When the average particle size of the sintered particles 21 is 1 μm or more, grinding treatment becomes unnecessary, and impurities such as Fe and oxygen are less likely to be mixed in.

[0068] The oxygen content of the metal-Si sintered body 20 is preferably 0.5 wt% or less, more preferably 0.1 wt% or less, even more preferably 0.05 wt% or less, and particularly preferably 0.03 wt% or less, from the viewpoint of suppressing particle generation when manufacturing a film (thin film) using a sputtering target obtained by firing a sintered body of metal-Si powder 10, and improving the yield of the film product.

[0069] The flexural strength of the metal-Si sintered body 20 is not particularly limited, but is preferably 100 MPa or higher, more preferably 100 to 500 MPa, even more preferably 150 to 500 MPa, and particularly preferably 200 to 500 MPa. If the strength of the sintered body 20 is high, cracking is less likely to occur during grinding and bonding processes when joining the sintered body 20 to a substrate or the like. As a result, the yield of film-containing products (film products) is increased, and the productivity of film products is improved. Furthermore, even when high power is applied to the sintered body 20 during sputtering, cracking problems are less likely to occur.

[0070] The metal-Si sintered body 20 can be a one-phase sintered body or a two-phase sintered body depending on its composition, and a two-phase sintered body is preferred for forming a fine crystalline phase within the grains (sintered particles 21).

[0071] When the metal-Si sintered body 20 is a two-phase sintered body, both crystalline phase particles 11 and the two-phase material 12 are present. For example, in the case of a composition of 42 wt% chromium (Cr) and 58 wt% silicon (Si), the crystalline phase consists of two CrSi phases and a Si phase, the crystalline phase particles 11 are two CrSi phases, and the material 12 (two-phase system) consists of two CrSi phases and a Si phase. The crystalline phase particles 11 and the two-phase material 12 become finer as the cooling rate increases. The finer the crystalline phase particles 11 and the two-phase material 12, the higher the sintering density at low temperatures, resulting in a larger process margin during production. Therefore, the productivity of the metal-Si sintered body 20 is improved.

[0072] Examples of metals for the metal-Si sintered body 20 include chromium (Cr), molybdenum (Mo), tungsten (W), barium (Ba), calcium (Ca), magnesium (Mg), strontium (Sr), iron (Fe), titanium (Ti), tantalum (Ta), and cobalt (Co). Among these, chromium (Cr), molybdenum (Mo), and tungsten (W) are preferred, and chromium (Cr) is particularly preferred.

[0073] The metal-Si sintered body 20 can be manufactured, for example, by firing the metal-Si powder 10 under pressure.

[0074] For firing, a pressurized firing furnace such as a hot press furnace is used. In this case, the diffusion coefficient of silicon is higher compared to when using a non-pressurized furnace, making it easier to increase the density of the sintered body 20.

[0075] The hot press pressure during firing is preferably 50 MPa or less. In this case, compared to when the hot press pressure during firing exceeds 50 MPa, it is easier to prepare the pressurized hot press mold. When producing large sintered bodies, the hot press pressure is preferably 5 to 50 MPa, more preferably 5 to 20 MPa, and particularly preferably 5 to 10 MPa.

[0076] The firing temperature is preferably 1100°C to 1800°C. In this case, the density of the sintered body 20 increases sufficiently compared to when the firing temperature is below 1100°C, and it is possible to prevent the sintered body 20 from melting regardless of the hot press pressure, compared to when the firing temperature exceeds 1300°C.

[0077] The cooling rate after firing is not particularly limited and can be determined appropriately considering the capacity of the sintering furnace, the size and shape of the sintered body, its susceptibility to cracking, etc.

[0078] The holding time during firing should preferably be between 1 and 5 hours. A holding time shorter than 1 hour reduces temperature unevenness in the furnace and hot press mold, making it easier to obtain a uniform structure. Furthermore, productivity is improved compared to holding times longer than 5 hours.

[0079] There are no particular restrictions on the atmosphere during firing, but a vacuum or an inert atmosphere such as argon is preferred.

[0080] The metal-Si sintered body 20 can be processed into various shapes. A plate-shaped metal-Si sintered body 20 can be obtained, for example, by grinding it using a machining equipment such as a surface grinder, cylindrical grinder, lathe, cutting machine, or machining center.

[0081] <Sputtering target> Next, the sputtering target, a fourth aspect of the present invention, will be described. The sputtering target of the fourth aspect of the present invention includes a metal-Si sintered body 20. When the sputtering target is composed of a metal-Si sintered body 20, the metal-Si sintered body 20 shown in Figure 2 also serves as the sputtering target.

[0082] The above-described sputtering target can have low oxygen content and high strength. Therefore, the sputtering target is less likely to crack even when the output of the sputtering equipment is high, which makes it possible to increase the productivity of manufacturing thin films, and because it has a low oxygen content, it is possible to suppress the generation of particles due to abnormal discharge during sputtering.

[0083] The sputtering target may be bonded to a backing plate and backing tube made of oxygen-free copper or titanium, etc., using a bonding material such as indium solder, as needed.

[0084] <Method for manufacturing thin films> Next, the method for manufacturing the fifth side of the present invention will be described with reference to Figure 3. Figure 3 is a cross-sectional view showing a thin film formed by the method for forming the fifth side of the present invention.

[0085] As shown in Figure 3, the method for manufacturing a thin film of the present invention includes the step of forming a metal-Si thin film 41 on a substrate 42 by sputtering using the sputtering target described above, and obtaining a thin film formed body 40.

[0086] The above method for manufacturing a thin film makes it possible to increase the productivity of manufacturing the thin film 41 because the sputtering target is less likely to crack even when the output of the sputtering apparatus is high. Furthermore, because the sputtering target has a low oxygen content, it is possible to suppress the generation of particles due to abnormal discharge during sputtering.

[0087] The substrate 42 is not particularly limited as long as it is made of a material capable of supporting the thin film 41, but examples of substrates 42 include glass, silicon, and sapphire substrates.

[0088] The thickness of the thin film 41 can be, for example, 1 μm or less. [Examples]

[0089] The present invention will be described in more detail below with reference to examples, but the present invention is not limited thereto. , reference example In the comparative examples, the average particle size of crystalline phase particles, the average particle size of metal-Si particles, the density (relative density) of the sintered body, the average particle size of sintered particles constituting the sintered body, the flexural strength of the sintered body, the oxygen content, the amount of metal impurities, the relative density of the lightly loaded density to the true density, and the presence or absence of the crystalline phase in the crystalline phase particles were measured as follows.

[0090] (1) Average particle size of crystalline phase particles Samples were prepared by embedding powder obtained by the gas atomization method (gas atomized powder) in resin, cutting the samples, and polishing the cross-sections. Three arbitrary points on the cross-sections were then observed and photographed using a scanning electron microscope (SEM) under the following conditions. The particle size of the crystalline phase particles was measured from the obtained powder microstructure images (SEM images) using the diameter method, and the 50% particle size of the crystalline phase particles was calculated as the average particle size from the measured particle size. Particle size measurements were performed on all (more than 300) crystalline phase particles in the image. Here, the diameter method is a method in which the particle size of the crystalline phase particle is defined as the diameter at which the diameter of a circle is minimized when the entire crystalline phase particle is placed inside the circle. In this case, the diameter of the circle is minimized when the crystalline phase particle is in contact with the circumference of the circle at least at two points. (Observation conditions for scanning electron microscope) Acceleration voltage: 10kV Measurement magnification: 1500x

[0091] (2) Average particle size of metal-Si particles The average particle size of the metal-Si particles was calculated as follows: First, the metal-Si particles were passed through a multi-stage sieve (25, 32, 53, 75, 90, 106, 150, 250 μm), and the powder remaining on the sieve was collected to measure the particle size distribution of the powder. Then, based on the particle size distribution of the metal-Si particles, the particle size corresponding to D50 was calculated as the average particle size of the metal-Si particles.

[0092] (3) Density of the sintered body (relative density) The relative density d of the sintered body was measured in accordance with JIS R 1634. Specifically, the bulk density was measured by the Archimedes method, and the relative density of the sintered body was calculated based on the following formula. Relative density of sintered body = 100 × bulk density / true density The true density d1 of the sintered body is given by the weight a[g] of crystalline phase A and the weight b[g] of crystalline phase B, and the true density Ma[g / cm³] of each. 3 ], Mb[g / cm 3 It was calculated using the arithmetic mean expressed by the following formula. d1 = (a + b) / ((a / Ma) + (b / Mb))

[0093] (4) Average particle size of sintered particles constituting the sintered body After mirror-polishing one surface of the sintered body, three arbitrary points among the particles constituting the sintered body were observed and photographed using a scanning electron microscope under the following conditions. The particle size of the particles constituting the sintered body was measured from the obtained sintered body microstructure images using the diameter method, and the 50% particle size was calculated as the average particle size from the measured particle sizes. Particle size measurements were performed on all particles (more than 300) within the image. (Observation conditions for scanning electron microscope) Acceleration voltage: 10kV Measurement magnification: 1500

[0094] (5) Flexural strength of the sintered body The flexural strength of the sintered body was measured in accordance with JIS R 1601. Specifically, a sample was prepared, and the flexural strength was measured by performing a three-point bending test on this sample. The measurement conditions were as follows. (Measurement conditions for bending strength) Distance between fulcrums: 30mm Sample size: 3 x 4 x 40 mm Head speed: 0.5 mm / min

[0095] (6) Oxygen content The oxygen content of the powder and samples cut from any part of the sintered body surface after grinding at least 1 mm was used to analyze the oxygen content using the following measurement method and apparatus, and the analyzed value was defined as the oxygen content (measurement data). Measurement method: Impulse furnace melting - infrared absorption spectroscopy Equipment: Oxygen and nitrogen analyzer (LECO TC436 model)

[0096] (7) Amount of metal impurities For powder and samples cut from any portion after grinding at least 1 mm from the surface of the sintered body after firing, the amount of metal impurities was analyzed using the following measurement method, and the analytical value was defined as the amount of metal impurities (measurement data). Measurement method: Glow discharge mass spectrometry (GDMS)

[0097] (8) Relative density of lightly loaded equipment relative to true density The light packaging density of the powder was measured using the method specified in JIS Z 2504. The relative density (%) of the light packaging density to the true density of the powder was then calculated based on the following formula. Relative density (%) of light packaging density relative to true density of powder = 100 × Light density of powder / True density of powder The true density d2 of the powder is given by the weight a[g] of crystalline phase A and the weight b[g] of crystalline phase B, and the true density Ma[g / cm³] of each. 3 ], Mb[g / cm 3 It was calculated using the arithmetic mean expressed by the following formula. d2 = (a + b) / ((a / Ma) + (b / Mb))

[0098] (9) Presence or absence of crystalline phase in crystalline phase particles Samples were prepared by embedding powder obtained by the gas atomization method (gas atomized powder) in resin, cutting the samples, and polishing the cross-sections. The cross-sections were then tilted 70° in a scanning electron microscope, and electron beams were irradiated onto the crystalline phase particles in the cross-section. Diffraction patterns from the crystalline phase particles were obtained, and the presence or absence of the crystalline phase in the crystalline phase particles was confirmed based on the image of these diffraction patterns. If a diffraction pattern was observed, it was determined that the crystalline phase particles contained the crystalline phase.

[0099] (Example 1) The powder was prepared by gas atomization as follows. Specifically, first, Cr flakes (4N) and Si flakes (5N) were mixed in a carbon crucible to obtain a mixture. At this time, the content of Cr flakes (4N) and Si flakes (5N) in the mixture was set to 42 wt% and 58 wt%, respectively. Then, the Cr flakes and Si flakes were melted in the carbon crucible at a melting temperature of 1650°C to form a molten metal, which was then dropped, and gas was injected onto the molten metal at a gas pressure of 7 MPa. In this way, a powder was obtained. Subsequently, the obtained powder was passed through a sieve (sieve size: 300 μm) in a glove box (oxygen concentration: 0.1 wt% or less) to adjust the particle size of the powder.

[0100] Next, this powder was placed in the recess of a carbon mold (17mm x 45mm x 7mm) and fired using the hot press method under the following firing conditions. (Firing conditions) Firing furnace: Hot press furnace Heating rate: 200°C / hour Heating atmosphere: Vacuum / Depressurized atmosphere Firing temperature: 1200℃ Pressure: 20 MPa Baking time: 3 hours

[0101] Thus, a sintered body with dimensions of 17 mm × 45 mm × 7 mmt and no microcracks was obtained. The properties of the powder and sintered body are shown in Tables 1 and 2, respectively. A cross-sectional view of the powder obtained by the gas atomization method is shown in Figure 4. Figure 4 shows the powder structure image (SEM image) obtained by cutting a sample obtained by embedding the gas atomized powder in resin, polishing the cross-section, and observing it with a scanning electron microscope (SEM). The gas atomized powder is the powder after particle size adjustment. The density of the sintered body is CrSi2 (true density 4.98 [g / cm³]). 3 The content of crystalline phase A, which consists of ]), is 87 wt%, and the true density of Si is 2.3 [g / cm³]. 3 The true density was calculated using the true density calculated assuming that the content of crystalline phase B, consisting of ]), is 13 wt%.

[0102] (Example 2) The powder was prepared by gas atomization as follows. Specifically, first, Cr flakes (4N) and Si flakes (5N) were mixed in a carbon crucible to obtain a mixture. At this time, the content of Cr flakes (4N) and Si flakes (5N) in the mixture was set to 18 wt% and 82 wt%, respectively. Then, the Cr flakes and Si flakes were melted in the carbon crucible at a melting temperature of 1650°C to form a molten metal, which was then dropped, and gas was injected onto the molten metal at a gas pressure of 7 MPa. In this way, powder was produced by the gas atomization method. Subsequently, the obtained powder was passed through a sieve (sieve size: 300 μm) in a glove box (oxygen concentration: 0.1 wt% or less) to adjust the particle size of the powder.

[0103] Next, this powder was placed in the recess of a carbon mold (17mm x 45mm x 7mm) and fired using the hot press method under the following firing conditions. (Firing conditions) Firing furnace: Hot press furnace Heating rate: 200°C / hour Heating atmosphere: Vacuum / Depressurized atmosphere Firing temperature: 1275℃ Pressure: 30 MPa Baking time: 3 hours

[0104] Thus, a sintered body with dimensions of 17 mm × 45 mm × 7 mmt and no microcracks was obtained. The properties of the powder and the sintered body are shown in Tables 1 and 2, respectively. The density of the sintered body is CrSi2 (true density 4.98 [g / cm³]). 3 The content of crystalline phase A, which consists of ]), is 37 wt%, and the true density of Si is 2.3 [g / cm³]. 3 The true density was calculated using the assumption that the content of crystalline phase B, consisting of ]), was 63 wt%.

[0105] (Examples 3-4) Powder and sintered bodies were prepared in the same manner as in Example 2, except that the gas pressure used as the gas atomization condition was changed as shown in Table 1. The characteristics of the powder and sintered bodies are shown in Tables 1 and 2, respectively.

[0106] (Example 5) Powder was produced by the gas atomization method as follows. That is, first, Cr flakes (4N) and Si flakes (5N) were mixed in a carbon crucible to obtain a mixture. At this time, the contents of Cr flakes (4N) and Si flakes (5N) in the mixture were made 29 wt% and 71 wt% respectively. Then, the Cr flakes and Si flakes were melted in the carbon crucible at a melting temperature of 1600 °C to form a molten metal, and the molten metal was dropped, and gas was injected into the molten metal at a gas pressure of 7 MPa. Thus, powder was produced by the gas atomization method. Subsequently, the obtained powder was passed through a sieve (sieve size: 300 μm) in a glove box (oxygen concentration: 0.1 wt% or less) to adjust the particle size of the powder.

[0107] Next, this powder was placed in a recess (17 mm × 45 mm × 7 mm) of a carbon mold and fired by the hot press method. (Firing conditions) Firing furnace: Hot press furnace Heating rate: 200 °C / hour Heating atmosphere: Vacuum reduced pressure atmosphere Firing temperature: 1250 °C Pressure: 20 MPa Firing time: 3 hours

[0108] Thus, a sintered body having a size of 17 mm × 45 mm × 7 mm and no microcracks was obtained. The properties of the powder and the sintered body are shown in Table 1 and Table 2 respectively. The density of the sintered body was calculated using the true density calculated assuming that the content of crystal phase A composed of CrSi2 (true density 4.98 [g / cm 3 ) was 51 wt% and the content of crystal phase B composed of Si (true density 2.3 [g / cm 3 ) was 49 wt%.

[0109] (Example 6) Powder was produced by the gas atomization method as follows. Specifically, first, Cr flakes (4N) and Si flakes (5N) were mixed in a carbon crucible to obtain a mixture. At this time, the content of Cr flakes (4N) and Si flakes (5N) in the mixture was set to 48 wt% and 52 wt%, respectively. Then, the Cr flakes (4N) and Si flakes (5N) were melted in the carbon crucible at a melting temperature of 1690°C to form a molten metal, which was then dropped, and gas was injected onto the molten metal at a gas pressure of 7 MPa. In this way, powder was produced by the gas atomization method. Subsequently, the obtained powder was passed through a sieve (sieve size: 300 μm) in a glove box (oxygen concentration: 0.1 wt% or less) to adjust the particle size of the powder.

[0110] Next, this powder was placed into the recesses of a carbon mold (17mm x 45mm x 7mm) and fired using the hot press method. (Firing conditions) Firing furnace: Hot press furnace Heating rate: 200°C / hour Heating atmosphere: Vacuum / Depressurized atmosphere Firing temperature: 1300℃ Pressure: 20 MPa Baking time: 3 hours

[0111] Thus, a sintered body with dimensions of 17 mm × 45 mm × 7 mmt and no microcracks was obtained. The properties of the powder and the sintered body are shown in Tables 1 and 2, respectively. The density of the sintered body is CrSi2 (true density 4.98 [g / cm³]). 3 The calculation was performed assuming that the content of crystalline phase A, which consists of ]), was 100 wt%.

[0112] (Example 7) The powder was prepared by gas atomization as follows. Specifically, first, Cr flakes (4N) and Si flakes (5N) were mixed in a carbon crucible to obtain a mixture. At this time, the content of Cr flakes (4N) and Si flakes (5N) in the mixture was set to 80 wt% and 20 wt%, respectively. Then, the Cr flakes (4N) and Si flakes (5N) were melted in the carbon crucible at a melting temperature of 1950°C to form a molten metal, which was then dropped, and gas was injected onto the molten metal at a gas pressure of 7 MPa. In this way, powder was produced by the gas atomization method. Subsequently, the obtained powder was passed through a sieve (sieve size: 300 μm) in a glove box (oxygen concentration: 0.1 wt% or less) to adjust the particle size of the powder.

[0113] Next, this powder was placed into the recesses of a carbon mold (17mm x 45mm x 7mm) and fired using the hot press method. (Firing conditions) Firing furnace: Hot press furnace Heating rate: 200°C / hour Heating atmosphere: Vacuum / Depressurized atmosphere Firing temperature: 1600℃ Pressure: 40 MPa Baking time: 3 hours

[0114] Thus, a sintered body with dimensions of 17 mm × 45 mm × 7 mmt and no microcracks was obtained. The properties of the powder and the sintered body are shown in Tables 1 and 2, respectively. The density of the sintered body is Cr3Si (true density 6.46 [g / cm³]). 3 The content of crystalline phase A, which consists of Cr5Si3 (true density 5.87 [g / cm³), is 48 wt%, and the true density of Cr5Si3 (true density 5.87 [g / cm³) is 5.87 [g / cm³]. 3 The true density was calculated using the true density calculated assuming that the content of crystalline phase B, consisting of ]), is 52 wt%.

[0115] ( Reference example 1 ) The powder obtained in Example 1 was passed through a sieve (sieve size: 150 μm) in a glove box (oxygen concentration: 0.1 wt% or less) to adjust the particle size of the powder, and the powder remaining on the 150 μm sieve was used.

[0116] Next, this powder was fired using the hot press method in the same manner as in Example 1. Thus, a sintered body with dimensions of 17 mm × 45 mm × 7 mmt and no microcracks was obtained. The properties of the powder and the sintered body are shown in Tables 1 and 2, respectively. The density of the sintered body is Cr2Si (true density 4.98 [g / cm³]). 3 The content of crystalline phase A, which consists of ]), is 87 wt%, and the true density of Si is 2.3 [g / cm³]. 3 The true density was calculated using the true density calculated assuming that the content of crystalline phase B, consisting of ]), is 13 wt%.

[0117] (Example 9) The powder obtained in Example 1 was passed through a sieve (sieve size: 32 μm) in a glove box (oxygen concentration: 0.1 wt% or less) to adjust the particle size of the powder.

[0118] Next, this powder was fired using the hot press method in the same manner as in Example 1. Thus, a sintered body with dimensions of 17 mm × 45 mm × 7 mmt and no microcracks was obtained. The properties of the powder and the sintered body are shown in Tables 1 and 2, respectively. The density of the sintered body is Cr2Si (true density 4.98 [g / cm³]). 3 The content of crystalline phase A, which consists of ]), is 87 wt%, and the true density of Si is 2.3 [g / cm³]. 3 The true density was calculated using the true density calculated assuming that the content of crystalline phase B, consisting of ]), is 13 wt%.

[0119] (Example 10) The powder obtained in Example 1 was passed through a sieve (mesh size: 106 μm) in a glove box (oxygen concentration: 0.1 wt% or less) to adjust the particle size of the powder. Subsequently, the powder that had passed through the above sieve (mesh size: 106 μm) was further sieved (mesh size: 90 μm) to adjust the particle size, and the powder remaining on the 90 μm sieve was used.

[0120] Next, this powder was fired using the hot press method in the same manner as in Example 1. Thus, a sintered body with dimensions of 17 mm × 45 mm × 7 mmt and no microcracks was obtained. The properties of the powder and the sintered body are shown in Tables 1 and 2, respectively. The density of the sintered body is Cr2Si (true density 4.98 [g / cm³]). 3 The content of crystalline phase A, which consists of ]), is 87 wt%, and the true density of Si is 2.3 [g / cm³]. 3 The true density was calculated using the true density calculated assuming that the content of crystalline phase B, consisting of ]), is 13 wt%.

[0121] (Comparative Example 1) A mixture of 18 wt% Cr powder (4N) and 82 wt% Si powder (5N) was pre-sintered at 1250°C to obtain a pre-sintered body, which was then pulverized. The pulverized pre-sintered body was then placed in an iron can, degassed under vacuum, the can was welded, and the body was fired using the HIP (Hot Isostatic Pressing) method under the following firing conditions to obtain a sintered body. (Firing conditions) Heating rate: 200°C / hour Temperature rise atmosphere: Ar Firing temperature: 1250℃ Pressure: 100MPa Baking time: 1 hour

[0122] The properties of the sintered bodies obtained in this way are shown in Tables 1 and 2, respectively. The density of the sintered body is CrSi2 (true density 4.98 [g / cm³]). 3 The content of crystalline phase A, which consists of ]), is 37 wt%, and the true density of Si is 2.3 [g / cm³]. 3 The true density was calculated using the assumption that the content of crystalline phase B, consisting of ]), was 63 wt%.

[0123] (Comparative Example 2) 42 wt% Cr powder (4N) and 58 wt% Si powder (5N) were mixed, and the mixed powder was pre-sintered at 1250°C to obtain a pre-sintered body, which was then pulverized. Subsequently, the pulverized pre-sintered body was fired using the hot-press method under the following firing conditions to obtain a sintered body. (Firing conditions) Firing furnace: Hot press furnace Heating rate: 200°C / hour Heating atmosphere: Vacuum / Depressurized atmosphere Firing temperature: 1200℃ Pressure: 20 MPa Baking time: 3 hours

[0124] The properties of the sintered bodies obtained in this way are shown in Tables 1 and 2. The obtained powder is shown in Figure 5. Figure 5 shows an image of the powder obtained by observation with a scanning electron microscope (SEM), and the powder is the powder obtained after the pre-sintered body has been crushed. The density of the sintered body is given by: Crystal phase A:CrSi2 (true density 4.98 [g / cm³] 3 The content of crystalline phase A, which consists of ]), is 87 wt%, and the true density of Si is 2.3 [g / cm³]. 3 The true density was calculated using the true density calculated assuming that the content of crystalline phase B, consisting of ]), is 13 wt%.

[0125] (Comparative Example 3) Fine CrSi2 powder (average particle size 5 μm) and fine Si powder (average particle size 9 μm) were mixed and fired using the hot-press method at the temperature, pressure, and holding time shown in Table 2 to obtain a sintered body. The properties of the resulting sintered body are shown in Table 2. The density of the sintered body is CrSi2 (true density 4.98 [g / cm³]). 3 The content of crystalline phase A, which consists of ]), is 87 wt%, and the true density of Si is 2.3 [g / cm³]. 3 The true density was calculated using the true density calculated assuming that the content of crystalline phase B, consisting of ]), is 13 wt%.

[0126] [Table 1] [Table 2]

[0127] Although the present invention has been described in detail with reference to specific embodiments, it will be apparent to those skilled in the art that various changes and modifications are possible without departing from the spirit and scope of the invention. This application is based on Japanese Patent Application No. 2020-091321, filed on May 26, 2020, which is incorporated by reference in its entirety. All references cited herein are incorporated as a whole. [Explanation of Symbols]

[0128] 10...Metal-Si powder, 10A...Metal-Si particles, 11...Crystal phase particles, 12...Substance, 20...Metal-Si sintered body, 21...Sintered particles, 40...Thin film forming body, 41...Thin film, 42...Substrate.

Claims

1. It contains metal-Si-based particles that include multiple crystalline phase particles, The crystalline phase particles include a crystalline phase containing a compound of metal and Si, The crystalline phase particles have an average particle size of 10 μm or less. The aforementioned metal is Cr, Contains less than 0.5 wt% oxygen, Metal-Si powder.

2. The metal-Si-based powder according to claim 1, wherein the crystalline phase particles have an average particle size of 5 μm or less.

3. The metal-Si powder according to claim 1 or 2, wherein the metal-Si particles have an average particle size of 5 to 100 μm.

4. A metal-Si powder according to any one of claims 1 to 3, containing 0.03 wt% or less of oxygen.

5. The metal-Si powder according to any one of claims 1 to 4, wherein the relative density of the lightly loaded material to the true density is 50% or more.

6. The metal-Si powder according to any one of claims 1 to 5, wherein the total amount of metal impurities is 300 ppm by mass or less.

7. The metal-Si powder according to any one of claims 1 to 6, wherein the number of crystalline phase particles is 10 or more and 500 or less.

8. A method for producing a metal-Si powder according to any one of claims 1 to 7, A process of heating a mixture of metal and Si to melt it and form a molten state, A method for producing metal-Si powder, comprising the step of injecting gas into the molten liquid.

9. A method for producing a metal-Si sintered body obtained by firing a metal-Si powder according to any one of claims 1 to 7.

Citation Information

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