A silicon-molybdenum alloy tubular target material and its preparation method and application

Through wet ball milling and hot isostatic pressing, the problems of poor mixing uniformity and forming performance of silicon-molybdenum targets were solved, and high-density large-size silicon-molybdenum tubular targets were prepared for use in the fields of electronic gate materials and thin films.

CN119736586BActive Publication Date: 2025-09-19KONFOONG MATERIALS INTERNATIONAL CO LTD
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Patent Information

Application Number
CN202411862385.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-17
Publication Date
2025-09-19
Estimated Expiration
2044-12-17

AI Technical Summary

Technical Problem

Existing technologies make it difficult to prepare high-density, large-sized silicon-molybdenum targets, and the mixing uniformity and molding performance of silicon powder and molybdenum powder are poor, making it difficult to meet the requirements of the high-end electronics industry.

Method used

Silicon powder and molybdenum powder were mixed by wet ball milling, and a binder was added. Then cold isostatic pressing and hot isostatic pressing were performed to prepare silicon-molybdenum alloy tubular targets.

Benefits of technology

The silicon-molybdenum alloy tubular target material with high density and internal uniformity meets the performance requirements of the high-end electronics industry and is suitable for electronic gate materials and electronic thin films.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to the technical field of target material preparation, and specifically to a silicon-molybdenum alloy tubular target material, a preparation method and application thereof. The process of wet ball milling silicon powder and molybdenum powder is adopted to improve the uniformity of the mixed powder; a binder is added to improve its forming performance, thereby realizing the forming of large-sized tubular targets and improving the mechanical processing performance of green billets; finally, a hot isostatic pressing process is adopted for densification. The prepared silicon-molybdenum alloy tubular target material has high density and good internal uniformity, and can meet the high performance requirements of the tubular target material.
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Description

Technical Field

[0001] The present 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 targets are commonly used in vacuum sputtering processes. Because the oxide gate formed by sputtering silicon-molybdenum targets maintains stable contact with polysilicon, and this silicide can withstand high-temperature treatment without decomposing into oxides, it exhibits excellent resistance to oxidation and chemical corrosion. Therefore, silicon-molybdenum targets are widely used in electronic gate materials and thin film applications.

[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 existing technology have low density and cannot meet the target quality requirements of the high-end electronics industry. They 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 involves 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 surface of the particles, 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 producing a molybdenum-silicon target, comprising: providing molybdenum powder and silicon powder, mixing the molybdenum powder and silicon powder to form a molybdenum-silicon mixed powder; and sintering the molybdenum-silicon mixed powder using a hot pressing process to form a molybdenum-silicon target. The molybdenum-silicon target produced using this method has a high density, but the method is primarily suitable for silicon-molybdenum alloy targets with a high molybdenum content.

[0005] CN 105483624A discloses a method for manufacturing a molybdenum-silicon target and a combination thereof. The method comprises: providing molybdenum powder and silicon powder; mixing the molybdenum powder and silicon powder using a mixing process to form a mixed powder; cold pressing the mixed powder to form a molybdenum-silicon target blank; and vacuum hot pressing and sintering the molybdenum-silicon target blank to form a molybdenum-silicon target. This manufacturing method can produce a molybdenum-silicon target with a high density, but is only applicable to flat circular molybdenum-silicon 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 and mix it 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 existing technology, it is necessary to provide a method for preparing large-sized tubular silicon-molybdenum targets 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 its preparation method and application, 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 a 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-sized tubular targets and improving the mechanical processing performance of green billets; finally, a hot isostatic pressing process is used for densification, 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 unlisted values ​​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 being 100 wt%, in the silicon powder and molybdenum powder in step (1), the mass fraction of molybdenum powder is 10-50 wt%, and the balance is silicon powder.

[0019] The mass proportion 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. Other values ​​not listed within the numerical range are also applicable.

[0020] Preferably, the adhesive 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 use in 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 ​​hours, for example, it can be 23 hours, 23.5 hours, 24 hours, 24.5 hours or 25 hours, but is not limited to the listed values. 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, it can be 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, it can be 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, it can be 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 sheath.

[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 at a rotation speed of 10-15 r / min for 23-25 ​​hours, drying the resulting mixture and cold isostatically pressing it at 150-250 MPa for a holding time of 15-30 minutes 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 balance 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 wet ball milling process comprises anhydrous ethanol, wherein the mass of the anhydrous ethanol is 20-50 wt% of the total mass of the silicon powder, molybdenum powder, and anhydrous ethanol; the wet ball milling process comprises zirconium oxide balls having diameters of 5 mm, 10 mm, and 15 mm, respectively, in a mass ratio of 1:(9-11):(9-11); and the mass ratio of the ball milling balls to the total mass of the silicon powder and molybdenum powder is 1:(1.5-2.5);

[0043] (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 600-900° 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, which is prepared by the method for preparing the silicon-molybdenum alloy tubular target described in the first aspect.

[0045] The silicon-molybdenum alloy tubular target 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.

[0046] In a third aspect, the present invention provides an application of the silicon-molybdenum alloy tubular target as described in the second aspect, wherein the silicon-molybdenum alloy tubular target 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 thin film, thereby ensuring 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 a 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-sized tubular targets and improving the mechanical processing performance of green billets; finally, a hot isostatic pressing process 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 of the tubular target. DETAILED DESCRIPTION

[0050] The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the embodiments are merely 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. The preparation method of the silicon-molybdenum alloy tubular target material includes the following steps:

[0053] (1) Wet ball milling of silicon powder, molybdenum powder and epoxy resin at a rotation speed of 13 r / min for 24 hours, drying the resulting mixture and cold isostatic pressing 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 100 wt%, the mass of the molybdenum powder in the silicon powder and the molybdenum powder accounts for 30 wt%, and the balance is silicon powder; the mass of the epoxy resin is 0.6 wt% of the total mass of the silicon powder and the molybdenum powder;

[0054] The wet ball milling medium used in the mixing was anhydrous ethanol, the mass of which was 30 wt% of the total mass of the silicon powder, molybdenum powder, and anhydrous ethanol; the wet ball milling balls used in the mixing included zirconia balls with diameters of 5 mm, 10 mm, and 15 mm, respectively, with a mass ratio of 1:10:10; and the mass ratio of the ball milling balls to the total mass of the silicon powder and molybdenum powder was 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. The preparation method of the silicon-molybdenum alloy tubular target material includes the following steps:

[0058] (1) Wet ball milling of silicon powder, molybdenum powder and acrylic resin at a rotation speed of 10 r / min for 25 hours, drying the resulting mixture and cold isostatic pressing 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 balance is silicon powder; the mass of the acrylic resin is 0.2wt% of the total mass of the silicon powder and the molybdenum powder;

[0059] The wet ball milling medium used in the mixing was anhydrous ethanol, the mass of which was 20 wt% of the total mass of the silicon powder, molybdenum powder, and anhydrous ethanol; the wet ball milling balls used in the mixing included zirconia balls with diameters of 5 mm, 10 mm, and 15 mm, respectively, with a mass ratio of 1:9:9; and the mass ratio of the ball milling balls to the total mass of the silicon powder and molybdenum powder was 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. The preparation method of the silicon-molybdenum alloy tubular target material includes the following steps:

[0063] (1) Wet ball milling of silicon powder, molybdenum powder and polyimide resin at a rotation speed of 15 r / min for 23 h, drying the resulting mixture and cold isostatic pressing at 250 MPa for 15 min to obtain a silicon-molybdenum alloy billet; the silicon powder has a particle size of 8 μm and a purity of 5N; the molybdenum powder has a particle size of 3 μm and a purity of 3N5; based on a total mass fraction of 100 wt%, the mass of the silicon powder and the molybdenum powder accounts for 50 wt%, and the remainder is silicon powder; the mass of the polyimide resin is 1 wt% of the total mass of the silicon powder and the molybdenum powder;

[0064] The wet ball milling process used anhydrous ethanol as the milling medium, with the mass of the anhydrous ethanol accounting for 50 wt% of the total mass of the silicon powder, molybdenum powder, and anhydrous ethanol. The wet ball milling process used zirconium oxide balls with diameters of 5 mm, 10 mm, and 15 mm, respectively, with a mass ratio of 1:11:11. The mass ratio of the ball milling balls to the total mass of the silicon powder and molybdenum powder was 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 0.1 wt% 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 1.5 wt% 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 single 10 mm diameter zirconia balls, the rest are the same as those in Example 1.

[0072] Example 7

[0073] 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 pressure of the cold isostatic pressing treatment in step (2) to 130 MPa, the rest is the same as that of Example 1.

[0074] Example 8

[0075] 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 pressure of the cold isostatic pressing treatment in step (2) to 270 MPa, the rest is the same as that of Example 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 Example 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 Example 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 Example 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 Example 1.

[0080] Comparative Example 1

[0081] This comparative example 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 no epoxy resin is 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. The preparation method of the silicon-molybdenum alloy tubular target 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 tissue uniformity testing using SEM, and the results were classified as "uniform", "relatively uniform", and "uneven". The density was measured using 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] As can be seen from Table 1, the silicon-molybdenum alloy tubular target prepared by the preparation method provided by the present invention has good internal uniformity and density, high billet strength, and is easy to process and shape. It can produce large-sized silicon-molybdenum alloy tubular targets with 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 limit range will reduce the internal uniformity and density of the silicon-molybdenum alloy tubular target.

[0090] From the comparison between Example 1 and 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 the inability to achieve the forming of large-sized tubular targets; from the comparison between Example 1 and Comparative Example 2, it can be seen that the powder mixing effect is significantly reduced by dry grinding compared with 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 the green body; finally, hot isostatic pressing is used for densification. The prepared silicon-molybdenum alloy tubular target has high density and good internal uniformity, which can meet the high performance requirements as a tubular target.

[0092] The above description is only a specific embodiment 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 fall 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) Wet ball milling is performed to mix silicon powder, molybdenum powder and a binder, and the resulting mixture is subjected to cold isostatic pressing at 150-250 MPa to obtain a silicon-molybdenum alloy billet; based on the total mass fraction of 100 wt%, the mass of the molybdenum powder in the silicon powder and the molybdenum powder is 30 wt%, and the balance is silicon powder; the binder comprises any one of epoxy resin, acrylic resin or polyimide resin or a combination of at least two thereof; the mass of the binder is 0.2-1 wt% of the total mass of the silicon powder and the molybdenum powder; The ball milling medium used in the wet ball milling includes anhydrous ethanol; the ball milling balls used in the wet ball milling include zirconia balls with diameters of 5 mm, 10 mm, and 15 mm, respectively; (2) The silicon-molybdenum alloy blank obtained in step (1) is subjected to degreasing treatment and hot isostatic pressing sintering at 600-700° C. 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.

3. The preparation method according to claim 1, characterized in that The purity of the silicon powder in step (1) is 5N.

4. The preparation method according to claim 1, characterized in that The particle size of the molybdenum powder in step (1) is 3-5 μm.

5. The preparation method according to claim 1, characterized in that The purity of the molybdenum powder in step (1) is 3N5.

6. The preparation method according to claim 1, characterized in that The mass of the anhydrous ethanol in step (1) is 20-50wt% of the total amount of silicon powder, molybdenum powder and anhydrous ethanol.

7. The preparation method according to claim 1, characterized in that The mass ratio of the zirconia balls with diameters of 5 mm, 10 mm and 15 mm in step (1) is 1:(9-11):(9-11).

8. The preparation method according to claim 1, characterized in that 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).

9. The preparation method according to claim 1, characterized in that The rotation speed of the wet ball milling mixing in step (1) is 10-15 r / min.

10. The preparation method according to claim 1, characterized in that The wet ball milling mixing time in step (1) is 23-25 ​​hours.

11. The preparation method according to claim 1, characterized in that The mixed material in step (1) is dried before cold isostatic pressing.

12. The preparation method according to claim 1, characterized in that The holding time of the cold isostatic pressing treatment in step (1) is 15-30 minutes.

13. The preparation method according to claim 1, characterized in that The silicon-molybdenum alloy blank is processed before the degreasing treatment in step (2).

14. The preparation method according to claim 1, characterized in that The pressure of the hot isostatic pressing sintering in step (2) is 100-150 MPa.

15. The preparation method according to claim 1, characterized in that The hot isostatic pressing sintering time in step (2) is 2-4 hours.

16. The preparation method according to claim 1, characterized in that The hot isostatic pressing sintering in step (2) is carried out in a stainless steel sheath.

17. The preparation method according to claim 1, characterized in that The preparation method comprises the following steps: (1) Wet ball milling of silicon powder, molybdenum powder and a binder at a rotation speed of 10-15 r / min for 23-25 ​​h, drying the resulting mixture and cold isostatic pressing at 150-250 MPa for a holding time of 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 100 wt%, the mass of the molybdenum powder in the silicon powder and the molybdenum powder accounts for 30 wt%, and the balance is silicon powder; the mass of the binder is 0.2-1 wt% of the total amount of the silicon powder and the molybdenum powder; the binder comprises any one of epoxy resin, acrylic resin or polyimide resin or a combination of at least two thereof; The wet milling process comprises anhydrous ethanol, wherein the mass of the anhydrous ethanol is 20-50 wt % of the total mass of the silicon powder, molybdenum powder, and anhydrous ethanol; the wet milling process comprises zirconium oxide balls having diameters of 5 mm, 10 mm, and 15 mm, respectively, in a mass ratio of 1:(9-11):(9-11); and the ratio of the mass of the ball milling balls to the total mass of the silicon powder and molybdenum powder is 1:(1.5-2.5); (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 600-700°C, a pressure of 100-150 MPa, and a time of 2-4 hours to obtain the silicon-molybdenum alloy tubular target.

18. 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 17.

19. A use of the silicon-molybdenum alloy tubular target according to claim 18, 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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