A method of manufacturing an alloy target

Abstract

The application relates to the technical field of target material preparation, and provides a preparation method of an alloy target material, which comprises the following steps: providing target material alloy powder; performing isostatic pressing forming treatment on the target material alloy powder to form a blank; surrounding adsorbent sheets and / or hydrogen storage materials around the blank; and then performing first sintering treatment to obtain the alloy target material. According to the preparation method, the adsorbent sheets and / or hydrogen storage materials are used for auxiliary sintering, the adsorbent sheets can absorb CO2, N2 and other impurities in a sintering environment, promote the rapid discharge of gas in pores of a sintered body, promote the migration and shrinkage of substances, and thus the porosity and defects of the sintered body are greatly reduced, and the purity, density, composition and uniformity of the alloy target material are improved. The hydrogen storage materials release hydrogen in the sintering process to consume O2 in the sintering environment, effectively inhibit oxygen impurities, and reduce the oxygen content of the alloy target material by reducing metal oxides of the sintered body into water vapor, thereby solving the problem that a conventional sintering furnace cannot directly sinter hydrogen.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of target material preparation, and particularly relates to a preparation method of an alloy target material. BACKGROUND

[0002] As the core material of vacuum coating technology, the purity, density and composition uniformity of the alloy target material directly affect the film performance and further affect the quality of the terminal product. Common preparation methods of the alloy target material mainly include a melting and casting method and a powder metallurgy method. The melting and casting method is to form an alloy melt by vacuum melting of metal raw materials with a certain ratio, then pour into a mold for forming, and then form an alloy target material through mechanical processing or subsequent deformation treatment. However, the molten liquid is easy to produce bubbles in the pouring process, and for multi-element metal components with large differences in melting point and density, segregation is also easy to occur, thereby affecting the density, composition and uniformity of the alloy target material. The powder metallurgy method is to form a target blank by pressing and sintering of metal powder raw materials with a certain ratio, and then mechanically processing to form an alloy target material. However, impurities such as oxygen and nitrogen are easy to be introduced in the powder processing and sintering process, thereby affecting the purity of the composition of the alloy target material. The insufficient purity has become a key bottleneck for the application of domestic alloy target materials in core industries such as advanced semiconductors and display panels, resulting in a high dependence on imports of domestic ultra-high purity alloy target materials in high-end application fields.

[0003] Therefore, the existing preparation method of the alloy target material cannot simultaneously consider the problems of ultra-high purity, high density, composition and uniformity. SUMMARY

[0004] The application aims to provide a preparation method of an alloy target material, and aims to solve the technical problem that the existing preparation method of the alloy target material cannot simultaneously consider ultra-high purity, high density, composition and uniformity.

[0005] To achieve the above application purposes, the technical scheme adopted by the application is as follows:

[0006] The application provides a preparation method of an alloy target material, comprising the following steps:

[0007] Providing a target alloy powder;

[0008] Isostatic pressing the target alloy powder to form a green compact;

[0009] Surrounding the adsorbent sheet and / or hydrogen storage material around the four sides of the green compact, and then performing a first sintering treatment to obtain an alloy target material.

[0010] Compared with the prior art, the application has the following beneficial effects:

[0011] The preparation method of the alloy target provided by the application adopts adsorbent sheet and / or hydrogen storage material to assist sintering, the adsorbent sheet can absorb O2, N2, CO2 and other impurities in the sintering environment, effectively promote the rapid discharge of gas in the pores of the sintered body, promote the shrinkage of the material, thereby greatly reducing the pores and defects, improving the purity, density, composition and uniformity of the alloy target, and solving the problem that the residual pores are formed due to the failure of the gas in the pores to diffuse in time in the traditional sintering, thereby hindering the shrinkage of the sintered body. The hydrogen storage material releases hydrogen gas to consume O2 in the sintering environment during the sintering process, effectively inhibits oxygen impurities, and also reduces the metal oxides of the sintered body to generate water vapor, thereby greatly reducing the oxygen content of the alloy target, improving the purity of the alloy target, and solving the problem that the conventional sintering furnace cannot directly sinter with hydrogen. In addition, the preparation method has no special requirements for the sintering equipment, has low cost, and is suitable for large-scale industrial production. BRIEF DESCRIPTION OF DRAWINGS

[0012] In order to more clearly illustrate the technical solutions in the embodiments of the application, the drawings needed to be used in the embodiments or prior art description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the application, and other drawings can be obtained by those skilled in the art without creative labor.

[0013] Figure 1 is a flow chart of the preparation method of the alloy target provided by the embodiments of the application;

[0014] Figure 2 is a cross-sectional view of the hydrogen storage material used in the preparation method of the alloy target provided by the embodiments of the application.

[0015] In the drawings, various reference signs represent:

[0016] 1 - slow-release shell, 2 - hydrogen storage alloy powder. DETAILED DESCRIPTION

[0017] In order to make the technical problems, technical solutions and beneficial effects to be solved by the application more clearly understood, the application will be further described in detail below in combination with embodiments. It should be understood that the specific embodiments described herein are only used to explain the application and not to limit the application.

[0018] In the target sintering process, if hydrogen is to be introduced, special requirements are required for the equipment. The conventional vacuum sintering furnace cannot be directly used for hydrogen sintering, and a special hydrogen sintering furnace must be used, and the furnace at least needs to meet: (1) explosion-proof sealing: the furnace body must be designed with full sealing to prevent hydrogen leakage from causing explosion; (2) equipped with high-precision atmosphere control system and multiple safety systems: high-purity hydrogen needs to be introduced, and it is necessary to ensure that the air in the furnace is completely exhausted before hydrogen is introduced, and a nitrogen replacement channel, a high-precision flow control system, a safety monitoring system such as a leakage alarm system, an automatic cutting-off gas source and power source, and a water cooling protection system are configured to prevent the high-temperature failure of the sealing ring; (3) the heating element needs to be resistant to hydrogen embrittlement: conventional resistance wires are easily embrittled by hydrogen, and molybdenum, tungsten and other hydrogen-resistant materials need to be used. It can be seen that the internal structure of the sintering furnace that meets the hydrogen introduction requirement is extremely complex, not only the cost is high, but also the maintenance frequency is high and the operation is complex, and a dedicated person is needed to maintain; in addition, it has high risk of flammability and explosion. Therefore, the hydrogen storage material assisted sintering used in the present application can safely and conveniently provide a controllable reducing environment, and will not introduce impurities into the target material, and significantly improve the oxygen content and density of the alloy target material and other properties. The problem that the conventional vacuum sintering furnace cannot be used for hydrogen sintering is solved, the disadvantages of high cost, difficult maintenance and high risk of using a special hydrogen sintering furnace are avoided, and the problem that the hydrogen sintering furnace cannot be used for the preparation of medium and low value-added target materials is also solved.

[0019] The embodiment of the present application provides a preparation method of an alloy target material, as shown in the following formula: Figure 1 The embodiment of the present application provides a preparation method of an alloy target material, as shown in the following formula:

[0020] S01: providing a target alloy powder;

[0021] S02: isostatic pressing and forming treatment of the target alloy powder to form a green body;

[0022] S03: surrounding the adsorbent sheet and / or hydrogen storage material around the green body, and then performing first sintering treatment to obtain an alloy target material.

[0023] The preparation method of the alloy target provided by the embodiment of the application adopts adsorbent sheet and / or hydrogen storage material to assist sintering, the adsorbent sheet can absorb O2, N2, CO2 and other impurities in the sintering environment, effectively promote the rapid discharge of gas in the pores of the sintered body, promote the shrinkage of the material, thereby greatly reducing the pores and defects, improving the purity, density, composition and uniformity of the alloy target, and solving the problem that the sintered body is hindered from shrinking due to the residual pores formed by the failure of the gas in the pores to diffuse in time in the traditional sintering. The hydrogen storage material releases hydrogen gas to consume O2 in the sintering environment during the sintering process, effectively inhibits oxygen impurities, and can also reduce the metal oxides of the sintered body to generate water vapor, thereby greatly reducing the oxygen content of the alloy target, improving the purity of the alloy target, and solving the problem that the conventional sintering furnace cannot directly sinter with hydrogen. In addition, the preparation method has no special requirements for the sintering equipment, has low cost, and is suitable for large-scale industrial production.

[0024] In the embodiment, the target alloy powder includes any one of zinc telluride alloy powder, aluminum scandium alloy powder, copper gallium alloy powder, molybdenum niobium alloy powder, molybdenum tungsten alloy powder, and neodymium iron boron alloy powder. These target alloy powders of the embodiment can be obtained by purchase, and of course, can also be prepared according to the techniques, conditions and the like described in the literature or books in the art, and the purity of the target alloy powder is required to be ≥99.99%, and the particle size is 10-50 μm.

[0025] In the embodiment, the step of isostatic pressing the target alloy powder includes: filling the target alloy powder into a mold, and then performing cold isostatic pressing treatment under a pressure of 200-300 MPa, and maintaining the pressure for 0.5-2 h.

[0026] In the embodiment, the distance between the adsorbent sheet and the green body is ≥0.1 cm, or the distance between the hydrogen storage material and the green body is ≥0.1 cm. The distance range can ensure that the oxygen, nitrogen and other impurities around the green body are quickly adsorbed by the adsorbent sheet or quickly consumed by the hydrogen released by the hydrogen storage material, and can also avoid contact with the green body to prevent the sintered body from being adhered and new impurities from being introduced.

[0027] In the embodiment, the thickness of the adsorbent sheet is 0.05-0.5 cm.

[0028] In the embodiment, the adsorbent sheet is selected from a zirconium-based alloy or a titanium-based alloy.

[0029] In the embodiments, the zirconium-based alloy comprises Zr and M1 in a mass ratio of (70~90):(10~30), where M1 is selected from one or more combinations of Ti, V, Al, Fe, Co, La, Ce, Pr, Nd, and Y. These zirconium-based alloys exhibit high chemical affinity for O, N, H, and C, and can continue to absorb these elements at temperatures ranging from 500 to 1400°C, significantly reducing the oxygen and nitrogen content of the target material. Furthermore, the multi-element solid solution alloying improves the stability of the antioxidant film, prevents passivation failure, and effectively extends the adsorption lifespan of the zirconium-based alloy.

[0030] In the embodiments, the titanium-based alloy comprises Ti and M2 in a mass ratio of (60~90):(10~40), where M2 is selected from one or more combinations of Zr, Mo, Ni, V, Al, Fe, and Mn. These titanium-based alloys exhibit high chemical affinity for O, N, H, and C, and can continue to absorb these elements at temperatures ranging from 500 to 1400°C, significantly reducing the oxygen and nitrogen content of the target material. Furthermore, the multi-element solid solution alloying improves the stability of the antioxidant film, prevents passivation failure, and effectively extends the adsorption lifespan of the titanium-based alloy.

[0031] In an embodiment, such as Figure 2 As shown, the hydrogen storage material includes a slow-release shell 1 and hydrogen storage alloy powder 2 filled in the slow-release shell 1. The hydrogen storage alloy powder 2 is used to provide hydrogen release. The slow-release shell 1 is provided with pores to control the hydrogen release rate of the hydrogen storage alloy powder 2.

[0032] In an embodiment, the steps for preparing the sustained-release shell include: mixing sustained-release material powder, pore-forming agent, binder and ethanol to obtain a slurry; casting the slurry into a blank to obtain a green body; and subjecting the green body to pre-firing treatment and second sintering treatment to obtain the sustained-release shell.

[0033] In the embodiments, the pore-forming agent is selected from any one of starch, urea, ammonium bicarbonate, and polymethyl methacrylate.

[0034] In the embodiments, the amount of pore-forming agent added is 1-10% of the mass of the sustained-release material powder, and the particle size of the pore-forming agent is 0.5-50 μm. By controlling the amount and particle size of the pore-forming agent, the pore size and porosity range of the sustained-release shell can be effectively controlled, thereby ensuring that the sustained-release shell can accurately control the hydrogen release rate.

[0035] In the embodiments, the pre-calcination treatment temperature is 300~600℃ and the time is 1~4h; the second sintering treatment temperature is 1500~2400℃ and the time is 4~24h. Pores are formed by removing the pore-forming agent through pre-calcination, and then the density and strength of the slow-release shell are improved by sintering, and pores of the target particle size are formed.

[0036] In embodiments, the thickness of the slow-release shell is 0.01-0.2 cm, and the pore size of the pores is 0.3-35 μm. The thickness and pore size of the slow-release shell in the embodiments can ensure that the mechanical strength is sufficient to withstand loading and handling, while ensuring that the pore structure does not collapse at high temperatures, thereby maintaining the slow-release effect.

[0037] In embodiments, the porosity is 0.8-8%. The porosity range in the embodiments can accurately control the hydrogen release rate, form a weak reduction sintering environment, consume oxygen in the sintering environment, and reduce metal oxides in the sintered body to form water vapor, thereby effectively inhibiting oxidation of the alloy target material and not causing hydrogen embrittlement or bulging, thereby significantly reducing the oxygen content of the alloy target material.

[0038] In embodiments, the material of the slow-release shell is selected from one or more of molybdenum, tungsten, niobium, and tantalum. These metals do not react with hydrogen, do not cause hydrogen embrittlement, and can be repeatedly used. At the same time, these metals have high melting points, specific heat capacities, and thermal conductivities, have large heat storage capacity per unit volume, and can quickly and uniformly heat, thereby effectively inhibiting fluctuations in the furnace temperature and improving the uniformity of the furnace temperature, thereby further improving the uniformity of the target material grains.

[0039] In embodiments, the particle size of the hydrogen storage alloy powder is 100-500 μm. This particle size range can ensure the packing density and avoid clogging of the pores of the slow-release shell.

[0040] In embodiments, the hydrogen storage alloy powder is selected from any one of a titanium-based hydrogen storage alloy powder, a zirconium-based hydrogen storage alloy powder, and a vanadium-based hydrogen storage alloy powder.

[0041] In embodiments, the titanium-based hydrogen storage alloy powder includes Ti and M3, and M3 is selected from one or more of Fe, Mn, Cr, Zr, and V; for example, the titanium-based hydrogen storage alloy powder can be TiFe, Ti 0.8 Zr 0.2 Mn 2-x Cr x (x=0.2, 0.4, 0.6, 0.8, and 1.0), Ti i0.9 Zr 0.2 Mn 1.8 V 0.2 , Ti 0.9 Zr x Mn 1.8-y Cr y V 0.2 (x=0.1, 0.15, and 0.2; y=0.2 and 0.4), etc.

[0042] In embodiments, the zirconium-based hydrogen storage alloy powder includes Zr and M4, and M4 is selected from one or more of V, Cr, Mn, Ni, Fe, and Ti; for example, the zirconium-based hydrogen storage alloy powder can be ZrV2, ZrCr2, ZrMn2, Zr 0.8 Ti0.2 Mn 0.44 Cr 0.11 V 0.44 Ni 1.32 etc.

[0043] In embodiments, the vanadium-based hydrogen storage alloy powder comprises V and M5, and M5 is selected from one or more combinations of Ti, Zr, Cr, Fe, Mn, Ni; for example, the vanadium-based hydrogen storage alloy powder can be V 0.3 Ti 0.35 Cr 0.25 Fe 0.1 , V 0.7 Zr 0.1 Ni 0.2 etc.

[0044] In embodiments, before the hydrogen storage alloy powder is injected into the slow-release shell, the steps of pretreatment, activation and hydrogen absorption treatment are further included. Specifically, the step of pretreatment can include: placing the hydrogen storage alloy powder in a hydrogen absorption reactor, vacuumizing to below 0.1 Pa, then heating to 100-150℃ to remove surface-adsorbed impurities such as H2O, CO2, O2, etc. The step of activation treatment can include: vacuumizing the hydrogen absorption reactor to below 10 -2 Pa, then starting to heat to 200-400℃, then introducing hydrogen gas with a purity of 99.99%, so that the pressure of the hydrogen absorption reactor is 1-5 MPa, and holding for 0.5-2 h; then heating to 400℃-600℃ and reducing the pressure to release hydrogen; repeating the hydrogen absorption-hydrogen release process 2-5 times, so as to break the passivation layer on the surface of the hydrogen storage alloy and improve the hydrogen absorption and release capacity. The step of hydrogen absorption treatment can include: vacuumizing the hydrogen absorption reactor to below 10 -2 Pa, then heating to 50-100℃, then introducing hydrogen gas with a purity of 99.99%, so that the pressure of the hydrogen absorption reactor is 1-5 MPa, and holding for 0.5-2 h before closing the valve to stop hydrogen absorption. Of course, the steps of pretreatment, activation and hydrogen absorption treatment can also be pretreated, activated and hydrogen-absorbed according to the actual material quality of the hydrogen storage alloy powder, and according to the techniques, conditions, etc. described in the literature or books in the art.

[0045] In embodiments, the first sintering treatment has a vacuum degree of 10 -2 ~10 -3 Pa, a temperature of 500-1400℃, and a time of 4-24 h.

[0046] In embodiments, the adsorbent sheet and the hydrogen storage material are used to assist sintering, which effectively improves the purity, density, composition and uniformity of the alloy target material, and the hydrogen storage material can also be reused. When the hydrogen release of the hydrogen storage alloy powder of the hydrogen storage material is complete, the hydrogen storage alloy powder can be taken out to be re-hydrogenated and then injected into the slow-release shell, so that recycling is realized and the cost is reduced.

[0047] The application will be described in detail below with reference to specific embodiments.

[0048] Embodiment 1

[0049] The embodiment provides a preparation method of a zinc telluride target material, comprising the following steps:

[0050] S11: purchasing zinc telluride powder with a purity of greater than or equal to 99.99% and a particle size of 10-50 μm;

[0051] S12: forming treatment: filling the zinc telluride powder into a mold, and performing cold isostatic pressing forming treatment under a pressure of 250 MPa, and keeping the pressure for 1 h to form a green body;

[0052] S13: preparing a hydrogen storage material:

[0053] The molybdenum powder (with a particle size of 2-15 μm), starch (with a particle size of 5-30 μm), polyvinyl alcohol and ethanol are ball-mixed to obtain a slurry; the slurry is loaded into a vacuum tank, and after vacuum defoaming, the slurry is injected into a sealed graphite mold cavity under a pressure of 1 MPa until no water drops come out of the mold, the mold is opened, and the solidified green body is taken out and kept at room temperature for 24 h to obtain the green body; the green body is placed in a vacuum sintering furnace, vacuumizing is started and the pressure is reduced to 5*10 -2 Pa, then the temperature is raised to 400 ℃ for pre-sintering for 2 h, and then the temperature is raised from 400 ℃ to 2100 ℃ for second sintering for 18 h to obtain a slow-release shell; wherein the addition amount of the starch is 5% of the mass of the molybdenum powder, and the addition amount of the polyvinyl alcohol is 0.5% of the mass of the molybdenum powder;

[0054] The purchased ferrotitanium alloy powder is placed in a hydrogen absorption reaction kettle, vacuumizing is performed to reduce the pressure to below 0.1 Pa, and the temperature is raised to 130 ℃ and kept for 1 h; vacuumizing is performed on the hydrogen absorption reaction kettle to reduce the pressure to below 10 -2 Pa, the temperature is raised to 300 ℃, then hydrogen gas (with a purity of 99.99%) is introduced, the pressure of the hydrogen absorption reaction kettle is adjusted to 2 MPa, and the pressure is kept for 1 h; then the temperature is raised to 500 ℃ and the hydrogen gas is released by reducing the pressure; the hydrogen absorption-hydrogen release process is repeated for 3 times; after vacuumizing the hydrogen absorption reaction kettle to reduce the pressure to below 10 -2 Pa, the temperature is raised to 75 ℃, then hydrogen gas (with a purity of 99.99%) is introduced, the pressure of the hydrogen absorption reaction kettle is adjusted to 3 MPa, the pressure is kept for 1 h, then the valve is closed to stop hydrogen absorption, and the hydrogen-filled ferrotitanium hydrogen storage alloy powder is obtained;

[0055] The ferrotitanium hydrogen storage alloy powder is injected into the slow-release shell, and then the slow-release shell is sealed by welding to obtain the hydrogen storage material;

[0056] It is detected that the porosity of the slow-release shell is 3.5%, and the pore size is 4.1-25 μm;

[0057] S14: placing the green body in a vacuum sintering furnace, surrounding the adsorbent sheet and the hydrogen storage material around the green body, opening the vacuum to 5x10 -2 Pa, and then heating to 950℃, holding for 12h, to obtain the zinc telluride target; wherein the thickness of the adsorbent sheet is 0.2cm, the material is a zirconium-based alloy with a mass ratio of Zr, Co, and Ce of 75:23:2, the distance between the adsorbent sheet and the green body is 0.2cm, and the distance between the hydrogen storage material and the green body is 0.5cm.

[0058] Example 2

[0059] This example provides a method for preparing a zinc telluride target, which differs from Example 1 in that only an adsorbent sheet is used to surround the green body. That is, step S13 is not included; step S14 is placing the green body in a vacuum sintering furnace, surrounding the adsorbent sheet around the green body, opening the vacuum to 5x10 -2 Pa, and then heating to 950℃, holding for 12h, to obtain the zinc telluride target; wherein the thickness of the adsorbent sheet is 0.2cm, the material is a zirconium-based alloy with a mass ratio of Zr, Co, and Ce of 75:23:2, and the distance between the adsorbent sheet and the green body is 0.2cm.

[0060] Example 3

[0061] This example provides a method for preparing a zinc telluride target, which differs from Example 1 in that only a hydrogen storage material is used to surround the green body. That is, step S14 is placing the green body in a vacuum sintering furnace, surrounding the hydrogen storage material around the green body, opening the vacuum to 5x10 -2 Pa, and then heating to 950℃, holding for 12h, to obtain the zinc telluride target; wherein the distance between the hydrogen storage material and the green body is 0.5cm.

[0062] Example 4

[0063] This example provides a method for preparing a zinc telluride target, which differs from Example 1 in that:

[0064] Step S11 is replacing the "zinc telluride powder" with "aluminum-scandium alloy powder".

[0065] Example 5

[0066] This example provides a method for preparing a zinc telluride target, which differs from Example 1 in that:

[0067] Step S11 is replacing the "zinc telluride powder" with "copper-gallium alloy powder".

[0068] Example 6

[0069] This example provides a method for preparing a zinc telluride target, which differs from Example 1 in that:

[0070] Step S11 is to replace the "zinc telluride powder" with "nickel vanadium alloy powder".

[0071] Example 7

[0072] The embodiment provides a preparation method of a zinc telluride target material, which is different from the example 1 in that:

[0073] Step S13 is to replace the "titanium iron alloy powder" with "ZrV2 alloy powder", and replace the "titanium iron hydrogen storage alloy powder" with "ZrV2 hydrogen storage alloy powder".

[0074] Comparative Example 1

[0075] The comparative example provides a preparation method of a zinc telluride target material, which comprises the following steps:

[0076] S1: purchasing zinc telluride powder with a purity of ≥99.99% and a particle size of 10-50 μm;

[0077] S2: forming treatment: filling the zinc telluride powder into a mold, and performing cold isostatic pressing forming treatment under a pressure of 250 MPa, and keeping pressure for 1 h to form a green body;

[0078] S3: sintering treatment: placing the green body in a vacuum sintering furnace, opening the vacuum to 5x10 -2 Pa or below, then heating to 950 ℃, and keeping temperature for 12 h to obtain the zinc telluride target material.

[0079] Related performance test analysis:

[0080] 1. The O and N contents in each target material prepared in the examples 1-7 and the comparative example 1 are respectively tested by using an oxygen-nitrogen analyzer, wherein the O content in the zinc telluride powder is <24 ppm, the N content is <12 ppm; the O content in the aluminum scandium alloy powder is <26 ppm, the N content is <11 ppm; the O content in the copper gallium alloy powder is <25 ppm, the N content is <10 ppm; the O content in the nickel vanadium alloy powder is <27 ppm, the N content is <13 ppm.

[0081] 3. After the target materials prepared in the examples 1-7 and the comparative example 1 are plastic sealed, the actual densities of the target materials are respectively tested by using the Archimedes test density method, and the relative densities are calculated by taking the theoretical density as a benchmark, through the relative density = actual density / theoretical density x 100%.

[0082] The test results are shown in Table 1 as follows:

[0083] Table 1

[0084]

[0085] As can be seen from Table 1, the density of the target material prepared in Examples 1-7 is significantly higher than that of Comparative Example 1, and the O, N and total impurity contents of the target material prepared in Examples 1-7 are significantly lower than those of Comparative Example 1, indicating that the adsorbent sheet and / or hydrogen storage material are used to assist sintering in the embodiments of the present application, the adsorbent sheet can absorb O2, N2, CO2 and other impurities in the sintering environment, promote the rapid discharge of gas in the pores of the sintered body, promote the shrinkage of the material, thereby greatly reducing the pores and defects, and improving the density and purity of the alloy target material. The hydrogen storage material releases hydrogen gas to consume O2 in the sintering environment during the sintering process, effectively inhibits oxygen impurities, and also reduces the metal oxides in the sintered body to generate water vapor, thereby reducing the oxygen content of the alloy target material.

[0086] The density of the target material prepared in Example 1 is significantly higher than that of Examples 2-3, and the O, N and total impurity contents of the target material prepared in Example 1 are significantly lower than those of Examples 2-3, indicating that the adsorbent sheet and hydrogen storage material are used to assist sintering in the embodiments of the present application, the adsorbent sheet absorbs O2, N2, CO2 and other impurities in the sintered body and the sintering environment, and the hydrogen storage material consumes O2 in the sintering environment to inhibit oxygen impurities, and reduces the metal oxides to generate water vapor, thereby reducing the oxygen content of the alloy target material, and thus the two synergistically improve the purity and density of the target material.

[0087] The above only describes the preferred embodiments of the present application and is not intended to limit the present application, and any modifications, equivalent replacements and improvements made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. A method of producing an alloy target material, characterized by, The method comprises the following steps: providing a target alloy powder; isostatic pressing the target alloy powder to form a green body; surrounding a hydrogen storage material around the green body, and then performing a first sintering treatment to obtain an alloy target; wherein the hydrogen storage material comprises a slow-release shell and a hydrogen storage alloy powder filled in the slow-release shell, the hydrogen storage alloy powder is used to provide hydrogen release, and the slow-release shell is provided with pores for controlling the hydrogen release rate of the hydrogen storage alloy powder.

2. The production method according to claim 1, wherein The step of surrounding the hydrogen storage material around the green body further comprises surrounding the hydrogen storage material and an adsorbent sheet around the green body; wherein the distance between the adsorbent sheet and the green body is greater than or equal to 0.1 cm, and the distance between the hydrogen storage material and the green body is greater than or equal to 0.1 cm.

3. The production method according to claim 2, wherein The thickness of the adsorbent sheet is 0.05-0.5 cm; and / or, the adsorbent sheet is selected from a zirconium-based alloy or a titanium-based alloy.

4. The production method according to claim 3, wherein The zirconium-based alloy comprises Zr and M1 in a mass ratio of (70-90):(10-30), and the M1 is selected from one or more of Ti, V, Al, Fe, Co, La, Ce, Pr, Nd, and Y; or, the titanium-based alloy comprises Ti and M2 in a mass ratio of (60-90):(10-40), and the M2 is selected from one or more of Zr, Mo, Ni, V, Al, Fe, and Mn.

5. The production method according to claim 1, wherein At least one of the following conditions is met: The thickness of the slow-release shell is 0.01-0.2 cm; The pore size of the pores is 0.3-35 μm; The porosity of the slow-release shell is 0.8-8%; The material of the slow-release shell is selected from one or more of molybdenum, tungsten, niobium, and tantalum; The particle size of the hydrogen storage alloy powder is 100-500 μm; The hydrogen storage alloy powder is selected from any one of a titanium-based hydrogen storage alloy powder, a zirconium-based hydrogen storage alloy powder, and a vanadium-based hydrogen storage alloy powder.

6. The production method according to claim 5, wherein The titanium-based hydrogen storage alloy powder comprises Ti and M3, and the M3 is selected from one or more of Fe, Mn, Cr, Zr, and V; and / or, the zirconium-based hydrogen storage alloy powder comprises Zr and M4, and the M4 is selected from one or more of V, Cr, Mn, Ni, Fe, and Ti; and / or, the vanadium-based hydrogen storage alloy powder comprises V and M5, and the M5 is selected from one or more of Ti, Zr, Cr, Fe, Mn, and Ni.

7. The production method according to claim 1, wherein The step of preparing the slow-release shell comprises: mixing a slow-release material powder, a pore-forming agent, a binder, and ethanol to obtain a slurry; injecting the slurry into a mold to form a green body; performing a pre-sintering treatment and a second sintering treatment on the green body to obtain a slow-release shell.

8. The production method according to claim 7, wherein At least one of the following conditions is met: The pore-forming agent is selected from any one of starch, urea, ammonium bicarbonate, and polymethyl methacrylate; The addition amount of the pore-forming agent is 1-10% of the mass of the slow-release material powder; The particle size of the pore-forming agent is 0.5-50 μm; The temperature of the pre-sintering treatment is 300-600 ℃, and the time is 1-4 h; The temperature of the second sintering treatment is 1500-2400 ℃, and the time is 4-24 h.

9. The production method according to any one of claims 1 to 8, wherein At least one of the following conditions is met: The vacuum degree of the first sintering treatment is 10 -2 ~10 -3 Pa, temperature is 500~1400℃, time is 4~24h; The purity of the target alloy powder is greater than or equal to 99.99%, and the particle size is 10-50 μm; The target alloy powder includes any one of zinc telluride alloy powder, aluminum scandium alloy powder, copper gallium alloy powder, molybdenum niobium alloy powder, molybdenum tungsten alloy powder and neodymium iron boron alloy powder. The target alloy powder includes any one of zinc telluride alloy powder, aluminum scandium alloy powder, copper gallium alloy powder, molybdenum niobium alloy powder, molybdenum tungsten alloy powder and neodymium iron boron alloy powder.

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