A nickel-platinum-cerium alloy target material and a method for manufacturing the same

Abstract

The application belongs to the technical field of target material preparation, and discloses a nickel-platinum-cerium alloy target material and a preparation method thereof, the preparation method comprising the following steps: step 2: liquid cerium, liquid nickel and liquid platinum are respectively put into a gas-water combined atomization device to perform gas-water combined atomization powdering and granulating, drying and screening by a screening machine to obtain nickel powder A, platinum powder A and cerium powder A; step 3: the nickel powder A, the platinum powder A and the cerium powder A are sequentially subjected to wet ball milling and centrifugal separation to obtain nickel powder B, platinum powder B and cerium powder B, and the nickel powder B, the platinum powder B and the cerium powder B are mixed to obtain a nickel-platinum-cerium alloy powder; wherein in step 2, the liquid for water atomization in the gas-water combined atomization powdering and granulating is a mixed liquid composed of water, sulfuric acid / hydrogen peroxide micro-etching agent and a dispersing agent, and the ratio of the water, the sulfuric acid / hydrogen peroxide micro-etching agent and the dispersing agent is 10:0.5-1:1-2. The nickel powder, the platinum powder and the cerium powder with small average particle size and good sphericity obtained by the application are used for preparing the nickel-platinum-cerium alloy target material.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of target materials, in particular to a nickel-platinum-cerium alloy target material. BACKGROUND

[0002] Ultra-high purity, high utilization rate and good deposition uniformity are excellent characteristics pursued by high-quality target materials. Therefore, on the basis of the basic preparation method of the target material, the process needs to be continuously optimized to improve the quality of the target material. Specifically, improving the quality of the target material from high purity, reducing the grain size of the target material, and other organizational structure control will become the development trend of the preparation process of nickel-platinum alloy target materials.

[0003] With the development of aerospace and automobile industry, the service performance requirements of metal materials are becoming higher and higher. Therefore, high-temperature-resistant materials with higher high-temperature strength, creep resistance, oxidation resistance, corrosion resistance and dimensional stability need to be developed. As an active element with excellent performance, rare earth element Ce has the advantages of being widely used and cost-effective. The effect of adding Ce on improving the performance of alloy target materials is very significant.

[0004] Nickel-platinum-cerium alloy target material is widely used as an excellent contact material in semiconductor manufacturing. Nickel-platinum-cerium alloy target material has become a key material for ensuring semiconductor devices and developing semiconductor technology. Its growing demand provides opportunities and challenges for the development of China's precious metal target material manufacturing industry.

[0005] Since there is not much research on nickel-platinum-cerium alloy target material in the prior art, the preparation of nickel-platinum-cerium alloy target material needs to go through research and development from scratch. D1: Chinese patent 202210176058.6 discloses a high-strength chromium-aluminum alloy target material and a preparation method thereof. The chromium-aluminum alloy target material contains aluminum and chromium elements, wherein the aluminum element accounts for not less than 15% by weight, and the rest is chromium element. Its characteristics are high strength or toughness, easy to process into complex shape, and not easy to crack or break. The main process of preparing the target material includes mixing of chromium powder, aluminum powder and other doped powders, packaging and degassing, hot isostatic pressing, machining, etc.

[0006] The above-mentioned patent also discloses a method for preparing a high-strength chromium-aluminum alloy target material, comprising the following steps:

[0007] B1, powder mixing: preparing chromium powder and aluminum powder, mixing the chromium powder and aluminum powder uniformly to form a mixture; wherein the aluminum powder accounts for not less than 15%;

[0008] B2, packaging and degassing: loading the mixture into a metal package, welding the end cover and the air pipe, and then heating and degassing;

[0009] B3, hot isostatic pressing: after the air is extracted, the air extraction pipe on the package is flattened and welded to seal and perform hot isostatic pressing to obtain a chromium-aluminum target blank;

[0010] B4, machining: removing the package of the chromium-aluminum target blank after hot isostatic pressing, and machining into a finished target material.

[0011] The above patent prepares a chromium-aluminum alloy target material containing aluminum elements, and its preparation method can be used as a reference for preparing a nickel-platinum-cerium alloy target material. However, experiments have found that the performance of the nickel-platinum-cerium alloy target material prepared only by the steps of the above patent cannot meet the development needs of the aerospace and automobile industries, mainly due to the following two reasons:

[0012] (1) The particle size and sphericity of the raw nickel powder, platinum powder, and cerium powder are not good enough, resulting in a decrease in the density and other properties of the nickel-platinum-cerium alloy target material;

[0013] (2) The oxygen content in the raw nickel powder, platinum powder, and cerium powder is too high, resulting in a large number of target material organizational holes, poor mechanical processing performance of the target material, and an increased cracking tendency of the target material during the coating process.

[0014] Based on the above reasons, it is necessary to develop a nickel-platinum-cerium alloy target material preparation method that can effectively improve the comprehensive performance of the nickel-platinum-cerium alloy target material and reduce the number of organizational holes in the nickel-platinum-cerium alloy target material to meet the development needs of semiconductor products for the aerospace and automobile industries. SUMMARY

[0015] One of the purposes of the present application is to provide a preparation method of a nickel-platinum-cerium alloy target material to solve the technical problem that there is no technology in the prior art that can effectively improve the comprehensive performance of the nickel-platinum-cerium alloy target material and reduce the number of organizational holes in the nickel-platinum-cerium alloy target material for the nickel-platinum-cerium alloy target material itself.

[0016] Another purpose of the present application is to provide a nickel-platinum-cerium alloy target material with high comprehensive performance that can meet the development needs of semiconductor products for the aerospace and automobile industries.

[0017] To achieve the above purpose, the present application provides a preparation method of a nickel-platinum-cerium alloy target material, comprising the following steps:

[0018] Step 1: Put cerium, nickel, and platinum metal raw materials into a smelting furnace to heat and smelt into liquid cerium, liquid nickel, and liquid platinum;

[0019] Step 2: Put the liquid cerium, liquid nickel, and liquid platinum into a gas-water combined atomization device to perform gas-water combined atomization, powder making, and granulation, and perform drying and screening to obtain nickel powder A, platinum powder A, and cerium powder A;

[0020] Step 3: the nickel powder A, platinum powder A, cerium powder A are sequentially subjected to wet ball milling and centrifugal separation to obtain nickel powder B, platinum powder B, cerium powder B, and the nickel powder B, platinum powder B, cerium powder B are mixed to obtain the nickel platinum cerium alloy powder;

[0021] Step 4: the nickel platinum cerium alloy powder obtained in step 3 is loaded into a mold, the mold is sealed and subjected to vacuum thermal degassing treatment;

[0022] Step 5: the mold after vacuum thermal degassing in step 4 is placed into a hot isostatic pressing furnace for cold pressure sintering to obtain a nickel platinum cerium alloy target blank;

[0023] Step 6: the nickel platinum cerium alloy target blank is sequentially subjected to machining, detection, cleaning and drying to obtain a nickel platinum cerium alloy target material;

[0024] In step 2, the liquid for water atomization in the gas-water combined atomization powder making and granulation is a mixed liquid composed of water, sulfuric acid / hydrogen peroxide micro-etching agent and dispersant, and the ratio of the water, sulfuric acid / hydrogen peroxide micro-etching agent and dispersant is 10:0.5-1:1-2.

[0025] Further, the specific operation of step 1 is that the cerium metal raw material is put into a smelting furnace and heated to 850℃ for smelting for 60 minutes to obtain liquid cerium, the nickel metal raw material is put into a smelting furnace and heated to 1500℃ for smelting for 60 minutes to obtain liquid nickel, and the platinum metal raw material is put into a smelting furnace and heated to 1800℃ for smelting for 60 minutes to obtain liquid platinum.

[0026] Further, in step 2, the gas for gas atomization in the gas-water combined atomization powder making and granulation is nitrogen, the gas pressure is 0.9MPa, the angle between the nitrogen jet direction and the vertical downward direction is 45°, the liquid for water atomization is a mixed liquid composed of water, sulfuric acid / hydrogen peroxide micro-etching agent and dispersant, the water pressure is 130MPa, and the angle between the water jet direction and the vertical downward direction is 35°.

[0027] Further, the specific operation of step 3 is that the nickel powder A and zirconia balls are added into a ball milling tank in a mass ratio of 1:5, argon is filled, isopropyl alcohol is added, wet ball milling and centrifugal separation are carried out to obtain the nickel powder B, the ball milling speed is 200r / min, and the ball milling time is 2h; the platinum powder A and cerium powder A are respectively subjected to wet ball milling and centrifugal separation in the same way to obtain the platinum powder B and cerium powder B; then the nickel powder B, platinum powder B and cerium powder B are put into a V-type mixer and mixed for 12h to obtain the nickel platinum cerium alloy powder.

[0028] Further, the temperature for vacuum thermal degassing in step 4 is 300-500℃, the vacuum degree is greater than 1×10-3Pa and less than 8×10 -3 Pa, and the holding time is 1-5h.

[0029] Preferably, the cold state pressure sintering of step 5 is specifically operated as follows: first, heated to 300-600 DEG C, and then preheated isostatic pressing treatment is carried out under the pressure of 90-180 MPa for 1-8 h, then heated to 800-1000 DEG C, and then hot isostatic pressing treatment is carried out under the pressure of 90-180 MPa for 3-8 h, and then the mold is removed to obtain the nickel platinum cerium alloy target blank.

[0030] Further, the process of loading the nickel platinum cerium alloy powder into the mold in step 4 needs to be carried out under inert gas protection.

[0031] Preferably, the dispersant is one or more of sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, fatty acid polyethylene glycol ester and polyether.

[0032] Preferably, in the nickel platinum cerium alloy powder of step 3, the mass ratio of the nickel powder B, the platinum powder B and the cerium powder B is 93.2-97.1:2.3-5.6:0.6-1.2.

[0033] The application further discloses a nickel platinum cerium alloy target prepared by the preparation method.

[0034] Beneficial effects

[0035] Compared with the prior art, the application has at least the following advantages:

[0036] (1) The gas-water combined atomization powder granulation technology and the ball milling technology are combined to effectively control the particle size and sphericity of the nickel powder, the platinum powder and the cerium powder, so that the nickel powder, the platinum powder and the cerium powder with small average particle size and good sphericity are obtained for preparing the nickel platinum cerium alloy target, thereby improving the comprehensive performance of the nickel platinum cerium alloy target.

[0037] (2) In the gas-water combined atomization powder granulation, the mixed liquid composed of water, sulfuric acid / hydrogen peroxide micro-etching agent and dispersant is used as the water atomization liquid, so that the direct contact reaction between water and metal liquid is effectively reduced, the oxygen content of the powder is reduced, the dispersant has good wetting and dispersing effect due to the steric hindrance effect, the dispersibility of the powder is improved, the surface activity of the particles or the powder is increased, the tap density of the powder is improved, the electrostatic is removed, the flowability is increased, and the segregation phenomenon is eliminated; on the other hand, the dispersant can produce a synergistic effect with the micro-etching agent, the dispersant improves the wettability of the metal surface, can further promote the adsorption of the micro-etching agent on the metal surface, improves the etching efficiency, and finally obtains the powder with near-spherical shape, high tap density and low oxygen content.

[0038] (3) The present application further reduces the oxygen content of the nickel powder, platinum powder and cerium powder particles by using sulfuric acid / hydrogen peroxide micro-etchant to corrode the oxide film on the surface of the nickel powder, platinum powder and cerium powder particles in the gas-water combined atomization powder preparation and granulation, and then using a ball milling process to further break and remove the oxide film on the surface of the nickel powder, platinum powder and cerium powder particles that have been corroded, thereby significantly reducing the number of holes in the prepared nickel platinum cerium alloy target material and effectively improving the performance of the nickel platinum cerium alloy target material;

[0039] (4) The present application prepares the nickel platinum cerium alloy target material by the cold state pressurized sintering method, and the step-by-step heating, pressurizing and temperature and pressure maintaining method can further ensure that the target material can be fully sintered, improve the comprehensive performance of the target material, and at the same time reduce the production cost of the nickel platinum cerium alloy target material. BRIEF DESCRIPTION OF DRAWINGS

[0040] The present application will be further described below in combination with the drawings and examples;

[0041] Figure 1 is the target material structure diagram of Example 2 of the present application;

[0042] Figure 2 is the target material structure diagram of Comparative Example 1 of the present application;

[0043] Figure 3 is the target material structure diagram of Comparative Example 2 of the present application;

[0044] Figure 4 is the target material structure diagram of Comparative Example 3 of the present application;

[0045] Figure 5 is the target material structure diagram of Comparative Example 4 of the present application;

[0046] Figure 6 is the target material structure diagram of Comparative Example 5 of the present application. DETAILED DESCRIPTION

[0047] The present application will be further described below in combination with the drawings and examples;

[0048] In order to explain the technical content of the present application in detail, the following further describes the embodiments.

[0049] In the following examples and comparative examples, centrifugal separation is a common technique for those skilled in the art, and the material is placed in a centrifuge for centrifugal separation, and the specific operation steps are not described in detail; at the same time, the machining of the target material is the existing technology of the target material, and the specific operation steps are not described in detail.

[0050] Example 1

[0051] A nickel platinum cerium alloy target is prepared by the following steps:

[0052] Step 1: Put cerium metal raw material into a smelting furnace and heat to 850℃ for 60 min to obtain liquid cerium, put nickel metal raw material into the smelting furnace and heat to 1500℃ for 60 min to obtain liquid nickel, and put platinum metal raw material into the smelting furnace and heat to 1800℃ for 60 min to obtain liquid platinum;

[0053] Step 2: Put the liquid cerium, liquid nickel and liquid platinum into a gas-water combined atomization device respectively for gas-water combined atomization, drying and screening to obtain nickel powder A, platinum powder A and cerium powder A; the gas for gas atomization is nitrogen, the gas pressure is 0.9 MPa, the angle between the nitrogen jet direction and the vertical downward direction is 45°, the liquid for water atomization is a mixed liquid composed of water, sulfuric acid / hydrogen peroxide micro-etching agent and sodium tripolyphosphate, the water pressure is 130 MPa, and the angle between the water jet direction and the vertical downward direction is 35°;

[0054] Step 3: Put nickel powder A and zirconia balls into a ball mill tank according to a mass ratio of 1:5, fill in argon and add isopropyl alcohol for wet ball milling and centrifugal separation to obtain nickel powder B, the ball milling speed is 200 r / min, and the ball milling time is 2 h; in the same way, platinum powder A and cerium powder A are wet ball milled and centrifugally separated to obtain platinum powder B and cerium powder B; then the nickel powder B, platinum powder B and cerium powder B are put into a V-type mixer and mixed for 12 h to obtain a nickel platinum cerium alloy powder;

[0055] Step 4: Put the nickel platinum cerium alloy powder obtained in step 3 into a mold under the protection of argon, seal the mold and perform vacuum thermal degassing treatment, the vacuum thermal degassing temperature is 400℃, the vacuum degree is 6×10 -3 Pa, and the holding time is 3 h;

[0056] Step 5: Put the mold after vacuum thermal degassing in step 4 into a hot isostatic pressing furnace for cold-state pressure sintering, first heat to 500℃, then preheat isostatic pressing treatment under a pressure of 150 MPa for 2 h, then heat to 1000℃, and then hot isostatic pressing treatment under a pressure of 150 MPa for 6 h, remove the mold, and obtain a nickel platinum cerium alloy target blank;

[0057] Step 6: Machine, detect, clean and dry the nickel platinum cerium alloy target blank in sequence to obtain a nickel platinum cerium alloy target material;

[0058] In step 2, the ratio of water, sulfuric acid / hydrogen peroxide micro-etching agent and sodium tripolyphosphate is 10:0.5:1;

[0059] The mass ratio of the nickel powder B, the platinum powder B and the cerium powder B in the nickel platinum cerium alloy powder of step 3 is 94:5.2:0.8.

[0060] Example 2

[0061] A nickel platinum cerium alloy target is prepared by the following steps:

[0062] Step 1: Put the cerium metal raw material into a smelting furnace and heat to 850℃ for 60 minutes to obtain liquid cerium, put the nickel metal raw material into the smelting furnace and heat to 1500℃ for 60 minutes to obtain liquid nickel, and put the platinum metal raw material into the smelting furnace and heat to 1800℃ for 60 minutes to obtain liquid platinum;

[0063] Step 2: Put the liquid cerium, the liquid nickel and the liquid platinum into a gas-water combined atomization device respectively to perform gas-water combined atomization, drying and screening to obtain nickel powder A, platinum powder A and cerium powder A; the gas for gas atomization is nitrogen, the gas pressure is 0.9MPa, the angle between the nitrogen jet direction and the vertical downward direction is 45°, the liquid for water atomization is a mixed liquid composed of water, sulfuric acid / hydrogen peroxide micro-etching agent and sodium pyrophosphate, the water pressure is 130MPa, and the angle between the water jet direction and the vertical downward direction is 35°;

[0064] Step 3: Put the nickel powder A and zirconia balls into a ball mill tank according to a mass ratio of 1:5, fill in argon and add isopropyl alcohol to perform wet ball milling and centrifugal separation to obtain nickel powder B, the ball milling speed is 200r / min, and the ball milling time is 2h; in the same way, the platinum powder A and the cerium powder A are respectively subjected to wet ball milling and centrifugal separation to obtain platinum powder B and cerium powder B; then the nickel powder B, the platinum powder B and the cerium powder B are put into a V-type mixer to mix for 12h to obtain a nickel platinum cerium alloy powder;

[0065] Step 4: Put the nickel platinum cerium alloy powder obtained in step 3 into a mold under the protection of argon, seal the mold and perform vacuum thermal degassing treatment, the vacuum thermal degassing temperature is 400℃, the vacuum degree is 6x10 -3 Pa, and the holding time is 3h;

[0066] Step 5: Put the mold after vacuum thermal degassing in step 4 into a hot isostatic pressing furnace to perform cold-state pressure sintering, first heat to 300℃, then perform pre-heat isostatic pressing treatment under the pressure of 180MPa for 8h, then heat to 800℃, perform hot isostatic pressing treatment under the pressure of 120MPa for 8h, remove the mold and obtain a nickel platinum cerium alloy target blank;

[0067] Step 6: Perform machining, detection, cleaning and drying on the nickel platinum cerium alloy target blank in sequence to obtain a nickel platinum cerium alloy target;

[0068] The ratio of water, sulfuric acid / hydrogen peroxide micro-etching agent and sodium pyrophosphate in step 2 is 10:1:2;

[0069] The mass ratio of the nickel powder B, the platinum powder B and the cerium powder B in the nickel platinum cerium alloy powder of step 3 is 94:5.2:0.8.

[0070] Example 3

[0071] A nickel platinum cerium alloy target is prepared by the following steps:

[0072] Step 1: The cerium metal raw material is put into a smelting furnace and heated to 850 DEG C for 60 min to obtain liquid cerium, the nickel metal raw material is put into a smelting furnace and heated to 1500 DEG C for 60 min to obtain liquid nickel, and the platinum metal raw material is put into a smelting furnace and heated to 1800 DEG C for 60 min to obtain liquid platinum;

[0073] Step 2: The liquid cerium, the liquid nickel and the liquid platinum are respectively put into a gas-water combined atomization device for gas-water combined atomization, drying and screening to obtain a nickel powder A, a platinum powder A and a cerium powder A; wherein the gas for gas atomization in the gas-water combined atomization is nitrogen, the gas pressure is 0.9 MPa, the angle between the nitrogen jet direction and the vertical downward direction is 45 DEG, the liquid for water atomization is a mixed liquid composed of water, sulfuric acid / hydrogen peroxide micro-etching agent and fatty acid polyethylene glycol ester, the water pressure is 130 MPa, and the angle between the water jet direction and the vertical downward direction is 35 DEG;

[0074] Step 3: The nickel powder A and zirconia balls are added into a ball mill tank according to a mass ratio of 1:5, argon is filled, isopropyl alcohol is added for wet ball milling and centrifugal separation to obtain a nickel powder B, the ball milling speed is 200 r / min, and the ball milling time is 2 h; the platinum powder A and the cerium powder A are respectively wet ball milled and centrifugally separated in the same way to obtain a platinum powder B and a cerium powder B; then the nickel powder B, the platinum powder B and the cerium powder B are put into a V-type mixer for mixing for 12 h to obtain a nickel platinum cerium alloy powder;

[0075] Step 4: The nickel platinum cerium alloy powder obtained in step 3 is loaded into a mold under the protection of argon, the mold is sealed and vacuum heat degassing treatment is performed, the vacuum heat degassing temperature is 400 DEG C, the vacuum degree is 6*10 -3 Pa, and the holding time is 3 h;

[0076] Step 5: The mold after the vacuum heat degassing in step 4 is put into a hot isostatic pressing furnace for cold-state pressure sintering, first heated to 600 DEG C, preheated isostatic pressing treatment is performed at 100 MPa for 1 h, then heated to 1000 DEG C, hot isostatic pressing treatment is performed at 150 MPa for 5 h, the mold is removed, and a nickel platinum cerium alloy target blank is obtained;

[0077] Step 6: the nickel platinum cerium alloy target blank is obtained by machining, testing, cleaning and drying in sequence;

[0078] In step 2, the ratio of water, sulfuric acid / hydrogen peroxide micro-etching agent and fatty acid polyethylene glycol ester is 10:0.5:2.

[0079] In the nickel platinum cerium alloy powder of step 3, the mass ratio of nickel powder B, platinum powder B and cerium powder B is 94:5.2:0.8.

[0080] Example 4

[0081] The same as example 2, except that in the nickel platinum cerium alloy powder of step 3, the mass ratio of nickel powder B, platinum powder B and cerium powder B is 96:2.8:1.2.

[0082] Comparative Example 1

[0083] The same as example 2, except that in step 2, the liquid for water atomization in the gas-water combined atomization powder preparation granulation is water.

[0084] Comparative Example 2

[0085] The same as example 2, except that in step 2, the liquid for water atomization in the gas-water combined atomization powder preparation granulation is a mixed liquid composed of water and sulfuric acid / hydrogen peroxide micro-etching agent, and the ratio of water to sulfuric acid / hydrogen peroxide micro-etching agent is 10:3.

[0086] Comparative Example 3

[0087] The same as example 2, except that in step 2, the liquid for water atomization in the gas-water combined atomization powder preparation granulation is a mixed liquid composed of water and sodium pyrophosphate, and the ratio of water to sodium pyrophosphate is 10:3.

[0088] Comparative Example 4

[0089] The same as example 2, except that the ball milling step in step 3 is cancelled, and the nickel powder A, platinum powder A and cerium powder A are directly put into the V-type mixer for mixing for 12h to obtain the nickel platinum cerium alloy powder.

[0090] Comparative Example 5

[0091] The same as example 2, except that step 5 is changed to: the mold after vacuum thermal degassing in step 4 is put into a hot isostatic pressing furnace and heated to 800℃, and hot isostatic pressing treatment is carried out under a pressure of 120MPa for 16h, and then the mold is removed to obtain the nickel platinum cerium alloy target blank.

[0092] Performance test

[0093] Target density was measured by Archimedes displacement method;

[0094] Target purity was measured by inductively coupled plasma optical emission spectrometer;

[0095] Target average grain size was measured by X-ray diffractometer;

[0096] Target microstructure was obtained by metallographic analyzer.

[0097] The nickel platinum cerium alloy target materials prepared in Examples 1-4 and Comparative Examples 1-5 were tested for performance according to the above test methods, and the results are shown in Table 1 and Figures 1-6

[0098] Table 1 Performance test results of nickel platinum cerium alloy target materials prepared in Examples 1-4 and Comparative Examples 1-5

[0099]

[0100]

[0101] According to the results in Table 1, it can be seen that:

[0102] ​According to the data comparison of the embodiment 2 and the comparative examples 1, 2 and 3, it can be seen that the mixed liquid composed of water, sulfuric acid / hydrogen peroxide micro-etchant and dispersant as the liquid for water atomization can effectively improve the performance of the nickel platinum cerium alloy target material, and the reason is that the sulfuric acid / hydrogen peroxide micro-etchant can effectively reduce the direct contact reaction of water and metal liquid, and reduce the oxygen content of the powder. At the same time, the dispersant has good wetting and dispersing effect due to the steric hindrance effect, can improve the dispersibility of the powder, increase the surface activity of the particles or powder, improve the tap density of the powder, remove static electricity, increase fluidity, and prevent segregation. On the other hand, the dispersant can produce synergistic effect with the micro-etchant, the dispersant improves the wettability of the metal surface, can further promote the adsorption of the micro-etchant on the metal surface, improve the etching efficiency, and finally obtain the powder with near-spherical shape, high tap density and low oxygen content, so as to prepare the nickel platinum cerium alloy target material with high density, high purity and small average grain size. The comparative example 1 only uses water as the liquid for water atomization, on the one hand, the nickel, platinum and cerium powder particles appear partial aggregation phenomenon in the gas-water combined atomization process, which leads to the poor average particle size and sphericity of the nickel, platinum and cerium powder particles, and on the other hand, the direct contact reaction of water and metal liquid and the lack of etchant to damage the oxide film on the surface of the nickel, platinum and cerium powder particles increase the oxygen content of the nickel, platinum and cerium powder particles, thereby reducing the performance of the nickel platinum cerium alloy target material. The comparative example 2 only uses sulfuric acid / hydrogen peroxide micro-etchant combined with water, although it can effectively reduce the oxygen content of the nickel, platinum and cerium powder particles, but it does not solve the partial aggregation phenomenon of the nickel, platinum and cerium powder particles in the gas-water combined atomization process, so that the oxygen content of the nickel, platinum and cerium powder particles is not reduced too much. The aggregated particles not only have large particle size and poor sphericity, but also have oxygen wrapped inside the particles in the aggregation process, which makes it difficult for the micro-etchant to reduce the oxygen content. Therefore, in the preparation process of the nickel, platinum and cerium powder particles, the simple use of sulfuric acid / hydrogen peroxide micro-etchant combined with water as the liquid for water atomization, although it slightly improves the comprehensive performance of the nickel platinum cerium alloy target material prepared by the comparative example 1, but the improvement is not obvious and the average grain size of the target material is larger. The comparative example 3 only uses dispersant combined with water, although it can effectively reduce the average grain size of the target material, but the oxygen content of the powder particles is not reduced, which leads to the unobvious improvement of the performance of the target material.

[0103] According to the data comparison of the embodiment 2 and the comparative example 4, it can be seen that the lack of ball milling step to further process the nickel, platinum and cerium powder particles obtained by gas-water combined atomization will seriously affect the preparation performance of the target material, and the reason is that the ball milling step can further remove the oxide film on the surface of the nickel, platinum and cerium powder particles which have been corroded, thereby greatly reducing the oxygen content of the nickel, platinum and cerium powder particles, and the ball milling can further improve the sphericity and particle size uniformity of the powder, thereby improving the comprehensive performance of the prepared target material.

[0104] According to the comparison of the data of the embodiment 2 and the comparative example 5, it can be seen that the cold pressure sintering method of step-by-step heating, pressure increasing and temperature and pressure maintaining adopted in the present application can obviously improve the sintering effect of the target material and promote the comprehensive performance of the target material.

[0105] The embodiments presented herein are merely examples selected from combinations of all possible embodiments. The appended claims should not be limited by the embodiments that illustrate the present application. Some numerical ranges include sub-ranges within them, and variations in these ranges should also be covered by the appended claims.

Claims

1. A method for preparing a nickel-platinum-cerium alloy target, characterized in that, Includes the following steps: Step 1: Add cerium, nickel, and platinum metal raw materials to a smelting furnace and heat to melt them into liquid cerium, liquid nickel, and liquid platinum, respectively; Step 2: Liquid cerium, liquid nickel, and liquid platinum are respectively fed into a gas-water combined atomization device for gas-water combined atomization to form powder and granules, and then dried and sieved by a sieve to obtain nickel powder A, platinum powder A, and cerium powder A; Step 3: Sequentially perform wet ball milling and centrifugal separation on nickel powder A, platinum powder A, and cerium powder A to obtain nickel powder B, platinum powder B, and cerium powder B. Mix nickel powder B, platinum powder B, and cerium powder B to obtain nickel-platinum-cerium alloy powder. Step 4: Load the nickel-platinum-cerium alloy powder obtained in Step 3 into the mold, seal the mold, and then perform vacuum thermal degassing treatment. Step 5: Place the mold after vacuum hot degassing in Step 4 into a hot isostatic pressing furnace for cold pressure sintering to obtain a nickel-platinum-cerium alloy target blank. Step 6: The nickel-platinum-cerium alloy target blank is sequentially machined, inspected, cleaned, and dried to obtain the nickel-platinum-cerium alloy target material; In step 2, the liquid used for water atomization in the combined air-water atomization granulation process is a mixed liquid composed of water, sulfuric acid / hydrogen peroxide micro-etching agent, and dispersant, wherein the ratio of water, sulfuric acid / hydrogen peroxide micro-etching agent, and dispersant is 10:0.5-1:1-2. In the nickel-platinum-cerium alloy powder of step 3, the mass ratio of nickel powder B, platinum powder B, and cerium powder B is 94-96: 2.8-5.2：0.8-1.2。 2. The method for preparing the nickel-platinum-cerium alloy target according to claim 1, characterized in that, The specific operation of step 1 is as follows: put cerium metal raw material into a smelting furnace and heat it to 850°C for 60 minutes to obtain liquid cerium; put nickel metal raw material into a smelting furnace and heat it to 1500°C for 60 minutes to obtain liquid nickel; put platinum metal raw material into a smelting furnace and heat it to 1800°C for 60 minutes to obtain liquid platinum.

3. The method for preparing the nickel-platinum-cerium alloy target according to claim 1, characterized in that, In step 2, the gas used for gas-water combined atomization granulation is nitrogen, with a pressure of 0.9 MPa and an angle of 45° between the nitrogen injection direction and the vertical downward direction. The liquid used for water atomization is a mixture of water, sulfuric acid / hydrogen peroxide micro-etching agent, and dispersant, with a water pressure of 130 MPa and an angle of 35° between the water injection direction and the vertical downward direction.

4. The method for preparing the nickel-platinum-cerium alloy target according to claim 1, characterized in that, The specific operation of step 3 is as follows: nickel powder A and zirconia balls are added to a ball mill jar at a mass ratio of 1:5, argon gas is introduced and isopropanol is added for wet ball milling and centrifugation to obtain nickel powder B. The ball milling speed is 200 r / min and the ball milling time is 2 h. Platinum powder A and cerium powder A are wet ball milled and centrifuged in the same way to obtain platinum powder B and cerium powder B. Then, nickel powder B, platinum powder B and cerium powder B are put into a V-type mixer and mixed for 12 h to obtain nickel-platinum-cerium alloy powder.

5. The method for preparing the nickel-platinum-cerium alloy target according to claim 1, characterized in that, In step 4, the temperature for vacuum thermal degassing is 300-500℃, and the vacuum degree is greater than 1×10⁻⁶. -3 Pa is less than 8 × 10 -3 Pa, heat preservation time is 1-5 hours.

6. The method for preparing the nickel-platinum-cerium alloy target according to claim 1, characterized in that, The specific operation of the cold pressure sintering in step 5 is as follows: first, heat the temperature to 300-600℃, and hold it at 90-180MPa pressure for 1-8 hours for preheating isostatic pressing treatment. Then, heat the temperature to 800-1000℃, and hold it at 90-180MPa pressure for 3-8 hours for hot isostatic pressing treatment. Remove the mold to obtain the nickel-platinum-cerium alloy target blank.

7. The method for preparing the nickel-platinum-cerium alloy target material according to any one of claims 1-6, characterized in that, The process of loading nickel-platinum-cerium alloy powder into the mold in step 4 must be carried out under inert gas protection.

8. The method for preparing the nickel-platinum-cerium alloy target according to claim 1, characterized in that, The dispersant is one or more of sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, fatty acid polyethylene glycol ester, and polyether.

9. A nickel-platinum-cerium alloy target material, characterized in that, It was prepared using the method for preparing nickel-platinum-cerium alloy targets as described in any one of claims 1-8.

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