Zinc oxide titanium yttrium powder, target material and preparation method of powder and target material

Abstract

The application belongs to the technical field of oxide target materials, and discloses a zinc titanium yttrium oxide powder, a target material, and a preparation method of the powder and the target material. The preparation method comprises the following steps: step 1: after yttrium oxide powder, titanium oxide powder, pure water and a first dispersant are mixed and pre-dispersed, wet grinding is performed to obtain slurry one; step 2: after zinc oxide powder, pure water and a second dispersant are added to the slurry one and mixed and pre-dispersed, wet grinding is performed to obtain slurry two; step 3: after a binder is added to the slurry two and mixed and pre-dispersed, wet grinding is performed to obtain slurry three; and step 4: the slurry three is sequentially subjected to air-water combined atomization granulation, mixing and screening to obtain the zinc titanium yttrium oxide powder. In the step 4, the air pressure of the air atomization of the air-water combined atomization granulation is 0.6-0.8 MPa, the included angle between the air jet direction and the vertical downward direction is 30-50°, the water pressure of the water atomization is 50-150 MPa, and the included angle between the water jet direction and the vertical downward direction is 30-50°.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of oxide target materials, in particular to a zinc titanium yttrium oxide powder, a target material and a preparation method of the zinc titanium yttrium oxide powder and the target material. BACKGROUND

[0002] Zinc oxide (ZnO) is a kind of wide-bandgap semiconductor material with a hexagonal wurtzite structure. It has the advantages of a large band gap coefficient, a high exciton binding energy and a low dielectric constant. In addition, it also has excellent semiconductor and electro-optical characteristics. Therefore, it has a profound research and development in the research on light-emitting diodes, solar cells and sensors.

[0003] The photoelectric properties of ZnO thin films can be regulated by doping other elements. Research shows that double-element or multi-element doping can fully utilize the advantages of each element doping. TiO2 and Y2O3 are beneficial to regulating the crystalline quality, light transmittance, band gap and resistivity of ZnO target materials and sputtered thin films.

[0004] Since the preparation of zinc titanium yttrium oxide powder and target material is not studied in the current disclosed technology, the preparation technology of other oxide powders and target materials needs to be referred to. For example, D1: Chinese Patent Application 202310678889.8 discloses an indium oxide doped titanium tantalum cerium target material and a preparation method thereof. The preparation method is as follows: indium oxide, titanium oxide, tantalum oxide and cerium oxide powders are weighed according to the molar ratio of 90.5-92.5:1.5-2.5:3-5:1.5-2.5, then added into pure water with a dispersing agent and stirred to disperse uniformly to obtain slurry one; then indium oxide powder, a dispersing agent and water are added and wet ground to obtain slurry two; then a binder is added and mixed and then wet ground to obtain slurry three; then the slurry is sprayed and granulated, then mixed and sieved to obtain a mixed powder; finally, the mixed powder is degreased and sintered after being molded and cold isostatic pressed to obtain the indium oxide doped titanium tantalum cerium target material. By limiting the composition ratio of the oxide powders and combining with the specific preparation process, the performance of the target material can be significantly improved.

[0005] According to the technical inspiration given by the technical solution of the above-mentioned patent, the doping of titanium oxide and yttrium oxide needs to be mixed, dispersed, wet ground, then sprayed and granulated to obtain a mixed oxide powder, and then cold isostatic pressed and sintered to prepare a zinc titanium yttrium oxide target material. However, it is found through experiments that the particle size uniformity and sphericity of the zinc titanium yttrium oxide powder prepared by the above-mentioned oxide powder preparation process are difficult to balance. Either the sphericity of the oxide particles is good but the particle size distribution of the powder is uneven, or the particle size distribution of the powder is even but the sphericity of the oxide particles is poor, both of which will lead to a decline in the performance of the prepared zinc titanium yttrium oxide target material.

[0006] Therefore, a technology capable of balancing the particle size uniformity and specific surface area of the zinc titanium yttrium oxide powder is needed to improve the performance of the zinc titanium yttrium oxide target and thus improve the performance of the sputtered film.

[0007] D2: An article entitled "Preparation of Microspherical Metal Powder by Water-gas Atomization Method" published in Materials Research and Application, Vol. 10, No. 3, September 2016 discloses a water-gas atomization method combining the advantages of water atomization and gas atomization. In the atomization process, it is found that the molten metal stream is broken by the gas flow and high-pressure water flow in turn, and the broken metal droplets shrink into spherical shape under the action of surface tension. The research results show that the yield of 316L metal powder D50 (8-13 μm) prepared by the atomization method reaches 78.3%, and the tap density exceeds 4.7 g / cm 3 ; the morphology of the powder is nearly spherical, and the structure is austenite and ferrite coexisting.

[0008] D3: Chinese patent 202220283288.8 discloses a water-gas combined atomization powder making device. The technical solution includes a cylinder, a support frame, an atomization pipe, an electric push rod, a rotating shaft, and a connecting ring. The atomization pipe is inserted and installed on one side of the inner wall of the upper end of the cylinder, the electric push rod is installed on the inner wall of the side of the cylinder away from the atomization pipe, the first motor is arranged on one side of the outer wall of the lower end of the electric push rod, the support frame is installed on one side of the outer wall of the first motor, the bearing is embedded and installed on one side of the outer wall of the support frame, the rotating shaft is rotatably installed in the bearing, the fixed frame is installed on one side of the outer wall of the upper end of the rotating shaft, and the connecting ring is installed on the outer wall of the fixed frame. By arranging the atomization pipe, the rotating shaft, and the connecting ring, the effect of facilitating the cleaning of the inner wall of the atomization pipe is achieved, the movement direction of the fine droplets in the atomization pipe is avoided from being affected, the atomization pipe is avoided from being blocked, and the smoothness of the movement of the fine droplets in the atomization pipe is ensured.

[0009] Based on the technical inspiration of D2 and D3, the water-gas combined atomization method can be used to balance the sphericity and particle size uniformity of the zinc titanium yttrium oxide powder. However, experiments show that the use of the process disclosed in D2 to granulate the zinc titanium yttrium oxide powder does not greatly improve the performance of the zinc titanium yttrium oxide target. Through multiple performance tests, it is known that the oxygen content of the oxide powder also has a great influence on the performance of the target.

[0010] The oxygen in the oxide powder, especially the thickness, distribution state, and content of the particle surface oxide film, has a great influence on the performance of the target and the sputtered film. A thick and continuously distributed oxide film hinders the ceramization process during sintering, reduces the interfacial bonding strength between particles, hinders the spreading and wetting of the liquid phase, directly affects the densification degree, strength, toughness, and other performance indicators of the sintered body, and thus affects the comprehensive mechanical properties of the target and the use performance of the plated film.

[0011] Therefore, the excessive oxygen content will directly affect the thickness of the oxide film on the surface of the oxide powder, and the excessive oxygen content will reduce the uniformity of the oxygen distribution in the particles. If the oxygen in the oxide particles cannot be uniformly and dispersedly distributed at the grain boundaries and the interior, holes will appear in the target material, and the density and other properties of the target material will also decrease. The oxide target material will not exhibit its own characteristics if the oxygen content in the oxide particles is too low, and will become an unqualified product.

[0012] Therefore, it is necessary to develop a technology for adjusting the oxygen content of the zinc titanium yttrium oxide particles to improve the performance of the zinc titanium yttrium oxide target material. SUMMARY

[0013] One of the purposes of the present application is to provide a preparation method of zinc titanium yttrium oxide powder, so as to solve the technical problem that the oxygen content of the zinc titanium yttrium oxide powder particles prepared by the prior art cannot be effectively controlled, thereby affecting the performance of the zinc titanium yttrium oxide target material.

[0014] Another purpose of the present application is to provide a zinc titanium yttrium oxide powder, which has a low oxygen content, and the oxygen content value can meet the needs of the target material itself, and a high-performance zinc titanium yttrium oxide target material is prepared.

[0015] Meanwhile, the present application also provides a zinc titanium yttrium oxide target material prepared by using the above-mentioned zinc titanium yttrium oxide powder, which has a high relative density, electrical conductivity and bending strength of the target material, and can meet the high performance requirements of the sputtered film.

[0016] Further, the present application also provides a preparation method of zinc titanium yttrium oxide target material, so as to prepare a high-performance zinc titanium yttrium oxide target material.

[0017] In order to achieve the above-mentioned purposes, the present application provides a preparation method of zinc titanium yttrium oxide powder, which specifically comprises the following steps:

[0018] Step 1: After mixing, pre-dispersing and wet grinding, a slurry one is obtained by using yttrium oxide powder, titanium oxide powder, pure water and a first dispersant;

[0019] Step 2: After mixing, pre-dispersing and wet grinding, a slurry two is obtained by adding zinc oxide powder, pure water and a second dispersant to the slurry one;

[0020] Step 3: After mixing, pre-dispersing and wet grinding, a slurry three is obtained by adding a binder to the slurry two;

[0021] Step 4: After air-water combined atomization granulation, mixing and screening, a zinc titanium yttrium oxide powder is obtained by using the slurry three;

[0022] The gas pressure of the gas atomization in the gas-water combined atomization and granulation in step 4 is 0.6-0.8 MPa, and the angle between the gas spraying direction and the vertical downward direction is 30-50°; the water pressure of the water atomization is 50-150 MPa, and the angle between the water spraying direction and the vertical downward direction is 30-50°.

[0023] Preferably, the mass ratio of the yttrium oxide powder, the titanium oxide powder and the zinc oxide powder is 0.1-2:0.5-2:96-99.4.

[0024] Further, in step 1, the first dispersant is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate and sodium hexadecyl benzene sulfonate; the first dispersant accounts for 2-10% of the total mass of the added yttrium oxide, titanium oxide, pure water and the first dispersant, the solid content in the slurry is between 35-75%, the pre-dispersion time is 10-30 min, the rotation speed of the wet milling is 600-1800 r / min, the wet milling time is 6-18 h, and the particle size D50 of the slurry one is less than 7 μm.

[0025] Further, in step 2, the second dispersant is one or more of polyvinylpyrrolidone, acrylic ester and ethylene bis-stearamide; the second dispersant accounts for 2-10% of the total mass of the added zinc oxide powder, pure water and the second dispersant, the solid content in the slurry is between 35-75%, the pre-dispersion time is 10-30 min, the rotation speed of the wet milling is 600-1800 r / min, the wet milling time is 3-12 h, and the particle size D50 of the slurry two is less than 5 μm.

[0026] Further, in step 3, the binder is one of a mixture of polyvinyl alcohol and polyethylene glycol, polyvinyl alcohol and polyvinyl butyral; the binder accounts for 1-15% of the total mass of the added yttrium oxide, titanium oxide and zinc oxide; the pre-dispersion time is 10-30 min, the rotation speed of the wet milling is 600-1800 r / min, the wet milling time is 2-10 h, and the particle size D50 of the slurry three is less than 3 μm.

[0027] The application further discloses a zinc titanium yttrium oxide powder prepared by the above method.

[0028] Meanwhile, the application discloses a zinc titanium yttrium oxide target material, which is prepared by sequentially fine die pressing, cold isostatic pressing, pre-burning and degreasing and sintering of the above zinc titanium yttrium oxide powder and then cooling.

[0029] The application further discloses a preparation method of the above zinc titanium yttrium oxide target material, which specifically comprises the following steps.

[0030] Step a: sequentially performing die pressing and cold isostatic pressing on the zinc titanium yttrium oxide powder to obtain a target blank;

[0031] Step b: Put the target blank into the debinding furnace for pre-burning debinding to obtain a preform;

[0032] Step c: Put the preform into the sintering furnace for sintering, and obtain the zinc titanium yttrium oxide target after cooling to room temperature;

[0033] In the step a, the pressure for molding is 20-95 Mpa, and the forming time is 60-180 s; the pressure for cold isostatic pressing is 200-500 Mpa, and the forming time is 60-180 s.

[0034] Further, in the step b, the pre-burning debinding temperature is 400-600℃, the holding time is 10-15 h, the heating rate is 0.3-0.6℃ / min, and the cooling rate is 1℃ / min.

[0035] Further, in the step c, the sintering temperature is 1200-1500℃, the heating rate is 0.3-1℃ / min, the holding time is 4-12 h, and the cooling rate is 1℃ / min.

[0036] Beneficial effects

[0037] Compared with the prior art, the present application has at least the following advantages:

[0038] (1) The present application adopts the gas-water combined atomization method, which can not only balance the improvement of the sphericity and the average degree of particle size of the zinc titanium yttrium oxide powder, but also reduce the oxygen content of the zinc titanium yttrium oxide powder, thereby improving the performance of the zinc titanium yttrium oxide target under specific gas pressure, gas injection angle, water pressure and water injection angle;

[0039] (2) The present application finds that the gas-water combined atomization method for breaking the zinc titanium yttrium oxide particles can have a certain influence on the oxygen content of the zinc titanium yttrium oxide particles, and the oxygen content of the zinc titanium yttrium oxide particles can be controlled when the oxide particles are broken under specific gas atomization, water atomization pressure and injection angle, so that the oxygen is uniformly distributed in the zinc titanium yttrium oxide particles, thereby improving the performance of the zinc titanium yttrium oxide target;

[0040] (3) The present application uses zinc titanium yttrium oxide powder with high oxygen content to prepare the zinc titanium yttrium oxide target, and the prepared zinc titanium yttrium oxide target has high target relative density, conductivity and target bending strength. BRIEF DESCRIPTION OF DRAWINGS

[0041] The present application will be further described below in combination with the drawings and examples;

[0042] Figure 1 is the sphericity graph of Example 1 of the present application;

[0043] Figure 2 is the morphology graph of Comparative Example 1 of the present application;

[0044] Figure 3 is a morphology chart of Invention Comparative Example 2;

[0045] Figure 4 is a morphology chart of Invention Comparative Example 3. DETAILED DESCRIPTION

[0046] The application will be further described in conjunction with the examples below, but does not constitute any limitation to the application, any limited number of modifications made within the scope of the claims of the application is still within the scope of the claims of the application.

[0047] In order to illustrate the technical content of the application, the following further illustrates in conjunction with the embodiments.

[0048] It should be noted that, since standing to dry moisture, mixing and screening are conventional technical means for powder preparation in the art, and the specific process will not be described in more detail.

[0049] Example 1

[0050] A zinc oxide titanium yttrium powder is prepared by the following steps:

[0051] Step 1: The yttrium oxide, titanium oxide and zinc oxide with a purity of 4N are weighed according to the mass ratio of 0.1:0.5:99.4 for standby;

[0052] Step 2: The yttrium oxide powder and titanium oxide powder are added to a slurry barrel containing pure water and the first dispersant polyvinylpyrrolidone, mixed together for pre-dispersion for 15 min, then pumped into a sand mill for wet grinding to obtain slurry one, wherein the first dispersant accounts for 2% of the total mass of the added yttrium oxide, titanium oxide, pure water and first dispersant, the solid content in the slurry is 35%, the grinding speed is 1200r / min, the grinding time is 8h, and the particle size D50 of the slurry one is 1.235μm;

[0053] Step 3: The zinc oxide powder, pure water and the second dispersant polyvinylpyrrolidone are added to the slurry one and mixed, pre-dispersed for 30 min, then pumped into a sand mill for wet grinding to obtain slurry two, wherein the second dispersant accounts for 3% of the total mass of the added zinc oxide, pure water and second dispersant, the solid content in the slurry is 53%, the grinding speed is 1200r / min, the grinding time is 12h, and the particle size D50 of the slurry two is 0.948μm;

[0054] Step 4: The binder polyvinyl alcohol and polyethylene glycol are added to the slurry two, mixed, pre-dispersed for 20 min, and then pumped into a sand mill for wet grinding to obtain slurry three, wherein the binder accounts for 5% of the total mass of the added yttrium oxide, titanium oxide and zinc oxide, the grinding speed is 1200 r / min, the grinding time is 8 h, and the particle size D50 of the slurry three is 0.589 μm;

[0055] Step 5: The slurry three is subjected to gas-water combined atomization granulation, and the obtained powder is subjected to standing to remove moisture, then mixed and sieved to obtain the zinc oxide titanium yttrium powder;

[0056] In the gas-water combined atomization granulation of step 5, the gas pressure of gas atomization is 0.6 MPa, the gas is nitrogen, the angle between the gas injection direction and the vertical downward direction is 30°, the water pressure of water atomization is 90 MPa, and the angle between the water injection direction and the vertical downward direction is 40°.

[0057] Example 2

[0058] A zinc oxide titanium yttrium powder is prepared by the following steps:

[0059] Step 1: Yttrium oxide, titanium oxide and zinc oxide with a purity of 4N are weighed according to a mass ratio of 0.1:0.5:99.4 for standby;

[0060] Step 2: The yttrium oxide powder and the titanium oxide powder are added to a slurry barrel containing pure water and a first dispersant polyvinylpyrrolidone, mixed and pre-dispersed for 15 min, then pumped into a sand mill for wet grinding to obtain slurry one, wherein the first dispersant accounts for 2% of the total mass of the added yttrium oxide, titanium oxide, pure water and first dispersant, the solid content in the slurry is 35%, the grinding speed is 1200 r / min, the grinding time is 8 h, and the particle size D50 of the slurry one is 1.235 μm;

[0061] Step 3: The zinc oxide powder, pure water and a second dispersant polyvinylpyrrolidone are added to the slurry one, mixed and pre-dispersed for 30 min, then pumped into a sand mill for wet grinding to obtain slurry two, wherein the second dispersant accounts for 3% of the total mass of the added zinc oxide, pure water and second dispersant, the solid content in the slurry is 53%, the grinding speed is 1200 r / min, the grinding time is 12 h, and the particle size D50 of the slurry two is 0.948 μm;

[0062] Step 4: The binder polyvinyl alcohol and polyethylene glycol are added to the slurry two, mixed, pre-dispersed for 20 min, and then pumped into a sand mill for wet grinding to obtain slurry three, wherein the binder accounts for 5% of the total mass of the added yttrium oxide, titanium oxide and zinc oxide, the grinding speed is 1200 r / min, the grinding time is 8 h, and the particle size D50 of the slurry three is 0.589 μm;

[0063] Step 5: The slurry three is subjected to gas-water combined atomization granulation, and the obtained powder is subjected to standing and dry water removal, followed by mixing and screening to obtain a zinc oxide titanium yttrium powder;

[0064] In the step 5, the gas pressure of the gas atomization of the gas-water combined atomization granulation is 0.8 MPa, the gas is nitrogen, the angle between the gas injection direction and the vertical downward direction is 50°, the water pressure of the water atomization is 90 MPa, and the angle between the water injection direction and the vertical downward direction is 40°.

[0065] Example 3

[0066] A zinc oxide titanium yttrium powder is prepared by the following steps:

[0067] Step 1: Yttrium oxide, titanium oxide and zinc oxide with a purity of 4N are weighed according to a mass ratio of 0.1:0.5:99.4 for standby;

[0068] Step 2: The yttrium oxide powder and the titanium oxide powder are added into a slurry barrel containing pure water and a first dispersant polyvinylpyrrolidone, mixed and pre-dispersed for 15 min, and then pumped into a sand mill for wet grinding to obtain a slurry one, wherein the first dispersant accounts for 2% of the total mass of the added yttrium oxide, titanium oxide, pure water and first dispersant, the solid content in the slurry is 35%, the grinding speed is 1200 r / min, the grinding time is 8 h, and the particle size D50 of the slurry one is 1.235 μm;

[0069] Step 3: The zinc oxide powder, pure water and a second dispersant polyvinylpyrrolidone are added to the slurry one, mixed and pre-dispersed for 30 min, and then pumped into a sand mill for wet grinding to obtain a slurry two, wherein the second dispersant accounts for 3% of the total mass of the added zinc oxide, pure water and second dispersant, the solid content in the slurry is 53%, the grinding speed is 1200 r / min, the grinding time is 12 h, and the particle size D50 of the slurry two is 0.948 μm;

[0070] Step 4: A binder polyvinyl alcohol and polyethylene glycol are added to the slurry two, mixed, pre-dispersed for 20 min, and then pumped into a sand mill for wet grinding to obtain a slurry three, wherein the binder accounts for 5% of the total mass of the added yttrium oxide, titanium oxide and zinc oxide, the grinding speed is 1200 r / min, the grinding time is 8 h, and the particle size D50 of the slurry three is 0.589 μm;

[0071] Step 5: The slurry three is subjected to gas-water combined atomization granulation, and the obtained powder is subjected to standing and dry water removal, followed by mixing and screening to obtain a zinc oxide titanium yttrium powder;

[0072] The gas pressure of the gas atomization in the gas-water combined atomization and granulation in step 5 is 0.6 MPa, the gas is nitrogen, and the angle between the gas injection direction and the vertical downward direction is 30°; the water pressure of the water atomization is 150 MPa, and the angle between the water injection direction and the vertical downward direction is 30°.

[0073] Example 4

[0074] A zinc titanium yttrium oxide powder is prepared by the following steps:

[0075] Step 1: Yttrium oxide, titanium oxide and zinc oxide with a purity of 4N are weighed according to a mass ratio of 0.3:0.8:98.9 for later use;

[0076] Step 2: The yttrium oxide powder and the titanium oxide powder are added into a slurry barrel containing pure water and a first dispersant sodium hexadecyl benzene sulfonate, mixed together for pre-dispersion for 15 min, and then pumped into a sand mill for wet grinding to obtain slurry one, wherein the first dispersant accounts for 2% of the total mass of the added yttrium oxide, titanium oxide, pure water and first dispersant, the solid content in the slurry is 45%, the grinding speed is 1200 r / min, the grinding time is 8 h, and the particle size D50 of the slurry one is 1.197 μm;

[0077] Step 3: The zinc oxide powder, pure water and a second dispersant acrylate are added into the slurry one, mixed, pre-dispersed for 30 min, and then pumped into a sand mill for wet grinding to obtain slurry two, wherein the second dispersant accounts for 3% of the total mass of the added zinc oxide, pure water and second dispersant, the solid content in the slurry is 53%, the grinding speed is 1200 r / min, the grinding time is 12 h, and the particle size D50 of the slurry two is 0.768 μm;

[0078] Step 4: A binder polyvinyl butyral is added into the slurry two, mixed, pre-dispersed for 20 min, and then pumped into a sand mill for wet grinding to obtain slurry three, wherein the binder accounts for 5% of the total mass of the added yttrium oxide, titanium oxide and zinc oxide, the grinding speed is 1200 r / min, the grinding time is 8 h, and the particle size D50 of the slurry three is 0.529 μm;

[0079] Step 5: The slurry three is subjected to gas-water combined atomization and granulation, the obtained powder is subjected to standing and dry water removal, and then mixed and screened to obtain a zinc titanium yttrium oxide powder.

[0080] The gas pressure of the gas atomization in the gas-water combined atomization and granulation in step 5 is 0.7 MPa, the gas is nitrogen, and the angle between the gas injection direction and the vertical downward direction is 40°; the water pressure of the water atomization is 50 MPa, and the angle between the water injection direction and the vertical downward direction is 50°.

[0081] Example 5

[0082] A kind of zinc oxide titanium yttrium powder, is prepared using the following steps:

[0083] Step 1: the purity of 4N yttrium oxide, titanium oxide and zinc oxide are weighed according to the mass ratio of 1.9:1.8:96.7 for standby;

[0084] Step 2: the yttrium oxide powder, titanium oxide powder is added into the slurry barrel containing pure water and the first dispersant polyvinylpyrrolidone, mixed together for pre-dispersion 15 min, then pumped into sand mill for wet grinding to obtain slurry one, wherein the first dispersant accounts for 2% of the total mass of yttrium oxide, titanium oxide, pure water and the first dispersant added, the solid content in the slurry is 35%, the grinding speed is 1200r / min, the grinding time is 8h, and the particle size D50 of slurry one is 1.163 μm;

[0085] Step 3: zinc oxide powder, pure water and second dispersant polyvinylpyrrolidone are added to slurry one, mixed, pre-dispersed for 30 min, then pumped into sand mill for wet grinding to obtain slurry two, wherein the second dispersant accounts for 3% of the total mass of zinc oxide, pure water and the second dispersant added, the solid content in the slurry is 53%, the grinding speed is 1200r / min, the grinding time is 12h, and the particle size D50 of slurry two is 0.894 μm;

[0086] Step 4: the binder polyvinyl alcohol and polyethylene glycol are added to slurry two, mixed, pre-dispersed for 20 min, then pumped into sand mill for wet grinding to obtain slurry three, wherein the binder accounts for 5% of the total mass of yttrium oxide, titanium oxide and zinc oxide added, the grinding speed is 1200r / min, the grinding time is 8h, and the particle size D50 of slurry three is 0.483 μm;

[0087] Step 5: the slurry three is subjected to air-water combined atomization granulation, and the obtained powder is subjected to static drying to remove water, then mixed and screened to obtain zinc oxide titanium yttrium powder;

[0088] In step 5, the air pressure of air atomization in air-water combined atomization granulation is 0.6 MPa, the gas is nitrogen, and the angle between the gas injection direction and the vertical downward direction is 30°;The water pressure of water atomization is 90 MPa, and the angle between the water injection direction and the vertical downward direction is 40°.

[0089] Comparative Example 1

[0090] Generally the same as Example 1, except that in step 5, air-water combined atomization granulation is replaced by water atomization, no gas is introduced into the air-water combined atomization device, the water pressure of water atomization is 90 MPa, and the angle between the water injection direction and the vertical downward direction is 40°.

[0091] Comparative Example 2

[0092] The same as Example 1 except that in the step 5, the gas-water combined atomization granulation was replaced by gas atomization granulation, no liquid was introduced into the gas-water combined atomization device, the gas pressure was 0.6 MPa, the gas was nitrogen, and the angle between the gas jet direction and the vertical downward direction was 30°.

[0093] Comparative Example 3

[0094] The same as Example 1 except that in the step 5, the gas pressure of the gas atomization of the gas-water combined atomization granulation was 0.5 MPa, the gas was nitrogen, and the angle between the gas jet direction and the vertical downward direction was 30°; the water pressure of the water atomization was 90 MPa, and the angle between the water jet direction and the vertical downward direction was 40°.

[0095] Comparative Example 4

[0096] The same as Example 1 except that in the step 5, the gas pressure of the gas atomization of the gas-water combined atomization granulation was 0.6 MPa, the gas was nitrogen, and the angle between the gas jet direction and the vertical downward direction was 75°; the water pressure of the water atomization was 90 MPa, and the angle between the water jet direction and the vertical downward direction was 40°.

[0097] Comparative Example 5

[0098] The same as Example 1 except that in the step 5, the gas pressure of the gas atomization of the gas-water combined atomization granulation was 0.6 MPa, the gas was nitrogen, and the angle between the gas jet direction and the vertical downward direction was 15°; the water pressure of the water atomization was 90 MPa, and the angle between the water jet direction and the vertical downward direction was 40°.

[0099] Comparative Example 6

[0100] The same as Example 1 except that in the step 5, the gas pressure of the gas atomization of the gas-water combined atomization granulation was 1 MPa, the gas was nitrogen, and the angle between the gas jet direction and the vertical downward direction was 30°; the water pressure of the water atomization was 90 MPa, and the angle between the water jet direction and the vertical downward direction was 40°.

[0101] Comparative Example 7

[0102] The same as Example 1 except that in the step 5, the gas pressure of the gas atomization of the gas-water combined atomization granulation was 0.6 MPa, the gas was nitrogen, and the angle between the gas jet direction and the vertical downward direction was 30°; the water pressure of the water atomization was 40 MPa, and the angle between the water jet direction and the vertical downward direction was 40°.

[0103] Comparative Example 8

[0104] The same as example 1, except that the gas pressure of the gas atomization of the gas-water combined atomization granulation is 0.6 MPa, the gas is nitrogen, and the angle between the gas injection direction and the vertical downward direction is 30°; the water pressure of the water atomization is 90 MPa, and the angle between the water injection direction and the vertical downward direction is 77.5°.

[0105] Comparative example 9

[0106] The same as example 1, except that the gas pressure of the gas atomization of the gas-water combined atomization granulation is 0.6 MPa, the gas is nitrogen, and the angle between the gas injection direction and the vertical downward direction is 30°; the water pressure of the water atomization is 90 MPa, and the angle between the water injection direction and the vertical downward direction is 77.5°.

[0107] Comparative example 10

[0108] The same as example 1, except that the gas pressure of the gas atomization of the gas-water combined atomization granulation is 0.6 MPa, the gas is nitrogen, and the angle between the gas injection direction and the vertical downward direction is 30°; the water pressure of the water atomization is 90 MPa, and the angle between the water injection direction and the vertical downward direction is 77.5°.

[0109] Performance test

[0110] The morphology of the zinc titanium yttrium oxide powder obtained in examples 1-5 and comparative examples 1-10 was measured and observed by a specific surface area pore size analyzer, a scanning electron microscope, and an oxygen-nitrogen analyzer, to obtain the average particle size and oxygen content percentage of the zinc titanium yttrium oxide powder, and the results are shown in table 1.

[0111] Table 1: Performance test results of the zinc titanium yttrium oxide powder obtained in examples 1-5 and comparative examples 1-10

[0112]

[0113]

[0114] According to the results in table 1, it can be seen that:

[0115] According to the comparison of the data of example 1 and comparative examples 1 and 2, it can be seen that the zinc titanium yttrium oxide powder is granulated by the gas-water combined atomization method, which can significantly reduce the average particle size and oxygen content of the zinc titanium yttrium oxide powder, so that the oxygen is uniformly distributed in the zinc titanium yttrium oxide particles, thereby improving the performance of the zinc titanium yttrium oxide target material.

[0116] According to the data comparison of the embodiment 1 and the comparative examples 3, 4 and 5, it can be seen that the gas pressure and the gas injection direction angle in the gas-water combined atomization have great influence on the average particle size and the oxygen content of the zinc oxide titanium yttrium powder; when the gas pressure is less than 0.6 MPa or the gas injection direction angle is not in the range of the application, the average particle size of the powder is larger and the oxygen content is higher.

[0117] The data of the comparative examples 6 and 8 prove that too large gas pressure or too large liquid pressure will not have great influence on the performance of the zinc oxide titanium yttrium powder, but the production cost will be increased.

[0118] According to the data comparison of the embodiment 1 and the comparative examples 6, 7 and 9, it can be seen that the water pressure and the water injection direction angle in the gas-water combined atomization have great influence on the average particle size and the oxygen content of the zinc oxide titanium yttrium powder; when the water pressure is less than 100 MPa or the water injection direction angle is not in the range of the application, the average particle size of the powder is larger and the oxygen content is higher.

[0119] The sphericity of the zinc oxide titanium yttrium powder particles of the embodiment 1 and the comparative examples 1-3 is observed by a scanning electron microscope, and the results can be seen from the following Figures 1-4 , which shows that the gas-water combined atomization with specific pressure and specific injection angle can effectively improve the sphericity of the zinc oxide titanium yttrium powder particles, and can also effectively control the oxygen content of the zinc oxide titanium yttrium powder, so as to avoid the performance of the zinc oxide titanium yttrium target material produced by the zinc oxide titanium yttrium powder with too much oxygen from being reduced.

[0120] Preparation and performance test of zinc oxide titanium yttrium target material

[0121] The zinc oxide titanium yttrium powder prepared in the embodiment 1-5 and the comparative examples 1-10 is used to prepare a zinc oxide titanium yttrium target material according to the following steps to obtain the application examples 1-5 and the application comparative examples 1-10.

[0122] Step a: the zinc oxide titanium yttrium powder is sequentially subjected to die pressing and cold isostatic pressing to obtain a target blank;

[0123] Step b: the target blank is placed into a debinding furnace to be pre-burned and debound to obtain a preform;

[0124] Step c: the preform is placed into a sintering furnace to be sintered to obtain a zinc oxide titanium yttrium target material;

[0125] In the step a, the pressure of the die pressing is 90T and the forming time is 120s; the pressure of the cold isostatic pressing is 360Mpa and the forming time is 120s.

[0126] Further, in the step b, the heating rate is 0.3℃ / min to heat to 500℃ and keep for 10h, and then the cooling rate is 1℃ / min to decrease to room temperature.

[0127] Further, the step c is heated to 1400 DEG C at a heating rate of 1 DEG C / min for 12 h, and then cooled to room temperature at a cooling rate of 1 DEG C / min to obtain the zinc titanium yttrium oxide target.

[0128] Performance test

[0129] The relative density of the target is measured by Archimedes drainage method;

[0130] The conductivity of the target is measured by four-probe test technology;

[0131] The average grain size of the target is measured by using an X-ray diffractometer;

[0132] The bending strength of the target is measured by a universal testing machine;

[0133] The zinc titanium yttrium oxide targets prepared in application examples 1-5 and application comparative examples 1-10 are tested according to the above test methods, and the results are shown in Table 2.

[0134] Table 2 Performance test results of the zinc titanium yttrium oxide targets prepared in application examples 1-5 and application comparative examples 1-10

[0135]

[0136]

[0137] According to the results in Table 2, it can be seen that:

[0138] The gas-water combined atomization technology adopted in the application, the pressure and the spray angle of gas atomization, and the pressure and the spray angle of water atomization are more critical to the performance of the indium gallium aluminum oxide target, because the indium gallium aluminum oxide powder prepared by the gas-water combined atomization has the advantages of small average particle size and low oxygen content.

[0139] The indium gallium aluminum oxide target prepared by the application has the advantages of high density, high conductivity, excellent average grain size and bending strength performance.

[0140] The examples presented herein are merely selected embodiments according to a combination of all possible embodiments. The appended claims should not be limited by the embodiments described herein. Some numerical ranges used in the claims include sub-ranges within them, and variations in these ranges should also be covered by the appended claims.

Claims

1. A method for preparing zinc titanium yttrium oxide powder, characterized in that: The specific steps include: Step 1: Yttrium oxide powder, titanium oxide powder, pure water and a first dispersant are mixed, pre-dispersed and then wet-grinded to obtain slurry 1; Step 2: Add zinc oxide powder, pure water and a second dispersant to slurry 1, mix and pre-disperse, and then wet grind to obtain slurry 2; Step 3: Add a binder to the slurry 2, mix, pre-disperse, and then wet grind to obtain slurry 3; Step 4: subjecting the slurry 3 to air-water combined atomization granulation, mixing and screening in sequence to obtain zinc oxide titanium yttrium powder; The gas pressure of the gas atomization in the gas-water combined atomization granulation in step 4 is 0.6-0.8 MPa, and the angle between the gas injection direction and the vertical downward direction is 30-50°; the water pressure of the water atomization is 50-150 MPa, and the angle between the water injection direction and the vertical downward direction is 30-50°; The mass ratio of the yttrium oxide powder, the titanium oxide powder and the zinc oxide powder is 0.1-2:0.5-2:96-99.

4.

2. The method for preparing zinc oxide titanium yttrium powder according to claim 1, wherein In step 1, the first dispersant is one of polyvinyl pyrrolidone, sodium dodecylbenzenesulfonate, and sodium hexadecylbenzenesulfonate; the first dispersant accounts for 2-10% of the total mass of the added yttrium oxide, titanium oxide, pure water, and the first dispersant, and the solid content in the slurry is between 35-75%; the pre-dispersion time is 10-30 minutes, the wet grinding speed is 600-1800 r / min, the wet grinding time is 6-18 hours, and the particle size D50 of the slurry is less than 7 μm.

3. The method for preparing zinc oxide titanium yttrium powder according to claim 1, wherein In step 2, the second dispersant is one or more of polyvinyl pyrrolidone, acrylate, and ethylene bisstearamide; the second dispersant accounts for 2-10% of the total mass of the added zinc oxide powder, pure water, and the second dispersant, and the solid content in the slurry is between 35-75%; the pre-dispersion time is 10-30 minutes; the wet grinding speed is 600-1800 r / min, the wet grinding time is 3-12 hours, and the particle size D50 of the second slurry is less than 5 μm.

4. The method for preparing zinc oxide titanium yttrium powder according to claim 1, wherein In step 3, the binder is a mixture of polyvinyl alcohol and polyethylene glycol, polyvinyl alcohol, and polyvinyl butyral; the binder accounts for 1-15% of the total mass of the added yttrium oxide, titanium oxide, and zinc oxide; the pre-dispersion time is 10-30 minutes; the wet grinding speed is 600-1800 r / min, the wet grinding time is 2-10 hours, and the particle size D50 of slurry three is less than 3 μm.

5. A zinc oxide titanium yttrium powder, characterized in that: The zinc oxide titanium yttrium powder is prepared by the preparation method of any one of claims 1 to 4.

6. A zinc oxide titanium yttrium target, characterized in that: The zinc oxide titanium yttrium powder according to claim 5 is finely molded, cold isostatically pressed, pre-sintered and degreased, and then sintered and cooled to obtain the zinc oxide titanium yttrium target.

7. A method for preparing a zinc oxide titanium yttrium target according to claim 6, characterized in that: The specific steps include: Step a: subjecting titanium oxide yttrium powder to molding and cold isostatic pressing in sequence to obtain a target blank; Step b: placing the target material blank into a degreasing furnace for pre-sintering and degreasing to obtain a preform; Step c: placing the preform into a sintering furnace and sintering it until the temperature drops to room temperature to obtain the zinc oxide titanium yttrium target; Wherein, the molding pressure in step a is 20-95 MPa, and the molding time is 60-180 s; the cold isostatic pressing pressure is 200-500 MPa, and the molding time is 60-180 s.

8. The method for preparing the zinc oxide titanium yttrium target according to claim 7, characterized in that: The temperature of the pre-calcination and degreasing in step b is 400-600° C., the holding time is 10-15 hours, the heating rate is 0.3-0.6° C. / min, and the cooling rate is 1° C. / min.

9. The method for preparing the zinc oxide titanium yttrium target according to claim 7, characterized in that: In the step c, the sintering temperature is 1200-1500° C., the heating rate is 0.3-1° C. / min, the holding time is 4-12 hours, and the cooling rate is 1° C. / min.

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