W-y2o3-zno target material and method for manufacturing the same

Abstract

The application belongs to the technical field of target material production, and discloses a preparation method of W-Y2O3-ZnO target material, which comprises the following steps: firstly, tungsten powder, yttrium oxide powder and zinc oxide powder are mixed according to a mass ratio of 55-65:20-35:5-15 to prepare a powder; then, the powder is put into a vacuum hot pressing furnace and heated to 1000-1500 DEG C at a heating rate of 5-10 DEG C / min, and kept for 30-120 min; then, the environmental pressure is increased to 20-40 MPa at a rate of 2-5 MPa / min, and kept for 20-60 min; then, the temperature is decreased to room temperature, the pressure is reduced to standard atmospheric pressure, and the W-Y2O3-ZnO target material is obtained through machining; the particle size of the tungsten powder in step 1 is 2-30 μm, the particle size of the yttrium oxide powder is 10-20 μm, and the particle size of the zinc oxide powder is 10-20 μm; the W-Y2O3-ZnO target material prepared by the above method has high density; in addition, the application also discloses a W-Y2O3-ZnO target material.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of target materials, in particular to a W-Y2O3-ZnO target material and a preparation method thereof. BACKGROUND

[0002] Indium is a semiconductor rare metal, and its reserves in nature are relatively small. With the development of the electronic industry, the demand for indium is increasing, so the recycling of indium is becoming more and more important. ITO target material is the main consumer of indium, and has accounted for more than 75% of the total consumption of indium. However, the utilization rate of ITO target material sputtering film is generally about 60%, and the rest is waste target, so the recycling of ITO waste target material is particularly important, which not only realizes the recycling of resources, but also has huge economic benefits.

[0003] Chinese patent application 201310412822.6 discloses a high-density zinc oxide-based target material and a preparation method thereof, which comprises the following steps in sequence:

[0004] Mixing step: a binder and water are added to the raw materials, mixed uniformly to obtain a uniform slurry, and then the slurry is dried and powdered to obtain dry powder particles with uniform particle size distribution;

[0005] Binder removal and degassing step: the dry powder particles are loaded into a corresponding size package, and binder removal and degassing treatment is performed;

[0006] Hot isostatic pressing step: after the package is sealed and welded after the binder removal and degassing, hot isostatic pressing treatment is performed;

[0007] Annealing step: the ingot after removing the package is subjected to annealing treatment;

[0008] The zinc oxide-based target material prepared by the above method has high density, the relative density can reach more than 99% of the theoretical density; the density is uniform, the density of each part is almost the same; the size of the prepared target material is large, which can reach 500mmx500mmx50mm; there are no pores and loose, the grain size is small, and the average grain size is not greater than 30μm;

[0009] As can be seen from the specification of the scheme, the raw material also includes a doping source, the doping source is at least one of indium oxide powder, gallium oxide powder, lithium oxide powder, manganese powder, yttrium oxide powder, zirconium oxide powder, tungsten powder, silver powder, copper powder, tin oxide powder, bismuth powder, cobalt powder, nickel powder, titanium powder, molybdenum powder, chromium powder, vanadium oxide powder, boron powder and aluminum oxide powder, and the mass ratio of the total mass of the zinc source and the oxygen source to the mass of the doping source is 5:1 to 500:1.

[0010] Further observation of the embodiments of this scheme shows that embodiments 1-6 of this scheme respectively describe the preparation of pure zinc oxide target material, the preparation of indium gallium doped zinc oxide target material, the preparation of boron doped zinc oxide target material, the preparation of aluminum doped zinc oxide target material, the preparation of yttrium doped zinc oxide target material, and the preparation of cobalt doped zinc oxide target material. At least from the embodiments of this scheme, it can be seen that this scheme does not record the improvement effect of tungsten and yttrium co-doped on zinc oxide-based target material.

[0011] Chinese patent application 202011549209.5 discloses a magnesium-doped zinc oxide magnetron sputtering target material and a preparation method thereof, which comprises the following steps: (1) doping magnesium oxide powder and third oxide powder into zinc oxide powder, mixing with ethanol solution to form a slurry;

[0012] (2) drying, sieving and obtaining the powder for forming after ball milling the slurry;

[0013] (3) cold isostatic pressing the powder to form a green body;

[0014] (4) slowly heating the green body to 900-1150℃, keeping the temperature for 30-90min, then quickly heating to the sintering temperature of 1300-1450℃, keeping the temperature for 120-480min, and slowly cooling to form a semi-finished product; cutting and polishing to obtain the magnesium-doped zinc oxide magnetron sputtering target material.

[0015] The magnesium-doped zinc oxide magnetron sputtering target material prepared by the above scheme has high density, with a relative density of more than 95%, and a low resistivity of 4x10-2, which is much lower than the resistivity of the target material in the prior art, has good conductivity, and can meet the needs of film production line medium frequency rapid sputtering, further improving production efficiency and reducing cost.

[0016] Further observation of the above scheme shows that in step 1, the above scheme states that magnesium oxide powder and third oxide powder can be doped into zinc oxide powder, and states that the third oxide powder includes any one or more of titanium oxide, aluminum oxide, gallium oxide, indium oxide, cerium oxide, yttrium oxide, tin oxide, tungsten oxide, and molybdenum oxide;

[0017] However, actual observation of the embodiments of this scheme shows that although embodiments 1-3 of this scheme all add third oxide powder to the zinc oxide powder for doping, embodiments 1-3 do not record the specific third oxide powder that is doped.

[0018] And the target materials prepared by the above two schemes are both based on zinc oxide as the matrix and doping other oxides into the zinc oxide matrix, while the tungsten content in the target material prepared by the present application is significantly higher than that of other oxides, therefore, the target material prepared by the present application is based on tungsten as the matrix.

[0019] The problem to be solved by the present application is to provide a preparation method capable of preparing a high-density W-Y2O3-ZnO target material. SUMMARY

[0020] The present application aims to provide a preparation method capable of preparing a high-density W-Y2O3-ZnO target material.

[0021] To achieve the above-mentioned purpose, the present application discloses a preparation method of a W-Y2O3-ZnO target material, comprising the following steps:

[0022] Step 1: tungsten powder, yttrium oxide powder and zinc oxide powder are mixed in a mass ratio of 55-65:20-35:5-15 to obtain a powder;

[0023] Step 2: the powder obtained in step 1 is put into a vacuum hot pressing furnace and heated to 1000-1500℃ at a heating rate of 5-10℃ / min for 30-120min, then the ambient pressure is increased to 20-40MPa at a rate of 2-5MPa / min and kept for 20-60min, then reduced to room temperature and reduced to standard atmospheric pressure, and then machined to obtain a W-Y2O3-ZnO target material;

[0024] In step 1, the particle size of the tungsten powder is 2-30μm, the particle size of the yttrium oxide powder is 10-20μm, and the particle size of the zinc oxide powder is 10-20μm.

[0025] Preferably, the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder in step 1 is 58-62:28-32:10.

[0026] Preferably, when the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder is 55-58:32-35:10-15, the particle size of the tungsten powder is 15-30μm, the particle size of the yttrium oxide powder is 10-15μm, and the particle size of the zinc oxide powder is 10-15μm.

[0027] When the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder is 62-65:20-28:5-10, the particle size of the tungsten powder is 2-10μm, the particle size of the yttrium oxide powder is 10-20μm, and the particle size of the zinc oxide powder is 10-20μm.

[0028] Preferably, when the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder is 55-58:32-35:10-15, the pressure of the vacuum hot pressing furnace in step 2 is 30-40MPa.

[0029] When the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder is 62-65:20-28:5-10, the pressure of the vacuum hot pressing furnace in step 2 is 20-30MPa.

[0030] In addition, the application further discloses a preparation method of the W-Y2O3-ZnO target material, and the W-Y2O3-ZnO target material is prepared by the preparation method.

[0031] The application has the beneficial effects that the tungsten powder, the yttrium oxide powder and the zinc oxide powder are mixed to prepare the W-Y2O3-ZnO target material with high density, and it is surprisingly found that when the tungsten powder, the yttrium oxide powder and the zinc oxide powder have a specific mass ratio, the relative density of the target material can be effectively improved by adjusting the particle sizes of the tungsten powder, the yttrium oxide powder and the zinc oxide powder. DETAILED DESCRIPTION

[0032] The application will be clearly and completely described below by combining the embodiments of the application, and it should be noted that the specific conditions are not indicated in the embodiments in the description of the application, and the conventional conditions or the conditions recommended by the manufacturers are used. The reagents or instruments used are not indicated by the manufacturers, and are conventional products that can be purchased in the market.

[0033] Embodiment 1

[0034] Step 1: the tungsten powder, the yttrium oxide powder and the zinc oxide powder are mixed according to a mass ratio of 55:35:15 to prepare a powder;

[0035] Step 2: the powder prepared in step 1 is put into a vacuum hot pressing furnace, and heated to 1000 DEG C at a heating rate of 5 DEG C / min for 30 min, then the environmental pressure is increased to 20 MPa at a rate of 2 MPa / min and kept for 20 min, then decreased to room temperature and reduced to standard atmospheric pressure, and then machined to obtain the W-Y2O3-ZnO target material;

[0036] In step 1, the particle size of the tungsten powder is 10 μm, the particle size of the yttrium oxide powder is 20 μm, and the particle size of the zinc oxide powder is 20 μm.

[0037] Embodiment 2

[0038] Step 1: the tungsten powder, the yttrium oxide powder and the zinc oxide powder are mixed according to a mass ratio of 65:20:5 to prepare a powder;

[0039] Step 2: the powder prepared in step 1 is put into a vacuum hot pressing furnace, and heated to 1500 DEG C at a heating rate of 10 DEG C / min for 120 min, then the environmental pressure is increased to 20 MPa at a rate of 5 MPa / min and kept for 60 min, then decreased to room temperature and reduced to standard atmospheric pressure, and then machined to obtain the W-Y2O3-ZnO target material;

[0040] The particle size of the tungsten powder in step 1 is 15 μm, the particle size of the yttria powder is 15 μm, and the particle size of the zinc oxide powder is 15 μm.

[0041] Example 3

[0042] Step 1: tungsten powder, yttria powder, and zinc oxide powder are mixed in a mass ratio of 60:30:10 to prepare a powder;

[0043] Step 2: the powder prepared in step 1 is put into a vacuum hot pressing furnace and heated to 1250°C at a heating rate of 8°C / min for 60 min, then the ambient pressure is increased to 20 MPa at a rate of 3 MPa / min and held for 40 min, then decreased to room temperature and reduced to standard atmospheric pressure, and machined to obtain a W-Y2O3-ZnO target material;

[0044] The particle size of the tungsten powder in step 1 is 15 μm, the particle size of the yttria powder is 15 μm, and the particle size of the zinc oxide powder is 15 μm.

[0045] Example 4

[0046] Step 1: tungsten powder, yttria powder, and zinc oxide powder are mixed in a mass ratio of 55:35:15 to prepare a powder;

[0047] Step 2: the powder prepared in step 1 is put into a vacuum hot pressing furnace and heated to 1000°C at a heating rate of 5°C / min for 30 min, then the ambient pressure is increased to 20 MPa at a rate of 2 MPa / min and held for 20 min, then decreased to room temperature and reduced to standard atmospheric pressure, and machined to obtain a W-Y2O3-ZnO target material;

[0048] The particle size of the tungsten powder in step 1 is 30 μm, the particle size of the yttria powder is 10 μm, and the particle size of the zinc oxide powder is 10 μm.

[0049] Example 5

[0050] Step 1: tungsten powder, yttria powder, and zinc oxide powder are mixed in a mass ratio of 65:20:5 to prepare a powder;

[0051] Step 2: the powder prepared in step 1 is put into a vacuum hot pressing furnace and heated to 1000°C at a heating rate of 5°C / min for 30 min, then the ambient pressure is increased to 20 MPa at a rate of 2 MPa / min and held for 20 min, then decreased to room temperature and reduced to standard atmospheric pressure, and machined to obtain a W-Y2O3-ZnO target material;

[0052] The particle size of the tungsten powder in step 1 is 2 μm, the particle size of the yttria powder is 15 μm, and the particle size of the zinc oxide powder is 15 μm.

[0053] Example 6

[0054] The same as example 4, except that step 2 is specifically as follows: the powder prepared in step 1 is put into a vacuum hot pressing furnace and heated to 1000℃ at a heating rate of 5℃ / min for 30min, then the ambient pressure is increased to 40MPa at a rate of 2MPa / min and kept for 20min, then decreased to room temperature and reduced to standard atmospheric pressure, and then machined to obtain a W-Y2O3-ZnO target;

[0055] The particle size of the tungsten powder in step 1 is 30μm, the particle size of the yttria powder is 10μm, and the particle size of the zinc oxide powder is 10μm.

[0056] Example 7

[0057] The same as example 5, except that step 2 is specifically as follows: the powder prepared in step 1 is put into a vacuum hot pressing furnace and heated to 1000℃ at a heating rate of 5℃ / min for 30min, then the ambient pressure is increased to 40MPa at a rate of 2MPa / min and kept for 20min, then decreased to room temperature and reduced to standard atmospheric pressure, and then machined to obtain a W-Y2O3-ZnO target;

[0058] The particle size of the tungsten powder in step 1 is 2μm, the particle size of the yttria powder is 15μm, and the particle size of the zinc oxide powder is 15μm.

[0059] Comparative Example 1

[0060] The same as example 1, except that the mass ratio of the tungsten powder, yttria powder, and zinc oxide powder is 15:35:55.

[0061] Comparative Example 2

[0062] The same as example 1, except that the mass ratio of the tungsten powder, yttria powder, and zinc oxide powder is 50:15:40.

[0063] Comparative Example 3

[0064] The same as example 1, except that the mass ratio of the tungsten powder, yttria powder, and zinc oxide powder is 70:33:2.

[0065] Comparative Example 4

[0066] The same as example 1, except that the same mass of magnesium oxide powder is used instead of yttria powder.

[0067] Comparative Example 5

[0068] The same as example 1, except that step 2 is specifically as follows: the powder prepared in step 1 is put into a vacuum hot pressing furnace and heated to 1000℃ at a heating rate of 5℃ / min for 30min, then the ambient pressure is increased to 50MPa at a rate of 2MPa / min and kept for 20min, then decreased to room temperature and reduced to standard atmospheric pressure, machined, to obtain the target material.

[0069] Comparative example 6

[0070] The same as example 1, except that step 2 is specifically as follows: the powder prepared in step 1 is put into a vacuum hot pressing furnace and heated to 1000℃ at a heating rate of 5℃ / min for 30min, then the ambient pressure is increased to 10MPa at a rate of 2MPa / min and kept for 20min, then decreased to room temperature and reduced to standard atmospheric pressure, machined, to obtain the target material.

[0071] Performance test:

[0072] The relative density of the target materials prepared in examples 1-7 and comparative examples 1-6 is tested by the Archimedes drainage method, and the results are as follows:

[0073]

[0074]

[0075] Result analysis:

[0076] 1. It can be seen from examples 1-3 that under the same particle size and pressure, example 3 has a better relative density than examples 1 and 2.

[0077] 2. It can be seen from examples 1, 4 and 6 that under the same mass ratio, the relative density of the target material is improved to a certain extent after the particle size of the tungsten powder, yttrium oxide powder and zinc oxide powder is optimized in example 4.

[0078] And the relative density of the target material is further improved after the pressure in step 2 of example 6 is further optimized.

[0079] 3. It can be seen from examples 2, 5 and 7 that under the same mass ratio, the relative density of the target material is improved to a certain extent after the particle size of the tungsten powder, yttrium oxide powder and zinc oxide powder is optimized in example 7.

[0080] And the relative density of the target material is further improved after the pressure in step 2 of example 5 is further optimized.

[0081] 4. As can be seen from Example 1 and Comparative Example 1, the present application cannot effectively improve the relative density of the target during the production of the zinc tungstate yttrium oxide target with zinc as the main element;

[0082] Meanwhile, as can be seen from Comparative Example 4, after the doping element is replaced, the preparation method described in the present application also cannot effectively improve the relative density of the target.

[0083] 5. In the production process of Comparative Example 5, although the pressure in the hot pressing process of step 2 is greatly increased, the relative density of the target is improved to a certain extent compared with Example 1, but the target cracks, so too large hot pressing pressure can improve the relative density of the target to a certain extent, but may cause the target to crack.

[0084] The above examples are the preferred embodiments of the present application, but the embodiments of the present application are not limited by the above examples, and any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present application should be equivalent replacement methods, and are included in the protection scope of the present application.

Claims

1. A method for producing a W-Y2O3-ZnO target material, characterized by, The method comprises the following steps: Step 1: mixing tungsten powder, yttrium oxide powder and zinc oxide powder according to a mass ratio of 55-65:20-35:5-15 to obtain a powder; Step 2: putting the powder obtained in step 1 into a vacuum hot pressing furnace, heating at a heating rate of 5-10 ℃ / min to 1000-1500 ℃, maintaining for 30-120 min, then increasing the ambient pressure to 20-40 MPa at a rate of 2-5 MPa / min and maintaining for 20-60 min, then decreasing to room temperature and reducing the pressure to standard atmospheric pressure, machining to obtain a W-Y2O3-ZnO target material; In step 1, the particle size of the tungsten powder is 2-30 μm, the particle size of the yttrium oxide powder is 10-20 μm, and the particle size of the zinc oxide powder is 10-20 μm.

2. The method of producing a W-Y2O3-ZnO target according to claim 1, characterized by, In step 1, the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder is 58-62:28-32:

10.

3. The method for preparing the W-Y₂O₃-ZnO target material according to claim 1, characterized in that, When the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder is 55-58:32-35:10-15, the particle size of the tungsten powder is 15-30 μm, the particle size of the yttrium oxide powder is 10-15 μm, and the particle size of the zinc oxide powder is 10-15 μm; When the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder is 62-65:20-28:5-10, the particle size of the tungsten powder is 2-10 μm, the particle size of the yttrium oxide powder is 10-20 μm, and the particle size of the zinc oxide powder is 10-20 μm.

4. The method for preparing the W-Y₂O₃-ZnO target material according to claim 1, characterized in that, When the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder is 55-58:32-35:10-15, the pressure of the vacuum hot pressing furnace in step 2 is 30-40 MPa; When the mass ratio of the tungsten powder, the yttrium oxide powder and the zinc oxide powder is 62-65:20-28:5-10, the pressure of the vacuum hot pressing furnace in step 2 is 20-30 MPa.

5. A W-Y2O3-ZnO target material, characterized by, The W-Y2O3-ZnO target material prepared by the method of any one of claims 1-4 has a relative density greater than or equal to 95%.

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