ATO target material and preparation method thereof

Abstract

The invention belongs to the technical field of ATO target material preparation, and discloses an ATO target material and a preparation method thereof.The ATO target material is obtained by mixing and sintering 90-95.5 wt% of SnO2 powder, 3-8.5 wt% of Sb2O3 powder and 1.5-2 wt% of ZnO powder; wherein the particle size D50 of the SnO2 powder is 0.5-2 [mu] m, the particle size D50 of the Sb2O3 powder is 3-15 [mu] m, and the particle size D50 of the ZnO powder is 3-15 [mu] m. Through particle size matching of the SnO2 powder, the Sb2O3 powder and the ZnO powder, the target material sintering promoting effect of ZnO is fully exerted, and the relative density of the target material is effectively improved.

Description

Technical Field

[0001] The invention relates to the technical field of ATO target material preparation, and in particular to an ATO target material and a preparation method thereof. Background Art

[0002] Tin dioxide is a broadband metal oxide semiconductor material with a direct band gap and stable physical and chemical properties. Its film has good optical and electrical properties as well as good flame retardancy and thermal stability. It is a low-cost oxide semiconductor film material.

[0003] In applications, the performance of tin dioxide is usually further improved by doping with different elements. Common doping elements include F, In, Sb, Te, etc. These doped tin dioxides are collectively called transparent conductive oxides. Common ones include FTO (fluorine-doped tin dioxide), ITO (indium-doped tin dioxide) and ATO (antimony-doped tin dioxide). ITO is expensive because indium is a rare metal, and the preparation process of FTO is relatively complicated. Therefore, ATO has been widely studied in recent years and has broad application prospects.

[0004] Prior art 1: Chinese patent application 202310941084.8 discloses a high-density zinc oxide-doped indium-free target material and a preparation method thereof. The preparation method of a high-density zinc oxide-doped indium-free target material provided by the present invention comprises the following steps: (1) raw material selection, (2) slurry ball milling, (3) slurry sand milling, (4) powder granulation, (5) primary molding, (6) secondary molding, and (7) pressure sintering.

[0005] Prior art 1 adopts a composite doping method and pressure sintering, firstly mixing zinc oxide, antimony oxide and tin oxide, and then subjecting them to ball milling, sand milling, granulation and finally pressure sintering; this method further improves the density of the prepared target material; although the specification of prior art 1 records that the relative density of the target material obtained is not less than 99.5%, the target materials obtained in its embodiments are all lower than 99.5%, indicating that although it adopts a specific preparation method to effectively improve the density of the target material, there is still room for improvement. Summary of the invention

[0006] One of the purposes of the present invention is to provide an ATO target material, which effectively improves the relative density of the target material by mixing and doping tin oxide and antimony oxide powders of specific particle sizes and combining them with zinc oxide powder of specific dosage and specific particle size.

[0007] Another object of the present invention is to provide a method for preparing an ATO target material. The target material prepared by the method can greatly improve the relative density of the target material and can fully inhibit the volatilization of antimony oxide during the sintering process.

[0008] To achieve the above-mentioned purpose, the present invention provides an ATO target material, which is obtained by mixing and sintering 90-95.5wt% SnO2 powder, 3-8.5wt% Sb2O3 powder, and 1.5-2wt% ZnO powder; wherein the particle size D50 of the SnO2 powder is 0.5-2μm, the particle size D50 of the Sb2O3 powder is 3-15μm, and the particle size D50 of the ZnO powder is 3-15μm.

[0009] Doping zinc oxide in the ATO target material has the effect of promoting the sintering of the target material, but since it cannot be doped in large quantities, its sintering-promoting effect is limited. Based on this, the present invention effectively improves the sintering-promoting effect of zinc oxide by controlling the particle size of tin oxide and antimony oxide powders, thereby increasing the relative density of the target material.

[0010] In the technical solution of the present invention, the ATO target material of the present invention can be obtained by mixing tin oxide, antimony oxide and zinc oxide powders and then adopting a conventional hot pressing sintering process, and a very high relative density of the target material can also be achieved.

[0011] In order to further improve the relative density of the target material, the present invention also discloses a method for preparing the above-mentioned ATO target material, comprising the following steps:

[0012] Step 1: Mix SnO2 powder, Sb2O3 powder and ZnO powder evenly;

[0013] Step 2: Sinter the powder mixed evenly in step 1 at 800-1000° C. for 3-5 hours to obtain a sintered green blank;

[0014] Step 3: crushing the sintered green billet to obtain sintered powder;

[0015] Step 4: Sinter the sintered powder at a sintering temperature of 900-1000° C. and a sintering pressure of 50-80 MPa for 50-80 min to obtain an ATO target.

[0016] The ATO target material preparation method of the present invention performs high-temperature sintering to initially grow and shape the grains of tin oxide, antimony oxide and zinc oxide, then crushes the grown and shaped grains into powders with uniform D50 particle size, and then performs hot pressing and sintering to obtain a target material with uniformity and relative density.

[0017] The present invention performs the first sintering to shape the grain growth of antimony oxide to obtain a sintered green billet, then crushes the sintered green billet into powder particles with uniform particle size, and then performs hot pressing sintering, thereby further improving the relative density of the target material.

[0018] Furthermore, the step 1 adopts dry mixing.

[0019] Furthermore, the particle size D50 of the sintered powder obtained in step 3 is ≤2 μm.

[0020] Furthermore, after the sintering in step 2 is completed, the furnace needs to be cooled to obtain a sintered green billet.

[0021] Furthermore, after the sintering in step 4 is completed, the ATO target material needs to be cooled in the furnace to obtain the ATO target material.

[0022] Beneficial Effects

[0023] Compared with the prior art, the present invention has at least the following advantages:

[0024] (1) The present invention uses the particle size matching of SnO2 powder, Sb2O3 powder and ZnO powder to give full play to the effect of ZnO in promoting the sintering of the target material and effectively improve the relative density of the target material;

[0025] (2) The present invention increases the amount of ZnO powder added to the conventional ATO target, and the difference in particle size between ZnO powder, SnO2 powder and Sb2O3 powder effectively promotes sintering and increases the relative density of the target, while greatly improving the ability to inhibit the volatilization of SnO2, ensuring that the electrochemical performance of the target will not be significantly reduced due to the volatilization of SnO2;

[0026] (3) The present invention discloses a method for preparing an ATO target material, wherein the first sintering is performed to shape the grain growth of antimony oxide to obtain a sintered green billet, and then the sintered green billet is crushed into powder particles of uniform particle size, and then hot-pressed sintering is performed, thereby further improving the relative density of the target material. DETAILED DESCRIPTION

[0027] The present invention will be further described below in conjunction with the embodiments, but it does not constitute any limitation to the present invention. Any limited number of modifications made within the scope of the claims of the present invention are still within the scope of the claims of the present invention.

[0028] In order to explain the technical content of the present invention in detail, further description is given below in conjunction with the implementation modes.

[0029] In the following examples and comparative examples, unless otherwise specified, the parts and % refer to parts by mass and percentage by mass, respectively.

[0030] Example 1

[0031] An ATO target is prepared by the following steps:

[0032] Step 1: 90 parts of SnO2 powder with a particle size D50 of 2 μm, 8 parts of Sb2O3 powder with a particle size D50 of 3 μm, and 2 parts of ZnO powder with a particle size D50 of 5 μm are mixed by a dry method to obtain a uniform mixed powder;

[0033] Step 2: Place the mixed powder in a vacuum hot pressing furnace, heat it to 900°C, pressurize it to 80 MPa, and sinter it for 350 minutes to obtain the target material.

[0034] Example 2

[0035] An ATO target is prepared by the following steps:

[0036] Step 1: 90 parts of SnO2 powder with a particle size D50 of 0.5 μm, 8 parts of Sb2O3 powder with a particle size D50 of 10 μm, and 2 parts of ZnO powder with a particle size D50 of 8 μm are mixed by a dry method to obtain a uniform mixed powder;

[0037] Step 2: Place the mixed powder into a sintering furnace and heat to 900°C for 5 hours to obtain a sintered green blank;

[0038] Step 3: Put the sintered green billet into a pulverizer for pulverization to obtain sintered powder with a particle size D50≤2μm;

[0039] Step 4: Place the sintered powder into a vacuum hot press furnace, heat it to 900°C, and pressurize it to 80Mpa, and sinter it for 50 minutes to obtain the target material.

[0040] Example 3

[0041] An ATO target is prepared by the following steps:

[0042] Step 1: 95.5 parts of SnO2 powder with a particle size D50 of 1 μm, 3 parts of Sb2O3 powder with a particle size D50 of 15 μm, and 1.5 parts of ZnO powder with a particle size D50 of 3 μm are mixed by a dry method to obtain a uniform mixed powder;

[0043] Step 2: Place the mixed powder into a sintering furnace and heat to 800°C for 4 hours to obtain a sintered green blank;

[0044] Step 3: Put the sintered green billet into a pulverizer for pulverization to obtain sintered powder with a particle size D50≤2μm;

[0045] Step 4: Place the sintered powder into a vacuum hot press furnace, heat it to 1000°C, pressurize it to 50 MPa, and sinter it for 80 minutes to obtain the target material.

[0046] Example 4

[0047] An ATO target is prepared by the following steps:

[0048] Step 1: 94 parts of SnO2 powder with a particle size D50 of 1 μm, 4.3 parts of Sb2O3 powder with a particle size D50 of 12 μm, and 1.7 parts of ZnO powder with a particle size D50 of 10 μm are mixed by a dry method to obtain a uniform mixed powder;

[0049] Step 2: Place the mixed powder into a sintering furnace and heat to 1000°C for 3 hours to obtain a sintered green blank;

[0050] Step 3: Put the sintered green billet into a pulverizer for pulverization to obtain sintered powder with a particle size D50≤2μm;

[0051] Step 4: Place the sintered powder into a vacuum hot press furnace, heat it to 950°C, pressurize it to 60 MPa, and sinter it for 60 minutes to obtain the target material.

[0052] Comparative Example 1

[0053] It is generally the same as Example 1, except that the particle size D50 of the SnO2 powder is 0.3 μm.

[0054] Comparative Example 2

[0055] It is generally the same as Example 1, except that the particle size D50 of the SnO2 powder is 5 μm.

[0056] Comparative Example 3

[0057] It is generally the same as Example 1, except that the particle size D50 of the Sb2O3 powder is 1 μm.

[0058] Comparative Example 4

[0059] It is generally the same as Example 1, except that the particle size D50 of the Sb2O3 powder is 20 μm.

[0060] Comparative Example 5

[0061] It is generally the same as Example 1, except that the particle size D50 of the ZnO powder is 1 μm.

[0062] Comparative Example 6

[0063] It is generally the same as Example 1, except that the particle size D50 of the ZnO powder is 25 μm.

[0064] Comparative Example 7

[0065] It is generally the same as Example 2, except that the mass fraction of the ZnO powder with a particle size D50 of 8 μm is 1 part.

[0066] Comparative Example 8

[0067] It is generally the same as Example 2, except that the mass fraction of the ZnO powder with a particle size D50 of 8 μm is 3 parts.

[0068] Product quality testing

[0069] Relative density: Archimedean drainage method.

[0070] The relative density and target composition of the ATO targets obtained in Examples 1-4 and Comparative Examples 1-8 were tested, and the results are shown in Table 1.

[0071] Table 1 ATO target product quality test results obtained in Examples 1-4 and Comparative Examples 1-8

[0072] Relative density% Example 1 95.6％ Example 2 98.3％ Example 3 98.7％ Example 4 98.2％ Comparative Example 1 90.8％ Comparative Example 2 87.6％ Comparative Example 3 90.3％ Comparative Example 4 90.5％ Comparative Example 5 89.9％ Comparative Example 6 88.5％ Comparative Example 7 92.6％ Comparative Example 8 90.7％

[0073] According to the results in Table 1, we can see that:

[0074] According to the data of Examples 1-4, the present invention fully exerts the effect of ZnO in promoting target sintering and effectively improves the relative density of the target by matching the particle sizes of SnO2 powder, Sb2O3 powder and ZnO powder; and according to the comparison of the data of Example 1 and Example 2, the present invention first performs a first sintering to shape the grain growth of antimony oxide to obtain a sintered blank, and then crushes the sintered blank into powder particles of uniform particle size, and then performs hot pressing sintering, thereby further improving the relative density of the target.

[0075] According to the data comparison between Example 1 and Comparative Examples 1-6, it can be seen that in the technical solution of the present invention, the particle size selection of SnO2 powder, Sb2O3 powder and ZnO powder has a more obvious effect on the relative density of the target material, indicating that the present invention has a synergistic effect of improving the relative density of the target material through the particle size matching of SnO2 powder, Sb2O3 powder and ZnO powder.

[0076] According to the data comparison between Example 2 and Comparative Example 7, when the dosage of ZnO is too low, the effect of promoting the sintering of the target material is greatly reduced, resulting in a significant decrease in the relative density of the obtained target material.

[0077] According to the data comparison between Example 2 and Comparative Example 8, it can be seen that when the dosage of ZnO is too high, the relative density of the obtained target material shows a significant decrease, and is even lower than that of Comparative Example 7. The possible reason is that too much ZnO affects the uniformity between the components of the target material and the crystal growth, resulting in a significant decrease in the relative density of the target material.

[0078] The embodiments presented herein are only embodiments selected according to the combination of all possible embodiments. The appended claims should not be limited by the embodiments describing the present invention. Some numerical ranges used in the claims include sub-ranges therein, and the changes in these ranges should also be covered by the appended claims.

Claims

1. An ATO target, characterized in that: It is obtained by mixing and sintering 90-95.5wt% SnO2 powder, 3-8.5wt% Sb2O3 powder and 1.5-2wt% ZnO powder; wherein the particle size D50 of the SnO2 powder is 0.5-2μm, the particle size D50 of the Sb2O3 powder is 3-15μm, and the particle size D50 of the ZnO powder is 3-15μm.

2. A method for preparing an ATO target material as claimed in claim 1, characterized in that: The steps include: Step 1: Mix SnO2 powder, Sb2O3 powder and ZnO powder evenly; Step 2: Sinter the powder mixed evenly in step 1 at 800-1000° C. for 3-5 hours to obtain a sintered green blank; Step 3: crushing the sintered green billet to obtain sintered powder; Step 4: Sinter the sintered powder at a sintering temperature of 900-1000° C. and a sintering pressure of 50-80 MPa for 50-80 min to obtain an ATO target.

3. The method for preparing an ATO target according to claim 2, characterized in that: The step 1 adopts dry mixing.

4. The method for preparing an ATO target according to claim 2, characterized in that: The particle size D50 of the sintered powder obtained in step 3 is ≤2 μm.

5. The method for preparing an ATO target according to claim 2, characterized in that: After the sintering in step 2 is completed, the furnace needs to be cooled to obtain a sintered green billet.

6. The method for preparing an ATO target according to claim 2, characterized in that: After the sintering in step 4 is completed, the ATO target material needs to be cooled in the furnace to obtain the ATO target material.