Indium cerium oxide target and method for manufacturing the same

Abstract

The application belongs to the field of target materials, and discloses a preparation method of an indium cerium oxide target material, which comprises the following steps: mixing indium oxide powder, cerium oxide powder, a dispersing agent and water, and then spray granulating to obtain mixed powder A; sintering the mixed powder A; mixing indium hydroxide powder with the sintered mixed powder A and compression molding to obtain a target material blank; and sintering the target material blank to obtain the indium cerium oxide target material. In the application, the indium hydroxide powder is selected to replace the commonly used organic binder in the prior art, so that the generation of black spots by the organic binder in the sintering process is prevented; and the indium hydroxide powder is dehydrated in the sintering process, and water hinders the sintering densification process at high temperature, so that a low-density target material is obtained.

Description

Technical Field

[0001] This invention belongs to the field of target materials, and relates to a conductive oxide material and its preparation method, specifically to an indium cerium oxide target and its preparation method. Background Technology

[0002] Transparent conductive oxide thin films exhibit high transmittance of visible light and high reflectivity of infrared light, while also possessing excellent conductivity. Therefore, they are widely used in solar cells, liquid crystal displays, light-emitting diodes, and thermal radiation reflectors. Common methods for preparing transparent conductive oxide thin films include vacuum evaporation, chemical vapor deposition, spraying, magnetron sputtering, and sol-gel methods. Among these, vacuum evaporation utilizes high current to generate high heat energy, causing the target material to evaporate or sublimate into energetic gaseous particles that are deposited onto the surface of the material to be coated, forming a thin film. This method offers advantages such as simple film formation, high film purity and density, and unique film structure and properties.

[0003] In existing technologies, other elements are typically doped into the target material to improve the performance of the conductive film. For example, when preparing indium oxide powder targets, cerium is doped to improve the infrared transmittance of the conductive oxide film. To prepare cerium-doped targets, indium hydroxide powder, cerium oxide powder, and an organic binder are usually mixed to obtain a mixture, which is then pressed and sintered to obtain the target material. However, black spots (impurities) are prone to appear in the organic binder during sintering, affecting target evaporation in subsequent vapor deposition processes. Furthermore, impurity deposition during vapor deposition can easily lead to nodule formation on the coating surface, affecting the coating quality. Summary of the Invention

[0004] In view of the defects and deficiencies of the existing technology, the present invention provides, firstly, a method for preparing indium cerium oxide target material; and secondly, the present invention provides indium cerium oxide obtained by the above preparation method.

[0005] In a first aspect, the present invention provides a method for preparing an indium cerium oxide target, comprising the following steps: Step 1: Mix and grind indium oxide powder, cerium oxide powder, dispersant and water to prepare a slurry, and then spray granulate the slurry to obtain mixed powder A; Step 2: Sinter mixed powder A, then mix indium hydroxide powder and sintered mixed powder A, press into shape, and obtain target material blank; Step 3: Sinter the target blank to obtain the indium cerium oxide target.

[0006] The mass ratio of indium hydroxide powder added in step 2 to indium oxide powder added in step 1 is 90~96:3~7.

[0007] Preferably, in step 1, the mass ratio of indium oxide powder, cerium oxide powder, dispersant and water is 90~96∶1~3∶1~5∶35~45.

[0008] Preferably, the dispersant is any one or more of polyvinylpyrrolidone (PVP), sodium dodecylbenzenesulfonate (SDBS), and sodium hexadecylbenzenesulfonate; and the water is any one or two of pure water or deionized water.

[0009] Preferably, the mass concentration of the dispersant is 15-30%.

[0010] Preferably, step 1 includes the following steps: Step 101: Mix cerium oxide powder, dispersant and water and grind to obtain cerium oxide powder slurry; Step 102: Indium oxide powder and dispersant are added to the cerium oxide powder slurry and then ground to obtain a mixed slurry of cerium oxide powder and indium oxide powder.

[0011] Further optimization is made in step 101, where the mass of the dispersant is 1-5% of the mass of the cerium oxide powder slurry; the grinding speed is 1200-1800 r / min; and the grinding time is 10-22 h.

[0012] Further preferred, in step 102, the mass of the dispersant is 1-15% of the total mass of the indium oxide powder and the dispersant added in step 102; the grinding speed is 1200~1800 r / min, and the grinding time is 8~15 h.

[0013] Preferably, in step 1, during spray granulation, the outlet air temperature is 70~85℃ and the atomizer frequency is 110~120Hz.

[0014] Preferably, the sintering temperature in step 2 is higher than the sintering temperature in step 3, and the temperature difference between the sintering temperatures in step 2 and step 3 is 150~220℃.

[0015] Preferably, in step 2, when sintering the mixed powder A, the temperature is increased to 1100~1500℃ at a heating rate of 0.5~1℃ / min and held for 6~12h.

[0016] Preferably, in step 2, the pressure during pressing is 15~20T.

[0017] Preferably, in step 3, when sintering the target blank, the temperature is raised to 1280~1320℃ at a heating rate of 0.3~0.7℃ / min and held for 8~12h.

[0018] Secondly, the present invention provides an indium cerium oxide target material, which is prepared by the above-described preparation method.

[0019] Compared with the prior art, one or more technical solutions provided by the present invention have at least one of the following beneficial effects: (1) The present invention utilizes the high viscosity of indium hydroxide powder to replace the organic binder commonly used in the prior art, thereby reducing the possibility of black spots being generated during the sintering process; and the indium hydroxide powder will dehydrate during the sintering process, and the water evaporates at high temperature, which hinders the densification process of the target material sintering, thereby obtaining a low-density target material.

[0020] (2) In this invention, the indium oxide powder and cerium oxide powder are sintered first to pre-treat the raw materials, so as to avoid significant shrinkage during subsequent sintering of the target material blank and facilitate control of the target material size. Attached Figure Description

[0021] Figure 1 A physical image of the target material prepared according to Example 1 of the present invention; Figure 2 A physical image of the target material prepared in Comparative Example 1 provided by the present invention; Figure 3 A physical image of the target material prepared in Comparative Example 2 provided by the present invention; Figure 4 This is a physical image of the target material prepared in Comparative Example 3 provided by the present invention. Detailed Implementation

[0022] The present invention provides the following specific technical solutions.

[0023] In a first aspect, the present invention provides a method for preparing an indium cerium oxide target, comprising the following steps: Step 1: Mix and grind indium oxide powder, cerium oxide powder, dispersant and water to prepare a slurry, and then spray granulate the slurry to obtain mixed powder A; Step 2: Sinter mixed powder A, then mix indium hydroxide powder and sintered mixed powder A, press into shape, and obtain target material blank; Step 3: Sinter the target blank to obtain the indium cerium oxide target.

[0024] The mass ratio of indium hydroxide powder added in step 2 to indium oxide powder added in step 1 is 90~96:3~7.

[0025] In existing technologies, adding organic binders during target preparation can easily lead to black spots appearing on the target after sintering, affecting the vapor deposition of the target film. The inventors discovered that using indium hydroxide powder to replace the organic binder offers several advantages: First, indium hydroxide powder has high viscosity, preventing the formation of black spots during sintering; second, indium hydroxide powder dehydrates during sintering, and water at high temperatures hinders the densification process, resulting in a low-density target; third, the addition of indium hydroxide powder does not introduce other impurities into the target, improving its purity.

[0026] Furthermore, the present invention performs sintering treatment on the raw material powder before pressing the target blank, which can prevent the target blank from shrinking significantly during subsequent sintering, thereby better controlling the target size.

[0027] Preferably, in step 1, the mass ratio of indium oxide powder, cerium oxide powder, dispersant and water is 90~96∶1~3∶1~5∶35~45.

[0028] In actual production, the amounts of dispersant and water can be adjusted according to actual needs, as long as the amount of dispersant added meets the dispersion effect and can be completely discharged during the subsequent sintering process. The amount of water added mainly affects the subsequent spray granulation process. If too much water is added, the spray granulation process will take too long, resulting in energy waste and increased costs. If too little water is added, it will be detrimental to grinding, affecting grinding uniformity and making the spray process difficult to carry out. Therefore, the inventors proposed the above-mentioned preferred range.

[0029] Preferably, the dispersant is any one or more of polyvinylpyrrolidone (PVP), sodium dodecylbenzenesulfonate (SDBS), and sodium hexadecylbenzenesulfonate; the water is pure water or deionized water.

[0030] In actual operation, the preferred raw materials are: indium hydroxide powder with a purity of 4N, indium oxide powder with a purity of 4N, and cerium oxide powder with a purity of 4N; pure water or deionized water is used as raw materials to avoid introducing impurities.

[0031] In step 1, cerium oxide powder, dispersant and water are mixed and then ground to obtain cerium oxide powder slurry; then indium oxide powder and dispersant are added to the cerium oxide powder slurry and ground to obtain a mixed slurry of cerium oxide powder and indium oxide powder.

[0032] In actual production, cerium oxide powder is first dispersed, and then indium oxide powder is added and dispersed. This stepwise mixing can result in better dispersion, better grinding, and more uniform particle size.

[0033] Further optimization is made in step 101, where the mass of the dispersant is 1-5% of the mass of the cerium oxide powder slurry; the grinding speed is 1200-1800 r / min; and the grinding time is 10-22 h.

[0034] Further preferred, in step 102, the mass of the dispersant is 1-15% of the total mass of the indium oxide powder and the dispersant added in step 102; the grinding speed is 1200~1800 r / min, and the grinding time is 8~15 h.

[0035] In actual production, the mixture is pre-dispersed before grinding to make the distribution of each material more uniform, resulting in a more uniform particle distribution in the target material and improving the quality of the target material.

[0036] Preferably, in step 1, during spray granulation, the outlet air temperature is 70~85℃ and the atomizer frequency is 110~120Hz.

[0037] Preferably, the sintering temperature in step 2 is higher than the sintering temperature in step 3.

[0038] Preferably, in step 2, when sintering the mixed powder A, the temperature is increased to 1100~1500℃ at a heating rate of 0.5~1℃ / min and held for 6~12h.

[0039] The inventors discovered through research that if the sintering temperature is too low, the mixed powder will not shrink completely during sintering, which will lead to significant shrinkage during the subsequent target sintering process; if the sintering temperature is too high, the mixed powder will stick together, making it impossible to carry out subsequent processes.

[0040] Preferably, in step 2, the pressure during pressing is 15~20T.

[0041] Preferably, in step 3, when sintering the target blank, the temperature is raised to 1280~1320℃ at a heating rate of 0.3~0.7℃ / min and held for 8~12h.

[0042] The inventors discovered through research that both excessively high and excessively low sintering temperatures can easily lead to cracks on the surface of the target material. Excessively high sintering temperatures can cause the grains of the target material to gradually grow and the density to increase, while also causing a certain volume expansion of the target material, resulting in some cracks. Excessively low sintering temperatures can lead to incomplete bonding between powders, resulting in low internal strength of the target material.

[0043] Secondly, the present invention provides an indium cerium oxide target material, which is prepared by the above-described preparation method.

[0044] To make the technical problems, technical solutions and technical advantages of the present invention clearer, a detailed description will be given below with reference to specific examples. However, the scope of protection of the present invention is not limited to the following specific embodiments.

[0045] Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the scope of the invention.

[0046] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this invention can be purchased from the market or prepared by existing methods.

[0047] Example 1: A method for preparing an indium cerium oxide target includes the following steps: Step 1: Weigh out indium oxide powder, cerium oxide powder, and indium hydroxide powder according to a mass ratio of 92:3:5 and set aside.

[0048] Step 2: Add pure water to the slurry tank. The mass ratio of pure water to cerium oxide powder weighed in Step 1 is 1:20. Add the cerium oxide powder weighed in Step 1 and a 20% PVP solution sequentially to the slurry tank for pre-dispersion. The dispersion time is 30 minutes, and the dispersion speed is 100 rpm, to obtain a cerium oxide powder slurry. The mass of PVP solution added in the preparation of the cerium oxide powder slurry is 4% of the total mass of cerium oxide powder, pure water, and PVP solution. Then, use a pneumatic diaphragm pump to pump the cerium oxide powder slurry into a sand mill for grinding. The grinding time is 16 hours, and the grinding speed is 1500 rpm.

[0049] Step 3: The indium oxide powder and 20% PVP solution weighed in Step 1 are added to the cerium oxide powder slurry for pre-dispersion. The dispersion time is 30 min and the dispersion speed is 100 rpm, resulting in a mixed slurry of cerium oxide powder and indium oxide powder. When preparing the mixed slurry of cerium oxide powder and indium oxide powder, the mass of the added PVP solution is 4% of the total mass of the indium oxide powder and the PVP solution added in Step 3. Then, the mixed slurry of cerium oxide powder and indium oxide powder is pumped into a sand mill for grinding using a pneumatic diaphragm pump for 8 h, during which the grinding speed is 1500 r / min.

[0050] Step 4: The slurry of the ground cerium oxide powder and indium oxide powder is fed into a spray drying tower for spray granulation, followed by mixing and sieving to obtain mixed powder A, wherein the outlet air temperature is 75℃ and the atomizer frequency is 120Hz.

[0051] Step 5: The mixed powder A is loaded into an alumina crucible and sintered in a sintering furnace at a temperature of 1450℃, a heating rate of 1℃ / min, and a holding time of 8h.

[0052] Step 6: Mix the indium hydroxide powder weighed in step 1 with the sintered mixed powder A, and mix them using a mixer for 6 hours.

[0053] Step 7: Take 100g of the powder obtained in step 6 and pour it into a 30*40mm mold and press it at 15T to obtain the target preform.

[0054] Step 8: Sinter the target blank in a sintering furnace, heating it to 1300℃ at a rate of 0.5℃ / min and holding it at that temperature for 10 hours.

[0055] Example 2: A method for preparing an indium cerium oxide target includes the following steps: Step 1: Weigh out indium oxide powder, cerium oxide powder, and indium hydroxide powder according to a mass ratio of 90:3:7 and set aside.

[0056] Step 2: Add pure water to the slurry tank. The mass ratio of pure water to cerium oxide powder weighed in Step 1 is 3:35. Add the cerium oxide powder weighed in Step 1 and a 15% PVP solution sequentially to the slurry tank for pre-dispersion. The dispersion time is 30 minutes, and the dispersion speed is 100 rpm, to obtain a cerium oxide powder slurry. When preparing the cerium oxide powder slurry, the mass of the added SDBS solution is 1% of the total mass of the cerium oxide powder, pure water, and SDBS solution. Then, use a pneumatic diaphragm pump to pump the cerium oxide powder slurry into a sand mill for grinding. The grinding time is 10 hours, and the grinding speed is 1200 rpm.

[0057] Step 3: The indium oxide powder and 15% PVP (by mass concentration) weighed in Step 1 are added to the cerium oxide powder slurry for pre-dispersion. The dispersion time is 30 min and the dispersion speed is 100 rpm, resulting in a mixed slurry of cerium oxide powder and indium oxide powder. When preparing the mixed slurry of cerium oxide powder and indium oxide powder, the mass of the added SDBS solution is 1% of the total mass of the indium oxide powder and the SDBS solution added in Step 3. Then, the mixed slurry of cerium oxide powder and indium oxide powder is pumped into a sand mill for grinding using a pneumatic diaphragm pump for 8 h, wherein the grinding speed is 1200 r / min.

[0058] Step 4: The slurry of the ground cerium oxide powder and indium oxide powder is fed into a spray drying tower for spray granulation, followed by mixing and sieving to obtain mixed powder A, wherein the outlet air temperature is 70℃ and the atomizer frequency is 120Hz.

[0059] Step 5: The mixed powder A is loaded into an alumina crucible and sintered in a sintering furnace at a temperature of 1100℃, a heating rate of 0.5℃ / min, and a holding time of 6h.

[0060] Step 6: Mix the indium hydroxide powder weighed in step 1 with the sintered mixed powder A, and mix them using a mixer for 6 hours.

[0061] Step 7: Take 100g of the powder obtained in Step 7 and pour it into a 30*40mm mold and press it at 15T to obtain the target preform.

[0062] Step 8: Sinter the target blank in a sintering furnace, heating it to 1280℃ at a rate of 0.3℃ / min and holding it at that temperature for 8 hours.

[0063] Example 3: A method for preparing an indium cerium oxide target includes the following steps: Step 1: Weigh out indium oxide powder, cerium oxide powder, and indium hydroxide powder according to a mass ratio of 94:3:3 for later use.

[0064] Step 2: Add pure water to the slurry tank. The mass ratio of pure water to cerium oxide powder weighed in Step 1 is 1:45. Add the cerium oxide powder weighed in Step 1 and a 20% PVP solution sequentially to the slurry tank for pre-dispersion. The dispersion time is 30 min, and the dispersion speed is 100 rpm, to obtain a cerium oxide powder slurry. When preparing the cerium oxide powder slurry, the mass of the sodium hexadecylbenzenesulfonate solution is 5% of the total mass of the cerium oxide powder, pure water, and sodium hexadecylbenzenesulfonate solution. Then, use a pneumatic diaphragm pump to pump the cerium oxide powder slurry into a sand mill for grinding. The grinding time is 22 h, and the grinding speed is 1800 r / min.

[0065] Step 3: The indium oxide powder and 20% PVP solution weighed in Step 1 are added to the cerium oxide powder slurry for pre-dispersion. The dispersion time is 30 min and the dispersion speed is 100 rpm, resulting in a mixed slurry of cerium oxide powder and indium oxide powder. When preparing the mixed slurry of cerium oxide powder and indium oxide powder, the mass of the added sodium hexadecylbenzenesulfonate solution is 15% of the total mass of the indium oxide powder and the sodium hexadecylbenzenesulfonate solution added in Step 3. Then, the mixed slurry of cerium oxide powder and indium oxide powder is pumped into a sand mill for grinding using a pneumatic diaphragm pump for 15 h, wherein the grinding speed is 1500 r / min.

[0066] Step 4: The slurry of the ground cerium oxide powder and indium oxide powder is fed into a spray drying tower for spray granulation, followed by mixing and sieving to obtain mixed powder A, wherein the outlet air temperature is 85℃ and the atomizer frequency is 120Hz.

[0067] Step 5: The mixed powder A is loaded into an alumina crucible and sintered in a sintering furnace at a temperature of 1500℃, a heating rate of 1℃ / min, and a holding time of 12h.

[0068] Step 6: Mix the indium hydroxide powder weighed in step 1 with the sintered mixed powder A, and mix them using a mixer for 6 hours.

[0069] Step 7: Take 100g of the powder obtained in Step 7 and pour it into a 30*40mm mold and press it at 15T to obtain the target preform.

[0070] Step 8: Sinter the target blank in a sintering furnace, heating it to 1320℃ at a rate of 0.7℃ / min and holding it at that temperature for 12 hours.

[0071] Comparative Example 1: A method for preparing an indium cerium oxide target includes the following steps: Step 1: Weigh out indium oxide powder and cerium oxide powder according to a mass ratio of 97:3 and set aside.

[0072] Step 2: Add pure water to the slurry tank. The mass ratio of pure water to cerium oxide powder weighed in Step 1 is 1:20. Add the cerium oxide powder weighed in Step 1 and a 20% PVP solution sequentially to the slurry tank for pre-dispersion. The dispersion time is 30 minutes, and the dispersion speed is 100 rpm, to obtain a cerium oxide powder slurry. The mass of PVP solution added in the preparation of the cerium oxide powder slurry is 4% of the total mass of cerium oxide powder, pure water, and PVP solution. Then, use a pneumatic diaphragm pump to pump the cerium oxide powder slurry into a sand mill for grinding. The grinding time is 16 hours, and the grinding speed is 1500 rpm.

[0073] Step 3: The indium oxide powder and 20% PVP solution weighed in Step 1 are added to the cerium oxide powder slurry for pre-dispersion. The dispersion time is 30 min and the dispersion speed is 100 rpm, resulting in a mixed slurry of cerium oxide powder and indium oxide powder. When preparing the mixed slurry of cerium oxide powder and indium oxide powder, the mass of the added PVP solution is 4% of the total mass of the indium oxide powder and the PVP solution added in Step 3. Then, the mixed slurry of cerium oxide powder and indium oxide powder is pumped into a sand mill for grinding using a pneumatic diaphragm pump for 8 h, during which the grinding speed is 1500 r / min.

[0074] Step 4: The slurry of the ground cerium oxide powder and indium oxide powder is fed into a spray drying tower for spray granulation, followed by mixing and sieving to obtain mixed powder A, wherein the outlet air temperature is 75℃ and the atomizer frequency is 120Hz.

[0075] Step 5: The mixed powder A is loaded into an alumina crucible and sintered in a sintering furnace at a temperature of 1450℃, a heating rate of 1℃ / min, and a holding time of 8h.

[0076] Step 6: Mix polyvinyl alcohol, deionized water and the mixed powder A obtained from sintering in Step 5. The mass of polyvinyl alcohol added is 1% of the mass of mixed powder A obtained from sintering in Step 5, and the mass of deionized water is 4% of the mass of mixed powder A obtained from sintering in Step 5. Mix the materials using a mixer for 6 hours.

[0077] Step 7: Take 100g of the powder obtained in step 6 and pour it into a 30*40mm mold and press it at 15T to obtain the target preform.

[0078] Step 8: Sinter the target blank in a sintering furnace, heating it to 1300℃ at a rate of 0.5℃ / min and holding it at that temperature for 10 hours.

[0079] Comparative Example 2: A method for preparing an indium cerium oxide target includes the following steps: Step 1: Weigh out indium oxide powder, cerium oxide powder, and indium hydroxide powder according to a mass ratio of 92:3:5 and set aside.

[0080] Step 2: Add pure water to the slurry tank. The mass ratio of pure water to cerium oxide powder weighed in Step 1 is 1:20. Add the cerium oxide powder weighed in Step 1 and a 20% (w / w) PVP solution sequentially to the slurry tank for pre-dispersion. The dispersion time is 30 min, and the dispersion speed is 100 rpm, to obtain a cerium oxide powder slurry. The mass of PVP solution added in the preparation of the cerium oxide powder slurry is 4% of the total mass of cerium oxide powder, pure water, and PVP solution. Then, use a pneumatic diaphragm pump to pump the cerium oxide powder slurry into a sand mill for grinding. The grinding time is 16 h, and the grinding speed is 1500 r / min.

[0081] Step 3: The indium oxide powder and 20% PVP solution weighed in Step 1 are added to the cerium oxide powder slurry for pre-dispersion. The dispersion time is 30 min and the dispersion speed is 100 rpm, resulting in a mixed slurry of cerium oxide powder and indium oxide powder. When preparing the mixed slurry of cerium oxide powder and indium oxide powder, the mass of the added PVP solution is 4% of the total mass of the indium oxide powder and the PVP solution added in Step 3. Then, the mixed slurry of cerium oxide powder and indium oxide powder is pumped into a sand mill for grinding using a pneumatic diaphragm pump for 8 h, during which the grinding speed is 1500 r / min.

[0082] Step 4: The slurry of the ground cerium oxide powder and indium oxide powder is fed into a spray drying tower for spray granulation, followed by mixing and sieving to obtain mixed powder A, wherein the outlet air temperature is 75℃ and the atomizer frequency is 120Hz.

[0083] Step 5: Mix the indium hydroxide powder and mixed powder A weighed in step 1 using a mixer for 6 hours.

[0084] Step 6: Take 100g of the powder obtained in step 5 and pour it into a 30*40mm mold and press it at 15T to obtain the target blank.

[0085] Step 7: Sinter the target blank in a sintering furnace, heating it to 1300℃ at a rate of 0.5℃ / min and holding it at that temperature for 10 hours.

[0086] Comparative Example 3: The difference from Example 1 is that in step 1, indium oxide powder, cerium oxide powder, and indium hydroxide powder are weighed in a mass ratio of 87:3:10 for later use.

[0087] The relative density and shrinkage rate of the target materials prepared in Examples 1-3 and Comparative Examples 1-3 were tested, and the test results are shown in Table 1.

[0088] Table 1 - Morphology, relative density, and shrinkage rate of the targets prepared in Examples 1-4 and Comparative Examples 1-2 Figure 1 Here is a physical image of the target material prepared in Example 1. Figure 1 It can be clearly seen that the target material prepared in Example 1 has good formability, and multiple targets have the same shape and size, smooth surface, no cracks, and no black spots. Figure 2 Here is a physical image of the target material prepared in Comparative Example 1, by... Figure 2 It can be clearly seen that the target material prepared in Comparative Example 1 has a rough surface, black spots, and cracks at the top and bottom. Comparing the surface condition and relative density of the target materials prepared in Example 1 and Comparative Example 1, it can be seen that using indium hydroxide powder instead of binder can avoid the appearance of black spots on the surface of the target material and can reduce the relative density of the target material.

[0089] Figure 3 Here is a physical image of the target material prepared in Comparative Example 2, by... Figure 3 It can be clearly seen that the target material prepared in Comparative Example 2 has a rough surface, black dirt, and unevenness on the circumference of the upper and lower end faces. Comparing the surface condition and relative density of the targets prepared in Example 1 and Comparative Example 2, it can be seen that: pre-sintering the mixture of indium oxide powder and cerium oxide powder to pre-treat the raw materials can avoid significant shrinkage during the subsequent sintering of the target material blank, making it easier to control the target size; and by sintering the mixture of indium oxide powder and cerium oxide powder, the dispersant can be released, avoiding dirt on the target surface.

[0090] Figure 4 Here is a physical image of the target material prepared in Comparative Example 3, by... Figure 4It is clearly visible that the target material prepared in Comparative Example 3 has many cracks. Through the cracks, numerous pores can be faintly seen inside the target material, indirectly proving that the target material prepared in Comparative Example 3 has a loose structure. Indium hydroxide powder decomposes into indium oxide powder after sintering. In fact, the mass ratio of indium oxide powder, cerium oxide powder, and indium hydroxide powder in Example 1 and Comparative Example 3 is 97:3. Figure 1 and Figure 4 The inventors investigated that the differences in the surface condition and relative density of the prepared target materials may be due to the following: Indium hydroxide powder participates in the reaction as a binder. The binder (indium hydroxide powder) added in Comparative Example 3 is twice that in Example 1. Adding too much indium hydroxide powder results in too much water vapor generated by the thermal decomposition of indium hydroxide powder, which leads to too many pores inside the target material, resulting in more cracks in the target material, which cracks upon contact.

[0091] The above-described embodiments are merely preferred embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the technical scope of the present invention, based on the technical solution and concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A method for preparing an indium cerium oxide target, characterized in that, Includes the following steps: Step 1: Mix and grind indium oxide powder, cerium oxide powder, dispersant and water to prepare a slurry, and then spray granulate the slurry to obtain mixed powder A; Step 2: Sinter mixed powder A, then mix indium hydroxide powder and sintered mixed powder A, press and shape to obtain target blank; when sintering mixed powder A, heat to 1100~1500℃ and hold for 6~12h. Step 3: Sinter the target blank to obtain the indium cerium target; when sintering the target blank, heat to 1280~1320℃ and hold for 8~12 hours. The mass ratio of indium hydroxide powder added in step 2 to indium oxide powder added in step 1 is 3~7:90~96.

2. The method for preparing the indium cerium oxide target as described in claim 1, characterized in that, In step 1, the mass ratio of indium oxide powder, cerium oxide powder, dispersant and water is 90~96∶1~3∶1~5∶35~45.

3. The method for preparing the indium cerium oxide target as described in claim 1 or 2, characterized in that, The dispersant is any one or more of polyvinylpyrrolidone (PVP), sodium dodecylbenzenesulfonate (SDBS), and sodium hexadecylbenzenesulfonate; the water is pure water.

4. The method for preparing the indium cerium oxide target as described in claim 1, characterized in that, Step 1 includes the following steps: Step 101: Mix cerium oxide powder, dispersant and water and then grind to obtain cerium oxide powder slurry; Step 102: Indium oxide powder and dispersant are added to the cerium oxide powder slurry and then ground to obtain a mixed slurry of cerium oxide powder and indium oxide powder.

5. The method for preparing the indium cerium oxide target as described in claim 4, characterized in that, In step 101, the mass of the dispersant is 1-5% of the mass of the cerium oxide powder slurry; the grinding speed is 1200-1800 r / min, and the grinding time is 10-22 h; in step 102, the mass of the dispersant is 1-15% of the total mass of the indium oxide powder and the dispersant added in step 102; the grinding speed is 1200-1800 r / min, and the grinding time is 8-15 h.

6. The method for preparing the indium cerium oxide target as described in claim 1, characterized in that, The sintering temperature in step 2 is higher than that in step 3, and the temperature difference between the sintering temperatures in step 2 and step 3 is 150~220℃.

7. The method for preparing the indium cerium oxide target as described in claim 6, characterized in that, In step 2, when sintering the mixed powder A, the temperature is increased to 1100~1500℃ at a heating rate of 0.5~1℃ / min.

8. The method for preparing the indium cerium oxide target as described in claim 6, characterized in that, In step 3, when sintering the target blank, the temperature is increased to 1280~1320℃ at a heating rate of 0.3~0.7℃ / min.

9. The method for preparing the indium cerium oxide target as described in claim 1, characterized in that, In step 1, during spray granulation, the outlet air temperature is 70~85℃ and the atomizer frequency is 110~120Hz.

10. An indium cerium oxide target material, characterized in that, It is prepared by the preparation method described in any one of claims 1 to 9.

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