Low-resistance and high-density ito target material and preparation method thereof
Patent Information
- Application Number
- CN202610833713.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-06-10
- Publication Date
- 2026-08-18
AI Technical Summary
[0005]本发明的目的是提供一种低电阻高致密的ITO靶材及其制备方法,以解决现有技术中ITO靶材难以同时实现超低电阻率、超高致密度和良好机械性能的技术问题
1)本发明以微米级氧化铟、氧化锡为基质,搭配纳米级氧化钨、氧化钛作为掺杂助剂,二者形成高效协同。与现有技术中单一掺杂或固相混合不均导致的导电性波动相比,本发明的纳米掺杂助剂可在烧结过程中均匀扩散至晶格内部,有效增加载流子浓度并降低晶界散射,使靶材电阻率稳定控制在≤3.0×10-5Ω·cm,较传统ITO靶材降低一个数量级以上。
Smart Images

Figure SMS_1
Abstract
Description
Technical Field
[0001] This invention relates to a low-resistivity, high-density indium tin oxide (ITO) target and its preparation method, belonging to the field of target technology. Background Technology
[0002] Indium tin oxide (ITO) sputtering targets are widely used in the fabrication of transparent electrodes for optoelectronic devices such as liquid crystal displays (LCDs), organic light-emitting diodes (OLEDs), touch screens, and solar cells due to their excellent optical transparency and conductivity. As these technologies advance towards higher performance and lower cost, more stringent requirements are being placed on the performance of ITO sputtering targets: on the one hand, the resistivity of the target needs to be further reduced to improve coating efficiency and film conductivity; on the other hand, the density and mechanical strength of the target need to be increased to reduce abnormal discharge (arc firing) and target cracking during sputtering, thereby extending its service life.
[0003] The resistivity of traditional ITO sputtering targets (In2O3:SnO2 = 90:10 wt.%) is typically 1-2 × 10⁻⁶. -4 The indium content is on the order of Ω·cm, with a relative density of approximately 98-99%. To reduce costs, the industry has begun exploring ITO sputtering targets with low indium content. For example, patent CN118084480B discloses an ITO sputtering target with low indium content, which, by adding Sb₂O₃ as a sintering aid, achieves a relative density ≥99.5% and a resistivity ≤1×10⁻⁶ by high-temperature, short-time sintering. -3 The target material has a resistivity of Ω·cm. However, its resistivity is still lower than that of traditional ITO.
[0004] To improve performance, multi-doping strategies have been extensively studied. For example, patent CN121494528A discloses a gallium (Ga) and cerium (Ce) co-doped ITO target, which reduces resistivity to 1.1 × 10⁻⁶ through precise mixing and stepped sintering. -4 While achieving resistivity below Ω·cm and high flexural strength (≥230MPa), this method, despite its excellent performance, suffers from expensive doping elements (Ga, Ce) and complex fabrication processes with demanding equipment requirements. Therefore, developing a novel ITO target material and its fabrication method that can reduce resistivity, increase density, control costs, and simplify the process is of significant industrial value. Summary of the Invention
[0005] The purpose of this invention is to provide a low-resistivity, high-density ITO target and its preparation method, so as to solve the technical problem that ITO targets in the prior art are difficult to achieve ultra-low resistivity, ultra-high density and good mechanical properties at the same time.
[0006] To achieve the above-mentioned technical objectives, the present invention adopts the following technical solution: A method for preparing a low-resistivity, high-density ITO target includes the following steps: S1: After mixing the raw materials indium oxide and tin oxide powder in a certain proportion, disperse them in deionized water to prepare a suspension with a solid content of 20-40wt%. Adjust the pH to 3-5 with dilute hydrochloric acid to obtain mixed suspension A. S2: Disperse the dopant and composite sintering aid in deionized water containing anionic polyelectrolyte to prepare a suspension with a solid content of 5-15%, and sonicate to obtain mixed suspension B. S3: Under stirring conditions, the mixed suspension B obtained in step S2 is slowly added dropwise to the mixed suspension A obtained in step S1. After the addition is completed, stirring is continued for 1-3 hours. Then, the mixture is filtered, washed, and dried to obtain the composite powder. S4: The composite powder obtained in step S3 is subjected to cold isostatic pressing at a pressure of 150-300MPa for 5-15 minutes to obtain a green blank. S5: After degreasing the green blank obtained in step S4, place it in a hot pressing sintering furnace and perform two-stage hot pressing sintering in an atmosphere with an oxygen volume concentration of ≥90%. After sintering, cool it to room temperature with the furnace to obtain the target ITO target material.
[0007] Preferably, the raw materials in steps S1 and S2, by weight, include: 85-95 parts indium oxide, 5-10 parts tin oxide, 1-3 parts doping agent, and 0.15-0.5 parts composite sintering aid; the indium oxide and tin oxide are both micron-sized powders with an average particle size D50 of 1-10 μm; the doping agent and composite sintering aid are both nano-sized powders with an average particle size D50 of 20-100 nm.
[0008] Preferably, the doping aid is composed of tungsten oxide and titanium oxide in a mass ratio of (1-3):1; the composite sintering aid is composed of copper oxide and boron oxide in a mass ratio of (8-10):1.
[0009] Preferably, the anionic polyelectrolyte is sodium polyacrylate, sodium polystyrene sulfonate, or sodium carboxymethyl cellulose, and its addition amount is 0.5-2% of the total mass of the dopant and composite sintering aid.
[0010] Preferably, in step S3, the volume ratio of the mixed suspension A to the mixed suspension B is (2~3):1; the mixed suspension B is added dropwise at a uniform rate over 2-5 hours.
[0011] Preferably, in step S4, before cold isostatic pressing, the composite powder is pre-pressed at 20-40 MPa.
[0012] Preferably, in step S5, the degreasing treatment is carried out in an oxygen atmosphere with an oxygen flow rate of 0.5-1.5 L / min, a heating rate of 1-2 °C / min, a degreasing temperature of 550-600 °C, and a holding time of 3-4 h.
[0013] Preferably, the two-stage hot pressing sintering process is as follows: First stage: heating to 1420-1500℃ at a rate of 5-10℃ / min, applying an axial pressure of 10-20MPa, and holding for 1-2 hours; Second stage: cooling to 1220-1320℃ at a rate of 2-5℃ / min, while simultaneously increasing the axial pressure to 30-50MPa, and holding for 2-4 hours.
[0014] Preferably, in step S5, the hot pressing sintering furnace is a vacuum hot pressing furnace. After the degreased green body is placed in, a vacuum is first drawn to 10. -2 If the pressure drops below 0.5 Pa, refill with oxygen to atmospheric pressure and maintain a dynamic oxygen flow rate of 0.5-2 L / min.
[0015] The present invention also provides an ITO target prepared by the above-described method for preparing low-resistivity, high-density ITO target.
[0016] Compared with the prior art, the beneficial effects of the present invention are: 1) This invention uses micron-sized indium oxide and tin oxide as the matrix, combined with nano-sized tungsten oxide and titanium oxide as doping agents, forming a highly efficient synergistic effect. Compared with the conductivity fluctuations caused by single doping or uneven solid-phase mixing in existing technologies, the nano-doping agents of this invention can uniformly diffuse into the crystal lattice during sintering, effectively increasing the carrier concentration and reducing grain boundary scattering, thus stabilizing the target material resistivity at ≤3.0×10⁻⁶. -5 The Ω·cm is more than an order of magnitude lower than that of traditional ITO targets.
[0017] 2) This invention employs a composite sintering aid formed by the combination of copper oxide and boron oxide, which work synergistically. B2O3 forms a glassy phase at low temperatures to wet the particle surface, while CuO and In2O3 form a low-temperature eutectic liquid phase, effectively reducing the sintering activation energy of the powder and promoting interparticle diffusion and grain boundary bonding, thereby significantly lowering the sintering temperature and increasing the densification rate. Combined with electrostatic self-assembly technology, the aid is uniformly distributed among the particle gaps. In a two-stage hot-pressing sintering process: the first stage achieves rapid densification at high temperature and low pressure, while the second stage eliminates closed pores and inhibits grain growth at low temperature and high pressure. The final target material has a relative density ≥99.9%, solving the problems of high porosity and insufficient densification in traditional ITO targets.
[0018] 3) This invention achieves a target material with a relative density ≥99.7% and resistivity ≤2.9×10⁻⁶ by precisely proportioning and uniformly combining the matrix, doping agent, and composite sintering aid. -5While achieving a strength of Ω·cm, the three-point bending strength is ≥240MPa, realizing a simultaneous improvement in conductivity, density, and mechanical strength, which can meet the stringent requirements of high-power magnetron sputtering coating for the comprehensive performance of the target material. Detailed Implementation
[0019] The technical solution of the present invention will be further described below with reference to specific embodiments, but it is not limited thereto.
[0020] Example 1 A method for preparing a low-resistivity, high-density ITO target includes the following steps: S1: Mix 85 kg of indium oxide and 10 kg of tin oxide powder, disperse them in deionized water to make a suspension with a solid content of 20 wt%, and adjust the pH to 3 with dilute hydrochloric acid to obtain mixed suspension A; the indium oxide and tin oxide are both micron-sized powders with an average particle size D50 of 10 μm.
[0021] S2: Disperse 1 kg of doping agent and 0.15 kg of composite sintering aid in deionized water containing anionic polyelectrolyte to prepare a suspension with a solid content of 5%, and sonicate to obtain mixed suspension B; the doping agent and composite sintering aid are both nano-sized powders with an average particle size D50 of 20 nm; the doping agent is composed of tungsten oxide and titanium oxide in a mass ratio of 1:1; the composite sintering aid is composed of copper oxide and boron oxide in a mass ratio of 8:1; the anionic polyelectrolyte is sodium polyacrylate, and its addition amount is 0.5% of the total mass of the doping agent and composite sintering aid.
[0022] S3: Under stirring conditions, the mixed suspension B obtained in step S2 is slowly added dropwise to the mixed suspension A obtained in step S1. After the addition is completed, stirring is continued for 1 hour. Then, the mixture is filtered, washed, and dried to obtain the composite powder. The volume ratio of mixed suspension A to mixed suspension B is 2:1. The mixed suspension B is added dropwise at a uniform rate within 2 hours.
[0023] S4: First, the composite powder obtained in step S3 is pre-pressed at 20MPa, and then cold isostatic pressing is performed at 300MPa for 5 minutes to obtain the green blank.
[0024] S5: Degrease the green blank obtained in step S4. Specifically, the process is carried out in an oxygen atmosphere with an oxygen flow rate of 0.5 L / min, a heating rate of 1℃ / min, a degreasing temperature of 600℃, and a holding time of 3h. After degreasing, the degreased blank is placed in a vacuum hot press furnace, and then a vacuum is first drawn to 10. -2Below Pa, oxygen is refilled to atmospheric pressure, and the oxygen dynamic flow rate is maintained at 0.5 L / min. Two-stage hot pressing sintering is carried out in an atmosphere with an oxygen volume concentration of ≥90%. The specific process is as follows: First stage: the temperature is raised to 1420℃ at a rate of 5℃ / min, an axial pressure of 10MPa is applied, and the temperature is held for 1 hour; Second stage: the temperature is lowered to 1220℃ at a rate of 2℃ / min, while the axial pressure is increased to 30MPa, and the temperature is held for 2 hours; After sintering, the furnace is cooled to room temperature to obtain the target ITO target material.
[0025] Example 2 A method for preparing a low-resistivity, high-density ITO target includes the following steps: S1: Mix 90 kg of indium oxide and 8 kg of tin oxide powder, disperse them in deionized water to make a suspension with a solid content of 30 wt%, and adjust the pH to 4 with dilute hydrochloric acid to obtain mixed suspension A; the indium oxide and tin oxide are both micron-sized powders with an average particle size D50 of 5 μm.
[0026] S2: Disperse 2 kg of doping agent and 0.3 kg of composite sintering aid in deionized water containing anionic polyelectrolyte to prepare a suspension with a solid content of 10%, and sonicate to obtain mixed suspension B; the doping agent and composite sintering aid are both nano-sized powders with an average particle size D50 of 60 nm; the doping agent is composed of tungsten oxide and titanium oxide in a mass ratio of 2:1; the composite sintering aid is composed of copper oxide and boron oxide in a mass ratio of 9:1; the anionic polyelectrolyte is sodium polystyrene sulfonate, and its addition amount is 1.5% of the total mass of the doping agent and composite sintering aid.
[0027] S3: Under stirring conditions, the mixed suspension B obtained in step S2 is slowly added dropwise to the mixed suspension A obtained in step S1. After the addition is completed, stirring is continued for 2 hours. Then, the mixture is filtered, washed, and dried to obtain the composite powder. The volume ratio of mixed suspension A to mixed suspension B is 2.5:1. The mixed suspension B is added dropwise at a uniform rate within 4 hours.
[0028] S4: First, the composite powder obtained in step S3 is pre-pressed at 30MPa, and then cold isostatic pressing is performed at 250MPa for 10 minutes to obtain the green blank.
[0029] S5: Degrease the green blank obtained in step S4. Specifically, the process is carried out in an oxygen atmosphere with an oxygen flow rate of 1.0 L / min, a heating rate of 1.5 °C / min, a degreasing temperature of 580 °C, and a holding time of 3 h. After degreasing, the degreased blank is placed in a vacuum hot press furnace, and then a vacuum is first drawn to 10. -2Below Pa, oxygen is refilled to atmospheric pressure, and the oxygen dynamic flow rate is maintained at 1 L / min. Two-stage hot pressing sintering is carried out in an atmosphere with an oxygen volume concentration of ≥90%. The specific process is as follows: First stage: the temperature is raised to 1480℃ at a rate of 8℃ / min, an axial pressure of 15MPa is applied, and the temperature is held for 2 hours; Second stage: the temperature is lowered to 1300℃ at a rate of 4℃ / min, while the axial pressure is increased to 40MPa, and the temperature is held for 3 hours; After sintering, the furnace is cooled to room temperature to obtain the target ITO target material.
[0030] Example 3 A method for preparing a low-resistivity, high-density ITO target includes the following steps: S1: Mix 95 kg of indium oxide and 5 kg of tin oxide powder, disperse them in deionized water to make a suspension with a solid content of 40 wt%, and adjust the pH to 5 with dilute hydrochloric acid to obtain mixed suspension A; the indium oxide and tin oxide are both micron-sized powders with an average particle size D50 of 1 μm.
[0031] S2: Disperse 3 kg of doping agent and 0.5 kg of composite sintering aid in deionized water containing anionic polyelectrolyte to prepare a suspension with a solid content of 15%, and sonicate to obtain mixed suspension B; the doping agent and composite sintering aid are both nano-sized powders with an average particle size D50 of 100 nm; the doping agent is composed of tungsten oxide and titanium oxide in a mass ratio of 3:1; the composite sintering aid is composed of copper oxide and boron oxide in a mass ratio of 10:1; the anionic polyelectrolyte is sodium carboxymethyl cellulose, and its addition amount is 2% of the total mass of the doping agent and composite sintering aid.
[0032] S3: Under stirring conditions, the mixed suspension B obtained in step S2 is slowly added dropwise to the mixed suspension A obtained in step S1. After the addition is completed, stirring is continued for 3 hours. Then, the mixture is filtered, washed, and dried to obtain the composite powder. The volume ratio of mixed suspension A to mixed suspension B is 3:1. The mixed suspension B is added dropwise at a uniform rate within 5 hours.
[0033] S4: First, the composite powder obtained in step S3 is pre-pressed at 40MPa, and then cold isostatic pressing is performed at 300MPa for 15 minutes to obtain the green blank.
[0034] S5: Degrease the green blank obtained in step S4. Specifically, the process is carried out in an oxygen atmosphere with an oxygen flow rate of 1.5 L / min, a heating rate of 2 °C / min, a degreasing temperature of 550 °C, and a holding time of 4 h. After degreasing, the degreased blank is placed in a vacuum hot press furnace, and then a vacuum is first drawn to 10. -2Below Pa, oxygen is refilled to atmospheric pressure, and the oxygen dynamic flow rate is maintained at 2L / min. Two-stage hot pressing sintering is carried out in an atmosphere with an oxygen volume concentration of ≥90%. The specific process is as follows: First stage: the temperature is raised to 1500℃ at a rate of 10℃ / min, an axial pressure of 20MPa is applied, and the temperature is held for 1 hour; Second stage: the temperature is lowered to 1320℃ at a rate of 5℃ / min, while the axial pressure is increased to 50MPa, and the temperature is held for 2 hours; After sintering, the furnace is cooled to room temperature to obtain the target ITO target material.
[0035] Comparative Example 1 A conventional ITO target material has the following raw material composition: indium oxide: 90 kg (micron-sized powder, average particle size D50 = 5 μm), tin oxide: 8 kg (micron-sized powder, average particle size D50 = 5 μm), and antimony trioxide (Sb₂O₃): 2.5 kg (approximately 2.55% of the total mass of the matrix material). Unlike Example 2, this material does not contain any doping aids; instead, antimony trioxide is used as a sintering aid instead of the composite sintering aid.
[0036] The specific preparation method is as follows: (1) Place indium oxide, tin oxide and antimony trioxide powder in a planetary ball mill, add anhydrous ethanol as the dispersion medium, use zirconia balls as grinding balls, the ball-to-material mass ratio is 2:1, the rotation speed is 250 rpm, and the ball milling is carried out for 24 hours.
[0037] (2) The ball-milled slurry was dried at 80°C for 12 hours and passed through a 200-mesh sieve to obtain a mixed powder.
[0038] (3) The mixed powder is pre-molded under a pressure of 30 MPa; then it is cold isostatically pressed at a pressure of 300 MPa for 15 minutes to obtain the green blank.
[0039] (4) The green blank obtained in step (3) is degreased. Specifically, it is carried out in an oxygen atmosphere with an oxygen flow rate of 1.5 L / min, a heating rate of 2℃ / min, a degreasing temperature of 550℃, and a holding time of 4h. After degreasing, the degreased blank is placed in a vacuum hot press furnace, and then a vacuum is first drawn to 10. -2 Below Pa, oxygen is refilled to atmospheric pressure, and the oxygen dynamic flow rate is maintained at 2L / min. Two-stage hot pressing sintering is carried out in an atmosphere with an oxygen volume concentration of ≥90%. The specific process is as follows: First stage: the temperature is raised to 1500℃ at a rate of 10℃ / min, an axial pressure of 20MPa is applied, and the temperature is held for 1 hour; Second stage: the temperature is lowered to 1320℃ at a rate of 5℃ / min, while the axial pressure is increased to 50MPa, and the temperature is held for 2 hours; After sintering, the furnace is cooled to room temperature to obtain the target ITO target material.
[0040] Comparative Example 2 A low-resistance, high-density ITO target material is prepared in a manner similar to that of Example 2, except that only a composite sintering aid is used in step S2, and no doping aid is used.
[0041] Comparative Example 3 A low-resistivity, high-density ITO target material is prepared in a manner similar to that of Example 2, except that antimony trioxide is used instead of the composite sintering aid of the present invention in step S2.
[0042] Comparative Example 4 A low-resistance, high-density ITO target material is prepared in a manner similar to that of Example 2, except that the composite sintering aid in step S2 is only copper oxide.
[0043] Comparative Example 5 A low-resistance, high-density ITO target material is prepared in a manner similar to that of Example 2, except that the composite sintering aid in step S2 is only boron oxide.
[0044] Comparative Example 6 A low-resistivity, high-density ITO target material is prepared in a manner similar to that in Example 2, except that the mass ratio of copper oxide to boron oxide in the composite sintering aid in step S2 is 6:1.
[0045] Comparative Example 7 A low-resistivity, high-density ITO target material is prepared in a manner similar to that of Example 2, except that the mass ratio of copper oxide to boron oxide in the composite sintering aid in step S2 is 11:1.
[0046] Comparative Example 8 A low-resistance, high-density ITO target is prepared in a manner similar to that of Example 2, except that the doping agent in step S2 is tungsten oxide.
[0047] Comparative Example 9 A low-resistance, high-density ITO target is prepared in a manner similar to that of Example 2, except that the doping agent in step S2 is titanium oxide.
[0048] Comparative Example 10 A low-resistance, high-density ITO target is prepared in a manner similar to that of Example 2, except that the doping agent in step S2 is composed of tungsten oxide and titanium oxide in a mass ratio of 0.8:1.
[0049] Comparative Example 11 A low-resistance, high-density ITO target is prepared in a manner similar to that of Example 2, except that the doping agent in step S2 is composed of tungsten oxide and titanium oxide in a mass ratio of 3.5:1.
[0050] Performance testing The relative density, resistivity, and three-point bending strength of the ITO targets prepared in Examples 1-3 and Comparative Examples 1-11 were tested, and the results are shown in Table 1.
[0051] Table 1 Performance Test Results
[0052] As can be seen from the results in Table 1 above, the relative density of Examples 1-3 all exceeded 99.7%, and the resistivity was stable at 2.2~2.9×10⁻⁶. -5 Within the Ω·cm range, the flexural strength at all three points exceeded 240 MPa, significantly better than that of the comparative examples. The results of Comparative Examples 1-3 show that the resistivity of the target material obtained in Comparative Example 1, using a conventional antimony trioxide sintering agent, reached as high as 12.5 × 10⁻⁶ MPa. -4 The resistivity of Comparative Example 2 and Comparative Example 3 is 8.5 × 10 Ω·cm. -5 Ω·cm and 92×10 -5 The resistivity of the composite sintering aid, measured in Ω·cm, is significantly higher than that of Example 2. This indicates a substantial synergistic effect between the doping agent and the composite sintering aid of this invention. Both are indispensable; neither component alone can achieve the dual breakthrough of low resistivity and high density. Comparative Examples 4-7 further confirm that CuO and B2O3 in the composite sintering aid used in this invention must be used in a specific ratio range to achieve the best synergistic effect, ensuring both density and conductivity and strength. The resistivity of Comparative Example 8 is higher than that of Example 2, indicating that the lack of Ti-optimized mobility leads to performance degradation. The resistivity of Comparative Example 9 is as high as 7.2 × 10⁻⁶. -5 The resistivity was much higher than that of Example 2, indicating that the lack of W provided a high carrier concentration. The results of Comparative Examples 10 and 11 showed that the resistivity increased significantly when the W:Ti ratio deviated from the range of the present invention. This also shows that the two components in the doping agent used in the present invention must be used synergistically within a specific ratio range in order to achieve both high carrier concentration and high mobility, and thus the lowest resistivity.
[0053] It should be noted that the above embodiments are merely some preferred embodiments of the present invention, and not all embodiments. Obviously, based on the above embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of the present invention.
Claims
1. A method for preparing a low-resistivity, high-density ITO target, characterized in that, Includes the following steps: S1: After mixing the raw materials indium oxide and tin oxide powder in a certain proportion, disperse them in deionized water to prepare a suspension with a solid content of 20-40wt%. Adjust the pH to 3-5 with dilute hydrochloric acid to obtain mixed suspension A. S2: Disperse the dopant and composite sintering aid in deionized water containing anionic polyelectrolyte to prepare a suspension with a solid content of 5-15%, and sonicate to obtain mixed suspension B. S3: Under stirring conditions, the mixed suspension B obtained in step S2 is slowly added dropwise to the mixed suspension A obtained in step S1. After the addition is completed, stirring is continued for 1-3 hours. Then, the mixture is filtered, washed, and dried to obtain the composite powder. S4: The composite powder obtained in step S3 is subjected to cold isostatic pressing at a pressure of 150-300MPa for 5-15 minutes to obtain a green blank. S5: After degreasing the green blank obtained in step S4, place it in a hot pressing sintering furnace and perform two-stage hot pressing sintering in an atmosphere with an oxygen volume concentration of ≥90%. After sintering, cool it to room temperature with the furnace to obtain the target ITO target material.
2. The method for preparing the low-resistivity, high-density ITO target material according to claim 1, characterized in that, The raw materials in steps S1 and S2, by weight, include: 85-95 parts indium oxide, 5-10 parts tin oxide, 1-3 parts doping agent, and 0.15-0.5 parts composite sintering aid; the indium oxide and tin oxide are both micron-sized powders with an average particle size D50 of 1-10 μm; the doping agent and composite sintering aid are both nano-sized powders with an average particle size D50 of 20-100 nm.
3. The method for preparing the low-resistivity, high-density ITO target material according to claim 2, characterized in that, The doping aid is composed of tungsten oxide and titanium oxide in a mass ratio of (1-3):1; the composite sintering aid is composed of copper oxide and boron oxide in a mass ratio of (8-10):
1.
4. The method for preparing the low-resistivity, high-density ITO target material according to claim 1, characterized in that, The anionic polyelectrolyte is sodium polyacrylate, sodium polystyrene sulfonate, or sodium carboxymethyl cellulose, and its addition amount is 0.5-2% of the total mass of the dopant and composite sintering aid.
5. The method for preparing the low-resistivity, high-density ITO target material according to claim 1, characterized in that, In step S3, the volume ratio of the mixed suspension A to the mixed suspension B is (2~3):1; the mixed suspension B is added dropwise at a uniform rate over 2-5 hours.
6. The method for preparing the low-resistivity, high-density ITO target material according to claim 1, characterized in that, In step S4, before cold isostatic pressing, the composite powder is pre-pressed at 20-40 MPa.
7. The method for preparing the low-resistivity, high-density ITO target material according to claim 1, characterized in that, In step S5, the degreasing treatment is carried out in an oxygen atmosphere with an oxygen flow rate of 0.5-1.5 L / min, a heating rate of 1-2 °C / min, a degreasing temperature of 550-600 °C, and a holding time of 3-4 h.
8. The method for preparing the low-resistivity, high-density ITO target material according to claim 1, characterized in that, The two-stage hot pressing sintering process is as follows: First stage: heat up to 1420-1500℃ at a rate of 5-10℃ / min, apply axial pressure of 10-20MPa, and hold for 1-2 hours. Second stage: Cool down to 1220-1320℃ at a rate of 2-5℃ / min, while increasing the axial pressure to 30-50MPa, and hold for 2-4 hours.
9. The method for preparing the low-resistivity, high-density ITO target material according to claim 1, characterized in that, In step S5, the hot pressing sintering furnace is a vacuum hot pressing furnace. After the degreased green body is placed in, a vacuum is first drawn to 10. -2 If the pressure drops below 0.5 Pa, refill with oxygen to atmospheric pressure and maintain a dynamic oxygen flow rate of 0.5-2 L / min.
10. The ITO target prepared by the method for preparing low-resistivity, high-density ITO target as described in any one of claims 1-9.
Citation Information
Patent Citations
Gallium-cerium co-doped ITO target material and preparation method thereof
CN121494528A