High-mobility indium germanium zirconium titanium oxide target material and preparation method thereof

Abstract

The invention belongs to the technical field of target material preparation, and discloses a high-mobility indium germanium zirconium titanium oxide target material and a preparation method thereof. The preparation method comprises the following steps: mixing In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder according to a specific ratio, carrying out ball milling and granulation on the mixed powder to obtain mixed oxide powder, then sequentially carrying out die forming and cold isostatic pressing forming on the mixed oxide powder to obtain a target material green body, and sintering the green body in an oxygen atmosphere. The indium germanium zirconium titanium oxide target material with high mobility, low resistivity and high density can be prepared by accurately regulating and controlling the doping proportion of GeO2, ZrO2 and TiO2 and the sintering temperature. The target material has no impurity phase, is high in density and has important industrial application value.

Description

Technical Field

[0001] This invention belongs to the field of target material preparation technology, specifically relating to a high-mobility indium germanium zirconium titanium oxide target and its preparation method. Background Technology

[0002] Transparent conductive oxide (TCO) thin films are a class of inorganic thin-film materials that combine electrical conductivity and light transmittance, and are widely used in optoelectronic devices such as flat panel displays, solar cells, light-emitting devices, and touch panels. TCO thin films are typically prepared using magnetron sputtering technology, which offers advantages such as dense film layers, strong adhesion, uniform thickness, and suitability for large-area coating, making it highly applicable in industrial production. High-quality TCO thin films must simultaneously possess high mobility and low resistivity. Mobility relates to carrier transport efficiency, while resistivity affects conductivity. As the performance requirements of optoelectronic devices increase, TCO thin films are developing towards higher mobility and lower energy consumption, placing higher demands on their core target materials.

[0003] Currently, the most widely used TCO thin film material is indium tin oxide (ITO). ITO thin films exhibit high transmittance and low resistivity in the visible light band, meeting the requirements of most traditional optoelectronic devices. The high relative density of the ITO target ensures the compactness and uniformity of the material structure, thereby guaranteeing the continuity of the charge carrier channels and the stability of the film deposition. As applications expand from traditional displays to fields with higher performance requirements, existing ITO materials, due to their relatively low mobility, are no longer sufficient to meet the comprehensive performance requirements of TCO thin films in terms of conductivity and transmittance, limiting further improvements in their overall performance.

[0004] To address the aforementioned issues, co-doping with multiple oxides has become an effective means of improving target mobility. By controlling carrier concentration and improving crystal structure, electron scattering can be significantly reduced, and mobility and density can be increased.

[0005] Chinese patent application No. 202210174352.3, entitled "A Ceramic Target for Solar Cells and Its Preparation Method," discloses a ceramic target composed of indium oxide as the main component and various oxides such as yttrium oxide, gallium oxide, and cerium oxide. The TCO thin film prepared using this target achieves a mobility of 48.35–66.32 cm⁻¹. 2 / V·s.

[0006] Chinese Patent Application No. 202211462828.X, entitled "Preparation of a Low-Resistivity, High-Mobility Oxide Target Material," discloses a low-resistivity, high-mobility oxide target material and its preparation method. The metal oxide in the target material blank is composed of praseodymium oxide, indium oxide, gallium oxide, and zinc oxide. The mobility of this target material reaches 30.8–34.3 cm⁻¹. 2 / V·s.

[0007] In summary, it is evident that the formulation and preparation method significantly affect the migration rate of TCO films. Therefore, the technical problem to be solved in this case is to maximize the migration rate of the target material by optimizing the target formulation and preparation method. Summary of the Invention

[0008] The purpose of this invention is to provide a method for preparing high-mobility indium germanium zirconium titanium oxide (INO) targets. By introducing GeO2, ZrO2, and TiO2 into the In2O3 system and optimizing the doping ratio and sintering conditions, the method utilizes the effects of GeO2 in widening the bandgap, improving near-infrared transmittance, and promoting liquid-phase sintering. Combined with the advantages of Zr and Ti transition elements in reducing the effective mass of charge carriers and scattering ionized impurities, the method achieves synergistic optimization of charge carrier concentration and crystal structure, thereby significantly improving the mobility and density of the target material and reducing resistivity.

[0009] The present invention also aims to provide a high-mobility indium germanium zirconium titanium oxide target material prepared by the above method, which has high mobility, low resistivity and high density, and is free of impurity phases and secondary phase structures.

[0010] This invention provides a method for preparing a high-mobility indium germanium zirconium titanium oxide target, the method comprising the following steps:

[0011] a. Mix In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder to obtain a mixed powder;

[0012] b. The mixed powder is mixed with a dispersant, a binder and deionized water, and then ball-milled to obtain a mixed slurry;

[0013] c. After drying the mixed slurry, grind and disperse it, and then sieve it to obtain mixed oxide powder;

[0014] d. The mixed oxide powder is sequentially subjected to compression molding and cold isostatic pressing to obtain a target green body;

[0015] e. The target green is sintered in an oxygen atmosphere to obtain the high-mobility indium germanium zirconium titanium target.

[0016] In step a of the above preparation method, the molar ratio of In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder in the mixed powder is 100:1~2:0.5~1.5:0~0.5.

[0017] In step a of the above preparation method, the purity of In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder in the mixed powder is greater than 99.9%, and the powder particle size is D50 = 0.1~0.7μm and D90 = 0.7~1.9μm.

[0018] In step b of the above preparation method, the mass of the dispersant is 0.3% to 0.5% of the mass of the mixed powder, and the dispersant is one of polyvinylpyrrolidone (K29-32) or sodium hexadecylbenzenesulfonate.

[0019] In step b of the above preparation method, the mass of the binder is 5.0% to 8.0% of the mass of the mixed powder, and the binder is one or more of polyvinyl alcohol (weight average molecular weight Mw 85000 to 124000) or polyvinyl butyral (weight average molecular weight Mw 70,000 to 100,000).

[0020] In step b of the above preparation method, the mass concentration of the mixed powder in the mixed slurry is 0.72-0.84 g / ml.

[0021] In step b of the above preparation method, the ball milling speed is 230-280 r / min and the ball milling time is 5-8 h.

[0022] In step c of the above preparation method, the sieving includes coarse sieving and fine sieving. The coarse sieving uses a sieve with a mesh size of 20 to 60, and the fine sieving uses a sieve with a mesh size of 80 to 120.

[0023] In step d of the above preparation method, the molding pressure is 5-10 MPa and the pressing time is 40-90 s.

[0024] In step d of the above preparation method, the pressure of the cold isostatic pressing is 250-280 MPa, and the pressing time is 30-90 s.

[0025] In step e of the above preparation method, the sintering process specifically includes the following steps: (1) first, the sintering furnace is evacuated to a vacuum degree ≤10-1Pa, and then oxygen is introduced to the standard atmospheric pressure; (2) the temperature is raised to 300-700℃ at a heating rate of 1-2℃ / min and held for 1-4h to perform degreasing treatment; (3) the temperature is raised to the sintering temperature at a heating rate of 1-3℃ / min, the sintering temperature is 1400-1600℃, and after reaching the sintering temperature, the holding time is 1-3h; (4) the temperature is lowered to 1350-1550℃ at a cooling rate of 1-3℃ / min, and held at this temperature for 2-5h; (5) the temperature is lowered to 300℃ at a cooling rate of 1-5℃ / min and then cooled with the furnace, and the oxygen is turned off when the temperature drops below 200℃, thus obtaining the high-mobility indium germanium zirconium titanium target.

[0026] This invention provides a high-mobility indium germanium zirconium titanium oxide target material prepared using the above-described method, with a relative density of 97.82%–98.92% and a mobility of 87.89–115.4 cm⁻¹.2 / V·s, the bulk carrier concentration is 2.07×10 20 ~3.85×10 20 / cm 3 The resistivity is 0.167 to 0.336 mΩ·cm, and the target material has uniform grain size with no secondary phase structure between or inside the grains.

[0027] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0028] 1. By introducing GeO2 into the In2O3 system, the band gap of In2O3 can be effectively widened, thereby improving the near-infrared transmittance. In addition, GeO2 has a relatively low melting point (1115℃), which can promote liquid phase sintering and significantly reduce the sintering temperature.

[0029] 2. The d orbitals of transition metals Zr and Ti have higher energy levels than the 5s orbitals of In, and possess multiple valence electrons. Furthermore, the orbital hybridization between the d orbitals of transition metals and the 5s orbitals of In is relatively weak under the symmetry of In₂O₃ crystals. This allows them to effectively reduce the effective mass m of charge carriers during carrier transport. e And ionized impurity scattering. Compared with traditional Sn doping, lower Zr and Ti doping concentrations are required to achieve the same carrier concentration, reducing the damage of impurities to the crystal structure.

[0030] 3. Through the synergistic effect of GeO2, ZrO2, and TiO2, the carrier concentration and distribution were optimized, the uniformity and density of the crystal structure were improved, and electron scattering was significantly reduced. The highest target mobility obtained in the final fabrication reached 115.4 cm⁻¹. 2 / V·s, with a resistivity as low as 0.167mΩ·cm, significantly better than traditional materials.

[0031] 4. By effectively controlling the doping ratio of GeO2, ZrO2 and TiO2 and the sintering temperature, the mobility and density of the target material are significantly improved, while the resistivity is reduced simultaneously. Moreover, the target material does not contain other impurity phase components, and there is no secondary phase structure between or inside the grains, which has high industrial application value. Attached Figure Description

[0032] Figure 1 Here is a SEM image of the high-mobility indium germanium zirconium titanium oxide target prepared in this invention, wherein... Figure 1 From middle a to Figure 1 The numbers 'e' in the image correspond to the SEM images of the targets obtained in Examples 1 to 5, respectively. Figure 1 From middle a to Figure 1 The microstructure of the target material shows that the grain size is uniform and no secondary phase structure is observed between or inside the grains. Detailed Implementation

[0033] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0034] Unless otherwise specified, all test materials and reagents used in the following examples are commercially available.

[0035] Unless otherwise specified in the embodiments, the techniques or conditions described in the literature in this field or in accordance with the product manual may be followed.

[0036] The purity of the In2O3, GeO2, ZrO2, and TiO2 powders used in this invention is greater than 99.9%, the particle size D50 is in the range of 0.1–0.7 μm, and the D90 is in the range of 0.7–1.9 μm. The mobility, resistivity, and bulk carrier concentration parameters of the high-mobility indium germanium zirconium titanium oxide target were characterized by a Hall effect tester (CH-70). During the test, the sample was tested at room temperature, and the resistivity was measured using the standard four-probe method. The carrier concentration and mobility were calculated by combining the Hall voltage signal.

[0037] Example 1

[0038] Preparation method of high-mobility indium germanium zirconium titanium oxide target:

[0039] a. Mix In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder in a molar ratio of 100:2:0.5:0.5 to obtain a mixed powder;

[0040] b. Mix the powder with 0.5 wt% polyvinylpyrrolidone (K29-32), 5.572 wt% polyvinyl alcohol (weight average molecular weight Mw 85000~124000) and 60 g of deionized water, and ball mill at 250 rpm for 6 h to obtain a mixed slurry.

[0041] c. After drying the mixed slurry, grind and disperse it, and pass it through 40 and 100 mesh sieves to obtain mixed oxide powder;

[0042] d. Weigh a certain mass of mixed oxide powder, place it in a Φ10 steel mold for molding, the molding pressure is 5MPa, the pressing time is 60s, and then perform cold isostatic pressing, the cold isostatic pressing pressure is 265MPa, the pressing time is 60s, to obtain the target green blank.

[0043] e. Place the target green in the sintering furnace. The sintering process of the target specifically includes: (1) first evacuating the sintering furnace to a vacuum degree ≤10. -1 Pa, then oxygen is introduced to standard atmospheric pressure; (2) the temperature is increased to 650°C at a heating rate of 1.5°C / min, and degreasing is performed for 2 hours; (3) the temperature is increased to sintering temperature at a heating rate of 2°C / min, the sintering temperature is 1520°C, and the holding time is 2 hours; (4) the temperature is decreased to 1470°C at a cooling rate of 2°C / min, and the holding time is 3 hours; (5) the temperature is decreased to 300°C at a cooling rate of 4°C / min and then cooled with the furnace. The oxygen is turned off when the temperature drops below 200°C, and the high-mobility indium germanium zirconium titanium target material of this embodiment is obtained.

[0044] The relative density of the high-mobility indium germanium zirconium titanium oxide target obtained in this embodiment was 98.73%, and the mobility was 115.4 cm⁻¹. 2 / V·s, the bulk carrier concentration is 3.04×10 20 / cm 3 Its resistivity is 0.178 mΩ·cm.

[0045] Example 2

[0046] Preparation method of high-mobility indium germanium zirconium titanium oxide target:

[0047] a. Mix In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder in a molar ratio of 100:1.5:1:0.5 to obtain a mixed powder;

[0048] b. The mixed powder is mixed with 0.5 wt% polyvinylpyrrolidone (K29-32) and 5.572 wt% polyvinyl alcohol (weight average molecular weight Mw 85000~124000), and ball-milled at a speed of 250 rpm for 6 h to obtain a mixed slurry.

[0049] c. After drying the mixed slurry, grind and disperse it, and pass it through 40 and 100 mesh sieves to obtain mixed oxide powder;

[0050] d. Weigh a certain mass of mixed oxide powder, place it in a Φ10 steel mold for molding, the molding pressure is 5MPa, the pressing time is 60s, and then perform cold isostatic pressing, the cold isostatic pressing pressure is 265MPa, the pressing time is 60s, to obtain the target green blank.

[0051] e. Place the target green in the sintering furnace. The sintering process of the target specifically includes: (1) first evacuating the sintering furnace to a vacuum degree ≤10. -1Pa, then oxygen is introduced to standard atmospheric pressure; (2) the temperature is increased to 650°C at a heating rate of 1.5°C / min, and degreasing is performed for 2 hours; (3) the temperature is increased to sintering temperature at a heating rate of 2°C / min, the sintering temperature is 1520°C, and the holding time is 2 hours; (4) the temperature is decreased to 1470°C at a cooling rate of 2°C / min, and the holding time is 3 hours; (5) the temperature is decreased to 300°C at a cooling rate of 4°C / min and then cooled with the furnace. The oxygen is turned off when the temperature drops below 200°C, and the high-mobility indium germanium zirconium titanium target material of this embodiment is obtained.

[0052] The relative density of the high-mobility indium germanium zirconium titanium oxide target obtained in this embodiment was 98.48%, and the mobility was 108 cm⁻¹. 2 / V·s, the bulk carrier concentration is 3.04×10 20 / cm 3 Its resistivity is 0.19 mΩ·cm.

[0053] Example 3

[0054] Preparation method of high-mobility indium germanium zirconium titanium oxide target:

[0055] a. Mix In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder in a molar ratio of 100:2:0.5:0 to obtain a mixed powder;

[0056] b. The mixed powder is mixed with 0.5 wt% polyvinylpyrrolidone (K29-32), 3 wt% polyvinyl alcohol (weight average molecular weight Mw 85000~124000), and 3 wt% polyvinyl butyral (weight average molecular weight Mw 70,000~100,000), and ball-milled at a speed of 250 rpm for 6 h to obtain a mixed slurry.

[0057] c. After drying the mixed slurry, grind and disperse it, and pass it through 40 and 100 mesh sieves to obtain mixed oxide powder;

[0058] d. Weigh a certain mass of mixed oxide powder, place it in a Φ10 steel mold for molding, the molding pressure is 5MPa, the pressing time is 60s, and then perform cold isostatic pressing, the cold isostatic pressing pressure is 265MPa, the pressing time is 60s, to obtain the target green blank.

[0059] e. Place the target green in the sintering furnace. The sintering process of the target specifically includes: (1) first evacuating the sintering furnace to a vacuum degree ≤10. -1Pa, then oxygen is introduced to standard atmospheric pressure; (2) the temperature is increased to 650°C at a heating rate of 1.5°C / min, and degreasing is performed for 2 hours; (3) the temperature is increased to sintering temperature at a heating rate of 2°C / min, the sintering temperature is 1520°C, and the holding time is 2 hours; (4) the temperature is decreased to 1470°C at a cooling rate of 2°C / min, and the holding time is 3 hours; (5) the temperature is decreased to 300°C at a cooling rate of 4°C / min and then cooled with the furnace. The oxygen is turned off when the temperature drops below 200°C, and the high-mobility indium germanium zirconium titanium target material of this embodiment is obtained.

[0060] The relative density of the high-mobility indium germanium zirconium titanium oxide target obtained in this embodiment was 98.42%, and the mobility was 98.05 cm⁻¹. 2 / V·s, the bulk carrier concentration is 2.27×10 20 / cm 3 Its resistivity is 0.281 mΩ·cm.

[0061] Example 4

[0062] Preparation method of high-mobility indium germanium zirconium titanium oxide target:

[0063] a. Mix In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder in a molar ratio of 100:1.5:1:0 to obtain a mixed powder;

[0064] b. The mixed powder was ball-milled with 0.5 wt% polyvinylpyrrolidone (K29-32) and 5.572 wt% polyvinyl butyral (weight average molecular weight Mw 70,000-100,000) at a ball mill speed of 250 rpm for 6 h to obtain a mixed slurry.

[0065] c. After drying the mixed slurry, grind and disperse it, and pass it through 40 and 100 mesh sieves to obtain mixed oxide powder;

[0066] d. Weigh a certain mass of mixed oxide powder, place it in a Φ10 steel mold for molding, the molding pressure is 5MPa, the pressing time is 60s, and then perform cold isostatic pressing, the cold isostatic pressing pressure is 265MPa, the pressing time is 60s, to obtain the target green blank.

[0067] e. Place the target green in the sintering furnace. The sintering process of the target specifically includes: (1) first evacuating the sintering furnace to a vacuum degree ≤10. -1Pa, then oxygen is introduced to standard atmospheric pressure; (2) the temperature is increased to 650°C at a heating rate of 1.5°C / min, and degreasing is performed, with a holding time of 2h; (3) the temperature is increased to sintering temperature at a heating rate of 2°C / min, the sintering temperature is 1490°C, and the holding time is 2h; (4) the temperature is decreased to 1440°C at a cooling rate of 2°C / min, and the holding time is 3h; (5) the temperature is decreased to 300°C at a cooling rate of 4°C / min and then cooled with the furnace, and the oxygen is turned off when the temperature drops below 200°C, thus obtaining the high-mobility indium germanium zirconium titanium target of this embodiment.

[0068] The relative density of the high-mobility indium germanium zirconium titanium oxide target obtained in this embodiment was 98.21%, and the mobility was 112.1 cm⁻¹. 2 / V·s, the bulk carrier concentration is 2.68×10 20 / cm 3 Its resistivity is 0.208 mΩ·cm.

[0069] Example 5

[0070] Preparation method of high-mobility indium germanium zirconium titanium oxide target:

[0071] a. Mix In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder in a molar ratio of 100:1:1.5:0 to obtain a mixed powder;

[0072] b. The mixed powder is mixed with 0.5 wt% sodium cetylbenzenesulfonate and 5.572 wt% polyvinyl alcohol (weight average molecular weight Mw 85000~124000) and ball-milled at a speed of 250 rpm for 6 h to obtain a mixed slurry.

[0073] c. After drying the mixed slurry, grind and disperse it, and pass it through 40 and 100 mesh sieves to obtain mixed oxide powder;

[0074] d. Weigh a certain mass of mixed oxide powder, place it in a Φ10 steel mold for molding, the molding pressure is 5MPa, the pressing time is 60s, and then perform cold isostatic pressing, the cold isostatic pressing pressure is 265MPa, the pressing time is 60s, to obtain the target green blank.

[0075] e. Place the target green in the sintering furnace. The sintering process of the target specifically includes: (1) first evacuating the sintering furnace to a vacuum degree ≤10. -1Pa, then oxygen is introduced to standard atmospheric pressure; (2) the temperature is increased to 650°C at a heating rate of 1.5°C / min, and degreasing is performed for 2 hours; (3) the temperature is increased to sintering temperature at a heating rate of 2°C / min, the sintering temperature is 1490°C, and the holding time is 2 hours; (4) the temperature is decreased to 1450°C at a cooling rate of 2°C / min, and the holding time is 3 hours; (5) the temperature is decreased to 300°C at a cooling rate of 4°C / min and then cooled with the furnace. The oxygen is turned off when the temperature drops below 200°C, and the high-mobility indium germanium zirconium titanium target of this embodiment is obtained.

[0076] The relative density of the high-mobility indium germanium zirconium titanium oxide target obtained in this embodiment was 98.39%, and the mobility was 99.84 cm⁻¹. 2 / V·s, the bulk carrier concentration is 3.39×10 20 / cm 3 Its resistivity is 0.185 mΩ·cm.

[0077] Example 6

[0078] Compared with Example 1, in this embodiment, the sintering temperature in step (3) is 1550℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1500℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0079] Example 7

[0080] Compared with Example 1, in this embodiment, the sintering temperature in step (3) is 1490℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1440℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0081] Example 8

[0082] Compared with Example 1, in this embodiment, the sintering temperature in step (3) is 1460℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1410℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0083] Example 9

[0084] Compared with Example 1, in this embodiment, the sintering temperature in step (3) is 1430℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1380℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0085] Example 10

[0086] Compared with Example 2, in this embodiment, the sintering temperature in step (3) is 1550℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1500℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0087] Example 11

[0088] Compared with Example 2, in this embodiment, the sintering temperature in step (3) is 1490℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1440℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0089] Example 12

[0090] Compared with Example 3, in this embodiment, the sintering temperature in step (3) is 1430℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1380℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0091] Example 13

[0092] Compared with Example 4, in this embodiment, the sintering temperature in step (3) is 1490℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1440℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0093] Example 14

[0094] Compared with Example 4, in this embodiment, the sintering temperature in step (3) is 1460℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1410℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0095] Example 15

[0096] Compared with Example 4, in this embodiment, the sintering temperature in step (3) is 1430℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1380℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0097] Example 16

[0098] Compared with Example 5, in this embodiment, the sintering temperature in step (3) is 1490℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1440℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0099] Example 17

[0100] Compared with Example 5, in this embodiment, the sintering temperature in step (3) is 1460℃ and the holding time is 2h. Then, in step (4), the temperature is reduced to 1410℃ at a cooling rate of 2℃ / min and the holding time is 3h. The rest are the same.

[0101] Comparative Example 1

[0102] Compared with Example 1, this comparative example uses In2O3 powder and TiO2 powder mixed at a mass ratio of 99.7wt%:0.3wt%, with the rest remaining the same.

[0103] Comparative Example 2

[0104] Compared with Example 1, this comparative example uses In2O3 powder and ZrO2 powder mixed at a mass ratio of 99.7wt%:0.3wt%, with the rest remaining the same.

[0105] Comparative Example 3

[0106] Compared with Example 1, this comparative example uses In2O3 powder and GeO2 powder mixed at a mass ratio of 99.7wt%:0.3wt%, with the rest remaining the same.

[0107] The performance test results show that, in Examples 1-5, the synergistic effect of each component promotes the preparation of germanium-zirconium-titanium targets with higher mobility and lower resistivity. Comparing Examples 1-5, Examples 1 and 4 exhibit superior overall performance, further demonstrating that adding appropriate amounts of transition elements (Zr and Ti) can improve the mobility and relative density of indium oxide targets while reducing their resistivity.

[0108] A comparison of Examples 6, 7, 8, 9 and Example 1, Examples 10, 11 and Example 2, Examples 12 and Example 3, Examples 13, 14, 15 and Example 4, Examples 16, 17 and Example 5 shows that sintering temperature affects the mobility, resistivity and relative density of the target material. Therefore, by controlling the sintering temperature and adjusting the parameters of the target material, the applicability of indium germanium zirconium titanium oxide targets can be greatly expanded.

[0109] Table 1: Performance of the target materials prepared in Examples 1-5 and Comparative Examples 1-20

[0110]

[0111] The above description of the embodiments is intended to enable those skilled in the art to understand and use the invention. It will be apparent to those skilled in the art that various modifications can be made to these embodiments, and the general principles described herein can be applied to other embodiments without inventive effort. Therefore, the present invention is not limited to the above embodiments, and any improvements and modifications made by those skilled in the art based on the disclosure of the present invention without departing from the scope of the invention should be within the protection scope of the present invention.

Claims

1. A method for preparing a high-mobility indium germanium zirconium titanium oxide target, characterized in that, The preparation method includes the following steps: a. Mix In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder to obtain a mixed powder; b. The mixed powder is mixed with a dispersant, a binder and deionized water, and then ball-milled to obtain a mixed slurry; c. After drying the mixed slurry, grind and disperse it, and then sieve it to obtain mixed oxide powder; d. The mixed oxide powder is sequentially subjected to compression molding and cold isostatic pressing to obtain a target green body; e. The target green is sintered in an oxygen atmosphere to obtain the high-mobility indium germanium zirconium titanium target.

2. The method for preparing the high-mobility indium germanium zirconium titanium oxide target according to claim 1, characterized in that, The molar ratio of In2O3 powder, GeO2 powder, ZrO2 powder and TiO2 powder in the mixed powder is 100:1~2:0.5~1.5:0~0.5, and the mass concentration of the mixed powder in the mixed slurry is 0.72-0.84 g / ml.

3. The method for preparing the high-mobility indium germanium zirconium titanium oxide target according to claim 1, characterized in that, The mass of the dispersant is 0.3% to 0.5% of the mass of the mixed powder, and the dispersant is one of polyvinylpyrrolidone (K29 to K32) or sodium hexadecylbenzenesulfonate.

4. The method for preparing the high-mobility indium germanium zirconium titanium oxide target according to claim 1, characterized in that, The binder accounts for 5.0% to 8.0% of the mass of the mixed powder, and the binder is one or more of polyvinyl alcohol with a weight average molecular weight of 70,000 to 100,000 or polyvinyl butyral.

5. The method for preparing the high-mobility indium germanium zirconium titanium oxide target according to claim 1, characterized in that, The ball milling speed is 230-280 r / min, and the ball milling time is 5-8 h.

6. The method for preparing the high-mobility indium germanium zirconium titanium oxide target according to claim 1, characterized in that, The sieving process includes a coarse sieve and a fine sieve. The coarse sieve uses a screen with a mesh size of 20 to 60, and the fine sieve uses a screen with a mesh size of 80 to 120.

7. The method for preparing the high-mobility indium germanium zirconium titanium oxide target according to claim 1, characterized in that, The molding pressure is 5-10 MPa, and the pressing time is 40-90 s.

8. The method for preparing the high-mobility indium germanium zirconium titanium oxide target according to claim 1, characterized in that, The pressure for cold isostatic pressing is 250–280 MPa, and the pressing time is 30–90 s.

9. The method for preparing the high-mobility indium germanium zirconium titanium oxide target according to claim 1, characterized in that, The sintering process specifically includes the following steps: (1) First, the sintering furnace is evacuated to a vacuum degree ≤10. -1 Pa, then oxygen is introduced to standard atmospheric pressure; (2) the temperature is raised to 300-700℃ at a heating rate of 1-2℃ / min and held for 1-4h for degreasing treatment; (3) the temperature is raised to sintering temperature at a heating rate of 1-3℃ / min, the sintering temperature is 1400-1600℃, and after reaching the sintering temperature, the holding time is 1-3h; (4) the temperature is lowered to 1350-1550℃ at a cooling rate of 1-3℃ / min, and held at this temperature for 2-5h; (5) the temperature is lowered to 300℃ at a cooling rate of 1-5℃ / min and then cooled with the furnace, and the oxygen is turned off when the temperature drops below 200℃, thus obtaining high-mobility indium germanium zirconium titanium oxide target material.

10. A high-mobility indium germanium zirconium titanium oxide target material prepared by any one of claims 1-9, characterized in that, The high-mobility indium germanium zirconium titanium oxide target has uniform grain size, with no secondary phase structure between or within the grains, a relative density of 97.82%–98.92%, and a mobility of 87.89–115.4 cm⁻¹. 2 / V·s, the bulk carrier concentration is 2.07×10 20 ~3.85×10 20 / cm 3 Its resistivity is 0.167–0.336 mΩ·cm.

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