Indium gallium zinc oxide target material and preparation method and application thereof
By combining indium oxide, zinc oxide, gallium oxide and antimony pentoxide, the problem of high-temperature sintering of IGZO targets was solved, the preparation of low-cost and high-quality targets was achieved, and the stability and uniformity of the materials were improved.
Patent Information
- Application Number
- CN202510830887.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-20
- Publication Date
- 2025-10-17
AI Technical Summary
In the existing technology, the preparation of IGZO targets requires ultra-high temperature and long-term sintering, which leads to high costs. In addition, indium and zinc are easily volatile at high temperatures, affecting the target composition, making it difficult to prepare high-quality IGZO targets at low cost.
A combination of indium oxide, zinc oxide, gallium oxide and antimony pentoxide is used. Antimony pentoxide decomposes and releases oxygen during heating, which inhibits the decomposition of indium oxide and zinc oxide, provides a liquid phase to lower the sintering temperature, and regulates the carrier concentration through gallium oxide to optimize the conductive properties.
Achieve stability and uniformity of IGZO target at lower temperature, reduce excessive evaporation of indium oxide and zinc oxide, lower sintering temperature, increase material density, and ensure stability and uniformity of target.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of metal target material, in particular to an indium gallium zinc oxide target material and a preparation method and application thereof. BACKGROUND
[0002] Driven by three application waves of notebook computers, displays and televisions, display technology has undergone several developments, and high-resolution, color-bright, low-power display screens have become the first choice of people. Thin film transistor driven liquid crystal display (TFT-LCD) has shown excellent results in research, and TFT devices have been widely concerned as the key research object. Although amorphous silicon (alpha-Si) TFT devices as active layer have been widely used due to their low cost and simple preparation, but the mobility of alpha-Si TFT devices is too insufficient to meet the needs of high refresh display technology, and is gradually replaced by amorphous indium gallium zinc oxide (alpha-IGZO) TFT. The mobility of alpha-IGZO TFT device is more than 20 times that of alpha-Si TFT device, and the alpha-IGZO film has good uniformity, good stability, simple process and high transparency, which can meet the needs of fast response, large size, high resolution and other requirements of display. In existing coating technology, magnetron sputtering is widely used in industry due to its large-area film formation, easy control of thin film growth, stable film quality and strong thin film adhesion. High-quality IGZO thin films are generally prepared by magnetron sputtering method, and IGZO target material is the key factor to determine the quality of the thin film. Traditional preparation of IGZO target material requires ultra-high temperature sintering for a long time, which is high in cost and indium and zinc are easy to volatilize at high temperature, thereby seriously affecting the composition of the target material. Therefore, it is an important problem to be solved to prepare high-quality IGZO target material at low cost at low temperature. SUMMARY
[0003] The present application aims to at least solve one of the technical problems existing in the prior art. To this end, the present application proposes an indium gallium zinc oxide target material, which can effectively reduce the sintering temperature of the target material and the volatilization rate of the raw material without additional oxygen.
[0004] A first aspect of the present application proposes an indium gallium zinc oxide target material, comprising the following preparation raw materials calculated by weight parts:
[0005]
[0006] 1. The above components, indium oxide can generally form free electrons during heating process, zinc oxide enhances electron mobility by increasing oxygen defect density, the oxide solid solution formed between indium oxide and zinc oxide has good chemical stability and thermal stability, can exist stably at high temperature and provide excellent electrical conductivity; gallium oxide forms a variety of oxide solid solutions with indium oxide and zinc oxide, which helps to improve the thermal stability and chemical stability of IGZO, Ga 3+ ions can adjust the carrier concentration of indium oxide and zinc oxide, and through the doping effect of gallium oxide, the electronic structure of the material is adjusted, thereby improving its electrical conductivity and transparency; antimony pentoxide can continuously decompose and release oxygen during sintering process, and the oxygen can react with indium oxide and zinc oxide to prevent their reduction or decomposition, thereby stabilizing the composition of the target material. Through the formation of a liquid phase, antimony pentoxide not only accelerates the sintering process, but also reduces the sintering temperature. Low-temperature sintering helps to improve the density of the material and reduce the excessive evaporation or reduction of indium oxide and zinc oxide, thereby ensuring the stability and uniformity of the target material.
[0007] 2. The combined action of indium oxide, zinc oxide, gallium oxide and antimony pentoxide can promote sintering at a lower temperature and reduce the decomposition and loss of components that may occur during the sintering process. Indium oxide, zinc oxide and gallium oxide optimize the electrical conductivity of IGZO by adjusting the carrier concentration, while antimony pentoxide prevents the decomposition of indium oxide and zinc oxide by providing an oxygen source, ensuring the stable electrical conductivity of IGZO material, especially during high-temperature sintering process, which can effectively inhibit the decomposition of indium oxide and zinc oxide. Antimony pentoxide can continuously decompose and release oxygen during heating process, which inhibits the decomposition of indium oxide and zinc oxide, while the substance has a low melting point, providing a liquid phase for the sintering process and reducing the sintering temperature of the target material. Specifically, antimony pentoxide can continuously decompose and release oxygen during sintering process, and the oxygen can react with indium oxide and zinc oxide to prevent their reduction or decomposition, thereby stabilizing the composition of the target material. Through the formation of a liquid phase, antimony pentoxide not only accelerates the sintering process, but also reduces the sintering temperature. Low-temperature sintering helps to improve the density of the material and reduce the excessive evaporation or reduction of indium oxide and zinc oxide, thereby ensuring the stability and uniformity of the target material.
[0008] According to some embodiments of the present application, the purity of the indium oxide is ≥ 99.99%.
[0009] According to some embodiments of the present application, the purity of the gallium oxide is ≥ 99.99%.
[0010] According to some embodiments of the present application, the purity of the zinc oxide is ≥ 99.99%.
[0011] According to some embodiments of the present application, the preparation raw materials of the indium gallium zinc oxide target further comprise an additive; the additive comprises a dispersant and a binder.
[0012] According to some embodiments of the present application, the dispersant comprises polyacrylamide.
[0013] According to some embodiments of the present application, the binder comprises polyvinyl alcohol.
[0014] According to some embodiments of the present application, the indium gallium zinc oxide target comprises the following preparation raw materials by weight:
[0015]
[0016] According to some embodiments of the present application, the preparation raw materials of the indium gallium zinc oxide target further comprise water.
[0017] A second aspect of the present application provides a preparation method of an indium gallium zinc oxide target, comprising the following steps:
[0018] S1, mixing and dispersing the indium oxide powder, the gallium oxide powder, the zinc oxide powder and the antimony pentoxide powder, and then spray granulating to obtain a mixed oxide powder;
[0019] S2, shaping the oxide powder and then sintering.
[0020] According to some embodiments of the present application, step S1 comprises: mixing the indium oxide powder, the gallium oxide powder, the zinc oxide powder, the antimony pentoxide powder, a dispersant and water, and then pouring into a grinder to obtain a mixed slurry; the amount of pure water added is consistent with the weight of the powder; a binder is added to the mixed slurry, and after stirring for 1-2 hours, spray granulation can be performed to obtain the mixed oxide powder.
[0021] According to some embodiments of the present application, the preparation method of the antimony pentoxide comprises: mixing antimony trioxide and hydrogen peroxide, and then refluxing and reacting.
[0022] The present application synthesizes antimony pentoxide powder with sintering activity, which can continuously release oxygen during heating and inhibit the decomposition of indium oxide and zinc oxide. At the same time, the substance has a low melting point, which provides a liquid phase for the sintering process and reduces the sintering temperature of the target material.
[0023] According to some embodiments of the present application, the particle size of the antimony pentoxide powder is 10-12 nm.
[0024] According to some embodiments of the present application, the preparation method of the indium oxide comprises a chemical precipitation method.
[0025] According to some embodiments of the present application, the method for preparing indium oxide comprises dissolving indium ingot, drying indium hydroxide at room temperature by using chemical precipitation method, and then forming indium oxide powder by high-temperature calcination.
[0026] According to some embodiments of the present application, the specific surface area of the indium oxide powder is 12m 2 / g~20m 2 / g.
[0027] The surface area within the above range has high reactivity, excellent dispersibility and processability, and good sintering performance.
[0028] According to some embodiments of the present application, the forming method comprises cold isostatic pressing.
[0029] According to some embodiments of the present application, the pressure holding time of the cold isostatic pressing is 30~40min, and the pressure of the cold isostatic pressing is 200~250Mpa.
[0030] According to some embodiments of the present application, the sintering conditions comprise: increasing the temperature of the formed body to 650~750℃ at a temperature increasing rate of 1.5~3℃ / min, holding for 3~4h, then increasing the temperature to 1320~1410℃ at a temperature increasing rate of 0.5~1℃ / min, holding for 8~10h, and then cooling.
[0031] According to some embodiments of the present application, the sintering further comprises processing; the processing steps comprise placing the sintered target in a lathe, polishing the target with 400-mesh and 800-mesh grinding wheels respectively, fixing the target with smooth surface on a copper back plate by using an indium layer, and completing the binding process.
[0032] The third aspect of the present application provides an application of the indium gallium zinc oxide target in reflective film, conductive film, and organic light emitting diode. DETAILED DESCRIPTION
[0033] The concept and technical effects of the present application will be described below in combination with embodiments, so as to fully understand the purposes, features and effects of the present application. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments of the present application, other embodiments obtained by those skilled in the art without creative labor are within the protection scope of the present application.
[0034] In the description of the application, the description of the terms “one embodiment”, “some embodiments”, “exemplary embodiment”, “example”, “specific example”, or “some examples” means that the specific features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the application. In the description, the exemplary description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0035] Unless otherwise specified, “room temperature” in the application means 25℃±5℃.
[0036] Unless otherwise specified, “about” in the application means that the allowable error is within ±2%.
[0037] Unless otherwise specified, the specific conditions in the embodiments are carried out according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not specified by the manufacturer, and are all conventional products that can be purchased on the market.
[0038] Gallium oxide powder and zinc oxide powder are purchased from Shanghai Maikelin Biochemical Technology Co., Ltd., product numbers are G810511 and 768612 respectively;
[0039] Antimony trioxide powder and hydrogen peroxide are purchased from Shanghai Maikelin Biochemical Technology Co., Ltd., product numbers are 768559 and H792072 respectively.
[0040] The first aspect embodiment of the application provides an indium gallium zinc oxide target material, which comprises the following preparation raw materials calculated by weight parts:
[0041]
[0042] In combination with the first aspect, in some embodiments of the application, the purity of the indium oxide is ≥99.99%.
[0043] In combination with the first aspect, in some embodiments of the application, the purity of the gallium oxide is ≥99.99%.
[0044] In combination with the first aspect, in some embodiments of the application, the purity of the zinc oxide is ≥99.99%.
[0045] In combination with the first aspect, in some embodiments of the application, the preparation raw materials of the indium gallium zinc oxide target material further comprise an additive; the additive comprises a dispersing agent and a binder.
[0046] In combination with the first aspect, in some embodiments of the application, the dispersing agent comprises polyacrylamide.
[0047] With reference to the first aspect, in some embodiments of the present application, the binder comprises polyvinyl alcohol.
[0048] With reference to the first aspect, in some embodiments of the present application, the indium gallium zinc oxide target material comprises the following preparation raw materials in parts by weight:
[0049]
[0050] With reference to the first aspect, in some embodiments of the present application, the preparation raw materials of the indium gallium zinc oxide target material further comprise water.
[0051] The second aspect of the present application provides a preparation method of an indium gallium zinc oxide target material, comprising the following steps:
[0052] S1, mixing and dispersing the indium oxide powder, the gallium oxide powder, the zinc oxide powder and the antimony pentoxide powder, and then spray granulating to obtain a mixed oxide powder;
[0053] S2, shaping the oxide powder and then sintering.
[0054] With reference to the second aspect, in some embodiments of the present application, step S1 comprises: mixing the indium oxide powder, the gallium oxide powder, the zinc oxide powder, the antimony pentoxide powder, a dispersing agent and water, and then pouring into a grinder to obtain a mixed slurry, the amount of pure water added is consistent with the weight of the powder, adding a binder in the mixed slurry, and then stirring for 1-2 hours before spray granulating to obtain the mixed oxide powder.
[0055] With reference to the second aspect, in some embodiments of the present application, the preparation method of the antimony pentoxide comprises: mixing antimony trioxide and hydrogen peroxide and then refluxing to react.
[0056] The present application synthesizes antimony pentoxide powder with sintering activity, which can continuously release oxygen during heating process, thereby inhibiting the decomposition of indium oxide and zinc oxide. Meanwhile, the substance has a low melting point, which provides a liquid phase for the sintering process, thereby reducing the sintering temperature of the target material.
[0057] With reference to the second aspect, in some embodiments of the present application, the particle size of the antimony pentoxide powder is 10-12 nm.
[0058] With reference to the second aspect, in some embodiments of the present application, the preparation method of the indium oxide comprises a chemical precipitation method.
[0059] With reference to the second aspect, in some embodiments of the present application, the preparation method of the indium oxide comprises dissolving indium ingot, drying to obtain indium hydroxide at room temperature using a chemical precipitation method, and then forming indium oxide powder after high-temperature calcination.
[0060] In combination with the second aspect, in some embodiments of the present application, the specific surface area of the indium oxide powder is 12 m 2 / g to 20 m 2 / g.
[0061] The surface area within the above range has high reactivity, excellent dispersibility and processability, and good sintering performance.
[0062] According to some embodiments of the present application, in combination with the second aspect, in some embodiments of the present application, the forming method comprises cold isostatic pressing forming.
[0063] In combination with the second aspect, in some embodiments of the present application, the pressure holding time of the cold isostatic pressing forming is 30-40 min, and the pressure of the cold isostatic pressing forming is 200-250 MPa.
[0064] In combination with the second aspect, in some embodiments of the present application, the sintering conditions comprise: increasing the temperature of the formed body to 650-750℃ at a temperature increasing rate of 1.5-3℃ / min, holding for 3-4h, then increasing the temperature to 1320-1410℃ at a temperature increasing rate of 0.5-1℃ / min, holding for 8-10h, and then cooling.
[0065] In combination with the second aspect, in some embodiments of the present application, the sintering further comprises processing; the processing step comprises placing the sintered target material in a lathe, polishing with 400-mesh and 800-mesh grinding wheels respectively, fixing the target material with a smooth surface on a copper back plate using an indium layer, and completing the binding process.
[0066] The third aspect of the present application provides an application of the IGZO target material in a reflective film, a conductive film, and an organic light-emitting diode.
[0067] Embodiment 1
[0068] The present embodiment provides an IGZO target material and a preparation method thereof, and the preparation raw material of the IGZO target material is composed of the following components with the following mass fractions:
[0069] 15 parts of indium oxide powder, 29 parts of gallium oxide powder, 54 parts of zinc oxide powder, and 0.05 parts of antimony pentoxide powder;
[0070] The IGZO target material preparation steps are as follows:
[0071] S1, the indium oxide powder, gallium oxide powder, zinc oxide powder, antimony pentoxide powder and 0.4% of the total mass of the above-mentioned powder dispersant are mixed and poured into a grinder to obtain a mixed slurry, the amount of pure water added is consistent with the weight of the powder, the zirconium beads used have a particle size of 1mm, 1.5% of the total mass of the above-mentioned powder is added to the mixed slurry as a binder, and the slurry is stirred for 1.5 hours before spray granulation, the mixed oxide powder is then loaded into a 1m×0.5m×0.2m mold, plastic sealed, and cold isostatic pressing is performed, the holding time is 30min, and the forming pressure is 220Mpa to obtain a blank;
[0072] S2, the blank is placed horizontally in a sintering furnace, a normal pressure atmosphere is maintained, the temperature is raised to 750℃ at a rate of 1.5℃ / min, and the temperature is maintained for 3h to complete the debinding process; then the temperature is raised to 1410℃ at a rate of 0.5℃ / min, and the temperature is maintained for 7h to complete the sintering process. Finally, the furnace is cooled to room temperature, and an IGZO target material is obtained;
[0073] S3, the sintered target material is placed in a lathe, and the surface of the target material is polished with a 400-mesh and an 800-mesh grinding wheel, respectively, and then the target material with a smooth surface is fixed on a copper back plate using an indium layer to complete the binding process.
[0074] Example 2
[0075] The present embodiment provides an IGZO target material and a preparation method thereof, and the preparation raw material of the IGZO target material is composed of the following components with the following mass fractions:
[0076] 30 parts of indium oxide powder, 30 parts of gallium oxide powder, 30 parts of zinc oxide powder, and 0.03 parts of antimony pentoxide powder;
[0077] S1, the indium oxide powder, gallium oxide powder, zinc oxide powder, and antimony pentoxide powder and 0.3% of the total mass of the above-mentioned powder dispersant are mixed and poured into a grinder to obtain a mixed slurry, the amount of pure water added is consistent with the weight of the powder, the zirconium beads used have a particle size of 1mm, 1% of the total mass of the above-mentioned powder is added to the mixed slurry as a binder, and the slurry is stirred for 1 hour before spray granulation, the mixed oxide powder is then loaded into a 1m×0.5m×0.2m mold, plastic sealed, and cold isostatic pressing is performed, the holding time is 30min, and the forming pressure is 200Mpa.
[0078] S2, the blank is placed horizontally in a sintering furnace, a normal pressure atmosphere is maintained, the temperature is raised to 750℃ at a rate of 1.5℃ / min, and the temperature is maintained for 3h to complete the debinding process; then the temperature is raised to 1410℃ at a rate of 0.5℃ / min, and the temperature is maintained for 7h to complete the sintering process. Finally, the furnace is cooled to room temperature, and an IGZO target material is obtained;
[0079] S3, the sintered target material is placed in a lathe, polished with 400 mesh and 800 mesh grinding wheels respectively, and the target material with smooth surface obtained is fixed on a copper back plate using an indium layer to complete the binding process.
[0080] Example 3
[0081] The embodiment provides an IGZO target material and a preparation method thereof. The preparation raw material of the IGZO target material is composed of the following components in mass fraction:
[0082] 45 parts of indium oxide powder, 32 parts of gallium oxide powder, 25 parts of zinc oxide powder and 0.01 part of antimony pentoxide powder;
[0083] S1, the indium oxide powder, the gallium oxide powder, the zinc oxide powder, the antimony pentoxide powder and 0.5% of the dispersant of the total mass of the powders are mixed and then poured into a grinding machine to obtain a mixed slurry, the amount of pure water added is consistent with the weight of the powder, the zirconium beads used have a particle size of 1 mm, 2% of the total mass of the powders is added to the mixed slurry as a binder, and after stirring for 1.5 hours, spray granulation can be performed, the mixed oxide powder is filled into a 1m*0.5m*0.2m mold, plastic encapsulation is performed, cold isostatic pressing is performed, the pressure maintaining time is 30 min, the molding pressure is 250Mpa, and the embryo is obtained;
[0084] S2, the embryo is placed in a sintering furnace in a horizontal manner, a normal pressure atmosphere is maintained, the temperature is raised to 650 DEG C at a rate of 1.5 DEG C / min, and the temperature is maintained for 3h to complete the degreasing process; then the temperature is raised to 1350 DEG C at a rate of 0.5 DEG C / min, and the temperature is maintained for 7h to complete the sintering process, finally, the furnace is cooled to room temperature, and the IGZO target material can be obtained.
[0085] S3, the sintered target material is placed in a lathe, polished with 400 mesh and 800 mesh grinding wheels respectively, and the target material with smooth surface obtained is fixed on a copper back plate using an indium layer to complete the binding process.
[0086] Comparative Example 1
[0087] The comparative example provides an IGZO target material and a preparation method thereof. The preparation raw material of the IGZO target material is composed of the following components in mass fraction:
[0088] 15 parts of indium oxide powder, 29 parts of gallium oxide powder and 54 parts of zinc oxide powder, and no antimony pentoxide powder;
[0089] The IGZO target material preparation steps are as follows:
[0090] S1, the indium oxide powder, gallium oxide powder, zinc oxide powder and 0.4% of the total mass of the above-mentioned powder dispersant mixed after pouring into the grinder, get mixed slurry, the amount of pure water added is consistent with the weight of the powder, the zirconium bead size used is 1mm, 1.5% of the total mass of the above-mentioned powder is added to the mixed slurry, and the binder is stirred for 1.5 hours before spray granulation can be carried out, and the mixed oxide powder is packed into a 1m×0.5m×0.2m mold, plastic sealed, and cold isostatic pressing forming is carried out, the holding pressure time is 30min, and the forming pressure is 220Mpa;
[0091] S2, place the embryo in the sintering furnace, keep the normal pressure atmosphere, increase the temperature to 750℃ at the rate of 1.5℃ / min, keep the temperature for 3h, complete the debinding process, then increase the temperature to 1500℃ at the rate of 0.5℃ / min, keep the temperature for 7h, complete the sintering process, finally, cool down to room temperature with the furnace, IGZO target material can be obtained.
[0092] S3, place the sintered target material in the lathe, polish it with 400 mesh and 800 mesh grinding wheels respectively, fix the target material with smooth surface on the copper back plate using indium layer, complete the binding process.
[0093] Comparative Example 2
[0094] The present comparative example provides an IGZO target material and a preparation method thereof, the preparation raw material of the IGZO target material is composed of the following components with mass fraction:
[0095] 30 parts of indium oxide powder, 30 parts of gallium oxide powder, 30 parts of zinc oxide powder, and no antimony pentoxide powder;
[0096] The IGZO target material preparation steps are as follows:
[0097] S1, the indium oxide powder, gallium oxide powder, zinc oxide powder and 0.3% of the dispersant are mixed and poured into the grinder to obtain a mixed slurry, the amount of pure water added is consistent with the weight of the powder, the zirconium bead size used is 1mm, 1% of the binder is added to the mixed slurry, and the spray granulation can be carried out after stirring for 1 hour, and the mixed oxide powder is packed into a 1m×0.5m×0.2m mold, plastic sealed, and cold isostatic pressing forming is carried out, the holding pressure time is 30min, and the forming pressure is 200Mpa to obtain the embryo;
[0098] S2, place the embryo in the sintering furnace, keep the normal pressure atmosphere, increase the temperature to 700℃ at the rate of 1.5℃ / min, keep the temperature for 3h, complete the debinding process, then increase the temperature to 1480℃ at the rate of 0.5℃ / min, keep the temperature for 7h, complete the sintering process, finally, cool down to room temperature with the furnace, IGZO target material can be obtained;
[0099] S3, the sintered target material is placed in a lathe, polished with 400 mesh and 800 mesh grinding wheels respectively, and the target material with smooth surface obtained is fixed on a copper back plate using an indium layer to complete the binding process.
[0100] Comparative Example 3
[0101] The present comparative example provides an IGZO target material and a preparation method thereof, and the preparation raw material of the IGZO target material is composed of the following components with mass fractions:
[0102] 45 parts of indium oxide powder, 32 parts of gallium oxide powder, 25 parts of zinc oxide powder, and no antimony pentoxide powder;
[0103] The IGZO target material preparation steps are as follows:
[0104] S1, the indium oxide powder, gallium oxide powder, zinc oxide powder, and 0.5% dispersant are mixed and poured into a grinding machine to obtain a mixed slurry, the amount of pure water added is consistent with the weight of the powder, the zirconium beads used have a particle size of 1 mm, 2% binder is added to the mixed slurry, and after stirring for 1.5 hours, spray granulation can be performed to obtain a mixed oxide powder which is filled into a 1m x 0.5m x 0.2m mold, plastic encapsulated, and cold isostatic pressing formed, with a holding pressure time of 30 min and a forming pressure of 250Mpa to obtain a blank;
[0105] S2, the blank is placed flat in a sintering furnace, kept in a normal pressure atmosphere, raised to 650℃ at a heating rate of 1.5℃ / min, and held for 3h to complete the degreasing process; then raised to 1450℃ at a heating rate of 0.5℃ / min, and held for 7h to complete the sintering process, finally, cooled to room temperature with the furnace, and an IGZO target material can be obtained;
[0106] S3, the sintered target material is placed in a lathe, polished with 400 mesh and 800 mesh grinding wheels respectively, and the target material with smooth surface obtained is fixed on a copper back plate using an indium layer to complete the binding process.
[0107] Comparative Example 4
[0108] The present comparative example provides an IGZO target material and a preparation method thereof, and the difference between the present comparative example and Comparative Example 3 is only in the mass fraction of part of the preparation raw material components: 45 parts of indium oxide powder, 32.01 parts of gallium oxide powder, and 25 parts of zinc oxide powder, and no antimony pentoxide powder.
[0109] Comparative Example 5
[0110] The present comparative example provides an IGZO target material and a preparation method thereof, and the difference between the present comparative example and Example 1 is only that bismuth oxide is used instead of antimony pentoxide, and the other conditions are the same.
[0111] The excessive liquid phase generated by bismuth pentoxide under the above conditions can cause poor densification of the target material at a lower temperature, thereby affecting the structural stability of the target material. If the liquid phase is excessive, the sintering process can become unstable, and even pores or bubbles can occur in the target material, affecting the mechanical and electrical properties of the target material.
[0112] Comparative Example 6
[0113] The present comparative example provides an IGZO target material and a preparation method thereof. The only difference between the present comparative example and Example 1 is that the amount of antimony pentoxide is 0.08 parts, and the other conditions are the same.
[0114] Under the above conditions, bismuth pentoxide causes uneven oxygen release, causing local over-oxidation of indium and zinc oxide, and possibly insufficient oxidation in other areas, thereby causing material inhomogeneity, especially during high-temperature sintering. Excessive oxygen can promote the volatilization or reduction of components such as indium oxide and zinc oxide, resulting in material loss and affecting the raw material volatilization rate.
[0115] Test Example 1
[0116] The relative density of the target material prepared in the present example and the comparative example was determined by the Archimedes drainage method. The volatilization rate is the weight loss ratio before and after sintering, and the calculation formula is as follows:
[0117] Relative density = actual density / theoretical density x 100%;
[0118] Volatilization rate = (weight before sintering - weight after sintering / weight before sintering) x 100%.
[0119] The mass ratio of In, Ga, and Zn elements before and after sintering was tested by XRF.
[0120] Table 1 Performance test data of examples and comparative examples
[0121]
[0122]
[0123] As can be seen from the examples and comparative examples, the addition of antimony pentoxide can continuously release oxygen during heating, inhibit the decomposition of indium oxide and zinc oxide, and at the same time, the substance has a low melting point, providing a liquid phase for the sintering process. Reducing the sintering temperature of the target material can effectively reduce the sintering temperature of the target material, reduce the volatilization of In and Zn components in the target material, and effectively reduce the sintering temperature of the target material and the volatilization rate of the raw material without additional oxygen.
[0124] The above has been described in detail in combination with the embodiments of the present application, but the present application is not limited to the above-described embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present application.
Claims
1. An indium gallium zinc oxide target, characterized in that: The preparation comprises the following raw materials calculated by weight:
2. The indium gallium zinc oxide target according to claim 1, characterized in that The raw materials for preparing the indium gallium zinc oxide target material also include auxiliary agents; the auxiliary agents include dispersants and binders.
3. The indium gallium zinc oxide target according to claim 2, characterized in that The preparation comprises the following raw materials calculated by weight:
4. A method for preparing an indium gallium zinc oxide target according to any one of claims 1 to 3, characterized in that: The steps include: S1, mixing and dispersing the indium oxide powder, the gallium oxide powder, the zinc oxide powder and the antimony pentoxide powder, and spray granulating the mixture to obtain a mixed oxide powder; S2, forming the oxide powder and then sintering it.
5. The method for preparing an indium gallium zinc oxide target according to claim 4, wherein: The preparation method of antimony pentoxide comprises: mixing antimony trioxide and hydrogen peroxide and subjecting the mixture to a reflux reaction.
6. The method for preparing an indium gallium zinc oxide target according to claim 4, wherein: The particle size of the antimony pentoxide powder is 10-12 nm.
7. The method for preparing an indium gallium zinc oxide target according to claim 4, wherein: The forming method includes cold isostatic pressing.
8. The method for preparing an indium gallium zinc oxide target according to claim 5, wherein: The holding time of the cold isostatic pressing is 30 to 40 minutes, and the pressure of the cold isostatic pressing is 200 to 250 MPa.
9. The method for preparing an indium gallium zinc oxide target according to claim 5, wherein: The sintering conditions include: heating the green body obtained after molding to 650-750° C. at a heating rate of 1.5-3° C. / min, keeping the temperature for 3-4 hours, then heating the green body to 1320-1410° C. at a heating rate of 0.5-1° C. / min, keeping the temperature for 8-10 hours, and then cooling.
10. Use of the indium gallium zinc oxide target according to any one of claims 1 to 3 in a reflective film, a conductive film, or an organic light emitting diode.
Citation Information
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