A high-density, high-mobility indium oxide doped target and its preparation method

Abstract

The application relates to the technical field of target materials, and particularly discloses a high-density high-mobility indium oxide doped target material and a preparation method thereof. The high-density high-mobility indium oxide doped target material comprises the following raw materials in parts by weight: 90-98 parts of indium oxide, 5-8 parts of tin oxide, 1-3 parts of rare earth oxide, 0.5-1.5 parts of a binder, 0.5-0.8 parts of a dispersing agent, and 0.3-0.5 parts of a stabilizer; and the binder is carboxymethyl cellulose and polyvinyl alcohol. The high-density high-mobility indium oxide doped target material has high compactness and high mobility under the synergistic action of various components.

Description

Technical Field

[0001] This application relates to the field of target technology, and more specifically, to a high-density, high-mobility indium oxide doped target and its preparation method. Background Technology

[0002] Indium oxide (IO) sputtering targets possess excellent chemical stability and optical properties. Compared to metal sputtering targets, they exhibit higher optical transmittance and electrical conductivity, making them widely used in transparent conductive films, magnetic materials, and other fields. With the continuous development of electronic devices, the requirements for IO sputtering targets are becoming increasingly stringent.

[0003] However, traditional indium oxide (IO) sputtering targets currently exhibit low density and mobility, which limits their application in high-end devices. Therefore, there is an urgent need to investigate a method to increase the density of IO sputtering targets while maintaining their high mobility. Summary of the Invention

[0004] To improve the density and mobility of indium oxide targets, this application provides a high-density, high-mobility indium oxide doped target and its preparation method.

[0005] In a first aspect, this application provides a high-density, high-mobility indium oxide doped target, employing the following technical solution:

[0006] A high-density, high-mobility indium oxide doped target comprises the following raw materials in parts by weight: 90-98 parts indium oxide, 5-8 parts tin oxide, 1-3 parts rare earth oxide, 0.5-1.5 parts binder, 0.5-0.8 parts dispersant, and 0.3-0.5 parts stabilizer, wherein the binder is carboxymethyl cellulose and polyvinyl alcohol.

[0007] By employing the above technical solutions, adding appropriate amounts of rare earth oxides to indium oxide and tin oxide raw materials can promote the growth of oxide crystals, improve crystallinity and grain boundary quality, thereby increasing carrier mobility and the density of the indium oxide target. Adding carboxymethyl cellulose and polyvinyl alcohol as binders to the indium oxide target can promote the growth and bonding of indium oxide and tin oxide crystals, reduce grain boundary defects and impurities, enhance the transport channels of the indium oxide target, and thus improve its mobility. Simultaneously, carboxymethyl cellulose and polyvinyl alcohol can enhance the viscosity between the components of the indium oxide target system and strengthen the bonding between oxide particles, thereby increasing the density of the indium oxide target.

[0008] Preferably, the rare earth oxide is at least one selected from lanthanum oxide, praseodymium oxide, neodymium oxide, and yttrium oxide.

[0009] By adopting the above technical solutions, lanthanum can improve the optical properties of indium oxide (IO) targets, while neodymium can enhance their optical, electrical, and magnetic properties. Simultaneously, adding rare earth elements, primarily lanthanum oxide, praseodymium oxide, neodymium oxide, and yttrium oxide, to IO targets can introduce additional energy levels, improve carrier transport performance in the crystal lattice, and increase electron mobility. Furthermore, doping with appropriate amounts of rare earth elements can enhance the grain boundary bonding ability of IO targets, thereby increasing their density.

[0010] Preferably, the dispersant is one of polyacrylic acid and polyethylene glycol.

[0011] By adopting the above technical solutions, polyethylene glycol can affect the surface potential of the indium oxide target system particles through hydrogen bond adsorption, and polyacrylic acid can change the surface potential of the target particles through negatively charged carboxyl groups. Through the combined effect of electrostatic and steric hindrance effects, the dispersion performance of the indium oxide target system can be improved.

[0012] Preferably, the stabilizer is at least one of magnesium oxide, aluminum oxide, and zirconium oxide.

[0013] By adopting the above technical solution and using magnesium oxide, aluminum oxide, and zirconium oxide as stabilizers, the size and structure of indium oxide target grains can be controlled, the fragility of indium oxide target can be reduced, the thermal stability and wear resistance of indium oxide target can be improved, and thus the stability of indium oxide target can be enhanced.

[0014] Preferably, the indium oxide target material also includes 1-3 parts of chloroauric acid and 3-5 parts of polyvinylpyrrolidone.

[0015] By employing the above technical solutions, depositing an appropriate amount of gold nanoparticles on the surface of indium oxide particles can modulate the carrier transport channels and improve the mobility of the indium oxide target. Modifying the surface of each particle in the indium oxide target system with polyvinylpyrrolidone can enhance the dispersibility of the indium oxide target system and improve the density and stability of the indium oxide target.

[0016] Preferably, nano-gold particles are deposited on the surface of indium oxide in advance by chloroauric acid to form indium oxide composite particles. Then, polyvinylpyrrolidone is dissolved and mixed with the composite indium oxide particles by heating. After the reaction, the mixture is cooled, filtered, and washed to obtain modified indium oxide particles.

[0017] By adopting the above technical solution, gold nanoparticles are first deposited on the surface of indium oxide particles, and then polyvinylpyrrolidone is used to modify the surface of the composite indium oxide particles. This can promote the uniform embedding of gold nanoparticles on the surface of indium oxide particles, and at the same time enhance the dispersibility of the modified indium oxide particles.

[0018] Secondly, this application provides a method for preparing a high-density, high-mobility indium oxide doped target, employing the following technical solution:

[0019] A method for preparing a high-density, high-mobility indium oxide doped target includes the following specific steps:

[0020] Indium oxide, tin oxide, rare earth oxides, binders, dispersants and stabilizers are mixed and ground, and then spray granulation, molding and cold isostatic pressing are performed in sequence to obtain a green blank. The green blank is then sintered to obtain a high-density, high-mobility indium oxide doped target.

[0021] By adopting the above technical solution, the prepared indium oxide target material can maintain good mobility under the synergistic effect of various components, and at the same time enhance the density of the indium oxide target material.

[0022] Preferably, the molding pressure is 25-50 MPa, and the cold isostatic pressing pressure is 350-450 MPa.

[0023] Preferably, the sintering includes heat treatment and high-temperature sintering, wherein the heat treatment temperature is 400-600℃ and the high-temperature sintering temperature is 1500-1600℃.

[0024] By adopting the above technical solution, preheating the target blank can oxidize and volatilize the chemical reagents in the indium oxide target. At the same time, heat treatment can remove the pores in the blank, thereby improving the density of the indium oxide target.

[0025] In summary, this application has the following beneficial effects:

[0026] 1. Because the addition of appropriate amounts of rare earth oxides to the indium oxide and tin oxide raw materials in this application can promote the growth of oxide crystals, improve the crystal structure, increase the carrier mobility, and increase the density of the indium oxide target. Simultaneously, the use of carboxymethyl cellulose and polyvinyl alcohol as binders in the indium oxide target enhances the viscosity between particles in the indium oxide target system, thereby increasing the density of the indium oxide target.

[0027] 2. In this application, gold nanoparticles are pre-deposited on the surface of indium oxide particles, and then the surface is modified with polyvinylpyrrolidone, which promotes the preparation of indium oxide target material to have high mobility while maintaining good dispersibility. Detailed Implementation

[0028] The present application will be further described in detail below with reference to the embodiments.

[0029] The average relative molecular mass of polyacrylic acid is 4000.

[0030] The average relative molecular mass of polyethylene glycol is 30,000.

[0031] Polyvinylpyrrolidone (PVP) K30 was selected.

[0032] The molecular weight of polyvinyl alcohol is 120,000.

[0033] Example

[0034] Example 1

[0035] This embodiment provides a high-density, high-mobility indium oxide doped target, comprising the following raw materials in parts by weight: 94 kg indium oxide, 7 kg tin oxide, 2 kg rare earth oxide, 1 kg binder, 0.7 kg dispersant, and 0.4 kg stabilizer. The rare earth oxide is lanthanum oxide, the binder is a mixture of carboxymethyl cellulose and polyvinyl alcohol with a mass ratio of 1:1, the dispersant is polyacrylic acid, and the stabilizer is zirconium oxide with an average particle size of 50-80 nm.

[0036] The preparation method of high-density, high-mobility indium oxide doped target includes the following specific steps:

[0037] S1: Indium oxide, tin oxide, rare earth oxides, dispersant and stabilizer are mixed, pure water is added, and the mixture is ball-milled at 450 rpm for 12 hours. Then, a binder is added and the grinding continues to obtain a mixed slurry with a solid content of 28%. The mixed slurry is then placed in a spray drying tower for spray granulation at a temperature of 240℃. After sieving, an oxide mixed powder with an average particle size of 30-50 μm is obtained.

[0038] S2: The oxide mixed powder is pre-pressed at 35 MPa for 15 min, then cold isostatically pressed at 400 MPa for 30 min to obtain an oxide blank. The oxide blank is then heat-treated by heating to 500℃ at a heating rate of 2.0℃ / min and holding for 60 min, then heating to 1550℃ at a heating rate of 1.5℃ / min and holding for 11 hours, and then cooling to room temperature at a cooling rate of 1.0℃ / min to obtain a high-density, high-mobility indium oxide doped target.

[0039] Example 2

[0040] The difference between Example 2 and Example 1 is that the amount of indium oxide used in the high-density, high-mobility indium oxide doped target material is 90 kg, the amount of tin oxide is 8 kg, the amount of rare earth oxide is 1 kg, the amount of binder is 0.5 kg, the amount of dispersant is 0.5 kg, and the amount of stabilizer is 0.3 kg.

[0041] Example 3

[0042] The difference between Example 3 and Example 1 is that the amount of indium oxide used in the high-density, high-mobility indium oxide doped target material is 98 kg, the amount of tin oxide is 5 kg, the amount of rare earth oxide is 3 kg, the amount of binder is 1.5 kg, the amount of dispersant is 0.8 kg, and the amount of stabilizer is 0.5 kg.

[0043] Example 4

[0044] The difference between Example 4 and Example 1 is that the rare earth oxide in the high-density, high-mobility indium oxide doped target material is a mixture of praseodymium oxide and neodymium oxide, with a mass ratio of praseodymium oxide to neodymium oxide of 1:1.

[0045] Example 5

[0046] The difference between Example 5 and Example 1 is that the rare earth oxides in the high-density, high-mobility indium oxide doped target material are a mixture of lanthanum oxide, praseodymium oxide and yttrium oxide, with a mass ratio of lanthanum oxide, praseodymium oxide and yttrium oxide of 1:1:1.

[0047] Example 6

[0048] The difference between Example 6 and Example 1 is that the dispersant in the high-density, high-mobility indium oxide doped target material is polyethylene glycol.

[0049] Example 7

[0050] The difference between Example 7 and Example 1 is that the stabilizer in the high-density, high-mobility indium oxide doped target material is magnesium oxide.

[0051] Example 8

[0052] The difference between Example 8 and Example 1 is that the high-density, high-mobility indium oxide doped target material also includes 2 kg of chloroauric acid.

[0053] The preparation method of high-density, high-mobility indium oxide doped target includes the following specific steps:

[0054] S1: Indium oxide was pre-cleaned sequentially with ammonia, water, and anhydrous ethanol. Chloroauric acid and potassium chloride were mixed in a mass ratio of 1:5 to form a chloroauric acid-potassium chloride solution. Indium oxide was then added to the chloroauric acid-potassium chloride solution and kept at a constant temperature of 25°C in a water bath. Oxygen was removed by nitrogen for 10 minutes. Gold nanoparticles were deposited on the surface of the indium oxide particles using cyclic voltammetry. The electroplating parameters were: potential range of (-0.3V)-(-1.15V), scan rate of 50mV / s, and 20 scan cycles to obtain indium oxide composite particles.

[0055] S2: Indium oxide composite particles, tin oxide, rare earth oxides, dispersant and stabilizer are mixed, pure water is added, and the mixture is ball-milled at 450 rpm for 12 h. Then, a binder is added and the grinding continues to obtain a mixed slurry with a solid content of 28%. The mixed slurry is then placed in a spray drying tower for spray granulation at a temperature of 240 ℃. After sieving, an oxide mixed powder with an average particle size of 30-50 μm is obtained.

[0056] S3: The oxide mixed powder is pre-pressed at 35 MPa for 15 min, then cold isostatically pressed at 400 MPa for 30 min to obtain an oxide preform. The oxide preform is then heat-treated by heating to 500℃ at a heating rate of 2.0℃ / min and holding for 60 min, then heating to 1550℃ at a heating rate of 1.5℃ / min and holding for 11 hours, and finally cooling to room temperature at a cooling rate of 1.0℃ / min to obtain a high-density, high-mobility indium oxide doped target.

[0057] Example 9

[0058] The difference between Example 9 and Example 8 is that the high-density, high-mobility indium oxide doped target material also includes 4 kg of polyvinylpyrrolidone.

[0059] The preparation method of high-density, high-mobility indium oxide doped target includes the following specific steps:

[0060] S1: Indium oxide was pre-cleaned sequentially with ammonia, water, and anhydrous ethanol. Chloroauric acid and potassium chloride were mixed in a mass ratio of 1:5 to form a chloroauric acid-potassium chloride solution. Indium oxide was then added to the chloroauric acid-potassium chloride solution and kept at a constant temperature of 25°C in a water bath. Oxygen was removed by nitrogen for 10 min. Gold nanoparticles were deposited on the surface of the indium oxide particles using cyclic voltammetry. The electroplating parameters were: potential range of (-0.3V)-(-1.15V), scan rate of 50mV / s, and 20 scan cycles, to obtain indium oxide composite particles. Polyvinylpyrrolidone was then dissolved in n-butanol and mixed with the indium oxide composite particles. The mixture was heated to boiling and stirred for 2 h. After cooling to room temperature, the particles were filtered, washed, and dried at a constant temperature of 110°C to obtain modified indium oxide particles.

[0061] S2: Modified indium oxide particles, tin oxide, rare earth oxides, dispersant and stabilizer are mixed, pure water is added, and the mixture is ball-milled at 450 rpm for 12 h. Then, a binder is added and the mixture is further ground to obtain a mixed slurry with a solid content of 28%. The mixed slurry is then placed in a spray drying tower for spray granulation at a temperature of 240 ℃. After sieving, an oxide mixed powder with an average particle size of 30-50 μm is obtained.

[0062] S3: The oxide mixed powder is pre-pressed at 35 MPa for 15 min, then cold isostatically pressed at 400 MPa for 30 min to obtain an oxide preform. The oxide preform is then heat-treated by heating to 500℃ at a heating rate of 2.0℃ / min and holding for 60 min, then heating to 1550℃ at a heating rate of 1.5℃ / min and holding for 11 hours, and finally cooling to room temperature at a cooling rate of 1.0℃ / min to obtain a high-density, high-mobility indium oxide doped target.

[0063] Example 10

[0064] The difference between Example 10 and Example 9 is that the amount of polyvinylpyrrolidone used in the high-density, high-mobility indium oxide doped target material is 3 kg, and the amount of chloroauric acid used is 1 kg.

[0065] Example 11

[0066] The difference between Example 11 and Example 9 is that the amount of polyvinylpyrrolidone used in the high-density, high-mobility indium oxide doped target material is 5 kg, and the amount of chloroauric acid used is 3 kg.

[0067] Comparative Example

[0068] Comparative Example 1

[0069] The difference between Comparative Example 1 and Example 1 is that rare earth oxides are not used in the high-density, high-mobility indium oxide doped target material.

[0070] Comparative Example 2

[0071] The difference between Comparative Example 2 and Example 1 is that no binder is used in the high-density, high-mobility indium oxide doped target material.

[0072] Comparative Example 3

[0073] The difference between Comparative Example 3 and Example 1 is that polyvinyl alcohol is not used in the high-density, high-mobility indium oxide doped target material.

[0074] The performance testing was conducted on the high-density, high-mobility indium oxide doped targets provided in Examples 1-11 and Comparative Examples 1-3 of this application. The specific test results are shown in Table 1.

[0075] Detection methods

[0076] I. Density

[0077] The density of the high-density, high-mobility indium oxide doped target prepared in this application was tested using the Archimedes density method, and the relative density was calculated based on the true density.

[0078] II. Mobility

[0079] The high-density, high-mobility indium oxide doped target prepared in this application was tested using the Hall effect method, and the carrier mobility was calculated.

[0080] Table 1: Performance Test Results

[0081]

[0082]

[0083] The performance test results show that in Examples 1-7, the synergistic effect of each component promotes the high mobility and density of the indium oxide target prepared in this application. In Examples 8-11, adding appropriate amounts of chloroauric acid and polyvinylpyrrolidone to the indium oxide target raw material further improves the mobility and density of the indium oxide target. This further demonstrates that depositing gold nanoparticles on the surface of indium oxide particles can improve the mobility of the indium oxide target, and then modifying the surface of the indium oxide particles with polyvinylpyrrolidone can further improve the dispersibility of the indium oxide particles in the target, thereby increasing the density of the indium oxide target.

[0084] A comparison of Comparative Examples 1, 2, 3 and Example 1 shows that Comparative Example 1, which does not use rare earth oxides, has a significantly reduced target density and mobility. Comparative Example 2, which does not use binders, and Comparative Example 3, which does not use polyvinyl alcohol, both have an impact on the target density. This further illustrates that the existing single indium oxide target has low density and mobility, which limits the application of indium oxide targets.

[0085] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A high-density high-mobility indium oxide-doped target material, characterized by, The raw materials include the following weight parts: indium oxide 90-98 parts, tin oxide 5-8 parts, rare earth oxide 1-3 parts, binder 0.5-1.5 parts, dispersant 0.5-0.8 parts, stabilizer 0.3-0.5 parts, chloroauric acid 1-3 parts, and polyvinylpyrrolidone 3-5 parts; the binder is carboxymethyl cellulose and polyvinyl alcohol; nano gold particles are deposited on the surface of the indium oxide by chloroauric acid in advance to form indium oxide composite particles, then the polyvinylpyrrolidone is dissolved and mixed with the indium oxide composite particles and heated, cooled after reaction, filtered and washed to obtain modified indium oxide particles; The preparation method of the high-density high-mobility indium oxide doped target material comprises the following specific steps: The indium oxide, tin oxide, rare earth oxide, binder, dispersant and stabilizer are mixed and ground, and then spray granulation, die pressing and cold isostatic pressing are sequentially performed to obtain a green body, and then the green body is sintered to obtain the high-density high-mobility indium oxide doped target material; the sintering comprises heat treatment and high-temperature sintering, the heat treatment temperature is 400-600 DEG C, and the high-temperature sintering is 1500-1600 DEG C.

2. The high-density high-mobility indium oxide-doped target material of claim 1, wherein, The rare earth oxide is at least one of lanthanum oxide, praseodymium oxide, neodymium oxide and yttrium oxide.

3. The high density high mobility indium oxide doped target of claim 1, wherein, The dispersant is one of polyacrylic acid and polyethylene glycol.

4. The high density high mobility indium oxide doped target of claim 1, wherein, The stabilizer is at least one of magnesium oxide, aluminum oxide and zirconium oxide.

5. A method of producing a high-density high-mobility indium oxide-doped target according to any one of claims 1 to 4, characterized by, The method comprises the following specific steps: The indium oxide, tin oxide, rare earth oxide, binder, dispersant and stabilizer are mixed and ground, and then spray granulation, die pressing and cold isostatic pressing are sequentially performed to obtain a green body, and then the green body is sintered to obtain the high-density high-mobility indium oxide doped target material; the sintering comprises heat treatment and high-temperature sintering, the heat treatment temperature is 400-600 DEG C, and the high-temperature sintering is 1500-1600 DEG C.

6. The method of producing a high-density high-mobility indium oxide-doped target according to claim 5, characterized by, The die pressing pressure is 25-50 MPa, and the cold isostatic pressing pressure is 350-450 MPa.

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