CN113277549A - Indium tin oxide powder and preparation method thereof - Google Patents
Indium tin oxide powder and preparation method thereof Download PDFInfo
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- CN113277549A CN113277549A CN202110659682.7A CN202110659682A CN113277549A CN 113277549 A CN113277549 A CN 113277549A CN 202110659682 A CN202110659682 A CN 202110659682A CN 113277549 A CN113277549 A CN 113277549A
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Abstract
The invention discloses indium tin oxide powder and a preparation method thereof. The preparation method comprises the following steps: s1: adding metal indium and metal tin into water, and then adding sulfuric acid, heating and dissolving to obtain a mixed solution; s2: evaporating and crystallizing the mixed solution to obtain a mixed solid; s3: mixing the mixed solid, a precipitator, a solvent and a surfactant, performing hydrothermal reaction, centrifuging, washing and drying to obtain an indium tin oxide precursor; s4: and calcining the indium tin oxide precursor to obtain the indium tin oxide powder. According to the invention, the indium and tin metal react with sulfuric acid, and then the mixed solid of indium sulfate and stannous sulfate containing crystal water is obtained through evaporation and crystallization and is used as a raw material for preparing indium tin oxide powder, so that on one hand, the purity of the raw material can be ensured, and further the purity and yield of the indium tin oxide powder are improved; on the other hand, the influence on the quality of the indium tin oxide powder caused by the corrosivity of chloride ions due to the use of a chloride ion-containing raw material is avoided.
Description
Technical Field
The invention belongs to the technical field of indium tin oxide powder production, and particularly relates to indium tin oxide powder and a preparation method thereof.
Background
Indium Tin Oxide (ITO) is mainly characterized by a combination of optical conduction and optical transparency, and is mainly used in the fabrication of liquid crystal displays, organic light emitting diodes, touch screens, and the like. At present, methods for producing indium tin oxide powder at home and abroad mainly comprise a coprecipitation method, a direct sintering method, a hydrothermal method, an electrochemical method and the like. However, the preparation method is different, and the morphology and properties of indium tin oxide are also different, such as: the indium tin oxide powder prepared by the coprecipitation method has the advantages of uneven particle distribution, large morphology difference, serious component segregation and short service life.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention provides an ito powder and a method for preparing the same.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of indium tin oxide powder comprises the following steps:
s1: adding metal indium and metal tin into water, and then adding sulfuric acid, heating and dissolving to obtain a mixed solution;
s2: evaporating and crystallizing the mixed solution to obtain a solid;
s3: mixing the mixed solid, a precipitator, a solvent and a surfactant, performing hydrothermal reaction, centrifuging, washing and drying to obtain an indium tin oxide precursor;
s4: and calcining the indium tin oxide precursor to obtain the indium tin oxide powder.
According to the invention, metal indium and metal tin react with sulfuric acid, and then mixed solid is obtained through evaporation and crystallization and is used as a raw material for preparing indium tin oxide powder, so that on one hand, the purity of the solid in S2 can be ensured, and the purity and yield of indium tin oxide are improved; in another aspect, the mixed solid In S2 is In2(SO4)3·5H2O and SnSO4The mixed solid obtained in S2 is a sulfate of indium and tin containing crystal water, instead of traditional indium chloride tetrahydrate and tin chloride pentahydrate, because chloride ions are corrosive, the service life of the target material is influenced, and SO4 2-The target prepared by the indium tin oxide powder has long service life.
The purities of the metal indium and the metal tin are both more than 4.5N; the indium tin oxide powder is in a powder state, and the indium tin oxide powder is in a nano spherical structure on the microcosmic aspect.
In a preferred embodiment of the present invention, in S3, the precipitant is ethylenediamine, the solvent is ethanol, and the surfactant is polyvinylpyrrolidone.
The ethylenediamine is used as a precipitator, so that particles in a reaction system are uniform and are not easy to agglomerate. The polyvinylpyrrolidone surfactant may facilitate the dissolution of ethylenediamine.
In a preferred embodiment of the present invention, in S3, the mass ratio of the solid, the precipitant, the solvent, and the surfactant is mixed solid: a precipitant: solvent: surfactant 1: 0.1-0.8: 20-50: 1 to 1.5.
The applicant discovers through a great amount of scientific experiments that the indium tin oxide prepared by the method with the addition amounts of the mixed solid, the precipitator, the solvent and the surfactant within the limited range has long service life, high purity and good yield.
In a preferred embodiment of the present invention, in S1, the molar ratio of the metal indium to the metal tin is 2 to 3: 1; the mass ratio of the total mass of the metal indium and the metal tin to the sulfuric acid is 1: 1-1.5.
The amount of water added in S1 according to the present invention is larger than that of the metallic indium and the metallic tin. The invention adds water before adding acid to increase the contact area between acid and metal and increase the reaction rate.
In a preferred embodiment of the present invention, the temperature for heating and dissolving in S1 is 50 to 120 ℃.
In a preferred embodiment of the present invention, the temperature of the evaporative crystallization in S2 is 100 to 150 ℃.
In a preferred embodiment of the present invention, in S3, the hydrothermal reaction temperature is 150 to 250 ℃ and the reaction time is 10 to 15 hours.
The pressure of the hydrothermal reaction is 10-15 kPa.
In a preferred embodiment of the present invention, in S3, the rotation speed of the centrifuge is 2000 to 10000 rpm; washing by using a cleaning agent with the volume ratio of ethanol to water being 3: 1; the drying temperature is 90-120 ℃, and the drying time is 10-12 h.
In a preferred embodiment of the present invention, in S4, the calcination temperature is 300 to 1000 ℃, and the calcination time is 3 to 8 hours.
The indium tin oxide precursor is calcined according to the parameters, so that on one hand, crystal water of the indium tin oxide precursor can be removed to obtain indium tin oxide powder with high purity and high yield; on the other hand, the surfactant and other materials of the indium tin oxide target material can be removed, and the indium tin oxide target material with high purity and longer service life can be obtained.
The invention also claims the indium tin oxide powder prepared by the preparation method of the indium tin oxide powder.
Compared with the prior art, the invention has the following beneficial effects: according to the method, the indium sulfate and stannous sulfate mixed solid containing the crystal water is obtained by reacting the indium metal and the tin metal with the sulfuric acid and then performing evaporative crystallization to serve as a raw material for preparing the indium tin oxide powder, so that on one hand, the purity of the indium sulfate and stannous sulfate mixed solid containing the crystal water can be ensured, and the purity and the yield of the indium tin oxide powder are further improved; on the other hand, the mixed solid of the indium sulfate containing the crystal water and the stannous sulfate obtained in the step S2 is used as a raw material for preparing the indium tin oxide, and the traditional indium chloride tetrahydrate and tin chloride pentahydrate are not used, so that the technical problems that the thickness of the indium tin oxide target is thin, and the density of the target is reduced by chloride ions are solved, and therefore, the target prepared from the indium tin oxide powder is long in service life and high in purity.
Drawings
FIG. 1 is an XRD pattern of ITO powder according to example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of ITO powder according to embodiment 1 of the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The embodiment of the preparation method of the indium tin oxide powder comprises the following specific steps:
s1: adding metal indium, metal tin and pure water with the purity of 4.5N into a dissolving kettle, wherein the pure water is over the metal indium and the metal tin, adding sulfuric acid, raising the temperature to 50 ℃, and carrying out dissolving reaction for 12 hours to obtain a mixed solution; the molar ratio of the metal indium to the metal tin is 2: 1, the mass ratio of the total mass of the metal indium and the metal tin to the sulfuric acid is 1: 1;
s2: evaporating and crystallizing the dissolved mixed solution at the temperature of 100 ℃ to prepare mixed solid;
s3: mixing the mixed solid, ethylenediamine, absolute ethyl alcohol and polyvinylpyrrolidone according to the mass ratio of the mixed solid: ethylene diamine: anhydrous ethanol: polyvinylpyrrolidone ═ 1: 0.1: 20: 1, adding the mixture into a 500ml high-temperature and high-pressure resistant reaction kettle, carrying out hydrothermal reaction at the reaction temperature of 150 ℃ for 10 hours, centrifuging at the centrifugal speed of 2000rpm, washing with a cleaning solution prepared from absolute ethyl alcohol and pure water according to the volume ratio of 3:1, and finally drying at 100 ℃ for 10 hours to obtain an indium tin oxide precursor;
s4: and calcining the indium tin oxide precursor at 300 ℃ for 8h to obtain the indium tin oxide powder.
FIG. 1 is an XRD pattern of ITO powder according to example 1 of the present invention; reference (JCPDS #06-0416) in the figure is the XRD standard card pattern of indium tin oxide, and example 1 is the XRD pattern of the indium tin oxide powder prepared in example 1. From fig. 1, it can be seen that the XRD characteristic peaks of the ito powder prepared in example 1 correspond to those of the ito standard card and are free from impurity peaks, indicating that ito is successfully prepared in the present application.
FIG. 2 is a scanning electron microscope image of ITO powder according to embodiment 1 of the present invention. As can be seen from the figure, the ITO powder is microscopically granular and small.
Example 2
The embodiment of the preparation method of the indium tin oxide powder comprises the following specific steps:
s1: adding metal indium, metal tin and pure water with the purity of 4.5N into a dissolving kettle, wherein the pure water is over the metal indium and the metal tin, adding sulfuric acid, raising the temperature to 120 ℃, and carrying out dissolving reaction for 10 hours to obtain a mixed solution; the molar ratio of the metal indium to the metal tin is 3:1, the mass ratio of the total mass of the metal indium and the metal tin to the sulfuric acid is 1: 1.5;
s2: evaporating and crystallizing the dissolved mixed solution at the temperature of 150 ℃ to prepare mixed solid;
s3: mixing the mixed solid, ethylenediamine, absolute ethyl alcohol and polyvinylpyrrolidone according to the mass ratio of the mixed solid: ethylene diamine: anhydrous ethanol: polyvinylpyrrolidone ═ 1: 0.8: 50: 1.5, adding the mixture into a 500ml high-temperature and high-pressure resistant reaction kettle, carrying out hydrothermal reaction at the reaction temperature of 250 ℃ for 15h, centrifuging at the centrifugal speed of 10000rpm, washing by using absolute ethyl alcohol and pure water according to the volume ratio of 3:1, and finally drying at 90 ℃ for 12h to obtain an indium tin oxide precursor;
s4: and calcining the indium tin oxide precursor at 1000 ℃ for 3h to obtain the indium tin oxide powder.
Example 3
The preparation method of the indium tin oxide powder is only different from the preparation method of the indium tin oxide powder in the embodiment 1: in the step S3, the mass ratio of the mixed solid, the ethylenediamine, the anhydrous ethanol, and the polyvinylpyrrolidone is mixed solid: ethylene diamine: anhydrous ethanol: polyvinylpyrrolidone ═ 1: 0.8: 50: 1.5.
example 4
The preparation method of the indium tin oxide powder is only different from the preparation method of the indium tin oxide powder in the embodiment 1: in the step S3, the mass ratio of the mixed solid, the ethylenediamine, the anhydrous ethanol, and the polyvinylpyrrolidone is mixed solid: ethylene diamine: anhydrous ethanol: polyvinylpyrrolidone ═ 1: 0.4: 35: 1.2.
example 5
The preparation method of the indium tin oxide powder is only different from the preparation method of the indium tin oxide powder in the embodiment 1: in the step S3, the mass ratio of the mixed solid, the ethylenediamine, the anhydrous ethanol, and the polyvinylpyrrolidone is mixed solid: ethylene diamine: anhydrous ethanol: polyvinylpyrrolidone ═ 1: 0.6: 40: 1.4.
example 6
The preparation method of the indium tin oxide powder is only different from the preparation method of the indium tin oxide powder in the embodiment 1: in the step S2, the temperature of the evaporative crystallization is 120 ℃.
Example 7
The preparation method of the indium tin oxide powder is only different from the preparation method of the indium tin oxide powder in the embodiment 1: in the step S2, the temperature of the evaporative crystallization is 130 ℃.
Example 8
The preparation method of the indium tin oxide powder is only different from the preparation method of the indium tin oxide powder in the embodiment 1: in the step S2, the temperature of evaporative crystallization is 150 ℃.
Example 9
The preparation method of the indium tin oxide powder is only different from the preparation method of the indium tin oxide powder in the embodiment 1: in the step S4, the indium tin oxide precursor is calcined at 500 ℃ for 8 h.
Example 10
The preparation method of the indium tin oxide powder is only different from the preparation method of the indium tin oxide powder in the embodiment 1: in the step S4, the indium tin oxide precursor is calcined at 800 ℃ for 8 h.
Example 11
The preparation method of the indium tin oxide powder is only different from the preparation method of the indium tin oxide powder in the embodiment 1: in the step S4, the indium tin oxide precursor is calcined at 1000 ℃ for 8 h.
Comparative example 1
The comparative example of the preparation method of the indium tin oxide powder comprises the following specific steps:
s1: indium chloride tetrahydrate and tin chloride pentahydrate are mixed according to a molar ratio of 2: 1 mixing into a mixed solid;
s2: mixing the mixed solid, ethylenediamine, absolute ethyl alcohol and polyvinylpyrrolidone according to the mass ratio of the mixed solid: ethylene diamine: anhydrous ethanol: polyvinylpyrrolidone ═ 1: 0.1: 20: 1, adding the mixture into a 500ml high-temperature and high-pressure resistant reaction kettle, carrying out hydrothermal reaction at the reaction temperature of 150 ℃ for 10 hours, centrifuging at the centrifugal speed of 2000rpm, washing with a cleaning solution prepared from absolute ethyl alcohol and pure water according to the volume ratio of 3:1, and finally drying at 100 ℃ for 10 hours to obtain an indium tin oxide precursor;
s3: and calcining the indium tin oxide precursor at 300 ℃ for 8h to obtain the indium tin oxide powder.
Comparative example 2
The comparative example of the preparation method of the indium tin oxide powder comprises the following specific steps:
s1: adding metal indium, metal tin and pure water with the purity of 4.5N into a dissolving kettle, wherein the pure water is over the metal indium and the metal tin, adding sulfuric acid, raising the temperature to 50 ℃, and carrying out dissolving reaction for 12 hours to obtain a mixed solution; the molar ratio of the metal indium to the metal tin is 2: 1, the mass ratio of the total mass of the metal indium and the metal tin to the sulfuric acid is 1: 1;
s2: evaporating and crystallizing the dissolved mixed solution at the temperature of 100 ℃ to prepare mixed solid;
s3: mixing the mixed solid, ethylenediamine and absolute ethyl alcohol according to the mass ratio of the mixed solid: ethylene diamine: anhydrous ethanol ═ 1: 0.1: 20, adding the mixture into a 500ml high-temperature and high-pressure resistant reaction kettle, carrying out hydrothermal reaction at the reaction temperature of 150 ℃ for 10 hours, centrifuging at the centrifugal speed of 2000rpm, washing by using a cleaning solution of absolute ethyl alcohol and pure water according to the volume ratio of 3:1, and finally drying at 100 ℃ for 10 hours to obtain an indium tin oxide precursor;
s4: and calcining the indium tin oxide precursor at 300 ℃ for 8h to obtain the indium tin oxide powder.
Comparative example 3
The only difference between the preparation method of the indium tin oxide powder in the comparative example and the preparation method of the indium tin oxide powder in the example 1 is that: in the step S4, the indium tin oxide precursor is calcined at 1100 ℃ for 8 h.
Examples of effects
Test samples: indium tin oxide powders prepared in examples 1 to 11 and comparative examples 1 to 3.
The test method comprises the following steps: and (3) density testing: cooling, statically pressing and sintering a test sample to obtain an indium tin oxide target material, and testing the density of the target material; and testing the resistivity of the test sample by using a four-probe resistivity tester.
TABLE 1 Performance data for ITO targets prepared in examples 1-11 and comparative examples 1-3
As can be seen from Table 1, the ITO targets prepared in examples 1-11 of the present invention have much higher resistivity and higher target density than the ITO targets prepared in comparative examples 1-3. Comparison of the performance data of the target material in the comparative example 1 and the performance data of the target material in the example 1 shows that the indium tin oxide target material prepared by the method of the invention, which uses the mixed solid of indium sulfate containing crystal water and stannous sulfate obtained in S2 as a raw material for preparing indium tin oxide, is better in resistivity and target material compactness than the traditional indium chloride tetrahydrate and stannic chloride pentahydrate. Comparative example 2 is compared with example 1, and shows that the surface activity affects the solubility of reaction components, affects the dispersibility, causes the generated indium tin oxide particles to agglomerate, and further affects the component uniformity, density and resistivity of the target material. Comparative example 3 is compared with example 1, and illustrates that the calcination of the indium tin oxide precursor in step S4 affects the resistivity and the target compactness of the indium tin oxide target prepared from the indium tin oxide powder.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation method of the indium tin oxide powder is characterized by comprising the following steps:
s1: adding metal indium and metal tin into water, and then adding sulfuric acid, heating and dissolving to obtain a mixed solution;
s2: evaporating and crystallizing the mixed solution to obtain a mixed solid;
s3: mixing the mixed solid, a precipitator, a solvent and a surfactant, performing hydrothermal reaction, centrifuging, washing and drying to obtain an indium tin oxide precursor;
s4: and calcining the indium tin oxide precursor to obtain the indium tin oxide powder.
2. The method according to claim 1, wherein in S3, the precipitant is ethylenediamine, the solvent is ethanol, and the surfactant is polyvinylpyrrolidone.
3. The method according to claim 1, wherein in S3, the mass ratio of the mixed solid, the precipitant, the solvent, and the surfactant is mixed solid: a precipitant: solvent: surfactant 1: 0.1-0.8: 20-50: 1 to 1.5.
4. The method for preparing ito powder according to claim 1, wherein the molar ratio of the metallic indium to the metallic tin in S1 is 2 to 3: 1; the mass ratio of the total mass of the metal indium and the metal tin to the sulfuric acid is 1:1 to 1.5.
5. The method according to claim 1, wherein the temperature for heating and dissolving in S1 is 50-120 ℃.
6. The method as claimed in claim 1, wherein the temperature of the evaporation crystallization in S2 is 100-150 ℃.
7. The method of claim 1, wherein the hydrothermal reaction temperature in S3 is 150 ℃ and 250 ℃ and the reaction time is 10-15 h.
8. The method according to claim 1, wherein in S3, the rotation speed of the centrifuge is 2000-10000 rpm; washing by using a cleaning agent with the volume ratio of ethanol to water being 3: 1; the drying temperature is 90-120 ℃, and the drying time is 10-12 h.
9. The method for preparing ITO powder of claim 1, wherein in S4, the calcination temperature is 300-1000 ℃ and the calcination time is 3-8 h.
10. An indium tin oxide powder produced by the method for producing an indium tin oxide powder according to any one of claims 1 to 9.
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