CN102557115B - Preparation method of spherical tin-doped indium oxide nanopowder - Google Patents
Preparation method of spherical tin-doped indium oxide nanopowder Download PDFInfo
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Abstract
The invention provides a preparation method of spherical tin-doped indium oxide nanopowder. The method comprises the steps: (1) weighing a water-soluble indium salt and dissolving the water-soluble indium salt in deionized water, adding a tin salt serving as a doping agent, and fully stirring at room temperature to obtain a mixture solution; (2) adding ammonia water or an ammonia salt into the mixture solution to regulate a pH value to be 9-11 to generate a precursor; (3) transferring the precursor into a reaction kettle, and carrying out hydrothermal synthesis reaction for 3-120 hours at the temperature of 260-360 DEG C to obtain a reaction product; and (4) cooling the reaction product in the reaction kettle to room temperature, and then cleaning the reaction product with the deionized water and drying, thereby obtaining the spherical tin-doped indium oxide nanopowder of nanometer particle diameter. The tin-doped indium oxide nanopowder prepared by using the method disclosed by the invention is spherical in appearance and has the average particle size of being 20-400nm.
Description
Technical field
The present invention relates to the photoelectric functional material field, more specifically relate to a kind of hydrothermal synthesis method for preparing spherical tin-doped indium oxide nanopowder.
Background technology
Electrically conducting transparent tin-doped indium oxide semiconductor material is due to its special optical characteristics and electrology characteristic, a lot of fields have been widely used in, as liquid-crystal display (LCD), plasma display (PDP), Organic Light Emitting Diode (OLED) and solar cell etc.In transparent conductive oxide family, tin-doped indium oxide is current technical development and the most ripe material of application.N-shaped semiconductor material as a kind of electrically conducting transparent.Due to its characteristic that there is stable chemistry and mechanical property and have electrically conducting transparent concurrently, also there is no to find to substitute its transparent conductive material at present.Those skilled in the art still is devoted to study new technology of preparing (comprising the technology of preparing of tin-doped indium oxide nano powder and moulding and the sintering technology of tin-doped indium oxide sputtering target material) at present, and wish by the quality and performance that should be used for improving product of new technology, improve the utilization ratio of target product, and then reduce costs.
The method for preparing at present nano-powder has coprecipitation method, thermal evaporation, chemical Vapor deposition process and hydrothermal synthesis method etc.But the main method prepared for tin-doped indium oxide has high temperature gas phase method and liquid phase method.What liquid phase method was widely applied is coprecipitation method, and that hydrothermal method application prepares tin-doped indium oxide nano powder is still rare.Hydrothermal synthesis method is compared with other synthetic technologys, and the powder degree of crystallinity of the method synthesized is high, and crystalline state is complete, and diameter of particle narrow distribution range and pattern are easy to control.For industrial production, with other synthetic methods, compare, hydrothermal synthesis method technique is relatively simple, synthesis condition is easy to control, there is higher production efficiency and lower production cost, synthetic powder has the characteristics of single dispersion, and even particle size distribution, without carrying out roasting, can obtain highly purified tin-doped indium oxide nano powder.
Chinese patent CN1412117A and CN101117236A disclose the method for utilizing aqua-solution method to prepare tin-doped indium oxide nano powder.It is that solute mixes and soluble in water by a certain percentage that the method all adopts indium salt and pink salt, and by adding basic solvent as sodium hydroxide, potassium hydroxide and other chemical substances are as various acid, alcohol etc., pass through again suction filtration, drying, high-temperature roasting and make tin-doped indium oxide nano powder.Although the method can prepare varigrained tin-doped indium oxide nano powder, its technological process is comparatively complicated, and process is wayward, can not effectively control the pattern of powder.But also there is the deficiency of two aspects: the one, used a large amount of chemical reagent, as alcohol, alkali, acid etc., not only increased production cost, and can work the mischief and pollute operator and environment; It two is that the powder of the method synthesized must just can obtain the tin-doped indium oxide nano powder of different-grain diameter through roasting at a certain temperature.And the roasting powder has not only increased manufacturing cost, also increased preparation cycle.The drawbacks such as the powder that simultaneously prepared by roasting method has easy reunion, and particle diameter is wayward.
In addition, Chinese patent CN1978323A has announced a kind of solvent-thermal method that utilizes and has prepared tin-doped indium oxide nano powder.The method is utilized the alkoxide of indium and tin, nitrate, the inferior salt of sulfuric acid etc. are soluble in water, add a large amount of complexing agents as tartrate, amino acid, ethylene glycol simultaneously, glycerol, the organic solvents such as methyl ethyl diketone, carry out hydro-thermal reaction 3-24 hour through the 130-260 degree, can obtain the tin-doped indium oxide powder of particle diameter 6-25 nanometer.The method has also been used a large amount of organic chemical reagents, has not both met the requirement of green environmental protection technique, has also increased production cost, and the particle diameter that simultaneously prepares powder is too little, is unfavorable for the later stage preparation of target materials.
Summary of the invention
It is simple that technical problem to be solved by this invention is to provide a kind of method, the method of synthetic tin-doped indium oxide nano powder with low cost, described method can be in the situation that with an organic solvent and without calcination process directly do not prepare tin-doped indium oxide nano powder.
In order to solve the problems of the technologies described above, the invention provides a kind of method for preparing spherical tin-doped indium oxide nano powder by hydrothermal synthesis method, the method comprises the steps:
(1) take water-soluble indium salt and it dissolved in deionized water, then adding the pink salt as doping agent, after at room temperature fully stirring, obtaining mixing solutions,
(2) in described mixing solutions, add ammoniacal liquor or ammonium salt to adjust pH=9-11, generate presoma;
(3) described presoma is moved in reactor, carry out hydrothermal synthesis reaction 3-120 hour and obtain reaction product at the temperature of 260-360 degree centigrade;
(4) reaction product is cooled in reactor to room temperature, then, with deionized water cleaning reaction product and after drying, can obtains the spherical tin-doped indium oxide powder of nanometer particle size.
In a preferred embodiment of the invention, described water-soluble indium salt is selected from indium chloride, indium nitrate, indium sulfate, indium acetate or their combination.
In a preferred embodiment of the invention, described pink salt is selected from tin chloride, nitric acid tin, tin sulphate, tin acetate or their combination.
In a preferred embodiment of the invention, described ammonium salt is bicarbonate of ammonia.
In a preferred embodiment of the invention, the concentration of the water-soluble indium salt in described mixing solutions is 0.1～5.0mol/L, is preferably 0.5～4.0mol/L.
In a preferred embodiment of the invention, described in step (1), the molar ratio of pink salt and water-soluble indium salt is 0.01-0.30, is preferably 0.01-0.1, the mol ratio based on tin ion and indium ion.
In a preferred embodiment of the invention, the hydrothermal synthesis reaction in step (3) preferably carries out 6-48 hour.
Method of the present invention has following useful technique effect:
1. the pattern of prepared nanometer tin doped indium oxide powder is approximately spherical, and median size is 20-400nm;
2. not with an organic solvent, having avoided the harm to human body of contaminate environment and organic chemical reagent, is a kind of eco-friendly technology of preparing;
3. preparation technology is simple and the cycle is short;
4. synthetic powder, without calcination process, without grinding, directly can obtain the nanometer tin doped indium oxide powder of single dispersion, for industrial production, has simplified production technique, has reduced equipment investment, has reduced production cost, is applicable to scale operation;
5. prepared spherical powder is conducive to the sintering of target, and the relative density of sintered compact can reach more than 99%, and grain-size is less than 4 microns;
6. parallel lamination and/or the parallel vertical of biscuit in sintering oven arranged modes of emplacement, not only improved target list furnace output, and is beneficial to preparation high-density target;
7. utilize the slurry casting forming technique, can obtain large-size target, overall dimension can reach 400mm to 800mm.
The accompanying drawing explanation:
The TEM figure that Fig. 1 is prepared tin-doped indium oxide powder in embodiment 6.
Embodiment:
In the method for the invention, at first water-soluble indium salt is dissolved in deionized water, thereby then add as the pink salt of doping agent and at room temperature fully stir and obtain mixing solutions in order to mixture is fully dissolved; With adding ammoniacal liquor or ammonium salt to adjust pH=9-11 in backward described mixing solutions, generate presoma; Presoma is moved in reactor, and described reactor preferred liner has tetrafluoroethylene or is coated with the alkali corrosion resistance metal inner lining of impregnating material, and reacts 3-120 hour at the temperature of 260-360 degree centigrade; Reaction makes reaction product naturally cool to room temperature in reactor after finishing, and then from reactor, takes out reaction product washed with de-ionized water 1～5 time, and then dries, thereby can obtain the tin-doped indium oxide powder.Pattern by transmission electron microscopy analysis (TEM) observable gained tin-doped indium oxide powder is also measured its median size.
The tin-doped indium oxide powder that utilizes aforesaid method to prepare can prepare highdensity tin-doped indium oxide target.At first take as above the tin-doped indium oxide powder of preparation, add binding agent for example after polyvinyl alcohol granulation, compression molding or slurry casting moulding obtain molding biscuit; Then the parallel lamination of molding biscuit and/or parallel vertical be arranged in high temperature resistant compound rest and send in stove, stacking number of plies 3-5 layer, interlamellar spacing 3-6 centimetre; It is standard that the columns that parallel vertical arrange to be placed mainly be take workspace size in stove, and the general shared total spatial of biscuit is advisable to be no more than 70% of workspace in stove, and column pitch is 3-5 centimetre; After skimming treatment, be heated to the temperature of 1300-1650 ℃ with the temperature rise rate of 1-10 ℃/min, then pass into the oxygen that flow is 0.5-38L/min, and keep furnace pressure 0.6-1.2 * 10
5handkerchief, thus carry out with this understanding sintering, and sintering time continues 5-20 hour; Make sintered compact can obtain the tin-doped indium oxide target after cooling in stove, the density of gained target is more than 99% of tin-doped indium oxide theoretical density, and the overall dimension of gained target can reach 400mm * 800mm * 12mm.
Below by some specific embodiments, the present invention is further illustrated, and purpose is that help is understood content of the present invention and not limits the scope of the invention.
Embodiment
Embodiment 1
Take the indium chloride of 3.5 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 0.5mol/L.The tin chloride that adds again 0.35 mole, the mol ratio that makes tin ion and indium metal ion is 0.1, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 260 degrees celsius, hydrothermal treatment consists is 6 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the tin-doped indium oxide powder of single dispersion.By tem analysis, can determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 20nm left and right.
Embodiment 2
Take the indium chloride of 3.5 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 0.5mol/L.The tin chloride that adds again 0.35 mole, the mol ratio that makes tin ion and indium metal ion is 0.1, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 300 degrees celsius, hydrothermal treatment consists is 6 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the tin-doped indium oxide powder of single dispersion.Crossing tem analysis can determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 50nm left and right.
Embodiment 3
Take the indium chloride of 3.5 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 0.5mol/L.The tin chloride that adds again 0.35 mole, the mol ratio that makes tin ion and indium metal ion is 0.1, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 360 degrees celsius, hydrothermal treatment consists is 6 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the tin-doped indium oxide powder of single dispersion.By tem analysis, determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 100nm left and right.
Embodiment 4
Take the indium chloride of 3.5 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 0.5mol/L.The tin chloride that adds again 0.35 mole, the mol ratio that makes tin ion and indium metal ion is 0.1, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 360 degrees celsius, hydrothermal treatment consists is 12 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the tin-doped indium oxide powder of single dispersion.By tem analysis, determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 150nm left and right.
Embodiment 5
Take the indium chloride of 3.5 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 0.5mol/L.The tin chloride that adds again 0.35 mole, the mol ratio that makes tin ion and indium metal ion is 0.1, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 360 degrees celsius, hydrothermal treatment consists is 24 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the tin-doped indium oxide powder of single dispersion.By tem analysis, determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 350-400nm left and right.
Embodiment 6
Take the indium chloride of 3.5 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 0.5mol/L.The tin chloride that adds again 0.175 mole, the mol ratio that makes tin ion and indium metal ion is 0.05, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 300 degrees celsius, hydrothermal treatment consists is 6 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the tin-doped indium oxide powder of single dispersion.The TEM figure that Fig. 1 is tin-doped indium oxide powder prepared in embodiment 6.By tem analysis, determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 80nm left and right.
Embodiment 7
Take the indium chloride of 28 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 4.0mol/L.The nitric acid tin that adds again 0.28 mole, the mol ratio that makes tin ion and indium metal ion is 0.01, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 300 degrees celsius, hydrothermal treatment consists is 6 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the tin-doped indium oxide powder of single dispersion.By tem analysis, determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 40nm left and right.
Embodiment 8
Take the indium chloride of 3.5 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 0.5mol/L.The nitric acid tin that adds again a certain amount of 0.35 mole, the mol ratio that makes tin ion and indium metal ion is 0.1, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=10 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 300 degrees celsius, hydrothermal treatment consists is 48 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the white tin-doped indium oxide powder of single dispersion.By tem analysis, determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 200nm left and right.
Embodiment 9
Take the indium sulfate of 3.5 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 0.5mol/L.The tin sulphate that adds again 0.035 mole, the mol ratio that makes tin ion and indium metal ion is 0.01, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 300 degrees celsius, hydrothermal treatment consists is 6 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the white tin-doped indium oxide powder of single dispersion.By tem analysis, determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 30-35nm left and right.
Embodiment 10
Take the indium nitrate of 3.5 moles and be dissolved in 7 liters of ionized waters, being mixed with the solution that volumetric molar concentration is 0.5mol/L.The nitric acid tin that adds again 0.35 mole, the mol ratio that makes tin ion and indium metal ion is 0.1, at room temperature after abundant stirring and dissolving, drip 25% ammoniacal liquor to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 300 degrees celsius, hydrothermal treatment consists is 6 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the white tin-doped indium oxide powder of single dispersion.By tem analysis, determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 40-50nm left and right.
Embodiment 11
Take the indium chloride of 7 moles and be dissolved in 7 liters of deionized waters, being mixed with the solution that volumetric molar concentration is 1.0mol/L.The nitric acid tin that adds again 0.7 mole, the mol ratio that makes tin ion and indium metal ion is 0.1, at room temperature after abundant stirring and dissolving, drip bicarbonate of ammonia to pH value of solution=11 with autotitrator, solution is proceeded to the tetrafluoroethylene of 10L or be coated with in the stainless steel cauldron of alkali corrosion resistance metal inner lining of impregnating material, the compactedness of reactor is 70%, and under 300 degrees celsius, hydrothermal treatment consists is 6 hours.Product, through deionized water wash approximately 5 times, is removed acid ion and foreign ion, dries 6-12 hour under 100 degrees centigrade, can obtain the tin-doped indium oxide powder of single dispersion.By tem analysis, determine, in described tin-doped indium oxide powder, the pattern of particle is spherical, and median size is in the 60-70nm left and right.
Claims (9)
1. a method for preparing tin-doped indium oxide nano powder, the method comprises the steps:
(1) take water-soluble indium salt and it dissolved in deionized water, then adding the pink salt as doping agent, and obtaining mixing solutions after at room temperature fully stirring,
(2) in described mixing solutions, add ammoniacal liquor or ammonium salt to adjust pH=9-11, generate presoma,
(3) described presoma is moved in reactor, carry out hydrothermal synthesis reaction 6-120 hour and obtain reaction product at the temperature of 260-360 degree centigrade, and
(4) reaction product is cooled in reactor to room temperature, then, with deionized water cleaning reaction product and after drying, can obtains the spherical tin-doped indium oxide powder of nanometer particle size.
2. according to the process of claim 1 wherein that described water-soluble indium salt is selected from indium chloride, indium nitrate, indium sulfate, indium acetate or their combination.
3. according to the process of claim 1 wherein that described pink salt is selected from tin chloride, nitric acid tin, tin sulphate, tin acetate or their combination.
4. according to the process of claim 1 wherein that described ammonium salt is bicarbonate of ammonia.
5. according to the process of claim 1 wherein that the concentration of described water-soluble indium salt is 0.1～5.0mol/L.
6. according to the method for claim 5, the concentration of wherein said water-soluble indium salt is 0.5～4.0mol/L.
7. according to the process of claim 1 wherein that the molar ratio at pink salt described in step (1) and water-soluble indium salt is 0.01-0.30, the mol ratio based on tin ion and indium ion.
8. according to the method for claim 7, wherein the molar ratio at pink salt described in step (1) and water-soluble indium salt is 0.01-0.1, the mol ratio based on tin ion and indium ion.
9. according to the process of claim 1 wherein that described hydrothermal synthesis reaction carries out 6-48 hour.
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Address after: 753000 No. 119 metallurgical Road, Dawukou District, Shizuishan, the Ningxia Hui Autonomous Region Co-patentee after: NATIONAL ENGINEERING RESEARCH CENTER FOR SPECIAL METAL MATERIALS OF TANTALUM AND NIOBIUM. Patentee after: NORTHWEST RARE METAL MATERIALS RESEARCH INSTITUTE NINGXIA Co.,Ltd. Address before: 753000 No. 119 metallurgical Road, Dawukou District, Shizuishan, the Ningxia Hui Autonomous Region Co-patentee before: NATIONAL ENGINEERING RESEARCH CENTER FOR SPECIAL METAL MATERIALS OF TANTALUM AND NIOBIUM. Patentee before: NORTHWEST RARE METAL MATERIAL Research Institute |
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Effective date of registration: 20180716 Address after: 753000 No. 119 metallurgical Road, Dawukou District, Shizuishan, the Ningxia Hui Autonomous Region Patentee after: Ningxia medium color new materials Co.,Ltd. Address before: 753000 No. 119 metallurgical Road, Dawukou District, Shizuishan, the Ningxia Hui Autonomous Region Co-patentee before: NATIONAL ENGINEERING RESEARCH CENTER FOR SPECIAL METAL MATERIALS OF TANTALUM AND NIOBIUM. Patentee before: NORTHWEST RARE METAL MATERIALS RESEARCH INSTITUTE NINGXIA Co.,Ltd. |