CN112457025B - Preparation method of nano ITO powder with large specific surface area - Google Patents
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Abstract
The invention relates to a preparation method of nano ITO powder with large specific surface area, which comprises the following steps: dissolving metal indium in dilute acid solution, and adding saturated solution of stannic chloride; adding a precipitator, controlling the reaction temperature to be 60-80 ℃, and controlling the pH value of the reaction liquid to be 6.5-7.5; adding a conversion agent, controlling the pH value of the feed liquid to be 9.0-10.0, heating to near boiling, and keeping the temperature for 20-40 min; adding a neutralizing agent, and controlling the pH value of the feed liquid to be 6.5-7.5; cleaning, filtering and drying; decomposing, cooling, pulverizing, and sieving. The preparation method has the advantages of wide raw material sources, simple process, mild reaction conditions, safety and no pollution, the purity of the prepared nano ITO powder exceeds 99.995 percent, the particle size is less than 50nm, the specific surface area exceeds 60 square meters per gram, the maximum reaches 120 square meters per gram, and the relative density of the target material exceeds 99.7 percent, thereby being capable of meeting the requirement of film coating with higher performance.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method of nano ITO powder with large specific surface area.
Background
The nanometer ITO powder is a novel multifunctional inorganic material for the 21 st century, shows a plurality of special properties due to the characteristics of grain fineness and large specific surface area, shows a plurality of special functions in the aspects of conductivity, optics, magnetism and the like, has more important application value in a plurality of fields of ITO target materials, chemical industry, electronics, optics and the like, and has magical effect which cannot be compared with the common ITO powder. The excellent performance and the attractive application prospect of the nano ITO powder enable the research and development and the production of the nano ITO powder to have great potential market.
The conventional method for preparing ITO powder: firstly, mixing indium oxide and tin oxide powder by a mechanical method, and then calcining to obtain the indium oxide-tin oxide powder; another method for preparing the ultrafine composite powder is an aqueous solutionThe method comprises the following steps. Adding precipitant into the mixed metal salt solution containing indium and tin ions, because the dissociated ions exist in the solution in a uniform phase, obtaining precipitates consisting of various uniform phases of components after reaction, and then carrying out heat treatment to obtain the ultrafine ITO particles. The traditional method has the following disadvantages: 1. in the mechanical method, due to the agglomeration of particles, the mixing uniformity of different oxides in the ITO powder is limited, the quality of the ITO target material is influenced, and further the conductivity, the light transmittance and the adhesion with the substrate of the ITO film are influenced; 2. the hydrolysis environment of the aqueous solution method can only be carried out in nitrate and organic salt solution, and only specific precipitating agents such as urea, hexamethylenetetramine and the like can be used, so that the production process has high cost, complex process conditions, difficult control of hydrolysis conditions, long reaction time and difficult realization of large-scale industrialization; the hydrolysis environment is carried out in inorganic salt solution, and soda ash, caustic soda or ammonia water and the like are used as hydrolysis precipitating agents, the production process is relatively simple, but the specific surface area of the product is less than 30m 2 (g), poor performance.
Chinese patent application document "preparation method of nano-grade indium tin oxide composite powder (grant publication number: CN 100554204)", discloses a process for preparing nano-grade indium tin oxide composite powder by coprecipitation method, which is characterized in that metal indium and metal tin are respectively dissolved by inorganic strong acid or mixed strong acid aqueous solution, or soluble metal indium salt and metal tin salt are dissolved in water, the prepared two solutions are mixed, precipitating agent is added under the condition of strongly stirring the mixed solution to generate indium tin coprecipitate, after washing with water, washing with organic solvent and solid-liquid separation, organic solvent is added to carry out azeotropic distillation, filter cake is dried, scattered and calcined to obtain ultrafine ITO composite powder. The invention has the advantages that the ITO target material sintered by the indium tin oxide powder prepared by the process through a simple process has the relative theoretical density of more than 99 percent; the method has the disadvantages that azeotropic distillation is required in an organic solvent in which water and ethanol exist, the process conditions are complex, the purity of the product is influenced by adopting the organic solvent, and the method is not environment-friendly; the specific surface area of the prepared powder particles is 30-60 square meters per gram, and the requirement of film coating with higher performance is difficult to meet.
Disclosure of Invention
The invention aims to provide a preparation method of nano ITO powder with large specific surface area, which has the advantages of low cost, simple production process, convenient operation, safety and no pollution, and solves the problems of complex process, generally low specific surface area and the like in the prior art of common ITO powder.
The technical scheme adopted by the invention is as follows:
a preparation method of nano ITO powder with large specific surface area comprises the following steps:
s1: acid dissolution: dissolving metallic indium In dilute acid solution, heating to near boiling, after indium is completely dissolved, converting In from mixed solution 2 O 3 With SnO 2 Adding a saturated solution of tin tetrachloride according to the mass ratio of 9:1, and uniformly stirring to obtain a mixed solution with the total concentration of indium and tin ions of 2-4 mol/L;
s2: and (3) precipitation: adding a precipitator into the mixed solution, controlling the reaction temperature to be 60-80 ℃, the reaction time to be 30-50 min, continuously stirring until the precipitation is complete, and controlling the pH value of the feed liquid to be 6.5-7.5;
s3: and (3) transformation: adding a conversion agent into the feed liquid, controlling the pH value of the feed liquid to be 9.0-10.0, heating to be close to boiling, and then preserving heat for 20-40 min;
s4: neutralizing: adding a neutralizing agent into the feed liquid, and controlling the pH of the feed liquid to be 6.5-7.5;
s5: cleaning, filtering and drying: carrying out liquid-solid separation on the feed liquid after the neutralization reaction is finished, washing filter residues until no chloride ions exist, and then drying at 50-150 ℃ and-0.1-1.0 MPa to obtain dry powder;
s6: and (3) decomposition and crushing: calcining and decomposing the dried powder at 300-600 ℃, and preserving heat for 50-70 min; and cooling the completely decomposed material to room temperature, and then crushing and screening to obtain the nano ITO powder.
Further, in step S1, the dilute acid solution is one of dilute sulfuric acid, dilute hydrochloric acid, or dilute nitric acid, and the concentration is 6 to 12 mol/L.
Further, in the step S1, the saturated solution of tin tetrachloride is prepared from analytically pure tin tetrachloride pentahydrate crystals.
Further, in step S2, the precipitant is one of ammonium bicarbonate, sodium bicarbonate or potassium bicarbonate.
Further, in step S2, the precipitant is ammonium bicarbonate.
Further, in the step S2, the stirring speed is 50-100 r/min.
Further, in step S3, the converting agent is ammonia water.
Further, in step S3, the temperature rise rate is 5 to 10 ℃/min.
Further, in step S4, the neutralizing agent is acetic acid.
Further, in the step S6, the particle size of the nano ITO powder is 20 to 50 nm.
The invention has the beneficial effects that:
1. the initial concentration of the indium ion concentration has certain influence on the quality of the nano ITO product, the indium ion concentration is too low, the reaction rate and the conversion rate are low, impurities are easy to adsorb, the indium ion concentration is too high, and agglomeration is easy to generate.
2. The method adopts a weakly alkaline substance as a precipitator, the reaction is carried out under a near-neutral condition, the reaction condition is mild, the particle size of the product basic carbonate is relatively uniform, but the basic carbonate contains much crystal water and is difficult to clarify and difficult to filter; firstly, under the condition of adding ammonia water and heating to be close to boiling, the generated basic carbonate precipitate can be promoted to be completely converted into hydroxide precipitate, the conversion is carried out between solid phases, the generated hydroxide has fine particle size, is loose and porous, and can effectively increase the specific surface area; secondly, a buffer solution can be formed with ammonium chloride in the precipitation mixed solution, and the pH value of the solution is controlled to be 9.0-10.0, so that metal impurities such as zinc, copper, cobalt, nickel and the like can be effectively separated, and the purity of the product is improved; thirdly, adding ammonia water to further convert the indium ions which are not completely reacted into indium hydroxide precipitate, thereby improving the yield of the product; the hydroxide precipitate does not contain crystal water, and the solution is adjusted to be neutral by acid, so that the problems that the product is not easy to filter and the impurities are not easy to clean can be well solved.
3. The invention reasonably designs a combined process of precipitation and conversion, wherein the precipitation step adopts a low-temperature high-rotation-speed process, and regular fine-granularity carbonate crystal seeds can be prepared; the nucleation speed of the hydroxide can be accelerated and promoted by the action of the crystal seeds and the reasonable control of the temperature rise rate in the conversion process, and the problem of uneven particle size distribution is effectively avoided.
4. The method has mild reaction conditions, smooth operation process, good continuity, low cost, simple production process and convenient operation, can prepare the high-performance nano ITO powder with the purity of more than 99.995 percent, the particle size of less than 50nm, the minimum of 20nm, the specific surface area of more than 60 square meters per gram, the maximum of 120 square meters per gram and the relative target density of more than 99.7 percent as described in example 4, can meet the requirement of film coating of higher-performance films, has great prospect and is suitable for popularization and application.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A preparation method of nano ITO powder with large specific surface area comprises the following steps:
s1: acid dissolution: dissolving metal indium In dilute sulfuric acid solution with the concentration of 6mol/L, heating to be close to boiling, and after indium is completely dissolved, converting In the mixed solution 2 O 3 With SnO 2 Adding saturated solution of stannic chloride according to the mass ratio of 9:1, and uniformly stirring to obtain mixed solution with the total concentration of indium and tin ions being 2 mol/L; the saturated solution of the stannic chloride is prepared by analytically pure stannic chloride pentahydrate crystals;
s2: and (3) precipitation: adding sodium bicarbonate into the mixed solution, controlling the reaction temperature at 60 ℃, the reaction time at 30min, continuously stirring at the stirring speed of 50r/min until the precipitation is complete, and controlling the pH value of the feed liquid at 6.5;
s3: and (3) transformation: adding ammonia water into the feed liquid, controlling the pH value of the feed liquid to be 9.0, heating to be close to boiling, wherein the heating rate is 5 ℃/min, and then keeping the temperature for 20 min;
s4: neutralizing: adding acetic acid into the feed liquid, and controlling the pH of the feed liquid to be 6.5;
s5: cleaning, filtering and drying: carrying out liquid-solid separation on the feed liquid after the neutralization reaction is finished, washing filter residues with deionized water until no chloride ion exists, and then drying at 50 ℃ and-0.1 MPa to obtain dry powder;
s6: and (3) decomposition and crushing: calcining the dried powder at 300 deg.C for decomposition, and maintaining the temperature for 50 min; cooling the completely decomposed materials to room temperature, pulverizing, and sieving to obtain material with particle diameter of 20nm and specific surface area of 120m 2 Nano ITO powder per gram.
Example 2
A preparation method of nano ITO powder with large specific surface area comprises the following steps:
s1: acid dissolution: dissolving indium metal In dilute hydrochloric acid solution with the concentration of 9mol/L, heating to be nearly boiling, and after indium is completely dissolved, converting In the mixed solution 2 O 3 With SnO 2 Adding saturated solution of stannic chloride according to the mass ratio of 9:1, and uniformly stirring to obtain mixed solution with the total concentration of indium and stannic ions being 3 mol/L; the saturated solution of the stannic chloride is prepared by analytically pure stannic chloride pentahydrate crystals;
s2: and (3) precipitation: adding ammonium bicarbonate into the mixed solution, controlling the reaction temperature at 70 ℃, the reaction time at 40min, continuously stirring at the stirring speed of 75r/min until the precipitation is complete, and controlling the pH value of the feed liquid at 7.0;
s3: and (3) transformation: adding ammonia water into the feed liquid, controlling the pH value of the feed liquid to be 9.5, heating to be close to boiling, wherein the heating rate is 8 ℃/min, and then preserving heat for 30 min;
s4: neutralizing: adding acetic acid into the feed liquid, and controlling the pH value to be 7.0;
s5: cleaning, filtering and drying: carrying out liquid-solid separation on the feed liquid after the neutralization reaction is finished, washing filter residues by deionized water until no chloride ion exists, and then drying at 100 ℃ and-0.05 MPa to obtain dry powder;
s6: and (3) decomposition and crushing: calcining the dried powder at 450 deg.C for decomposition, and maintaining the temperature for 60 min; cooling the completely decomposed materials to room temperature, pulverizing, and sieving to obtain particles with particle diameter of 30nm and specific surface area of 80m 2 Per gram of nano ITO powder.
Example 3
A preparation method of nano ITO powder with large specific surface area comprises the following steps:
s1: acid dissolution: dissolving metallic indium In dilute nitric acid solution with the concentration of 12mol/L, heating to be nearly boiling, and after indium is completely dissolved, converting In the mixed solution 2 O 3 With SnO 2 Adding a saturated solution of tin tetrachloride according to the mass ratio of 9:1, and uniformly stirring to obtain a mixed solution with the total concentration of indium and tin ions of 4 mol/L; the saturated solution of the stannic chloride is prepared by analytically pure stannic chloride pentahydrate crystals;
s2: and (3) precipitation: adding potassium bicarbonate into the mixed solution, controlling the reaction temperature at 80 ℃, the reaction time at 50min, continuously stirring at the stirring speed of 100r/min until the precipitation is complete, and controlling the pH value of the feed liquid at 7.2;
s3: and (3) transformation: adding ammonia water into the feed liquid, controlling the pH value of the feed liquid to be 10.0, heating to be close to boiling, wherein the heating rate is 10 ℃/min, and then preserving heat for 40 min;
s4: neutralizing: adding acetic acid into the feed liquid, and controlling the pH value to be 7.5;
s5: cleaning, filtering and drying: carrying out liquid-solid separation on the feed liquid after the neutralization reaction is finished, washing filter residues by using deionized water until no chloride ion exists, and then drying at 150 ℃ under 1.0MPa to obtain dry powder;
s6: and (3) decomposition and crushing: calcining the dried powder at 600 deg.C for decomposition, and maintaining the temperature for 70 min; cooling the completely decomposed materials to room temperature, pulverizing, and sieving to obtain powder with particle diameter of 50nm and specific surface area of 60m 2 Nano ITO powder per gram.
Comparative example 1
Essentially the same as example 2, except that no conversion and neutralization steps were included.
Comparative example 2
The nano-sized indium tin oxide composite powder was prepared by the method of example 6 in the Chinese patent application document "preparation method of nano-sized indium tin oxide composite powder (publication No. CN 100554204)".
Example 4 comparative experiment
ICP-MS is adopted to carry out powder chemical element analysis detection and calculation, TEM is adopted to measure the particle size of the powder, a specific surface area tester is adopted to measure the specific surface area of the powder, a density tester is adopted to measure the relative density of the target material of the powder, and the specific surface area, the target material relative density and the purity of the nano ITO powder prepared in examples 1-3 and comparative example 1 and the wood nano indium tin oxide composite powder prepared in comparative example 2 are obtained, and the results are shown in Table 1.
TABLE 1 comparison of Properties of products prepared in examples 1 to 3 and comparative examples 1 to 2
| Group of | Purity/%) | Particle size/nm | Sintering temperature/. degree.C | Specific surface area per square meter per gram | Relative density of target/%) |
| Comparative example 1 | 99.99 | 25 | 450 | 32 | 98.5 |
| Comparative example 2 | 99.99 | 25 | 520 | 32 | 98.4 |
| Example 1 | 99.995 | 20 | 300 | 120 | 99.7 |
| Example 2 | 99.997 | 30 | 450 | 80 | 99.8 |
| Example 3 | 99.996 | 50 | 600 | 60 | 99.7 |
As can be seen from Table 1, compared with comparative examples 1 and 2, the purity, specific surface area and target relative density of the nano ITO powder prepared in examples 1-3 of the invention are greatly improved, and are superior to those of comparative examples 1 and 2. The method converts the basic carbonate precipitate into hydroxide precipitate through the steps of conversion and neutralization, the converted substance is carried out between solid phases, the conversion rate is high, the particle size is fine, the particles are loose and porous, and the filtering is easy, so that the purity, the specific surface area and the target material relative density are improved, the purity is over 99.995 percent, the specific surface area is over 60 square meters per gram, the maximum is 120 square meters per gram, and the target material relative density is over 99.7 percent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. A preparation method of large specific surface area nano ITO powder is characterized by comprising the following steps:
s1: acid dissolution: dissolving metallic indium In dilute acid solution, heating to near boiling, after indium is completely dissolved, converting In from mixed solution 2 O 3 With SnO 2 Adding a saturated solution of tin tetrachloride according to the mass ratio of 9:1, and uniformly stirring to obtain a mixed solution with the total concentration of indium and tin ions of 2-4 mol/L;
s2: and (3) precipitation: adding a precipitator into the mixed solution, controlling the reaction temperature to be 60-80 ℃, the reaction time to be 30-50 min, continuously stirring until the precipitation is complete, and controlling the pH value of the feed liquid to be 6.5-7.5;
s3: and (3) transformation: adding a conversion agent into the feed liquid, controlling the pH value of the feed liquid to be 9.0-10.0, heating to be close to boiling, and then preserving heat for 20-40 min;
s4: neutralizing: adding a neutralizing agent into the feed liquid, and controlling the pH of the feed liquid to be 6.5-7.5;
s5: cleaning, filtering and drying: carrying out liquid-solid separation on the feed liquid after the neutralization reaction is finished, washing filter residues until no chloride ions exist, and then drying at 50-150 ℃ and-0.1-1.0 MPa to obtain dry powder;
s6: and (3) decomposition and crushing: calcining and decomposing the dried powder at 300-600 ℃, and preserving heat for 50-70 min; cooling the completely decomposed material to room temperature, and then crushing and screening to obtain nano ITO powder;
in step S2, the precipitant is one of ammonium bicarbonate, sodium bicarbonate or potassium bicarbonate; the stirring speed is 50-100 r/min;
in the step S3, the transforming agent is ammonia water; the temperature rise rate is 5-10 ℃/min.
2. The method for preparing nano ITO powder with large specific surface area according to claim 1, wherein the method comprises the following steps: in step S1, the dilute acid solution is one of dilute sulfuric acid, dilute hydrochloric acid or dilute nitric acid, and the concentration is 6-12 mol/L.
3. The method for preparing nano ITO powder with large specific surface area according to claim 1, wherein the method comprises the following steps: in the step S1, the saturated solution of tin tetrachloride is prepared from analytically pure tin tetrachloride pentahydrate crystals.
4. The method for preparing nano ITO powder with large specific surface area according to claim 1, wherein the method comprises the following steps: in step S2, the precipitant is ammonium bicarbonate.
5. The method for preparing nano ITO powder with large specific surface area according to claim 1, wherein the method comprises the following steps: in step S4, the neutralizing agent is acetic acid.
6. The method for preparing nano ITO powder with large specific surface area according to claim 1, wherein the method comprises the following steps: in the step S6, the particle size of the nano ITO powder is 20-50 nm.
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| JP2006264989A (en) * | 2005-03-22 | 2006-10-05 | Dowa Mining Co Ltd | Indium oxide powder and method for producing the same |
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