CN113060757A - Method for preparing porous hollow spherical indium tin oxide powder - Google Patents
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Abstract
The invention discloses a method for preparing porous hollow spherical indium tin oxide powder, which is characterized in that the porous hollow spherical indium tin oxide powder is prepared by a coprecipitation method assisted by pollen serving as a template and sodium citrate serving as a morphology control agent, and the indium tin oxide powder prepared by the method is a micron-sized porous hollow sphere. As pollen is used as a template, the obtained microsphere powder has uniform particle size and good dispersibility, and the particle size is about 20 mu m; sodium citrate is used as a morphology control agent, so that a large number of nano-spheres are formed on the surface of the indium tin oxide microsphere, and the surface area of the indium tin oxide microsphere is increased. The preparation method has the advantages of simple process, convenient operation, low requirement on equipment, and green and nontoxic used additive.
Description
Technical Field
The invention relates to the field of porous hollow structure oxides, in particular to preparation of porous hollow spherical indium tin oxide powder.
Background
Transparent conductive oxide materials are widely used in various optoelectronic devices due to their excellent optical and electrical properties. The indium tin oxide is a product of tin-doped indium oxide, is an N-type semiconductor material, has low resistivity and excellent optical properties such as high visible light transmittance, infrared light reflectance, ultraviolet absorption rate and the like, and is widely applied to the fields of flat panel displays, solar cells, functional glass, gas sensors and the like.
The porous hollow spherical powder has great application potential in various fields of photocatalysis, adsorption, sensors, sustained-release capsules and the like due to the special structure.
There are various methods for preparing indium tin oxide powder, such as coprecipitation method, hydrothermal method, solvothermal method, sol-gel method, etc. Among them, the coprecipitation method has been successfully applied to industrial production for a long time, has the advantages of easy operation, simple equipment, low cost, easy mass production and the like, and is one of the commonly used methods for preparing oxide powder.
The Netherlands colloid and surface A (Colloids and Surfaces A2017, 529 and 503-507) reports that aspartic acid and PEG-4000 are used as additives, a hydrothermal method is adopted to react for 12 hours at 120 ℃, and calcination treatment is combined to obtain hollow spherical indium oxide powder for photocatalytic degradation of organic pollutants; british Material Chemistry A (Journal of Materials Chemistry A2014, 2,5455-5461) reports a mixed solvent thermal method adopting sodium citrate as an additive, the mixed solvent thermal method is used for reacting for 16 hours at 200 ℃, and the porous hollow spherical indium oxide powder is obtained by combining with calcination treatment and is used for photocatalytic degradation of organic pollutants; british Journal of Chemistry 2009,33,1109-1115 reports that hexamethylenediamine is used as an additive, polyethylene glycol is used as a solvent, the reaction is carried out at 210 ℃ for 24 hours, and the hollow tubular indium oxide powder is prepared by combining calcination treatment and is also used for photocatalysis. The indium oxide powder with the hollow structure reported above has good effect when used for photocatalysis, but the preparation process is complex, long-time reaction is required under the condition of high temperature and high pressure, and meanwhile, the additive or the solvent has certain toxicity. Therefore, the method has important significance for preparing the powder with the porous hollow structure by exploring an environment-friendly synthetic route which is simple in process, convenient to operate, safe and nontoxic.
Disclosure of Invention
The invention aims to overcome the problems of toxic additives, complex reaction procedures, harsh reaction conditions and the like in the prior art, and provides a simple method for preparing porous hollow spherical indium tin oxide powder, wherein the used additives are pollen and sodium citrate, are safe and nontoxic and cannot cause human harm or environmental pollution, and the method can be realized under simple equipment and normal-pressure room temperature conditions.
The technical scheme adopted by the invention is as follows: firstly, pretreating pollen by adopting absolute ethyl alcohol, then dispersing the pretreated pollen in the absolute ethyl alcohol, adding sodium citrate and water, and marking as a solution A; the raw materials for preparing the indium-tin salt solution, namely the solution B, adopt metal indium and SnCl4·5H2And O, uniformly mixing the solution A and the solution B, adding a precipitator to enable the pH of the solution to be 8-11, standing at room temperature for 1-48 h, separating and washing out the obtained precursor precipitate, drying, and calcining to obtain the indium tin oxide powder.
The pollen in the scheme is rape pollen or lotus pollen, the pretreatment process is to disperse the pollen in absolute ethyl alcohol according to 0.05-0.5 g/ml, stir for 8-24 h, separate the pollen, repeat for 3-5 times, and dry the obtained pollen for later use;
in the scheme, the solution A is prepared by dispersing the pretreated pollen in absolute ethyl alcohol according to 0.02-0.1 g/ml, adding a small amount of water according to the molar ratio of indium ions to sodium citrate of 1: 0.5-1: 5 to dissolve the sodium citrate;
indium-tin salt solution in the above schemeThe preparation of the solution is that metal indium with the purity of more than 99.99 percent is dissolved In concentrated hydrochloric acid with the mass fraction of 37 percent, and after the metal indium is completely dissolved, water is added for dilution to ensure that the concentration of indium ions is 0.03-0.3 mmol/ml according to the mass ratio m (In)2O3):m(SnO2) Adding SnCl as 9:14·5H2O；
The precipitant in the scheme adopts ammonia water or sodium hydroxide aqueous solution;
the separation and washing of the precipitate in the scheme refers to that the precipitate is centrifugally separated and then washed for 3-5 times by deionized water and absolute ethyl alcohol respectively;
the calcination in the scheme is carried out at 580-800 ℃ for 0.5-4 h;
the invention has the technical effects that: pollen and sodium citrate are used as additives, the obtained indium tin oxide powder is a micron-sized hollow sphere with uniform particle size of about 20 mu m, a large number of nanospheres are attached to the surface of the microsphere, the particle size is about 300nm, and the surface area is 36.80m2(ii) in terms of/g. The method has simple process and low requirement on experimental equipment, and the used additive is green and nontoxic.
The porous hollow spherical indium tin oxide powder prepared by the method has adsorption performance and good adsorption stability to rhodamine B.
Description of the drawings:
FIG. 1 is an SEM image of ITO powder prepared by the method of the present invention.
The specific implementation mode is as follows:
the method comprises the following specific implementation steps:
(1) weighing rape pollen or lotus pollen, dispersing into absolute ethyl alcohol, stirring for 8-24 h, separating out pollen, repeating for 3-5 times, and drying the obtained pollen for later use;
(2) dispersing the pretreated pollen in absolute ethyl alcohol, adding weighed sodium citrate and a proper amount of water under the stirring state, and continuing stirring;
(3) weighing a certain amount of metal indium, adding the metal indium into concentrated hydrochloric acid until the metal indium is completely dissolved, adding water for dilution, and then weighing m (In) according to the mass ratio2O3):m(SnO2) Weighing SnCl (9: 1)4·5H2Adding O into the indium salt solution, and uniformly stirring to prepare an indium-tin salt mixed solution;
(4) uniformly mixing a pollen solution containing sodium citrate and an indium-tin salt solution, and adding a precipitator under the stirring state until the pH value of the solution is 8-11;
(5) and standing for 1-48 h after the alkali is added, centrifugally separating out precipitates, washing with deionized water and absolute ethyl alcohol respectively, drying the obtained precursor, and calcining at 580-800 ℃ for 0.5-4 h to obtain the indium tin oxide powder.
The invention is described in more detail below by way of a few specific examples.
Comparative example: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of pre-treated rape pollen was weighed out and dispersed in 50ml of absolute ethanol. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid, adding water to dilute to 50ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, surface without nanospheres, and specific surface area of 13.71m2·g-1。
Example 1: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was dispersed in 50ml of absolute ethanol, 0.64g of sodium citrate and 5ml of water were added, and stirring was continued. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid with the mass fraction of 37%, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 8.5, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powderThe particle size of the powder is about 20 μm, and a small amount of small balls with the size of about 300nm are carried on the surface of the powder. The specific surface area of the indium tin oxide powder is 17.88m2·g-1。
Example 2: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was dispersed in 50ml of absolute ethanol, 0.64g of sodium citrate and 5ml of water were added, and stirring was continued. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid with the mass fraction of 37%, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, small amount of small balls with size of 300nm on the surface, and specific surface area of 18.52m2·g-1。
Example 3: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was dispersed in 50ml of absolute ethanol, 0.64g of sodium citrate and 5ml of water were added, and stirring was continued. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid with the mass fraction of 37%, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 10, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, small amount of small balls with size of 300nm on the surface, and specific surface area of 18.36m2·g-1。
Example 4: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. Weighing 2.5g of pretreated rapePollen is dispersed in 50ml of absolute ethanol, 0.64g of sodium citrate and 5ml of water are added, and stirring is continued. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid with the mass fraction of 37%, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 650 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, small amount of small balls with size of 300nm on the surface, and specific surface area of 19.02m2·g-1。
Example 5: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was dispersed in 50ml of absolute ethanol, 1.28g of sodium citrate and 5ml of water were added, and stirring was continued. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid with the mass fraction of 37%, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, small amount of small balls with size of 300nm on the surface, and specific surface area of 24.78m2·g-1。
Example 6: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was dispersed in 50ml of absolute ethanol, 1.28g of sodium citrate and 5ml of water were added, and stirring was continued. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid with the mass fraction of 37%, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 9, standing for 24 hr, centrifuging, and precipitatingWashing the precipitate with water, washing with alcohol, drying, calcining at 650 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of about 20 μm, small amount of spheres of about 300nm on the surface, and specific surface area of 25.64m2·g-1。
Example 7: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was weighed out and dispersed in 50ml of absolute ethanol, 2.5g of sodium citrate and 5ml of water were added and stirred continuously. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid with the mass fraction of 37%, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, large amount of small balls with size of 300nm on the surface, and specific surface area of 36.80m2·g-1。
Example 8: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was weighed out and dispersed in 50ml of absolute ethanol, 2.5g of sodium citrate and 5ml of water were added and stirred continuously. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid with the mass fraction of 37%, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 650 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, large amount of small balls with size of 300nm on the surface, and specific surface area of 33.58m2·g-1。
Example 9: weighing rape pollen, dispersing in anhydrous ethanol, and stirringSeparating pollen for 12 hr, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was weighed out and dispersed in 50ml of absolute ethanol, 2.5g of sodium citrate and 5ml of water were added and stirred continuously. Weighing 0.25g of metal indium, dissolving the metal indium in concentrated sulfuric acid with the mass fraction of 95%, adding water to dilute the solution to 45ml, and adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, adding ammonia water as precipitant to adjust pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, large amount of small balls with size of 300nm on the surface, and specific surface area of 36.30m2·g-1。
Example 10: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was weighed out and dispersed in 50ml of absolute ethanol, 2.5g of sodium citrate and 5ml of water were added and stirred continuously. Weighing 0.25g of metal indium, dissolving in 65% concentrated nitric acid by mass, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, selecting ammonia water as precipitant, adding ammonia water to adjust pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, large amount of small balls with size of 300nm on the surface, and specific surface area of 35.88m2·g-1。
Example 11: weighing rape pollen, dispersing into anhydrous ethanol, stirring for 12 hr, separating pollen, repeating for 4 times, and drying the obtained pollen. 2.5g of the pretreated rape pollen was weighed out and dispersed in 50ml of absolute ethanol, 2.5g of sodium citrate and 5ml of water were added and stirred continuously. Weighing 0.25g of metal indium, dissolving the metal indium in a mixed solution of concentrated hydrochloric acid with the mass fraction of 37% and concentrated nitric acid with the mass fraction of 65%, adding water to dilute the solution to 45ml, and adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, selecting ammonia water as precipitant, adding ammonia water to adjust pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with ethanol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, large amount of small balls with size of 300nm on the surface, and specific surface area of 33.76m2·g-1。
Example 12: weighing flos Nelumbinis pollen, dispersing in anhydrous ethanol, stirring for 12 hr, separating out pollen, repeating for 4 times, and drying the obtained pollen for use. 2.5g of the pretreated rape pollen was weighed out and dispersed in 50ml of absolute ethanol, 2.5g of sodium citrate and 5ml of water were added and stirred continuously. Weighing 0.25g of metal indium, dissolving in concentrated hydrochloric acid with the mass fraction of 37%, adding water to dilute to 45ml, adding 0.078g of SnCl4·5H2And O, stirring uniformly. Mixing the two solutions, stirring, selecting ammonia water as precipitant, adding ammonia water to adjust final solution pH to 9, standing for 24 hr, centrifuging to separate precipitate, washing with water, washing with alcohol, drying, calcining at 600 deg.C for 2 hr to obtain porous hollow spherical indium tin oxide powder with particle diameter of 20 μm, large amount of small balls with size of 300nm on the surface, and specific surface area of indium tin oxide powder of 29.08m2·g-1。
Application example: the pollutant simulated adsorption removal experiment is carried out on the comparative example and the example.
And (3) adding 0.05g of indium tin oxide powder obtained in the comparative examples and the examples into 50ml of organic dye rhodamine B solution with the concentration of 4.8mg/L, stirring in a dark place, taking a small amount of solution every 20min to measure the absorbance of the solution, converting the solution into the residual concentration C of rhodamine B in the solution after adsorption by a standard curve method, calculating the adsorption capacity of the comparative examples and the examples under corresponding conditions, and adsorbing for 4 hours to achieve adsorption balance.
The state in which neither the concentration of the adsorbate in the solution nor the concentration on the surface of the adsorbent changes is called adsorption equilibrium, and the adsorption value at which adsorption reaches adsorption equilibrium is called equilibrium adsorption amount.
The adsorption experiments were carried out on the indium tin oxide powders prepared in the comparative example and the examples, and the results are shown in table 1.
Table 1 shows the adsorption amount and adsorption removal rate of rhodamine B in the comparative examples and examples.
As can be seen from Table 1, the material disclosed by the invention has an adsorption effect on rhodamine B.
Claims (6)
1. A method for preparing porous hollow spherical indium tin oxide powder comprises the following steps: dispersing the pretreated pollen in absolute ethyl alcohol, adding sodium citrate and water, and stirring to obtain a solution A; preparing or preparing a mixed solution, namely solution B, by using indium and tin metal or soluble salts of indium and tin as raw materials; and mixing and stirring the solution A and the solution B, adding a precipitator for coprecipitation to obtain precursor precipitate, washing the precipitate, drying and calcining to obtain the indium tin oxide powder. The method is characterized in that: the porous hollow spherical indium tin oxide powder is prepared by using pollen as a template and sodium citrate as a morphology control agent through an auxiliary coprecipitation method.
2. The method of dispersing pretreated pollen in absolute ethanol, adding sodium citrate and water, stirring to obtain solution A as claimed in claim 1, wherein: the pollen is rape flower pollen or lotus flower pollen, the pollen is dispersed in absolute ethyl alcohol according to the proportion of 0.05-0.5 g/ml, the stirring is carried out for 8-24 hours, the pollen is separated out, the repetition is carried out for 3-5 times, and then the obtained pollen is dried. Dispersing the pretreated pollen into absolute ethyl alcohol according to 0.02-0.1 g/ml, adding sodium citrate and water, stirring to obtain a solution A, adding a small amount of water to dissolve the sodium citrate according to the molar ratio of indium ions to the sodium citrate of 1: 0.5-1: 5, and thus obtaining the pollen.
3. The method according to claim 1, wherein the mixed solution (solution B) is prepared or prepared from indium or tin metal or soluble salts thereof, and comprises the following steps: the indium tin oxide can be obtained by dissolving metal indium or metal tin In strong acid and then adding water for dilution, or can be obtained by dissolving water-soluble indium salt or tin salt In water, wherein the purity of the metal indium and the metal tin is more than 99.99%, the strong acid is one of hydrochloric acid, nitric acid and sulfuric acid or any combination of the hydrochloric acid, the nitric acid and the sulfuric acid, and the tin is added according to the mass ratio m (In)2O3):m(SnO2) The ratio of indium ions in the solution B is 9:1, and the concentration of indium ions in the solution B is 0.03-0.3 mmol/ml.
4. The method comprises the steps of mixing and stirring the solution A and the solution B according to claim 1, adding a precipitator for coprecipitation to obtain a precursor precipitate, washing and drying the precipitate. The method is characterized in that: and mixing and stirring the solution A and the solution B for 0.5-1 h, adding a precipitator to enable the pH of the solution to be 8-11, obtaining a precursor precipitate, standing for 1-48 h, wherein the precipitator is ammonia water or sodium hydroxide aqueous solution, and the washing comprises washing with deionized water and washing with absolute ethyl alcohol.
5. Calcining the precursor precipitate according to claim 1 to obtain indium tin oxide powder, characterized in that: the calcination temperature is 580-800 ℃, and the calcination time is 0.5-4 h.
6. The application of the porous hollow spherical indium tin oxide powder prepared by the method of claim 1 in adsorbing an organic dye rhodamine B.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731527A (en) * | 2016-01-29 | 2016-07-06 | 北京化工大学 | Coprecipitation preparation method of nanoscale indium tin oxide powder |
| CN106542569A (en) * | 2015-09-17 | 2017-03-29 | 天津工业大学 | A kind of preparation method of flower ball-shaped tin ash |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106542569A (en) * | 2015-09-17 | 2017-03-29 | 天津工业大学 | A kind of preparation method of flower ball-shaped tin ash |
| CN105731527A (en) * | 2016-01-29 | 2016-07-06 | 北京化工大学 | Coprecipitation preparation method of nanoscale indium tin oxide powder |
Non-Patent Citations (1)
| Title |
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| A. AHAMED FAZIL ET AL.: ""A facile bio-replicated synthesis of SnO2 motifs with porous surface by using pollen grains of Peltophorum pterocarpum as a template"", 《MICROPOROUS AND MESOPOROUS MATERIALS》 * |
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