CN103771497A - Process for preparing ITO (indium tin oxide) powder - Google Patents
Process for preparing ITO (indium tin oxide) powder Download PDFInfo
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- CN103771497A CN103771497A CN201310739825.0A CN201310739825A CN103771497A CN 103771497 A CN103771497 A CN 103771497A CN 201310739825 A CN201310739825 A CN 201310739825A CN 103771497 A CN103771497 A CN 103771497A
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Abstract
The invention relates to preparation of ITO (indium tin oxide) powder, in particular to a process for preparing ITO powder. The process comprises the following steps: dissolving indium in nitric acid, adding excessive ammonium hydroxide and stirring; adding stannic chloride in the solution obtained in the last step, and heating and stirring to obtain a precipitation solution of indium tin hydroxide; heating and concentrating the precipitation solution to obtain indium tin hydroxide colloid; grinding the colloid; calcining the ground colloid to obtain indium tin mixture; drying the mixture to obtain the ITO powder. According to the process, a new concentration process is adopted to prepare an ITO precursor, and then a wet grinding method is carried out to finally obtain the nano-grade ITO powder. The provided new ITO powder process is low in preparation cost and simple.
Description
Technical field
The present invention relates to producing of ito powder, is a kind of technique of preparing ito powder specifically.
Background technology
ITO(tin indium oxide) main component be that stannic oxide is solid-solubilized in the composite oxides in Indium sesquioxide.ITO has good photoelectric properties, and the film that contains ITO has high electroconductibility and visible light transmission, is widely used in the various fields such as solar cell, liquid crystal indicator, touch-control electroplax.In general ito powder adopts and is prepared as follows method: utilize respectively indium metal and metallic tin to obtain indium oxide powder and stannic oxide powder, then by indium oxide powder and stannic oxide powder blending dispersion.Due to the dissolution rate of the indium metal as basic material and metallic tin, solvent temperature, in and the control condition such as pH value, neutral temperature and stirring velocity be difficult to realize completely sameization, make the particle diameter of indium oxide powder and stannic oxide powder and the density variation of prepared target larger, affected the quality of ito thin film.In the prior art, adopting coprecipitation method to prepare ito powder is a kind of conventional method, by the aqueous solution of InCl3 and SnCl4 formation soluble in water as the aqueous solution that contains indium ion and tin ion, in this aqueous solution, drip the throw out that alkaline solution contains indium and tin as ammoniacal liquor etc. with acquisition, then filter, calcine this throw out, obtain ito powder.This method is difficult to the nano level ito powder of preparation,
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of new technique of preparing ito powder, this technique can make nano level ito powder.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of technique of preparing ito powder, and it comprises the following steps:
(1) indium is dissolved in nitric acid, then adds excess of ammonia water to stir;
(2) in above-mentioned solution, add tin tetrachloride, and heated and stirred, indium tin hydroxide precipitation solution obtained;
(3) heating concentrating and precipitating solution, obtains indium tin hydroxide colloid;
(4) grind colloid;
(5) colloid after calcining and grinding, obtains indium tin mixture;
(6) drying composite, obtains ito powder.
As preferably, indium tin is 9.45:1 by the mass ratio of Indium sesquioxide and stannic oxide.
As preferably, in step (2), Heating temperature is 50--70 ℃, heat-up time 10-20min.
As preferably, in step (3), Heating temperature is 60～80 ℃, and concentration time is 6～10h.
As preferably, colloid is grinding after being cooled to room temperature.
As preferably, when grinding, add dehydrated alcohol and binding agent.
As preferably, calcining temperature is 500--800 ℃.
As preferably, in step (6), adopt spraying dry.
Compared with prior art, the present invention adopts concentrated novel process to make ITO presoma, has then prepared nano level ito powder in conjunction with the method for wet grinding, and a kind of new technique of preparing ito powder is provided, and not only preparation cost is low for it, and technique is simple.
Embodiment
Below method of the present invention is described in further detail: it comprises the following steps:
First, indium is dissolved in nitric acid, reaction generates indium nitrate, and adopts dissolving of nitric acid, speed; Add excess of ammonia water to stir, it reacts with indium nitrate and generates indium hydroxide again, and excess of ammonia water reacts with tin tetrachloride, by heating strong stirring, thereby makes indium tin hydroxide precipitation solution;
Then, heating concentrating and precipitating solution, obtains indium tin hydroxide colloid, and colloid grinds after being cooled to room temperature again, the then colloid after calcining and grinding, thus obtain indium tin mixture; Finally, drying composite, obtains ito powder.In an embodiment, get indium, tin tetrachloride, nitric acid, ammoniacal liquor according to reaction mol ratio, guarantee that indium tin is 9.45:1 by the mass ratio of Indium sesquioxide and stannic oxide.Refer to following examples:
Embodiment 1
First, indium is dissolved in nitric acid, then adds ammoniacal liquor to stir, after 10min, add tin tetrachloride, be heated to 50 ℃, and strong stirring, after 10min; Temperature is adjusted to 60 ℃, adopt thickener that reactant is concentrated into colloid, after 6h, stop concentrating, after colloid is cooled to room temperature, be delivered to nano-level grinder, add dehydrated alcohol and binding agent to carry out ball milling, after ball milling, adopt 500 ℃ of calcinings, and the dry calcined material of spraying, ito powder obtained.Analysis records powder diameter size for 52.3nm.
Embodiment 2
Indium is dissolved in nitric acid, then adds ammoniacal liquor to stir, after 10min, add tin tetrachloride, be heated to 60 ℃, and strong stirring, after 15min; Temperature is adjusted to 70 ℃, adopt thickener that reactant is concentrated into colloid, after 8h, stop concentrating, after colloid is cooled to room temperature, be delivered to nano-level grinder, add dehydrated alcohol and binding agent to carry out ball milling, after ball milling, adopt 700 ℃ of calcinings, and the dry calcined material of spraying, ito powder obtained.Analysis records powder diameter size for 27.4nm.
Embodiment 3
Indium is dissolved in nitric acid, then adds ammoniacal liquor to stir, after 10min, add tin tetrachloride, be heated to 70 ℃, and strong stirring, after 20min; Temperature is adjusted to 70 ℃, adopt thickener that reactant is concentrated into colloid, after 10h, stop concentrating, after colloid is cooled to room temperature, be delivered to nano-level grinder, add dehydrated alcohol and binding agent to carry out ball milling, after ball milling, adopt 800 ℃ of calcinings, and the dry calcined material of spraying, ito powder obtained.Analysis records powder diameter size for 31.1nm.
Above-mentioned embodiment is used for illustrative purposes only, and be not limitation of the present invention, the those of ordinary skill in relevant technologies field, without departing from the spirit and scope of the present invention, can also make various variations and modification, therefore all technical schemes that are equal to also should belong to category of the present invention.
Claims (8)
1. a technique of preparing ito powder, it comprises the following steps:
(1) indium is dissolved in nitric acid, then adds excess of ammonia water to stir;
(2) in above-mentioned solution, add tin tetrachloride, and heated and stirred, indium tin hydroxide precipitation solution obtained;
(3) heating concentrating and precipitating solution, obtains indium tin hydroxide colloid;
(4) grind colloid;
(5) colloid after calcining and grinding, obtains indium tin mixture;
(6) drying composite, obtains ito powder.
2. method according to claim 1, is characterized in that: indium tin is 9.45:1 by the mass ratio of Indium sesquioxide and stannic oxide.
3. method according to claim 1, is characterized in that: Heating temperature is 50--70 ℃ in step (2), heat-up time 10-20min.
4. method according to claim 1, is characterized in that: in step (3), Heating temperature is 60～80 ℃, and concentration time is 6～10h.
5. method according to claim 1, is characterized in that: colloid is grinding after being cooled to room temperature.
6. method according to claim 1, is characterized in that: when grinding, add dehydrated alcohol and binding agent.
7. method according to claim 1, is characterized in that: calcining temperature is 500--800 ℃.
8. method according to claim 1, is characterized in that: in step (6), adopt spraying dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310739825.0A CN103771497A (en) | 2013-12-27 | 2013-12-27 | Process for preparing ITO (indium tin oxide) powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310739825.0A CN103771497A (en) | 2013-12-27 | 2013-12-27 | Process for preparing ITO (indium tin oxide) powder |
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| CN103771497A true CN103771497A (en) | 2014-05-07 |
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| CN201310739825.0A Pending CN103771497A (en) | 2013-12-27 | 2013-12-27 | Process for preparing ITO (indium tin oxide) powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104386738A (en) * | 2014-11-03 | 2015-03-04 | 广东先导稀材股份有限公司 | Preparation method of indium tin oxide |
| CN112521164A (en) * | 2020-12-15 | 2021-03-19 | 株洲火炬安泰新材料有限公司 | Process for preparing ITO powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101439870A (en) * | 2008-12-09 | 2009-05-27 | 南昌航空大学 | Preparation of nano-scale indium and tin oxides blue powder |
| CN103318949A (en) * | 2013-06-24 | 2013-09-25 | 长安大学 | Low temperature solid phase preparation method of indium tin oxide nano particle powder |
-
2013
- 2013-12-27 CN CN201310739825.0A patent/CN103771497A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101439870A (en) * | 2008-12-09 | 2009-05-27 | 南昌航空大学 | Preparation of nano-scale indium and tin oxides blue powder |
| CN103318949A (en) * | 2013-06-24 | 2013-09-25 | 长安大学 | Low temperature solid phase preparation method of indium tin oxide nano particle powder |
Non-Patent Citations (2)
| Title |
|---|
| TAKAFUMI SASAKI等: "One-step solvothermal synthesis of cubic-shaped ITO nanoparticles precisely controlled in size and shape and their electrical resistivity", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| TOR OLAV LØVENG SUNDE等: "Transparent and conducting ITO thin films by spin coating of an aqueous precursor solution", 《J. MATER. CHEM.》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104386738A (en) * | 2014-11-03 | 2015-03-04 | 广东先导稀材股份有限公司 | Preparation method of indium tin oxide |
| CN104386738B (en) * | 2014-11-03 | 2016-09-07 | 广东先导稀材股份有限公司 | A kind of preparation method of indium tin metal oxide |
| CN112521164A (en) * | 2020-12-15 | 2021-03-19 | 株洲火炬安泰新材料有限公司 | Process for preparing ITO powder |
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Application publication date: 20140507 |