CN103864138A - Method of preparing nano ITO (Indium Tin Oxide) powder at low temperature - Google Patents
Method of preparing nano ITO (Indium Tin Oxide) powder at low temperature Download PDFInfo
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- CN103864138A CN103864138A CN201410037506.XA CN201410037506A CN103864138A CN 103864138 A CN103864138 A CN 103864138A CN 201410037506 A CN201410037506 A CN 201410037506A CN 103864138 A CN103864138 A CN 103864138A
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Abstract
The invention relates to preparation of ITO (Indium Tin Oxide) power and in particular relates to a method of preparing nano ITO powder at a low temperature. The method comprises the following steps: adding indium tin alloy powder into nitric acid liquor, adding ion liquid 1-butyl-3-methylimidazole trifluoromethanesulfonate and sodium hydroxide liquor, heating and stirring, and reacting to generate indium tin oxide precipitate liquor; centrifuging and separating the precipitate liquor to obtain indium tin hydroxide, washing the indium tin hydroxide with water, vacuum-drying; placing the dried indium tin oxide in a high-pressure kettle, and heating the high-pressure kettle after charging a high-pressure protective gas; keeping gas pressure in the high-pressure kettle stable and obtaining ITO powder after the reaction is completed. According to the invention, the reaction is carried out in ionic liquid, and obtained reactant is uniform in grain size and a little in pollution. The method disclosed by the invention takes the indium tin alloy as the material and ensures the grain size of the prepared ITO powder to be uniform. And the nano ITO powder can be prepared at the temperature not higher than 300 DEG C, so that not only is the method energy-saving, but also the method is safe.
Description
Technical field
The present invention relates to producing of ito powder, is the method that low temperature is prepared 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, thereby the particle diameter of indium oxide powder and stannic oxide powder and the density variation of prepared target are larger, affect 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.But this common method not only easily causes homogeneity and the sintering character of the ito powder of preparing poor; And consumption of organic solvent is larger, high volatility, easily causes chemical pollution.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of method of preparing nano-ITO powder, the ito powder of preparing according to the method is comparatively homogeneity of particle diameter not only, and preparation process temperature is low, chemical pollution is few.
The technical scheme that the present invention solves the problems of the technologies described above employing is: low temperature is prepared the method for nano-ITO powder, and it comprises the following steps:
(1) indium stannum alloy powder is added in salpeter solution, then add ionic liquid 1-butyl-3-methyl imidazolium fluoroform sulphonate and sodium hydroxide solution, heated and stirred, reaction generates indium tin hydroxide precipitation solution;
(2) centrifugation precipitation solution, obtains indium tin hydroxide, washes indium tin hydroxide with water, vacuum-drying;
(3) dried indium tin hydroxide is placed in autoclave, and after being filled with high voltage protective gas, autoclave is heated;
(4) by the purging valve release guard gas of autoclave, keep autoclave internal gas pressure stable, after having reacted, obtain ito powder.
As preferably, in step (1), indium and tin are take the mass ratio of Indium sesquioxide and stannic oxide as 9.45:1.
As preferably, step (1) temperature of reaction is 80--110 ℃, and the reaction times is 15--20h.
As preferably, step (1) is controlled the pH value of precipitation solution at 7--8
As preferably, in step (3), shielding gas is argon gas.
As preferably, described argon gas is 0.8--1.2MPa at the pressure of autoclave.
As preferably, in step (3), Heating temperature is 220--300 ℃, and be 3.5--4.5h heat-up time.
The present invention compared with prior art, has the following advantages:
1, reaction is carried out in ionic liquid, and the reactant particle diameter obtaining is even, pollutes few;
2, take indium stannum alloy as raw material, by by indium stannum alloy and nitric acid reaction, when having realized Indium sesquioxide and stannic oxide, generate, avoided prior art prepare respectively Indium sesquioxide with in stannic oxide process owing to being difficult to realize the deviation of the particle diameter that sameization of control condition bring, guarantee that the particle diameter of ito powder of preparation is even.
3, utilization of the present invention just not can be made into nano-ITO powder higher than the temperature of 300 ℃, not only energy-conservation, and safety.
Embodiment
Below method of the present invention is described in further detail: it comprises the following steps:
First, indium stannum alloy powder is added in salpeter solution, then add ionic liquid 1-butyl-3-methyl imidazolium fluoroform sulphonate and sodium hydroxide solution, heated and stirred, reaction generates indium tin hydroxide precipitation solution; Wherein indium stannum alloy can adopt several different methods preparation, as carried out under vacuum condition by tin and indium are mixed in that heat is melted, pressurization, cooling, grind, obtain indium stannum alloy powder.The present invention, take indium stannum alloy as raw material, is dissolved in nitric acid by indium stannum alloy, generates the polymer of metastannic acid, and the oxyhydroxide of itself and indium is precipitated simultaneously.Meanwhile, because ionic liquid is to be made up of large organic cation and less inorganic anion, it has lower surface tension, and not only in the time preparing indium tin hydroxide, nucleation rate is higher, and the particle diameter of particle is less; And the indium tin hydroxide of preparation has good stability.In addition, the hydrophobic grouping that ionic liquid has and high polar group have high guidance quality, are conducive to indium tin hydroxide and form ordered structure, lay the foundation for preparing the uniform ito powder of particle diameter.Ionic liquid also provides the environment of preparing of an anhydrous and trace water, can impel producer that the balance of reaction is conducive to crystal to carrying out, thereby can suppress the generation of other oxyhydroxide and some unformed materials.Due to ionic liquid very easily hydrolysis under microbial process, can reduce chemical pollution.
Generate after indium tin hydroxide precipitation solution, centrifugation precipitation solution, obtains indium tin hydroxide, washes indium tin hydroxide with water, vacuum-drying; Again dried indium tin hydroxide is placed in autoclave, and after being filled with high voltage protective gas, autoclave is heated; When after temperature rise, gas pressure intensity raises, and now by the purging valve release guard gas of autoclave, keeps autoclave internal gas pressure stable.The gas that just should repeatedly discharge as excessive in pressure in reactor, obtains ito powder after final reaction completes.Refer to following examples:
Embodiment 1
Make indium stannum alloy powder according to indium and tin take the mass ratio of Indium sesquioxide and stannic oxide as 9.45:1, add in salpeter solution, add again ionic liquid 1-butyl-3-methyl imidazolium fluoroform sulphonate and sodium hydroxide solution, be heated to 80 ℃, stirring reaction 15h, and the pH value of controlling solution is 7, centrifugation precipitation solution, obtain indium tin hydroxide, wash indium tin hydroxide with water, 50 ℃ of vacuum-dryings; Dried indium tin hydroxide is placed in autoclave, and is filled with the argon gas of 0.8MPa, gradually Heating temperature is raised to 300 ℃ from 220 ℃, after reaction 3.5, sample thief electronic microscope photos, ito powder maximum particle diameter is in 28nm left and right, and minimum grain size is in 22nm left and right.
Embodiment 2
Make indium stannum alloy powder according to indium and tin take the mass ratio of Indium sesquioxide and stannic oxide as 9.45:1, add in salpeter solution, add again ionic liquid 1-butyl-3-methyl imidazolium fluoroform sulphonate and sodium hydroxide solution, be heated to 90 ℃, stirring reaction 20h, and the pH value of controlling solution is 7, centrifugation precipitation solution, obtain indium tin hydroxide, wash indium tin hydroxide with water, 50 ℃ of vacuum-dryings; Dried indium tin hydroxide is placed in autoclave, and is filled with the argon gas of 1MPa, gradually Heating temperature is raised to 300 ℃ from 220 ℃, after reaction 4, sample thief electronic microscope photos, ito powder maximum particle diameter is in 18nm left and right, and minimum grain size is about 13nm.
Embodiment 3
Make indium stannum alloy powder according to indium and tin take the mass ratio of Indium sesquioxide and stannic oxide as 9.45:1, add in salpeter solution, add again ionic liquid 1-butyl-3-methyl imidazolium fluoroform sulphonate and sodium hydroxide solution, be heated to 110 ℃, stirring reaction 20h, and the pH value of controlling solution is 8, centrifugation precipitation solution, obtain indium tin hydroxide, wash indium tin hydroxide with water, 50 ℃ of vacuum-dryings; Dried indium tin hydroxide is placed in autoclave, and is filled with the argon gas of 1.2MPa, gradually Heating temperature is raised to 300 ℃ from 220 ℃, after reaction 4.5, sample thief electronic microscope photos, ito powder maximum particle diameter is in 23nm left and right, and minimum grain size is about 18nm.
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 (7)
1. low temperature is prepared the method for nano-ITO powder, and it comprises the following steps:
(1) indium stannum alloy powder is added in salpeter solution, then add ionic liquid 1-butyl-3-methyl imidazolium fluoroform sulphonate and sodium hydroxide solution, heated and stirred, reaction generates indium tin hydroxide precipitation solution;
(2) centrifugation precipitation solution, obtains indium tin hydroxide, washes indium tin hydroxide with water, vacuum-drying;
(3) dried indium tin hydroxide is placed in autoclave, and after being filled with high voltage protective gas, autoclave is heated;
(4) by the purging valve release guard gas of autoclave, keep autoclave internal gas pressure stable, after having reacted, obtain ito powder.
2. method according to claim 1, is characterized in that: in step (1), indium and tin are take the mass ratio of Indium sesquioxide and stannic oxide as 9.45:1.
3. method according to claim 1, is characterized in that: step (1) temperature of reaction is 80--110 ℃, and the reaction times is 15--20h.
4. method according to claim 1, is characterized in that: step (1) is controlled the pH value of precipitation solution 7-8.
5. method according to claim 1, is characterized in that: in step (3), shielding gas is argon gas.
6. method according to claim 5, is characterized in that: described argon gas is 0.8--1.2MPa at the pressure of autoclave.
7. method according to claim 1, is characterized in that: in step (3), Heating temperature is 220--300 ℃, and be 3.5--4.5h heat-up time.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851371A (en) * | 2021-02-02 | 2021-05-28 | 株洲火炬安泰新材料有限公司 | Method for preparing nano ITO powder at low temperature |
| CN112919900A (en) * | 2021-02-02 | 2021-06-08 | 株洲火炬安泰新材料有限公司 | Target material forming and pressing method based on cold isostatic pressing |
| CN115321585A (en) * | 2022-08-09 | 2022-11-11 | 先导薄膜材料有限公司 | Washing process of indium hydroxide |
Citations (2)
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| CN102127782A (en) * | 2011-01-18 | 2011-07-20 | 上海交通大学 | Method for preparing super-hydrophobic indium antimonide film by deposition in ionic liquid |
| CN102719863A (en) * | 2011-01-18 | 2012-10-10 | 上海交通大学 | Method for depositing and preparing super-hydrophobic indium antimonide thin film from ionic liquid |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127782A (en) * | 2011-01-18 | 2011-07-20 | 上海交通大学 | Method for preparing super-hydrophobic indium antimonide film by deposition in ionic liquid |
| CN102719863A (en) * | 2011-01-18 | 2012-10-10 | 上海交通大学 | Method for depositing and preparing super-hydrophobic indium antimonide thin film from ionic liquid |
Non-Patent Citations (2)
| Title |
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| 吴庆海: ""离子液体中纳米氧化铟、氧化锡和ITO粉末的制备及性能研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 张贤高: ""ITO纳米粉的低温制备"", 《中国优秀硕士学位论文全文数据库 基础科学辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851371A (en) * | 2021-02-02 | 2021-05-28 | 株洲火炬安泰新材料有限公司 | Method for preparing nano ITO powder at low temperature |
| CN112919900A (en) * | 2021-02-02 | 2021-06-08 | 株洲火炬安泰新材料有限公司 | Target material forming and pressing method based on cold isostatic pressing |
| CN112919900B (en) * | 2021-02-02 | 2022-12-02 | 株洲火炬安泰新材料有限公司 | Target material forming and pressing method based on cold isostatic pressing |
| CN115321585A (en) * | 2022-08-09 | 2022-11-11 | 先导薄膜材料有限公司 | Washing process of indium hydroxide |
| CN115321585B (en) * | 2022-08-09 | 2023-08-11 | 先导薄膜材料(安徽)有限公司 | Indium hydroxide washing process |
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Application publication date: 20140618 |