CN1528670A - In2O3 and ITO monodisperse nano powder hydrothermal preparation method - Google Patents
In2O3 and ITO monodisperse nano powder hydrothermal preparation method Download PDFInfo
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- CN1528670A CN1528670A CNA2003101112237A CN200310111223A CN1528670A CN 1528670 A CN1528670 A CN 1528670A CN A2003101112237 A CNA2003101112237 A CN A2003101112237A CN 200310111223 A CN200310111223 A CN 200310111223A CN 1528670 A CN1528670 A CN 1528670A
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- ito
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Abstract
The invention relates to a hydrothermal preparing method of In2O3 and ITO monodisperse nano powder, dissolving metals In and Sn in inorganic acid to prepare a certain concentration mixed solution, and then processing by anion exchange resin to obtain colloid solution, placing the colloid solution from which the resin has been separated in the high-pressure reacting kettle, to react at the hydrothermal temperature of 150-260deg.C for 4-24h, washing the resultant by pure water to vacuum-filter, drying at 100-105deg.C for 6-12h, calcining at 500-1000deg.C for 2-4h, and then obtaining the In2O3 and ITO monodisperse nano powder whose average particle size is not greater than 100nm observed by scanning electron microscope and whose maximum particle size is not greater than 1.5mu m measured by laser particle measurer on the condition that the In2O3 and ITO powder is dispersed by pure water and ultrasonic wave without dispersing agent.
Description
Technical field
The present invention relates to the starting material In of ITO target
2O
3, ITO preparation method, particularly ITO target dispersed nano In
2O
3, the ITO powder the preparation method.
Background technology
Be accompanied by the development of liquid-crystal display, indium tin oxide (ITO) requirement that is used for transparency electrode sharply increases.At present, developed country in the world is used to prepare the ITO material as states such as Japan, the U.S., Britain, France with the indium about half.They generally adopt indium tin oxide to make target, with direct current magnetron sputtering process target are made ito thin film then.This film is to visible transparent, and energy strong reflection infrared light has low membrane resistance, thereby obtains increasingly extensive application at aspects such as liquid-crystal display, heat-protecting glass, solar cell and collector, the frost prevention of vehicle window mist elimination.In view of ITO target and film widespread use in a lot of fields thereof, domestic existing many productions and R﹠D institution all are being engaged in the research of this respect, but all still be in the junior stage at present, domestic needed ITO target of display device producer and powder product at present still can only dependence on import.For preparation target used ito powder, require very strictly, not only want the purity height, and want fine size, dispersing property good, therefore, need reinforcement to prepare the research of ito powder technology.The technological method of preparation ITO composite powder has multiple, as liquid-phase precipitation method, decompression voloxidation process, melt spray burning method, spray heating decomposition etc.As having in the ITO dispersed nano powder of open source literature report:
1, " chemical liquid phase coprecipitation preparation of nano level In
2O
3(SnO
2) powder " " powder metallurgy industry " .1999,9 (5). introduced with pure indium, SnCl
45H
2O is a raw material, adopts the chemical liquid phase coprecipitation method to prepare nano level In
2O
3(SnO
2) powder.Utilize laboratory facilities such as XRD, TEM, SEM, BET and chemical analysis to the thing of made powder mutually, pattern, composition, granularity etc. carried out preliminary sign.Result of study shows: the powder that coprecipitation method makes is high-purity, monophasic nanoscale powder, and median size is 30nm;
2, " suspension of indium tin oxide and the preparation method and its usage of powder ", Chinese patent＜application number〉99810088, set forth based on the suspension of indium tin oxide and being prepared as follows of powder: in the presence of one or more surface modification compositions, the precursor of precipitation of indium tin-oxide in the solution of one or more solvents; Calcine resulting powder after removing solvent; And then add one or more surface modification compositions and one or more solvents; Resulting mixture forms suspension, and randomly liquid component is removed from described suspension, so that obtain powder through grinding or dispersion treatment.Resulting powder can randomly be handled by being shaped becomes tangible body.The indium tin oxide material that obtains therefrom is especially suitable for use as the coating material of microelectronics and optoelectronic applications.
3, Chinese patent＜application number〉01107509, the preparation method of indium, tin-oxide composite powder has proposed the preparation method of a kind of indium, tin-oxide composite powder, is after indium metal and metallic tin (weighing by weight percentage) are dissolved emulsification respectively, behind the thorough mixing, allow its co-precipitation, washing is filtered, oven dry again, calcination, quenching at last grinds, product.The present invention has the composite powder that can directly obtain the chemical ingredients homogeneous by the various chemical reactions in the solution; Ultra-fine the material for preparing narrow diameter distribution and good fluidity easily.
4, people such as Japanese Kochi University Yanagisawa (Journal of Materials Research, 2000,15 (6): 1404-1408) mentioned a kind of method of Hydrothermal Preparation ITO powder in the literature.This method is taked ammonia precipitation process indium (tin) salts solution, with generate the hydro-thermal presoma---indium hydroxide (tin) carries out hydro-thermal reaction (300 ℃), obtain the ITO nano-powder through filtration, vacuum-drying, calcining at last.In this method preparation process because to introduce ammoniacal liquor be precipitation agent, the hydro-thermal presoma product size-grade distribution that it obtains is very wide, in order to reach the purpose of dissolving the macrobead presoma fully, need increase considerably hydrothermal temperature (being not less than 300 ℃), simultaneously for indium and tin are precipitated fully, need to use excess of ammonia water precipitation agent, thereby cause in the high-temperature water thermal process, understanding in the solution effusion ammonia, so that the voltage endurance capability of hydro-thermal reaction equipment needs to improve greatly (theoretical pressure just is not less than 20MPa), and the introducing of ammoniacal liquor has caused the decline of water heating apparatus high-temperature anticorrosion ability.
We recognize from above-mentioned open source literature, various preparation In
2O
3The method of powder all has its relative merits, is that time of these two kinds of methods preparations is very fast as decompression voloxidation process and melt spray burning method, but needs expensive equipment, and the degree of oxidation of metal is difficult to control, and the homogeneity of powder is bad; Spray heating decomposition is to produce In with spraying into the high-temperature zone thermolysis after the atomizing of indium metal salts solution
2O
3Powder needing to be characterized in special equipment, the difficult control of decomposition course complexity, condition, but can make sphericity powder preferably; Liquid-phase precipitation method is a raw material with indium metal or indium metal salt, prepares In with precipitation mode in solution
2O
3Powder, its characteristics are for adopting common chemical industry equipment, and flow process is simple, but the particle diameter of powder is difficult to control condition, and introduce impurity easily.
Technology contents
The inventor is through arduous research and test, found that a kind of technology is simple, constant product quality, cost be lower, found a kind of equipment simple, manageable In
2O
3, ITO dispersed nano powder hydrothermal preparing process.
The object of the present invention is achieved like this: a kind of In
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that with a certain amount of indium metal and metallic tin, indium metal and metallic tin are with SnO
2: In
2O
3Weight percent meter, per-cent when per-cent is 0, promptly prepare In between 0～0.25
2O
3Powder, otherwise promptly prepare the ITO powder, be dissolved in the mineral acid, the concentration of the mixing solutions that is made into is 0.5～3.0mol/L, again mixing solutions is carried out plastic resin treatment and obtains colloidal solution, inserts colloidal solution in the autoclave and carries out hydro-thermal, hydrothermal temperature is 180～260 ℃, the described hydro-thermal reaction time is 4～24h, with product washing, filtration, promptly prepares In after drying, the calcining after reaction is finished
2O
3, ITO dispersed nano powder.
Above-described mineral acid includes the mixing acid of any two kinds of arbitrary proportions among hydrochloric acid, nitric acid, sulfuric acid or the above-mentioned three or above-mentioned three's arbitrary proportion mixing acid.Described colloidal solution is to handle mixing solutions by resin anion(R.A) to obtain.The resin of handling is polystyrene strong base or acrylic acid series weak base type macroporous type or gel-type anionresin and after handling mixing solutions and obtaining colloidal solution, anionite-exchange resin regenerate to prepare against under strong alkali environments such as sodium hydroxide, potassium hydroxide and reused in the future.。Described washing is with pure water or the water washing of electronics secondary.Described vacuum or the negative pressure filtration of being filtered into.Described drying is to carry out under 100-105 ℃, and the time is that 6～12h gets final product, and calcining is to carry out under 500～1000 ℃, and the time is that 2～4h gets final product.The In for preparing
2O
3, the ITO powder observes the median size≤100nm of powder under scanning electron microscope, with pure water and ultrasonic dispersing, do not add under the condition of dispersion agent, adopts the maximum particle diameter≤1.5 μ m of laser particle analyzer test.
Compared with prior art, outstanding substantive distinguishing features of the present invention and obvious improvement are:
1, the In for preparing
2O
3, the ITO nano-powder has the purity height, monodispersity is good, the median size≤100nm of powder, ITO target size: 〉=500*500mm, ITO density: 〉=99%, have important use to be worth in display device transparent conductive film field.
2, the hydrothermal synthesis method operation is simple, and easy handling is suitable for suitability for industrialized production.
3, have that reunion, the equipment that can reduce powder are simple, cost is low, operational safety, advantage such as pollution-free.
Embodiment
Further specify outstanding feature of the present invention below by example, only never limit the present invention in explanation the present invention.
Embodiment 1, to take indium metal be starting material, with dissolving metal, is mixed with the indium chloride high concentration solution with hydrochloric acid, is mixed with 0.5M indiumchloride solution 200mL subsequently, and 40 gram D301 macroporous type anionite-exchange resin are added in the mixing solutions.Adopt magnetic stirring apparatus stirred solution 30min, filter with 50 purpose gauzes subsequently, anionite-exchange resin on the gauze adopts the sodium hydroxide solution regeneration of pH=13 in order to reuse in the future, colloidal solution after the filtration is transferred in the autoclave that has the tetrafluoroethylene liner, 3 ℃/min of average rate intensification, to 180 ℃, hydro-thermal reaction 6h, cool to room temperature with the furnace, unload still, with pure water washing reaction product and multipass repeatedly, through vacuum filtration, behind 100 ℃ of dry 8h, the 900 ℃ of calcining 3h, promptly obtain reaction product.
The In for preparing
2O
3Powder is observed powder under scanning electron microscope median size is 60nm, with pure water and ultrasonic dispersing, does not add under the condition of dispersion agent, and adopting the maximum particle diameter of laser particle analyzer test is 1.0 μ m.
Embodiment 2, to take indium metal, metallic tin be starting material, with hydrochloric acid with dissolving metal, be mixed with indium chloride, tin chloride high concentration solution, be mixed with 1.0M indium chloride, 0.05M tin chloride mixing solutions 200mL subsequently, and 40 gram D301 macroporous type anionite-exchange resin are added in the mixing solutions.Adopt magnetic stirring apparatus stirred solution 30min, filter with 50 purpose gauzes subsequently, anionite-exchange resin on the gauze adopts the sodium hydroxide solution regeneration of pH=13 in order to reuse in the future, colloidal solution after the filtration is transferred in the autoclave that has the tetrafluoroethylene liner, 3 ℃/min of average rate intensification, to 230 ℃, hydro-thermal reaction 16h cools to room temperature with the furnace, unloads still, with pure water washing reaction product and multipass repeatedly, through vacuum filtration, behind 102 ℃ of dry 8h, the 900 ℃ of calcining 3h, promptly obtain reaction product.
The ITO powder for preparing is observed powder under scanning electron microscope median size is 60nm, with pure water and ultrasonic dispersing, does not add under the condition of dispersion agent, and adopting the maximum particle diameter of laser particle analyzer test is 1.0 μ m.
Embodiment 3, to take indium metal, metallic tin be starting material, with nitric acid with dissolving metal, be mixed with indium nitrate, nitric acid tin high concentration solution, be mixed with 2.0M indium nitrate, 0.1M nitric acid tin mixing solutions 500mL subsequently, and 100 grams, 201 * 7 gel-type anionite-exchange resin are added in the mixing solutions.Adopt magnetic stirring apparatus to stir 45min, filter with 100 purpose gauzes subsequently, anionite-exchange resin on the gauze adopts the sodium hydroxide solution regeneration of pH=13 in order to reuse in the future, colloidal solution after the filtration is transferred in the autoclave that has the tetrafluoroethylene liner, 3 ℃/min of average rate intensification, to 200 ℃, hydro-thermal reaction 24h, cool to room temperature with the furnace, unload still, with pure water washing reaction product and multipass repeatedly, through vacuum filtration, behind 103 ℃ of dry 12h, the 1000 ℃ of calcining 4h, promptly obtain reaction product.
The ITO powder for preparing is observed powder under scanning electron microscope median size is 90nm, with pure water and ultrasonic dispersing, does not add under the condition of dispersion agent, and adopting the maximum particle diameter of laser particle analyzer test is 1.5 μ m.
Embodiment 4, to take indium metal, metallic tin be starting material, with nitric acid with dissolving metal, be mixed with indium nitrate, nitric acid tin high concentration solution, be mixed with 3.0M indium nitrate, 0.1M nitric acid tin mixing solutions 500mL subsequently, and 100 grams, 201 * 7 gel-type anionite-exchange resin are added in the mixing solutions.Adopt magnetic stirring apparatus to stir 45min, filter with 100 purpose gauzes subsequently, anionite-exchange resin on the gauze adopts the sodium hydroxide solution regeneration of pH=13 in order to reuse in the future, colloidal solution after the filtration is transferred in the autoclave that has the tetrafluoroethylene liner, 3 ℃/min of average rate intensification, to 220 ℃, hydro-thermal reaction 20h, cool to room temperature with the furnace, unload still, with pure water washing reaction product and multipass repeatedly, through vacuum filtration, behind 100-105 ℃ of dry 12h, the 1000 ℃ of calcining 4h, promptly obtain reaction product.
The ITO powder for preparing is observed powder under scanning electron microscope median size is 90nm, with pure water and ultrasonic dispersing, does not add under the condition of dispersion agent, and adopting the maximum particle diameter of laser particle analyzer test is 1.5 μ m.
Claims (9)
1. In
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that indium metal and metallic tin are dissolved in the mineral acid, the concentration of the mixing solutions that is made into is 0.5～3.0mol/L, again mixing solutions is carried out plastic resin treatment and obtain colloidal solution, insert colloidal solution in the autoclave and carry out hydro-thermal, hydrothermal temperature is 180～260 ℃, the described hydro-thermal reaction time is 4～24h, after reaction is finished product is washed, filters, prepare ITO dispersed nano powder after drying, the calcining, described indium metal and metallic tin are with SnO
2: In
2O
3Weight percent meter, per-cent is between 0～0.25.
2. In according to claim 1
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that described mineral acid includes the mixing acid of any two kinds of arbitrary proportions among hydrochloric acid, nitric acid, sulfuric acid or the above-mentioned three or above-mentioned three's arbitrary proportion mixing acid.
3. In according to claim 1
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that described colloidal solution is the solution that is obtained by polystyrene strong base or acrylic acid series weak base type macropore or gel-type anion exchange process mixing solutions.
4. according to claim 1 and 3 described In
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that described anionite-exchange resin after handling mixing solutions and obtaining colloidal solution, under strong alkali environments such as sodium hydroxide, potassium hydroxide regeneration standby.
5. In according to claim 1
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that described washing is with pure water or the water washing of electronics secondary.
6. In according to claim 1
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that described vacuum or the negative pressure filtration of being filtered into.
7. In according to claim 1
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that described drying is to carry out under 100-105 ℃, the time is 6～12h.
8. In according to claim 1
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that the calcining be under 500～1000 ℃, to carry out, the time is 2～4h.
9. In according to claim 1
2O
3, ITO dispersed nano powder hydrothermal preparing process, it is characterized in that the described In for preparing
2O
3, the ITO powder observes the median size≤100nm of powder under scanning electron microscope, with pure water and ultrasonic dispersing, do not add under the condition of dispersion agent, adopts the maximum particle diameter≤1.5 μ m of laser particle analyzer test.
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|---|---|---|---|
| CN 200310111223 CN1237006C (en) | 2003-10-10 | 2003-10-10 | In2O3 and ITO monodisperse nano powder hydrothermal preparation method |
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|---|---|---|---|
| CN 200310111223 CN1237006C (en) | 2003-10-10 | 2003-10-10 | In2O3 and ITO monodisperse nano powder hydrothermal preparation method |
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| CN1237006C CN1237006C (en) | 2006-01-18 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100343173C (en) * | 2005-09-30 | 2007-10-17 | 桂林电子工业学院 | Prepn of monodisperse nanometer In-Sn oxide powder |
| CN100364897C (en) * | 2005-02-25 | 2008-01-30 | 昆明理工大学 | Prepn process of nano In-Sn oxide powder |
| CN100378871C (en) * | 2005-01-07 | 2008-04-02 | 中南大学 | In203-Sn02 nano film coating material and its preparing method |
| CN100412535C (en) * | 2006-04-21 | 2008-08-20 | 湖南大学 | Prepn process of ITO nanometer line and its gas sensor |
| CN100465099C (en) * | 2005-12-08 | 2009-03-04 | 华东理工大学 | Method for preparing ITO powder with high sintering activity |
| CN102176351A (en) * | 2011-03-08 | 2011-09-07 | 东华大学 | Method for manufacturing ITO/PDMS (indium tin oxide/ polydimethylsiloxane) conductive composite material in filter paper template mode |
| CN102176348A (en) * | 2011-01-10 | 2011-09-07 | 东华大学 | Preparation of indium-tin oxide/PDMS(polydimethylsiloxane) resin conducting material based on textile template |
| CN102332325A (en) * | 2011-10-13 | 2012-01-25 | 扬州大学 | In (indium)-Sn (stannum)-Mo (molybdenum)-Nb (niobium)-codoped transparent conductive film and manufacturing method thereof |
| CN102786080A (en) * | 2012-07-18 | 2012-11-21 | 中国科学院福建物质结构研究所 | Indium tin oxide compound, its preparation method and its photocatalytic application |
| CN107153083A (en) * | 2017-05-22 | 2017-09-12 | 江苏时瑞电子科技有限公司 | A kind of preparation method of gas containing nitrogen oxide sensor |
| CN107867715A (en) * | 2017-11-07 | 2018-04-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of tin dioxide nanometer material for low concentration Nitrogen dioxide testing and products thereof and application |
-
2003
- 2003-10-10 CN CN 200310111223 patent/CN1237006C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100378871C (en) * | 2005-01-07 | 2008-04-02 | 中南大学 | In203-Sn02 nano film coating material and its preparing method |
| CN100364897C (en) * | 2005-02-25 | 2008-01-30 | 昆明理工大学 | Prepn process of nano In-Sn oxide powder |
| CN100343173C (en) * | 2005-09-30 | 2007-10-17 | 桂林电子工业学院 | Prepn of monodisperse nanometer In-Sn oxide powder |
| CN100465099C (en) * | 2005-12-08 | 2009-03-04 | 华东理工大学 | Method for preparing ITO powder with high sintering activity |
| CN100412535C (en) * | 2006-04-21 | 2008-08-20 | 湖南大学 | Prepn process of ITO nanometer line and its gas sensor |
| CN102176348A (en) * | 2011-01-10 | 2011-09-07 | 东华大学 | Preparation of indium-tin oxide/PDMS(polydimethylsiloxane) resin conducting material based on textile template |
| CN102176348B (en) * | 2011-01-10 | 2012-09-05 | 东华大学 | Preparation of indium-tin oxide/PDMS(polydimethylsiloxane) resin conducting material based on textile template |
| CN102176351A (en) * | 2011-03-08 | 2011-09-07 | 东华大学 | Method for manufacturing ITO/PDMS (indium tin oxide/ polydimethylsiloxane) conductive composite material in filter paper template mode |
| CN102332325A (en) * | 2011-10-13 | 2012-01-25 | 扬州大学 | In (indium)-Sn (stannum)-Mo (molybdenum)-Nb (niobium)-codoped transparent conductive film and manufacturing method thereof |
| CN102786080A (en) * | 2012-07-18 | 2012-11-21 | 中国科学院福建物质结构研究所 | Indium tin oxide compound, its preparation method and its photocatalytic application |
| CN107153083A (en) * | 2017-05-22 | 2017-09-12 | 江苏时瑞电子科技有限公司 | A kind of preparation method of gas containing nitrogen oxide sensor |
| CN107867715A (en) * | 2017-11-07 | 2018-04-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of tin dioxide nanometer material for low concentration Nitrogen dioxide testing and products thereof and application |
| CN107867715B (en) * | 2017-11-07 | 2019-06-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of tin dioxide nanometer material for low concentration Nitrogen dioxide testing and products thereof and application |
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