CN102863014A - Preparation method of shape-controllable nano indium oxides - Google Patents
Preparation method of shape-controllable nano indium oxides Download PDFInfo
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- CN102863014A CN102863014A CN201210395936XA CN201210395936A CN102863014A CN 102863014 A CN102863014 A CN 102863014A CN 201210395936X A CN201210395936X A CN 201210395936XA CN 201210395936 A CN201210395936 A CN 201210395936A CN 102863014 A CN102863014 A CN 102863014A
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Abstract
The invention relates to a preparation method of shape-controllable nano indium oxides, wherein indium compounds and sodium acetates are respectively dispersed into solution of glycols and water at the room temperature to prepare suspension liquid; then the suspension liquid is put into a reactor to prepare the indium compounds through the solvent thermal reaction; and the nano indium oxides are obtained by washing, drying and annealing. The shape of the prepared nano indium oxides comprises nanocrystalline, nanorod and nano square body. The preparation method prepares indium oxide nano-structures with different shapes by controlling the proportion of the water in raw materials without any templates and structure-directing agent. The preparation method has the advantages of simple process, easily-gained raw materials and low production cost.
Description
Technical field
The present invention relates to a kind of compound of indium, especially a kind of preparation method of pattern nano indium oxide with controllable.
Background technology
Indium sesquioxide is a kind of very important transparent semiconductor material, in the past few decades, people conduct extensive research it, and Indium sesquioxide direct band gap at room temperature is about 3.6eV, is widely used in opto-electronic device, solar cell, liquid-crystal display and gas sensor etc.
In recent years, nanosecond science and technology have obtained the development of advancing by leaps and bounds, the preparation of nano indium oxide and be applied to one of focus in recent years science and technology research both at home and abroad.At present, the preparation method of Indium sesquioxide nanometer has vacuum thermal evaporation method, sputtering method, sol-gel method, chemical Vapor deposition process etc.Preparation method's difference because of the Indium sesquioxide nanometer, make the nano indium oxide structure of making varied, its crystal proterties, pattern, degree of crystallinity etc. are depended in the application of simultaneous oxidation indium, and crystal proterties of Indium sesquioxide, pattern, degree of crystallinity etc. all depend on the selection of its synthetic method.For example, in the CN102234130A Chinese invention patent application of announcing on November 9th, 2011 disclosed " a kind of easy method for preparing Indium sesquioxide nanometer side body ", it is quaternary microemulsion and the sodium hydroxide solution reaction that utilizes nonionogenic tenside alkyl polyoxyethylene ether, cosurfactant n-Octanol, hexanaphthene and the indium nitrate aqueous solution to form, obtain presoma through the hydro-thermal assisted reaction again, roasting obtains relatively uniformly Indium sesquioxide cubes of pattern size through retort furnace.In the disclosure file, the solvent of its use is many and pollution is arranged, and can only be preparation Indium sesquioxide nanocubes.
Summary of the invention
Many and can only prepare a kind of deficiency of nano indium oxide of pattern in order to overcome in the prior art preparation nano indium oxide solvent for use, the invention provides a kind of preparation method of pattern nano indium oxide with controllable.This preparation method's technique is simple, raw materials used being easy to get, and production cost is low, only by the ratio of the water in the conditioned reaction system, can prepare the different indium oxide nanostructure of pattern without any need for template and structure directing agent.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of pattern nano indium oxide with controllable is characterized in that: process the following step:
(1), ethylene glycol and water are joined in the beaker according to a certain percentage, mix, get aqueous glycol solution, in this aqueous glycol solution, the volume of described water is 3～33% of overall solution volume;
(2), indium chloride and Sodium acetate trihydrate are joined in the step (1) in the resulting aqueous glycol solution by a certain percentage, stirring at room is even, gets suspension; Wherein, the quality of described indium chloride and Sodium acetate trihydrate and be 4.8%～5.6% of aqueous glycol solution quality, the mass ratio of described indium chloride and described Sodium acetate trihydrate is 1:3～5;
(3), the suspension that step (2) is obtained is transferred in the polytetrafluoroethyllining lining stainless steel cauldron of then this liner being packed into, envelope still;
(4), reactor is heated to 150～200 ℃ after, be incubated 4～24 hours;
(5), carry out suction filtration after naturally cooling to room temperature, the product that will obtain after then will reacting adopts distilled water and ethanol repeatedly to wash successively, obtains the compound of indium;
The compound of the indium that (6) step (5) is obtained is put into dry 5 h of 60 ℃ of vacuum drying ovens;
(7) compound of dried indium was annealed 0.5～2 hour under 400～800 ℃, naturally cool to room temperature, namely get the nano indium oxide of different-shape.
The present invention at room temperature is distributed to indium chloride and Sodium acetate trihydrate to prepare suspension in the aqueous glycol solution, then suspension is put into have in the teflon-lined reactor and made the Indium sesquioxide solid by solvent thermal reaction, again through distilled water and washing with alcohol, dry, high temperature annealing obtains the nano indium oxide of nanocrystalline, nanometer rod or nanometer side's body behind the naturally cooling.The present invention is by the proportioning of water in the simple adjustment reaction system, without any need for masterplate, structure directing agent namely prepared the different indium oxide nanostructure of pattern, for pattern controllable oxidization indium nanostructure synthetic provides a kind of easily method.This preparation method's technique is simple, raw materials used being easy to get, and production cost is low.
Description of drawings
The present invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is the XRD figure of products therefrom;
Fig. 2 is the SEM figure of embodiment 1 products therefrom;
Fig. 3 is the SEM figure of embodiment 2 products therefroms;
Fig. 4 is the SEM figure of embodiment 3 products therefroms;
Fig. 5 is the SEM figure of embodiment 4 products therefroms;
Fig. 6 is the SEM figure of embodiment 5 products therefroms.
Embodiment
Embodiment 1
A kind of preparation method of pattern nano indium oxide with controllable, its process the following step:
(1), add 32.3mL ethylene glycol and 1mL water in the 100 mL beakers, mix, get aqueous glycol solution;
(2), the indium chloride of 0.44g and the Sodium acetate trihydrate of 1.8g are joined in the aqueous glycol solution of gained, stirring at room evenly after, get suspension; In this suspension, the mass ratio of indium chloride and Sodium acetate trihydrate is 1:4, the quality of indium chloride and Sodium acetate trihydrate and be 4.8% of aqueous glycol solution quality;
(3), resulting suspension is transferred in the tetrafluoroethylene reaction vessel, suspension accounts for 80% of tetrafluoroethylene reaction vessel volume, the stainless steel cauldron of then reactor being packed into, envelope still;
(4), after being heated to 200 ℃, reactor is incubated 4h;
(5), carry out suction filtration after naturally cooling to room temperature, the product that will obtain after then will reacting adopts distilled water and ethanol respectively to wash 3 times, obtains Indium sesquioxide;
(6), the Indium sesquioxide that obtains is put into dry 5 h of 60 ℃ of vacuum drying ovens;
(7) dried Indium sesquioxide was annealed 0.5 hour under 800 ℃, naturally cool to room temperature, namely get nano indium oxide.
As seen from Figure 1, the present embodiment preparation is the Indium sesquioxide of Emission in Cubic.SEM picture by Fig. 2 can find out, the Indium sesquioxide of preparation is nanocrystalline, and particle diameter is about 10 nm, and granular size is homogeneous relatively, and particle surface is more coarse, is uniformly dispersed.
A kind of preparation method of pattern nano indium oxide with controllable, its process the following step:
(1), add 25mL ethylene glycol and 5mL water in the 100 mL beakers, mix, get aqueous glycol solution;
(2), the indium chloride of 0.6g and the Sodium acetate trihydrate of 1.8g are joined in the aqueous glycol solution of gained, stirring at room evenly after, get suspension; In this suspension, the mass ratio of indium chloride and Sodium acetate trihydrate is 1:3, the quality of indium chloride and Sodium acetate trihydrate and be 5.45% of aqueous glycol solution quality;
(3), resulting suspension is transferred in the tetrafluoroethylene reaction vessel, this suspension accounts for 80% of tetrafluoroethylene reaction vessel volume, the stainless steel cauldron of then reactor being packed into, envelope still;
(4), after being heated to 180 ℃, reactor is incubated 12h;
(5), carry out suction filtration after naturally cooling to room temperature, the product that will obtain after then will reacting adopts distilled water and ethanol respectively to wash 3 times, obtains InOOH;
(6), will obtain InOOH and put into dry 5 h of 60 ℃ of vacuum drying ovens;
(7), with dried InOOH in 600 ℃ of lower annealing 1 hour, naturally cool to room temperature, namely get nano indium oxide.
XRD figure and Fig. 1 of the product of the present embodiment are similar, are Emission in Cubic oxidation indium.SEM picture by Fig. 3 can find out, the Indium sesquioxide of preparation is nanometer rod homogeneous, that two ends are sharp-pointed, and the diameter of the nanometer rod that these are long is about 110 nm, and length is between 800 –, 1500 nm.In addition, some nanometer rod combine and have formed nano rod bundle.
Embodiment 3
A kind of preparation method of pattern nano indium oxide with controllable, its process the following step:
(1), add 20mL ethylene glycol and 10mL water in the 100 mL beakers, mix, get aqueous glycol solution;
(2), the indium chloride of 0.6g and the Sodium acetate trihydrate of 1.8g are joined in the aqueous glycol solution of gained, stirring at room evenly after, get suspension; In this suspension, the mass ratio of indium chloride and Sodium acetate trihydrate is 1:3, the quality of indium chloride and Sodium acetate trihydrate and be 5.6% of aqueous glycol solution quality;
(3), resulting suspension is transferred in the tetrafluoroethylene reaction vessel, suspension accounts for 90% of tetrafluoroethylene reaction vessel volume, the stainless steel cauldron of then reactor being packed into, envelope still;
(4), after being heated to 160 ℃, reactor is incubated 18h;
(5), carry out suction filtration after naturally cooling to room temperature, the product that will obtain after then will reacting adopts distilled water and ethanol respectively to wash 4 times, obtains indium hydroxide;
(6), the indium hydroxide that obtains is put into dry 5 h of 60 ℃ of vacuum drying ovens;
(7), with dried indium hydroxide in 400 ℃ of lower annealing 2 hours, naturally cool to room temperature, namely get nano indium oxide.
XRD figure and Fig. 1 of the product of the present embodiment are similar, are Emission in Cubic oxidation indium.SEM picture by Fig. 4 can find out, the Indium sesquioxide of preparation is nanometer blocks.The length of side of most of nanometer blocks also has the length of side of a small amount of nanometer blocks about 100 nm at 20-40 nm.
Embodiment 4
A kind of preparation method of pattern nano indium oxide with controllable, its process the following step:
(1), add 26mL ethylene glycol and 4mL water in the 100 mL beakers, mix, get aqueous glycol solution;
(2), the indium chloride of 0.36g and the Sodium acetate trihydrate of 1.8g are joined in the aqueous glycol solution of gained, stirring at room evenly after, get suspension; In this suspension, the mass ratio of indium chloride and Sodium acetate trihydrate is 1:5, the quality of indium chloride and Sodium acetate trihydrate and be 4.89% of aqueous glycol solution quality;
(3), resulting suspension is transferred in the tetrafluoroethylene reaction vessel, make suspension account for 70% of tetrafluoroethylene reaction vessel volume, the stainless steel cauldron of then reactor being packed into, envelope still;
(4), after being heated to 150 ℃, reactor is incubated 24h;
(5), carry out suction filtration after naturally cooling to room temperature, the product that will obtain after then will reacting adopts distilled water and ethanol respectively to wash 3 times, obtains the compound of indium;
(6), the compound of the indium that obtains is put into dry 5 h of 60 ℃ of vacuum drying ovens;
(7), with the compound of dried indium in 500 ℃ of lower annealing 1.5 hours, naturally cool to room temperature, namely get nano indium oxide.
XRD figure and Fig. 1 of the product of the present embodiment are similar, are Emission in Cubic oxidation indium.SEM picture by Fig. 5 can find out, the Indium sesquioxide of preparation is the mixture of nano particle and nanometer rod.Wherein, majority is nanometer rod and nanometer rod composition, and the diameter of nanometer rod is at 100～300nm, and length also has a small amount of nano particle to exist at 1000～1600nm, and its particle diameter is about 50nm.
Embodiment 5
A kind of preparation method of pattern nano indium oxide with controllable, its process the following step:
(1), add 22.5mL ethylene glycol and 7.5mL water in the 100 mL beakers, mix, get aqueous glycol solution;
(2), the indium chloride of 0.44g and the Sodium acetate trihydrate of 1.8g are joined in the aqueous glycol solution of gained, stirring at room evenly after, get suspension; In this suspension, the mass ratio of indium chloride and Sodium acetate trihydrate is 1:4, the quality of indium chloride and Sodium acetate trihydrate and be 5.14% of aqueous glycol solution quality;
(3), resulting suspension is transferred in the tetrafluoroethylene reaction vessel, make suspension account for 80% of tetrafluoroethylene reaction vessel volume, the stainless steel cauldron of then reactor being packed into, envelope still;
(4) after being heated to 200 ℃, reactor is incubated 12h;
(5) carry out suction filtration after naturally cooling to room temperature, the product that will obtain after then will reacting adopts distilled water and ethanol respectively to wash 2 times, obtains the compound of indium;
(6) compound of the indium that obtains is put into dry 5 h of 60 ℃ of vacuum drying ovens;
(7) compound of dried indium was annealed 1.8 hours under 450 ℃, naturally cool to room temperature, namely get nano indium oxide.
XRD figure and Fig. 1 of the product of the present embodiment are similar, are Emission in Cubic oxidation indium.SEM picture by Fig. 6 can find out, the Indium sesquioxide of preparation is the mixture of nanometer blocks and nanometer rod.The length of side of most of nanometer blocks also has a small amount of nanometer rod and nanometer rod composition to exist at 20-40 nm, and wherein about maximum nanometer rod diameter 300nm, length is about 1500nm.
Claims (1)
1. the preparation method of a pattern nano indium oxide with controllable is characterized in that: through the following step:
(1), ethylene glycol and water are joined in the beaker according to a certain percentage, mix, get aqueous glycol solution, in this aqueous glycol solution, the volume of described water is 3～33% of overall solution volume;
(2), indium chloride and Sodium acetate trihydrate are joined in the step (1) in the resulting aqueous glycol solution by a certain percentage, stirring at room is even, gets suspension; Wherein, the quality of described indium chloride and Sodium acetate trihydrate and be 4.8%～5.6% of aqueous glycol solution quality, the mass ratio of described indium chloride and described Sodium acetate trihydrate is 1:3～5;
(3), the suspension that step (2) is obtained is transferred in the polytetrafluoroethyllining lining stainless steel cauldron of then this liner being packed into, envelope still;
(4), reactor is heated to 150～200 ℃ after, be incubated 4～24 hours;
(5), carry out suction filtration after naturally cooling to room temperature, the product that will obtain after then will reacting adopts distilled water and ethanol repeatedly to wash successively, obtains the compound of indium;
The compound of the indium that (6) step (5) is obtained is put into dry 5 h of 60 ℃ of vacuum drying ovens;
(7) compound of dried indium was annealed 0.5～2 hour under 400～800 ℃, naturally cool to room temperature, namely get the nano indium oxide of different-shape.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478410A (en) * | 2014-12-10 | 2015-04-01 | 中国人民解放军电子工程学院 | Preparation method of nano H-In2O3 ceramic |
| CN105129841A (en) * | 2015-05-16 | 2015-12-09 | 青岛科技大学 | Preparation method of indium oxide with octahedral morphology |
| CN105271371A (en) * | 2015-10-12 | 2016-01-27 | 武汉工程大学 | Flower-shaped indium oxide microrod material, and preparation method and application thereof |
| CN106517312A (en) * | 2017-01-16 | 2017-03-22 | 清华大学 | Nanometer indium oxide and preparation method thereof |
| CN115784297A (en) * | 2022-11-21 | 2023-03-14 | 西安近代化学研究所 | Spindle-shaped In 2 O 3 Preparation method and application of nano material |
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| CN101182031A (en) * | 2007-11-27 | 2008-05-21 | 山东大学 | Method for preparing indium oxide nano thread ordered aggregation |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478410A (en) * | 2014-12-10 | 2015-04-01 | 中国人民解放军电子工程学院 | Preparation method of nano H-In2O3 ceramic |
| CN105129841A (en) * | 2015-05-16 | 2015-12-09 | 青岛科技大学 | Preparation method of indium oxide with octahedral morphology |
| CN105271371A (en) * | 2015-10-12 | 2016-01-27 | 武汉工程大学 | Flower-shaped indium oxide microrod material, and preparation method and application thereof |
| CN106517312A (en) * | 2017-01-16 | 2017-03-22 | 清华大学 | Nanometer indium oxide and preparation method thereof |
| CN106517312B (en) * | 2017-01-16 | 2018-08-28 | 清华大学 | A kind of nano indium oxide and preparation method thereof |
| CN115784297A (en) * | 2022-11-21 | 2023-03-14 | 西安近代化学研究所 | Spindle-shaped In 2 O 3 Preparation method and application of nano material |
| CN115784297B (en) * | 2022-11-21 | 2024-03-29 | 西安近代化学研究所 | Spindle-shaped In 2 O 3 Preparation method and application of nano material |
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Application publication date: 20130109 |