CN100534908C - Process for preparing In2O3 nano-wire - Google Patents
Process for preparing In2O3 nano-wire Download PDFInfo
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- CN100534908C CN100534908C CNB2007100459135A CN200710045913A CN100534908C CN 100534908 C CN100534908 C CN 100534908C CN B2007100459135 A CNB2007100459135 A CN B2007100459135A CN 200710045913 A CN200710045913 A CN 200710045913A CN 100534908 C CN100534908 C CN 100534908C
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- nano wire
- mentioned
- nanometer
- in2o3
- white
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Abstract
The present invention relates to process of making nanometer In2O3 line in great length-to-diameter ratio, and belongs to the field of nanometer material preparing technology. Through forming complex with oxalic acid as the complexing agent and soluble In salt in certain pH condition, hydrothermal treating the complex at certain temperature to obtain white nanometer In(OH)3 precursor, and final calcining the precursor at 400 deg.c, the ultimate product nanometer In2O3 line is obtained. Serial analyses on the ultimate product show that the nanometer In2O3 line in cubic body-centered phase has diameter of 40-60 nm and length of 2-10 microns.
Description
Technical field
The present invention relates to a kind of In
2O
3The manufacture method of nano wire, the metal nanometer material manufacturing process technology field.
Technical background
In
2O
3Be a kind of important semiconductor material with wide forbidden band, have in fields such as semi-conducting material, gas sensitive material and optical materials comparatively widely and use In
2O
3Nano material is the focus that people study always.At present, about making In
2O
3The report of nano wire is less, and traditional manufacture method mainly is vapour deposition process and thermal evaporation.These two kinds of methods exist required producing apparatus costliness, energy expenditure height, the not high shortcoming of resulting product purity.Adopt wet chemistry method directly to make one dimension In
2O
3Nano material has obvious superiority, does not for example need the product purity of special equipment, gained higher, is suitable for a large amount of manufacturings, is convenient to suitability for industrialized production etc.But because In
2O
3Usually have high symmetric cubic-crystal, therefore be not easy to make the bigger In of draw ratio with wet chemistry method
2O
3Nano wire.
Summary of the invention
The purpose of this invention is to provide a kind of In
2O
3The manufacture method of nano wire.
For achieving the above object, the present invention adopts following technical scheme:
A kind of In
2O
3The manufacture method of nano wire is characterized in that the concrete steps of this method are:
A. with solubility indium salt and oxalic acid, the mol ratio by 3: 1～2 is dissolved in the deionized water;
B. regulate pH value to 2.0～3.0 of above-mentioned solution, vigorous stirring obtains the gluey turbid liquid of a kind of white;
C. the gluey turbid liquid of above-mentioned white is sealed the back under 160-220 ℃ of temperature, be incubated 24-48 hour; With products obtained therefrom with deionized water wash after, vacuum-drying under 60 ℃ of temperature, can obtain white In (OH)
3The nano wire presoma;
D. with above-mentioned In (OH)
3The nano wire presoma can obtain In in 280-600 ℃ of lower calcining 3-30 minute
2O
3The nano wire product.
Above-mentioned solubility indium salt is indium chloride or indium nitrate.
Adopt NaOH or potassium hydroxide solution to come the pH value of regulator solution.
The present invention adopts hydro-thermal-calcining path to make the In of high length-diameter ratio
2O
3Nano wire, purity is higher, be easy in a large amount of manufacturings, method advanced person, the document at home and abroad report is not arranged.
Description of drawings
Fig. 1 is X-ray powder diffraction (XRD) spectrogram of the product of the inventive method preparation
Fig. 2 is Thermal Synthetic Analysis (TG-DSC) spectrogram of the product of the inventive method preparation
Fig. 3 is transmission electron microscope (TEM) collection of illustrative plates of the product of the inventive method preparation
Fig. 4 is scanning electronic microscope (SEM) collection of illustrative plates of the product of the inventive method preparation
Embodiment:
Embodiment one: raw material is indium chloride, oxalic acid and sodium hydroxide.
E. take by weighing 0.94g indium chloride and 0.134g oxalic acid, it is dissolved in the deionized water of 40mL;
F. add about 0.128gNaOH in mentioned solution, adjusting pH value is to the 2.9-3.0, and vigorous stirring obtains the gluey turbid liquid of a kind of white;
G. after above-mentioned mixed solution being stirred 1 hour, be transferred in the 50mL reactor of a cleaning sealing;
H. aforesaid reaction vessel is placed 180 ℃ of baking ovens, be incubated 30 hours;
I. take out reactor, after the product with deionized water washing that obtains, place 60 ℃ baking oven vacuum-drying, can obtain the In (OH) of white
3The nano wire presoma.
J. with above-mentioned In (OH)
3The nano wire presoma can obtain In in 400 ℃ of lower calcinings 5 minutes
2O
3The nano wire product.
Embodiment two: raw material is indium nitrate, oxalic acid and potassium hydroxide.
K. take by weighing 0.94g indium chloride and 0.134g oxalic acid, it is dissolved in the deionized water of 40mL;
L. add about 0.128gNaOH in mentioned solution, regulate about pH value to 2.0, vigorous stirring obtains the gluey turbid liquid of a kind of white;
M. after above-mentioned mixed solution being stirred 1 hour, be transferred in the 50mL reactor of a cleaning sealing;
N. with aforesaid reaction vessel as in 220 ℃ of baking ovens, be incubated 48 hours;
O. take out reactor, after the product with deionized water washing that obtains, place 60 ℃ baking oven vacuum-drying, can obtain the In (OH) of white
3The nano wire presoma.
P. with above-mentioned In (OH)
3The nano wire presoma can obtain In in 600 ℃ of lower calcinings 30 minutes
2O
3The nano wire product.
Analyze (TG-DSC), transmission electron microscope (TEM) and scanning electronic microscope characterization methods such as (SEM) crystalline phase, pattern and the size etc. of product are analyzed with X-ray powder diffraction (XRD), comprehensive heat.Analysis result shows the In that can successfully produce the body-centred cubic phase with the inventive method
2O
3Nano wire, its diameter are 40-60nm, and length is 2-10 μ m.
Claims (3)
1. In
2O
3The manufacture method of nano wire is characterized in that the concrete steps of this method are:
A. with solubility indium salt and oxalic acid, the mol ratio by 3: 1～2 is dissolved in the deionized water;
B. regulate pH value to 2.0～3.0 of above-mentioned solution, vigorous stirring obtains the gluey turbid liquid of a kind of white;
C. the gluey turbid liquid of above-mentioned white is sealed the back under 160-220 ℃ of temperature, be incubated 24-48 hour; With products obtained therefrom with deionized water wash after, vacuum-drying under 60 ℃ of temperature, can obtain white In (OH)
3The nano wire presoma;
D. with above-mentioned In (OH)
3The nano wire presoma can obtain In in 280-600 ℃ of lower calcining 3-30 minute
2O
3The nano wire product.
2. In according to claim 1
2O
3The manufacture method of nano wire is characterized in that above-mentioned solubility indium salt is inidum chloride or indium nitrate.
3. In according to claim 1
2O
3The manufacture method of nano wire is characterized in that adopting NaOH or potassium hydroxide solution to come the pH value of regulator solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100459135A CN100534908C (en) | 2007-09-13 | 2007-09-13 | Process for preparing In2O3 nano-wire |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100459135A CN100534908C (en) | 2007-09-13 | 2007-09-13 | Process for preparing In2O3 nano-wire |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101148266A CN101148266A (en) | 2008-03-26 |
| CN100534908C true CN100534908C (en) | 2009-09-02 |
Family
ID=39248979
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100459135A Expired - Fee Related CN100534908C (en) | 2007-09-13 | 2007-09-13 | Process for preparing In2O3 nano-wire |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100534908C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515257A (en) * | 2012-01-16 | 2012-06-27 | 济南大学 | Preparation method for nano-In2O3 gas-sensing material of hollow fiber structure |
| CN105668612A (en) * | 2016-03-15 | 2016-06-15 | 济南大学 | Preparation method of hexagonal-tube-shaped indium oxide with complex as precursor |
| CN105967223A (en) * | 2016-05-05 | 2016-09-28 | 扬州大学 | Tubular indium hydroxide/indium oxide micro-nano material synthesis method |
| CN110436514A (en) * | 2018-05-05 | 2019-11-12 | 北京化工大学 | The preparation method and application of transition metal element doped flower-shaped indium oxide gas sensitive |
| CN116143167A (en) * | 2023-02-22 | 2023-05-23 | 重庆大学 | Growing In based on polycrystalline InSe 2 O 3 Method for preparing nanowire |
-
2007
- 2007-09-13 CN CNB2007100459135A patent/CN100534908C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 氧化铟纳米材料的水热合成、结构表征及其气敏性能研究. 徐甲强等.传感技术学报，第20卷第1期. 2007 |
| 氧化铟纳米材料的水热合成、结构表征及其气敏性能研究. 徐甲强等.传感技术学报，第20卷第1期. 2007 * |
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| Publication number | Publication date |
|---|---|
| CN101148266A (en) | 2008-03-26 |
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Granted publication date: 20090902 Termination date: 20120913 |