CN102060320B - Method for preparing indium oxide hollow sphere at low temperature - Google Patents
Method for preparing indium oxide hollow sphere at low temperature Download PDFInfo
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- CN102060320B CN102060320B CN2010105451625A CN201010545162A CN102060320B CN 102060320 B CN102060320 B CN 102060320B CN 2010105451625 A CN2010105451625 A CN 2010105451625A CN 201010545162 A CN201010545162 A CN 201010545162A CN 102060320 B CN102060320 B CN 102060320B
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- reaction
- hollow sphere
- temperature
- hollow ball
- indium sesquioxide
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Abstract
The invention relates to a method for preparing an indium oxide hollow sphere at low temperature, which is characterized by using In(NO3)3 as the raw material, ethanol as the solvent and three-block polymer P123 (polyoxyethylene-polyoxypropylene-polyoxyethylene, EO20PO70EO20, Mw=5800) as the additive, performing constant-temperature reaction at 120 to 150 DEG C for 4-10h, washing the product of reaction with water and ethanol, and drying to obtain In2O3 hollow sphere with good crystallization without calcinating at high temperature. The average diameter of the hollow sphere is about 500 nanometers and the wall thickness is dozens of nanometers. The method has the advantages of reasonable design and simple process, and the product of reaction has single phase, controllable appearance, even size distribution and low reaction temperature.
Description
Technical field
The invention belongs to Indium sesquioxide nano material preparation technical field, particularly the preparation method of Indium sesquioxide hollow structure under the lesser temps.
Background technology
Indium sesquioxide (In
2O
3) be a kind of important n-type semiconductor oxide, have high conductivity and visible light transmissivity.The Indium sesquioxide of nanostructure; Owing to the quantum confined effect with current carrier shows electricity, the optical property of many novelties, can be used for solar cell, transparent conductor, window well heater, opto-electronic device, flat-panel monitor, UV, visible light laser apparatus, detector, Organic Light Emitting Diode, building glass and transmitter etc.
Transmitter is one of the most promising Application Areas of nanoparticle.Along with the development of the modernization of industry and the concern of people's environmental pollution in recent years, people are to monitoring and prediction inflammable, explosive, toxic gas, the high performance gas sensor of seeking development.In the detection method of gas, Gas Sensors of Electric Resistance Semiconductors is occupied crucial status because of the gaseous species of its measurement is many, highly sensitive, cheap, simple for production.SnO
2, ZnO, Fe
2O
3Be applied to every field etc. traditional gas sensitive, but also have poor selectivity, problem such as service temperature is high, stability is satisfactory not to the utmost.Therefore, the application of the exploitation of novel material and nanotechnology has great significance to addressing the above problem.And Indium sesquioxide is compared with White tin oxide with zinc oxide as the up-and-coming youngster, though the Indium sesquioxide cost is high, surveying some gas, such as Cl
2, O
2, NH
3, NO
2, formaldehyde, hydrogen, ethanol has highly sensitive, swift characteristics during chlorophenol, therefore study also morely.
In
2O
3Be based on the absorption of gas to be measured and the caused electricity of surface reaction process that follows hard on is led variation as the principle of work of gas sensor, therefore increasing its specific surface area is an important channel of improving air-sensitive performance.Hollow ball has low density, high-specific surface area, the advantage of hypertonicity; And structure the regularly arranged of piece usually can cause orderly cavernous structure; For the absorption of gas provides bigger solid space, overcome the resistance of electronic migration, thereby can effectively improve the air-sensitive performance of material; Improve the sensitivity of device, shorten the gas time of response.
(CHEMISTRY COMMUNICATION 2009 4756-4758) has reported In Britain's " chemical communication "
3+Be adsorbed on the ligand polymer surface, calcine down for 550 ℃ and obtain bar-shaped hollow structure Indium sesquioxide; (CHEMISTRYCOMMUNICATION 2009, reported that 2747-2749) calcining 1h with InOOH and an ammonium nitrate down at 250-500 ℃ obtains the Indium sesquioxide hollow ball for Britain's " chemical communication "; Switzerland " transmitter and topworks, B collects: chemical sensor " (Sensors andActuators B:Chemical138,497-503,2009) has reported that 600 ℃ are calcined by In (NO down
3)
3Non-crystalline state presoma with the amino acid preparation has obtained the Indium sesquioxide hollow ball; Britain's " nanosecond science and technology " (Nanotechnology 19,345704,2008) has reported In
3+Be adsorbed on carbon ball surface, 500 ℃ of following calcinings remove the carbon elimination ball template and obtain the Indium sesquioxide hollow ball; U.S.'s " transmitter wall bulletin " (Sensor Letters 8 (2), 355-361,2010) has reported and has utilized solvent thermal process that the mixing solutions hydrolysis of indium chloride and sucrose obtains presoma, calcines presoma down at 600 ℃ then, has obtained the Indium sesquioxide hollow ball.Above preparation feedback all needs higher temperature of reaction, and process is complicated, needs higher cost, is unfavorable for a large amount of preparation Indium sesquioxide hollow balls.Therefore, the Indium sesquioxide nano material of explore simply, synthetic route being synthesized hollow structure efficiently has crucial meaning.
Summary of the invention
Defective to prior art; The present invention provides a kind of solvent thermal reaction that utilizes; Controlled at next step preparation pattern of relatively low temperature, the method for the Indium sesquioxide hollow ball of even size distribution is to overcome the defective of prior art temperature of reaction height and complex process.
A kind of low temperature of the present invention prepares the method for Indium sesquioxide hollow ball, it is characterized in that 1 mmole In (NO
3)
3Be dissolved in the 30mL ethanol, add 1～5g triblock polymer P123 (polyoxyethylene-poly-oxypropylene polyoxyethylene, EO
20PO
70EO
20, M
w=5800) and 1～3mL methane amide, be sealed in after the mixing in the polytetrafluoroethyllining lining stainless steel autoclave, 120-150 ℃ of reaction be more than 4 hours, product through washing, ethanol wash, spinning and drying, promptly obtain the Indium sesquioxide hollow ball.
Compared with prior art, the present invention prepares the method for Indium sesquioxide hollow ball, and temperature of reaction is low than prior art, and the products therefrom thing is mutually simple, and one-step synthesis reacts simple and easy to control, does not need high-temperature calcination; Prepared Indium sesquioxide hollow ball, mean diameter is about 500 nanometers, wall thickness tens nanometers.This method is reasonable in design, and technology is simple, and the product thing is mutually single, and pattern is controlled, even size distribution, and temperature of reaction is low.
Description of drawings
Fig. 1 is the In that adopts the inventive method preparation
2O
3The XRD figure spectrum of hollow ball.
Fig. 2 is In
2O
3The field emission microscope photo (SEM) of hollow ball.
Fig. 3 is In
2O
3The transmission electron microscope photo (TEM) of hollow ball.
Fig. 4 is In among Fig. 3
2O
3The corresponding high resolution transmission electron microscopy photo of hollow ball (HRTEM).
Embodiment
Embodiment 1:
A kind of preparation method of Indium sesquioxide hollow ball mainly comprises solvent thermal reaction-spinning-drying process, and concrete preparation process is following:
Take by weighing 1 mmole In (NO
3)
3Be dissolved in the 30mL ethanol, constant temperature stirs in 25 ℃ of water-baths, adds 1g triblock polymer P123 (polyoxyethylene-poly-oxypropylene polyoxyethylene, EO
20PO
70EO
20, M
w=5800) and the 2mL methane amide, obtain settled solution after the dissolving, transferring to volume then is in the polytetrafluoroethyllining lining stainless steel autoclave of 50mL.After the autoclave sealing, isothermal reaction 10h under 120 ℃ of conditions naturally cools to room temperature.Product in the still is inclined to, and spinning is respectively washed three times with deionized water and absolute ethyl alcohol, and vacuum-drying obtains the Indium sesquioxide hollow ball.
Constant temperature described in step reaction down is the baking oven that reaction kettle is placed the ability accurate temperature controlling, perhaps reaction kettle is placed the resistance furnace of ability accurate temperature controlling.
The preferred 50-60 of vacuum-drying temperature described in the step ℃.
The product thing uses X-ray powder diffraction (XRD) to test mutually; The instrument model is a Bruker D8X-x ray diffractometer x, and X-ray source is that Cu-K α radiation
scanning angle scope 2 θ are between 10 °～80 °.
Fig. 1 is the X-ray powder diffraction spectrogram of product.All diffraction peaks all fit like a glove with cubic phase oxygen indium (JCPDS Card No.06-0416), explain that product is single thing phase c-In
2O
3, unit cell parameters
The pattern of sample is observed with field emission microscope (FESEM) JSM-6700F.The visible product of FESEM photo that provides from Fig. 2 is a hollow ball, and mean diameter can be seen damaged ball wall in the photo about 500nm, and hollow ball is piled up by nano particle and formed, and it is outer coarse that particle packing forms, and forms irregular cavernous structure.
Fig. 3 is the transmission electron microscope photo of product, proves that further product is a hollow structure.
Fig. 4 is the high resolution transmission electron microscopy photo of product, can clearly observe lattice fringe, and lattice fringe spacing 0.24nh and 0.51nm correspond respectively to (411) crystal face and (200) crystal face of cubic phase oxygen indium.
More than analyze and confirmed that the product that experiment obtains is well-crystallized's a cubic phase oxygen indium hollow ball.
Embodiment 2:
Preparation process is with instance 1, and difference is: take by weighing 1 mmole In (NO
3)
3Be dissolved in the 30mL ethanol, constant temperature stirs in 25 ℃ of water-baths, adds 2g P123 and 2mL methane amide, obtains settled solution after the dissolving, and transferring to volume then is in the polytetrafluoroethyllining lining stainless steel autoclave of 50mL.After the autoclave sealing, isothermal reaction 10h under 120 ℃ of conditions.
Embodiment 3:
Preparation process is with instance 1, and difference is: take by weighing 1 mmole In (NO
3)
3Be dissolved in the 30mL ethanol, constant temperature stirs in 25 ℃ of water-baths, adds 1g P123 and 2mL methane amide, obtains settled solution after the dissolving, and transferring to volume then is in the polytetrafluoroethyllining lining stainless steel autoclave of 50mL.After the autoclave sealing, isothermal reaction 4h under 150 ℃ of conditions.
Claims (1)
1. a low temperature prepares the method for Indium sesquioxide hollow ball, it is characterized in that 1 mmole In (N0
3)
3Be dissolved in the 30mL ethanol, add 1～5g triblock polymer P123 and 1～3mL methane amide, be sealed in after the mixing in the polytetrafluoroethyllining lining stainless steel autoclave, 120-150 ℃ was reacted 4 to 10 hours; Product through washing, ethanol washes, spinning and drying, promptly obtains the Indium sesquioxide hollow ball, described triblock polymer P123 is a polyoxyethylene-poly-oxypropylene polyoxyethylene, EO
20PO
70EO
20, M
w=5800.
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|---|---|---|---|
| CN2010105451625A CN102060320B (en) | 2010-11-16 | 2010-11-16 | Method for preparing indium oxide hollow sphere at low temperature |
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|---|---|---|---|
| CN2010105451625A CN102060320B (en) | 2010-11-16 | 2010-11-16 | Method for preparing indium oxide hollow sphere at low temperature |
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| CN102060320B true CN102060320B (en) | 2012-06-27 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659175A (en) * | 2012-04-28 | 2012-09-12 | 河南大学 | Process for preparing nanometer indium sesquioxide |
| CN105967223A (en) * | 2016-05-05 | 2016-09-28 | 扬州大学 | Tubular indium hydroxide/indium oxide micro-nano material synthesis method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008118422A1 (en) * | 2007-03-26 | 2008-10-02 | The Trustees Of Columbia University In The City Of New York | Metal oxide nanocrystals: preparation and uses |
| CN101539537A (en) * | 2009-05-06 | 2009-09-23 | 北京化工大学 | Erbium-doped indium oxide gas-sensitive nano material, preparation method and application thereof |
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2010
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008118422A1 (en) * | 2007-03-26 | 2008-10-02 | The Trustees Of Columbia University In The City Of New York | Metal oxide nanocrystals: preparation and uses |
| CN101539537A (en) * | 2009-05-06 | 2009-09-23 | 北京化工大学 | Erbium-doped indium oxide gas-sensitive nano material, preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 汪婧妍等.氧化铟空心球的合成及其气敏性能研究.《电子元件与材料》.2010,第29卷(第2期),11-13. * |
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Granted publication date: 20120627 Termination date: 20121116 |