CN110482593A - A kind of tufted In2O3Preparation method - Google Patents
A kind of tufted In2O3Preparation method Download PDFInfo
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- CN110482593A CN110482593A CN201910770449.9A CN201910770449A CN110482593A CN 110482593 A CN110482593 A CN 110482593A CN 201910770449 A CN201910770449 A CN 201910770449A CN 110482593 A CN110482593 A CN 110482593A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01G15/00—Compounds of gallium, indium or thallium
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of tufted In2O3Preparation method by indium nitrate aqueous solution and urea liquid in mixed at room temperature, obtains clear solution under magnetic stirring, and surfactant SDS powder, stirring to abundant dissolution are added into mixed solution.Then it transfers the solution into the stainless steel autoclave of polytetrafluoroethyllining lining, reaction kettle aging at room temperature, then, reaction kettle is heated up, solid product is collected by centrifugation, is first washed with water for several times, ethanol washing is used again, it is dry, obtain pre-product In (OH)3, obtained pre-product is calcined in Muffle furnace, obtains target product nanometer indium sesquioxide.It is good for purity is high, crystal property that the beneficial effects of the invention are as follows products, and preparation method is simple and efficient.
Description
Technical field
The invention belongs to field of material technology, are related to a kind of tufted In2O3Preparation method.
Background technique
As a kind of novel n-type semiconductor metal oxide, gas sensitive material indium sesquioxide (In2O3) conduction
Property and transmission of visible light are very high, and forbidden bandwidth is predominantly located between 3.55-3.75eV.Because of micro-nano In2O3Ratio table
Area and surface-active are larger, thus indium oxide gas sensitive light, electricity, in terms of highlight excellent property, can
It is widely used in the fields such as solar battery, gas sensor, photoelectric device, flat-panel monitor, diode.By grinding for many years
Study carefully, finds In2O3Gas sensor can be used for detecting the gases such as isopropanol, ethyl alcohol, nitrogen dioxide, hydrogen.
Summary of the invention
The purpose of the present invention is to provide a kind of tufted In2O3Preparation method, the beneficial effects of the invention are as follows product purities
Height, crystal property are good, and preparation method is simple and efficient.
The technical scheme adopted by the invention is that under magnetic stirring, indium nitrate aqueous solution and urea liquid are mixed in room temperature
It closes, solvent is ethylene glycol, obtains clear solution, and surfactant SDS powder is added into mixed solution, is stirred to sufficiently molten
Solution.Then it transfers the solution into the stainless steel autoclave of polytetrafluoroethyllining lining, reaction kettle aging at room temperature connects
, reaction kettle is heated up, solid product is collected by centrifugation, is first washed with water for several times, then with ethanol washing, it is dry, obtain pre-product
In(OH)3, obtained pre-product is calcined in Muffle furnace, obtains target product nanometer indium sesquioxide.
Further, under magnetic stirring, indium nitrate aqueous solution and urea liquid are clarified in mixed at room temperature 15min
Solution, surfactant SDS powder is added into mixed solution, then it is poly- to transfer the solution into 100mL to abundant dissolution for stirring
In the stainless steel autoclave of tetrafluoroethene liner, reaction kettle is then warming up to 120 to reaction kettle by aging 16h at room temperature
DEG C and keep 5h, solid product is collected by centrifugation, is first washed with water 2-4 times, then with ethanol washing 2-3 times, it is dry at 100 DEG C
For 24 hours, pre-product In (OH) is obtained3, obtained pre-product is calcined in 500 DEG C of Muffle furnaces under the rate of heat addition of 10 DEG C/min
3h obtains target product nanometer indium sesquioxide.
Detailed description of the invention
Fig. 1 is In2O3X-ray diffracting spectrum；
Fig. 2 is In2O3(S) transmission electron microscope picture；
Fig. 3 is In2O3(N) transmission electron microscope picture；
Fig. 4 is In2O3At different temperatures to the sensitivity histogram of 100ppm ethyl alcohol.
Specific embodiment
The present invention is described in detail With reference to embodiment.
Tufted In of the present invention2O3Preparation method is that under magnetic stirring, indium nitrate aqueous solution and urea liquid are mixed in room temperature
15min is closed, clear solution is obtained, surfactant SDS (lauryl sodium sulfate) powder is added into mixed solution, stirring is extremely
Sufficiently dissolution.Then it transfers the solution into the stainless steel autoclave of 100mL polytetrafluoroethyllining lining, reaction kettle is in room temperature
Lower aging 16h.Then, reaction kettle is warming up to 120 DEG C and keeps 5h.Solid product is collected by centrifugation, is first washed with water 2-4 times,
It uses ethanol washing 2-3 times again, drying for 24 hours, obtains pre-product In (OH) at 100 DEG C3.By obtained pre-product 10
DEG C/rate of heat addition of min under calcine 3h in 500 DEG C of Muffle furnaces, obtain target product nanometer indium sesquioxide, be denoted as In2O3。
XRD test
To understand In2O3The ingredient and powder interior atoms and molecular information of powder, spy is to In2O3Powder has carried out X-
Diffraction test, this characterization use the In calcined at 500 DEG C2O3Powder sample, under obtained result shown in Fig. 1.By scheming
1 it is found that be located at spreading out at 21.8,30.8,35.7,38.1,42.1,45.9,51.3,56.3,59.4,60.8,62.4 and 63.9o
It penetrates peak and corresponds respectively to In2O3(211), (222), (400), (411), (332), (431), (440), (611), (541),
(622), (631) and (444) crystal face.Wherein (222) diffraction maximum is relatively stronger and sharp, this illustrates that crystal is selected along [111] direction
Tachyauxesis.All diffraction maximums with cubic phase In2O3(JCPDSNo.06-0416) standard diagram is completely the same.And it does not examine
Other miscellaneous peaks are measured, this has obtained the In of purity is high2O3Cubic phase crystallographic system, product crystal property are good.Transmission electron microscope analysis
For the shape characteristic for understanding product, we are target product In resulting to calcining2O3Transmission electron microscope analysis has been carried out,
It takes micro-example in sample cell first, appropriate dehydrated alcohol is added dropwise, then ultrasonic disperse 30min or more drips a small amount of test solution
On the copper mesh of transmission electron microscope, using transmission electron microscope, adjust resolution ratio, observe the particle size of sample, pattern and
Dispersion.
(a) is using SDS as surfactant, the In prepared by solvent of ethylene glycol in Fig. 22O3The pattern of nano-powder is saturating
Mirror figure, after surfactant SDS is added, In2O3The pattern of crystal has changed a lot, and agglomeration obviously weakens, product
Lens pattern is in wheat head shape, and after amplification, (b) is it can be seen that the pattern that nano particle after surfactant is added occurs in Fig. 2
Cluster-shaped structure is presented in biggish variation, and tufted structure is made of smaller nanometer rods, and have large number of orifices between nanometer rods
Gap, is conducive to the absorption of gas, to improve the air-sensitive performance of nano material.Shown in Fig. 3, Fig. 3 (a) is to be not added with surface-active
Agent, the In prepared using ethylene glycol as solvent2O3(N) pattern of nano-powder, does not have between particle and particle as we can see from the figure
Apparent boundary is nearly all adhered together, reunites than more serious.After amplification, by Fig. 3 (b) it can be seen that powder layer structure
It is unobvious.
In2O3At different temperatures to the sensitivity of 100ppm ethyl alcohol, as a result as shown in figure 4, it can be found that in temperature range
In when being 140-300 DEG C2O3Nano material gradually rises the sensitivity of 100ppm ethyl alcohol, and at 300 DEG C, sensitivity reaches maximum
Value, and the In when temperature range is 300-370 DEG C2O3Nano material gradually weakens the sensitivity of 100ppm ethyl alcohol.It is obtained by figure
The In at 300 DEG C2O3Sensitivity highest of the nano material to 100ppm ethyl alcohol, Ra/RgValue is about 41, it can thus be appreciated that 300 DEG C are
In2O3Best sensitive operating temperature.
The present invention is prepared for by hydrothermal synthesis method using ethylene glycol as solvent to add the In of surfactant SDS2O3。
Product is characterized using X-ray diffraction (XRD), transmission electron microscope (TEM) and air-sensitive Performance Test System, the results showed that
Prepared In2O3Product is In with high purity, that crystal property is good2O3Cubic system.In2O3Lens pattern change greatly, be in
Existing wheat head shape, is regular cluster-shaped after amplification, after surfactant SDS is added, has obtained the product of specific morphology.In2O3's
Best sensitive operating temperature is 300 DEG C at 100ppm, and the sensitivity under optimum working temperature is 41, and in optimum working temperature
At 300 DEG C, the sensitivity of the alcohol gas of low concentration (5ppm) is remained to reach 5 or so.At 300 DEG C, In2O3To ethyl alcohol and different
The response of propyl alcohol is higher, this shows In2O3There is higher selectivity to ethyl alcohol and isopropanol, then shows In2O3Gas sensing
Device can be widely applied in the industrial production.There is tremendous influence to product morphology whether the addition of SDS, and then affects material
Air-sensitive performance.Indium oxide using SDS preparation is tufted rule particle, and air-sensitive performance is good.Without using SDS preparation particle without
Specific shape is reunited serious, and air-sensitive performance is bad.It is recorded as In2O3 (S) using indium oxide prepared by SDS, does not use SDS system
Standby indium oxide is recorded as In2O3 (N).
The above is only not to make limit in any form to the present invention to better embodiment of the invention
System, any simple modification that embodiment of above is made according to the technical essence of the invention, equivalent variations and modification,
Belong in the range of technical solution of the present invention.
Claims (2)
1. a kind of tufted In2O3Preparation method, it is characterised in that: under magnetic stirring, by indium nitrate aqueous solution and urea liquid in
Mixed at room temperature obtains clear solution, and surfactant SDS powder, stirring to abundant dissolution are added into mixed solution.Then will
Solution is transferred in the stainless steel autoclave of polytetrafluoroethyllining lining, reaction kettle aging at room temperature, then, by reaction kettle
Heating, solid product is collected by centrifugation, is first washed with water for several times, then use ethanol washing, dry, obtain pre-product In (OH)3, will
To pre-product calcined in Muffle furnace, obtain target product nanometer indium sesquioxide.
2. according to a kind of tufted In described in claim 12O3Preparation method, it is characterised in that: it is described under magnetic stirring, by nitre
Sour indium aqueous solution and urea liquid obtain clear solution, surfactant are added into mixed solution in mixed at room temperature 15min
Then SDS powder, stirring transfer the solution into the stainless steel autoclave of 100mL polytetrafluoroethyllining lining to abundant dissolution
In, reaction kettle is then warming up to 120 DEG C and keeps 5h, solid product is collected by centrifugation reaction kettle by aging 16h at room temperature, first
It is washed with water 2-4 times, then with ethanol washing 2-3 times, drying for 24 hours, obtains pre-product In (OH) at 100 DEG C3, pre- by what is obtained
Product calcines 3h in 500 DEG C of Muffle furnaces under the rate of heat addition of 10 DEG C/min, obtains target product nanometer indium sesquioxide.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030168A (en) * | 2012-12-26 | 2013-04-10 | 陕西科技大学 | Preparation method of spindle-shaped CeO2 microcrystal |
| CN105129841A (en) * | 2015-05-16 | 2015-12-09 | 青岛科技大学 | Preparation method of indium oxide with octahedral morphology |
| CN105731527A (en) * | 2016-01-29 | 2016-07-06 | 北京化工大学 | Coprecipitation preparation method of nanoscale indium tin oxide powder |
| CN107827148A (en) * | 2017-11-21 | 2018-03-23 | 临沂大学 | A kind of chiasma type indium oxide nanometer material preparation method |
| CN108862374A (en) * | 2018-08-10 | 2018-11-23 | 临沂大学 | A kind of method that microwave method quickly prepares two-part spindle nano zinc oxide material |
-
2019
- 2019-08-20 CN CN201910770449.9A patent/CN110482593A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030168A (en) * | 2012-12-26 | 2013-04-10 | 陕西科技大学 | Preparation method of spindle-shaped CeO2 microcrystal |
| CN105129841A (en) * | 2015-05-16 | 2015-12-09 | 青岛科技大学 | Preparation method of indium oxide with octahedral morphology |
| CN105731527A (en) * | 2016-01-29 | 2016-07-06 | 北京化工大学 | Coprecipitation preparation method of nanoscale indium tin oxide powder |
| CN107827148A (en) * | 2017-11-21 | 2018-03-23 | 临沂大学 | A kind of chiasma type indium oxide nanometer material preparation method |
| CN108862374A (en) * | 2018-08-10 | 2018-11-23 | 临沂大学 | A kind of method that microwave method quickly prepares two-part spindle nano zinc oxide material |
Non-Patent Citations (2)
| Title |
|---|
| ZHU,H，等: "Self-assembled 3D microflowery In(OH)(3) architecture and its conversion to In2O3", 《JOURNAL OF PHYSICAL CHEMISTRY C》 * |
| 杨红晓: "溶剂热法合成氧化铟、氧化铈纳米结构及其性能研究", 《中国优秀博硕士学位论文全文数据库（博士） 工程科技Ⅰ辑》 * |
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