CN105540643A - Multipod-like indium oxide compound sensitive material and preparation and application thereof - Google Patents
Multipod-like indium oxide compound sensitive material and preparation and application thereof Download PDFInfo
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- CN105540643A CN105540643A CN201610095899.9A CN201610095899A CN105540643A CN 105540643 A CN105540643 A CN 105540643A CN 201610095899 A CN201610095899 A CN 201610095899A CN 105540643 A CN105540643 A CN 105540643A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a multipod-like indium oxide compound sensitive material and preparation and application thereof. The indium oxide compound sensitive material is composed of 4-12 copper doped indium oxide micron rods with the length being 100-2000 nm and the diameter being 100-800 nm. The preparation method includes the following steps that glucose, urea and copper salt are added to an indium salt water solution to be stirred and mixed, and a clear and transparent solution is obtained; a reaction is conducted for 6-10 hours at the temperature of 160-180 DEG C, an obtained product is subjected to centrifugation, washing, drying and baking, and a final target product is obtained. In the obtained product, copper enters lattices of indium oxide, the catalytic effect of indium oxide can be played, dissociation of oxygen ions adsorbed to the surface of multipod-like indium oxide is activated, the oxygen molecular weight in filling holes in the surface of the indium oxide and the filling rate are raised, the transfer speed of electrons on the surface of the indium oxide is greatly increased, and chemical and electronic properties of the indium oxide are improved.
Description
Technical field
The invention belongs to inorganic composite materials field, be specifically related to a kind of multiway shape Indium sesquioxide composite sensitive material and Synthesis and applications thereof.
Background technology
Metal oxide semiconductor material is because at detection poisonous and harmful, flammable explosive gas possesses response fast in recent years, sensitivity high and become the study hotspot in sensitive material field.Now, on market, most of gas sensor has achieved and has detected the air-sensitive of certain pure gas under certain condition, and achieves good economic benefit.But same gas sensitive can be issued in different operational temperature conditions and then seldom occur the product of two kinds of gas detection objects, and an excellent sensor depends primarily on the synthesis of its sensitive material and the physics preparation of gas sensitive device.
Indium sesquioxide (In
2o
3) be a kind of N-type semiconductor material of important broad stopband, possess high energy band, pollution-free, response sensitivity is high, response recovers the feature such as fast and be widely used in gas sensing field.In recent years, major part research mainly by regulate and control the surface properties of Indium sesquioxide, scale topography and doping other metal oxygenate or precious metal improve the air-sensitive performance of material further.
Three-dimensional micro nano structure owing to possessing large specific surface area, many adsorption sites, and be different from the features such as the simple geometry of a peacekeeping two-dimensional material and become the study hotspot in gas sensitive synthesis.Mix a small amount of on the basis of three-dimensional structure, cheap and the metal oxide catalyst that catalytic activity is high or noble metal catalyst can improve the performance of material to a certain extent further simultaneously.At present, about the research preparing this respect material is progressively carried out, this gas sensor tool for development of new measuring ability is of great significance.
Summary of the invention
The object of the invention is to provide a kind of Indium sesquioxide composite sensitive material with new shape characteristic and its preparation method and application, its preparation technology is simple, output is large, can effectively improve nitrogen peroxide sensitivity and selectivity at low temperatures, at high temperature higher sensitivity is shown to ethanol simultaneously, good selectivity, realizes same gas sensitive at low temperatures and high temperatures respectively to the double check of nitrogen peroxide and ethanol.
For achieving the above object, adopt technical scheme as follows:
A kind of multiway shape Indium sesquioxide composite sensitive material is 100 ~ 2000nm by 4-12 length, and diameter is the Copper-cladding Aluminum Bar Indium sesquioxide micron bar composition of 100 ~ 800nm.
The preparation method of above-mentioned multiway shape Indium sesquioxide composite sensitive material, comprises the following steps:
Glucose and urea and mantoquita are added the solution being uniformly mixed in indium salt brine solution and obtaining clear;
Obtain product at 160 ~ 180 DEG C of reaction 6 ~ 10h and obtain final target product through centrifugal, washing, drying, roasting.
By such scheme, described indium salt is indium chloride or indium nitrate.
By such scheme, described indium salt brine solution concentration is 0.033 ~ 0.067mol/L.
By such scheme, the mass ratio of glucose and urea is (0.25 ~ 4): 1.
By such scheme, mantoquita is cupric chloride or cupric nitrate, and the mol ratio of mantoquita and indium salt is (0.02-0.07): 1.
By such scheme, described roasting temperature in air atmosphere is 450-550 DEG C, and the time is 2-4h.
Above-mentioned multiway shape Indium sesquioxide composite sensitive material is applied to the detection to volatile organic matter gas.
Above-mentioned multiway shape Indium sesquioxide composite sensitive material is applied to the detection to nitrogen peroxide and alcohol gas.
Compared with prior art, beneficial effect of the present invention is:
The present invention result in the formation of this three-dimensional multiway shape structure due to the synergy of glucose and urea, this structure is because have the one dimension that is different from simple geometric structures and the large specific surface area of two-dimentional micro Nano material and many adsorption sites advantage, so have good sensitive property to gas.
Preparation method's copper of the present invention enters the intracell of Indium sesquioxide, the catalytic effect of cupric oxide can be played, activate dissociating of the Indium sesquioxide surface adsorption oxonium ion of multiway shape, increase oxygen molecule amount and the fill rate of Indium sesquioxide surface filling hole, greatly accelerate the transport velocity of electronics on Indium sesquioxide surface, promote chemistry and the Electronic Performance of Indium sesquioxide.
The Indium sesquioxide micron bar material of multiway shape can be improved further at low temperatures to the air-sensitive performance of nitrogen peroxide by copper doped.
This material not only has good air-sensitive performance to nitrogen peroxide at low temperatures, simultaneously at high temperature shows higher sensitivity and good selectivity to ethanol, achieves gas sensitive of the same race at different temperature respectively to the detection of nitrogen peroxide and ethanol.
Accompanying drawing explanation
Fig. 1: the SEM figure of the Indium sesquioxide micron bar of the multiway shape of Copper-cladding Aluminum Bar prepared by embodiment 1;
Fig. 2: the XRD figure of the Indium sesquioxide micron bar of the multiway shape of Copper-cladding Aluminum Bar prepared by embodiment 1;
Fig. 3: the EDX figure of the Indium sesquioxide micron bar of the multiway shape of Copper-cladding Aluminum Bar prepared by embodiment 1;
Fig. 4: the Indium sesquioxide micron bar of the multiway shape of Copper-cladding Aluminum Bar prepared by embodiment 1 and comparative example is at different temperatures to the air-sensitive response diagram of 50ppm nitrogen peroxide;
Fig. 5: the Indium sesquioxide micron bar of the multiway shape of Copper-cladding Aluminum Bar prepared by embodiment 1 is at different temperatures to the air-sensitive response diagram of 100ppm ethanol;
Fig. 6: the Indium sesquioxide micron bar of multiway shape prepared by the Indium sesquioxide micron bar of the multiway shape of Copper-cladding Aluminum Bar prepared by embodiment 1 and comparative example and comparative example is the air-sensitive response diagram of 20ppb ~ 100ppm nitrogen peroxide to concentration range under optimum temps;
Fig. 7: the Indium sesquioxide micron bar of multiway shape of Copper-cladding Aluminum Bar prepared by embodiment 1 under the optimum temps to nitrogen peroxide and ethanol to the air-sensitive response diagram of gas with various;
Embodiment
Following examples explain technical scheme of the present invention further, but not as limiting the scope of the invention.
Embodiment 1
A kind of Copper-cladding Aluminum Bar multiway shape In
2o
3micron bar, mantoquita and InCl
3mol ratio be 0.02:1, concrete steps are as follows:
Get the InCl of 2mmol
3in 30ml deionized water, after stirring 5min, obtain the solution of clear.Take glucose and the 3.5g urea of 3.5g, by glucose, urea and quantitative CuCl
2join in clear solution, and under magnetic stirring apparatus, stir 1h and ultrasonic disperse 30min, obtain water white transparency mixing solutions.This mixing solutions is transferred in the hydrothermal reaction kettle of 50ml, at 180 DEG C, obtains brownish black precipitated liquid after hydro-thermal reaction 8h.By for several times washing, centrifugal after obtain brownish black throw out, by this throw out dry 10h in the thermostatic drying chamber of 60 DEG C, finally in the air atmosphere of 500 DEG C, calcine 2h, obtain target product.
The product that the present embodiment obtains is through electron-microscope scanning, and as shown in Figure 1, to result this multiway shape Indium sesquioxide material be 100 ~ 1000nm by several length, and diameter is the micron bar composition of 100 ~ 700nm.Pass through Fig. 2, it is seen that the crystal formation of typical cube Indium sesquioxide, without any impurity peaks, illustrate that copper is by the intracell mixed into Indium sesquioxide, in order to confirm this point further, the ultimate analysis (EDX) of Fig. 3 can see the existence having copper clearly, and being mixed with really in Indium sesquioxide lattice of copper is described.
Comparative example
A kind of multiway shape In
2o
3the preparation method of micron bar, concrete steps are as follows:
Get the InCl of 2mmol
3in 30ml deionized water, after stirring 5min, obtain the solution of clear.Take glucose and the 3.5g urea of 3.5g, glucose, urea are joined in clear solution, and under magnetic stirring apparatus, stir 1h and ultrasonic disperse 30min, obtain water white transparency mixing solutions.This mixing solutions is transferred in the hydrothermal reaction kettle of 50ml, at 180 DEG C, obtains brownish black precipitated liquid after hydro-thermal reaction 8h.By for several times washing, centrifugal after obtain brownish black throw out, by this throw out dry 10h in the thermostatic drying chamber of 60 DEG C, finally in the air atmosphere of 500 DEG C, calcine 2h, obtain target product.
Example 1 and comparative example gained multiway shape In respectively
2o
3micron bar material is as sensitive material, and taking dehydrated alcohol as the coating slurries of solvent preparation 0.01g/mL, is 200nm ~ 400nm through being coated to the sensing layer thickness golden interdigital electrode obtaining gas sensitive.After drying in the shade, the gas sensor of preparation is placed in heat aging 24h on agingtable, finally carries out air-sensitive test.Result sees Fig. 4, Fig. 5, Fig. 6, Fig. 7 respectively.
Fig. 4 is Copper-cladding Aluminum Bar multiway shape In prepared by embodiment 1
2o
3the multiway shape In of micron bar material and comparative example
2o
3micron bar material is at different temperatures to the air-sensitive response diagram of 50ppm nitrogen peroxide, and optimal working temp is respectively 150 DEG C and 200 DEG C.Fig. 5 is Copper-cladding Aluminum Bar multiway shape In prepared by embodiment 1
2o
3micron bar material is at different temperatures to the air-sensitive response diagram of 100ppm ethanol, and optimal working temp is 300 DEG C.
Fig. 6 is that the bi-material of embodiment 1 and comparative example is at the air-sensitive response diagram to a series of different concns nitrogen peroxide, obviously, the Indium sesquioxide micron bar of copper doped is better to nitrogen peroxide gas sensing property than pure material, and the former can reach the detectability to nitrogen peroxide 20ppb concentration, be much better than the detectability of pure multiway shape Indium sesquioxide 500ppb, this is mainly owing to the catalytic activity that cupric oxide is good to nitrogen peroxide.
Fig. 7 is Copper-cladding Aluminum Bar multiway shape In prepared by embodiment 1
2o
3micron bar material, respectively under the optimum temps of nitrogen peroxide (300 DEG C) and ethanol (150 DEG C), is the air-sensitive response diagram of the carbon monoxide of 100ppm, hydrogen, ethanol, acetone, formaldehyde, methyl alcohol, toluene, nitrogen peroxide to concentration.Result illustrates under low temperature (150 DEG C), splendid selectivity is shown to nitrogen peroxide, under high temperature (300 DEG C), show good selectivity to ethanol, the double check function of this material has great significance for the research and development of novel gas sensitive.
Embodiment 2
A kind of Copper-cladding Aluminum Bar multiway shape In
2o
3the preparation method of micron bar, mantoquita and InCl
3mol ratio be 0.04:1, concrete steps are as follows:
Get the InCl of 2mmol
3in 30ml deionized water, after stirring 5min, obtain the solution of clear.Take glucose and the 3.5g urea of 3.5g, by the amount of this mass ratio (1:1) and quantitative CuCl
2join in clear solution, and under magnetic stirring apparatus, stir 1h and ultrasonic disperse 30min, obtain water white transparency mixing solutions.This mixing solutions is transferred in the hydrothermal reaction kettle of 50ml, at 180 DEG C, obtains brownish black precipitated liquid after hydro-thermal reaction 8h.By for several times washing, centrifugal after obtain brownish black throw out, by this throw out dry 10h in the thermostatic drying chamber of 60 DEG C, finally in the air atmosphere of 500 DEG C, calcine 2h, obtain target product.
Get appropriate Copper-cladding Aluminum Bar multiway shape Indium sesquioxide, using flower-shaped for the Copper-cladding Aluminum Bar obtained by the present embodiment Indium sesquioxide as sensitive material, taking dehydrated alcohol as the coating slurries of solvent preparation 0.01g/mL, is 200nm ~ 400nm through being coated to the sensing layer thickness golden interdigital electrode obtaining gas sensitive.After drying in the shade, the gas sensor of preparation is placed in heat aging 24h on agingtable, finally carries out air-sensitive test.Under the optimal reaction temperature of 150 DEG C, 100ppb is limited to nitrogen peroxide lowest detection.
Embodiment 3
A kind of Copper-cladding Aluminum Bar multiway shape In
2o
3micron bar, mantoquita and InCl
3mol ratio be 0.07:1, concrete steps are as follows:
Get the InCl of 2mmol
3in 30ml deionized water, after stirring 5min, obtain the solution of clear.Take glucose and the 3.5g urea of 3.5g, by glucose, urea and quantitative CuCl
2join in clear solution, and under magnetic stirring apparatus, stir 1h and ultrasonic disperse 30min, obtain water white transparency mixing solutions.This mixing solutions is transferred in the hydrothermal reaction kettle of 50ml, react 8h at 180 DEG C after, obtains brownish black precipitated liquid.By for several times washing, centrifugal after obtain brownish black throw out, by this throw out dry 10h in the thermostatic drying chamber of 60 DEG C, finally in the air atmosphere of 450 DEG C, calcine 4h, obtain target product.
Get appropriate Copper-cladding Aluminum Bar multiway shape Indium sesquioxide, using flower-shaped for the Copper-cladding Aluminum Bar obtained by the present embodiment Indium sesquioxide as sensitive material, taking dehydrated alcohol as the coating slurries of solvent preparation 0.01g/mL, is 200nm ~ 400nm through being coated to the sensing layer thickness golden interdigital electrode obtaining gas sensitive.After drying in the shade, the gas sensor of preparation is placed in heat aging 24h on agingtable, finally carries out air-sensitive test.Under the optimal reaction temperature of 150 DEG C, 400ppb is limited to nitrogen peroxide lowest detection.
Embodiment 4
A kind of Copper-cladding Aluminum Bar multiway shape In
2o
3micron bar, mantoquita and InCl
3mol ratio be 0.06:1, concrete steps are as follows:
Get the InCl of 2mmol
3in 30ml deionized water, after stirring 5min, obtain the solution of clear.Take glucose and the 3.5g urea of 3.5g, by glucose, urea and quantitative CuCl
2join in clear solution, and under magnetic stirring apparatus, stir 1h and ultrasonic disperse 30min, obtain water white transparency mixing solutions.This mixing solutions is transferred in the hydrothermal reaction kettle of 50ml, react 10h at 160 DEG C after, obtains brownish black precipitated liquid.By for several times washing, centrifugal after obtain brownish black throw out, by this throw out dry 10h in the thermostatic drying chamber of 60 DEG C, finally in the air atmosphere of 550 DEG C, calcine 2h, obtain target product.
Get appropriate Copper-cladding Aluminum Bar multiway shape Indium sesquioxide, using flower-shaped for the Copper-cladding Aluminum Bar obtained by the present embodiment Indium sesquioxide as sensitive material, taking dehydrated alcohol as the coating slurries of solvent preparation 0.01g/mL, is 200nm ~ 400nm through being coated to the sensing layer thickness golden interdigital electrode obtaining gas sensitive.After drying in the shade, the gas sensor of preparation is placed in heat aging 24h on agingtable, finally carries out air-sensitive test.Under the optimal reaction temperature of 150 DEG C, 200ppb is limited to nitrogen peroxide lowest detection.
Embodiment 5
A kind of Copper-cladding Aluminum Bar multiway shape In
2o
3micron bar, mantoquita and InCl
3mol ratio be 0.05:1, concrete steps are as follows:
Get the InCl of 2mmol
3in 30ml deionized water, after stirring 5min, obtain the solution of clear.Take glucose and the 3.5g urea of 3.5g, by glucose, urea and quantitative CuCl
2join in clear solution, and under magnetic stirring apparatus, stir 1h and ultrasonic disperse 30min, obtain water white transparency mixing solutions.This mixing solutions is transferred in the hydrothermal reaction kettle of 50ml, react 6h at 180 DEG C after, obtains brownish black precipitated liquid.By for several times washing, centrifugal after obtain brownish black throw out, by this throw out dry 10h in the thermostatic drying chamber of 60 DEG C, finally in the air atmosphere of 500 DEG C, calcine 3h, obtain target product.
Get appropriate Copper-cladding Aluminum Bar multiway shape Indium sesquioxide, using flower-shaped for the Copper-cladding Aluminum Bar obtained by the present embodiment Indium sesquioxide as sensitive material, taking dehydrated alcohol as the coating slurries of solvent preparation 0.01g/mL, is 200nm ~ 400nm through being coated to the sensing layer thickness golden interdigital electrode obtaining gas sensitive.After drying in the shade, the gas sensor of preparation is placed in heat aging 24h on agingtable, finally carries out air-sensitive test.Under the optimal reaction temperature of 150 DEG C, 150ppb is limited to nitrogen peroxide lowest detection.
Claims (9)
1. a multiway shape Indium sesquioxide composite sensitive material, is characterized in that by 4-12 length be 100 ~ 2000nm, and diameter is the Copper-cladding Aluminum Bar Indium sesquioxide micron bar composition of 100 ~ 800nm.
2. the preparation method of multiway shape Indium sesquioxide composite sensitive material according to claim 1, is characterized in that comprising the following steps:
Glucose and urea and mantoquita are added the solution being uniformly mixed in indium salt brine solution and obtaining clear;
Obtain product at 160 ~ 180 DEG C of reaction 6 ~ 10h and obtain final target product through centrifugal, washing, drying, roasting.
3. the preparation method of multiway shape Indium sesquioxide composite sensitive material as claimed in claim 1, is characterized in that described indium salt is indium chloride or indium nitrate.
4. the preparation method of multiway shape Indium sesquioxide composite sensitive material as claimed in claim 1, is characterized in that described indium salt brine solution concentration is 0.033 ~ 0.067mol/L.
5. the preparation method of multiway shape Indium sesquioxide composite sensitive material as claimed in claim 1, is characterized in that the mass ratio of glucose and urea is for (0.25 ~ 4): 1.
6. the preparation method of multiway shape Indium sesquioxide composite sensitive material as claimed in claim 1, it is characterized in that mantoquita is cupric chloride or cupric nitrate, the mol ratio of mantoquita and indium salt is (0.02-0.07): 1.
7. the preparation method of multiway shape Indium sesquioxide composite sensitive material as claimed in claim 1, it is characterized in that described roasting temperature in air atmosphere is 450-550 DEG C, the time is 2-4h.
8. multiway shape Indium sesquioxide composite sensitive material according to claim 1 is applied to the detection to volatile organic matter gas.
9. multiway shape Indium sesquioxide composite sensitive material according to claim 1 is applied to the detection to nitrogen peroxide and alcohol gas.
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| CN110261444A (en) * | 2019-06-24 | 2019-09-20 | 天津师范大学 | A kind of preparation method of the gas sensitive material for acetone gas sensor |
| CN113968589A (en) * | 2021-10-14 | 2022-01-25 | 沈阳化工大学 | Flower-like structure CuO-In2O3Preparation method and application of composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110261444A (en) * | 2019-06-24 | 2019-09-20 | 天津师范大学 | A kind of preparation method of the gas sensitive material for acetone gas sensor |
| CN113968589A (en) * | 2021-10-14 | 2022-01-25 | 沈阳化工大学 | Flower-like structure CuO-In2O3Preparation method and application of composite material |
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