CN105271371A - Flower-shaped indium oxide microrod material, and preparation method and application thereof - Google Patents
Flower-shaped indium oxide microrod material, and preparation method and application thereof Download PDFInfo
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- CN105271371A CN105271371A CN201510656520.2A CN201510656520A CN105271371A CN 105271371 A CN105271371 A CN 105271371A CN 201510656520 A CN201510656520 A CN 201510656520A CN 105271371 A CN105271371 A CN 105271371A
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Abstract
The invention relates to a preparation method and application of a flower-shaped indium oxide microrod material. The preparation method comprises: adding glucose and urea with a certain mass ratio into an indium salt aqueous solution, performing magnetic stirring at room temperature, transferring the colorless transparent solution into a hydrothermal reaction kettle, and reacting at a high temperature for hours, and performing centrifugation, washing, drying and calcining on the obtained product, so as to obtain the yellow target product flower-shaped indium oxide microrod material. The beneficial effects comprise that: 1) the related method is simple, friendly to environment and high in output; 2) by changing the usage amount of a reactant, the morphology of the material is controllable; 3) the prepared product possesses a stable mesoporous structure, is high in specific surface area, uniform in dimension and good in dispersity, and is in favor of gas molecule gas dispersion and surface reaction, and thus the product is improved in gas-sensitive performance; and 4) the material can overcome the defect that a conventional ethanol sensor is bad in selectivity when being applied to a gas sensitivity test.
Description
Technical field
The present invention relates to field of inorganic materials, be specifically related to a kind of preparation method and application of flower-shaped Indium sesquioxide micron bar material.
Background technology
Metal-oxide semiconductor (MOS) due to cheap, air-sensitive performance good, pollution-free, be easy to assembling, the advantage such as volume is little and be widely used in life and industrial gasses sensory field.Numerous metal oxide semiconductor is as SnO
2, TiO
2, ZnO, WO
3, In
2o
3the common concern of people is subject to Deng showing excellent properties in detection toxic and harmful.Wherein In
2o
3as a kind of important N-type semiconductor, possess wider energy gap, environmental friendliness, the advantages such as highly sensitive and response recovery time is short play an important role in gas sensor field.In recent years, for improving its gas sensing performance further, by regulation and control In
2o
3surface properties, size and pattern become study hotspot.Therefore, the In of various different-shape structure
2o
3, comprise nanofiber, nanometer rod, nanotube, nanocubes, nano-hollow ball etc. have been successfully synthesized and have applied.
Three-dimensional micro-nanometer structural material, owing to both having the advantage of one dimension and the large specific surface area of two-dimentional micro Nano material and many adsorption sites, also avoid the drawback that these nano materials easily reunite in application process simultaneously and is widely used in the numerous areas such as sensor, photochemical catalysis, lithium ion battery and becomes the study hotspot of recent years.Wherein in gas sensing field, because this three-dimensional micro-nano structure has large specific surface, special geometry and many adsorption sites of presenting, be conducive to the active adsorption area increasing gas molecule, thus realize the high air-sensitive property energy to certain gas.At present, hydrothermal synthesis method due to simple to operate, cost is low, pollution-free, the easily feature such as realization and be widely used in preparing various inorganic materials.Wherein, in the synthesis of the micro Nano material of numerous three-dimensional structure, some organic additives play an important role in the self-assembly of material structure unit as Growth In Space agent, thus have established solid basis for forming firm three-dimensional structure.In addition, we find, utilize the regulation and control that hydrothermal method passes through to regulate the addition of hydrothermal reaction condition or reactant can realize material morphology structure, this be the special material of high air-sensitive seeking optimum appearance structure provide effective means.
Summary of the invention
The object of this invention is to provide a kind of preparation method and application of flower-shaped Indium sesquioxide micron bar, involved preparation technology be simple, the morphology controllable of the large and material of output.The materials application prepared utilizing the method is in gas sensor, and do air-sensitive to ethanol and detect, find compared with the indium oxide particles of business, this material has a very large lifting to ethanol in sensitivity and selectivity.
To achieve these goals, the technical scheme that the present invention takes is as follows: a kind of flower-shaped Indium sesquioxide micron bar material, and it is by several length 0.5 ~ 2.2 μm, and diameter is the micron bar composition of 180 ~ 700nm.
By such scheme, it is 0.5 ~ 0.7 μm that described flower-shaped Indium sesquioxide micron bar material is preferably by several length, and diameter is the Indium sesquioxide micron bar composition of 180 ~ 210nm.
The preparation method of described flower-shaped Indium sesquioxide micron bar material, it is by adding the glucose of certain mass ratio and urea in the aqueous solution of indium salt, room temperature lower magnetic force stirs 0.5h ~ 1h, water white solution is transferred in hydrothermal reaction kettle, at high temperature after stoichiometric number hour, the product obtained through centrifugal, washing, dry, calcining, then can obtain the yellow flower-shaped Indium sesquioxide micron bar of target product.
By such scheme, described indium salt is indium chloride or indium nitrate, and the concentration of indium salts solution is 0.033 ~ 0.067mol/L.
By such scheme, the mass ratio of glucose and urea is (0.25 ~ 4): 1.By regulating the mass ratio of glucose and urea, the size of these flower-shaped Indium sesquioxide micron bars can effectively be regulated and controled.
By such scheme, hydrothermal temperature is 160 ~ 180 DEG C, reaction times 6 ~ 10h.
By such scheme, calcining temperature is in the air atmosphere of 450 DEG C ~ 550 DEG C, anneal 2 ~ 4h.
Described flower-shaped Indium sesquioxide micron bar material is as the application of gas sensing materials.Highly selective, highly sensitive and shorter response recovery time are shown to ethanol.Key step gas sensor being prepared by this materials application is: the coating slurries preparing 0.01g/mL using dehydrated alcohol as solvent are 200 ~ 400nm through being coated to the sensing layer thickness of the gas sensitive that golden interdigital electrode obtains.
Compared with prior art, the invention has the beneficial effects as follows:
1) adopt one step hydro thermal method, obtain a kind of flower-shaped Indium sesquioxide micron bar material.The method related to is simple, environmental friendliness, and output is high;
2) by changing the consumption of certain reactant, the pattern of this material can effectively be regulated and controled;
3) product that the present invention obtains has stable meso-hole structure, and specific surface area is high, size uniformity, favorable dispersity, is conducive to surface diffusion and the surface reaction of gas molecule, thus improves its air-sensitive performance.
4) this materials application is tested in air-sensitive, the shortcoming of traditional ethanol sensor poor selectivity can be overcome.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph adding the glucose of different mass ratio and the flower-shaped Indium sesquioxide micron bar of urea in embodiment 1;
Fig. 2 is the X-ray diffractogram of the flower-shaped Indium sesquioxide micron bar of best glucose and urea ratio (1:1) in embodiment 1;
Fig. 3 is that the flower-shaped Indium sesquioxide micron bar gas sensitive of optimum proportion in embodiment 1 is to the temperature-sensitivity of ethanol and concentration sensitivity figure;
Fig. 4 is that the flower-shaped Indium sesquioxide micron bar gas sensitive of optimum proportion in embodiment 1 is to the selectivity diagram of ethanol.
Embodiment
Below in conjunction with embodiment, the present invention will be further described in detail, but this explanation can not be construed as limiting the invention.
Embodiment 1
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, the amount of this mass ratio (1:1) is 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 yellow powder product.
Embodiment 2-5
Similarly, the glucose and the urea that take different mass ratio (4:0,4:1,2:1,1:2,0:4) join InCl
3in the aqueous solution, after similarity condition hydro-thermal reaction, then obtain the In of a series of different-shape and size
2o
3product, step is with embodiment 1.
Table one
| M (glucose): M (urea) | 4:1 | 2:1 | 1:1 | 1:2 |
| Mean length (μm) | 2.05 | 1.11 | 0.67 | 0.86 |
| Mean diameter (nm) | 656 | 354 | 200 | 514 |
As shown in Fig. 1 (a), when only adding glucose reagent, the Indium sesquioxide product obtained is unbodied multi-pore micron spherical structure, when only adding urea reagent, what obtain is unbodied micron cube structure, but when both have both at the same time, by the mass ratio of both changes, the flower-shaped Indium sesquioxide micron bar (see table one) of a series of different size can be obtained.Select the flower-shaped Indium sesquioxide sample of this minimum size as air-sensitive test material.Pass through Fig. 2, the very sharp-pointed Correlative characteristic peaks such as (211), (222), (400), (440), (622) can be seen, without other any impurity peaks, show that the Indium sesquioxide sample of this size has good degree of crystallinity.Preparing the coating slurries of 0.01g/mL using dehydrated alcohol as solvent, is 200 ~ 400nm through being coated to the sensing layer thickness of the gas sensitive that golden interdigital electrode obtains.After drying in the shade, the gas sensor of preparation is placed in heat aging 24h on agingtable, finally carries out air-sensitive test.Can be clear that from Fig. 3 and Fig. 4, compared with the indium oxide particles (being of a size of 50 ~ 100nm) of business, optimal working temp decrease and also under different concentration ethanol gas sensitivity all high than commercial material.The more important thing is, in the selectivity test of gas, for the gas of different types of 100ppm, the prepared sensitivity of flower-shaped Indium sesquioxide micron bar material to alcohol gas is higher than the material of commercialization, indicate the selectivity of this material to ethanol excellence, this solves the defect of general ethanol sensor poor selectivity well.
Claims (8)
1. a flower-shaped Indium sesquioxide micron bar material, it is 0.5 ~ 2.2 μm by several length, and diameter is the Indium sesquioxide micron bar composition of 180 ~ 700nm.
2. flower-shaped Indium sesquioxide micron bar material according to claim 1, is characterized in that, described flower-shaped Indium sesquioxide micron bar material is 0.5 ~ 0.7 μm by several length, and diameter is the Indium sesquioxide micron bar composition of 180 ~ 210nm.
3. the preparation method of flower-shaped Indium sesquioxide micron bar material according to claim 1, it is by adding the glucose of certain mass ratio and urea in the aqueous solution of indium salt, room temperature lower magnetic force stirs 0.5h ~ 1h, water white solution is transferred in hydrothermal reaction kettle, at high temperature after stoichiometric number hour, the product obtained through centrifugal, washing, dry, calcining, then can obtain the yellow flower-shaped Indium sesquioxide micron bar of target product.
4. the preparation method of flower-shaped Indium sesquioxide micron bar material according to claim 3, is characterized in that described indium salt is indium chloride or indium nitrate, and the concentration of indium salts solution is 0.033 ~ 0.067mol/L.
5. the preparation method of flower-shaped Indium sesquioxide micron bar material according to claim 3, is characterized in that the mass ratio of glucose and urea is for (0.25 ~ 4): 1.
6. the preparation method of flower-shaped Indium sesquioxide micron bar material according to claim 3, is characterized in that hydrothermal temperature is 160 ~ 180 DEG C, reaction times 6 ~ 10h.
7. the preparation method of flower-shaped Indium sesquioxide micron bar material according to claim 3, is characterized in that calcining temperature is in the air atmosphere of 450 DEG C ~ 550 DEG C, anneal 2 ~ 4h.
8. the flower-shaped Indium sesquioxide micron bar material described in claim 1 or 2 is as the application of gas sensing materials.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105540643A (en) * | 2016-02-22 | 2016-05-04 | 武汉工程大学 | Multipod-like indium oxide compound sensitive material and preparation and application thereof |
| CN106115771A (en) * | 2016-06-14 | 2016-11-16 | 南京大学 | A kind of In2o3the preparation method that polyhedron micron is brilliant |
| CN109781800A (en) * | 2019-01-25 | 2019-05-21 | 青岛大学 | A kind of gas sensor and preparation method thereof based on metal molybdate nanocomposite |
| 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 |
| CN110357606A (en) * | 2019-08-01 | 2019-10-22 | 东北大学 | A kind of In based on zeolite substrate2O3Nano material preparation and its application |
| CN112520783A (en) * | 2020-12-18 | 2021-03-19 | 西北师范大学 | Synthesis of cubic crystal indium oxide and application thereof in electrocatalytic nitrogen reduction |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105540643A (en) * | 2016-02-22 | 2016-05-04 | 武汉工程大学 | Multipod-like indium oxide compound sensitive material and preparation and application thereof |
| CN106115771A (en) * | 2016-06-14 | 2016-11-16 | 南京大学 | A kind of In2o3the preparation method that polyhedron micron is brilliant |
| CN109781800A (en) * | 2019-01-25 | 2019-05-21 | 青岛大学 | A kind of gas sensor and preparation method thereof based on metal molybdate nanocomposite |
| CN109781800B (en) * | 2019-01-25 | 2021-06-04 | 青岛大学 | Gas sensor based on metal molybdate nano composite material and preparation method thereof |
| 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 |
| CN110357606A (en) * | 2019-08-01 | 2019-10-22 | 东北大学 | A kind of In based on zeolite substrate2O3Nano material preparation and its application |
| CN112520783A (en) * | 2020-12-18 | 2021-03-19 | 西北师范大学 | Synthesis of cubic crystal indium oxide and application thereof in electrocatalytic nitrogen reduction |
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