CN105271371B - A kind of flower-shaped indium oxide micron bar material and its preparation method and application - Google Patents
A kind of flower-shaped indium oxide micron bar material and its preparation method and application Download PDFInfo
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- CN105271371B CN105271371B CN201510656520.2A CN201510656520A CN105271371B CN 105271371 B CN105271371 B CN 105271371B CN 201510656520 A CN201510656520 A CN 201510656520A CN 105271371 B CN105271371 B CN 105271371B
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Abstract
The present invention relates to the preparation method and application of flower-shaped indium oxide micron bar material, its by add certain mass than glucose and urea in the aqueous solution of indium salts, magnetic agitation at room temperature, the solution of water white transparency is transferred in hydrothermal reaction kettle, at high temperature after reaction a few hours, obtained product then can obtain the flower-shaped indium oxide micron bar of target product of yellow by centrifugation, washing, dry, calcining.The beneficial effects of the invention are as follows：1) method being related to is simple, environment-friendly, and yield is high；2) by changing the consumption of certain reactant, the pattern of the material can obtain effective regulation and control；3) product produced by the present invention has stable meso-hole structure, and specific surface area is high, size uniformity, favorable dispersibility, is conducive to the diffusion into the surface and surface reaction of gas molecule, so as to improve its air-sensitive performance；4) materials application is tested in air-sensitive, the shortcoming of traditional ethanol sensor poor selectivity can be overcome.
Description
Technical field
The present invention relates to field of inorganic materials, and in particular to the preparation method of a kind of flower-shaped indium oxide micron bar material and should
With.
Background technology
Metal-oxide semiconductor (MOS) because cheap, air-sensitive performance is good, pollution-free, be easily assembled to, small volume the advantages of
And it is widely used in life and industrial gasses sensory field.Numerous metal oxide semiconductors such as SnO2、TiO2、ZnO、
WO3、In2O3Deng detect toxic and harmful gas in terms of show excellent properties and by the common concern of people.Wherein In2O3Make
For a kind of important N-type semiconductor, possess wider energy gap, it is environment-friendly, sensitivity height and response recovery time are short etc.
Advantage plays an important role in gas sensor field.In recent years, it is further to improve its gas sensing performance, by adjusting
Control In2O3Surface nature, size and pattern turn into study hotspot.Therefore, the In of various different-shape structures2O3, including receive
Rice fiber, nanometer rods, nanotube, nanocube, nano-hollow ball etc. have been successfully synthesized and applied.
Three-dimensional micro-nanometer structural material is due to both having the big specific surface area of one-dimensional and two-dimentional micro Nano material and many
The advantage of adsorption site, is widely used in while also avoid the drawbacks of these nano materials are easily reunited in application process
The numerous areas such as sensor, photocatalysis, lithium ion battery and as recent years study hotspot.Wherein in gas sensing field
In, because this three-dimensional micro-nano structure has big ratio surface, special geometry and many adsorption potentials for showing
Point, is conducive to increasing effective adsorption area of gas molecule, so as to realize the high air-sensitive property energy to certain gas.At present, hydro-thermal is closed
It is pollution-free into method because simple to operate, cost is low, the features such as easily realizing and be widely used in preparing various inorganic material.
Wherein, in the synthesis of the micro Nano material of numerous three-dimensional structures, some organic additives are as Growth In Space agent in material knot
Played an important role in the self assembly of structure unit, so as to establish solid foundation to form firm three-dimensional structure.In addition,
It was found that can be realized to material morphology structure using hydro-thermal method by adjusting the addition of hydrothermal reaction condition or reactant
Regulation and control, this is that the high air-sensitive special material for seeking optimal appearance structure provides effective means.
The content of the invention
It is an object of the invention to provide a kind of preparation method and application of flower-shaped indium oxide micron bar, involved preparation work
Skill is simple, yield is big and material morphology controllable.By the materials application prepared using this method in gas sensor, ethanol is done
Air-sensitive detection, finds compared with the indium oxide particles of business, and the material has one very big to ethanol in sensitivity and selectivity
Lifting.
To achieve these goals, the technical scheme that the present invention takes is as follows：A kind of flower-shaped indium oxide micron bar material, its
It is that, by several 0.5~2.2 μm of length, a diameter of 180~700nm micron bar is constituted.
By such scheme, described flower-shaped indium oxide micron bar material is preferably by several length to be 0.5~0.7 μm, directly
Footpath constitutes for 180~210nm indium oxide micron bar.
The preparation method of described flower-shaped indium oxide micron bar material, its by add certain mass than glucose and urine
Element is in the aqueous solution of indium salts, and magnetic agitation 0.5h~1h, the solution of water white transparency is transferred in hydrothermal reaction kettle at room temperature,
At high temperature after reaction a few hours, obtained product then can obtain the target product of yellow by centrifugation, washing, dry, calcining
Flower-shaped indium oxide micron bar.
By such scheme, described indium salts are inidum chloride or indium nitrate, the concentration of indium salts solution for 0.033~
0.067mol/L。
By such scheme, the mass ratio of glucose and urea is (0.25~4):1.By the matter for adjusting glucose and urea
Amount ratio, the size of these flower-shaped indium oxide micron bars can effectively be regulated and controled.
By such scheme, hydrothermal temperature is 160~180 DEG C, 6~10h of reaction time.
By such scheme, calcining heat is in 450 DEG C~550 DEG C of air atmosphere, makes annealing treatment 2~4h.
Described flower-shaped indium oxide micron bar material as gas sensing materials application.High selection is shown to ethanol
Property, high sensitivity and shorter response recovery time.The materials application is prepared into mainly comprising the following steps for gas sensor：With anhydrous second
Alcohol prepares 0.01g/mL coating slurries, the coated sensing thickness to the gas sensitive obtained in golden interdigital electrode as solvent
Spend for 200~400nm.
Compared with prior art, the beneficial effects of the invention are as follows：
1) one step hydro thermal method is used, a kind of flower-shaped indium oxide micron bar material has been obtained.The method being related to is simple, environment friend
Good, yield is high；
2) by changing the consumption of certain reactant, the pattern of the material can obtain effective regulation and control；
3) product produced by the present invention has stable meso-hole structure, and specific surface area is high, size uniformity, favorable dispersibility,
Be conducive to the diffusion into the surface and surface reaction of gas molecule, so as to improve its air-sensitive performance.
4) materials application is tested in air-sensitive, the shortcoming of traditional ethanol sensor poor selectivity can be overcome.
Brief description of the drawings
Fig. 1 is the scanning of the flower-shaped indium oxide micron bar of the glucose of addition different quality ratio and urea in embodiment 1
Electron microscope；
Fig. 2 is optimal glucose and urea ratio (1 in embodiment 1:1) X-ray diffraction of flower-shaped indium oxide micron bar
Figure；
Fig. 3 be the flower-shaped indium oxide micron rod air-sensitive material of optimal proportion in embodiment 1 to temperature-sensitivity of ethanol and
Concentration sensitivity figure；
Fig. 4 is selective figure of the flower-shaped indium oxide micron rod air-sensitive material to ethanol of optimal proportion in embodiment 1.
Embodiment
With reference to embodiment, the present invention will be further described in detail, but this explanation will not be constituted to the present invention's
Limitation.
Embodiment 1
Take 2mmol InCl3In 30ml deionized waters, the solution of clear is obtained after stirring 5min.Weigh 3.5g
Glucose and 3.5g urea, by the mass ratio (1:1) amount is added in clear solution, and stirs 1h under magnetic stirring apparatus
And ultrasonic disperse 30min, obtain water white transparency mixed solution.The mixed solution is transferred in 50ml hydrothermal reaction kettle,
Brownish black precipitated liquid is obtained at 180 DEG C after hydro-thermal reaction 8h.By obtaining brownish black sediment after washing, centrifuging for several times, by this
Sediment dries 10h in 60 DEG C of thermostatic drying chamber, finally calcines 2h in 500 DEG C of air atmosphere, obtains yellow powder
Product.
Embodiment 2-5
Similarly, different quality ratio (4 is weighed:0,4:1,2:1,1:2,0:4) glucose and urea is added to InCl3Water
In solution, a series of different-shapes and the In of size are then obtained after similarity condition hydro-thermal reaction2O3Product, step be the same as Example
1。
Table one
| M (glucose):M (urea) | 4:1 | 2:1 | 1:1 | 1:2 |
| Average length (μm) | 2.05 | 1.11 | 0.67 | 0.86 |
| Average diameter (nm) | 656 | 354 | 200 | 514 |
As shown in Fig. 1 (a), when only adding glucose reagent, obtained indium oxide product is unbodied multi-pore micron
Spherical structure, when only adding urea reagent, what is obtained is unbodied micron cube structure, but when both have both at the same time, is led to
Cross and change both mass ratioes, a series of various sizes of flower-shaped indium oxide micron bars (being shown in Table one) can be obtained.Select this most
The flower-shaped indium oxide sample of small size is used as air-sensitive test material.Pass through Fig. 2, it can be seen that very sharp (211), (222),
(400), the Correlative characteristic peaks such as (440), (622), without other any impurity peaks, showing the indium oxide sample of the size has well
Crystallinity.Prepare 0.01g/mL coating slurries using absolute ethyl alcohol as solvent, it is coated to obtaining in golden interdigital electrode
The sensing layer thickness of gas sensitive is 200~400nm.After drying in the shade, the gas sensor of preparation is placed on agingtable and heated always
Change 24h, finally carry out air-sensitive test.From Fig. 3 and Fig. 4 it will be clear that with the indium oxide particles of business (size is 50~
100nm) compare, optimum working temperature decrease and also under different concentration ethanol gas sensitivity it is high all than commercial material.
Importantly, in the selectivity test of gas, for different types of 100ppm gas, prepared flower-shaped indium oxide
Sensitivity of the micron bar material to alcohol gas is higher than commercial material, indicates the material selectivity excellent to ethanol
Can, this solves the defect of general ethanol sensor poor selectivity well.
Claims (1)
1. the preparation method of flower-shaped indium oxide micron bar material, its by add certain mass than glucose and urea in indium salts
The aqueous solution in, magnetic agitation 0.5h~1h at room temperature, described indium salts are inidum chloride or indium nitrate, and the concentration of indium salts solution is
The mass ratio of 0.033~0.067mol/L, glucose and urea is (0.25~4):1, the solution of water white transparency is transferred to water
In thermal response kettle, hydrothermal temperature is 160~180 DEG C, and 6~10h of reaction time reacts after a few hours, obtained at high temperature
Product by centrifugation, washing, dry, calcining, then can obtain the flower-shaped indium oxide micron bar of target product of yellow, calcining heat
In 450 DEG C~550 DEG C of air atmospheres, to make annealing treatment 2~4h, described flower-shaped indium oxide micron bar material is by several length
Spend for 0.5~0.7 μm, a diameter of 180~210nm indium oxide micron bar is constituted.
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| 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 |
| 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 |
| CN110357606B (en) * | 2019-08-01 | 2020-12-01 | 东北大学 | In based on zeolite substrate2O3Preparation and application of nano material |
| 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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