CN110455874A - A kind of CoSn double metal oxide semiconductor material and preparation method thereof - Google Patents
A kind of CoSn double metal oxide semiconductor material and preparation method thereof Download PDFInfo
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- CN110455874A CN110455874A CN201910777866.6A CN201910777866A CN110455874A CN 110455874 A CN110455874 A CN 110455874A CN 201910777866 A CN201910777866 A CN 201910777866A CN 110455874 A CN110455874 A CN 110455874A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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Abstract
The invention belongs to a kind of CoSn double metal oxide semiconductor materials of gas sensor technical field and preparation method thereof.The material is made of Co the and Sn nano particle of different mol ratio example, and the molar ratio of Co and Sn are 0.1-10, nano particle diameter 20-50nm.Material of the invention can be used as gas sensitive detection material, detect to gases such as methane in environment, ethyl alcohol, ammonias, and preparation is easy, high income, have many performance advantages such as detection temperature is low, baseline is steady, sensitivity is high.
Description
Technical field
The invention belongs to gas sensor technical field more particularly to a kind of CoSn double metal oxide semiconductor material and
Preparation method.
Background technique
Resistor-type semiconductor gas sensor is a kind of gas sensor most widely used at present, has at low cost, sound
Answer many advantages such as fast, small in size, sensitivity is high.But current gas sensor especially Sn base semiconductor gas sensor exists
The high disadvantage of poor selectivity, power consumption, so, develop high-performance, highly selective, low-power consumption gas sensor has important meaning
Justice.
Gas sensitive is of great significance for lift gas sensor performance, wherein Sn base oxide material is quotient
The gas sensitive of product, detection gas type is extensive, but detects temperature compared with high, power consumption is big, detects poor specificity.Commercially available half
Conductor gas sensor, heating power consumption is up to 350mW, and has response simultaneously to multiple gases such as ammonia, VOC, to gas
Poor selectivity.
Summary of the invention
In view of the above-mentioned problems, the material is not by the invention proposes a kind of CoSn double metal oxide semiconductor material
Co and Sn nano particle with molar ratio forms, and the molar ratio of Co and Sn are 0.1-10, nano particle diameter 20-50nm.
The material is 14.1~50 to the sensitivity of 100ppm ethyl alcohol.
A kind of preparation method of CoSn double metal oxide semiconductor material, comprising the following steps:
1) metal salt for weighing Co and Sn respectively, is dissolved in the mixed solution of dehydrated alcohol or ethyl alcohol and methanol, stirs shape
At clear solution A；
2) it weighs precipitating reagent to be dissolved in the mixed solution of dehydrated alcohol or ethyl alcohol and methanol, stirring forms clear solution B；
3) solution A for obtaining step 1) rapidly joins in the solution B of step 2) formation, and sufficient standing obtains bimetallic
Oxide precursor precipitating；
4) the presoma precipitating that step 3) obtains is washed and is dried using dehydrated alcohol；
5) it by presoma depositing abrasive that step 4) obtains and calcines, obtains CoSn bimetallic oxide.
In the step 1), the metal salt is the nitrate or chlorate of Co, Sn.
In the solution B, precipitating reagent is 2-methylimidazole, and the molar ratio of precipitating reagent and metal salt is 1:4.
In the step 3), time of repose 12-24h.
In the step 5), the heating rate of calcination process is 2-10 DEG C/min, and calcination environment is air, and calcination temperature is
400~800 DEG C.
The beneficial effects of the present invention are:
1, preparation method of the present invention is simple and easy to do, and using coprecipitation, the bimetallic oxide metal that may make is uniform
Distribution；Meanwhile low raw-material cost, it is easy to amplify.
2, it uses 2-methylimidazole for precipitating reagent, forms the presoma of special construction using coordinate bond and metal salt
Grain, through high-temperature calcination, organic ligand volatilizees to form cavity, and controls metal oxide appearance structure.
3, CoSn double metal oxide semiconductor material prepared by the present invention is in Nanoparticulate, and partial size is small, is conducive to drop
Sensitive layer thickness in low sensor, and then the sensing response time is reduced, by the way of metal-doped, examined using Co base oxide
The advantage that testing temperature is low, baseline is steady, preparation CoSn bimetallic oxide reduce power consumption for promoting sensor response selectivity
With certain practice significance.
Detailed description of the invention
Fig. 1 is Co50Sn50O prepared by the embodiment of the present invention 1xEthyl alcohol air-sensitive performance test figure；
Fig. 2 is Co50Sn50O prepared by the embodiment of the present invention 1xMethane, ammonia air-sensitive performance test chart；
Fig. 3 is Co50Sn50O prepared by the embodiment of the present invention 1xSEM figure；
Fig. 4 is Co40Sn60O prepared by the embodiment of the present invention 2xEthyl alcohol air-sensitive performance test figure；
Fig. 5 is Co40Sn60O prepared by the embodiment of the present invention 2xSEM figure；
Fig. 6 is Co60Sn40O prepared by the embodiment of the present invention 3xEthyl alcohol air-sensitive performance test figure；
Fig. 7 is Co60Sn40O prepared by the embodiment of the present invention 3xSEM figure.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail:
Embodiment 1
0.88g Co (NO is weighed respectively3)2·6H2O and 0.69g SnCl2·2H2O is dissolved in 20mL dehydrated alcohol and 20mL first
In the mixed solution that alcohol is formed, is stirred at room temperature to metal salt whole dissolution and form homogeneous solution A, Co's and Sn rubs in solution A
You are than being 1:1；The 2-methylimidazole (referred to as: 2MI) for weighing 2.01g is dissolved in the mixing that 20mL dehydrated alcohol and 20mL methanol are formed
In solution, stirring to formation homogeneous solution B at room temperature；Solution A is rapidly joined into solution B, and is stood for 24 hours, it is heavy to obtain sky blue
It forms sediment, is washed and dried using dehydrated alcohol and precipitated to get to Co50Sn50-2MI presoma.
Co50Zn50-2MI presoma precipitating is fully ground, and weighs 0.5g and is placed in Muffle furnace, under air environment,
2 DEG C/min is warming up to 500 DEG C, keeps the temperature 2h, and Co50Sn50O is madex。
Co50Sn50O made from the present embodimentxDispersion forms uniform dispersion liquid in ethanol.Fig. 1 is shown
Co50Sn50OxTo the dynamic response curve of ethyl alcohol, concentration of alcohol be it is steps distribution (concentration gradient 2.5ppm, 5ppm,
10ppm, 20ppm, 30ppm, 50ppm, 80ppm, 100ppm), ladder-like distribution is also presented in response, is rung with 100ppm ethyl alcohol material
It should be with reference to reduced value.At 350 DEG C, Co50Sn50OxSensitivity to 100ppm ethyl alcohol is 47.1.
Fig. 2 show Co50Sn50O made from the present embodimentxIt is bent to the dynamic response of 100ppm methane, 100ppm ammonia
Line, at 350 DEG C, Co50Sn50OxSensitivity to 100ppm methane, 100ppm ammonia is respectively 25.9,40.3.
Fig. 3 show Co50Sn50O made from the present embodimentxScanning electron microscope (referred to as: SEM) figure, times magnification
Number is 20,000 times, is in granular form distribution.
Embodiment 2
0.70g Co (NO is weighed respectively3)2·6H2O and 0.83g SnCl2·2H2O is dissolved in 20mL dehydrated alcohol and 20mL first
In the mixed solution that alcohol is formed, is stirred at room temperature to metal salt whole dissolution and form homogeneous solution A, Co's and Sn rubs in solution A
You are than being 2:3；The 2-MI for weighing 2.01g is dissolved in the mixed solution that 20mL dehydrated alcohol and 20mL methanol are formed, and is stirred at room temperature
It mixes to formation homogeneous solution B；Solution A is rapidly joined into solution B, and stands 18h, sky blue precipitating is obtained, using dehydrated alcohol
It is washed and is dried and precipitated to get to Co40Sn60-2MI presoma.
Co40Sn60-2MI presoma precipitating is fully ground, and weighs 0.5g and is placed in Muffle furnace, under air environment,
2 DEG C/min is warming up to 500 DEG C, keeps the temperature 2h, and Co40Sn60O is madex。
Co40Sn60O made from the present embodimentxDispersion forms uniform dispersion liquid in ethanol.Fig. 4 is shown
Co40Sn60OxTo the dynamic response curve of ethyl alcohol, concentration of alcohol be it is steps distribution (concentration gradient 2.5ppm, 5ppm,
10ppm, 20ppm, 30ppm, 50ppm, 80ppm, 100ppm), ladder-like distribution is also presented in response, is rung with 100ppm ethyl alcohol material
It should be with reference to reduced value.At 350 DEG C, Co40Sn60OxSensitivity to 100ppm ethyl alcohol is 14.1.
Fig. 5 show Co40Sn60O made from the present embodimentxSEM figure, amplification factor be 20,000 times, be in Polyhedral Particles
Shape distribution.
Embodiment 3
1.06g Co (NO is weighed respectively3)2·6H2O and 0.55g SnCl2·2H2O is dissolved in 20mL dehydrated alcohol and 20mL first
In the mixed solution that alcohol is formed, is stirred at room temperature to metal salt whole dissolution and form homogeneous solution A, Co's and Sn rubs in solution A
You are than being 3:2；The 2-MI for weighing 2.01g is dissolved in the mixed solution that 20mL dehydrated alcohol and 20mL methanol are formed, and is stirred at room temperature
It mixes to formation homogeneous solution B；Solution A is rapidly joined into solution B, and is stood for 24 hours, sky blue precipitating is obtained, using dehydrated alcohol
It is washed and is dried and precipitated to get to Co60Sn40-2MI presoma.
Co60Sn40-2MI presoma precipitating is fully ground, and weighs 0.5g and is placed in Muffle furnace, under air environment,
2 DEG C/min is warming up to 500 DEG C, keeps the temperature 2h, and Co60Sn40O is madex。
Co60Sn40O made from the present embodimentxDispersion forms uniform dispersion liquid in ethanol.Fig. 6 is shown
Co60Sn40OxTo the dynamic response curve of ethyl alcohol, concentration of alcohol be it is steps distribution (concentration gradient 2.5ppm, 5ppm,
10ppm, 20ppm, 30ppm, 50ppm, 80ppm, 100ppm), ladder-like distribution is also presented in response, is rung with 100ppm ethyl alcohol material
It should be with reference to reduced value.At 350 DEG C, Co60Sn40OxSensitivity to 100ppm ethyl alcohol is 43.7.
Fig. 7 show Co60Sn40O made from the present embodimentxSEM figure, amplification factor is 20,000 times, is in granular form point
Cloth.
Claims (7)
1. a kind of CoSn double metal oxide semiconductor material, which is characterized in that the material by different mol ratio example Co and
The molar ratio of Sn nano particle composition, Co and Sn are 0.1-10, nano particle diameter 20-50nm.
2. CoSn double metal oxide semiconductor material according to claim 1, which is characterized in that the material is 350
DEG C when, be 14.1~50 to the sensitivity of 100ppm ethyl alcohol.
3. a kind of preparation method of CoSn double metal oxide semiconductor material according to claim 1, which is characterized in that
The following steps are included:
1) metal salt for weighing Co and Sn respectively, is dissolved in the mixed solution of dehydrated alcohol or ethyl alcohol and methanol, and stirring forms clear
Clear solution A；
2) it weighs precipitating reagent to be dissolved in the mixed solution of dehydrated alcohol or ethyl alcohol and methanol, stirring forms clear solution B；
3) solution A for obtaining step 1) rapidly joins in the solution B of step 2) formation, sufficient standing, obtains bimetallic oxidation
Object presoma precipitating；
4) the presoma precipitating that step 3) obtains is washed and is dried using dehydrated alcohol；
5) it by presoma depositing abrasive that step 4) obtains and calcines, obtains CoSn bimetallic oxide.
4. the preparation method of CoSn double metal oxide semiconductor material according to claim 2, which is characterized in that described
In step 1), the metal salt is the nitrate or chlorate of Co, Sn.
5. the preparation method of CoSn double metal oxide semiconductor material according to claim 2, which is characterized in that described
In solution B, precipitating reagent is 2-methylimidazole, and the molar ratio of precipitating reagent and metal salt is 1:4.
6. the preparation method of CoSn double metal oxide semiconductor material according to claim 2, which is characterized in that described
In step 3), time of repose 12-24h.
7. the preparation method of CoSn double metal oxide semiconductor material according to claim 2, which is characterized in that described
In step 5), the heating rate of calcination process is 2-10 DEG C/min, and calcination environment is air, and calcination temperature is 400~800 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113533451A (en) * | 2021-07-14 | 2021-10-22 | 中国人民解放军国防科技大学 | Co Co-doped with Sn and Mn3O4Nanosheet, preparation method and application of nanosheet as gas-sensitive material |
| CN114414634A (en) * | 2022-01-20 | 2022-04-29 | 重庆工商大学 | Iron-doped cobalt hydroxystannate gas sensor material and preparation method thereof |
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