CN107607588A - SnO is modified for gas sensor2Nano material - Google Patents
SnO is modified for gas sensor2Nano material Download PDFInfo
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- CN107607588A CN107607588A CN201710611962.4A CN201710611962A CN107607588A CN 107607588 A CN107607588 A CN 107607588A CN 201710611962 A CN201710611962 A CN 201710611962A CN 107607588 A CN107607588 A CN 107607588A
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Abstract
The invention discloses a kind of SnO is modified for gas sensor2Nano material, preparation method are：Using anhydrous stannic chloride as raw material, deionized water and N, N dimethylformamide are solvent, and solution heats up after being premixed with adjuvant, and reaction obtains SnO2Nano material, by SnO2Nano material is heat-treated after being well mixed with urea, and g C are made3N4The SnO of modification2Nano material.The characteristics of this method, is to realize g C3N4With SnO2The In-situ reaction of nano material, keeping SnO2G C are realized while structural intergrity3N4Surface modification, using the plurality of advantages that nano material specific surface area is big and composite electric transmission is fast, realize the structure of high sensitivity gas sensitive.Nano material prepared by the present invention can significant increase SnO2The sensitivity of gas sensitive.With the characteristics of preparation technology is simple, cost is low, its properties of product is stable, and gas sensitivity is high.
Description
Technical field
The invention belongs to gas sensor technology field, and in particular to a kind of to be modified SnO for gas sensor2Nanometer
Material, in particular for the g-C of gas sensor3N4Modify SnO2Nano material, and its preparation method and application.
Background technology
Metal oxide such as ZnO, SnO2、WO3Deng because with excellent performance, environment is friendly, aboundresources, cheap
The advantages that, it is the relatively broad gas sensitive of research.Modified by metal oxide surface, the technique such as metal/precious metal doping
The air-sensitive performance of material can be lifted, there is very extensive application in gas sensor field.
Determining the key factor of Semiconductor gas sensors material sensitivity includes：Specific surface area, nanometer material is built by chemical method
Material, allow material that there is larger specific surface area to increase contact of the material with object gas, and then lift the sensitivity of material；
The regulation and control of room/defect, by control system Lacking oxygen, the reactivity of object gas and sensitive material, Ke Yiti can be lifted
Rise the sensitivity of material；Build composite, using nano material specific surface area greatly and composite electric transmission soon it is many
Advantage, the structure of high sensitivity gas sensitive can be achieved.
g-C3N4As emerging two-dimensional material, boundless application prospect is shown in each field, especially with metal oxygen
The compound gas-sensitive property that can lift material of compound.
The content of the invention
For overcome the deficiencies in the prior art, present invention offer is a kind of to be modified SnO for gas sensor2Nanometer material
Material, the i.e. g-C for gas sensor3N4Modify SnO2Nano material.
Another object of the present invention is：Described in providing SnO is modified for gas sensor2Nano material is answered
With.
The a kind of of the present invention is modified SnO for gas sensor2The preparation method of nano material comprises the following steps：
The object of the invention is realized by following proposal：A kind of g-C for gas sensor3N4Modify SnO2Nano material, pass through
Following preparation methods obtain, and comprise the following steps：
（1）Using anhydrous stannic chloride as raw material, anhydrous stannic chloride is dissolved in the pre- miscible agents of 30 mL, anhydrous stannic chloride
Solution concentration is between 0.05M ~ 0.2M；
（2）By adjuvant and 30 mLN, dinethylformamide premix, 10 ~ 20 min are stirred, obtain adjuvant solution；
（3）Anhydrous stannic chloride solution and adjuvant solution are mixed, after 20 ~ 30 min are stirred at room temperature, solution is moved to and risen
Temperature is into 60 ~ 95 DEG C of water-bath, and after then stirring 2 ~ 5 h, by the sample of centrifugation, it is small to dry 4 ~ 12 at 60 ~ 70 DEG C
When；
（4）By above-mentioned dried sample and urea in mass ratio 1:3 ~ 10 premixs, then carry out being heat-treated to obtain g-C3N4Modification
SnO2Nano material, wherein, heat treatment condition is air atmosphere, and temperature is：200 ~ 250 DEG C 1 ~ 3 hour, 300 ~ 350 DEG C,
1.5 ~ 2.5 hours, 500 ~ 600 DEG C, 1.5 ~ 5 hours, programming rate was 1 ~ 4 DEG C/min.
On the basis of such scheme, described pre- miscible agent is DMF and deionized water mixed solvent,
N,N-dimethylformamide is 5 ~ 20 with deionized water volume ratio:100.
Described adjuvant is 1- methylimidazoles, 2-methylimidazole, 1, one kind or its combination in 2-methylimidazole.
On the basis of such scheme, the mol ratio of anhydrous stannic chloride and adjuvant is 1:3~5.
The present invention is matched somebody with somebody using passing through presoma and adjuvant premix under low temperature by system temperature change and each raw material
Than directly synthesizing SnO2Nano material simultaneously realizes that room regulates and controls, and then realizes g-C by heat treatment3N4Modify SnO2 nanometer materials
Material.Test result shows that this method can lift SnO2The sensitivity of nano material.There is provided it is a kind of by straightforward procedure obtain
g-C3N4Modify SnO2Nano material, SnO not only greatly improved2The air-sensitive performance of nano material, preparation technology is simple, cost
It is low, there is actual application value to the development for being pushed further into semiconductor gas sensing device.
The present invention provides a kind of above-mentioned g-C for gas sensor3N4Modify SnO2Applications to nanostructures, for gas
The g-C of dependent sensor3N4Modify SnO2Application of the nano material in gas sensor.
The present invention is advantageous in that：Realize g-C3N4With SnO2The In-situ reaction of nano material, keeping SnO2Structure is complete
G-C is realized while whole property3N4Surface modification, using nano material specific surface area greatly and composite electric transmission soon it is all
More advantages, realize the structure of high sensitivity gas sensitive.Nano material prepared by the present invention can significant increase SnO2Air-sensitive material
The sensitivity of material.With the characteristics of preparation technology is simple, cost is low, its properties of product is stable, and gas sensitivity is high.
Brief description of the drawings
Fig. 1 is the SnO of the present invention2Nano material and g-C3N4Compound electron scanning imaging（SEM）Figure；
Fig. 2 is SnO of the present invention2Nano material is with composite in 130 DEG C of Sensitivity comparison figures to acetone of operating temperature.
Embodiment
Embodiment 1
A kind of g-C for gas sensor3N4Modify SnO2Nano material, obtained by following preparation methods, including following step
Suddenly：
（1）Using anhydrous stannic chloride as raw material, the deionized water mixing of 5 ml DMF and 25mL is taken, then
Add 1.5 mmol stannic chloride pentahydrate, obtained solution A；
（2）4.5 mmol 1- methylimidazoles are placed in 30 mLN, premixed in dinethylformamide, stir 20 min, are made
Solution B；
（3）Solution A and solution B are mixed, after 20min is stirred at room temperature, solution is moved to and had warmed up into 65 DEG C of water-bath,
Then after stirring 5 h, the sample of centrifugation is dried 8 hours at 60 DEG C；
（4）By above-mentioned dried sample and urea in mass ratio 1:3 premixs, then carry out being heat-treated to obtain g-C3N4Modify SnO2
Nano material powder, wherein, heat treatment condition is air atmosphere, and temperature is：200 DEG C, 3 hours, 350 DEG C, 1.5 hours,
600 DEG C, 1.5 hours, programming rate is 2 DEG C/min.
Electron scanning imaging such as Fig. 1 is SnO of the invention2Nano material and g-C3N4Compound electron scanning imaging（SEM）
Shown in figure, powder made from the present embodiment is scattered to be applied on six pin earthenware air-sensitive testing elements, using WS-30A type gas sensitive elements
Response under part test system and test various concentrations to acetone gas, operating temperature are 130 DEG C, the acetone gas spirit to 10ppm
Sensitivity is reached for 19.8.
Embodiment 2
A kind of g-C for gas sensor3N4Modify SnO2Nano material, obtained by following preparation methods, including following step
Suddenly：
（1）Using anhydrous stannic chloride as raw material, 1.5 mL DMF and the mixing of 28.5 mL deionized waters are taken,
Then 6 mmol anhydrous stannic chloride, obtained solution A are added；
（2）By the 1 of 20 mmol, 2-methylimidazole and 30 mLN, dinethylformamide premix, 20 min, obtained solution are stirred
B；
（3）Solution A and solution B are mixed, after 30 min are stirred at room temperature, solution is moved to and had warmed up into 95 DEG C of water-bath,
Then after stirring 5 h, the sample of centrifugation is dried 12 hours at 70 DEG C；
（4）By above-mentioned dried sample and urea in mass ratio 1:5 premixs, then carry out being heat-treated to obtain g-C3N4Modify SnO2
Nano material powder, wherein, heat treatment condition is air atmosphere, and temperature is：250 DEG C, 1.5 hours, 350 DEG C, 2 hours,
550 DEG C, 5 hours, programming rate is 1 ~ 4 DEG C/min.
Powder made from the present embodiment is scattered to be applied on six pin earthenware air-sensitive testing elements, using WS-30A type air-sensitives
Response under element test system test various concentrations to acetone gas, operating temperature is 130 DEG C, to 10ppm acetone gas
Sensitivity is reached for 21.3.
Embodiment 3
A kind of g-C for gas sensor3N4Modify SnO2Nano material, obtained by following preparation methods, including following step
Suddenly：
（1）Using anhydrous stannic chloride as raw material, 3 mL DMF and the mixing of 27 mL deionized waters are taken, then
Add 3 mmol anhydrous stannic chloride, obtained solution A；
（2）By the 1 of 12 mmol, 2-methylimidazole adjuvant and 30 mLN, dinethylformamide premix, 20 min, system are stirred
Obtain solution B；
（3）Solution A and solution B are mixed, after 30 min are stirred at room temperature, solution is moved to and had warmed up into 85 DEG C of water-bath,
Then after stirring 4 h, the sample of centrifugation is dried 12 hours at 70 DEG C；
（4）By above-mentioned dried sample and urea in mass ratio 1:8 premixs, then carry out being heat-treated to obtain g-C3N4Modify SnO2
Nano material powder, wherein, heat treatment condition is air atmosphere, and temperature is：250 DEG C, 1.5 hours, 350 DEG C, 2 hours,
550 DEG C, 5 hours, programming rate is 1 ~ 4 DEG C/min.
Powder made from the present embodiment is scattered to be applied on six pin earthenware air-sensitive testing elements, using WS-30A type air-sensitives
Response under element test system test various concentrations to acetone gas, operating temperature is 130 DEG C, to 10ppm acetone gas
Sensitivity is reached for 18.4.
As shown in Fig. 2 g-C of the present invention3N4Modify SnO2Nano material same concentrations are to high sensitivity in SnO2。
Claims (5)
1. a kind of be modified SnO for gas sensor2Nano material, obtained by following preparation methods, including following step
Suddenly：
（1）Using anhydrous stannic chloride as raw material, anhydrous stannic chloride is dissolved in the pre- miscible agents of 30 mL, anhydrous stannic chloride
Solution concentration is between 0.05M ~ 0.2M；
（2）By adjuvant and 30 mLN, dinethylformamide premix, 10 ~ 20 min are stirred, obtain adjuvant solution；
（3）Anhydrous stannic chloride solution and adjuvant solution are mixed, after 20 ~ 30 min are stirred at room temperature, solution is moved to and risen
Temperature is into 60 ~ 95 DEG C of water-bath, and after then stirring 2 ~ 5 h, by the sample of centrifugation, it is small to dry 4 ~ 12 at 60 ~ 70 DEG C
When；
（4）By above-mentioned dried sample and urea in mass ratio 1:3 ~ 10 premixs, then carry out being heat-treated to obtain g-C3N4Modification
SnO2Nano material, wherein, heat treatment condition is air atmosphere, and temperature is：200 ~ 250 DEG C 1 ~ 3 hour, 300 ~ 350 DEG C,
1.5 ~ 2.5 hours, 500 ~ 600 DEG C, 1.5 ~ 5 hours, programming rate was 1 ~ 4 DEG C/min.
2. according to claim 1 be modified SnO for gas sensor2Nano material, it is characterised in that：Described
Pre- miscible agent is that DMF and deionized water mix, DMF and deionized water volume ratio be 5 ~
20:100。
3. according to claim 1 be modified SnO for gas sensor2Nano material, it is characterised in that：Described
Adjuvant is 1- methylimidazoles, 2-methylimidazole, 1, one kind or its combination in 2-methylimidazole.
4. it is modified SnO for gas sensor according to claim 1 or 32Nano material, it is characterised in that：It is anhydrous
The mol ratio of butter of tin and adjuvant is 1:3~5.
5. a kind of be modified SnO according to any one of claim 1-4 for gas sensor2Nano material is answered
With for acetone gas detection gas sensor.
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| CN201710611962.4A CN107607588B (en) | 2017-07-25 | 2017-07-25 | Modified SnO for gas sensors2Nano material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110396006A (en) * | 2019-07-16 | 2019-11-01 | 济南大学 | A kind of ZIF-8 film cladding SnO2Composite air-sensitive material and its preparation method and application |
| CN110841682A (en) * | 2019-11-09 | 2020-02-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of tin oxide modified graphite-like phase carbon nitride nanosheet, product and application thereof |
| CN110927219A (en) * | 2019-12-10 | 2020-03-27 | 苏州慧闻纳米科技有限公司 | Gas sensitive material, preparation method thereof and manufacturing method of gas sensor |
| CN112758975A (en) * | 2020-12-22 | 2021-05-07 | 华中科技大学 | CuO doped SnO2Nanoparticles and H2S gas sensor preparation method and product |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110396006A (en) * | 2019-07-16 | 2019-11-01 | 济南大学 | A kind of ZIF-8 film cladding SnO2Composite air-sensitive material and its preparation method and application |
| CN110396006B (en) * | 2019-07-16 | 2021-11-09 | 济南大学 | ZIF-8 film coated SnO2Composite gas-sensitive material and preparation method and application thereof |
| CN110841682A (en) * | 2019-11-09 | 2020-02-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of tin oxide modified graphite-like phase carbon nitride nanosheet, product and application thereof |
| CN110841682B (en) * | 2019-11-09 | 2022-09-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of tin oxide modified graphite-like phase carbon nitride nanosheet, product and application thereof |
| CN110927219A (en) * | 2019-12-10 | 2020-03-27 | 苏州慧闻纳米科技有限公司 | Gas sensitive material, preparation method thereof and manufacturing method of gas sensor |
| CN112758975A (en) * | 2020-12-22 | 2021-05-07 | 华中科技大学 | CuO doped SnO2Nanoparticles and H2S gas sensor preparation method and product |
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