CN109142627A - A kind of preparation method of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material - Google Patents
A kind of preparation method of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material Download PDFInfo
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- CN109142627A CN109142627A CN201810861789.8A CN201810861789A CN109142627A CN 109142627 A CN109142627 A CN 109142627A CN 201810861789 A CN201810861789 A CN 201810861789A CN 109142627 A CN109142627 A CN 109142627A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C01G19/02—Oxides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The present invention provides a kind of preparation method of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material.The preparation method specifically includes: using graphene oxide as base material, using two hydrated stannous chlorides as raw material, sodium hydroxide provides hydroxyl, using deionized water as solvent, cetyl trimethylammonium bromide is surfactant, using traditional hydro-thermal method, after washing and freeze-drying, three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material is finally obtained.This method simple production process, two-dimensional surface substrate provided by graphene effectively prevent the reunion of tin oxide nano piece, have increased considerably the specific surface area of material, obtain highly sensitive novel gas sensitive.
Description
Technical field
The present invention relates to be related to a kind of preparation side of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material
Method belongs to advanced nano-functional material fabricating technology field.
Background technique
Into after 21 century, global industry is rapidly developed, and brings huge benefit for the development of the mankind, but same with this
When, problem of environmental pollution is also increasingly severe, wherein especially gaseous contamination, not only generates massive losses to social property, together
When also can generate huge challenge to the health of the mankind.Therefore, people increasingly pay attention to the detection to toxic gas.Except this
Except, as the improvement of people's living standards, also most important about the detection of formaldehyde in the home decoration.Inspection for gas
There are many survey methods, wherein by the semiconductor gas sensor of metal oxide preparation due to its high sensitivity, long service life,
The advantages that at low cost and be widely used.Main metal oxide has SnO2、ZnO、Fe2O3Deng traditional gas sensitive, also have
In2O3, the novel gas sensitive such as NiO, CuO.That this experiment mainly discusses is SnO2Air-sensitive performance.SnO2It is a kind of typical N
Type semiconductor, forbidden bandwidth 3.6eV, SnO2With reversible to gas detection, the adsorption desorption time is short, physicochemical properties are steady
The advantages such as fixed, energy saving, expense be low, therefore be the emphasis of air-sensitive research field for a long time.In order to further increase SnO2
Air-sensitive performance can be effectively prevented the agglomeration of nano material by the addition preferable base material of electric conductivity, from
And improve the air-sensitive performance of material entirety.
For nano material, the variation of morphosis can generate large effect to the air-sensitive performance of material, no
It only can further improve SnO2The selectivity of gas sensitive, moreover it is possible to promote its sensitivity further.Have at present
The nanostructure SnO of variform2It is successfully prepared, such as Lin et al. (Lin, Ying, et al. "
Synergistically improved formaldehyde gas sensing properties of SnO2
microspheres by indium and palladium co-doping."Ceramics International 41.6
(2015): 7329-7336.) to mesoporous SnO2The successful preparation of microballoon.Due to single gas sensitive exist always it is certain
Limitation, so people increasingly pay close attention to the preparation for metal oxide composite air-sensitive material.With other base materials it is compound after,
On the one hand it prevents nano-metal-oxide from generating reunion, to increase the specific surface area of material, gas sensitive is inhaled
Attached more test gases；On the other hand, rGO is good conductor base material, can be accelerated between metal oxide and rGO
Electron-transport, so as to improve the air-sensitive performance of material, as Jian Zhang et al. (Jian Zhang, Jinjin Wu,
Xiaoxia Wang,Dawen Zeng,Changsheng Xie. Enhancing room-temperature NO2
sensing properties via forming heterojunction for NiO-rGO composited with
SnO2Nanoplates [J] Sensors & Actuators:B. Chemical, 2017,243.) have studied SnO2With
To the influence of gas sensing property after NiO-rGO is compound.SnO2Although a kind of traditional gas sensitive, with the compound neck of graphene
There are also many problems to need to solve in domain, therefore also needs further to study in this field.
Summary of the invention
The object of the present invention is to provide a kind of preparation sides of three-dimensional hierarchical structure graphene composite tin oxide nanometer sheet
Method, this method have that at low cost, easy to operate, yield is high and does not generate noxious material, therefore can be realized industrialized big rule
Mould production.Obtained three-dimensional hierarchical structure graphene composite tin oxide nanometer sheet effectively reduces the group of tin oxide nano piece
Poly- phenomenon, is obviously improved so that gas sensing property has, and can be applied to gas sensor field.Realize the technology of the object of the invention
Scheme is: a kind of preparation method of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material, it is characterised in that: with
Graphene oxide is as base material, and using two hydrated stannous chlorides as raw material, sodium hydroxide provides hydroxyl, cetyl trimethyl
Ammonium bromide is additive, using deionized water as solvent, using hydro-thermal method, and composite tin oxide nanometer sheet on the surface of graphene, finally
Obtain the three-dimensional hierarchical structure gas sensitive of graphene composite tin oxide nanometer sheet.Specific step is as follows:
(1) 20 ml deionized waters are first measured in beaker A, a certain amount of graphene oxide and 1 h of ultrasound is added, is added later
Simultaneously 20 min are stirred at room temperature in a certain amount of two hydrated stannous chloride, and wherein the concentration of graphene oxide is 0.015 ~ 0.019
Mol/L, the concentration of two hydrated stannous chlorides are 0.08 ~ 0.12 mol/L, control graphene oxide and two hydrated stannous chlorides
Molar ratio is 1:(5.3 ~ 6.3)；
(2) 20 ml deionized waters are measured in beaker B, weighing a certain amount of sodium hydroxide respectively, (concentration is 0.40 ~ 0.42
Mol/L) and cetyl trimethylammonium bromide (concentration is 0.08 ~ 0.12 mol/L) is in beaker, is stirred at room temperature 20
min；Wherein, the molar ratio of sodium hydroxide and cetyl trimethylammonium bromide is (3.5 ~ 5): 1；
(3) solution in beaker A is poured into beaker B, continues to stir 20 min at room temperature, so that solution mixing is equal
It is even；
(4) step (3) acquired solution is poured into 50 ml reaction kettles, 20 ~ 28 h is kept the temperature at 140 ~ 180 DEG C；What is obtained is heavy
Shallow lake is washed with deionized three times respectively, and dehydrated alcohol washes twice, and for the freeze-drying of next step, last time should be used
Deionization washing (should suitably be dispersed using ultrasonic cleaning machine, subtract less granular agglomeration) in the process；
(5) the centrifugation product that step (4) obtains is poured into surface plate, using freeze drier, by sample freezing, (temperature is -49
DEG C), the moisture in sample is removed by vacuumizing later, can be obtained the nanometer hierarchical structure of graphene composite tin oxide.
Detailed description of the invention
Fig. 1 is the XRD spectrum of three-dimensional hierarchical structure graphene composite tin oxide nanometer sheet.
Fig. 2 is that the FESEM of three-dimensional hierarchical structure graphene composite tin oxide nanometer sheet schemes.
Fig. 3 is that the TEM of three-dimensional hierarchical structure graphene composite tin oxide schemes.
Fig. 4 is three-dimensional hierarchical structure graphene composite tin oxide gas sensor under optimum working temperature to 20-1000 ppm
Alcohol gas sensitivity curve figure.
Fig. 5 is the response recovery curve of three-dimensional hierarchical structure graphene composite tin oxide gas sensor under optimum working temperature
Figure.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example:
Embodiment 1
(1) 20 ml deionized waters are first measured in beaker A, a certain amount of graphene oxide and 1 h of ultrasound is added, is added later
Simultaneously 20 min are stirred at room temperature in a certain amount of two hydrated stannous chloride, and wherein the concentration of graphene oxide is 0.015 mol/L,
The concentration of two hydrated stannous chlorides is 0.08 mol/L, and the molar ratio for controlling graphene oxide and two hydrated stannous chlorides is 1:
(5.3)；
(2) 20 ml deionized waters are measured in beaker B, weigh a certain amount of sodium hydroxide respectively (concentration is 0.40 mol/L)
With cetyl trimethylammonium bromide (concentration is 0.08 mol/L) in beaker, 20 min are stirred at room temperature；Wherein, hydrogen-oxygen
The molar ratio for changing sodium and cetyl trimethylammonium bromide is 3.5:1；
(3) solution in beaker A is poured into beaker B, continues to stir 20 min at room temperature, so that solution mixing is equal
It is even；
(4) step (3) acquired solution is poured into 50 ml reaction kettles, 20 h is kept the temperature at 140 DEG C；The precipitating of acquisition is used respectively
Deionized water is washed three times, and dehydrated alcohol washes twice, and for the freeze-drying of next step, last time should use deionized water
It washes and (should suitably be dispersed in the process using ultrasonic cleaning machine, subtract less granular agglomeration)；
(5) the centrifugation product that step (4) obtains is poured into surface plate, using freeze drier, by sample freezing, (temperature is -49
DEG C), the moisture in sample is removed by vacuumizing later, can be obtained the nanometer hierarchical structure of graphene composite tin oxide.
Embodiment 2
(1) 20 ml deionized waters are first measured in beaker A, a certain amount of graphene oxide and 1 h of ultrasound is added, is added later
Simultaneously 20 min are stirred at room temperature in a certain amount of two hydrated stannous chloride, and wherein the concentration of graphene oxide is 0.017 mol/L,
The concentration of two hydrated stannous chlorides is 0.10 mol/L, and the molar ratio for controlling graphene oxide and two hydrated stannous chlorides is 1:
5.9；
(2) 20 ml deionized waters are measured in beaker B, weigh a certain amount of sodium hydroxide respectively (concentration is 0.41 mol/L)
With cetyl trimethylammonium bromide (concentration is 0.10 mol/L) in beaker, 20 min are stirred at room temperature；Wherein, hydrogen-oxygen
The molar ratio for changing sodium and cetyl trimethylammonium bromide is 4:1；
(3) solution in beaker A is poured into beaker B, continues to stir 20 min at room temperature, so that solution mixing is equal
It is even；
(4) step (3) acquired solution is poured into 50 ml reaction kettles, 24 h is kept the temperature at 160 DEG C；The precipitating of acquisition is used respectively
Deionized water is washed three times, and dehydrated alcohol washes twice, and for the freeze-drying of next step, last time should use deionized water
It washes and (should suitably be dispersed in the process using ultrasonic cleaning machine, subtract less granular agglomeration)；
(5) the centrifugation product that step (4) obtains is poured into surface plate, using freeze drier, by sample freezing, (temperature is -49
DEG C), the moisture in sample is removed by vacuumizing later, can be obtained the nanometer hierarchical structure of graphene composite tin oxide.
Embodiment 3
(1) 20 ml deionized waters are first measured in beaker A, a certain amount of graphene oxide and 1 h of ultrasound is added, is added later
Simultaneously 20 min are stirred at room temperature in a certain amount of two hydrated stannous chloride, and wherein the concentration of graphene oxide is 0.019 mol/L,
The concentration of two hydrated stannous chlorides is 0.12 mol/L, and the molar ratio for controlling graphene oxide and two hydrated stannous chlorides is 1:
6.3；
(2) 20 ml deionized waters are measured in beaker B, weigh a certain amount of sodium hydroxide respectively (concentration is 0.42 mol/L)
With cetyl trimethylammonium bromide (concentration is 0.12 mol/L) in beaker, 20 min are stirred at room temperature；Wherein, hydrogen-oxygen
The molar ratio for changing sodium and cetyl trimethylammonium bromide is 5:1；
(3) solution in beaker A is poured into beaker B, continues to stir 20 min at room temperature, so that solution mixing is equal
It is even；
(4) step (3) acquired solution is poured into 50 ml reaction kettles, 28 h is kept the temperature at 180 DEG C；The precipitating of acquisition is used respectively
Deionized water is washed three times, and dehydrated alcohol washes twice, and for the freeze-drying of next step, last time should use deionized water
It washes and (should suitably be dispersed in the process using ultrasonic cleaning machine, subtract less granular agglomeration)；
(5) the centrifugation product that step (4) obtains is poured into surface plate, using freeze drier, by sample freezing, (temperature is -49
DEG C), the moisture in sample is removed by vacuumizing later, can be obtained the nanometer hierarchical structure of graphene composite tin oxide.
Claims (1)
1. a kind of preparation method of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material, specific synthesis step is such as
Under:
(1) 20 ml deionized waters are first measured in beaker A, a certain amount of graphene oxide and 1 h of ultrasound is added, is added later
Simultaneously 20 min are stirred at room temperature in a certain amount of two hydrated stannous chloride, and wherein the concentration of graphene oxide is 0.015 ~ 0.019
Mol/L, the concentration of two hydrated stannous chlorides are 0.08 ~ 0.12 mol/L, control graphene oxide and two hydrated stannous chlorides
Molar ratio is 1:(5.3 ~ 6.3)；
(2) 20 ml deionized waters are measured in beaker B, weighing a certain amount of sodium hydroxide respectively, (concentration is 0.40 ~ 0.42
Mol/L) and cetyl trimethylammonium bromide (concentration is 0.08 ~ 0.12 mol/L) is in beaker, is stirred at room temperature 20
min；Wherein, the molar ratio of sodium hydroxide and cetyl trimethylammonium bromide is (3.5 ~ 5): 1；
(3) solution in beaker A is poured into beaker B, continues to stir 20 min at room temperature, so that solution mixing is equal
It is even；
(4) step (3) acquired solution is poured into 50 ml reaction kettles, 20 ~ 28 h is kept the temperature at 140 ~ 180 DEG C；What is obtained is heavy
Shallow lake is washed with deionized three times respectively, and dehydrated alcohol washes twice, and for the freeze-drying of next step, last time should be used
Deionization washing (should suitably be dispersed using ultrasonic cleaning machine, subtract less granular agglomeration) in the process；
(5) the centrifugation product that step (4) obtains is poured into surface plate, using freeze drier, by sample freezing, (temperature is -49
DEG C), the moisture in sample is removed by vacuumizing later, can be obtained the nanometer hierarchical structure of graphene composite tin oxide.
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Cited By (2)
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| CN110498405A (en) * | 2019-08-21 | 2019-11-26 | 南京倍格电子科技有限公司 | A kind of graphene/tin oxide composite air-sensitive material and preparation method thereof |
| CN110577236A (en) * | 2019-10-09 | 2019-12-17 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of NiO modified tin dioxide nano material for gas sensor, product and application thereof |
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