CN107686125B - A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive - Google Patents
A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive Download PDFInfo
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- CN107686125B CN107686125B CN201710758015.8A CN201710758015A CN107686125B CN 107686125 B CN107686125 B CN 107686125B CN 201710758015 A CN201710758015 A CN 201710758015A CN 107686125 B CN107686125 B CN 107686125B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
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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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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive.The invention belongs to gas sensitive fields, and in particular to a kind of flower-shaped graded structure SnS of Al doping2The preparation method of gas sensitive.It is existing based on inorganic two-dimensional layer SnS the invention aims to solve2The NO of nano material2Sensor is unable to the problem of working and room temperature.Method: using stannic chloride pentahydrate as tin source, thiocarbamide is sulphur source, and ANN aluminium nitrate nonahydrate is silicon source, and using ethylene glycol as solvent, the flower-shaped graded structure SnS of Al doping is synthesized by the method for a step microwave heating2.Al produced by the present invention is adulterated into flower-shaped graded structure SnS2Gas sensor is made, which can detect the other NO of ppb concentration level at room temperature2, high sensitivity, safe and portable has broad application prospects.
Description
Technical field
The invention belongs to gas sensitive fields, and in particular to a kind of Al doping graded structure stannic disulfide gas sensitive
Preparation method.
Background technique
Nitrogen dioxide (NO2) to be that one kind for generating during industrial fuel burning and automotive emission is common toxic have
Evil gas is to generate acid rain with one of the main reason for causing photochemical fog, and in addition to polluting the environment, it is also threaten
The health of the mankind will cause respiratory disease and then cause serious harm to respiratory system when its concentration is more than 1ppm, because
This, to the NO under various environmental conditions2Real time on-line monitoring is carried out to be of great significance.In multiple types gas sensor,
Semiconductor transducer because have at low cost, method is easy, device volume is small, the advantages that can be integrated due to be concerned.And semiconductor
The core component of gas sensor is Semiconductor gas sensors material, therefore, design and prepare with efficient air-sensitive performance novel half
Conductor material is of great significance to the performance for improving gas sensor.
Stannic disulfide (SnS2) it is a kind of two-dimension nano materials with class graphene-structured, while having and biggish comparing table
Area and stronger electronegativity, because to NO2Gas has preferable selectivity and higher sensitivity and causes researcher
Concern, but at present pure SnS2Gas sensor also need to work (ACS Nano, 2015,9,10313.) at 120 DEG C,
Although existing method can reduce operating temperature while improving transducer sensitivity, sensor still needs to the work at 80 DEG C
To make, causes biosensor power consumption higher, preparation is complicated, and the side effect of heated current may cause and cause to be lost to element itself,
Therefore development can working and room temperature based on SnS2Gas sensor be of great significance.
Summary of the invention
The present invention is existing based on inorganic two-dimensional layer SnS in order to solve2The NO of nano material2Sensor is unable to room temperature work
The problem of making, and a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive is provided.
A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive of the present invention sequentially includes the following steps:
One, stannic chloride pentahydrate is added in ethylene glycol solution under the conditions of electromagnetic agitation, it is molten to stannic chloride pentahydrate
Xie Hou obtains mixed solution, and thiocarbamide and ANN aluminium nitrate nonahydrate, magnetic agitation is added into mixed solution under the conditions of electromagnetic agitation
Reaction solution is obtained after 10min~40min；The molar ratio of the stannic chloride pentahydrate, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:(1.5
~4): (0.01~0.05), the concentration of stannic chloride pentahydrate is 0.03~0.6mol/L in the mixed solution；
Two, the reaction solution for obtaining step 1 is fitted into microwave tube, is reacted under conditions of temperature is 170 DEG C~190 DEG C
Be centrifugated after 10min~30min, centrifugation products therefrom first use ethyl alcohol clean 3~5 times, then using deionized water cleaning 3~
5 times, it is put into vacuum oven drying, finally obtains Al doping graded structure SnS2Gas sensitive.
Beneficial effects of the present invention:
1, the present invention is prepared for Al doping graded structure SnS using a step microwave method2Gas sensitive, by regulating and controlling nine water
Close the controllable graded structure SnS of amount that aluminum nitrate is added2Conductive capability, realize room temperature NO2Response.
2, Al adulterates graded structure SnS2Gas sensitive is maintaining SnS2While graded structure, due to mixing for Al
Enter, improves based on graded structure SnS2The sensitivity of material gas sensor, at room temperature, the Al obtained using the present invention
Adulterate graded structure SnS2The gas sensor of gas sensitive preparation is to 2ppm NO2Sensitivity be 5.4.
Detailed description of the invention
Fig. 1 is that the Al that embodiment one obtains adulterates graded structure SnS2The scanning electron microscope (SEM) photograph of gas sensitive；
Fig. 2 is the graded structure SnS of different Al doping contents2X ray diffracting spectrum, a be pure SnS2Powder；b,c,d
The graded structure SnS of respectively 2%, 3% and 4%Al doping2；
Fig. 3 is pure SnS2High resolution transmission electron microscopy；
Fig. 4 is that the Al that embodiment one obtains adulterates graded structure SnS2The high resolution transmission electron microscopy of gas sensitive
Figure；
Fig. 5 is that the Al obtained using embodiment one adulterates graded structure SnS2Gas sensitive is at room temperature to various concentration
NO2Response -- recovery curve；
Fig. 6 is that the Al obtained using embodiment one adulterates graded structure SnS2Gas sensitive at room temperature sensitivity with NO2
The relation curve of concentration variation.
Specific embodiment
Specific embodiment 1: a kind of preparation of Al doping graded structure stannic disulfide gas sensitive of present embodiment
Method sequentially includes the following steps:
One, stannic chloride pentahydrate is added in ethylene glycol solution under the conditions of electromagnetic agitation, it is molten to stannic chloride pentahydrate
Xie Hou obtains mixed solution, and thiocarbamide and ANN aluminium nitrate nonahydrate, magnetic agitation is added into mixed solution under the conditions of electromagnetic agitation
Reaction solution is obtained after 10min~40min；The molar ratio of the stannic chloride pentahydrate, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:(1.5
~4): (0.01~0.05), the concentration of stannic chloride pentahydrate is 0.03~0.6mol/L in the mixed solution；
Two, the reaction solution for obtaining step 1 is fitted into microwave tube, is reacted under conditions of temperature is 170 DEG C~190 DEG C
Be centrifugated after 10min~30min, centrifugation products therefrom first use ethyl alcohol clean 3~5 times, then using deionized water cleaning 3~
5 times, it is put into vacuum oven drying, finally obtains Al doping graded structure SnS2Gas sensitive.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: five water four described in step 1
The molar ratio of stannic chloride, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:2:0.03.Other steps and parameter and one phase of specific embodiment
Together.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: five described in step 1
The molar ratio of water tin tetrachloride, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:2:0.05.Other steps and parameter and specific embodiment
One or two is identical.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: institute in step 1
The concentration for stating stannic chloride pentahydrate in mixed solution is 0.1mol/L.Other steps and parameter and specific embodiment one to three it
One is identical.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: in step 2
Temperature is reacted under conditions of being 180 DEG C.Other steps and parameter are identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: anti-in step 2
It is centrifugated after answering 20min.Other steps and parameter are identical as one of specific embodiment one to five.
Beneficial effects of the present invention are verified using following embodiment:
A kind of embodiment one: Al doping graded structure SnS2The preparation method of gas sensitive sequentially includes the following steps:
One, 0.3156g stannic chloride pentahydrate is added in 15mL ethylene glycol solution under conditions of electromagnetic agitation, to five
Mixed solution is obtained after the dissolution of water tin tetrachloride, 0.1370g thiocarbamide and 270 is added into mixed solution under the conditions of electromagnetic agitation
The ethylene glycol solution (concentration 0.1mol/L) of μ L ANN aluminium nitrate nonahydrate, magnetic agitation 20min obtain reaction solution；
Two, the reaction solution for obtaining step 1 is fitted into microwave tube, under conditions of temperature is 180 DEG C after reaction 20min
Centrifuge separation, centrifugation products therefrom first uses ethyl alcohol to clean 3~5 times, then is cleaned 3~5 times using deionized water, and it is dry to be put into vacuum
Dry case is dry, obtains Al doping graded structure SnS2Gas sensitive, wherein the doping of Al is 3%.
3%Al doping graded structure SnS is obtained using the method for embodiment one2Gas sensitive, scanning electron microscope (SEM) photograph is such as
Shown in Fig. 1, it can be seen that Al adulterates SnS2Graded structure is by SnS2The flower-like structure of nanometer sheet composition.The XRD of the material is composed
Figure is as shown in curve c in Fig. 2, with pure SnS2Compared to (the SnS of curve a), Al doping2XRD spectra in (001) crystal face diffraction
Peak is deviated to low angle direction, the mainly incorporation due to Al atom, so that (001) interplanar distance becomes larger, and other crystal faces
Peak position is almost without movement, but the remitted its fury at peak, also further illustrates the incorporation of Al so that SnS2Crystallinity die down.
HRTEM tests the doping for having also further demonstrated that Al atom, and Fig. 3 is pure SnS2HRTEM picture, (001) interplanar distance is
0.587nm；And Al adulterates SnS in Fig. 42HRTEM picture in, (001) interplanar distance be 0.642nm, illustrate the incorporation of Al only
(001) interplanar distance is set to become larger.
By the SnS of Al doping graded structure2Gas sensitive is dissolved in ethyl alcohol, is configured to the solution of 10mg/mL, ultrasound
After 10min, Al doping SnS is obtained2Dispersion liquid, Al is adulterated by SnS by the method for instillation2Dispersant liquid drop to electrode slice surface,
1h is dried under conditions of temperature is 70 DEG C, after alcohol solvent volatilization, the SnS of Al doping2It is uniform by being formed in electrode surface
Film, the electrode slice are used directly for air-sensitive performance test.
Air-sensitive performance, the sensitivity S of sensor is defined as: S=R are tested by electrochemical workstationg/Ra, wherein RaTo pass
The aerial resistance of sensor, RgIt is sensor in NO2In resistance value.Test results are shown in figure 5 for it, and test result shows
At room temperature, the SnS of the Al doping graded structure obtained using embodiment one2The gas sensor of gas sensitive preparation is being inhaled
Attached NO2After gas, the resistance value of sensor can be significantly increased, and with NO2Concentration is increasing, and the sensitivity of sensor is also bright
It is aobvious to increase, in NO2Sensitivity when concentration is 2ppm is 5.4, and pure SnS2It, can not at room temperature since conductive capability is poor
It is used as sensor.Fig. 6 is that the Al obtained using embodiment one adulterates the SnS of graded structure2The air-sensitive of gas sensitive preparation passes
The response sensitivity of sensor is with NO2The relation curve of concentration variation, NO2Concentration between 0.25~6ppm, transducer sensitivity with
NO2Concentration approximation changes linearly.
Embodiment two: the present embodiment and embodiment one the difference is that: stannic chloride pentahydrate described in step 1
Quality is 3.156g, and the quality of thiocarbamide is 1.370g, the ethylene glycol solution (concentration 0.1mol/L) of ANN aluminium nitrate nonahydrate
2.7mL.Other steps and parameter are the same as example 1.
Embodiment three: the present embodiment and embodiment one the difference is that: the second of ANN aluminium nitrate nonahydrate is added in step 1
90 μ L of glycol solution (concentration 0.1mol/L).Other steps and parameter are the same as example 1.
Example IV: the present embodiment and embodiment one the difference is that: the second of ANN aluminium nitrate nonahydrate is added in step 1
450 μ L of glycol solution (concentration 0.1mol/L).Other steps and parameter are the same as example 1.
Embodiment five: the present embodiment and embodiment one the difference is that: in step 2 under conditions of temperature is 190 DEG C
It is centrifugated after reaction 10min.Other steps and parameter are the same as example 1.
Embodiment six: the present embodiment and embodiment one the difference is that: in step 2 under conditions of temperature is 170 DEG C
It is centrifugated after reaction 30min.Other steps and parameter are the same as example 1.
The Al doping graded structure SnS that the present embodiment is obtained using embodiment one2The gas sensing of gas sensitive preparation
Device solves existing based on pure SnS2Gas sensor the problem of being unable to working and room temperature, and Al adulterates SnS2Sensor is in room temperature
Under sensitivity with higher, this is mainly due to the doping of Al atom to improve SnS2Conductive capability, while increasing point
Hierarchical organization SnS2The gas absorption active site on gas sensitive surface.
Claims (6)
1. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive, it is characterised in that Al doping graduation knot
The preparation method of structure stannic disulfide gas sensitive sequentially includes the following steps:
One, stannic chloride pentahydrate is added in ethylene glycol solution under the conditions of electromagnetic agitation, after stannic chloride pentahydrate dissolution,
Mixed solution is obtained, thiocarbamide and ANN aluminium nitrate nonahydrate, magnetic agitation 10min is added into mixed solution under the conditions of electromagnetic agitation
Reaction solution is obtained after~40min；The molar ratio of the stannic chloride pentahydrate, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:(1.5~4):
(0.01~0.05), the concentration of stannic chloride pentahydrate is 0.03~0.6mol/L in the mixed solution；
Two, the reaction solution for obtaining step 1 is fitted into microwave tube, reacts 10min under conditions of temperature is 170 DEG C~190 DEG C
It being centrifugated after~30min, centrifugation products therefrom first uses ethyl alcohol to clean 3~5 times, then is cleaned 3~5 times using deionized water,
It is dry to be put into vacuum oven, finally obtains Al doping graded structure SnS2Gas sensitive；The Al adulterates graded structure
SnS2Gas sensitive is used to prepare the nitrogen dioxide gas sensor to work at room temperature；The nitrogen dioxide gas to work at room temperature passes
Sensor is to 2ppmNO2Sensitivity be 5.4.
2. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, special
Sign is that the molar ratio of stannic chloride pentahydrate described in step 1, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:2:0.03.
3. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, special
Sign is that the molar ratio of stannic chloride pentahydrate described in step 1, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:2:0.05.
4. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, special
Sign is that the concentration of stannic chloride pentahydrate in mixed solution described in step 1 is 0.1mol/L.
5. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, special
Sign is in step 2 to react under conditions of temperature is 180 DEG C.
6. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, special
Sign is to be centrifugated after reacting 20min in step 2.
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| CN108562615B (en) * | 2018-01-02 | 2020-12-15 | 深圳市安泰安防技术有限公司 | Nitrogen dioxide leakage detection device working at room temperature |
| CN109211985B (en) * | 2018-09-01 | 2020-12-04 | 哈尔滨工程大学 | Flexible alkaline gas sensing chip and preparation method thereof |
| CN110095506A (en) * | 2019-04-04 | 2019-08-06 | 海南聚能科技创新研究院有限公司 | Au/SnS2Nitrogen dioxide gas sensor and preparation process and application |
| CN112578001B (en) * | 2019-09-30 | 2021-12-21 | 天津大学 | Gas sensitive material based on Zn-doped stannous sulfide, preparation method thereof and application thereof in methanol detection |
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