CN110095506A - Au/SnS2Nitrogen dioxide gas sensor and preparation process and application - Google Patents
Au/SnS2Nitrogen dioxide gas sensor and preparation process and application Download PDFInfo
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- CN110095506A CN110095506A CN201910268505.9A CN201910268505A CN110095506A CN 110095506 A CN110095506 A CN 110095506A CN 201910268505 A CN201910268505 A CN 201910268505A CN 110095506 A CN110095506 A CN 110095506A
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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
Abstract
The present invention relates to a kind of Au/SnS2Nitrogen dioxide gas sensor, including gas sensitive and heat the substrate, gas sensitive, which is spun on, heats the substrate surface；Gas sensitive includes golden simple substance nano particle and SnS2The nanocomposite that nanometer sheet is formed.Preparation process includes: step 1: acidic buffer being mixed with dehydrated alcohol, by SnCl2·2H2Stirring and dissolving in mixed liquor is added in O；Add Na2S2O3·5H2O and sulphur powder are poured into reaction kettle after stirring and are reacted, obtain yellow mercury oxide；By sediment undergoes washing, drying, SnS is obtained2；Step 2: by SnS2Dispersion, is added gold chloride and L-lysine is sufficiently stirred, and adds sodium citrate and carries out golden simple substance reduction；By products therefrom cleaning, drying, Au/SnS is obtained2；Step 3: by Au/SnS2Deionized water is added, is spun on after being fully ground and heats the substrate surface, it is dry, obtain Au/SnS2Nitrogen dioxide gas sensor.Preparation process of the present invention is simple, gained Au/SnS2With the application value in gas sensor is being prepared, sensor responds nitrogen dioxide sensitive, quick.
Description
Technical field
The invention belongs to nitrogen dioxide gas sensor technical fields, and in particular to a kind of Au/SnS2Nitrogen dioxide gas
Sensor and preparation process and application.
Background technique
Nitrogen dioxide gas is that one kind common are malicious pernicious gas, is mainly derived from the combustion of chemical dye in industrial production
Burning, discharge of vehicle exhaust etc. regard as a kind of most common, maximum air pollutants of harmfulness by health organization.It is long-term sudden and violent
Being exposed in the nitrogen dioxide gas environment of low concentration can be detrimental to health, such as induction pulmonary emphysema, bronchitis, asthma etc. are exhaled
Desorption system disease.The new side of such gas sensor application has been opened up in the application of low concentration Nitrogen dioxide testing in the field of medicine
To, such as the infection conditions of the diagnosis human lung tissue of the content by detecting characteristics of contaminated respiratory droplets nitrogen dioxide gas, identify anaphylaxis
Enteritis etc..Based on common nitrogen dioxide gas sensor is mainly studied with metal oxide, but this kind of gas sensing utensil
Have the shortcomings that operating temperature is high, easy to reunite, poor selectivity, its gas-sensitive property is caused to be difficult to reach requirement.
In recent years, with the big heat that two-dimension nano materials are studied, stannic disulfide nano material is in field of semiconductor materials
It is received more and more attention in research.The special stratiform two-dimensional structure of stannic disulfide nano material, stable physical chemistry are special
Property, so that it is detected low concentration nitrogen dioxide gas under cryogenic and shows good gas-sensitive property.Although stannic disulfide gas
The nitrogen dioxide gas for detecting low concentration under cryogenic may be implemented in body sensor, but longer response recovery time is still
Constrain extensive use of such sensor in daily life and production.Currently, how to shorten nitrogen dioxide gas sensor
Response recovery time, realize fast and accurately detection be still this field research hot and difficult issue.
Summary of the invention
In consideration of it, the present invention provides a kind of Au/SnS2Nitrogen dioxide gas sensor can accelerate dioxy under cryogenic
Change absorption and the desorption of nitrogen and nanocomposite surface, and shows excellent air-sensitive performance.
Technical solution of the present invention:
Au/SnS2Nitrogen dioxide gas sensor, including gas sensitive and heat the substrate, the gas sensitive is spun on institute
The surface heated the substrate is stated, coating thickness is 50 μm -100 μm；The gas sensitive includes golden simple substance nano particle and SnS2It receives
The nanocomposite that rice piece is formed.Spin coating is rotary coating, and gas sensitive is spun on to the surface heated the substrate, Ke Yibao
The thickness for demonstrate,proving coating is uniform, can more prepare the excellent nitrogen dioxide gas sensor of air-sensitive performance.
The SnS as a preferred technical solution,2The size range of nanometer sheet is 200nm-600nm.
The size range of the golden simple substance nano particle is 5nm-10nm as a preferred technical solution,.
It is described as a preferred technical solution, to heat the substrate as silicon substrate micro-hotplate；The front that heats the substrate is golden interdigital
Electrode, the back side have resistive heater；The heating temperature range of the resistive heater is 25 DEG C -350 DEG C.
The Au/SnS as a preferred technical solution,2Nanocomposite passes through solvent-thermal method-sedimentation two-step method system
It is standby.
Au/SnS2The preparation process of nitrogen dioxide gas sensor, comprising the following steps:
Step 1: using the mixed liquor of acidic buffer and dehydrated alcohol as solvent, by SnCl2·2H2Mixed liquor is added in O
In, for magnetic agitation until being completely dissolved, solution is colorless and transparent；Na is added later2S2O3·5H2O and sulphur powder, magnetic agitation
It pours into reaction kettle and is reacted after 30min-40min, reaction temperature is 185 DEG C -200 DEG C, and reaction time 6h-15h is obtained
Yellow mercury oxide；Gained yellow mercury oxide is used into deionized water, carbon disulfide, washes of absolute alcohol 3-6 times respectively, collects yellow
Sediment is put into drying in drying box, and two-dimensional SnS is prepared2Nanometer sheet；
Step 2: by the resulting SnS of step 12Nanometer sheet is scattered in deionized water, is separately added into gold chloride and L- relies
20min-30min is sufficiently stirred in propylhomoserin, and sodium citrate is then added dropwise and carries out golden simple substance nano particle reduction, reduction process is held
Continuous 15min-20min；Products therefrom is used to deionized water and washes of absolute alcohol 3-6 times respectively, puts in a drying box drying, is made
It is standby to obtain Au/SnS2Nanocomposite；
Step 3: by the resulting Au/SnS of step 22Deionized water is added in nanocomposite, is fully ground and is tuned into paste
Shape is spun on the surface heated the substrate, puts in a drying box 80 DEG C of dry 4h-6h, Au/SnS is prepared2Nitrogen dioxide
Gas sensor.
As a preferred technical solution, in the step 1, the pH value of acidic buffer is 3；Acidic buffer with it is anhydrous
The volume ratio of ethyl alcohol is 4:1；Sulphur powder, SnCl2·2H2O、Na2S2O3·5H2The mass ratio of O is 1:1.4:7.7.
The drying temperature of the step 1 and the step 2 is 80 DEG C as a preferred technical solution, drying time
For 12h-14h.
As a preferred technical solution, in the step 2, L-lysine, gold chloride, sodium citrate molar ratio be 1:
1:10。
The invention also discloses the Au/SnS being prepared using the preparation process2Nanocomposite is preparing gas
Application in quick element.
Compared with prior art, the invention has the benefit that
1. the present invention realizes the technique of precious metal doping metal sulfide using two-step method, raw material environmental protection prepares work
Skill is simple, is a kind of precious metal doping preparation process that can be suitble to extensive green production.
2. Au/SnS prepared by the present invention2Nanocomposite makes two-dimensional SnS2Nano material and golden simple substance nano particle
Synergistic effect has been played, application limitation of the single metal sulfide in gas sensor domain is overcome.Using Au/SnS2Nanometer
The nitrogen dioxide gas sensor operating temperature that composite material is prepared is 120 DEG C, and the response time is 34s at such a temperature,
Show short to low concentration nitrogen dioxide gas response time gas-sensitive property in low temperature detection environment.Meanwhile nitrogen dioxide
The integrated application of electronic component also may be implemented in the lower operating temperature of gas sensor.
It heats the substrate 3. of the invention as silicon substrate micro-hotplate, by by Au/SnS2It is micro- that nanocomposite is spin-coated on silicon substrate
The new micro nitrogen dioxide gas that low in energy consumption, heating response fastly, is easily integrated with other microelectronic components is prepared on hot plate to pass
Sensor.
Detailed description of the invention
Fig. 1 is the Au/SnS that the embodiment of the present invention 3 obtains2The Flied emission electron-microscope scanning of nanocomposite microstructure
Figure；
Fig. 2 is the Au/SnS that the embodiment of the present invention 3 obtains2The Flied emission electron-microscope scanning of nanocomposite microstructure
EDS figure；
Fig. 3 is the Au/SnS that the embodiment of the present invention 3 obtains2The HTEM of nanocomposite microstructure schemes；
Fig. 4 is the obtained nitrogen dioxide gas sensor of the embodiment of the present invention 3 in 120 DEG C of resistance to 8ppm nitrogen dioxide
Change curve；
Fig. 5 is the Au/SnS of the different doping ratios of the present invention2The nitrogen dioxide gas sensor of nanocomposite preparation
In 120 DEG C of response comparison diagrams to 8ppm nitrogen dioxide；
Fig. 6 is that the nitrogen dioxide gas sensor that the embodiment of the present invention 3 obtains interferes nitrogen dioxide and five kinds at 120 DEG C
The response comparison diagram of gas.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Below in conjunction with attached drawing and technical solution, a specific embodiment of the invention is further illustrated.
Embodiment 1
Au/SnS2Nitrogen dioxide gas sensor, including gas sensitive and heat the substrate, gas sensitive is spun on heating base
The surface of plate, coating thickness are 100 μm；Gas sensitive ingredient is golden simple substance nano particle and SnS2The nanometer that nanometer sheet is formed is multiple
Condensation material.Au/SnS2Nanocomposite passes through solvent-thermal method-sedimentation two-step method preparation；SnS2The size of nanometer sheet is
600nm；The size of golden simple substance nano particle is 10nm.Preparation process the following steps are included:
Step 1:, will using the mixed liquor of the 36.4mL acidic buffer of pH=3 and 9.12mL dehydrated alcohol as solvent
379.04mg SnCl2·2H2O is added in mixed liquor, and for magnetic agitation until being completely dissolved, solution is colorless and transparent；Later plus
Enter 2084.81mg Na2S2O3·5H2O and 270.76mg sulphur powder is poured into reaction kettle after magnetic agitation 40min and is reacted, instead
Answering temperature is 185 DEG C, and reaction time 15h obtains yellow mercury oxide；Gained yellow mercury oxide is used into deionized water, two respectively
Nitric sulfid, washes of absolute alcohol 3-6 times, removal unreacted complete sulphur powder and other impurities collect yellow mercury oxide and are put into drying
80 DEG C of dry 14h, are prepared two-dimensional SnS in case2Nanometer sheet；
Step 2: by the resulting SnS of step 12Nanometer sheet is scattered in deionized water, and it is (dense to be separately added into 5mL gold chloride
Degree is that 30min is sufficiently stirred in 0.01mol/L) and 5mL L-lysine (concentration 0.01mol/L), and 0.5mL is then added dropwise
Sodium citrate (concentration 0.1mol/L) carries out golden simple substance nano particle reduction, and reduction process continues 20min；By products therefrom point
Not Yong 3-6 removal impurity of deionized water and washes of absolute alcohol, put in a drying box 80 DEG C of dry 14h, Au/ be prepared
SnS2Nanocomposite；
Step 3: by the resulting Au/SnS of step 22Deionized water is added in nanocomposite, is fully ground and is tuned into paste
Shape is spun on the surface heated the substrate, and heating the substrate as front is golden interdigital electrode, and silicon substrate of the back side with resistive heater is micro-
Hot plate, the heating temperature range of resistive heater are 25 DEG C -350 DEG C；Later, 80 DEG C of dry 6h are put in a drying box, are prepared into
To Au/SnS2Nitrogen dioxide gas sensor.
Embodiment 2
Au/SnS2Nitrogen dioxide gas sensor, including gas sensitive and heat the substrate, gas sensitive is spun on heating base
The surface of plate, coating thickness are 50 μm；Gas sensitive is the Au/SnS of 0.1% gold medal simple substance nano particle doping preparation2Nanometer is multiple
Condensation material.Au/SnS2Nanocomposite passes through solvent-thermal method-sedimentation two-step method preparation；SnS2The size of nanometer sheet is
200nm；The size of golden simple substance nano particle is 5nm.Preparation process the following steps are included:
Step 1:, will using the mixed liquor of the 31.6mL acidic buffer of pH=3 and 8.33mL dehydrated alcohol as solvent
371.67mg SnCl2·2H2O is added in mixed liquor, and for magnetic agitation until being completely dissolved, solution is colorless and transparent；Later plus
Enter 2066.67mg Na2S2O3·5H2O and 266.67mg sulphur powder is poured into reaction kettle after magnetic agitation 30min and is reacted, instead
Answering temperature is 200 DEG C, and reaction time 6h obtains yellow mercury oxide；Gained yellow mercury oxide is used into deionized water, two sulphur respectively
Change carbon, washes of absolute alcohol 3-6 times, removal unreacted complete sulphur powder and other impurities collect yellow mercury oxide and be put into drying box
Interior 80 DEG C dry 12h, are prepared two-dimensional SnS2Nanometer sheet；
Step 2: by the resulting SnS of step 12Nanometer sheet weighs 50mg, is scattered in 15mL deionized water, is separately added into
20min is sufficiently stirred in 0.4mL gold chloride (concentration 0.01mol/L) and 0.4mL L-lysine (concentration 0.01mol/L), so
After 50 μ L sodium citrates (concentration 0.1mol/L) be added dropwise carry out golden simple substance nano particle reduction, reduction process is lasting
15min；Products therefrom is used to 3-6 removal impurity of deionized water and washes of absolute alcohol respectively, 80 DEG C is put in a drying box and does
Dry 12h, is prepared Au/SnS2Nanocomposite；
Step 3: by the resulting Au/SnS of step 22Deionized water is added in nanocomposite, is fully ground and is tuned into paste
Shape is spun on the surface heated the substrate, and heating the substrate as front is golden interdigital electrode, and silicon substrate of the back side with resistive heater is micro-
Hot plate, the heating temperature range of resistive heater are 25 DEG C -350 DEG C；Later, 80 DEG C of dry 4h are put in a drying box, are prepared into
The Au/SnS adulterated to 0.1% gold medal simple substance nano particle2Nitrogen dioxide gas sensor.
Embodiment 3
The present embodiment and embodiment 2 the difference is that: be added in step 2 2mL gold chloride, 2mL L-lysine,
0.2mL sodium citrate, remaining step, parameter are same as Example 2.According to the present embodiment, 0.5% gold medal simple substance can be prepared
The Au/SnS of nano particle doping2Nitrogen dioxide gas sensor.
Fig. 1 gives Au/SnS manufactured in the present embodiment2The Flied emission electron-microscope scanning figure of nanocomposite microstructure；
Fig. 2 gives Au/SnS manufactured in the present embodiment2The Flied emission electron-microscope scanning EDS of nanocomposite microstructure schemes, can be with
It learns and contains tri- kinds of elements of Au, Sn, S in prepared nanocomposite；Fig. 3 gives Au/SnS manufactured in the present embodiment2
The HTEM of nanocomposite microstructure schemes, further illustrate the nanocomposite be by golden simple substance nano particle and
SnS2Nanometer sheet is compounded to form.
Fig. 4 gives gas sensor manufactured in the present embodiment in 120 DEG C of resistance variations figures to 8ppm nitrogen dioxide.From
It, can as can be seen that gas sensor of the invention has very high response sensitivity to nitrogen dioxide at the working temperature in figure
Quickly nitrogen dioxide is responded.Fig. 6 give gas sensor manufactured in the present embodiment 120 DEG C to nitrogen dioxide and
The response comparison diagram of five kinds of interference gas.It can be seen from the figure that gas sensor of the invention is at the working temperature to dioxy
Change nitrogen and shows good gas sensing performance and excellent selection performance.
Embodiment 4
According to the Au/SnS for the Bu Tong golden simple substance nano particle doping ratio that embodiment 2 is prepared with embodiment 32Gas
Sensor is placed in dynamic test box, and senor operating temperature is 120 DEG C, then introduces nitrogen dioxide gas.Pass through multimeter
Measurement sensor is in air and in the sound using air as the resistance variations under the 8ppm nitrogen dioxide atmosphere of background, as sensor
Induction signal.Fig. 5 gives the Au/SnS of different doping ratios2The gas sensor of nanocomposite preparation is right at 120 DEG C
The response comparison diagram of 8ppm nitrogen dioxide.It can be seen from the figure that the Au/SnS of 0.5% gold medal simple substance nano particle doping preparation2
Gas sensor is best to the response sensitivity of nitrogen dioxide.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1.Au/SnS2Nitrogen dioxide gas sensor, including gas sensitive and heat the substrate, which is characterized in that the gas sensitive
It is spun on the surface heated the substrate, coating thickness is 50 μm -100 μm；The gas sensitive includes golden simple substance nano particle
And SnS2The nanocomposite that nanometer sheet is formed.
2. Au/SnS according to claim 12Nitrogen dioxide gas sensor, which is characterized in that the SnS2Nanometer sheet
Size range is 200nm-600nm.
3. Au/SnS according to claim 12Nitrogen dioxide gas sensor, which is characterized in that the gold simple substance nanometer
The size range of grain is 5nm-10nm.
4. Au/SnS according to claim 1 to 32Nitrogen dioxide gas sensor, which is characterized in that the heating base
Plate is silicon substrate micro-hotplate；For golden interdigital electrode, the back side has resistive heater in the front that heats the substrate；The resistive heater
Heating temperature range be 25 DEG C -350 DEG C.
5. Au/SnS according to claim 12Nitrogen dioxide gas sensor, which is characterized in that the Au/SnS2Nanometer
Composite material passes through solvent-thermal method-sedimentation two-step method preparation.
6. Au/SnS according to claim 12The preparation process of nitrogen dioxide gas sensor, which is characterized in that including with
Lower step:
Step 1: using the mixed liquor of acidic buffer and dehydrated alcohol as solvent, by SnCl2·2H2O is added in mixed liquor, magnetic
Until being completely dissolved, solution is colorless and transparent for power stirring；Na is added later2S2O3·5H2O and sulphur powder, magnetic agitation 30min-
It pours into reaction kettle and is reacted after 40min, reaction temperature is 185 DEG C -200 DEG C, reaction time 6h-15h, and it is heavy to obtain yellow
Starch；Gained yellow mercury oxide is used into deionized water, carbon disulfide, washes of absolute alcohol 3-6 times respectively, collects yellow mercury oxide
It is put into drying in drying box, two-dimensional SnS is prepared2Nanometer sheet；
Step 2: by the resulting SnS of step 12Nanometer sheet is scattered in deionized water, is separately added into gold chloride and L-lysine fills
Divide stirring 20min-30min, sodium citrate is then added dropwise and carries out golden simple substance nano particle reduction, reduction process is lasting
15min-20min；Products therefrom is used to deionized water and washes of absolute alcohol 3-6 times respectively, puts in a drying box drying, is prepared
Obtain Au/SnS2Nanocomposite；
Step 3: by the resulting Au/SnS of step 22Deionized water is added in nanocomposite, is fully ground and is tuned into paste, spin coating
In the surface heated the substrate, 80 DEG C of dry 4h-6h are put in a drying box, Au/SnS is prepared2Nitrogen dioxide gas passes
Sensor.
7. Au/SnS according to claim 62The preparation process of nitrogen dioxide gas sensor, which is characterized in that the step
In rapid one, the pH value of acidic buffer is 3；The volume ratio of acidic buffer and dehydrated alcohol is 4:1；Sulphur powder, SnCl2·2H2O、
Na2S2O3·5H2The mass ratio of O is 1:1.4:7.7.
8. Au/SnS according to claim 6 or 72The preparation process of nitrogen dioxide gas sensor, which is characterized in that institute
The drying temperature for stating step 1 and the step 2 is 80 DEG C, drying time 12h-14h.
9. Au/SnS according to claim 82The preparation process of nitrogen dioxide gas sensor, which is characterized in that the step
In rapid two, L-lysine, gold chloride, sodium citrate molar ratio be 1:1:10.
10. Au/SnS according to claim 62The Au/SnS that the preparation process of nitrogen dioxide gas sensor is prepared2
Nanocomposite is preparing the application in gas sensor.
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| CN111157589A (en) * | 2020-01-08 | 2020-05-15 | 大连理工大学 | Gold-modified flower-like SnS2Nitrogen dioxide gas sensor and preparation method thereof |
| CN111157578A (en) * | 2019-12-30 | 2020-05-15 | 电子科技大学 | Nitrogen dioxide sensor based on organic thin film transistor and preparation method thereof |
| CN113049645A (en) * | 2021-03-15 | 2021-06-29 | 吉林大学 | Based on two-dimentional stratiform SnS2NO of nanoflower semiconductor material2Gas sensor and preparation method thereof |
| CN114264702A (en) * | 2021-12-24 | 2022-04-01 | 安徽工业大学 | MXene @ Au self-repairing hydrogel gas-sensitive material, gas-sensitive element, gas sensor, preparation method and application of gas-sensitive element |
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| CN113049645A (en) * | 2021-03-15 | 2021-06-29 | 吉林大学 | Based on two-dimentional stratiform SnS2NO of nanoflower semiconductor material2Gas sensor and preparation method thereof |
| CN114264702A (en) * | 2021-12-24 | 2022-04-01 | 安徽工业大学 | MXene @ Au self-repairing hydrogel gas-sensitive material, gas-sensitive element, gas sensor, preparation method and application of gas-sensitive element |
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Application publication date: 20190806 |