CN109970108A - A kind of gas sensor and preparation method thereof based on nanometer nickel sulfide composite material - Google Patents
A kind of gas sensor and preparation method thereof based on nanometer nickel sulfide composite material Download PDFInfo
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- CN109970108A CN109970108A CN201910297177.5A CN201910297177A CN109970108A CN 109970108 A CN109970108 A CN 109970108A CN 201910297177 A CN201910297177 A CN 201910297177A CN 109970108 A CN109970108 A CN 109970108A
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- 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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Abstract
The invention belongs to gas sensor technical fields, are related to a kind of gas sensor and preparation method thereof based on nanometer nickel sulfide composite material；The Al of the sensor2O3NiS nanocomposite films, the preparation process of the sensor are as follows: first by Ni (NO are coated on insulating ceramics tube outer surface and annular gold electrode3)2NiS nanofiber is prepared by the method that electrostatic spinning technique combination hydrogen sulfide is calcined, metallic compound is prepared into metal oxide semiconductor nanofiber by electrostatic spinning technique again, then by NiS and metal oxide semiconductor nanocomposite mixed calcining and solid-state grinding preparation NiS nanocomposite, NiS nanocomposite is finally ground to the air-sensitive cream that paste is made, air-sensitive cream is coated on gas sensor, the gas sensor of nanometer nickel sulfide composite material is made；The gas sensor is good to ethyl alcohol progress response performance, and high sensitivity, selectivity is good, has quick response and regeneration rate, and have good long-time stability.
Description
Technical field:
The invention belongs to gas sensor technical fields, are related to the gas sensor of a kind of high gas response and selectivity, special
It is not a kind of gas sensor and preparation method thereof based on nanometer nickel sulfide composite material.
Background technique:
Ethyl alcohol is a kind of colourless liquid, there is aroma, and vapour pressure reaches 5.33kPa/19 DEG C, and fusing point is 114.1 DEG C, boiling point 78.3
DEG C, most organic solvents such as ether, chloroform, glycerol are miscible in, it can be miscible with arbitrary proportion with water；The density of opposite water is
0.79, the density of relative atmospheric is 1.59.It is a kind of flammable liquid, is mainly used for alcoholic beverage industry, organic synthesis, disinfection and use
Make solvent, is widely used in the every aspect of life.But anything has dual character.Since ethyl alcohol is volatile, steam
Explosive mixture can be formed with air, meets open fire, high thermal energy easily causes combustion explosion.It contacts and chemically reacts with oxidant
Or cause to burn.In the scene of a fire, heated container has explosion danger.Its steam is heavier than air, can be diffused into quite in lower
Remote place, chance open fire, which can draw, to strile-back.Alcohol gas easily pass through sucking, eat, the approach such as percutaneous absorbtion enter human body.Make
Then press down for a kind of common central nervous system depressant once it can cause nervous system excited first into human body
System.Human body, which sucks excessive ethyl alcohol, will appear the loss of consciousness, pupil expansion, breathes irregular, shock, mental and physical efforts circulatory failure and exhale
Inhale the life dangers such as stopping；Moreover, Long Term Contact high concentration this product can cause nose, eye, mucosal irritation symptom in production, and
Headache, it is dizzy, tired, emotional, tremble, nausea etc..More serious person can cause polyneuropathy, chronic gastritis, fatty liver,
Cirrhosis, cardiac damage and Organic mental disease etc..Long-term skin contact can cause drying, furfur, chap and dermatitis.
Based on the above analysis, the detection of alcohol gas is particularly important.Related data shows that the country is to ethyl alcohol at present
The live monitoring method for emergency of gas has gas detection tube method, portable gas chromatography method and gas speed test tube (Beijing labour protection institute
Product), Laboratory Monitoring method mainly has gas chromatography and potassium dichromate method, though these methods can detect alcohol gas
In the presence of, but its timeliness is poor, sensitivity is lower.Therefore, it is necessary to seek a kind of with highly sensitive and stable property second
Alcohol gas detection substance, convenient more Shangdi guarantee the life security of staff and laboratory teachers and students.
In the prior art, the Chinese patent of Publication No. CN106053556B discloses a kind of heterogeneous based on ZnO/SnO2
The high sensitivity of structural composite material and the alcohol gas sensor and preparation method thereof of low-detection lower limit, the patent use two steps
ZnO/SnO is made in hydro-thermal method2Composite material sensitive material, utilizes SnO2It is formed by heterojunction structure between ZnO and the two is right
The concerted catalysis of ethyl alcohol acts on, and then effectively improves gas sensor for the gas-sensitive property of ethyl alcohol；Publication No.
The Chinese patent of CN106770493A discloses a kind of CNTs@α-Fe2O3The acetone gas sensor of heterojunction composite and its
Preparation method, by outer surface band, there are two the oxide aluminium earthenware outer substrates of cyclic annular gold electrode parallel to each other and discrete, painting
It the metal oxide semiconductor gas sensitive material that overlays on oxide aluminium earthenware outer outer substrate surface and gold electrode and is placed in
Nichrome heating coil in ceramics pipe outer forms, and platinum filament wire is had on each gold electrode；Sensitive material is CNTs
With α-Fe2O3The compound hetero-junctions graded structure nano material of nanometer rods, the test result of gas-sensitive property show the gas sensing
Device, which carries out detection to low concentration acetone, has splendid long-time stability.
Nickel sulfide crystal is in brass yellow, and powder is in black；Density is 5.3-5.6g/mL, 25/4 DEG C.Fusing point is 797
℃；The advantages such as its with good stability, excellent chemical property, for preparing a kind of gas with long-time stability
Sensor has proper value very much, to solve the disadvantage that existing gas sensor timeliness is poor, sensitivity is lower, endeavours to seek one
Nanometer of the kind based on nickel sulfide meets the gas-detecting device of material.
Summary of the invention:
It is an object of the invention to overcome disadvantage of the existing technology, exist for existing room monitoring method of testing, in time
The disadvantage that property is poor, sensitivity is lower designs a kind of gas sensor based on nanometer nickel sulfide composite material and its preparation side
Method.
To achieve the goals above, the gas sensor of the present invention based on nanometer nickel sulfide composite material, master
Body structure includes the Al that 2 discrete annular gold electrodes are had by outer surface2O3Ceramics pipe outer passes through Al2O3Ceramics pipe outer
Internal nickel-cadmium coil and it is coated in Al2O3Sensitive material film on insulating ceramics tube outer surface and annular gold electrode
It constitutes, sensitive material is NiS nanocomposite.
The preparation method of gas sensor of the present invention based on nanometer nickel sulfide composite material includes: to receive NiS
Nano composite material thoroughly grinds the air-sensitive cream that paste is made in the agate mortar, and air-sensitive cream is then uniformly coated on gas and is passed
The Al of sensor2O3It on ceramic tube, is finally dried in vacuum overnight at 60 DEG C, the gas sensing of nanometer nickel sulfide composite material is made
Device.
The specific preparation process of NiS nanocomposite of the present invention are as follows:
(1) NiS nanofiber is prepared: by Ni (NO3)2The method preparation calcined by electrostatic spinning technique combination hydrogen sulfide
NiS nanofiber；
(2) it prepares metal oxide semiconductor nanofiber: metallic compound is partly led by electrostatic spinning technique preparation
Body metal oxide nanofibres；
(3) NiS nanocomposite is prepared: the matter by NiS and metal oxide semiconductor nanocomposite by 1/2-4
Amount proportion mixing carries out calcining and solid-state grinding preparation NiS nanocomposite.
Gas sensor of the present invention based on nanometer nickel sulfide composite material is specially NiS@In2O3Gas sensing
Device, NiS@In2O3The main structure of gas sensor includes the Al that 2 discrete annular gold electrodes are had by outer surface2O3Insulation
Ceramic tube passes through Al2O3Nickel-cadmium coil inside ceramics pipe outer and it is coated in Al2O3Insulating ceramics tube outer surface and
Sensitive material film on annular gold electrode is constituted, and sensitive material is NiS@In2O3Nanocomposite.
NiS@In of the present invention2O3The preparation method of gas sensor, the specific process steps are as follows:
Step 1: preparation NiS nanofiber: by Ni (NO3)2The method calcined by electrostatic spinning technique combination hydrogen sulfide
Prepare NiS nanofiber；Specific step is as follows:
(1) PVP of 2.2g is dissolved in the DMF solvent of 20ml, and by stirring to obtain homogeneous solution；
(2) Ni (NO of 2.0g is added to homogeneous solution again3)2, mixture magnetic agitation 12 hours at room temperature are made
Viscosity solution；
(3) then viscosity solution is fitted into the 10ml syringe with No. 22 needle points and carries out electrostatic spinning, electrostatic spinning
When apply voltage and be maintained at 17kV, injection flow control is 0.8ml/h, and the distance of needle tip to collector is 20cm, Static Spinning
Fiber mat is made after silk；
(4) obtained fiber mat is heated to 160 DEG C in air with the rate of heat addition of 1 DEG C/min and keeps the temperature 2 hours,
Stable fiber mat is made；
(5) finally, the H for being 99.999% in gas purity by stable fiber mat2With the heating of 1 DEG C/min in S atmosphere
Rate is heated to 700 DEG C and calcines 3-5 hours, and NiS nanofiber is made；
Step 2: preparation In2O3Nanofiber: by In (NO3)3·H2O prepares In by electrostatic spinning technique2O3Nanowire
Dimension；Specific step is as follows:
(1) by the In (NO of 0.5g3)3·H2O is added in the DMF solvent of 20ml, and is vigorously stirred 6 in a reagent bottle
Hour, In (NO is made3)3Mixture；
(2) PVP of 0.25g is dissolved in 3mL ethyl alcohol and is vigorously stirred in another reagent bottle 6 hours, PVP is made
Mixture；
(3) by In (NO3)3Mixture and PVP mixture mix by stirring together, are then charged into No. 22 needle points
10ml syringe in carry out electrostatic spinning, when electrostatic spinning, applies voltage and is maintained at 17kV, and injection flow control is 0.8ml/
H, the distance of needle tip to collector are 20cm, and nanofiber presoma is made；
(4) after electrostatic spinning, nanofiber presoma is heated to 160 DEG C in air with the rate of heat addition of 1 DEG C/min
And keep the temperature 2 hours, be then heated to 500 DEG C in air with the rate of heat addition of 1 DEG C/min and calcine 4 hours, In is made2O3It receives
Rice fiber；
Step 3: preparation NiS@In2O3Nanocomposite: by NiS and In2O3Nanofiber stoichiometrically matches mixed
Conjunction carries out calcining and solid-state grinding preparation NiS@In2O3Nanocomposite, the specific steps are as follows:
(1) firstly, by calcined NiS nanofiber and In2O3Nanofiber stoichiometrically matches at high operating temperatures
It is uniformly ground after mixing 1 hour；
(2) then, mixture is annealed in Ar gas 400 DEG C, is wherein 5% containing mass fraction in Ar gas
H2；
(3) finally, keeping the temperature 2 hours at 400 DEG C so that NiS@In2O3Nano-complex crystallization, is made after heat preservation
NiS@In2O3Nanocomposite；
The NiS nanofiber and In2O3The stoichiometric of nanofiber mixing prepares NiS@using quality proportioning
In2O3Nanocomposite, by NiS nanofiber and In2O360%NiS@is made according to the quality proportioning of 6:4 in nanofiber
40%In2O3, by NiS nanofiber and In2O370%NiS@30%In is made according to the quality proportioning of 7:3 in nanofiber2O3；It will
NiS nanofiber and In2O380%NiS@20%In is made according to the quality proportioning of 8:2 in nanofiber2O3；
Step 4: NiS@In2O3The preparation of gas sensor: by NiS@In2O3Nanocomposite is thorough in the agate mortar
The air-sensitive cream that paste is made is ground at bottom, then air-sensitive cream is uniformly coated on to the Al of gas sensor2O3On ceramic tube, finally
It is dried in vacuum overnight at 60 DEG C, NiS@In is made2O3Gas sensor.
NiS@In of the present invention2O3The raw material components of nanocomposite include: polyvinylpyrrolidone (PVP, Mw
=1500000), nickel nitrate hexahydrate (Ni (NO3) 26H2O), indium nitrate trihydrate (In (NO3)3·H2), O N, N- bis-
Methylformamide (DMF).
The present invention is to preparing above-mentioned three groups of NiS@In2O3Gas sensor is tested for the property, by In2O3In agate mortar
In thoroughly grind be made paste air-sensitive cream；Then air-sensitive cream is successively uniformly coated on gas sensor Al2O3On ceramic tube 1,
And be dried in vacuum overnight at 60 DEG C, In is made2O3Gas sensor, by In2O3Gas sensor and NiS@In2O3Gas sensing
Device compares experiment test performance；Here, the gas response amplitude of gas sensor is defined as S=Ra/Rg, wherein RaIt is empty
Resistance in gas, RgIt is the resistance under test gas, in addition, response or recovery time are the gas after applying or closing gas
Sensor output reaches its saturation state and spends time taking 90%.
By In2O3Gas sensor, 60%NiS@40%In2O3Gas sensor, 70%NiS@30%In2O3Gas sensing
Device and 80%NiS@20%In2O3Gas sensor carries out response measurement to 100ppm ethyl alcohol under 25 DEG C of -350 DEG C of different temperatures,
At 300 DEG C, mass ratio NiS:In2O3The 70%NiS@30%In of=7:32O3Gas sensor carries out 100ppm ethyl alcohol
Response performance is best.Therefore relevant test will be based on 70%NiS@30%In2O3Gas sensor carries out.
The present invention is by 70%NiS@30%In2O3Gas sensor is at 300 DEG C to 5ppm to 500ppm difference alcohol gas
Dynamic response and recovery characteristics are tested in concentration: with the increase of concentration of alcohol, 70%NiS@30%In2O3Gas sensor
Response sharply increases；When concentration of alcohol reaches 500ppm, response moves closer to saturation state, shows 70%NiS@30%
In2O3Gas sensor is sensitive to ethanol gas concentration variation sensing.
The present invention is by 70%NiS@30%In2O3Gas sensor and In2O3Gas sensor is right at 300 DEG C respectively
100ppm ethyl alcohol carries out cyclical stability test, as the result is shown: 70%NiS@30%In2O3Response (the R of gas sensora/Rg
=10.3) it is much higher than In2O3Response (the R of gas sensora/Rg=4.2)；This shows NiS@In2O3Nanocomposite surface
On the nano particle that echos it is more, cause specific surface area than increasing.
The present invention is by 70%NiS@30%In2O3Gas sensor carries out response characteristic survey to 100ppm ethyl alcohol at 300 DEG C
It tries, as the result is shown 70%NiS@30%In2O3The response time and recovery time of gas sensor are respectively 9s and 22s, this shows
70%NiS@30%In2O3Gas sensor has quick response and regeneration rate to alcohol gas.
The present invention tests display, 70%NiS@30%In by the 1st day to 60 days invariant feature2O3Gas sensor pair
The response amplitude of alcohol gas is always held at 10 or so, illustrates NiS@In2O3Gas sensor has good steady in a long-term
Property.
The present invention is by by 70%NiS@30%In2O3NiS@In2O3Gas sensor and In2O3Gas sensor is 300
Response characteristic test, 70%NiS@30%In are carried out to 100ppm different type gas at DEG C2O3NiS@In2O3Gas sensor
10.3 are reached to the gas response amplitude of 100ppm alcohol gas, illustrates NiS@In2O3Gas sensor has alcohol gas good
Good selectivity.
NiS@In of the present invention2O3The process flow of gas sensor detection alcohol gas are as follows:
Firstly, working as NiS@In2O3When gas sensor is in air, NiS@In2O3Electronics in material is from N-shaped In2O3
It is shifted to p-type NiS nanofiber, p-type NiS nanofiber and N-shaped In2O3Resistance increases at contact interface；
Then, when introducing ethanol molecule, CH3CH2OH will increase N-shaped In2O3In electron amount and reduce p-type NiS and receive
Hole concentration in rice fiber, p-type NiS nanofiber and N-shaped In2O3Resistance reduces at contact interface；
Finally, passing through NiS@In2O3Ethyl alcohol is dense in gas sensor resistance value or the significant changes of current value characterization air
NiS@In is realized in the variation of degree2O3Alarm function of the gas sensor to alcohol gas.
Compared with prior art, 70%NiS@30%In prepared by the present invention2O3Gas sensor carries out 100ppm ethyl alcohol
Response performance is best, high sensitivity, has quick response and regeneration rate, has good selectivity to alcohol gas, and
With good long-time stability.
Detailed description of the invention:
Fig. 1 is NiS@In of the present invention2O3The principle schematic diagram of gas sensor.
Fig. 2 is In of the present invention2O3Gas sensor and NiS@In2O3Gas sensor is right at different temperatures
100ppm ethyl alcohol response amplitude line chart.
Fig. 3 is NiS@In of the present invention2O3And In2O3Gas sensor is at 300 DEG C to 5ppm to 500ppm ethyl alcohol
The dynamic response and recovery characteristics curve graph of gas degree.
Fig. 4 is 70%NiS@30%In of the present invention2O3Gas sensor and In2O3Gas sensor is respectively 300
To 100ppm alcohol stability trial curve figure at DEG C.
Fig. 5 is 70%NiS@30%In of the present invention2O3Gas sensor carries out 100ppm ethyl alcohol at 300 DEG C
Resonse characteristic figure.
Fig. 6 is 70%NiS@30%In of the present invention2O3Response of the gas sensor in 1-60 days to alcohol gas
Amplitude line chart.
Fig. 7 is 70%NiS@30%In of the present invention2O3NiS@In2O3Gas sensor and In2O3Gas sensor
To 100ppm different type gas response characteristic histogram at 300 DEG C.
Fig. 8 is that the present invention relates to In2O3Meet front and back fermi level variation schematic illustration with p-type NiS nanofiber.
Specific embodiment:
The invention will be further described by way of example and in conjunction with the accompanying drawings.
Embodiment 1:
The gas sensor based on nanometer nickel sulfide composite material that the present embodiment is related to, main structure include by appearance
Face has the Al of 2 discrete annular gold electrodes2O3Ceramics pipe outer passes through Al2O3Nickel-cadmium line inside ceramics pipe outer
Enclose and be coated in Al2O3Sensitive material film on insulating ceramics tube outer surface and annular gold electrode is constituted, and sensitive material is
NiS nanocomposite.
The preparation method for the gas sensor based on nanometer nickel sulfide composite material that the present embodiment is related to includes: by NiS
Nanocomposite thoroughly grinds the air-sensitive cream that paste is made in the agate mortar, and air-sensitive cream is then uniformly coated on gas
The Al of sensor2O3It on ceramic tube, is finally dried in vacuum overnight at 60 DEG C, the gas that nanometer nickel sulfide composite material is made passes
Sensor.
The specific preparation process for the NiS nanocomposite that the present embodiment is related to are as follows:
(1) NiS nanofiber is prepared: by Ni (NO3)2The method preparation calcined by electrostatic spinning technique combination hydrogen sulfide
NiS nanofiber；
(2) it prepares metal oxide semiconductor nanofiber: metallic compound is partly led by electrostatic spinning technique preparation
Body metal oxide nanofibres；
(3) NiS nanocomposite is prepared: the matter by NiS and metal oxide semiconductor nanocomposite by 1/2-4
Amount proportion mixing carries out calcining and solid-state grinding preparation NiS nanocomposite.
Embodiment 2
The gas sensor based on nanometer nickel sulfide composite material that the present embodiment is related to is specially NiS@In2O3Gas passes
Sensor, NiS@In2O3The main structure of gas sensor includes the Al that 2 discrete annular gold electrodes are had by outer surface2O3Absolutely
Edge ceramic tube 1 passes through Al2O3Nickel-cadmium coil 2 inside ceramics pipe outer and it is coated in Al2O3Ceramics pipe outer appearance
Sensitive material film 3 on face and annular gold electrode is constituted, and sensitive material is NiS@In2O3Nanocomposite.
The NiS@In that the present embodiment is related to2O3The preparation method of gas sensor, the specific process steps are as follows:
Step 1: preparation NiS nanofiber: by Ni (NO3)2The method calcined by electrostatic spinning technique combination hydrogen sulfide
Prepare NiS nanofiber；Specific step is as follows:
(1) PVP of 2.2g is dissolved in the DMF solvent of 20ml, and by stirring to obtain homogeneous solution；
(2) Ni (NO of 2.0g is added to homogeneous solution again3)2, mixture magnetic agitation 12 hours at room temperature are made
Viscosity solution；
(3) then viscosity solution is fitted into the 10ml syringe with No. 22 needle points and carries out electrostatic spinning, electrostatic spinning
When apply voltage and be maintained at 17kV, injection flow control is 0.8ml/h, and the distance of needle tip to collector is 20cm, Static Spinning
Fiber mat is made after silk；
(4) obtained fiber mat is heated to 160 DEG C in air with the rate of heat addition of 1 DEG C/min and keeps the temperature 2 hours,
Stable fiber mat is made；
(5) finally, the H for being 99.999% in gas purity by stable fiber mat2With the heating of 1 DEG C/min in S atmosphere
Rate is heated to 700 DEG C and calcines 3-5 hours, and NiS nanofiber is made；
Step 2: preparation In2O3Nanofiber: by In (NO3)3·H2O prepares In by electrostatic spinning technique2O3Nanowire
Dimension；Specific step is as follows:
(1) by the In (NO of 0.5g3)3·H2It is small that 6 are vigorously stirred in the DMF solvent of O addition 20ml and in a reagent bottle
When, In (NO is made3)3Mixture；
(2) PVP of 0.25g is dissolved in the ethyl alcohol of 3mL and is vigorously stirred in another reagent bottle 6 hours, be made
PVP mixture；
(3) by In (NO3)3Mixture and PVP mixture mix by stirring together, are then charged into No. 22 needle points
10ml syringe in carry out electrostatic spinning, when electrostatic spinning, applies voltage and is maintained at 17kV, and injection flow control is 0.8ml/
H, the distance of needle tip to collector are 20cm, and nanofiber presoma is made；
(4) after electrostatic spinning, nanofiber presoma is heated to 160 DEG C in air with the rate of heat addition of 1 DEG C/min
And keep the temperature 2 hours, be then heated to 500 DEG C in air with the rate of heat addition of 1 DEG C/min and calcine 4 hours, In is made2O3It receives
Rice fiber；
Step 3: preparation NiS@In2O3Nanocomposite: by NiS and In2O3Nanofiber stoichiometrically matches mixed
Conjunction carries out calcining and solid-state grinding preparation NiS@In2O3Nanocomposite, the specific steps are as follows:
(1) firstly, by calcined NiS nanofiber and In2O3Nanofiber stoichiometrically matches at high operating temperatures
It is uniformly ground after mixing 1 hour；
(2) then, mixture is annealed in Ar gas 400 DEG C, is wherein 5% containing mass fraction in Ar gas
H2；
(3) finally, keeping the temperature 2 hours at 400 DEG C so that NiS@In2O3Nano-complex crystallization, is made after heat preservation
NiS@In2O3Nanocomposite；
The NiS nanofiber and In2O3The stoichiometric of nanofiber mixing prepares NiS@using quality proportioning
In2O3Nanocomposite, by NiS nanofiber and In2O360%NiS@is made according to the quality proportioning of 6:4 in nanofiber
40%In2O3, by NiS nanofiber and In2O370%NiS@30%In is made according to the quality proportioning of 7:3 in nanofiber2O3；It will
NiS nanofiber and In2O380%NiS@20%In is made according to the quality proportioning of 8:2 in nanofiber2O3；
Step 4: NiS@In2O3The preparation of gas sensor: by NiS@In2O3Nanocomposite is thorough in the agate mortar
The air-sensitive cream that paste is made is ground at bottom, then air-sensitive cream is uniformly coated on to the Al of gas sensor2O3On ceramic tube 1, finally
It is dried in vacuum overnight at 60 DEG C, NiS@In is made2O3Gas sensor.
The NiS@In that the present embodiment is related to2O3The raw material components of nanocomposite include: polyvinylpyrrolidone (PVP,
Mw=1500000), nickel nitrate hexahydrate (Ni (NO3) 26H2O), indium nitrate trihydrate (In (NO3)3·H2O),N,N-
Dimethylformamide (DMF) is purchased from Aladdin company (Aladdin), and is used without any purifying.
Embodiment 3
Three groups of NiS@In that the present embodiment prepares embodiment 22O3Gas sensor is tested for the property, by In2O3In Ma
It is thoroughly ground in Nao mortar and paste air-sensitive cream is made；Then air-sensitive cream is successively uniformly coated on gas sensor Al2O3Ceramics
It on pipe 1, and is dried in vacuum overnight at 60 DEG C, In is made2O3Gas sensor, by In2O3Gas sensor and NiS@In2O3Gas
Body sensor compares experiment test performance；Here, the gas response amplitude of gas sensor is defined as S=Ra/Rg, wherein
RaIt is the resistance in air, RgThe resistance under test gas, in addition, response or recovery time be apply or close gas it
Gas sensor output afterwards reaches its saturation state and spends time taking 90%.
As shown in Fig. 2, by In2O3Gas sensor, 60%NiS@40%In2O3Gas sensor, 70%NiS@30%
In2O3Gas sensor and 80%NiS@20%In2O3Gas sensor is under 25 DEG C of -350 DEG C of different temperatures to 100ppm ethyl alcohol
Carry out response measurement；As seen from the figure, four groups of inductors all show sensing characteristics related with temperature, 70%NiS@30%
In2O3Gas sensor and 80%NiS@20%In2O3Gas sensor response reach maximum value at 300 DEG C；In2O3Gas
Sensor (Ra/Rg=5.0) and 60%NiS@40%In2O3(Ra/Rg=5.7) gas sensor responds at 250 DEG C and reaches most
Big value；Because the content of indium is relatively high, with 70%NiS@30%In2O3Gas sensor and 80%NiS@20%In2O3
Gas sensor is compared, 60%NiS@40%In2O3Gas sensor shows lower optimum working temperature；According to reports,
In2O3The optimum working temperature of gas sensor is about 250 DEG C.With the further raising of temperature, the response of all devices starts
Decline rapidly.Therefore, as high-quality gas sensor, 300 DEG C are NiS@In2O3The optimum working temperature of gas sensor.This
Outside, 70%NiS@30%In2O3Gas sensor shows highest response, i.e. R in all samplesa/Rg=10.1, show:
At 300 DEG C, mass ratio NiS:In2O3The 70%NiS@30%In of=7:32O3Gas sensor rings 100ppm ethyl alcohol
Answer performance best.Therefore relevant test will be based on 70%NiS@30%In2O3Gas sensor carries out.
As shown in figure 3, by NiS@In2O3And In2O3Gas sensor is at 300 DEG C to 5ppm to 500ppm difference ethyl alcohol
Dynamic response and recovery characteristics are tested in gas concentration: with the increase of concentration of alcohol, In2O3Gas sensor is to alcohol gas
Response amplitude it is lower, and In2O3The response characteristic of gas sensor shows smooth trend 70%NiS@30%In2O3
The response of gas sensor sharply increases；When concentration of alcohol reaches 500ppm, response moves closer to saturation state, shows
70%NiS@30%In2O3Gas sensor has good sensitivity to ethanol gas concentration.
It is as shown in Figure 4: by by 70%NiS@30%In2O3Gas sensor and In2O3Gas sensor is respectively 300
Cyclical stability test is carried out to 100ppm ethyl alcohol at DEG C, as the result is shown: 70%NiS@30%In2O3The response of gas sensor
(Ra/Rg=10.3) it is much higher than In2O3Response (the R of gas sensora/Rg=4.2)；This shows NiS@In2O3Nanocomposite
The nano particle echoed on surface is more, causes specific surface area than increasing.
It is as shown in Figure 5: by by 70%NiS@30%In2O3Gas sensor rings 100ppm ethyl alcohol at 300 DEG C
Characteristic test is answered, as the result is shown 70%NiS@30%In2O3The response time and recovery time of gas sensor be respectively 9s and
22s, this shows 70%NiS@30%In2O3Gas sensor has quick response and regeneration rate to alcohol gas.
It is as shown in Figure 6: display, 70%NiS@30%In were tested by the 1st day to 60 days invariant feature2O3Gas sensing
Device is always held at 10 or so to the response amplitude of alcohol gas, illustrates NiS@In2O3Gas sensor has good long-term steady
It is qualitative.
As shown in fig. 7, by by 70%NiS@30%In2O3NiS@In2O3Gas sensor and In2O3Gas sensor exists
Response characteristic test, 70%NiS@30%In are carried out to 100ppm different type gas at 300 DEG C2O3NiS@In2O3Gas sensing
Device reaches 10.3 to the gas response amplitude of 100ppm alcohol gas, illustrates NiS@In2O3Gas sensor has alcohol gas
Good selectivity.
Embodiment 4
NiS@In described in Application Example 22O3The process flow of gas sensor detection alcohol gas are as follows: firstly, working as NiS@
In2O3When gas sensor is in air, NiS@In2O3Electronics in material is from N-shaped In2O3Turn to p-type NiS nanofiber
It moves, p-type NiS nanofiber and N-shaped In2O3Resistance increases at contact interface；Then, when introducing ethanol molecule, CH3CH2OH will
Increase N-shaped In2O3In electron amount and reduce the hole concentration in p-type NiS nanofiber, p-type NiS nanofiber and N-shaped
In2O3Resistance reduces at contact interface；Finally, passing through NiS@In2O3The significant changes of gas sensor resistance value or current value
The variation of concentration of alcohol in air is characterized, realizes NiS@In2O3Alarm function of the gas sensor to alcohol gas；Specific detection
Mechanism is as follows:
As shown in Fig. 8-e, when with different fermi level (EF) semiconductor material electrification when, the electronics of higher-energy
(e-) lower state not occupied will be reached by p-n junction, realize the balance of fermi level, the e being equivalent near p-n junction interface-1-
h-1(electron-hole) is compound, and when N-shaped and p-type semiconductor contact target gas, object gas is in interface depletion of charge current-carrying
Son will form depleted of electrons layer at the contact interface between N-shaped and p-type semiconductor；Due to the original E of semiconductorFThere are differences
Different, energy band bends, at the contact interface between N-shaped and p-type semiconductor formed potential barrier, electronics have to pass through potential barrier barrier with
Overcome the interface,
As shown in fig. 8-f: N-shaped In2O3Contact between p-type NiS nanofiber semiconductor leads to appointing in physical interface
Band structure bending on side in depletion layer, to adapt to fermi level (EF) balance；From the dynamic process of depleted of electrons layer
From the point of view of, N-shaped In2O3It is closely linked with p-type NiS nanofiber by calcination process and electrostatic interaction, N-shaped In2O3
Electronics (e in material-) it is majority carrier, hole (h+) it is principal carrier in p-type NiS nanofiber, as N-shaped In2O3With
When two kinds of materials of p-type NiS nanofiber be combined with each other, electronics is from N-shaped In2O3It is shifted to p-type NiS nanofiber, belongs to p-type NiS
The e of nanofiber-With belong to N-shaped In2O3H+It will be recombined at contact interface, the concentration of charge carrier is caused to drop rapidly
Low, resistance increases；When introducing ethanol molecule, CH3CH2OH will increase N-shaped In2O3In electron amount and reduce p-type NiS and receive
Hole concentration in rice fiber exhausts thinner layer thickness, and resistance reduces, and specific reaction is as follows:
C2H5OH+O2 -→CH3CHO+H2O(gas)+2e- (1)
CH3CHO+5O2 -→2CO2+2H2O(gas)+10e- (2)。
Claims (8)
1. a kind of gas sensor based on nanometer nickel sulfide composite material has 2 discrete annular gold electrodes by outer surface
Al2O3Ceramics pipe outer passes through Al2O3Nickel-cadmium coil inside ceramics pipe outer and it is coated in Al2O3Insulating ceramics
Sensitive material film on tube outer surface and annular gold electrode is constituted, it is characterised in that: sensitive material is the nano combined material of NiS
Material.
2. the gas sensor according to claim 1 based on nanometer nickel sulfide composite material, it is characterised in that: the base
In the preparation method of the gas sensor of nanometer nickel sulfide composite material include: by NiS nanocomposite in the agate mortar
The air-sensitive cream that paste is made thoroughly is ground, then air-sensitive cream is uniformly coated on to the Al of gas sensor2O3On ceramic tube, most
It is dried in vacuum overnight at 60 DEG C afterwards, the gas sensor of nanometer nickel sulfide composite material is made.
3. the gas sensor according to claim 1 based on nanometer nickel sulfide composite material, it is characterised in that: described
The specific preparation process of NiS nanocomposite are as follows:
(1) NiS nanofiber is prepared: by Ni (NO3)2NiS is prepared by the method that electrostatic spinning technique combination hydrogen sulfide is calcined to receive
Rice fiber；
(2) it prepares metal oxide semiconductor nanofiber: metallic compound is prepared into semiconductor gold by electrostatic spinning technique
Belong to oxide nanofiber；
(3) it prepares NiS nanocomposite: NiS and metal oxide semiconductor nanocomposite is matched by the quality of 1/2-4
Calcining and solid-state grinding preparation NiS nanocomposite are carried out than mixing.
4. the gas sensor according to claim 1 based on nanometer nickel sulfide composite material, it is characterised in that: the base
In the gas sensor of nanometer nickel sulfide composite material be specially NiS@In2O3Gas sensor, NiS@In2O3Gas sensor
Main structure include by outer surface have 2 discrete annular gold electrodes Al2O3Ceramics pipe outer passes through Al2O3Insulation pottery
Nickel-cadmium coil inside porcelain tube and it is coated in Al2O3Sensitive material on insulating ceramics tube outer surface and annular gold electrode
Film is constituted, and sensitive material is NiS@In2O3Nanocomposite.
5. the gas sensor according to claim 4 based on nanometer nickel sulfide composite material, it is characterised in that: described
NiS@In2O3The preparation method of gas sensor, the specific process steps are as follows:
Step 1: preparation NiS nanofiber: by Ni (NO3)2The method preparation calcined by electrostatic spinning technique combination hydrogen sulfide
NiS nanofiber；Specific step is as follows:
(1) PVP of 2.2g is dissolved in the DMF solvent of 20ml, and by stirring to obtain homogeneous solution；
(2) Ni (NO of 2.0g is added to homogeneous solution again3)2, by mixture magnetic agitation 12 hours at room temperature, viscosity is made
Solution；
(3) then viscosity solution is fitted into the 10ml syringe for having No. 22 needle points and carries out electrostatic spinning, when electrostatic spinning applies
Making alive is maintained at 17kV, and injection flow control is 0.8ml/h, and the distance of needle tip to collector is 20cm, after electrostatic spinning
Fiber mat is made；
(4) obtained fiber mat is heated to 160 DEG C in air with the rate of heat addition of 1 DEG C/min and keeps the temperature 2 hours, be made
Stable fiber mat；
(5) finally, the H for being 99.999% in gas purity by stable fiber mat2Added in S atmosphere with the rate of heat addition of 1 DEG C/min
Heat is to 700 DEG C and calcines 3-5 hours, and NiS nanofiber is made；
Step 2: preparation In2O3Nanofiber: by In (NO3)3·H2O prepares In by electrostatic spinning technique2O3Nanofiber；Tool
Steps are as follows for body:
(1) by the In (NO of 0.5g3)3·H2O is added in the DMF solvent of 20ml, and is vigorously stirred 6 hours in a reagent bottle,
In (NO is made3)3Mixture；
(2) PVP of 0.25g is dissolved in 3mL ethyl alcohol and is vigorously stirred in another reagent bottle 6 hours, PVP mixing is made
Object；
(3) by In (NO3)3Mixture and PVP mixture mix by stirring together, are then charged into No. 22 needle points
Carrying out electrostatic spinning in 10ml syringe, when electrostatic spinning, applies voltage and is maintained at 17kV, and injection flow control is 0.8ml/h,
The distance of needle tip to collector is 20cm, and nanofiber presoma is made；
(4) after electrostatic spinning, nanofiber presoma is heated to 160 DEG C in air with the rate of heat addition of 1 DEG C/min and is protected
Then temperature 2 hours is heated to 500 DEG C in air with the rate of heat addition of 1 DEG C/min and calcines 4 hours, In is made2O3Nanowire
Dimension；
Step 3: preparation NiS@In2O3Nanocomposite: by NiS and In2O3Nanofiber stoichiometrically matches mixing and carries out
Calcining and solid-state grinding preparation NiS@In2O3Nanocomposite, the specific steps are as follows:
(1) firstly, by calcined NiS nanofiber and In2O3Nanofiber stoichiometrically proportion mixing at high operating temperatures
It uniformly grinds 1 hour afterwards；
(2) then, mixture is annealed to 400 DEG C in Ar gas, the H for being wherein 5% containing mass fraction in Ar gas2；
(3) finally, keeping the temperature 2 hours at 400 DEG C so that NiS@In2O3Nano-complex crystallization, is made NiS@after heat preservation
In2O3Nanocomposite；
The NiS nanofiber and In2O3The stoichiometric of nanofiber mixing prepares NiS@In using quality proportioning2O3It receives
Nano composite material, by NiS nanofiber and In2O360%NiS@40%In is made according to the quality proportioning of 6:4 in nanofiber2O3,
By NiS nanofiber and In2O370%NiS@30%In is made according to the quality proportioning of 7:3 in nanofiber2O3；By NiS Nanowire
Dimension and In2O380%NiS@20%In is made according to the quality proportioning of 8:2 in nanofiber2O3；
Step 4: NiS@In2O3The preparation of gas sensor: by NiS@In2O3Nanocomposite is thoroughly ground in the agate mortar
Grind paste air-sensitive cream, then air-sensitive cream is uniformly coated on to the Al of gas sensor2O3On ceramic tube, finally 60
It is dried in vacuum overnight at DEG C, NiS@In is made2O3Gas sensor；
The NiS@In2O3The raw material components of nanocomposite include: polyvinylpyrrolidone, nickel nitrate hexahydrate, nitre
Sour indium trihydrate and N,N-dimethylformamide.
6. the gas sensor according to claim 5 based on nanometer nickel sulfide composite material, it is characterised in that: 300
DEG C when, the mass ratio be NiS:In2O3The 70%NiS@30%In of=7:32O3Gas sensor rings 100ppm ethyl alcohol
Answer performance best.
7. the gas sensor according to claim 5 based on nanometer nickel sulfide composite material, it is characterised in that: described
70%NiS@30%In2O3Gas sensor is tested 5ppm dynamic into 500ppm difference ethanol gas concentration at 300 DEG C and is rung
Should and recovery characteristics: with the increase of concentration of alcohol, 70%NiS@30%In2O3The response of gas sensor sharply increases, when
When concentration of alcohol reaches 500ppm, response moves closer to saturation state, 70%NiS@30%In2O3Gas sensor is to ethanol gas
Bulk concentration variation sensing is sensitive.
8. the gas sensor according to claim 5 based on nanometer nickel sulfide composite material, it is characterised in that: described
NiS@In2O3The process flow of gas sensor detection alcohol gas are as follows:
Firstly, working as NiS@In2O3When gas sensor is in air, NiS@In2O3Electronics in material is from N-shaped In2O3To p-type
The transfer of NiS nanofiber, p-type NiS nanofiber and N-shaped In2O3Resistance increases at contact interface；
Then, when introducing ethanol molecule, CH3CH2OH will increase N-shaped In2O3In electron amount and reduce p-type NiS Nanowire
Hole concentration in dimension, p-type NiS nanofiber and N-shaped In2O3Resistance reduces at contact interface；
Finally, passing through NiS@In2O3Concentration of alcohol in gas sensor resistance value or the significant changes of current value characterization air
NiS@In is realized in variation2O3Alarm function of the gas sensor to alcohol gas.
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