CN108169291A - The ethanol sensor of Zn doping CdS nano sensitive materials based on graded structure, preparation method and applications - Google Patents
The ethanol sensor of Zn doping CdS nano sensitive materials based on graded structure, preparation method and applications Download PDFInfo
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- CN108169291A CN108169291A CN201711362246.3A CN201711362246A CN108169291A CN 108169291 A CN108169291 A CN 108169291A CN 201711362246 A CN201711362246 A CN 201711362246A CN 108169291 A CN108169291 A CN 108169291A
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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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- 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
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
Abstract
A kind of ethanol sensor, preparation method and its application in a variety of environment in terms of detection alcohol vapour of the Zn doping CdS nano sensitive materials based on graded structure, belong to metal sulfide gas sensor technical field.By Al of the outer surface with two parallel, cyclic annular and separate gold electrodes2O3Ceramic tube substrate, coated in Al2O3The Zn doping CdS nano sensitive materials of graded structure on ceramic tube outer surface and gold electrode are placed in Al2O3Ni-Cd heating coil composition in ceramic tube.By mixing Zn elements on the CdS nanospheres of graded structure, the sensitivity to ethyl alcohol is improved, the Monitoring lower-cut of material is relatively low, and with quickly response resume speed and good repeatability, has broad application prospects in terms of detection level；Good characteristics simple with synthetic method, of low cost, small.
Description
Technical field
The invention belongs to metal sulfide gas sensor technical fields, and in particular to a kind of Zn based on graded structure
Adulterate ethanol sensor, preparation method and its answering in terms of detection alcohol vapour in a variety of environment of CdS nano sensitive materials
With.
Background technology
With the development of future information technology, sensor, will be in Information Technology Development as the means for obtaining information
Forward position, can widely be paid close attention to and commercial applications.The aggravation of air environmental pollution in recent years, industrial/household safety accident
Take place frequently, food/pharmaceutical quality severe and in fields such as medical treatment, social welfare, fossil energy, military project and aviation/space flight
Urgent need.Although having been obtained for very big progress in the research of oxide semiconductor gas sensor, in order to meet
Its requirement in each detection field, in addition to continue to conduct further research oxide semiconductor gas sensor with
Outside, we can also develop new nano material such as metal sulfide to improve the sensitivity of sensor, selectivity and reduce work
Temperature,.
In fact, deepen always constantly around the research for improving metal sulfide transducer sensitivity, especially
The improvement sensor performance that develops into of nanoscale science and technology provides good opportunity.Research shows that the identification work(of gas sensitive
Energy, conversion function and sensitive body utilization rate decide the sensitivity of metal sulfide semiconductor sensor.It is found that pass through
The metal sulfide composite material of heterogeneous dopant doping can significantly improve sensitivity and the selectivity of sensor.This is main
It is the carrier mobility that sensing material can be improved because of doping dissimilar metal ion, so as to improve its " conversion function ",
Secondly, some dissimilar metal dopants can be used as catalyst make to be happened at the corresponding redox reaction of semiconductor surface and obtain
Catalysis can improve the selectivity of sensor, improve " identification function " of sensing material.Based on this point, carry out dissimilar metal
The design and preparation of the metal sulfide semiconductor of doping have highly important science for the application of enlargement gas sensor
Meaning.
Invention content
The object of the present invention is to provide a kind of ethyl alcohol sensings of the Zn doping CdS nano sensitive materials based on graded structure
Device, preparation method and its application in a variety of environment in terms of detection alcohol vapour.The present invention is by carrying out semi-conducting material
Doping, increases the sensitivity of sensor, improves the response speed of sensor, improve the repeatability of sensor, promote such sensing
Device is in the functionization of field of gas detection.
The obtained sensor of the present invention has preferable selectivity, repeatability other than having higher sensitivity.
The Monitoring lower-cut of the sensor be 5ppm, the detection available for ethyl alcohol.Commercially available tubular structure sensor of the present invention,
Manufacture craft is simple, small, conducive to industrial batch production, therefore with important application value.
It is of the present invention based on graded structure Zn doping CdS ethanol sensors, by outer surface with two it is parallel,
The Al of cyclic annular and separate gold electrode2O3Ceramic tube substrate, coated in Al2O3Receiving on ceramic tube outer surface and gold electrode
Rice sensitive material is placed in Al2O3Ni-Cd heating coil composition in ceramic tube；It is characterized in that：Nano sensitive material is graduation
The Zn doping CdS materials of structure, and be prepared by following steps,
(1) ZnO of 0.05g is dissolved in the mixed solution of 10~15mL ethylenediamines and 20~30mL water, then added
Cd (the NO of 200~300 μ L, 0.1M3)2Aqueous solution and 200~300 μ L, 0.1M thiourea solution to above-mentioned mixed solution in,
It is sufficiently stirred 10~20min；
(2) by above-mentioned solution under the conditions of 150~190 DEG C 10~15h of hydro-thermal reaction；
(3) after reaction, obtained product is cooled to room temperature, then with water and ethyl alcohol alternately centrifuge washing,
Obtained product is dried, so as to obtain the Zn of graded structure doping CdS nano sensitive materials；
Involved sensor uses heater-type structure in the present invention, and concrete technology is as follows：
(1) Zn is taken to adulterate CdS nano sensitive materials, with ethyl alcohol in mass ratio 0.25~0.5：1 ratio uniform mixing shape
Into slurry；Al2O3 ceramics of the slurry coating on the surface with two gold electrodes parallel, cyclic annular and separate are dipped with hairbrush
Tube outer surface makes it be completely covered on Al2O3 ceramics tube outer surface and gold electrode；The thickness of nano sensitive material for 15~
30um；The internal diameter of Al2O3 ceramic tubes is 0.6~0.8mm, and outer diameter is 1.0~1.5mm, and length is 4~5mm；Single gold electrode
Width is 0.4~0.5mm, and the spacing of two gold electrodes is 0.5~0.6mm, and the platinum filament wire drawn on gold electrode is the length of
4~6mm；
(2) Al that nano sensitive material will have been coated2O3Ceramic tube is sintered 1~3h at 250~350 DEG C, then by resistance
Be worth ni-Cd heating coil (number of turn is 50~60 circles) for 30~40 Ω across Al2O3 ceramic tube insides, pass to direct current come for
Sensor provides suitable operating temperature；Finally the device being prepared is welded on general heater-type hexagonal tube socket；
(3) by above-mentioned device in 150~250 DEG C of air environments aging 5~7 days, so as to obtain based on graded structure
Zn doping CdS nano sensitive materials ethanol sensor.
Operation principle：
When Zn doping CdS ethanol sensors are placed in air, the oxygen molecule in air will capture electronics from CdS simultaneously
With O2 -、O-Or O2-Mode exist, material surface forms depletion layer, and resistance increases.When sensor connects under certain suitable temperature
When touching alcohol gas, alcohol gas molecule will be adsorbed in sensor surface, and release trapped electron returns to CdS conduction bands, so as to make CdS
Resistance declines.The sensitivity that we define sensor herein is S：S=Ra/Rg, wherein RaBetween two gold electrodes of sensor
Resistance in air, RgThe resistance after ethyl alcohol is contacted between two gold electrodes of sensor.
The ethanol sensor of Zn based on graded structure doping CdS prepared by the present invention has the following advantages：
1. can prepare the composite construction of graduation nano material using simple hydro-thermal method, synthetic method is simple, cost
It is cheap；
2. by adulterating Zn elements on graduate CdS nanospheres, the sensitivity to ethyl alcohol, the detection of material are improved
Lower limit is relatively low, and with quickly response resume speed and good repeatability, before having wide application in terms of the detection level
Scape；
3. using commercially available tubular type sensor, device technology is simple, small.
Description of the drawings
Fig. 1：Zn adulterates the structure diagram of CdS ethanol sensors；Fig. 1 (a) is sectional view, and Fig. 1 (b) shows for welded condition
It is intended to；
Fig. 2 is the SEM figures of CdS nano sensitive materials before and after Zn of the present invention doping, and wherein Fig. 2 (a), (b), (c) are mixed for Zn
The SEM figures of CdS nanospheres after miscellaneous, amplification factor is respectively 10000 times, 50000 times, 100000 times, Fig. 2 (d), (e), (f)
The SEM figures of CdS nano sensitive materials before being adulterated for Zn, amplification factor is respectively 10000 times, 50000 times, 100000 times；
Fig. 3 is spirit of the sensor at a temperature of different operating to 100ppm ethyl alcohol in the comparative example of the present invention and embodiment 1
Sensitivity comparison diagram；
Fig. 4 be the present invention comparative example and sensor in embodiment 1 when operating temperature is 225 DEG C to 100ppm difference gas
The selective comparison diagram of body；
Fig. 5 is that sensor device sensitivity-concentration of alcohol when operating temperature is 225 DEG C is special in the embodiment of the present invention 1
Linearity curve.
As shown in Figure 1, the names of the parts are：Annular gold electrode 1, Zn doping CdS nano sensitive materials 2, Al2O3Insulation pottery
Porcelain tube 3, nichrome heating coil 4, platinum filament pin 5；
As shown in Fig. 2, it can be seen from the figure that gained sample is graded structure (by low-dimensional nano structure as structure
Build the graduation 3-D nano, structure that unit assembles) nanosphere, and nanosphere pattern has apparent change before and after adulterating Zn
Change, CdS nanospheres are disorderly and unsystematic before adulterating Zn, and have a little reunion, and adulterate nanosphere more uniformity after Zn, nanometer rods
Radius be 30~50nm, a length of 0.5~-0.8 μm.
Fig. 3 is the comparison diagram of comparative example and embodiment 1 in the response of 225 DEG C of 5 kinds of gas with various to 100ppm.From figure
In as can be seen that embodiment compared to comparative example, all have a certain upgrade to the response of most of gas, to ethyl alcohol and toluene
It is particularly evident.
As shown in figure 4, the optimum working temperature of sensor is 225 DEG C in comparative example and embodiment 1, device pair at this time
The sensitivity of 100ppm ethyl alcohol is respectively 5.5 and 27.
As shown in figure 5, it is the sensitivity of 1 sensor of embodiment and concentration of alcohol in the range of 5~100ppm in concentration of alcohol
Relationship for linear relationship, also quickly increase with the increase sensitivity of concentration.
Sensitivity test method：Sensor is put into gas cabinet first, this is measured by the ammeter being connect with sensor
When resistance, obtain the i.e. R of the aerial resistance value of sensora；Then 5 are injected into gas cabinet using microsyringe~
The ethyl alcohol of 100ppm obtains the i.e. R of resistance value of the sensor in various concentration acetone by measuringg, according to the definition of sensitivity S
Formula S=Ra/Rg, the sensitivity of various concentration lower sensor is obtained by calculation, finally obtains the mark of concentration of alcohol-sensitivity
Quasi- working curve.It can be seen from the figure that the Monitoring lower-cut of 1 sensor of embodiment is 5ppm, sensitivity at this time is 3.3；When
When concentration of alcohol is 100ppm, the sensitivity of comparative example and embodiment 1 at this time is respectively 5.5 and 27.
Can R be measured by above-mentioned method during practical measurementa、Rg, obtain the mark with concentration of alcohol-sensitivity after Sensitirity va1ue
Quasi- working curve is compared, and can realize the measurement to unknown ethanol gas concentration.
Specific embodiment
Comparative example：
Heater-type ethanol sensor, specific manufacturing process are made using CdS nanospheres as sensitive material：
1. Cd (the NO of a concentration of 0.1M are first equipped with 50mL volumetric flasks3)2Aqueous solution and thiourea solution, then add 250
Cd (the NO of μ L3)2(0.1M) aqueous solution and thiocarbamide (0.1M) aqueous solution of 250 μ L are to 13mL ethylenediamines and 26mL deionized waters
In mixed solution, it is sufficiently stirred 10min；
2. by above-mentioned solution in 50mL hydrothermal reaction kettles are put into, reaction kettle is then put into baking oven under the conditions of 180 DEG C
React 12h；
3. obtained product after reaction, is cooled to room temperature, it, will then with water and ethyl alcohol alternately centrifuge washing
Obtained product is dried, so as to obtain the CdS nano sensitive materials of no Zn doping.
4. take appropriate CdS nanometer material obtained and ethyl alcohol 0.4mg in mass ratio:1mg is uniformly mixed to form slurry.With hair
Brush dips appropriate slurry and is coated in commercially available ceramic tube outer surface, makes it that the gold electrode (tubular ceramic substrate of outer surface be completely covered
Internal diameter be 0.7mm, outer diameter 1.1mm, length 4.5mm；Two ring-type gold electricity being mutually parallel are come on its outer surface
Pole, the single width of two electrodes are 0.4mm, spacing 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm).
5. coated ceramic tube is sintered 2h at 300 DEG C, 35 Ω ni-Cd heating coils are then passed through into Al2O3Ceramics
Inside pipe, direct current is passed to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal finally by platinum filament wire
On tube socket, so as to obtain CdS ethanol sensors.
6. finally by sensor in 200 DEG C of air environments aging 6 days, so as to obtain the ethyl alcohol of CdS nano sensitive materials
Sensor.
Embodiment 1：
Zn adulterates CdS metal sulfide semiconductors and makes ethanol sensor as sensitive material, and manufacturing process is first for 1.
Cd (the NO of a concentration of 0.1M are equipped with 50mL volumetric flasks3)2Aqueous solution and thiourea solution then add 0.05g ZnO to 13mL
In ethylenediamine and the mixed solution of 26mL deionized waters, it is sufficiently stirred 5min, then the Cd (NO by 250 μ L3)2(0.1M) aqueous solution
It is respectively added in above-mentioned mixed solution with thiocarbamide (0.1M) aqueous solution of 250 μ L；
2. by above-mentioned solution in 50mL hydrothermal reaction kettles are put into, reaction kettle is then put into baking oven under the conditions of 180 DEG C
React 12h；
3. obtained product after reaction, is cooled to room temperature, it, will then with water and ethyl alcohol alternately centrifuge washing
Obtained product is dried, so as to obtain the CdS nano sensitive materials of Zn doping.
4. take appropriate CdS nanometer material obtained and ethyl alcohol 0.4mg in mass ratio:1mg is uniformly mixed to form slurry.With hair
Brush dips appropriate slurry and is coated in commercially available ceramic tube outer surface, makes it that the gold electrode (tubular ceramic substrate of outer surface be completely covered
Internal diameter be 0.7mm, outer diameter 1.1mm, length 4.5mm；Two ring-type gold electricity being mutually parallel are come on its outer surface
Pole, the single width of two electrodes are 0.4mm, spacing 0.5mm；The platinum filament wire length drawn on gold electrode is 5mm).
5. coated ceramic tube is sintered 2h at 300 DEG C, 35 Ω ni-Cd heating coils are then passed through into Al2O3Ceramics
Inside pipe, direct current is passed to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal finally by platinum filament wire
On tube socket, so as to obtain CdS ethanol sensors.
6. finally by sensor in 200 DEG C of air environments aging 6 days, so as to obtain Zn doping CdS nano sensitive materials
Ethanol sensor.
Claims (5)
1. a kind of ethanol sensor of the Zn doping CdS nano sensitive materials based on graded structure, two are carried by outer surface
The Al of parallel, cyclic annular and separate gold electrode2O3Ceramic tube substrate, coated in Al2O3On ceramic tube outer surface and gold electrode
Nano sensitive material, be placed in Al2O3Ni-Cd heating coil composition in ceramic tube, the platinum filament wire drawn on gold electrode；Its
It is characterized in that：Nano sensitive material adulterates CdS materials, and be prepared by following steps for the Zn of graded structure,
(1) ZnO of 0.05g is dissolved in the mixed solution of 10~15mL ethylenediamines and 20~30mL water, then add 200~
Cd (the NO of 300 μ L, 0.1M3)2Aqueous solution and 200~300 μ L, 0.1M thiourea solution to above-mentioned mixed solution in, fully stir
Mix 10~20min；
(2) by above-mentioned solution under the conditions of 150~190 DEG C 10~15h of hydro-thermal reaction；
(3) after reaction, obtained product is cooled to room temperature, then with water and ethyl alcohol alternately centrifuge washing, incited somebody to action
To product be dried, so as to obtain the Zn of graded structure doping CdS nano sensitive materials.
2. a kind of ethanol sensor of Zn doping CdS nano sensitive materials based on graded structure as described in claim 1,
It is characterized in that：The thickness of nano sensitive material is 15~30um.
3. a kind of ethanol sensor of Zn doping CdS nano sensitive materials based on graded structure as described in claim 1,
It is characterized in that：Al2O3The internal diameter of ceramic tube is 0.6~0.8mm, and outer diameter is 1.0~1.5mm, and length is 4~5mm；Single gold
The width of electrode is 0.4~0.5mm, and the spacing of two gold electrodes is 0.5~0.6mm；The platinum filament wire drawn on gold electrode,
Length is 4~6mm.
4. the ethyl alcohol of the doping CdS nano sensitive materials of the Zn based on graded structure described in claims 1 to 3 any one passes
The preparation method of sensor, its step are as follows：
(1) Zn is taken to adulterate CdS nano sensitive materials, with ethyl alcohol in mass ratio 0.25~0.5：1 ratio uniform is mixed to form slurry
Material；Al of the slurry coating on the surface with two gold electrodes parallel, cyclic annular and separate is dipped with hairbrush2O3Outside ceramic tube
Surface makes it be completely covered on Al2O3On ceramic tube outer surface and gold electrode；
(2) Al that nano sensitive material will have been coated2O3Ceramic tube is sintered 1~3h at 250~350 DEG C, is then by resistance value
The ni-Cd heating coil of 30~40 Ω passes through Al2O3Ceramic tube inside passes to direct current to provide suitable work temperature for sensor
Degree；Finally the device being prepared is welded on general heater-type hexagonal tube socket；
(3) by above-mentioned device in 150~250 DEG C of air environments aging 5~7 days, so as to obtain the Zn based on graded structure
Adulterate the ethanol sensor of CdS nano sensitive materials.
5. the ethyl alcohol of the doping CdS nano sensitive materials of the Zn based on graded structure described in claims 1 to 3 any one passes
Sensor detects the application in terms of alcohol vapour in a variety of environment.
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Cited By (5)
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| CN108732214A (en) * | 2018-08-29 | 2018-11-02 | 吉林大学 | Based on PdO@In2O3The acetone gas sensor and preparation method thereof of compound nano sensitive material |
| CN109100397A (en) * | 2018-07-05 | 2018-12-28 | 吉林大学 | One kind being based on PANI@WO3The flexible flat formula ammonia gas sensor of hollow sphere nano sensitive material and its application |
| CN113219010A (en) * | 2021-05-19 | 2021-08-06 | 吉林大学 | Ethanol sensor of ZnO double-shell hollow structure microsphere sensitive material and preparation |
| CN113607785A (en) * | 2021-08-10 | 2021-11-05 | 南京工程学院 | Based on flower ball shaped Ag/Bi2WO6Ethanol gas sensor of sensitive material and preparation method thereof |
| CN114264703A (en) * | 2021-12-27 | 2022-04-01 | 吉林大学 | Cubic/hexagonal phase CdS composite nanomaterial-based n-propanol sensor and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114264703B (en) * | 2021-12-27 | 2023-08-18 | 吉林大学 | N-propanol sensor based on cubic/hexagonal phase CdS composite nano material and preparation method thereof |
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Application publication date: 20180615 |