CN105181762A - Co-Sn composite oxide ethyl alcohol sensor and preparation and application thereof - Google Patents
Co-Sn composite oxide ethyl alcohol sensor and preparation and application thereof Download PDFInfo
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- CN105181762A CN105181762A CN201510599580.5A CN201510599580A CN105181762A CN 105181762 A CN105181762 A CN 105181762A CN 201510599580 A CN201510599580 A CN 201510599580A CN 105181762 A CN105181762 A CN 105181762A
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Abstract
Provided are a Co-Sn composite oxide ethyl alcohol sensor prepared through a one-step water heating method, a preparation method and an application of the Co-Sn composite oxide ethyl alcohol sensor in detecting ethyl alcohol concentration in drunken driving and the atmospheric environment, and belongs to the technical field of gas sensors. The sensor is composed of an Al2O3 insulation ceramic tube sold in the market, Co-Sn composite oxide sensitive materials and a nickel-cadmium heating coil, wherein the outer surface of the Al2O3 insulation ceramic tube is provided with two annular gold electrodes, the outer surfaces of the annular gold electrodes and the outer surface of the Al2O3 insulation ceramic tube are coated with the Co-Sn composite oxide sensitive materials, and the nickel-cadmium heating coil penetrates through the interior of the Al2O3 insulation ceramic tube. The sensor has good linearity on ethyl alcohol with low concentration (a lower limit of detection is 1 ppm), the Co-Sn composite oxide ethyl alcohol sensor can be well applied to alcohol detection in drunken driving and the atmospheric environment due to the characteristics, and then driver driving safety and environment safety can be judged by detecting the ethyl alcohol concentration.
Description
Technical field
The invention belongs to gas sensor technical field, be specifically related to a kind of utilize a step hydrothermal method to prepare Co-Sn composite oxides ethanol sensor, preparation method and the application that detects in drunk driving and atmospheric environment in concentration of alcohol thereof.
Background technology
Distinguish from use-pattern, the sensor that ethanol sensor is divided into disposable ethanol sensor and repeatedly uses.The expiration formula ethanol test instrument having dropped into business use belongs to the sensor repeatedly used.The focus of research tends to sensor microminiaturization, rapid, accuracy and precise development, and various new material and new-type technology emerge in an endless stream, and are also widely used in ethanol sensor.
Ethanol is a kind of important raw material of industry, is widely used in the fields such as chemical industry, food industry, daily-use chemical industry and health care, has development prospect again in oil replacement simultaneously.Ethanol industry is again a with serious pollution industry while making outstanding contributions for national economy.Volatile at normal temperatures thus enter in air, can be used for sterilization, and as excellent organic solvent solubilized gas chromatography and inorganics.Drink and food at present containing ethanol gets more and more, especially in the majority with drinks in China.The illegal accident of driving when intoxicated increases increasingly, proposes new requirement to the dynamics of traffic administration and level.Therefore the concentration quick and precisely detecting ethanol has very important realistic meaning and practical value.
At present, be all in starting degree both at home and abroad to the research work of low-concentration ethanol gas sensor, the dedicated sensor for low-concentration ethanol gas does not also form effective industrialization.The practical principal element of restriction sensors with auxiliary electrode is exactly that the Monitoring lower-cut of sensor is higher and sensitivity is lower.In order to enable sensor have low-detection lower limit and high sensitivity, high performance sensitive material can be used realize.
Summary of the invention
The application that the object of this invention is to provide Co-Sn composite oxides ethanol sensor prepared by an a kind of step hydrothermal method, preparation method and detect in drunk driving and atmospheric environment in concentration of alcohol.The present invention, by carrying out a step compound to material, can reduce the Monitoring lower-cut of sensor, increases the sensitivity of sensor, promotes that this kind of sensor detects the practical of concentration of alcohol detection in drunk driving and atmospheric environment.
The sensor that the present invention obtains except having high sensitivity, low-detection lower limit, and has good selectivity and repeatability.The Monitoring lower-cut of this sensor is 1ppm, therefore can be used for the detection of ethanol content in drunk driving and atmospheric environment, and then judges the safety in driver driving and atmospheric environment.
As shown in Figure 1, Co-Sn composite oxides ethanol sensor of the present invention, is carried the Al of 2 annular gold electrodes (5) by commercially available outside surface
2o
3insulating ceramics pipe (1), be coated in annular gold electrode (5) and Al
2o
3the sensitive material (2) of insulating ceramics pipe (1) outside surface, through Al
2o
3insulating ceramics pipe (1) nickel-cadmium heater coil (3) forms; Each annular gold electrode (5) is upper simultaneously with 2 platinum lines (4), can obtain the resistance between two golden ring electrodes, according to defined formula and the S=R of sensitivity S by the resistance measured between platinum line
a/ R
g, through can be calculated the sensitivity of sensor.It is characterized in that: utilize Co-Sn composite oxides as sensitive material, the compound of cobalt/cobalt oxide changes the catalytic capability of tin-oxide nanometer film clips on the one hand, more reactivity site can be provided, these two aspects all significantly can improve the reaction efficiency of gas and sensitive material, and then improves the sensitivity of sensor.A large amount of heterojunction can be formed on the other hand between Co-Sn composite oxide particle and particle, the appearance of these heterojunction can provide more reactivity site, these two aspects all significantly can improve the reaction efficiency of gas and sensitive material, and then improves the sensitivity of sensor.In addition, the sensor of tubular structure and the manufacture craft of oxide simply, are beneficial to industrial batch production.
The concrete manufacturing process of Co-Sn composite oxides ethanol sensor of the present invention is:
(1) first by 5.88gNa
3c
6h
5o
72H
2o, 0.9gSnCl
22H
2o, 0.95gCoCl
26H
2o, 5ml ethylenediamine, 10mlNaOH (0.4M) solution are dissolved in 20ml water when stirring, and stir and form homogeneous solution in 30 minutes;
(2) (1) mixed solution is put into 45ml polytetrafluoroethylkettle kettle to seal, put into 180 DEG C of baking ovens 12 hours, after terminating, Temperature fall is to room temperature, by sample collection ethanol and deionized water centrifugal after to be put in double dish 80 DEG C several hours, collection sample;
(3) above-mentioned nano gas sensitive material is calcined 2 hours at 300 DEG C, obtain gas sensitive material, this sensitive material and deionized water are mixed into pasty state, are then evenly coated in the insulation Al that commercially available outside surface carries 2 annular gold electrodes (5)
2o
3ceramic pipe (1) surface, form the sensitive material film (2) of 10 ~ 40 microns, the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, internal diameter is 0.8 ~ 1.0mm, and makes sensitive material cover annular gold electrode (5) completely;
(4) toast about 15 minutes under infrared lamp, after sensitive material drying, insulation Al
2o
3ceramic pipe (1) is calcined 2 hours at 300 DEG C; Then be that the NI-G heater coil (3) of 30 ~ 40 Ω is through insulation Al by resistance value
2o
3ceramic pipe (1) is inner as heater strip, is finally carried out welding and encapsulating according to general heater-type gas sensor by above-mentioned device, thus obtains Co-Sn composite oxides ethanol sensor of the present invention.
The sensitive mechanism of Co-Sn composite oxides ethanol sensor is: be adsorbed on sensitive material surface when oxygen molecule and sensor contacts, and oxygen molecule captures electronics from composite oxides conduction band, forms O
-, such as formula (1)-(3).
When temperature is lower than (1), (2) reaction occur when 150 DEG C, the oxygen molecule of absorption is with O
2 -form exists; When temperature is 150-400 DEG C of scope, (1), (2) and (3) reaction occur, and the working temperature of Co-Sn composite oxides ethanol sensor is at 200 DEG C, so the oxygen molecule of absorption is with O
-form exists.Can bring when oxygen in oxide material ingress of air curved, and form depletion layer on surface, the resistance of sensor raises.When sensor contacts with ethanol, ethanol can with the O on material
-react (4).
C
2H
5OH+6O
-→2CO
2+3H
2O+6e
-(4)
Discharged by the electrons that oxygen molecule seizes before, come back in the conduction band of Co-Sn composite oxides, the curved degree of bringing in material reduces, and forms depletion layer disappearance before, and the resistance of sensor reduces.R
afor sensor contacts the resistance after oxygen in atmosphere, R
gfor the resistance after sensor contacts ethanol, the resistance of survey sensor in air and ethanol is also by the sensitivity S defined formula of sensor: S=R
a/ R
g, can be calculated the sensitivity of sensor.
Advantage of the present invention:
(1) sensor utilizes material C o-Sn composite oxides, and it has good conductivity and chemical stability;
(2) utilize oxidation step cobalt composite tin oxide that the sensitivity of sensor can be made to significantly improve, promote that it is practical;
(3) Co-Sn composite oxides nanometer sheet utilizes hydrothermal method and one-step synthesis, and method is simple, the cheap commercial production being beneficial to mass.
Accompanying drawing explanation
The structural representation of Fig. 1: Co-Sn composite oxides ethanol sensor;
Fig. 2: comparative example, embodiment 1, embodiment 2 and embodiment 3, embodiment 4 working temperatures-Sensitivity comparison figure;
Fig. 3: the standard working curve of embodiment 2 pairs of concentration of alcohol-sensitivity.
As shown in Figure 1, each component names is: Al
2o
3insulating ceramics pipe (1), sensitive material (2), nickel-cadmium coil (3), platinum line (4), annular gold electrode (5);
The device of Fig. 2 made by comparative example and embodiment 1,2,3,4 is to the change curve of the sensitivity of 100ppm ethanol with working temperature.As can be seen from the figure, the optimum temperature of comparative example is at 225 DEG C, and sensitivity is 7.5.The optimum working temperature of embodiment 1,2,3,4 is 200 DEG C, and now sensitivity is respectively 2.1,201,93,17.Under optimum working temperature, the sensitivity of embodiment 2 is the highest, and the optimum working temperature of embodiment 2 is lower than the optimum working temperature of comparative example, and lower optimum working temperature is conducive to reducing power consumption.As can be seen here, the reaction efficiency of sensitive material and ethanol can be improved by Co-Sn composite oxides, and then obtain one there is highly sensitive Co-Sn composite oxides ethanol sensor.
Fig. 3 is the standard working curve of embodiment 2 in the concentration of alcohol-sensitivity of optimum working temperature 200 DEG C.Sensitivity test method: first sensor is put into gas cabinet, records the resistance at now platinum line two ends by the reometer be connected with sensor, obtain the aerial resistance value of sensor and R
a; Then use microsyringe in gas cabinet, injects the ethanol of 1 ~ 800ppm, obtain the resistance value of sensor in different concentration ethanol and R by measurement
g, according to the defined formula S=R of sensitivity S
a/ R
g, by calculating the sensitivity of variable concentrations lower sensor, finally obtain the standard working curve of concentration of alcohol-sensitivity.As can be seen from the figure, the Monitoring lower-cut of this sensor is 1ppm, and sensitivity is now 2.3; When concentration of alcohol is 800ppm, sensitivity is now 554.R is recorded by above-mentioned way during actual measurement
a, R
g, contrast with the standard working curve of concentration of alcohol-sensitivity after obtaining Sensitirity va1ue, thus obtain the ethanol content in human body respiration.In addition, as shown in the figure as gas concentration less (<100ppm), transducer sensitivity linear better, these features make Co-Sn composite oxides ethanol sensor can be good at being applied to ethanol in drunk driving and atmospheric environment to detect.
Embodiment
Comparative example:
Heater-type ethanol sensor is made, its concrete manufacturing process using tin-oxide nanometer film clips as sensitive material:
(1) first by 5.88gNa
3c
6h
5o
72H
2o, 1.8gSnCl
22H
2o, 5ml ethylenediamine, 10mlNaOH (0.4M) solution are dissolved in 20ml water when stirring, and stir and form homogeneous solution in 30 minutes;
(2) (1) mixed solution is put into 45ml polytetrafluoroethylkettle kettle to seal, put into 180 DEG C of baking ovens 12 hours, after terminating, Temperature fall is to room temperature, by sample collection ethanol and deionized water centrifugal after to be put in double dish 80 DEG C several hours, collection sample;
(3) above-mentioned nano gas sensitive material is calcined 2 hours at 300 DEG C, obtain gas sensitive material, this sensitive material and deionized water are mixed into pasty state, are then evenly coated in the insulation Al that commercially available outside surface carries 2 annular gold electrodes (5)
2o
3ceramic pipe (1) surface, form the sensitive material film (2) of 10 ~ 40 microns, the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, internal diameter is 0.8 ~ 1.0mm, and makes sensitive material cover annular gold electrode (5) completely;
(4) toast about 15 minutes under infrared lamp, after sensitive material drying, insulation Al
2o
3ceramic pipe (1) is calcined 2 hours at 300 DEG C; Then be that the NI-G heater coil (3) of 30 ~ 40 Ω is through insulation Al by resistance value
2o
3ceramic pipe (1) is inner as heater strip, is finally carried out welding and encapsulating according to general heater-type gas sensor by above-mentioned device, thus obtains Co-Sn composite oxides ethanol sensor of the present invention.
Embodiment 1:
The Co-Sn composite oxides that Elements C o/Sn mol ratio is 0.67:1 in reactant make ethanol sensor as sensitive material, and its manufacturing process is
(1) first by 7.35gNa
3c
6h
5o
72H
2o, 0.9gSnCl
22H
2o, 1.43gCoCl
26H
2o, 5ml ethylenediamine, 10mlNaOH (0.4M) solution are dissolved in 20ml water when stirring, and stir and form homogeneous solution in 30 minutes;
(2) (1) mixed solution is put into 45ml polytetrafluoroethylkettle kettle to seal, put into 180 DEG C of baking ovens 12 hours, after terminating, Temperature fall is to room temperature, by sample collection ethanol and deionized water centrifugal after to be put in double dish 80 DEG C several hours, collection sample;
(3) above-mentioned nano gas sensitive material is calcined 2 hours at 300 DEG C, obtain gas sensitive material, this sensitive material and deionized water are mixed into pasty state, are then evenly coated in the insulation Al that commercially available outside surface carries 2 annular gold electrodes (5)
2o
3ceramic pipe (1) surface, form the sensitive material film (2) of 10 ~ 40 microns, the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, internal diameter is 0.8 ~ 1.0mm, and makes sensitive material cover annular gold electrode (5) completely;
(4) toast about 15 minutes under infrared lamp, after sensitive material drying, insulation Al
2o
3ceramic pipe (1) is calcined 2 hours at 300 DEG C; Then be that the NI-G heater coil (3) of 30 ~ 40 Ω is through insulation Al by resistance value
2o
3ceramic pipe (1) is inner as heater strip, is finally carried out welding and encapsulating according to general heater-type gas sensor by above-mentioned device, thus obtains Co-Sn composite oxides ethanol sensor of the present invention.
Embodiment 2:
The Co-Sn composite oxides that Elements C o/Sn mol ratio is 1:1 in reactant make ethanol sensor as sensitive material, and its manufacturing process is
(1) first by 5.88gNa
3c
6h
5o
72H2O, 0.9gSnCl
22H
2o, 0.95gCoCl
26H
2o, 5ml ethylenediamine, 10mlNaOH (0.4M) solution are dissolved in 20ml water when stirring, and stir and form homogeneous solution in 30 minutes;
(2) (1) mixed solution is put into 45ml polytetrafluoroethylkettle kettle to seal, put into 180 DEG C of baking ovens 12 hours, after terminating, Temperature fall is to room temperature, by sample collection ethanol and deionized water centrifugal after to be put in double dish 80 DEG C several hours, collection sample;
(3) above-mentioned nano gas sensitive material is calcined 2 hours at 300 DEG C, obtain gas sensitive material, this sensitive material and deionized water are mixed into pasty state, are then evenly coated in the insulation Al that commercially available outside surface carries 2 annular gold electrodes (5)
2o
3ceramic pipe (1) surface, form the sensitive material film (2) of 10 ~ 40 microns, the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, internal diameter is 0.8 ~ 1.0mm, and makes sensitive material cover annular gold electrode (5) completely;
(4) toast about 15 minutes under infrared lamp, after sensitive material drying, insulation Al
2o
3ceramic pipe (1) is calcined 2 hours at 300 DEG C; Then be that the NI-G heater coil (3) of 30 ~ 40 Ω is through insulation Al by resistance value
2o
3ceramic pipe (1) is inner as heater strip, is finally carried out welding and encapsulating according to general heater-type gas sensor by above-mentioned device, thus obtains Co-Sn composite oxides ethanol sensor of the present invention.
Embodiment 3:
The Co-Sn composite oxides that Elements C o/Sn mol ratio is 2:1 in reactant make ethanol sensor as sensitive material, and its manufacturing process is
(1) first by 4.41gNa
3c
6h
5o
72H
2o, 0.9gSnCl
22H
2o, 0.476gCoCl
26H
2o, 5ml ethylenediamine, 10mlNaOH (0.4M) solution are dissolved in 20ml water when stirring, and stir and form homogeneous solution in 30 minutes;
(2) (1) mixed solution is put into 45ml polytetrafluoroethylkettle kettle to seal, put into 180 DEG C of baking ovens 12 hours, after terminating, Temperature fall is to room temperature, by sample collection ethanol and deionized water centrifugal after to be put in double dish 80 DEG C several hours, collection sample;
(3) above-mentioned nano gas sensitive material is calcined 2 hours at 300 DEG C, obtain gas sensitive material, this sensitive material and deionized water are mixed into pasty state, are then evenly coated in the insulation Al that commercially available outside surface carries 2 annular gold electrodes (5)
2o
3ceramic pipe (1) surface, form the sensitive material film (2) of 10 ~ 40 microns, the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, internal diameter is 0.8 ~ 1.0mm, and makes sensitive material cover annular gold electrode (5) completely;
(4) toast about 15 minutes under infrared lamp, after sensitive material drying, insulation Al
2o
3ceramic pipe (1) is calcined 2 hours at 300 DEG C; Then be that the NI-G heater coil (3) of 30 ~ 40 Ω is through insulation Al by resistance value
2o
3ceramic pipe (1) is inner as heater strip, is finally carried out welding and encapsulating according to general heater-type gas sensor by above-mentioned device, thus obtains Co-Sn composite oxides ethanol sensor of the present invention.
Embodiment 4:
The Co-Sn composite oxides that Elements C o/Sn mol ratio is 10:1 in reactant make ethanol sensor as sensitive material, and its manufacturing process is
(1) first by 3.23gNa
3c
6h
5o
72H
2o, 0.9gSnCl
22H
2o, 0.095gCoCl
26H
2o, 5ml ethylenediamine, 10mlNaOH (0.4M) solution are dissolved in 20ml water when stirring, and stir and form homogeneous solution in 30 minutes;
(2) (1) mixed solution is put into 45ml polytetrafluoroethylkettle kettle to seal, put into 180 DEG C of baking ovens 12 hours, after terminating, Temperature fall is to room temperature, by sample collection ethanol and deionized water centrifugal after to be put in double dish 80 DEG C several hours, collection sample;
(3) above-mentioned nano gas sensitive material is calcined 2 hours at 300 DEG C, obtain gas sensitive material, this sensitive material and deionized water are mixed into pasty state, are then evenly coated in the insulation Al that commercially available outside surface carries 2 annular gold electrodes (5)
2o
3ceramic pipe (1) surface, form the sensitive material film (2) of 10 ~ 40 microns, the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, internal diameter is 0.8 ~ 1.0mm, and makes sensitive material cover annular gold electrode (5) completely;
(4) toast about 15 minutes under infrared lamp, after sensitive material drying, insulation Al
2o
3ceramic pipe (1) is calcined 2 hours at 300 DEG C; Then be that the NI-G heater coil (3) of 30 ~ 40 Ω is through insulation Al by resistance value
2o
3ceramic pipe (1) is inner as heater strip, is finally carried out welding and encapsulating according to general heater-type gas sensor by above-mentioned device, thus obtains Co-Sn composite oxides ethanol sensor of the present invention.
Claims (5)
1. a Co-Sn composite oxides ethanol sensor, by the Al of outside surface with 2 annular gold electrodes (5)
2o
3insulating ceramics pipe (1), be coated in annular gold electrode (5) and Al
2o
3the sensitive material (2) of insulating ceramics pipe (1) outside surface, through Al
2o
3the nickel-cadmium heater coil (3) that insulating ceramics pipe (1) is inner and platinum line (4) composition for conducting electricity; It is characterized in that: sensitive material (2) is Co-Sn composite oxides, this sensitive material is the preparation of employing one step hydrothermal technique, through calcining, is coated in annular gold electrode (5) and Al
2o
3insulating ceramics pipe (1) outside surface.
2. Co-Sn composite oxides ethanol sensor as claimed in claim 1, is characterized in that: the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, and internal diameter is 0.8 ~ 1.0mm.
3. the preparation method of a kind of Co-Sn composite oxides ethanol sensor according to claim 1, its step is as follows:
(1) first by 5.88gNa
3c
6h
5o
72H
2o, 0.9gSnCl
22H
2o, 0.95gCoCl
26H
2o, 5ml ethylenediamine, 10mlNaOH (0.4M) solution are dissolved in 20ml water when stirring, and stir and form homogeneous solution in 30 minutes;
(2) (1) mixed solution is put into 45ml polytetrafluoroethylkettle kettle to seal, put into 180 DEG C of baking ovens 12 hours, after terminating, Temperature fall is to room temperature, by sample collection ethanol and deionized water centrifugal after to be put in double dish 80 DEG C several hours, collection sample;
(3) above-mentioned nano gas sensitive material is calcined 2 hours at 300 DEG C, obtain gas sensitive material, this sensitive material and deionized water are mixed into pasty state, are then evenly coated in the insulation Al that commercially available outside surface carries 2 annular gold electrodes (5)
2o
3ceramic pipe (1) surface, form the sensitive material film (2) of 10 ~ 40 microns, the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, internal diameter is 0.8 ~ 1.0mm, and makes sensitive material cover annular gold electrode (5) completely;
(4) toast about 15 minutes under infrared lamp, after sensitive material drying, insulation Al
2o
3ceramic pipe (1) is calcined 2 hours at 300 DEG C; Then be that the NI-G heater coil (3) of 30 ~ 40 Ω is through insulation Al by resistance value
2o
3ceramic pipe (1) is inner as heater strip, is finally carried out welding and encapsulating according to general heater-type gas sensor by above-mentioned device, thus obtains Co-Sn composite oxides ethanol sensor of the present invention.
4. a kind of Co-Sn composite oxides ethanol sensor according to claim 1, it is characterized in that: step fabricated in situ Co-Sn composite oxides are as sensitive material, the compound of one side's cobalt/cobalt oxide changes the catalytic capability of tin-oxide nanometer film clips, more reactivity site can be provided, these two aspects all significantly can improve the reaction efficiency of gas and sensitive material, and then improve the sensitivity of sensor, on the other hand in Co-Sn composite oxide particle and a large amount of heterojunction can be formed between particle, the appearance of these heterojunction can provide more reactivity site, these two aspects all significantly can improve the reaction efficiency of gas and sensitive material, and then improve the sensitivity of sensor.
5. the application that detects in drunk driving and atmospheric environment of a kind of Co-Sn composite oxides ethanol sensor as claimed in claim 4, is characterized in that: for detecting concentration of alcohol in expiratory air and atmospheric environment.
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| CN110455874A (en) * | 2019-08-22 | 2019-11-15 | 有研工程技术研究院有限公司 | A kind of CoSn double metal oxide semiconductor material and preparation method thereof |
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| CN106970118A (en) * | 2017-03-28 | 2017-07-21 | 吉林大学 | A kind of CoO/SnO2Composition of sensitive material and preparation method thereof |
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| CN110616420A (en) * | 2019-10-24 | 2019-12-27 | 江西科技师范大学 | Preparation method of composite anti-corrosion coating for inner wall of waste incinerator |
| CN110616420B (en) * | 2019-10-24 | 2021-06-29 | 江西科技师范大学 | Preparation method of composite anti-corrosion coating for inner wall of waste incinerator |
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