CN110082406A - One kind being based on SnO2-Co3O4The dimethylbenzene gas sensor and preparation method thereof of hetero-junctions nanostructure sensitive material - Google Patents
One kind being based on SnO2-Co3O4The dimethylbenzene gas sensor and preparation method thereof of hetero-junctions nanostructure sensitive material Download PDFInfo
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Abstract
One kind being based on SnO2‑Co3O4The dimethylbenzene gas sensor and preparation method thereof of hetero-junctions nanostructure sensitive material, belongs to conductor oxidate gas sensor technical field.The ceramic tube substrate of two parallel, cyclic annular and separate gold electrodes is had, coated in the SnO on ceramic tube outer surface and gold electrode by outer surface2‑Co3O4Hetero-junctions nanostructure sensitive material, the nichrome heater strip being placed in ceramic tube composition；It is of the present invention to be based on SnO2‑Co3O4The sensor paraxylene of hetero-junctions nanostructure sensitive material shows excellent sensitivity (101.9~100ppm) and lower Monitoring lower-cut (0.05ppm).Prepare device simple process, it is small in size, be suitable for produce in enormous quantities, detection microenvironment in xylene pollution object space face have broad application prospects.
Description
Technical field
The invention belongs to conductor oxidate gas sensor technical fields, and in particular to one kind is based on SnO2-Co3O4It is different
The dimethylbenzene gas sensor and preparation method thereof of matter knot nanostructure sensitive material.
Background technique
Dimethylbenzene is widely used in the industries such as coating, resin, dyestuff, ink and makees solvent；For the row such as medicine, explosive, pesticide
Industry does synthon or solvent；Also it can be used as high octane gasoline component, be the important source material of organic chemical industry.However, being similar to
Other organic solvents, dimethylbenzene is to eyes and the irritating effect of the upper respiratory tract, when high concentration, there is anesthesia to make cental system
With.Therefore, it develops with highly sensitive and Trace gas detection lower limit dimethylbenzene gas sensor with highly important
Meaning.
In the gas sensor of huge number, using conductor oxidate as the resistor-type gas sensing utensil of sensitive material
Have the advantages that high sensitivity, Monitoring lower-cut are low, selectivity is good, response and resume speed are fast, production method is simple, cost is relatively low,
It is one of current most widely used gas sensor.With the development of nanometer science and technology, by gas sensitive regulation at receiving
Rice structure can greatly improve the specific surface area of material, increase active site, gas-sensitive property can be made to be improved.In addition,
By combining two kinds of gas sensitives, gas sensitive can be made further to be changed using the synergistic effect between them
Property, to obtain better gas-sensitive property.
Co3O4As a kind of representative p-type semiconductor functional material, be suitable for such as lithium ion battery, supercapacitor and
The application in the various fields such as heterogeneous catalysis, but since they usually have response more lower than n-type semiconductor, so including
Co3O4All p-type semiconductor oxides inside are seldom used for Application in Sensing with its primitive form.However have benefited from Co3O4Have
The advantages of good catalytic effect and high absorption oxygen, so that it still has very big Development volue in the application of sensory field.
By the way that two or more semiconductor combinations with different band gap to form hetero-junctions, can be optimized the air-sensitive of gas sensor
Characteristic.Therefore the present invention combines SnO2The advantages that high electron mobility and high chemical stability, to Co3O4Material further changes
Property, so that the gas-sensitive property of gas sensor significantly improves.
Summary of the invention
The object of the present invention is to provide one kind to be based on SnO2-Co3O4The diformazan benzene gas of hetero-junctions nanostructure sensitive material
Sensor and preparation method thereof.
Utilize SnO2-Co3O4Hetero-junctions nanostructure is as sensitive material, one side Co3O4All have to a variety of VOC gas
Preferable catalytic oxidation activity, and still can be played very for the lower gas of benzene,toluene,xylene one kind reactivity
Good catalytic effect；On the other hand pass through SnO2After modification, Co is greatly improved3O4Hetero-junctions nanostructure ratio table
Area, so that absorption oxygen ability enhancing, so more oxygen molecules can be caused to participate in reaction；Further, since SnO2With Co3O4It
Between the presence of hetero-junctions lead to the more obvious of the resistance variations of sensitive material so that the modulating action of carrier is more obvious.
The reaction efficiency of gas and sensitive material greatly improved in the collective effect of this three aspect, and then improves the sensitive of sensor
Degree.Commercially available tubular structure sensor manufacturing process of the present invention is simple, small in size, is conducive to industrial batch production,
Therefore there is important application value.
It is of the present invention to be based on SnO2-Co3O4The dimethylbenzene gas sensor of hetero-junctions nanostructure sensitive material, by
Outer surface has the ceramic tube substrate of two parallel, cyclic annular and separate gold electrodes, is coated in ceramic tube outer surface and gold
Sensitive material on electrode, the nichrome heater strip being placed in ceramic tube composition；It is characterized by: sensitive material is SnO2-
Co3O4Hetero-junctions nanostructure sensitive material, and be prepared by following steps:
(1) 15~30mL deionized water and 15~30mL ethylene glycol are measured first, are stirred evenly after being mixed；
(2) cobalt acetate (C is hydrated by the four of 0.2~0.3g4H6CoO4·4H2O), the polyvinylpyrrolidone of 0.4~0.6g
(PVP), the glutamic acid (L-Glutamic acid) of 0.4~0.6g is added to the deionized water of step (1) and the mixing of ethylene glycol
In solution；After stirring 10~20 minutes, the urea (CH of 0.1~0.2g is added4N2) and the five water chlorinations of 0.05~0.06g O
Tin (SnCl4.5H2O), and constantly stirring is kept until it is all dissolved；
(3) solution that step (2) obtains is transferred in water heating kettle, is taken after being kept for 12~14 hours at 150~190 DEG C
Out, by the multiple eccentric cleaning of precipitating deionized water and ethyl alcohol of generation after cooled to room temperature, after being dried at room temperature for again
It is calcined 1~2 hour at 400~500 DEG C, to obtain SnO2-Co3O4Hetero-junctions nanostructured powders.
It is of the present invention a kind of based on SnO2-Co3O4The dimethylbenzene gas sensor of hetero-junctions nanostructure sensitive material
Preparation method, its step are as follows:
1. taking suitable deionized water and SnO2-Co3O4Hetero-junctions nanostructured powders uniformly mix, and grind and to form paste
Then shape slurry dips a small amount of slurry and is uniformly coated on outer surface parallel with two, ring-type and gold electrode separate
Al2O3Ceramic pipe surface, forms the sensitive material film of 10~30 μ m-thicks, and makes sensitive material that annular gold electrode be completely covered；
2. being toasted 30~45 minutes under infrared lamp, after sensitive material film is dry, then by Al2O3Ceramic tube 400~
It is calcined 2~3 hours at 450 DEG C；Then the nickel chromium triangle heating coil that resistance value is 30~40 Ω is passed through into Al2O3Ceramic tube inside is made
For heater strip, finally above-mentioned device is welded and encapsulated according to heater-type gas sensor, to obtain based on SnO2-Co3O4
The dimethylbenzene gas sensor of hetero-junctions nanostructure sensitive material.
It is prepared by the present invention to be based on SnO2-Co3O4The dimethylbenzene gas sensor of hetero-junctions nanostructure sensitive material has
Following advantages:
1. successfully preparing SnO using simple one step hydro thermal method2-Co3O4Hetero-junctions nanostructure sensitive material, preparation
Method is simple, low in cost；
2. by by SnO2With Co3O4Two kinds of materials combine, and significantly improve Co3O4Base gas sensor paraxylene
Selectivity and sensitivity (101.9-100ppm) reduce the gas concentration Monitoring lower-cut (1.2-0.05ppm) of sensor, and have
There is good stability, has broad application prospects in terms of xylene content in detection microenvironment；
3. using commercially available tubular type sensor, device technology is simple, small in size, is suitable for producing in enormous quantities.
Detailed description of the invention
Fig. 1 a and Fig. 1 b are respectively pure Co3O4Nanostructure sensitive material and SnO2-Co3O4Hetero-junctions nanostructure sensitivity material
The SEM shape appearance figure of material；
Fig. 2 a, Fig. 2 b, Fig. 2 c are respectively pure Co3O4The low resolution of nanostructure sensitive material and high-resolution TEM
Figure；Fig. 2 d, Fig. 2 e, Fig. 2 f are respectively SnO2-Co3O4The low resolution and high-resolution TEM of hetero-junctions nanostructure sensitive material
Figure；
Fig. 3: pure Co3O4Nanostructure sensitive material and SnO2-Co3O4The XRD diagram of hetero-junctions nanostructure sensitive material；
Fig. 4: sensitivity of sensor at a temperature of different operating to 100ppm diformazan benzene gas in comparative example and embodiment
Curve；
Fig. 5 a: sensor is under optimum working temperature (175 DEG C) to 7 kinds of 100ppm under test gas in comparative example and embodiment
Selectivity curve；
Fig. 5 b: sensor is at a temperature of different operating to the selectivity curve of 7 kinds of 100ppm under test gas in embodiment；
Fig. 6: sensitivity-xylene concentration of the sensor under optimum working temperature (175 DEG C) in comparative example and embodiment
Characteristic curve
Fig. 7 a: sensor is under optimum working temperature (175 DEG C) to 0.05ppm~1ppm diformazan benzene gas in embodiment
Respond recovery curve；
Fig. 7 b: sensor is under optimum working temperature (175 DEG C) to 3ppm~200ppm diformazan benzene gas in embodiment
Respond recovery curve；
Fig. 8: sensor is under optimum working temperature (175 DEG C) to the sensitivity of 100ppm diformazan benzene gas in embodiment
Linearity curve steady in a long-term；
As shown in Figure 1, pure Co3O4Nanostructure sensitive material is bobbles shape, and single nanometer bobbles is made of nano wire, receives
The diameter of popped rice ball is about 2~4 μm.SnO2-Co3O4Hetero-junctions nanostructure sensitive material shows nano particle composition not
Regular texture.
As shown in Fig. 2, pure Co3O4The TEM figure and pattern shown in SEM figure of nanostructure sensitive material are unified, for by many
The nanometer bobbles structure that nano wire is constituted, high-resolution TEM figure shows the spacing of lattice of 0.286nm wide, with pure Co3O4(220)
Crystal face coincide.SnO2-Co3O4The TEM figure of hetero-junctions nanostructure sensitive material is unified with pattern shown in SEM figure, is nanometer
The irregular structure of grain composition, high-resolution TEM figure shows the spacing of lattice of 0.286nm and 0.334nm wide, respectively with Co3O4's
(220) and SnO2(1100) crystal face coincide.
As shown in figure 3, SnO2-Co3O4The XRD spectra and pure Co of hetero-junctions nanostructure sensitive material3O4Nanostructure is quick
The XRD spectra of sense material is compared, Co3O4Characteristic peak coincide, remaining characteristic peak and SnO2Characteristic peak matches, and without more
Remaining characteristic peak, it was demonstrated that SnO2-Co3O4Hetero-junctions nanostructure sensitive material is by SnO2With Co3O4Composition.
As shown in figure 4, the optimum working temperature of the sensor in comparative example and embodiment is 175 DEG C, device pair at this time
The sensitivity of 100ppm dimethylbenzene is respectively 6.2 and 101.9, and 16.4 times of sensitivity enhancement.
As shown in figure 5, biography under the conditions of optimum working temperature, for sensor in comparative example, in embodiment
The sensitivity enhancement of sensor is obvious, and the selectivity of paraxylene is best.Simultaneously under the conditions of different temperature, in embodiment
Sensor still paraxylene show best selectivity.
As shown in fig. 6, under the conditions of optimum working temperature, for sensor in comparative example, with dimethylbenzene gas
The sensitivity enhancement of the increase of bulk concentration, the sensor in embodiment is more obvious.
As shown in fig. 7, implementing ratio sensor shows excellent response and recovery characteristics to the dimethylbenzene of various concentration.This
Outside, the Monitoring lower-cut for implementing ratio sensor is lower, can achieve ppb rank, also has preferable response to low concentration dimethylbenzene, right
The sensitivity of 50ppb dimethylbenzene is 1.2.
As shown in figure 8, the sensor in embodiment at a temperature of 175 DEG C that works exists in 30 days of follow-on test
Sensitivity curve fluctuation in 100ppm diformazan benzene gas is smaller, shows its good long-time stability.
The sensitivity (p-type semiconductor) of device is defined as its resistance value in tested gas in test reducibility gas
(Rg) with resistance value (R in airaThe ratio between) size, as S=Rg/Ra.During the test, using static test system into
Row test.Device is placed in the gas tank of 50~80L, a certain amount of organic gas to be measured is inwardly injected, observes and records its resistance
Value variation, is obtained by calculation corresponding sensitivity number.
Specific embodiment
Comparative example 1:
With pure Co3O4Nanostructure makes dimethylbenzene sensor as sensitive material, specific manufacturing process:
(1) 20mL deionized water and 20mL ethylene glycol are measured first, are poured into beaker, and constantly stir；
(2) 0.25g tetra- is hydrated cobalt acetate, 0.5g polyvinylpyrrolidone, 0.5g glutamic acid be added to deionized water with
In the mixed uniformly beaker of ethylene glycol；After stirring 15 minutes, 0.2g urea is added, and keeps constantly stirring until it is complete
Portion's dissolution；
(3) above-mentioned solution is transferred in water heating kettle, is taken out after being kept for 12 hours at 160 DEG C, cooled to room temperature
Afterwards by the multiple eccentric cleaning of precipitating deionized water and ethyl alcohol of generation, 2 are calcined at 450 DEG C again after being then dried at room temperature for
Hour, to obtain pure Co3O4Nanostructure sensitive material powder.
(4) suitable deionized water and pure Co are taken3O4Nanostructure sensitive material powder uniformly mixes, and grinds and to form paste
Then shape slurry dips a small amount of slurry and is uniformly coated on the Al that outer surface comes with 2 annular gold electrodes2O3Ceramic pipe surface,
The sensitive material film of 40 μ m-thicks is formed, and makes sensitive material that annular gold electrode be completely covered；
(5) it is toasted 40 minutes under infrared lamp, after sensitive material is dry, Al2O3It is small that ceramic tube calcines 2 at 450 DEG C
When；Then the nickel chromium triangle heating coil that resistance value is 35 Ω is passed through into Al2O3Ceramic tube inside is as heater strip, finally by above-mentioned device
Part is welded and is encapsulated according to general heater-type gas sensor, to obtain based on pure Co3O4The two of nanostructure sensitive material
Toluene gas sensor.
Embodiment 1:
Use SnO2-Co3O4Hetero-junctions nanostructure makes dimethylbenzene sensor as sensitive material, specifically makes
Journey:
(1) 20mL deionized water and 20mL ethylene glycol are measured first, are poured into beaker, and constantly stir；
(2) 0.25g tetra- is hydrated cobalt acetate, 0.5g polyvinylpyrrolidone, 0.5g glutamic acid be added to deionized water with
In the mixed uniformly beaker of ethylene glycol；After stirring 15 minutes, 0.2g urea and 0.05g stannic chloride pentahydrate are added, and protect
Constantly stirring is held until it is all dissolved；
(3) above-mentioned solution is transferred in water heating kettle, is taken out after being kept for 12 hours at 160 DEG C, cooled to room temperature
Afterwards by the multiple eccentric cleaning of precipitating deionized water and ethyl alcohol of generation, 2 are calcined at 450 DEG C again after being then dried at room temperature for
Hour, to obtain SnO2-Co3O4Hetero-junctions nanostructured powders.
(4) suitable deionized water and SnO are taken2-Co3O4Hetero-junctions nanostructured powders uniformly mix, and grind and to form paste
Then shape slurry dips a small amount of slurry and is uniformly coated on the Al that outer surface comes with 2 annular gold electrodes2O3Ceramic pipe surface,
The sensitive material film of 40 μ m-thicks is formed, and makes sensitive material that annular gold electrode be completely covered；
(5) it is toasted 40 minutes under infrared lamp, after sensitive material is dry, Al2O3It is small that ceramic tube calcines 2 at 450 DEG C
When；Then the nickel chromium triangle heating coil that resistance value is 35 Ω is passed through into Al2O3Ceramic tube inside is as heater strip, finally by above-mentioned device
Part is welded and is encapsulated according to general heater-type gas sensor, to obtain based on SnO2-Co3O4Hetero-junctions nanostructure is quick
Feel the dimethylbenzene gas sensor of material.
Claims (2)
1. one kind is based on SnO2-Co3O4The dimethylbenzene gas sensor of hetero-junctions nanostructure sensitive material, is had by outer surface
The ceramic tube substrate of two parallel, cyclic annular and separate gold electrodes, coated in quick on ceramic tube outer surface and gold electrode
Sense material, the nichrome heater strip composition being placed in ceramic tube；It is characterized by: sensitive material is SnO2-Co3O4Hetero-junctions
Nanostructure sensitive material, and be prepared by following steps,
(1) 15~30mL deionized water and 15~30mL ethylene glycol are measured first, are stirred evenly after being mixed；
(2) glutamic acid for being hydrated cobalt acetates, the polyvinylpyrrolidone of 0.4~0.6g, 0.4~0.6g for the four of 0.2~0.3g
It is added in the deionized water of step (1) and the mixed solution of ethylene glycol；After stirring 10~20 minutes, 0.1 is added~
The urea of 0.2g and the stannic chloride pentahydrate of 0.05~0.06g, and constantly stirring is kept until it is all dissolved；
(3) solution that step (2) obtains is transferred in water heating kettle, is taken out after being kept for 12~14 hours at 150~190 DEG C,
By the multiple eccentric cleaning of precipitating deionized water and ethyl alcohol of generation after cooled to room temperature, exist again after being dried at room temperature for
It is calcined 1~2 hour at 400~500 DEG C, to obtain SnO2-Co3O4Hetero-junctions nanostructured powders.
2. described in claim 1 a kind of based on SnO2-Co3O4The dimethylbenzene gas sensing of hetero-junctions nanostructure sensitive material
The preparation method of device, its step are as follows:
1. taking suitable deionized water and SnO2-Co3O4Hetero-junctions nanostructured powders uniformly mix, and grind and form paste slurry
Then material dips a small amount of slurry and is uniformly coated on outer surface parallel with two, ring-type and gold electrode separate
Al2O3Ceramic pipe surface, forms the sensitive material film of 10~30 μ m-thicks, and makes sensitive material that annular gold electrode be completely covered；
2. being toasted 30~45 minutes under infrared lamp, after sensitive material film is dry, then by Al2O3Ceramic tube is 400~450
It is calcined 2~3 hours at DEG C；Then the nickel chromium triangle heating coil that resistance value is 30~40 Ω is passed through into Al2O3Ceramic tube inside, which is used as, to be added
Heated filament is finally welded and is encapsulated according to heater-type gas sensor, to obtain based on SnO2-Co3O4Hetero-junctions nanostructure
The dimethylbenzene gas sensor of sensitive material.
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Cited By (5)
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| CN110455891A (en) * | 2019-08-20 | 2019-11-15 | 吉林大学 | Based on CoWO4-Co3O4The dimethylbenzene gas sensor and preparation method thereof of hetero-junctions nanostructure sensitive material |
| CN111111677A (en) * | 2020-01-06 | 2020-05-08 | 辽宁大学 | Preparation method of tin oxide composite cobaltosic oxide photo-thermal catalyst and application of tin oxide composite cobaltosic oxide photo-thermal catalyst in thermal catalysis |
| CN111167434A (en) * | 2020-02-14 | 2020-05-19 | 辽宁大学 | Photocatalytic composite material Cr for degrading gaseous pollutants2O3-SnO2And preparation method and application thereof |
| CN113295737A (en) * | 2021-05-17 | 2021-08-24 | 电子科技大学长三角研究院(湖州) | Manganese-doped cobaltosic oxide porous nano flaky material and preparation method and application thereof |
| CN116145286A (en) * | 2023-01-03 | 2023-05-23 | 吉林大学 | Cobalt-based nanofiber sensitive material capable of effectively detecting ultralow-concentration xylene at low working temperature, preparation method and application |
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| CN111111677A (en) * | 2020-01-06 | 2020-05-08 | 辽宁大学 | Preparation method of tin oxide composite cobaltosic oxide photo-thermal catalyst and application of tin oxide composite cobaltosic oxide photo-thermal catalyst in thermal catalysis |
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| CN113295737A (en) * | 2021-05-17 | 2021-08-24 | 电子科技大学长三角研究院(湖州) | Manganese-doped cobaltosic oxide porous nano flaky material and preparation method and application thereof |
| CN113295737B (en) * | 2021-05-17 | 2022-10-18 | 电子科技大学长三角研究院(湖州) | Manganese-doped cobaltosic oxide porous nano flaky material and preparation method and application thereof |
| CN116145286A (en) * | 2023-01-03 | 2023-05-23 | 吉林大学 | Cobalt-based nanofiber sensitive material capable of effectively detecting ultralow-concentration xylene at low working temperature, preparation method and application |
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Application publication date: 20190802 |