CN105572175A - Preparation method and application of xylene gas sensor based on titanium dioxide nanosheet - Google Patents
Preparation method and application of xylene gas sensor based on titanium dioxide nanosheet Download PDFInfo
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- CN105572175A CN105572175A CN201610101704.7A CN201610101704A CN105572175A CN 105572175 A CN105572175 A CN 105572175A CN 201610101704 A CN201610101704 A CN 201610101704A CN 105572175 A CN105572175 A CN 105572175A
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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
Abstract
The invention relates to a preparation method of a xylene gas sensor, in particular to a gas-sensitive sensor which is constructed on the basis of a bi-metal co-doping two-dimensional nanomaterial and can be used for detecting the content of xylene gas in an environment, and belongs to the technical field of novel nano functional materials and environmental monitoring. The method comprises the steps that the iron and manganese bi-metal co-doping titanium dioxide nanosheet in-situ composited carbon nitride two-dimensional nanocomposite FeMn-TiO2/g-C3N4 is prepared firstly, and by means of the multiple characteristics that the material is large in specific surface area, mesopores can achieve high gas absorption, and electron transfer is affected by surface gas changes of the material and then affects the sensitivity, construction of the gas-sensitive sensor which has a sensitive and rapid response to the xylene gas is achieved.
Description
Technical field
The present invention relates to a kind of preparation method of dimethylbenzene gas sensor.Belong to Nano-function thin films and environmental monitoring technology field.
Background technology
Dimethylbenzene toluene is used as solvent and high-knock rating gasoline adjuvant in a large number, is also the important source material of organic chemical industry, volatile.Can there is neurasthenic syndrome, hepatomegaly in human body Long Term Contact dimethylbenzene, woman worker's menoxenia etc.Dry skin, chap, dermatitis.
Detection method for dimethylbenzene gas mainly contains chemical analysis method and instrument testing method.Though chemical analysis method is simple to operate, the shortcomings such as sensitivity is not high and cannot reuse; Instrument testing method, the main dimethylbenzene gas control instrument that uses quantitatively detects the toluene gas concentration in air, has highly sensitive, reusable, automaticity advantages of higher, and is widely applied in the middle of commercial production.
For the dimethylbenzene gas detecting instrument that instrument testing method uses, most crucial parts are gas sensors that P-xylene gas has qualitative, quantitative response, are namely coated with the gas sensor of different nano-functional material.Gas sensor is a kind of sensor detecting specific gas, and principle can be drifted about with the change of external environment based on the velocity of wave of SAW (Surface Acoustic Wave) device and frequency.It mainly comprises semiconductor gas sensor, catalytic combustion type gas sensor and Electro-chemical Gas Sensor etc., and wherein maximum are semiconductor gas sensors.
Sensitivity is the important sign of gas sensor gas-sensitive property.Sensitivity definition is the resistance value R of sensor in air atmosphere
awith the resistance value R of sensor in certain density tested gas atmosphere
gratio, namely
Therefore, probe into the gas sensing materials that adsorbability is strong, stability good, catalytic activity is high, P-xylene gas has specific recognition and can quantitatively detect, and then preparation have highly sensitive, response fast, the dimethylbenzene gas sensor of the characteristic such as release time is short has important using value to commercial production, human health, is also the Focal point and difficult point of environmental monitoring technology area research simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of prepare simple, highly sensitive, detect and can be used for the preparation method of the gas sensor of dimethylbenzene gas detect fast, prepared sensor, can be used for quick, the Sensitive Detection of dimethylbenzene gas.Based on this object, based on this object, first the present invention has prepared a kind of thermometal codope two-dimension nano materials, i.e. the titanium dioxide nanoplate In-situ reaction carbonitride two-dimensional nano compound substance FeMn-TiO of iron and manganese thermometal codope
2/ g-C
3n
4, utilize the large specific surface area of this material, mesoporous high gas absorption characteristic and electron transmission to affect responsive many characteristics by the change of material surface gas, achieve the structure that P-xylene gas has the gas sensor of sensitive, quick response.
The technical solution used in the present invention is as follows:
1., based on a preparation method for the dimethylbenzene gas sensor of titanium dioxide nanoplate, described titanium dioxide nanoplate is the titanium dioxide nanoplate In-situ reaction carbonitride two-dimensional nano compound substance FeMn-TiO of iron and manganese thermometal codope
2/ g-C
3n
4;
It is characterized in that, described preparation method comprises following preparation process:
(1) FeMn-TiO
2/ g-C
3n
4preparation;
(2) preparation of dimethylbenzene gas sensor;
Wherein, step (1) prepares FeMn-TiO
2/ g-C
3n
4concrete steps be:
First, get 0.8mmol molysite and 0.8 ~ 1.2mmol manganese salt joins in 5mL butyl titanate, in whipping process, slowly add 0.5 ~ 0.8mL hydrofluorite, 18 ~ 24 hours are reacted in a kettle. at 160 ~ 200 DEG C, after being cooled to room temperature, after ultrapure water and absolute ethyl alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 150 ~ 250mg and mix with 400mg melamine, and grind into powder; Then, the powder of grinding is put into muffle furnace, programming rate is 1 ~ 3 DEG C/min, calcines 0.5 ~ 5 hour at 480 ~ 560 DEG C; Finally, the powder after calcining is cooled to room temperature, i.e. obtained FeMn-TiO
2/ g-C
3n
4;
Described molysite is selected from one of following: iron sulfate, iron chloride, ferric nitrate;
Described manganese salt is selected from one of following: manganese sulfate, manganese chloride, manganese nitrate;
The concrete steps that step (2) prepares dimethylbenzene gas sensor are:
First, the FeMn-TiO of preparation in step (1) is got
2/ g-C
3n
4100mg and 0.5 ~ 2.0mmol sylvite are placed in mortar, add absolute ethyl alcohol, are evenly coated in insulating ceramics tube-surface and form film, at room temperature dry after being ground to pasty state; Then, the platinum filament of ceramic pipe both sides and heater strip are welded with base; Finally, the element welded is placed in detecting instrument, by regulating heating voltage to carry out burin-in process to 4.22V, i.e. obtained dimethylbenzene gas sensor;
Described sylvite is selected from one of following: potassium sulfate, potassium chloride, potassium nitrate.
2. the application of the dimethylbenzene gas sensor prepared by preparation method of the present invention, is characterized in that, can be applied to the detection of dimethylbenzene gas, detect and be limited to 0.001mg/m
3.
Useful achievement of the present invention
(1) dimethylbenzene gas sensor preparation of the present invention is simple, easy to operate, achieves and detects quick, sensitive, the high selectivity of toluene gas, have market development prospect;
(2) the present invention has prepared novel photochromics FeMn-TiO first
2/ g-C
3n
4fully contact with titanium dioxide nanoplate due to growth in situ on titanium dioxide nanoplate of iron, manganese, utilize the effect of metal surface plasma body and the mutual promoting action of the two of iron, manganese, effectively improve semiconductor substrate electron transmission ability and catalytic activity, although solve the larger and mesoporous high gas absorption characteristic of titanium dioxide nanoplate specific surface area to be applicable to air-sensitive host material, the technical matters that gas-sensitive activity is not high and impedance variation is unstable; Simultaneously due to carbonitride g-C
3n
4good electric conductivity, add titanium dioxide nanoplate abundant dispersion thereon, greatly increase electron transmission ability, solve the impedance of air-sensitive host material with gas change the technical matters that responds fast; And, by the doping of potassium ion, solve the technical matters of specific detection dimethylbenzene gas.Therefore, effective preparation of this material, has important scientific meaning and using value.
Embodiment
Embodiment 1FeMn-TiO
2/ g-C
3n
4preparation
First, 0.8mmol molysite is got and 0.8mmol manganese salt joins in 5mL butyl titanate, in whipping process, slowly add 0.5mL hydrofluorite, at 160 DEG C, react 24 hours, after being cooled to room temperature in a kettle., after ultrapure water and absolute ethyl alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 150mg and mix with 400mg melamine, and grind into powder; Then, the powder of grinding is put into muffle furnace, programming rate is 1 DEG C/min, calcines 5 hours at 480 DEG C; Finally, the powder after calcining is cooled to room temperature, i.e. obtained FeMn-TiO
2/ g-C
3n
4;
Described molysite is iron sulfate;
Described manganese salt is manganese sulfate.
Embodiment 2FeMn-TiO
2/ g-C
3n
4preparation
First, 0.8mmol molysite is got and 1.0mmol manganese salt joins in 5mL butyl titanate, in whipping process, slowly add 0.65mL hydrofluorite, at 180 DEG C, react 21 hours, after being cooled to room temperature in a kettle., after ultrapure water and absolute ethyl alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 200mg and mix with 400mg melamine, and grind into powder; Then, the powder of grinding is put into muffle furnace, programming rate is 2 DEG C/min, calcines 2 hours at 520 DEG C; Finally, the powder after calcining is cooled to room temperature, i.e. obtained FeMn-TiO
2/ g-C
3n
4;
Described molysite is iron chloride;
Described manganese salt is manganese chloride.
Embodiment 3FeMn-TiO
2/ g-C
3n
4preparation
First, 0.8mmol molysite is got and 1.2mmol manganese salt joins in 5mL butyl titanate, in whipping process, slowly add 0.8mL hydrofluorite, at 200 DEG C, react 18 hours, after being cooled to room temperature in a kettle., after ultrapure water and absolute ethyl alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 250mg and mix with 400mg melamine, and grind into powder; Then, the powder of grinding is put into muffle furnace, programming rate is 3 DEG C/min, calcines 0.5 hour at 560 DEG C; Finally, the powder after calcining is cooled to room temperature, i.e. obtained FeMn-TiO
2/ g-C
3n
4;
Described molysite is ferric nitrate;
Described manganese salt is manganese nitrate.
The preparation of embodiment 4 dimethylbenzene gas sensor
First, the FeMn-TiO of preparation in Example 1
2/ g-C
3n
4100mg and 0.5mmol potassium sulfate is placed in mortar, adds absolute ethyl alcohol, is evenly coated in insulating ceramics tube-surface and forms film, at room temperature dry after being ground to pasty state; Then, the platinum filament of ceramic pipe both sides and heater strip are welded with base; Finally, be placed in detecting instrument by the element welded, by regulating heating voltage to carry out burin-in process to 4.22V, namely obtained dimethylbenzene gas sensor, is applied to the detection of dimethylbenzene gas, detects and be limited to 0.001mg/m
3.
The preparation of embodiment 5 dimethylbenzene gas sensor
First, the FeMn-TiO of preparation in Example 2
2/ g-C
3n
4100mg and 1.2mmol potassium chloride is placed in mortar, adds absolute ethyl alcohol, is evenly coated in insulating ceramics tube-surface and forms film, at room temperature dry after being ground to pasty state; Then, the platinum filament of ceramic pipe both sides and heater strip are welded with base; Finally, be placed in detecting instrument by the element welded, by regulating heating voltage to carry out burin-in process to 4.22V, namely obtained dimethylbenzene gas sensor, is applied to the detection of dimethylbenzene gas, detects and be limited to 0.001mg/m
3.
The preparation of embodiment 6 dimethylbenzene gas sensor
First, the FeMn-TiO of preparation in Example 3
2/ g-C
3n
4100mg and 2.0mmol potassium nitrate is placed in mortar, adds absolute ethyl alcohol, is evenly coated in insulating ceramics tube-surface and forms film, at room temperature dry after being ground to pasty state; Then, the platinum filament of ceramic pipe both sides and heater strip are welded with base; Finally, be placed in detecting instrument by the element welded, by regulating heating voltage to carry out burin-in process to 4.22V, namely obtained dimethylbenzene gas sensor, is applied to the detection of dimethylbenzene gas, detects and be limited to 0.001mg/m
3.
Claims (2)
1., based on a preparation method for the dimethylbenzene gas sensor of titanium dioxide nanoplate, described titanium dioxide nanoplate is the titanium dioxide nanoplate In-situ reaction carbonitride two-dimensional nano compound substance FeMn-TiO of iron and manganese thermometal codope
2/ g-C
3n
4;
It is characterized in that, described preparation method comprises following preparation process:
(1) FeMn-TiO
2/ g-C
3n
4preparation;
(2) preparation of dimethylbenzene gas sensor;
Wherein, step (1) prepares FeMn-TiO
2/ g-C
3n
4concrete steps be:
First, get 0.8mmol molysite and 0.8 ~ 1.2mmol manganese salt joins in 5mL butyl titanate, in whipping process, slowly add 0.5 ~ 0.8mL hydrofluorite, 18 ~ 24 hours are reacted in a kettle. at 160 ~ 200 DEG C, after being cooled to room temperature, after ultrapure water and absolute ethyl alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 150 ~ 250mg and mix with 400mg melamine, and grind into powder; Then, the powder of grinding is put into muffle furnace, programming rate is 1 ~ 3 DEG C/min, calcines 0.5 ~ 5 hour at 480 ~ 560 DEG C; Finally, the powder after calcining is cooled to room temperature, i.e. obtained FeMn-TiO
2/ g-C
3n
4;
Described molysite is selected from one of following: iron sulfate, iron chloride, ferric nitrate;
Described manganese salt is selected from one of following: manganese sulfate, manganese chloride, manganese nitrate;
The concrete steps that step (2) prepares dimethylbenzene gas sensor are:
First, the FeMn-TiO of preparation in step (1) is got
2/ g-C
3n
4100mg and 0.5 ~ 2.0mmol sylvite are placed in mortar, add absolute ethyl alcohol, are evenly coated in insulating ceramics tube-surface and form film, at room temperature dry after being ground to pasty state; Then, the platinum filament of ceramic pipe both sides and heater strip are welded with base; Finally, the element welded is placed in detecting instrument, by regulating heating voltage to carry out burin-in process to 4.22V, i.e. obtained dimethylbenzene gas sensor;
Described sylvite is selected from one of following: potassium sulfate, potassium chloride, potassium nitrate.
2. the application of the dimethylbenzene gas sensor prepared by preparation method as claimed in claim 1, is characterized in that, can be applied to the detection of dimethylbenzene gas, detect and be limited to 0.001mg/m
3.
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| CN201610101704.7A CN105572175B (en) | 2016-02-25 | 2016-02-25 | A kind of preparation method and application of the dimethylbenzene gas sensor based on titanium dioxide nanoplate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108181301A (en) * | 2018-01-17 | 2018-06-19 | 四川大学 | A kind of sensor device and its analysis method for detecting CO gas |
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|---|---|---|---|---|
| CN108181301A (en) * | 2018-01-17 | 2018-06-19 | 四川大学 | A kind of sensor device and its analysis method for detecting CO gas |
| CN108181301B (en) * | 2018-01-17 | 2020-04-24 | 四川大学 | Sensor device for detecting carbon monoxide gas and analysis method thereof |
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| CN105572175B (en) | 2018-05-25 |
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