CN105572176B - A kind of preparation method and application of the toluene gas sensor based on base metal doped and compounded material - Google Patents
A kind of preparation method and application of the toluene gas sensor based on base metal doped and compounded material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of toluene gas sensor, the gas sensor constructed by specifically based on base metal doped and compounded material, available for toluene gas content in detection environment.Belong to Nano-function thin films and environmental monitoring technology field.The method comprises the steps of firstly, preparing a kind of New Two Dimensional nano composite material Mn TiO2/g‑C3N4, changed using the big specific surface area of the material, mesoporous high gas absorption characteristic and electron transmission by material surface gas and influence many characteristics of sensitivity, realize the structure to toluene gas with sensitive, quick response gas sensor.
Description
Technical field
The present invention relates to a kind of preparation method of toluene gas sensor, specifically based on base metal doped and compounded material
Constructed gas sensor, available for toluene gas content in detection environment.Belong to Nano-function thin films to supervise with environment
Survey technology field.
Background technology
Toluene is largely used as solvent and high-knock rating gasoline additive, and the important source material of organic chemical industry, volatile.People
Neurasthenic syndrome, hepatomegaly, woman worker's menoxenia etc. can occur for body Long Term Contact toluene.Dry skin, chap, dermatitis.
Mainly there are chemical analysis method and instrument testing method for the detection method of toluene gas.Though chemical analysis method operation letter
It is single, but sensitivity is not high and the shortcomings of can not reuse；Instrument testing method, mainly using toluene gas instrumentation to sky
Toluene gas concentration in gas carries out quantitative detection, has the advantages that high sensitivity, reusable, automaticity is high, and
It is widely applied among industrial production.
For toluene gas detector used in instrument testing method, most crucial part be have to toluene gas it is qualitative
The gas sensor of quantitative response, that is, the gas sensor coated with different nano-functional materials.Gas sensor is a kind of
The sensor of specific gas is detected, principle is that velocity of wave based on SAW device and frequency can be sent out with the change of external environment
Raw drift.It mainly includes semiconductor gas sensor, catalytic combustion type gas sensor and Electro-chemical Gas Sensor etc., its
It is middle it is most be semiconductor gas sensor.
Sensitivity is the important sign of gas sensor gas-sensitive property.Sensitivity definition is sensor in air atmosphere
Resistance valueR a With resistance value of the sensor in certain density tested gas atmosphereR g Ratio, i.e.,
Therefore, probe into that adsorptivity is strong, stability is good, catalytic activity is high, has specific recognition to toluene gas and can
The gas sensing materials quantitatively detected, and then prepare the toluene gas with the characteristic such as high sensitivity, response quickly, recovery time be short
Body sensor has important application value to industrial production, human health, while is also environmental monitoring technology area research
Emphasis and difficult point.
The content of the invention
It is an object of the invention to provide one kind prepares simple, high sensitivity, detection is quickly available is examined in toluene gas
The preparation method of the gas sensor of survey, prepared sensor, quick, Sensitive Detection available for toluene gas.Based on this
Purpose, the method comprises the steps of firstly, preparing a kind of New Two Dimensional nano composite material, i.e. additive Mn titanium dioxide nanoplate In-situ reaction
Carbonitride two-dimensional nano composite Mn-TiO2/g-C3N4, utilize the big specific surface area of the material, mesoporous high gas absorption characteristic
With electron transmission by material surface gas change and influence sensitivity many characteristics, realize have to toluene gas it is sensitive, fast
The structure of the gas sensor of speed response.
The technical solution adopted by the present invention is as follows：
1. a kind of preparation method of the toluene gas sensor based on base metal doped and compounded material, described is non-expensive
Metal-doped composite is additive Mn titanium dioxide nanoplate In-situ reaction carbonitride two-dimensional nano composite Mn-TiO2/
g-C3N4；
Characterized in that, described preparation method includes following preparation process：
（1）Mn-TiO2/g-C3N4Preparation；
（2）The preparation of toluene gas sensor；
Wherein, step（1）Prepare Mn-TiO2/g-C3N4Concretely comprise the following steps：
First, 0.8 ~ 1.2 mmol manganese salts are taken to be added in 5 mL butyl titanates, in whipping process, it is slowly added to 0.5 ~
0.8 mL hydrofluoric acid, react in a kettle 18 ~ 24 hours, after being cooled to room temperature at 160 ~ 200 DEG C, with ultra-pure water and anhydrous
Ethanol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Secondly, the dried solids of 150 ~ 250 mg and 400mg melamines are taken
Amine mixes, and grind into powder；Then, the powder of grinding is put into Muffle furnace, programming rate is 1 ~ 3 DEG C/min, 480
Calcined 0.5 ~ 5 hour at ~ 560 DEG C；Finally, the powder after calcining is cooled to room temperature, that is, Mn-TiO is made2/g-C3N4；
Described manganese salt is selected from one of following：Manganese sulfate, manganese chloride, manganese nitrate；
Step（2）Prepare concretely comprising the following steps for toluene gas sensor：
First, step is taken（1）The Mn-TiO of middle preparation2/g-C3N4100 mg and 0.5 ~ 2.0 mmol sylvite are placed in mortar
In, absolute ethyl alcohol is added, insulating ceramics pipe surface formation film is coated uniformly on after being ground to pasty state, dries at room temperature；So
Afterwards, the platinum filament of earthenware both sides and heater strip are welded with base；Finally, the element being welded is placed on detector
In device, burin-in process is carried out to 4.22V by adjusting heating voltage, that is, toluene gas sensor is made；
Described sylvite is selected from one of following：Potassium sulfate, potassium chloride, potassium nitrate.
2. the application of the toluene gas sensor prepared by preparation method of the present invention, it is characterised in that Ke Yiying
For the detection of toluene gas, detection is limited to 0.001 mg/m3。
The useful achievement of the present invention
（1）Toluene gas sensor of the present invention is prepared simply, easy to operate, is realized to the fast of toluene gas
Fast, sensitive, high selectivity detection, has market development prospect；
（2）The present invention is prepared for New-type matrix material Mn-TiO first2/g-C3N4, because manganese is on titanium dioxide nanoplate
Growth in situ and fully contacted with titanium dioxide nanoplate, using manganese metal surface plasma body act on, effectively increase
Semiconductor substrate electron transmission ability and catalytic activity, although it is bigger and mesoporous to solve titanium dioxide nanoplate specific surface area
High gas absorption characteristic is applied to air-sensitive host material, but the technical problem that gas-sensitive activity is not high and impedance variations are unstable；
Simultaneously because carbonitride g-C3N4Good electric conductivity, along with titanium dioxide nanoplate is fully dispersed thereon, greatly
Electron transmission ability is increased, the impedance of air-sensitive host material is solved and changes and the technical problem of quick response with gas；Moreover,
By the doping of potassium ion, solves the technical problem of specific detection toluene gas.Therefore, effective preparation of the material, tool
There are important scientific meaning and application value.
Embodiment
The Mn-TiO of embodiment 12/g-C3N4Preparation
First, take 0.8 mmol manganese salts to be added in 5 mL butyl titanates, in whipping process, be slowly added to 0.5 mL hydrogen
Fluoric acid, react in a kettle 24 hours, after being cooled to room temperature at 160 DEG C, with ultra-pure water and absolute ethyl alcohol centrifuge washing three times
Afterwards, it is dried in vacuo at 50 DEG C；Secondly, the dried solids of 150 mg are taken to be mixed with 400 mg melamines, and pulverize
End；Then, the powder of grinding is put into Muffle furnace, programming rate is 1 DEG C/min, is calcined 5 hours at 480 DEG C；Finally,
Powder after calcining is cooled to room temperature, that is, Mn-TiO is made2/g-C3N4；
Described manganese salt is manganese sulfate.
The Mn-TiO of embodiment 22/g-C3N4Preparation
First, take 1.0 mmol manganese salts to be added in 5 mL butyl titanates, in whipping process, be slowly added to 0.6 mL hydrogen
Fluoric acid, react in a kettle 21 hours, after being cooled to room temperature at 180 DEG C, with ultra-pure water and absolute ethyl alcohol centrifuge washing three times
Afterwards, it is dried in vacuo at 50 DEG C；Secondly, the dried solids of 200 mg are taken to be mixed with 400 mg melamines, and pulverize
End；Then, the powder of grinding is put into Muffle furnace, programming rate is 2 DEG C/min, is calcined 2 hours at 520 DEG C；Finally,
Powder after calcining is cooled to room temperature, that is, Mn-TiO is made2/g-C3N4；
Described manganese salt is manganese chloride.
The Mn-TiO of embodiment 32/g-C3N4Preparation
First, take 1.2 mmol manganese salts to be added in 5 mL butyl titanates, in whipping process, be slowly added to 0.8 mL hydrogen
Fluoric acid, react in a kettle 18 hours, after being cooled to room temperature at 200 DEG C, with ultra-pure water and absolute ethyl alcohol centrifuge washing three
After secondary, it is dried in vacuo at 50 DEG C；Secondly, the dried solids of 250 mg are taken to be mixed with 400 mg melamines, and pulverize
End；Then, the powder of grinding is put into Muffle furnace, programming rate is 3 DEG C/min, is calcined 0.5 hour at 560 DEG C；Most
Afterwards, the powder after calcining is cooled to room temperature, that is, Mn-TiO is made2/g-C3N4；
Described manganese salt is manganese nitrate.
The preparation of the toluene gas sensor of embodiment 4
First, the Mn-TiO prepared in Example 12/g-C3N4100 mg and 0.5 mmol potassium sulfates are placed in mortar,
Absolute ethyl alcohol is added, insulating ceramics pipe surface formation film is coated uniformly on after being ground to pasty state, dries at room temperature；Then,
The platinum filament of earthenware both sides and heater strip are welded with base；Finally, the element being welded is placed on detecting instrument
In, burin-in process is carried out to 4.22V by adjusting heating voltage, that is, toluene gas sensor is made, applied to toluene gas
Detection, detection are limited to 0.001 mg/m3。
The preparation of the toluene gas sensor of embodiment 5
First, the Mn-TiO prepared in Example 22/g-C3N4100 mg and 1.2 mmol potassium chloride are placed in mortar,
Absolute ethyl alcohol is added, insulating ceramics pipe surface formation film is coated uniformly on after being ground to pasty state, dries at room temperature；Then,
The platinum filament of earthenware both sides and heater strip are welded with base；Finally, the element being welded is placed on detecting instrument
In, burin-in process is carried out to 4.22V by adjusting heating voltage, that is, toluene gas sensor is made, applied to toluene gas
Detection, detection are limited to 0.001 mg/m3。
The preparation of the toluene gas sensor of embodiment 6
First, the Mn-TiO prepared in Example 32/g-C3N4100 mg and 2.0 mmol potassium nitrate are placed in mortar,
Absolute ethyl alcohol is added, insulating ceramics pipe surface formation film is coated uniformly on after being ground to pasty state, dries at room temperature；Then,
The platinum filament of earthenware both sides and heater strip are welded with base；Finally, the element being welded is placed on detecting instrument
In, burin-in process is carried out to 4.22V by adjusting heating voltage, that is, toluene gas sensor is made, applied to toluene gas
Detection, detection are limited to 0.001 mg/m3。
Claims (2)
1. a kind of preparation method of the toluene gas sensor based on base metal doped and compounded material, described base metal are mixed
Miscellaneous composite is additive Mn titanium dioxide nanoplate In-situ reaction carbonitride two-dimensional nano composite Mn-TiO2/g-C3N4；
Characterized in that, described preparation method includes following preparation process：
（1）Mn-TiO2/g-C3N4Preparation；
（2）The preparation of toluene gas sensor；
Wherein, step（1）Prepare Mn-TiO2/g-C3N4Concretely comprise the following steps：
First, take 0.8 ~ 1.2 mmol manganese salts to be added in 5 mL butyl titanates, in whipping process, be slowly added to 0.5 ~ 0.8
ML hydrofluoric acid, react in a kettle 18 ~ 24 hours, after being cooled to room temperature at 160 ~ 200 DEG C, with ultra-pure water and absolute ethyl alcohol
Centrifuge washing three times after, be dried in vacuo at 50 DEG C；Secondly, the dried solids of 150 ~ 250 mg are taken to be mixed with 400mg melamines
Close, and grind into powder；Then, the powder of grinding is put into Muffle furnace, programming rate is 1 ~ 3 DEG C/min, 480 ~ 560
Calcined 0.5 ~ 5 hour at DEG C；Finally, the powder after calcining is cooled to room temperature, that is, Mn-TiO is made2/g-C3N4；
Described manganese salt is selected from one of following：Manganese sulfate, manganese chloride, manganese nitrate；
Step（2）Prepare concretely comprising the following steps for toluene gas sensor：
First, step is taken（1）The Mn-TiO of middle preparation2/g-C3N4100 mg and 0.5 ~ 2.0 mmol sylvite are placed in mortar, are added
Enter absolute ethyl alcohol, be coated uniformly on insulating ceramics pipe surface formation film after being ground to pasty state, dry at room temperature；Then, will
Platinum filament and heater strip and the base of earthenware both sides are welded；Finally, the element being welded is placed in detecting instrument,
Burin-in process is carried out to 4.22V by adjusting heating voltage, that is, toluene gas sensor is made；
Described sylvite is selected from one of following：Potassium sulfate, potassium chloride, potassium nitrate.
2. the application of the toluene gas sensor prepared by preparation method as claimed in claim 1, it is characterised in that Ke Yiying
For the detection of toluene gas, detection is limited to 0.001 mg/m3。
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