CN105628745B - A kind of preparation method and application of the nitrogen dioxide gas sensor based on titania-based porous nano composite material - Google Patents
A kind of preparation method and application of the nitrogen dioxide gas sensor based on titania-based porous nano composite material Download PDFInfo
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- 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
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Abstract
The present invention relates to a kind of preparation method of nitrogen dioxide gas sensor, the gas sensor constructed by specifically based on Novel Titanium dioxide Quito hole nanocomposite, available for nitrogen dioxide 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 two-dimensional nano composite material Ce MoO of molybdenum oxide/titanium dioxide nanoplate of In-situ reaction cerium dopping on carbonitride3/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 sensitive many characteristics, realize the structure that there is sensitive, quick response gas sensor to nitrogen dioxide gas.
Description
Technical field
The present invention relates to a kind of preparation methods of nitrogen dioxide gas sensor.Belong to Nano-function thin films and environment
Monitoring technical field.
Background technology
Nitrogen dioxide is the gaseous material of a kind of brownish red, high activity, also known as hyponitric acid.Nitrogen dioxide or acid rain
One of the origin cause of formation, caused environmental effect is varied, including：Competition becomes with composition between wetland and terrestrial plant species
The influence of change, the reduction of atmospheric visibility, the acidification of surface water, eutrophication（Due to being rich in the nutrients algae such as nitrogen, phosphorus in water
Amount reproduction and lead to anoxic）And increase the content of toxins that fish and other aquatiles are harmful in water body.Human body sucks
After nitrogen dioxide, initial stage only has slight eye and upper respiratory tract irritation, such as pharyngeal uncomfortable, dry cough, often through a few hours extremely
Late-onset pulmonary edema, adult respiratory distress syndrome (ARDS) after ten a few houres or incubation period longer time, appearance is uncomfortable in chest, breathing is embarrassed
Compel, cough, coughing up frothy sputum, cyanosis etc..It can complicated with pneumothorax and mediastinal emphysema.
Mainly there are chemical analysis method and instrument testing method for the detection method of nitrogen dioxide gas.Though chemical analysis method is grasped
Make simple, but sensitivity is not high and the shortcomings of can not reuse；Instrument testing method, is mainly detected using nitrogen dioxide gas
Instrument carries out the nitrogen dioxide gas concentration in air quantitative detection, has high sensitivity, reusable, the degree of automation
The advantages that high, and be widely applied in industrial production.
For nitrogen dioxide gas detector used in instrument testing method, most crucial component is to nitrogen dioxide gas
Gas sensor with qualitative, quantitative response, that is, the gas sensor coated with different nano-functional materials.Gas sensing
Device is a kind of sensor for detecting specific gas, and principle is that velocity of wave based on SAW device and frequency can be with external environments
Change and drift about.It mainly includes semiconductor gas sensor, catalytic combustion type gas sensor and electrochemistry air-sensitive and passes
Sensor etc., wherein it is most be semiconductor gas sensor.
Sensitivity is the important characterization 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 strong adsorption, stability are good, catalytic activity is high, to nitrogen dioxide gas have specific recognition
With can quantify the gas sensing materials of detection, and then prepare with high sensitivity, response quickly, recovery time be short etc. the two of characteristics
Nitrogen oxide gas sensor has important application value to industrial production, human health, while is also environmental monitoring technology neck
The key points and difficulties of domain research.
Invention content
To prepare simple, high sensitivity, detection quickly available in titanium dioxide nitrogen the purpose of the present invention is to provide a kind of
The preparation method for the gas sensor that physical examination is surveyed, prepared sensor, quick, the sensitive inspection available for nitrogen dioxide gas
It surveys.Based on this purpose, the method comprises the steps of firstly, preparing a kind of New Two Dimensional nanocomposites --- titania-based porous nano
The two-dimensional nano composite material Ce- of molybdenum oxide/titanium dioxide nanoplate of In-situ reaction cerium dopping on composite material, i.e. carbonitride
MoO3/TiO2@g-C3N4, using the big specific surface area of the material, mesoporous high gas absorption characteristic and electron transmission by material surface
Gas changes and influences sensitive many characteristics, and realize has sensitive, quick response gas sensing to nitrogen dioxide gas
The structure of device.
The technical solution adopted by the present invention is as follows：
1. a kind of preparation method of the nitrogen dioxide gas sensor based on titania-based porous nano composite material,
Molybdenum oxide/nano titania of the titania-based porous nano composite material for In-situ reaction cerium dopping on carbonitride
The two-dimensional nano composite material Ce-MoO of piece3/TiO2@g-C3N4；
It is characterized in that, the preparation method includes following preparation process：
（1）Ce-MoO3/TiO2@g-C3N4Preparation；
（2）The preparation of nitrogen dioxide gas sensor；
Wherein, step（1）Prepare Ce-MoO3/TiO2@g-C3N4The specific steps are：
First, 0.6 ~ 1.0 mmol sodium molybdates and 0.8 ~ 1.2 mmol cerium salt is taken to be added in 5 mL butyl titanates, is stirred
During mixing, 0.5 ~ 0.8 mL hydrofluoric acid is slowly added to, reacts 18 ~ 24 hours, is cooled in a kettle at 160 ~ 200 DEG C
After room temperature, with ultra-pure water and absolute ethyl alcohol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Secondly, 150 ~ 250 mg is taken to dry
Solid afterwards mixes, and grind into powder with 400 mg melamines；Then, the powder of grinding is put into Muffle furnace, heated up
Speed is 1 ~ 3 DEG C/min, is calcined 0.5 ~ 5 hour at 480 ~ 560 DEG C；Finally, the powder after calcining is cooled to room temperature, i.e.,
Ce-MoO is made3/TiO2@g-C3N4；
The cerium salt is selected from one of following：Cerous sulfate, cerium chloride, cerous nitrate；
Step（2）Prepare nitrogen dioxide gas sensor the specific steps are：
First, step is taken（1）The Ce-MoO of middle preparation3/TiO2@g-C3N4100 mg and 0.5 ~ 2.0 mmol cerium oxide are put
In mortar, absolute ethyl alcohol is added in, insulating ceramics pipe surface formation film is coated uniformly on after being ground to paste, dries in the air at room temperature
It is dry；Then, the platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on
In detecting instrument, burin-in process is carried out to 4.22V by adjusting heating voltage, obtains nitrogen dioxide gas sensor.
2. the application of the nitrogen dioxide gas sensor prepared by preparation method as described in claim 1, feature exist
In can be applied to the detection of nitrogen dioxide gas, detection is limited to 0.005 mg/m3。
The useful achievement of the present invention
（1）Nitrogen dioxide gas sensor of the present invention is prepared simply, easy to operate, is realized to titanium dioxide nitrogen
Quick, sensitive, the highly selective detection of body has market development prospect；
（2）The present invention is prepared for New Two Dimensional nano material Ce-MoO for the first time3/TiO2@g-C3N4, due to cerium molybdenum oxide/
Growth in situ on titanium dioxide nanoplate and fully contacted with titanium dioxide nanoplate, utilize the metal surface plasma body of cerium
The mutual promoting action of both effect and molybdenum oxide and titanium dioxide, effectively increase semiconductor substrate electron transmission ability and
Catalytic activity, and to nitrogen dioxide gas specificity is corresponding for cerium, although solving titanium dioxide nanoplate specific surface area ratio
Larger and mesoporous high gas absorption characteristic is suitable for nitrogen dioxide air-sensitive host material, but gas-sensitive activity is not high and impedance variations
The technical issues of unstable；Simultaneously because carbonitride g-C3N4Good electric conductivity, along with titanium dioxide nanoplate on it
It is fully dispersed, greatly increase electron transmission ability, solve the impedance of air-sensitive host material with gas change and quickly ring
The technical issues of answering, therefore, effective preparation of the material has important scientific meaning and application value.
Specific embodiment
1 Ce-MoO of embodiment3/TiO2@g-C3N4Preparation
First, 0.6 mmol sodium molybdates and 0.8 mmol cerium salt is taken to be added in 5 mL butyl titanates, in whipping process,
0.5 mL hydrofluoric acid is slowly added to, is reacted in a kettle at 160 DEG C 24 hours, after being cooled to room temperature, with ultra-pure water and anhydrous
Ethyl alcohol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Secondly, the dried solids of 150 mg is taken to be mixed with 400 mg melamines
It closes, and grind into powder；Then, the powder of grinding is put into Muffle furnace, heating rate is 1 DEG C/min, at 480 DEG C
Calcining 5 hours；Finally, the powder after calcining is cooled to room temperature, obtains Ce-MoO3/TiO2@g-C3N4；
The cerium salt is cerous sulfate.
2 Ce-MoO of embodiment3/TiO2@g-C3N4Preparation
First, 0.8 mmol sodium molybdates and 1.0 mmol cerium salt is taken to be added in 5 mL butyl titanates, in whipping process,
0.65 mL hydrofluoric acid is slowly added to, is reacted in a kettle at 180 DEG C 21 hours, after being cooled to room temperature, with ultra-pure water and nothing
Water-ethanol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Secondly, the dried solids of 200 mg and 400 mg melamines are taken
Mixing, and grind into powder；Then, the powder of grinding is put into Muffle furnace, heating rate is 2 DEG C/min, at 520 DEG C
Lower calcining 2 hours；Finally, the powder after calcining is cooled to room temperature, obtains Ce-MoO3/TiO2@g-C3N4；
The cerium salt is cerium chloride.
3 Ce-MoO of embodiment3/TiO2@g-C3N4Preparation
First, 1.0 mmol sodium molybdates and 1.2 mmol cerium salt is taken to be added in 5 mL butyl titanates, in whipping process,
0.8 mL hydrofluoric acid is slowly added to, is reacted in a kettle at 200 DEG C 18 hours, after being cooled to room temperature, with ultra-pure water and nothing
Water-ethanol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Secondly, the dried solids of 250 mg and 400 mg melamines are taken
Mixing, and grind into powder；Then, the powder of grinding is put into Muffle furnace, heating rate is 3 DEG C/min, at 560 DEG C
Calcining 0.5 hour；Finally, the powder after calcining is cooled to room temperature, obtains Ce-MoO3/TiO2@g-C3N4；
The cerium salt is cerous nitrate.
The preparation of 4 nitrogen dioxide gas sensor of embodiment
First, the Ce-MoO prepared in Example 13/TiO2@g-C3N4100 mg and 0.5 mmol cerium oxide are placed in and grind
In alms bowl, absolute ethyl alcohol is added in, insulating ceramics pipe surface formation film is coated uniformly on after being ground to paste, dries at room temperature；
Then, the platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on detection
In instrument, burin-in process is carried out to 4.22V by adjusting heating voltage, nitrogen dioxide gas sensor is obtained, applied to two
The detection of nitrogen oxide gas, detection are limited to 0.005 mg/m3。
The preparation of 5 nitrogen dioxide gas sensor of embodiment
First, the Ce-MoO prepared in Example 23/TiO2@g-C3N4100 mg and 1.2 mmol cerium oxide are placed in and grind
In alms bowl, absolute ethyl alcohol is added in, insulating ceramics pipe surface formation film is coated uniformly on after being ground to paste, dries at room temperature；
Then, the platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on detection
In instrument, burin-in process is carried out to 4.22V by adjusting heating voltage, nitrogen dioxide gas sensor is obtained, applied to two
The detection of nitrogen oxide gas, detection are limited to 0.005 mg/m3。
The preparation of 6 nitrogen dioxide gas sensor of embodiment
First, the Ce-MoO prepared in Example 33/TiO2@g-C3N4100 mg and 2.0 mmol cerium oxide are placed in and grind
In alms bowl, absolute ethyl alcohol is added in, insulating ceramics pipe surface formation film is coated uniformly on after being ground to paste, dries at room temperature；
Then, the platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on detection
In instrument, burin-in process is carried out to 4.22V by adjusting heating voltage, nitrogen dioxide gas sensor is obtained, applied to two
The detection of nitrogen oxide gas, detection are limited to 0.005 mg/m3。
Claims (2)
1. a kind of preparation method of the nitrogen dioxide gas sensor based on titania-based porous nano composite material, described
Titania-based porous nano composite material is two of molybdenum oxide/titanium dioxide nanoplate of In-situ reaction cerium dopping on carbonitride
Wiener nano composite material Ce-MoO3/TiO2@g-C3N4；
It is characterized in that, the preparation method includes following preparation process：
（1）Ce-MoO3/TiO2@g-C3N4Preparation；
（2）The preparation of nitrogen dioxide gas sensor；
Wherein, step（1）Prepare Ce-MoO3/TiO2@g-C3N4The specific steps are：
First, 0.6 ~ 1.0 mmol sodium molybdates and 0.8 ~ 1.2 mmol cerium salt is taken to be added in 5 mL butyl titanates, it is stirred
Cheng Zhong is slowly added to 0.5 ~ 0.8 mL hydrofluoric acid, reacts 18 ~ 24 hours, be cooled to room temperature in a kettle at 160 ~ 200 DEG C
Afterwards, with ultra-pure water and absolute ethyl alcohol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Secondly, take 150 ~ 250 mg dried
Solid mixes, and grind into powder with 400 mg melamines；Then, the powder of grinding is put into Muffle furnace, heating rate
For 1 ~ 3 DEG C/min, calcined 0.5 ~ 5 hour at 480 ~ 560 DEG C；Finally, the powder after calcining is cooled to room temperature, obtained
Ce-MoO3/TiO2@g-C3N4；
The cerium salt is selected from one of following：Cerous sulfate, cerium chloride, cerous nitrate；
Step（2）Prepare nitrogen dioxide gas sensor the specific steps are：
First, step is taken（1）The Ce-MoO of middle preparation3/TiO2@g-C3N4100 mg and 0.5 ~ 2.0 mmol cerium oxide are placed in and grind
In alms bowl, absolute ethyl alcohol is added in, insulating ceramics pipe surface formation film is coated uniformly on after being ground to paste, dries at room temperature；
Then, the platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on detection
In instrument, burin-in process is carried out to 4.22V by adjusting heating voltage, obtains nitrogen dioxide gas sensor.
2. the application of the nitrogen dioxide gas sensor prepared by preparation method as described in claim 1, which is characterized in that can
To be applied to the detection of nitrogen dioxide gas, detection is limited to 0.005 mg/m3。
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| CN108786894B (en) * | 2018-07-02 | 2020-11-03 | 广东石油化工学院 | Graphite-phase carbon nitride/rare earth sodium molybdate heterojunction photocatalyst and preparation method and application thereof |
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