CN105606655B - A kind of preparation method and application of the acetone gas sensor based on two-dimentional porous nano composite material supported palladium - Google Patents
A kind of preparation method and application of the acetone gas sensor based on two-dimentional porous nano composite material supported palladium Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of acetone gas sensor, the gas sensor constructed by specifically based on New Two Dimensional nanocomposite, available for acetone 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 ceriums and the titanium dioxide nanoplate In-situ reaction carbonitride two-dimensional nano composite material CeCo TiO of cobalt dual-metal codope2/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 acetone gas.
Description
Technical field
The present invention relates to a kind of preparation methods of acetone gas sensor, belong to Nano-function thin films and environmental monitoring
Technical field.
Background technology
Acetone（Acetone, CH3COCH3）Also known as dimethyl ketone, it is simplest saturated ketone.It is a kind of water white transparency liquid
Body has special acrid odors.The organic solvents such as soluble easily in water and methanol, ethyl alcohol, ether, chloroform, pyridine.It is inflammable, volatile,
Chemical property is more active.Acute poisoning is mainly shown as the anesthetic effect of Central nervous system, occur weak, nauseous, headache,
It is dizzy, emotional.Vomiting, out of breath, spasm or even stupor occur for severe one.It is irritant to eye, nose, larynx.After oral, first there is mouth
Lip, throat have burn feeling, after there is dry, vomiting, stupor, acid poisoning and ketosis.
Mainly there are chemical analysis method and instrument testing method for the detection method of acetone 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 detects instrument to sky using acetone gas
Acetone gas concentration in gas carries out quantitative detection, has many advantages, such as high sensitivity, reusable, high degree of automation, and
It is widely applied in industrial production.
For acetone gas detector used in instrument testing method, most crucial component is with qualitative to acetone gas
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 variation of external environment
Raw drift.It mainly includes semiconductor gas sensor, catalytic combustion type gas sensor and Electro-chemical Gas Sensor etc.,
It is middle 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 that strong adsorption, stability are good, catalytic activity is high, have specific recognition and can to acetone gas
The gas sensing materials quantitatively detected, and then prepare the acetone gas with the characteristics 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
Key points and difficulties.
Invention content
Prepare that simple, high sensitivity, detection is quickly available is examined in acetone gas the purpose of the present invention is to provide a kind of
The preparation method of the gas sensor of survey, prepared sensor, quick, Sensitive Detection available for acetone gas.Based on this
Purpose, the method comprises the steps of firstly, preparing a kind of New Two Dimensional nanocomposites, the i.e. titanium dioxide of cerium and cobalt dual-metal codope
Nanometer sheet In-situ reaction carbonitride two-dimensional nano composite material CeCo-TiO2/g-C3N4, using the big specific surface area of the material, it is situated between
The high gas absorption characteristic in hole and electron transmission are changed by material surface gas and influence sensitive many characteristics, are realized to acetone
Gas has the structure of sensitive, quick response gas sensor.
The technical solution adopted by the present invention is as follows：
1. a kind of preparation method of the acetone gas sensor based on two-dimentional porous nano composite material supported palladium, described
Titanium dioxide nanoplate In-situ reaction carbonitride two dimension of the two-dimentional porous nano composite material for cerium and cobalt dual-metal codope
Nanocomposite CeCo-TiO2/g-C3N4, the palladium is Pd nano particle；
It is characterized in that, the preparation method includes following preparation process：
（1）CeCo-TiO2/g-C3N4Preparation；
（2）The preparation of acetone gas sensor；
Wherein, step（1）Prepare CeCo-TiO2/g-C3N4The specific steps are：
First, 0.8 mmol ceriums salt and 0.8 ~ 1.2 mmol cobalt salts is taken to be added in 5 mL butyl titanates, whipping process
In, 0.5 ~ 0.8 mL hydrofluoric acid is slowly added to, is reacted in a kettle at 160 ~ 200 DEG C 18 ~ 24 hours, after being cooled to room temperature,
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
It is mixed, and grind into powder with 400 mg melamines；Then, the powder of grinding is put into Muffle furnace, heating rate is 1 ~ 3
DEG C/min, it is calcined 0.5 ~ 5 hour at 480 ~ 560 DEG C；Finally, the powder after calcining is cooled to room temperature, obtains CeCo-
TiO2/g-C3N4；
The cerium salt is selected from one of following：Cerous sulfate, cerium chloride, cerous nitrate；
The cobalt salt is selected from one of following：Cobaltous sulfate, cobalt chloride, cobalt nitrate；
Step（2）Prepare acetone gas sensor the specific steps are：
First, step is taken（1）The CeCo-TiO of middle preparation2/g-C3N4100 mg and 0.5 ~ 2.0 mmol palladium bichlorides are placed in
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 acetone gas sensor.
2. the application of the acetone gas sensor prepared by preparation method of the present invention, which is characterized in that Ke Yiying
For the detection of acetone gas, detection is limited to 0.001 mg/m3。
The useful achievement of the present invention
（1）Acetone gas sensor of the present invention is prepared simply, easy to operate, is realized to the fast of acetone gas
Fast, sensitive, highly selective detection has market development prospect；
（2）The present invention is prepared for New-type matrix material CeCo-TiO for the first time2/g-C3N4, since cerium, cobalt are received in titanium dioxide
Rice on piece growth in situ and fully contacted with titanium dioxide nanoplate, using cerium, cobalt metal surface plasma body act on
And the mutual promoting action of the two, semiconductor substrate electron transmission ability and catalytic activity are effectively increased, solves titanium dioxide
Although titanium nanometer sheet specific surface area is bigger and mesoporous high gas absorption characteristic is suitable for air-sensitive host material, gas-sensitive activity
The technical issues of not high and impedance variations are unstable；Simultaneously because carbonitride g-C3N4Good electric conductivity, along with titanium dioxide
Titanium nanometer sheet on it fully dispersed, greatly increases electron transmission ability, solves air-sensitive host material impedance with gas
Body change and the technical issues of quick response；Moreover, by the doping of Metal Palladium, solves the skill of specific detection acetone gas
Art problem.Therefore, effective preparation of the material has important scientific meaning and application value.
Specific embodiment
1 CeCo-TiO of embodiment2/g-C3N4Preparation
First, 0.8 mmol ceriums salt and 0.8 mmol cobalt salts is taken to be added in 5 mL butyl titanates, in whipping process, is delayed
It is slow to add in 0.5 mL hydrofluoric acid, it is reacted in a kettle 24 hours, after being cooled to room temperature at 160 DEG C, with ultra-pure water and anhydrous second
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 CeCo-TiO2/g-C3N4；
The cerium salt is cerous sulfate；
The cobalt salt is cobaltous sulfate.
2 CeCo-TiO of embodiment2/g-C3N4Preparation
First, 0.8 mmol ceriums salt and 1.0 mmol cobalt salts is taken to be added in 5 mL butyl titanates, in whipping process, are delayed
It is slow to add in 0.65 mL hydrofluoric acid, it is reacted in a kettle 21 hours, after being cooled to room temperature at 180 DEG C, 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 200 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 2 DEG C/min, at 520 DEG C
Calcining 2 hours；Finally, the powder after calcining is cooled to room temperature, obtains CeCo-TiO2/g-C3N4；
The cerium salt is cerium chloride；
The cobalt salt is cobalt chloride.
3 CeCo-TiO of embodiment2/g-C3N4Preparation
First, 0.8 mmol ceriums salt and 1.2 mmol cobalt salts is taken to be added in 5 mL butyl titanates, in whipping process, are delayed
It is slow to add in 0.8 mL hydrofluoric acid, it is reacted in a kettle 18 hours, after being cooled to room temperature at 200 DEG C, 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 250 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 3 DEG C/min, is forged at 560 DEG C
It burns 0.5 hour；Finally, the powder after calcining is cooled to room temperature, obtains CeCo-TiO2/g-C3N4；
The cerium salt is cerous nitrate；
The cobalt salt is cobalt nitrate.
The preparation of 4 acetone gas sensor of embodiment
First, the CeCo-TiO prepared in Example 12/g-C3N4100 mg and 0.5 mmol palladium bichlorides are placed in mortar
In, 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；So
Afterwards, the platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on detector
In device, burin-in process is carried out to 4.22V by adjusting heating voltage, acetone gas sensor is obtained, applied to acetone gas
Detection, detection be limited to 0.001 mg/m3。
The preparation of 5 acetone gas sensor of embodiment
First, the CeCo-TiO prepared in Example 22/g-C3N4100 mg and 1.2 mmol palladium bichlorides are placed in mortar
In, 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；So
Afterwards, the platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on detector
In device, burin-in process is carried out to 4.22V by adjusting heating voltage, acetone gas sensor is obtained, applied to acetone gas
Detection, detection be limited to 0.001 mg/m3。
The preparation of 6 acetone gas sensor of embodiment
First, the CeCo-TiO prepared in Example 32/g-C3N4100 mg and 2.0 mmol palladium bichlorides are placed in mortar
In, 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；So
Afterwards, the platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on detector
In device, burin-in process is carried out to 4.22V by adjusting heating voltage, acetone gas sensor is obtained, applied to acetone gas
Detection, detection be limited to 0.001 mg/m3。
Claims (2)
1. a kind of preparation method of the acetone gas sensor based on two-dimentional porous nano composite material supported palladium, the two dimension
Porous nano composite material is answered for the titanium dioxide nanoplate In-situ reaction carbonitride two-dimensional nano of cerium and cobalt dual-metal codope
Condensation material CeCo-TiO2/g-C3N4, the palladium is Pd nano particle；
It is characterized in that, the preparation method includes following preparation process：
（1）CeCo-TiO2/g-C3N4Preparation；
（2）The preparation of acetone gas sensor；
Wherein, step（1）Prepare CeCo-TiO2/g-C3N4The specific steps are：
First, 0.8 mmol ceriums salt and 0.8 ~ 1.2 mmol cobalt salts is taken to be added in 5 mL butyl titanates, in whipping process, is delayed
It is slow to add in 0.5 ~ 0.8 mL hydrofluoric acid, it is reacted in a kettle 18 ~ 24 hours, after being cooled to room temperature at 160 ~ 200 DEG C, with super
Pure water and absolute ethyl alcohol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Secondly, take the dried solids of 150 ~ 250 mg with
400 mg melamines mix, and grind into powder；Then, the powder of grinding is put into Muffle furnace, heating rate is 1 ~ 3
DEG C/min, it is calcined 0.5 ~ 5 hour at 480 ~ 560 DEG C；Finally, the powder after calcining is cooled to room temperature, obtains CeCo-
TiO2/g-C3N4；
The cerium salt is selected from one of following：Cerous sulfate, cerium chloride, cerous nitrate；
The cobalt salt is selected from one of following：Cobaltous sulfate, cobalt chloride, cobalt nitrate；
Step（2）Prepare acetone gas sensor the specific steps are：
First, step is taken（1）The CeCo-TiO of middle preparation2/g-C3N4100 mg and 0.5 ~ 2.0 mmol palladium bichlorides are placed in mortar
In, 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；So
Afterwards, the platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on detector
In device, burin-in process is carried out to 4.22V by adjusting heating voltage, obtains acetone gas sensor.
2. the application of the acetone gas sensor prepared by preparation method as described in claim 1, which is characterized in that Ke Yiying
For the detection of acetone gas, detection is limited to 0.001 mg/m3。
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| CN108889325A (en) * | 2018-06-28 | 2018-11-27 | 陕西科技大学 | A kind of synthetic method of Pt nanoparticle catalyst |
| CN110711863A (en) * | 2019-11-06 | 2020-01-21 | 郑州大学 | AuPd alloy nanoparticle loaded 3DOM WO3Preparation method of (1) |
| CN112844436B (en) * | 2021-01-27 | 2022-05-17 | 宁波方太厨具有限公司 | Catalyst for removing formaldehyde and carbon monoxide by catalysis and preparation method thereof |
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