CN105628745A - Preparation method and application for nitrogen dioxide gas sensor based on titanium-dioxide-based porous nanocomposite - Google Patents
Preparation method and application for nitrogen dioxide gas sensor based on titanium-dioxide-based porous nanocomposite Download PDFInfo
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- CN105628745A CN105628745A CN201610101698.5A CN201610101698A CN105628745A CN 105628745 A CN105628745 A CN 105628745A CN 201610101698 A CN201610101698 A CN 201610101698A CN 105628745 A CN105628745 A CN 105628745A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- 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 invention relates to a preparation method for a nitrogen dioxide gas sensor, in particular to a gas sensor constructed based on a novel titanium-dioxide-based porous nanocomposite and belongs to the technical field of novel nanometer functional materials and environment monitoring.The sensor can be used for detecting the content of nitrogen dioxide gas in the environment.According to the method, the two-dimensional nanocomposite Ce-MoO3/TiO2@g-C3N4 obtained by means of in-situ compositing of a cerium-doped molybdenum oxide/titanium dioxide nanosheet on carbon nitride is prepared first, and the gas sensor which is sensitive and quickly responsive to nitrogen dioxide gas is constructed according to the characteristics of the material that the specific surface area is large, mesoporous gas absorption is high, and electron transfer affects sensitivity due to change in gas on the surface of the material.
Description
Technical field
The preparation method that the present invention relates to a kind of nitrogen dioxide gas sensor. Belong to Nano-function thin films and environmental monitoring technology field.
Background technology
Nitrogen dioxide is the gaseous material of a kind of brownish red, high activity, also known as hyponitric acid. One of nitrogen dioxide or the origin cause of formation of acid rain, the environmental effect brought is varied, including: the impact on competition between wetland and terrestrial plant species with composition change, the reduction of atmospheric visibility, the acidifying of surface water, eutrophication (owing to causing anoxia rich in the nutrient algal bloom such as nitrogen, phosphorus in water) and increase in water body and be harmful to Fish and other hydrobiological content of toxins. After human body sucks nitrogen dioxide, initial stage only has slight eye and upper respiratory tract irritation, such as pharyngeal discomfort, dry cough etc.,, there is uncomfortable in chest, respiratory distress, coughs, coughs up frothy sputum, cyanosis etc. in often Late-onset pulmonary edema, adult respiratory distress syndrome after a few hours to tens hour or incubation period longer time. Can complicated with pneumothorax and mediastinal emphysema.
Detection method for nitrogen dioxide gas mainly has chemical analysis method and instrument testing method. Though chemical analysis method is simple to operate, but sensitivity is not high and the shortcoming such as cannot reuse; Instrument testing method, the nitrogen dioxide gas concentration in air is carried out detection by quantitative by main use nitrogen dioxide gas instrumentation, has highly sensitive, reusable, automaticity advantages of higher, and is widely applied in the middle of commercial production.
For the nitrogen dioxide gas detector that instrument testing method uses, most crucial parts are the gas sensors that nitrogen dioxide 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 is based on the velocity of wave of SAW device and frequency can be drifted about with the change of external environment. It mainly includes 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 sensor resistance value R in air atmosphereaWith sensor resistance value R in certain density tested gas atmospheregRatio, namely
Therefore, probe into that adsorptivity is strong, stability good, the active height of catalysis, nitrogen dioxide gas had specific recognition and can the gas sensing materials of detection by quantitative, and then preparation have highly sensitive, response quickly, commercial production, human health are had important using value by the nitrogen dioxide gas sensor of the characteristic such as recovery time is short, are also emphasis and the difficult point of environmental monitoring technology area research simultaneously.
Summary of the invention
It is an object of the invention to provide a kind of prepare simple, highly sensitive, detect quickly available in the preparation method of gas sensor of nitrogen dioxide gas detection, prepared sensor, can be used for quick, the Sensitive Detection of nitrogen dioxide gas. Based on this purpose, the method comprises the steps of firstly, preparing the titania-based porous nano composite of a kind of New Two Dimensional nano composite material, i.e. the two-dimensional nano composite Ce-MoO of the molybdenum oxide/titanium dioxide nanoplate of In-situ reaction cerium dopping on carbonitride3/TiO2g-C3N4, utilize the specific surface area that this material is big, mesoporous high gas absorption characteristic and electron transmission to be affected many characteristics of sensitivity by the change of material surface gas, it is achieved that nitrogen dioxide gas has the structure of the gas sensor of response sensitive, quick.
The technical solution used in the present invention is as follows:
1. based on a preparation method for the nitrogen dioxide gas sensor of titania-based porous nano composite, the described two-dimensional nano composite Ce-MoO that titania-based porous nano composite is the molybdenum oxide/titanium dioxide nanoplate of In-situ reaction cerium dopping on carbonitride3/TiO2g-C3N4;
It is characterized in that, described preparation method includes following preparation process:
(1) Ce-MoO3/TiO2g-C3N4Preparation;
(2) preparation of nitrogen dioxide gas sensor;
Wherein, step (1) prepares Ce-MoO3/TiO2g-C3N4Concretely comprise the following steps:
First, take 0.6 ~ 1.0mmol sodium molybdate and 0.8 ~ 1.2mmol cerium salt joins in 5mL butyl titanate, in whipping process, it is slowly added to 0.5 ~ 0.8mL Fluohydric acid., react in a kettle. at 160 ~ 200 DEG C 18 ~ 24 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, take the dried solid of 150 ~ 250mg and mix with 400mg tripolycyanamide, and grind into powder; Then, putting in Muffle furnace by the powder of grinding, 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, namely prepares Ce-MoO3/TiO2g-C3N4;
Described cerium salt is selected from one of following: cerous sulfate, cerium chloride, cerous nitrate;
Step (2) prepares concretely comprising the following steps of nitrogen dioxide gas sensor:
First, the Ce-MoO of preparation in step (1) is taken3/TiO2g-C3N4100mg and 0.5 ~ 2.0mmol cerium oxide is placed in mortar, adds dehydrated alcohol, is coated uniformly on insulating ceramics tube-surface and forms film, at room temperature dry after being ground to pasty state; Then, the platinum filament of earthenware both sides and heater strip are welded with base; Finally, the element welded is placed in detecting instrument, carries out burin-in process by regulating heating voltage to 4.22V, namely prepare nitrogen dioxide gas sensor.
2. the application of the nitrogen dioxide gas sensor prepared by preparation method as claimed in claim 1, it is characterised in that can apply to the detection of nitrogen dioxide gas, detection is limited to 0.005mg/m3��
The useful achievement of the present invention
(1) nitrogen dioxide gas sensor of the present invention preparation is simple, easy to operate, it is achieved that the selective enumeration method quick, sensitive, high to nitrogen dioxide gas, has market development prospect;
(2) present invention is prepared for New Two Dimensional nano material Ce-MoO first3/TiO2g-C3N4Fully contact with titanium dioxide nanoplate due to cerium growth in situ on molybdenum oxide/titanium dioxide nanoplate, utilize the mutual promoting action of both the metal surface plasma body effect of cerium and molybdenum oxide and titanium dioxide, it is effectively increased semiconductor substrate electron transmission ability and catalysis activity, and cerium is corresponding to nitrogen dioxide gas ground specificity, although solve the relatively larger and mesoporous high gas absorption characteristic of titanium dioxide nanoplate specific surface area suitable in nitrogen dioxide air-sensitive host material, but the technical problem that gas-sensitive activity is not high and impedance variation is unstable; Simultaneously because carbonitride g-C3N4Good electric conductivity, add titanium dioxide nanoplate thereon fully dispersed, greatly increase electron transmission ability, solve the technical problem that air-sensitive host material impedance quickly responds with gas change, therefore, effective preparation of this material, has important scientific meaning and using value.
Detailed description of the invention
Embodiment 1Ce-MoO3/TiO2g-C3N4Preparation
First, take 0.6mmol sodium molybdate and 0.8mmol cerium salt joins in 5mL butyl titanate, in whipping process, it is slowly added to 0.5mL Fluohydric acid., reacts in a kettle. at 160 DEG C 24 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, take the dried solid of 150mg and mix with 400mg tripolycyanamide, and grind into powder; Then, putting in Muffle furnace by the powder of grinding, programming rate is 1 DEG C/min, calcines 5 hours at 480 DEG C; Finally, the powder after calcining is cooled to room temperature, namely prepares Ce-MoO3/TiO2g-C3N4;
Described cerium salt is cerous sulfate.
Embodiment 2Ce-MoO3/TiO2g-C3N4Preparation
First, take 0.8mmol sodium molybdate and 1.0mmol cerium salt joins in 5mL butyl titanate, in whipping process, it is slowly added to 0.65mL Fluohydric acid., reacts in a kettle. at 180 DEG C 21 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, take the dried solid of 200mg and mix with 400mg tripolycyanamide, and grind into powder; Then, putting in Muffle furnace by the powder of grinding, programming rate is 2 DEG C/min, calcines 2 hours at 520 DEG C; Finally, the powder after calcining is cooled to room temperature, namely prepares Ce-MoO3/TiO2g-C3N4;
Described cerium salt is cerium chloride.
Embodiment 3Ce-MoO3/TiO2g-C3N4Preparation
First, take 1.0mmol sodium molybdate and 1.2mmol cerium salt joins in 5mL butyl titanate, in whipping process, it is slowly added to 0.8mL Fluohydric acid., reacts in a kettle. at 200 DEG C 18 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, take the dried solid of 250mg and mix with 400mg tripolycyanamide, and grind into powder; Then, putting in Muffle furnace by the powder of grinding, 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, namely prepares Ce-MoO3/TiO2g-C3N4;
Described cerium salt is cerous nitrate.
The preparation of embodiment 4 nitrogen dioxide gas sensor
First, the Ce-MoO of preparation in Example 13/TiO2g-C3N4100mg and 0.5mmol cerium oxide is placed in mortar, adds dehydrated alcohol, is coated uniformly on insulating ceramics tube-surface and forms film, at room temperature dry after being ground to pasty state; Then, the platinum filament of earthenware both sides and heater strip are welded with base; Finally, being placed in detecting instrument by the element welded, carry out burin-in process by regulating heating voltage to 4.22V, namely prepare nitrogen dioxide gas sensor, be applied to the detection of nitrogen dioxide gas, detection is limited to 0.005mg/m3��
The preparation of embodiment 5 nitrogen dioxide gas sensor
First, the Ce-MoO of preparation in Example 23/TiO2g-C3N4100mg and 1.2mmol cerium oxide is placed in mortar, adds dehydrated alcohol, is coated uniformly on insulating ceramics tube-surface and forms film, at room temperature dry after being ground to pasty state; Then, the platinum filament of earthenware both sides and heater strip are welded with base; Finally, being placed in detecting instrument by the element welded, carry out burin-in process by regulating heating voltage to 4.22V, namely prepare nitrogen dioxide gas sensor, be applied to the detection of nitrogen dioxide gas, detection is limited to 0.005mg/m3��
The preparation of embodiment 6 nitrogen dioxide gas sensor
First, the Ce-MoO of preparation in Example 33/TiO2g-C3N4100mg and 2.0mmol cerium oxide is placed in mortar, adds dehydrated alcohol, is coated uniformly on insulating ceramics tube-surface and forms film, at room temperature dry after being ground to pasty state; Then, the platinum filament of earthenware both sides and heater strip are welded with base; Finally, being placed in detecting instrument by the element welded, carry out burin-in process by regulating heating voltage to 4.22V, namely prepare nitrogen dioxide gas sensor, be applied to the detection of nitrogen dioxide gas, detection is limited to 0.005mg/m3��
Claims (2)
1. based on a preparation method for the nitrogen dioxide gas sensor of titania-based porous nano composite, the described two-dimensional nano composite Ce-MoO that titania-based porous nano composite is the molybdenum oxide/titanium dioxide nanoplate of In-situ reaction cerium dopping on carbonitride3/TiO2g-C3N4;
It is characterized in that, described preparation method includes following preparation process:
(1) Ce-MoO3/TiO2g-C3N4Preparation;
(2) preparation of nitrogen dioxide gas sensor;
Wherein, step (1) prepares Ce-MoO3/TiO2g-C3N4Concretely comprise the following steps:
First, take 0.6 ~ 1.0mmol sodium molybdate and 0.8 ~ 1.2mmol cerium salt joins in 5mL butyl titanate, in whipping process, it is slowly added to 0.5 ~ 0.8mL Fluohydric acid., react in a kettle. at 160 ~ 200 DEG C 18 ~ 24 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, take the dried solid of 150 ~ 250mg and mix with 400mg tripolycyanamide, and grind into powder; Then, putting in Muffle furnace by the powder of grinding, 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, namely prepares Ce-MoO3/TiO2g-C3N4;
Described cerium salt is selected from one of following: cerous sulfate, cerium chloride, cerous nitrate;
Step (2) prepares concretely comprising the following steps of nitrogen dioxide gas sensor:
First, the Ce-MoO of preparation in step (1) is taken3/TiO2g-C3N4100mg and 0.5 ~ 2.0mmol cerium oxide is placed in mortar, adds dehydrated alcohol, is coated uniformly on insulating ceramics tube-surface and forms film, at room temperature dry after being ground to pasty state; Then, the platinum filament of earthenware both sides and heater strip are welded with base; Finally, the element welded is placed in detecting instrument, carries out burin-in process by regulating heating voltage to 4.22V, namely prepare nitrogen dioxide gas sensor.
2. the application of the nitrogen dioxide gas sensor prepared by preparation method as claimed in claim 1, it is characterised in that can apply to the detection of nitrogen dioxide gas, detection is limited to 0.005mg/m3��
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| CN113960250A (en) * | 2021-09-27 | 2022-01-21 | 山东大学 | Mixed gas detection system and method for shield tunnel |
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