CN103293193A - Titanium dioxide/graphene-based nitrogen dioxide sensor and preparation method thereof - Google Patents
Titanium dioxide/graphene-based nitrogen dioxide sensor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a titanium dioxide/graphene-based nitrogen dioxide sensor and a preparation method thereof. The sensor is composed of a ceramic substrate, electrodes, a titanium dioxide/graphene composite material, a heater, a thermocouple and a signal processing part, wherein the titanium dioxide/graphene composite material is a NO2-gas-sensitive functional material, and achieves the goal of sensing NO2 by measuring the variation of the material resistance when NO2 is adsorbed to the material surface; and the measured signal is resistance variations of the sensor or voltage and current variations in the circuit due to the resistance variations of the sensor. The sensor has the characteristics of low working temperature, wide temperature response range, high sensitivity, high detection limit and short response time.
Description
Technical field
The present invention relates to a kind of nitrogen dioxide sensor based on titania/Graphene and preparation method, being specifically related to a kind of is the resistance sensor of gas sensitive with titania/Graphene, according to the demarcation of titania/Graphene sensitive membrane resistance change under working temperature, realize NO
2Detect.
Background technology
NO
2Being a kind of atmosphere pollution of showing great attention to, is the key factor that ozone and acid rain form.Often be exposed to the NO of high concentration
2In the gaseous environment, can cause the disease of respiratory system.Automotive exhaust gas, industrial dye burning and the nitrogenous fertilizer production process of nitric acid all can make the NO in the surrounding environment
2Concentration increases.Simultaneously, at some special occasions, need be to NO
2Monitor in real time, the nitro oxidizer commonly used as the spacecraft propulsion agent easily resolves into NO
2, need whether reveal propellant and monitor.Therefore, NO
2Detection for environmental protection, human health and the NO significant, highly sensitive, that operating temperature range is wide, response speed is fast that keeps the safety in production
2The development of sensor is very necessary.
Metal oxide has absorption and catalysis double effect concurrently in the gas context of detection, belongs to surperficial control type.At NO
2In the detection method, metal oxide resistor (MOX) formula sensor has advantages such as simple in structure, easy to make.Metal oxide resistor (MOX) formula sensor generally based on oxidisability or reducibility gas when metal oxide surface absorption or the desorption, oxide resistor changes and obtains measuring-signal.Yet, such semiconductor transducer serviceability temperature higher (200 ℃-500 ℃), so the NO of development temperature low (room temperature to 200 ℃)
2Sensor has important practical significance.
Graphene is a kind of carbon nanomaterial with two-dimension plane structure, and its basic structural unit is stable hexatomic ring.Its special monoatomic layer structure makes its physicochemical property with many uniquenesses, comprises big specific surface area, excellent conducting performance etc.Utilize its big specific surface area can strengthen the absorption of gas.
Summary of the invention
The object of the invention is, a kind of nitrogen dioxide sensor based on titania/Graphene and preparation method are provided, this sensor is to be grouped into by ceramic bases, electrode, titania/graphene composite material, well heater and thermopair and signal processing part, uses titania/graphene composite material to be NO
2The gas-sensing function material is by measuring N O
2The variation of material resistance reaches NO when being adsorbed to material surface
2The purpose of sensing; Measuring-signal is that voltage, electric current change in the sensor resistance circuit that changes or cause thus; Sensor of the present invention has that working temperature is low, the temperature-responsive wide ranges, highly sensitive, detect limit for height, short feature of response time.
A kind of nitrogen dioxide sensor based on titania/Graphene of the present invention, this sensor is by ceramic bases, electrode, titania/graphene composite material, well heater and thermopair, signal processing and loudspeaker are formed, go up fixed electorde (2) in ceramic bases (1), by titania/graphene composite material (3) electrode (2) is communicated with, electrode (2) is connected with signal processor (5), well heater and thermopair (4) are fixed on the bottom of ceramic bases (1), with titania/graphene composite material (3) water or ethanol furnishing slurry, adopt spraying, smear or the method for electrochemical deposition is applied to and has silver, on the ceramic bases (1) of gold or copper electrode (2), dry naturally and get final product.
The preparation method of described nitrogen dioxide sensor based on titania/Graphene follows these steps to carry out:
The preparation of titania/graphene composite material (3):
A, use conventional H ummer method prepare the graphene oxide dispersion liquid, and the graphene oxide dispersion liquid with preparation is concentrated into 10 μ g/mL-10 mg/mL again;
B, get the graphene oxide dispersion liquid, adding concentration is the TiCl of 1 mmol/L-1 mol/L
4Or butyl titanate solution, stir, under room temperature-100 ℃ condition, react 1-168 h, obtain potpourri;
C, with the potpourri that step b obtains, make water and ethanol carry out ultrasonic dispersion and centrifuging respectively repeatedly;
D, the precipitation after will separating, dry under the temperature 10-90 ℃ of condition, be N at protective atmosphere
2, under the He, Ar inert gas, annealing is 10min-3 hour under the temperature 300-800 ℃ of condition, obtains titania/graphene composite material that mass ratio is 1000:1-20:3;
The preparation of sensor:
E, go up fixed electorde (2) in ceramic bases (1), by titania/graphene composite material (3) electrode (2) is communicated with, electrode (2) is connected with signal processor (5), well heater and thermopair (4) are fixed on the bottom of ceramic bases (1), with titania/graphene composite material (3) water or the ethanol furnishing slurry that obtains, employing sprays, smears or the method for electrochemical deposition is applied on the ceramic bases (1) that has silver, gold or copper electrode (2), dries naturally to get final product.
It is 3.6 mg/mL that step a graphene oxide dispersion liquid concentrates concentration.
TiCl among the step b
4Or the butyl titanate solution concentration is 0.1 mol/L, 70 ℃ of temperature of reaction, time 48h.
Baking temperature is 50 ℃ in the steps d, and protective atmosphere is N
2, annealing temperature is 500 ℃, and annealing time is 30 min, and the mass ratio of titania and Graphene is 20:1.
Ceramic bases among the step e (1) is plane, cylindric, and the material of ceramic bases (1) is glass or stupalith.
The method for making of electrode among the step e (2) is printing or ion sputtering plated film.
The present invention can carry out slurry earlier and apply in making sensor, laggard column electrode is made; The graphite that uses among the present invention, the titanium source, atmosphere, oxygenant can adopt commercially available material and reagent.
A kind of nitrogen dioxide sensor and preparation method based on titania/Graphene of the present invention, this sensor has low working temperature and wide temperature-responsive scope: room temperature to 300 ℃; High detectability and measurement range: greater than 2 ppb (part per billion, V/V); The short response time: about 200 s.NO of the present invention
2Sensor can be used as NO
2Alarm is demarcated this sensor earlier at specified temp, the sensor of demarcating is connected in the circuit, carries out NO under relevant temperature
2Detect.NO in test gas
2Concentration surpasses when warning value is set, and the resistance in the circuit, voltage or electric current surpass corresponding setting value, and this moment, warning system triggered, and sent alerting signal.
Description of drawings
Fig. 1 is NO of the present invention
2The sensor construction synoptic diagram;
Fig. 2 is the sem photograph of gas sensitive titania/Graphene of the present invention;
Fig. 3 is the X-ray diffractogram of gas sensitive titania/Graphene of the present invention;
Fig. 4 is NO of the present invention
2Sensor under 200 ℃ of conditions of temperature to variable concentrations NO
2Response curve: 5 ppb, 10 ppb, 50 ppb, 100 ppb, 200 ppb, 500 ppb figure;
Fig. 5 is NO of the present invention
2Sensor under 200 ℃ of conditions of temperature to NO
2Calibration map;
Fig. 6 is NO of the present invention
2Sensor is to 100ppb NO
2Gas response and response time figure.
Embodiment:
Below in conjunction with drawings and Examples this patent is elaborated:
Embodiment 1:
The making of sensor:
Go up fixed electorde (2) in ceramic bases (1), by titania/graphene composite material (3) electrode (2) is communicated with, electrode (2) is connected with signal processor (5), and well heater and thermopair (4) are fixed on the bottom of ceramic bases (1), as shown in Figure 1;
The preparation of titania/graphene composite material:
Use conventional H ummer method to prepare the graphene oxide dispersion liquid, the graphene oxide dispersion liquid with preparation is concentrated into 3.6 mg/mL again;
Get 1.12 mL graphene oxide dispersion liquids, adding 10 mL concentration is the TiCl of 0.1 mol/L
4Solution stirs, and reaction 48 h obtain potpourri under 70 ℃ of conditions of temperature;
Make water and ethanol carry out ultrasonic dispersion and centrifuging respectively repeatedly in potpourri;
With the precipitation after separating, under 50 ℃ of conditions of temperature after the drying, at N
2Under the atmosphere protection, 500 ℃ of annealing of temperature, 30 min obtain titania/graphene composite material that mass ratio is 20:1, and scanning electron microscope and X ray picture are respectively as shown in Figures 2 and 3;
Titania/graphene composite material water furnishing slurry with obtaining is applied on the ceramic bases (1) that has copper electrode 2, dry naturally, 200 ℃ of temperature to variable concentrations NO
2Respond, demarcate, according to calibration curve, carry out NO for 200 ℃ in temperature
2The detection of concentration.
Embodiment 2:
The making of sensor is carried out according to embodiment 1;
The preparation of titania/graphene composite material:
Use conventional H ummer method to prepare the graphene oxide dispersion liquid, the graphene oxide dispersion liquid with preparation is concentrated into 10 μ g/mL again;
Get 1 mL Graphene, adding 10 mL concentration is the TiCl of 1 mmol/L
4Solution stirs, and reacts 168 h at ambient temperature, obtains potpourri;
Make water and ethanol carry out ultrasonic dispersion and centrifuging respectively repeatedly in potpourri;
With the precipitation after separating, after the drying, under the Ar atmosphere protection, 800 ℃ of annealing of temperature, 10 min obtain titania/graphene composite material that mass ratio is 8:1 under 90 ℃ of conditions of temperature;
Titania/graphene composite material water furnishing slurry with obtaining is sprayed on the ceramic bases (1) that has copper electrode 2, dry naturally, with constant voltage mode, in room temperature to variable concentrations NO
2Respond, demarcate, according to calibration curve, carry out NO in room temperature
2The detection of concentration.
Embodiment 3:
The making of sensor is carried out according to embodiment 1;
The preparation of titania/graphene composite material:
Use conventional H ummer method to prepare the graphene oxide dispersion liquid, the graphene oxide dispersion liquid with preparation is concentrated into 10 mg/mL again;
Get 1 mL graphene oxide, adding 10 mL concentration is the TiCl of 1 mol/L
4Solution stirs, and reaction 1 h obtains potpourri under 100 ℃ of conditions of temperature;
Make water and ethanol carry out ultrasonic dispersion and centrifuging respectively repeatedly in potpourri;
With the precipitation after separating, after 25 ℃ of dryings, under the He atmosphere protection, 300 ℃ of annealing of temperature, 3 h obtain titania/graphene composite material that mass ratio is 80:1;
Titania/graphene composite material water furnishing slurry with obtaining is applied on the substrate of glass (1) that has silver electrode (2), dry naturally, with constant current mode, 300 ℃ of temperature to variable concentrations NO
2Respond, demarcate, according to calibration curve, carry out NO at 300 ℃
2The detection of concentration.
Embodiment 4:
The making of sensor is carried out according to embodiment 1;
The preparation of titania/graphene composite material:
Use conventional H ummer method to prepare the graphene oxide dispersion liquid, the graphene oxide dispersion liquid with preparation is concentrated into 3.6 mg/mL again;
Get 1.12 mL graphene oxides, adding 10 mL concentration is the TiCl of 0.1 mol/L
4Solution stirs, and reaction 48 h obtain potpourri under 70 ℃ of conditions of temperature;
Make water and ethanol carry out ultrasonic dispersion and centrifuging respectively repeatedly in potpourri;
With the precipitation after separating, dry under 50 ℃ of conditions of temperature, at N
2Under the atmosphere protection, 500 ℃ of annealing of temperature, 30 min obtain titania/graphene composite material that mass ratio is 20:1;
With the titania/graphene composite material that obtains ethanol furnishing slurry, on the plane ceramic bases (1) that is sprayed on, naturally dry, use ion sputtering plated film mode to make gold electrode on titania/Graphene sensitive material surface, be signal with the resistance variations, at 200 ℃ of NO to variable concentrations of temperature
2Respond, demarcate, according to calibration curve, carry out NO for 200 ℃ in temperature
2The detection of concentration.
Embodiment 5:
The making of sensor is carried out according to embodiment 1;
The preparation of titania/graphene composite material:
Use conventional H ummer method to prepare the graphene oxide dispersion liquid, the graphene oxide dispersion liquid with preparation is concentrated into 3.6 mg/mL again;
Get 1.12 mL graphene oxides, adding 10 mL concentration is the TiCl of 0.1 mol/L
4Solution stirs, and reaction 48 h obtain potpourri under 70 ℃ of conditions of temperature;
Make water and ethanol carry out ultrasonic dispersion and centrifuging respectively repeatedly in potpourri;
With the precipitation after separating, under 50 ℃ of conditions of temperature after the drying, at N
2Under the atmosphere protection, 500 ℃ of annealing of temperature, 30 min obtain titania/graphene composite material that mass ratio is 20:1;
With the titania/graphene composite material water furnishing slurry that obtains, method with electrochemical deposition, titania/graphene composite material is deposited in the cylindrical glass substrate (1), naturally dry, use the mode of printing, making silver electrode 2 on titania/graphene composite material surface, is signal with the resistance variations, at 200 ℃ of NO to variable concentrations of temperature
2Respond, demarcate, according to calibration curve, carry out NO for 200 ℃ in temperature
2The detection of concentration.
Embodiment 6:
The making of sensor is carried out according to embodiment 1;
The preparation of titania/graphene composite material:
Use conventional H ummer method to prepare the graphene oxide dispersion liquid, the graphene oxide dispersion liquid with preparation is concentrated into 10 μ g/mL again;
Get 1.12 mL Graphenes, slowly joining 10 mL concentration is 0.1 mol/L butyl titanate ethanolic solution, stirs, and reaction 48 h obtain potpourri under the room temperature condition;
Make water and ethanol carry out ultrasonic dispersion and centrifuging respectively repeatedly in potpourri;
With the precipitation after separating, after drying under 50 ℃ of conditions of temperature, at N
2Under the atmosphere protection, 500 ℃ of annealing of temperature, 30 min obtain titania/graphene composite material that mass ratio is 20:1;
Titania/graphene composite material water furnishing slurry with obtaining is applied in the substrate (1) that has copper electrode (2), dry naturally, 200 ℃ of temperature to 5-500 ppb concentration NO
2Respond, demarcate, according to calibration curve, carry out NO for 200 ℃ in temperature
2The detection of concentration.
Embodiment 7:
Press embodiment 1 with the NO that makes
2 Sensing element 200 ℃ of temperature to variable concentrations NO
2Respond, its result works as NO as shown in Figure 4
2Be adsorbed on material surface, its resistance reduces, and corresponding response concentration is 5 ppb, 10 ppb, 50 ppb, 100 ppb, 200 ppb, 500 ppb, and its calibration result fit equation as shown in Figure 5 is the Langmuir equation at constant temperature
, wherein
Be responsiveness, be defined as the ratio of resistance change and resistance initial value,
Be NO
2Concentration, parameter
,
Embodiment 8:
Press embodiment 1 with the NO that makes
2Sensing element is the NO of 100 ppb to concentration for 200 ℃ in temperature
2Response time, its result is for as shown in Figure 6, as NO
2Be adsorbed on material surface, its resistance reduces, and roughly is divided into 2 stages: response phase is 100 s-300 s fast; Saturation stage is 300 s-600 s, and be 100 s release time.
Embodiment 9:
With the NO that makes
2Sensing element is after demarcating under the specific temperature, as NO
2The core component of alarm connects power supply, and ammeter and warning system are carried out NO in corresponding temperature
2Monitoring in real time and warning.
Claims (7)
1. nitrogen dioxide sensor based on titania/Graphene, it is characterized in that this sensor is by ceramic bases, electrode, titania/graphene composite material, well heater and thermopair, signal processing and loudspeaker are formed, go up fixed electorde (2) in ceramic bases (1), by titania/graphene composite material (3) electrode (2) is communicated with, electrode (2) is connected with signal processor (5), well heater and thermopair (4) are fixed on the bottom of ceramic bases (1), with titania/graphene composite material (3) water or ethanol furnishing slurry, adopt spraying, smear or the method for electrochemical deposition is applied to and has silver, on the ceramic bases (1) of gold or copper electrode (2), dry naturally and get final product.
2. the preparation method of the nitrogen dioxide sensor based on titania/Graphene according to claim 1 is characterized in that following these steps to carrying out:
The preparation of titania/graphene composite material (3):
A, use conventional H ummer method prepare the graphene oxide dispersion liquid, and the graphene oxide dispersion liquid with preparation is concentrated into 10 μ g/mL-10 mg/mL again;
B, get the graphene oxide dispersion liquid, adding concentration is the TiCl of 1 mmol/L-1 mol/L
4Or butyl titanate solution, stir, under room temperature-100 ℃ condition, react 1-168 h, obtain potpourri;
C, with the potpourri that step b obtains, make water and ethanol carry out ultrasonic dispersion and centrifuging respectively repeatedly;
D, the precipitation after will separating, dry under the temperature 10-90 ℃ of condition, be N at protective atmosphere
2, under the He, Ar inert gas, annealing is 10 min-3 hours under the temperature 300-800 ℃ of condition, obtains titania/graphene composite material that mass ratio is 1000:1-20:3;
The preparation of sensor:
E, go up fixed electorde (2) in ceramic bases (1), by titania/graphene composite material (3) electrode (2) is communicated with, electrode (2) is connected with signal processor (5), well heater and thermopair (4) are fixed on the bottom of ceramic bases (1), with titania/graphene composite material (3) water or the ethanol furnishing slurry that obtains, employing sprays, smears or the method for electrochemical deposition is applied on the ceramic bases (1) that has silver, gold or copper electrode (2), dries naturally to get final product.
3. method according to claim 2 is characterized in that it is 3.6 mg/mL that step a graphene oxide dispersion liquid concentrates concentration.
4. method according to claim 2 is characterized in that the TiCl among the step b
4Or the butyl titanate solution concentration is 0.1 mol/L, 70 ℃ of temperature of reaction, time 48h.
5. method according to claim 2 is characterized in that baking temperature is 50 ℃ in the steps d, and protective atmosphere is N
2, annealing temperature is 500 ℃, and annealing time is 30 min, and the mass ratio of titania and Graphene is 20:1.
6. method according to claim 2 is characterized in that ceramic bases among the step e (1) for plane, cylindric, and the material of ceramic bases (1) is glass or stupalith.
7. method according to claim 2 is characterized in that the method for making of electrode among the step e (2) is printing or ion sputtering plated film.
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| CN104569076A (en) * | 2015-01-08 | 2015-04-29 | 上海师范大学 | Pencil drawing type NO2 sensing element and production method thereof |
| CN104914138A (en) * | 2015-07-03 | 2015-09-16 | 深圳市共进电子股份有限公司 | Humidity sensor, humidity sensor array and preparation method thereof |
| CN104958073A (en) * | 2015-07-03 | 2015-10-07 | 深圳市共进电子股份有限公司 | Humidity sensor, electronic device and respiration detection system and method |
| CN107064218A (en) * | 2016-10-31 | 2017-08-18 | 扬州大学 | Based on reduced graphene semiconductor room temperature nitrogen dioxide sensor preparation method |
| CN107219270A (en) * | 2017-06-01 | 2017-09-29 | 大连理工大学 | It is a kind of new based on redox graphene tungsten disulfide composite ammonia gas sensor and its preparation technology |
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| CN103995025A (en) * | 2014-05-16 | 2014-08-20 | 上海师范大学 | Printed type graphene-based NO2 gas-sensitive element and preparation method thereof |
| CN104569076A (en) * | 2015-01-08 | 2015-04-29 | 上海师范大学 | Pencil drawing type NO2 sensing element and production method thereof |
| CN104914138A (en) * | 2015-07-03 | 2015-09-16 | 深圳市共进电子股份有限公司 | Humidity sensor, humidity sensor array and preparation method thereof |
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| CN109690280B (en) * | 2016-10-31 | 2022-03-01 | 松下电器产业株式会社 | Chemical substance concentrator and chemical substance detection device |
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| CN107219270A (en) * | 2017-06-01 | 2017-09-29 | 大连理工大学 | It is a kind of new based on redox graphene tungsten disulfide composite ammonia gas sensor and its preparation technology |
| CN108275683A (en) * | 2018-01-17 | 2018-07-13 | 中国科学院过程工程研究所 | A kind of metal-base composites and its preparation method and application |
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| CN109896499B (en) * | 2019-03-04 | 2021-02-09 | 中国电子科技集团公司第四十九研究所 | Ceramic microstructure graphene gas sensor and manufacturing method thereof |
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