CN103293193B - A kind of nitrogen dioxide sensor based on titanium dioxide/graphene and preparation method - Google Patents
A kind of nitrogen dioxide sensor based on titanium dioxide/graphene and preparation method Download PDFInfo
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- CN103293193B CN103293193B CN201310234385.3A CN201310234385A CN103293193B CN 103293193 B CN103293193 B CN 103293193B CN 201310234385 A CN201310234385 A CN 201310234385A CN 103293193 B CN103293193 B CN 103293193B
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Abstract
The present invention relates to a kind of nitrogen dioxide sensor based on titanium dioxide/graphene and preparation method, this sensor is grouped into by ceramic bases, electrode, titanium dioxide/graphene composite material, well heater and thermopair and signal processing part, and use titanium dioxide/graphene composite material is NO
2gas-sensitive Functional Materials, by measuring NO
2the change being adsorbed to material resistance during material surface reaches NO
2the object of sensing; Measuring-signal is voltage, curent change in sensor resistance change or the circuit that causes thus; This sensor has that working temperature is low, temperature-responsive wide ranges, highly sensitive, detect limit for height, response time short feature.
Description
Technical field
The present invention relates to a kind of nitrogen dioxide sensor based on titanium dioxide/graphene and preparation method, being specifically related to a kind of take titanium dioxide/graphene as the resistance sensor of gas sensitive, according to the demarcation of titanium dioxide/graphene sensitive membrane resistance change at the 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 are formed.Often be exposed to the NO of high concentration
2in gaseous environment, the disease of respiratory system can be caused.The burning of automotive exhaust gas, industrial dye and nitric acid formulation fertilizer containing nitrogen production run all can make the NO in surrounding environment
2concentration increases.Meanwhile, at some special occasions, need NO
2carry out Real-Time Monitoring, nitro oxidizer as conventional in spacecraft propulsion agent easily resolves into NO
2, whether need reveal propellant and monitor.Therefore, NO
2detection for environmental protection, human health and keep the safety in production significant, highly sensitive, operating temperature range wide, the NO of fast response time
2the development of sensor is very necessary.
Metal oxide has absorption and catalysis double effect concurrently in gas detect, belongs to Surface controlled type.At NO
2in detection method, metal oxide resistor (MOX) formula sensor has the advantages such as structure is simple, easy to make.Metal oxide resistor (MOX) formula sensor generally based on oxidisability or reducibility gas when metal oxide surface absorption or desorption, oxide resistor changes and obtains measuring-signal.But, such semiconductor transducer serviceability temperature higher (200 DEG C-500 DEG C), the NO of therefore development temperature low (room temperature to 200 DEG C)
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 it have the physicochemical property of many uniquenesses, comprises large specific surface area, good electric conductivity etc.The specific surface area utilizing it large can strengthen the absorption of gas.
Summary of the invention
The object of the invention is, a kind of nitrogen dioxide sensor based on titanium dioxide/graphene and preparation method are provided, this sensor is grouped into by ceramic bases, electrode, titanium dioxide/graphene composite material, well heater and thermopair and signal processing part, and use titanium dioxide/graphene composite material is NO
2gas-sensitive Functional Materials, by measuring NO
2the change being adsorbed to material resistance during material surface reaches NO
2the object of sensing; Measuring-signal is voltage, curent change in sensor resistance change or the circuit that causes thus; Sensor of the present invention has that working temperature is low, temperature-responsive wide ranges, highly sensitive, detect limit for height, response time short feature.
A kind of nitrogen dioxide sensor based on titanium dioxide/graphene of the present invention, this sensor is by ceramic bases, electrode, titanium dioxide/graphene composite material, well heater and thermopair, signal processing and loudspeaker composition, at the upper fixed electorde (2) of ceramic bases (1), by titanium dioxide/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), by titanium dioxide/graphene composite material (3) water or ethanol furnishing slurry, adopt spraying, to smear or the method for electrochemical deposition is applied to silver, in the ceramic bases (1) of gold or copper electrode (2), naturally dry.
The preparation method of the described nitrogen dioxide sensor based on titanium dioxide/graphene, follows these steps to carry out:
The preparation of titanium dioxide/graphene composite material (3):
A, use conventional H ummer method are prepared graphene oxide dispersion, then the graphene oxide dispersion of preparation are concentrated into 10 μ g/mL-10 mg/mL;
B, get graphene oxide dispersion, add the TiCl that concentration is 1 mmol/L-1 mol/L
4or butyl titanate solution, stir, under room temperature-100 DEG C of conditions, react 1-168 h, obtain potpourri;
C, the potpourri that step b is obtained, Reusability water and ethanol carry out ultrasonic disperse and centrifuging respectively;
D, by the precipitation after being separated, dry under temperature 10-90 DEG C of condition, be N at protective atmosphere
2, under He, Ar inert gas, anneal under temperature 300-800 DEG C of condition 10min-3 hour, obtains the titanium dioxide/graphene composite material that mass ratio is 1000:1-20:3;
The preparation of sensor:
E, at the upper fixed electorde (2) of ceramic bases (1), by titanium dioxide/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), by titanium dioxide/graphene composite material (3) water that obtains or ethanol furnishing slurry, employing sprays, smear or the method for electrochemical deposition is applied in the ceramic bases (1) with silver, gold or copper electrode (2), naturally dries.
It is 3.6 mg/mL that step a graphene oxide dispersion concentrates concentration.
TiCl in step b
4or butyl titanate solution concentration is 0.1 mol/L, temperature of reaction 70 DEG C, time 48h.
In steps d, baking temperature is 50 DEG C, and protective atmosphere is N
2, annealing temperature is 500 DEG C, and annealing time is 30 min, and the mass ratio of titania and Graphene is 20:1.
In step e, ceramic bases (1) is for plane, cylindric, and the material of ceramic bases (1) is glass or stupalith.
In step e, the method for making of electrode (2) is printing or ion sputtering film coating.
The present invention first can carry out slurry coating in making sensor, and laggard column electrode makes; The graphite used in the present invention, titanium source, atmosphere, oxygenant can adopt commercially available material and reagent.
A kind of nitrogen dioxide sensor based on titanium dioxide/graphene of the present invention and preparation method, this sensor has low working temperature and wide temperature-responsive scope: room temperature to 300 DEG C; High detectability and measurement range: be greater than 2 ppb (part per billion, V/V); The shorter response time: about 200 s.NO of the present invention
2sensor can be used as NO
2alarm, first demarcates this sensor at specified temp, and calibrated sensor is connected in circuit, carries out NO at the corresponding temperature
2detect.As NO in test gas
2concentration exceedes when arranging warning value, and the resistance in circuit, voltage or electric current exceed corresponding setting value, and now warning system triggers, and sends alerting signal.
Accompanying drawing explanation
Fig. 1 is NO of the present invention
2sensor construction schematic diagram;
Fig. 2 is the scanning electron microscope (SEM) photograph of gas sensitive titanium dioxide/graphene of the present invention;
Fig. 3 is the X-ray diffractogram of gas sensitive titanium dioxide/graphene of the present invention;
Fig. 4 is NO of the present invention
2sensor under temperature 200 DEG C of conditions 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 temperature 200 DEG C of conditions 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 described in detail:
Embodiment 1:
The making of sensor:
At the upper fixed electorde (2) of ceramic bases (1), by titanium dioxide/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 titanium dioxide/graphene composite material:
Use conventional H ummer method to prepare graphene oxide dispersion, then the graphene oxide dispersion of preparation is concentrated into 3.6 mg/mL;
Get 1.12 mL graphene oxide dispersion, add the TiCl that 10 mL concentration are 0.1 mol/L
4solution, stirs, and reacts 48 h, obtain potpourri under temperature 70 C condition;
Potpourri Reusability water and ethanol are carried out ultrasonic disperse and centrifuging respectively;
By the precipitation after separation, under temperature 50 C condition after drying, at N
2under atmosphere protection, temperature 500 DEG C annealing 30 min, obtain the titanium dioxide/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;
By the titanium dioxide/graphene composite material water furnishing slurry obtained, be applied in the ceramic bases (1) with copper electrode 2, naturally dry, temperature 200 DEG C to variable concentrations NO
2carry out responding, demarcating, according to calibration curve, carry out NO temperature 200 DEG C
2the detection of concentration.
Embodiment 2:
The making of sensor is carried out according to embodiment 1;
The preparation of titanium dioxide/graphene composite material:
Use conventional H ummer method to prepare graphene oxide dispersion, then the graphene oxide dispersion of preparation is concentrated into 10 μ g/mL;
Get 1 mL Graphene, add the TiCl that 10 mL concentration are 1 mmol/L
4solution, stirs, and reacts 168 h at ambient temperature, obtains potpourri;
Potpourri Reusability water and ethanol are carried out ultrasonic disperse and centrifuging respectively;
By the precipitation after separation, under temperature 90 DEG C of conditions after drying, under Ar atmosphere protection, temperature 800 DEG C annealing 10 min, obtain the titanium dioxide/graphene composite material that mass ratio is 8:1;
By the titanium dioxide/graphene composite material water furnishing slurry obtained, be sprayed in the ceramic bases (1) with copper electrode 2, naturally dry, with constant voltage mode, in room temperature to variable concentrations NO
2carry out responding, demarcating, 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 titanium dioxide/graphene composite material:
Use conventional H ummer method to prepare graphene oxide dispersion, then the graphene oxide dispersion of preparation is concentrated into 10 mg/mL;
Get 1 mL graphene oxide, add the TiCl that 10 mL concentration are 1 mol/L
4solution, stirs, and reacts 1 h, obtain potpourri under temperature 100 DEG C of conditions;
Potpourri Reusability water and ethanol are carried out ultrasonic disperse and centrifuging respectively;
By the precipitation after separation, after 25 DEG C of dryings, under He atmosphere protection, temperature 300 DEG C annealing 3 h, obtain the titanium dioxide/graphene composite material that mass ratio is 80:1;
By the titanium dioxide/graphene composite material water furnishing slurry obtained, be applied in the substrate of glass (1) with silver electrode (2), naturally dry, with constant current mode, temperature 300 DEG C to variable concentrations NO
2carry out responding, demarcating, according to calibration curve, carry out NO at 300 DEG C
2the detection of concentration.
Embodiment 4:
The making of sensor is carried out according to embodiment 1;
The preparation of titanium dioxide/graphene composite material:
Use conventional H ummer method to prepare graphene oxide dispersion, then the graphene oxide dispersion of preparation is concentrated into 3.6 mg/mL;
Get 1.12 mL graphene oxides, add the TiCl that 10 mL concentration are 0.1 mol/L
4solution, stirs, and reacts 48 h, obtain potpourri under temperature 70 C condition;
Potpourri Reusability water and ethanol are carried out ultrasonic disperse and centrifuging respectively;
By the precipitation after separation, dry under temperature 50 C condition, at N
2under atmosphere protection, temperature 500 DEG C annealing 30 min, obtain the titanium dioxide/graphene composite material that mass ratio is 20:1;
By the titanium dioxide/graphene composite material ethanol furnishing slurry obtained, in the plane ceramic substrate (1) be sprayed on, naturally dry, ion sputtering film coating mode is used to make gold electrode on titanium dioxide/graphene sensitive material surface, take resistance variations as signal, at temperature 200 DEG C of NO to variable concentrations
2carry out responding, demarcating, according to calibration curve, carry out NO temperature 200 DEG C
2the detection of concentration.
Embodiment 5:
The making of sensor is carried out according to embodiment 1;
The preparation of titanium dioxide/graphene composite material:
Use conventional H ummer method to prepare graphene oxide dispersion, then the graphene oxide dispersion of preparation is concentrated into 3.6 mg/mL;
Get 1.12 mL graphene oxides, add the TiCl that 10 mL concentration are 0.1 mol/L
4solution, stirs, and reacts 48 h, obtain potpourri under temperature 70 C condition;
Potpourri Reusability water and ethanol are carried out ultrasonic disperse and centrifuging respectively;
By the precipitation after separation, under temperature 50 C condition after drying, at N
2under atmosphere protection, temperature 500 DEG C annealing 30 min, obtain the titanium dioxide/graphene composite material that mass ratio is 20:1;
By the titanium dioxide/graphene composite material water furnishing slurry obtained, by the method for electrochemical deposition, titanium dioxide/graphene composite material is made to be deposited in cylindrical glass substrate (1), naturally dry, use the mode of printing, making silver electrode 2 on titanium dioxide/graphene composite material surface, take resistance variations as signal, at temperature 200 DEG C of NO to variable concentrations
2carry out responding, demarcating, according to calibration curve, carry out NO temperature 200 DEG C
2the detection of concentration.
Embodiment 6:
The making of sensor is carried out according to embodiment 1;
The preparation of titanium dioxide/graphene composite material:
Use conventional H ummer method to prepare graphene oxide dispersion, then the graphene oxide dispersion of preparation is concentrated into 10 μ g/mL;
Get 1.12 mL Graphenes, slowly joining 10 mL concentration is 0.1 mol/L butyl titanate ethanolic solution, stirs, reacts 48 h, obtain potpourri under room temperature condition;
Potpourri Reusability water and ethanol are carried out ultrasonic disperse and centrifuging respectively;
By the precipitation after separation, under temperature 50 DEG C of conditions after drying, at N
2under atmosphere protection, temperature 500 DEG C annealing 30 min, obtain the titanium dioxide/graphene composite material that mass ratio is 20:1;
By the titanium dioxide/graphene composite material water furnishing slurry obtained, be applied in the substrate (1) with copper electrode (2), naturally dry, temperature 200 DEG C to 5-500 ppb concentration NO
2carry out responding, demarcating, according to calibration curve, carry out NO temperature 200 DEG C
2the detection of concentration.
Embodiment 7:
By the NO that embodiment 1 will make
2sensing element temperature 200 DEG C to variable concentrations NO
2respond, its result as shown in Figure 4, works as NO
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 as shown in Figure 5 fit equation is Langmuir equation at constant temperature
, wherein
for responsiveness, be defined as the ratio of resistance change and resistance initial value,
for NO
2concentration, parameter
,
.
Embodiment 8:
By the NO that embodiment 1 will make
2sensing element is the NO of 100 ppb to concentration temperature 200 DEG C
2response time, its result is as shown in Figure 6, when there being NO
2be adsorbed on material surface, its resistance reduces, and is roughly divided into 2 stages: response phase is 100 s-300 s fast; Saturation stage is 300 s-600 s, and release time is 100 s.
Embodiment 9:
By the NO made
2after sensing element is demarcated within specified temperatures, as NO
2the core component of alarm, connect power supply, ammeter and warning system, carry out NO in corresponding temperature
2real-Time Monitoring and warning.
Claims (4)
1. the preparation method based on the nitrogen dioxide sensor of titanium dioxide/graphene, it is characterized in that this sensor is by ceramic bases, electrode, titanium dioxide/graphene composite material, well heater and thermopair, signal processing and loudspeaker composition, at the upper fixed electorde (2) of ceramic bases (1), by titanium dioxide/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), by titanium dioxide/graphene composite material (3) water or ethanol furnishing slurry, adopt spraying, to smear or the method for electrochemical deposition is applied to silver, in the ceramic bases (1) of gold or copper electrode (2), naturally dry, concrete operations follow these steps to carry out:
The preparation of titanium dioxide/graphene composite material (3):
A, use conventional H ummer method are prepared graphene oxide dispersion, then the graphene oxide dispersion of preparation are concentrated into 10 μ g/mL-10 mg/mL;
B, get graphene oxide dispersion, add the TiCl that concentration is 1 mmol/L-1 mol/L
4or butyl titanate solution, stir, under room temperature-100 DEG C of conditions, react 1-168 h, obtain potpourri;
C, the potpourri that step b is obtained, Reusability water and ethanol carry out ultrasonic disperse and centrifuging respectively;
D, by the precipitation after being separated, dry under temperature 10-90 DEG C of condition, be N at protective atmosphere
2, under He, Ar inert gas, anneal under temperature 300-800 DEG C of condition 10 min-3 hour, obtains the titanium dioxide/graphene composite material that mass ratio is 1000:1-20:3;
The preparation of sensor:
E, at the upper fixed electorde (2) of ceramic bases (1), the method for making of electrode (2) is printing or ion sputtering film coating, by titanium dioxide/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), ceramic bases (1) is for plane, cylindric, the material of ceramic bases (1) is glass or stupalith, by titanium dioxide/graphene composite material (3) water that obtains or ethanol furnishing slurry, adopt spraying, to smear or the method for electrochemical deposition is applied to silver, in the ceramic bases (1) of gold or copper electrode (2), naturally dry.
2. the preparation method of the nitrogen dioxide sensor based on titanium dioxide/graphene according to claim 1, it is characterized in that in step a that graphene oxide dispersion concentrates concentration is 3.6 mg/mL.
3. the preparation method of the nitrogen dioxide sensor based on titanium dioxide/graphene according to claim 1, is characterized in that TiCl in step b
4or butyl titanate solution concentration is 0.1 mol/L, temperature of reaction 70 DEG C, time 48h.
4. the preparation method of the nitrogen dioxide sensor based on titanium dioxide/graphene according to claim 1, it is characterized in that in steps d, baking temperature is 50 DEG C, protective atmosphere is N
2, annealing temperature is 500 DEG C, and annealing time is 30 min, and the mass ratio of titania and Graphene is 20:1.
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| 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 |
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