CN102636522A - Graphene/ stannic oxide nanometer compounding resistance type film gas sensor and manufacturing method thereof - Google Patents

Graphene/ stannic oxide nanometer compounding resistance type film gas sensor and manufacturing method thereof Download PDF

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CN102636522A
CN102636522A CN2012100874321A CN201210087432A CN102636522A CN 102636522 A CN102636522 A CN 102636522A CN 2012100874321 A CN2012100874321 A CN 2012100874321A CN 201210087432 A CN201210087432 A CN 201210087432A CN 102636522 A CN102636522 A CN 102636522A
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graphene
stannic oxide
oxide nanometer
gas sensor
gold electrode
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李扬
杨慕杰
林乾乾
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a graphene/ stannic oxide nanometer compounding resistance type film gas sensor, which takes ceramics as a basal body. The surface of the ceramic basal body is photo-etched and evaporated with multiple pairs of interdigital gold electrodes, and is coated with gas-sensitive films of graphene and stannic oxide nanometer composite, and the manufactured resistance type film gas sensor has the advantages of simple manufacturing process and low cost. The gas-sensitive film is composed of a grapheme namosheet layer in a three-dimensional nano-structure and stannic oxide crystal particle composite with an orientated growth characteristic, the introduction of the graphene can favorably reduce the resistance of sensor elements, and the formation of the three-dimensional nano-structure can obviously enhance the specific surface area of the composite, thus the absorption and the diffusion of the gas can be promoted so as to greatly enhance the room temperature gas sensitive response sensitivity of elements. The graphene/stannic oxide nanometer compounding resistance type film gas sensor has the characteristics of high response sensitivity to low concentration ammonia, fast response, favorable recovering performanc, capability of carrying out the detection at the room temperature, and the like, which can be widely applied in the agricultural and industrial production process, and the room temperature detection and control of the concentration of ammonia in the atmospheric environment.

Description

Graphene/stannic oxide nanometer composite resistance film gas sensor and preparation method thereof
Technical field
The present invention relates to a kind of nano combined resistance type thin film gas sensor and preparation method thereof, especially Graphene/stannic oxide nanometer composite resistance film gas sensor and preparation method thereof with room temperature air-sensitive response characteristic.
Background technology
The progress of society provides wide space with the research that develops into sensor and the application of technology.Gas sensor is one type of important chemical sensor, has a wide range of applications in commercial production, process control, environmental monitoring and fields such as protection and anti-terrorism, and plays a part to become more and more important in development in science and technology and the people life in modern times.The high performance gas sensor that development has advantages such as high sensitivity, low cost, miniaturization, low-power consumption has received domestic and international extensive concern, and will realize the optimization of sensor performance, and key is to develop has the gas sensitive of excellent response characteristic simultaneously.Current is that the inorganic semiconductor of representative is to use one of gas sensitive the most widely with tin ash, titania etc.; It is easy that it has preparation; Advantages such as the detected gas kind is many; But also come with some shortcomings simultaneously, not high enough like response sensitivity, response recovery and response time etc. are ideal etc. not enough.Particularly this type gas sensitive and gas sensor need heat usually and under higher temperature, just can have air-sensitive response.This makes that its energy consumption is higher, is difficult to prepare portable apparatus.High working temperature influences the stability of sensor simultaneously, and does not suit to use in the place that has explosion hazard gases, makes its application receive certain limitation.In order to address this problem; Reduce the working sensor temperature so that realize that room temperature detects, adopt usually with doping such as inorganic semiconductor gas sensitive and noble metals, with material nanoization; Perhaps with method such as itself and conducting polymer gas sensitive be compound; In the hope of improving the sensitive material specific surface area, promote gas absorption and sensitive membrane surface reaction dynamic process etc., thereby increase response sensitivity at room temperature.In recent years, nanostructured carbon material research is very active, develops into one dimension CNT and two-dimentional Graphene from the fullerene of zero dimension.They also come into one's own in the preparation of sensor and the research on the improvement in performance.There have been a lot of reports to utilize the nanometer size effect of CNT and great specific surface area to prepare high sensitivity, the gas sensor of fast-response.Research is also found Graphene with the inorganic semiconductor gas sensitive is compound can obviously improve its response sensitivity, and adds fast-response, even is expected to realize that the high sensitivity gas under the room temperature responds.This respect research has become one of important directions of sensor research at present, develops very fast.
Summary of the invention
The purpose of this invention is to provide a kind of Graphene/stannic oxide nanometer composite resistance film gas sensor that at room temperature has high sensitivity gas response characteristic and preparation method thereof.
Graphene of the present invention/stannic oxide nanometer composite resistance film gas sensor; Has ceramic matrix; Have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode; On interdigital gold electrode, be connected with lead-in wire, be coated with air-sensitive film at ceramic matrix and interdigital gold electrode surfaces, this air-sensitive film is the nano-complex of Graphene and tin ash.
The preparation method of Graphene/stannic oxide nanometer composite resistance film gas sensor may further comprise the steps:
(1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
(2) compound concentration is 0.01 mg/mL ~ 5 mg/mL graphite oxide aqueous solutions; Add two hydration stannous chloride and ureas then; The weight ratio of graphite oxide aqueous solution, two hydration stannous chloride and urea is 1:0.00225 ~ 0.1125:0.005 ~ 0.05, and stirring and supersonic oscillations make abundant mixing, make precursor solution; Precursor solution is added in the water heating kettle to descend to react 1 ~ 12 hour at 80 ~ 120 ℃, make Graphene/stannic oxide nanometer complex solution;
(3) Graphene/stannic oxide nanometer complex solution with step (2) preparation drips the interdigital gold electrode surfaces with ceramic bases that is coated in step (1); 80~140 ℃ of following thermal treatments 0.5~3 hour, make Graphene/stannic oxide nanometer composite resistance film gas sensor.
Advantage of the present invention is:
1) prepared graphene/tin ash compound has meticulous 3-D nano, structure; Big specific surface area; Make sensor at room temperature have very high response sensitivity; Response and good response reversibility have solved the tin ash gas sensor and need heat the problem that at high temperature could work usually fast.
2) adopt one step of hydro-thermal method synthesizing graphite alkene/tin ash compound, method is simple to operate, and is with low cost, simple.And can be through the control hydro-thermal time, parameters such as the composition of hydrothermal temperature and precursor solution realize the regulation and control of composition, structure and the pattern etc. of compound easily.
3) introducing of graphene oxide in the nano-complex presoma; For the growth of tin dioxide nanocrystal grain provides good template, can obtain small-sized tin dioxide nano-particle thus, its can tight distribution on the graphene nano lamella of reduction; Also can assemble simultaneously and form petal shaped nano sheet filling Graphene lamella space; Formation has the 3-D nano, structure of very big specific surface area, can greatly promote gas absorption and diffusion, helps improving response sensitivity.In addition, the introducing of graphene oxide can also promote tin ash optionally along the growth of some high preferred orientations, and this also can promote catalytic reaction between itself and the detected gas, improves response sensitivity.
4) introducing of Graphene in the nano-complex can significantly improve the electric conductivity of composite gas sensor, avoids common tin ash gas sensor too high because of its room temperature resistance, and response sensitivity is extremely low and be difficult to the problem that realizes that room temperature detects.
5) adopt the presoma of stannous chloride as tin ash, do presoma than butter of tin etc. and prepare the bigger serface tin ash crystal with nano-scale more easily, and hydrothermal temperature is lower, the time is shorter.
6) adopt one step of hydro-thermal method in-situ preparing Graphene/stannic oxide nanometer compound, can significantly improve combining of Graphene and tin ash, improve the electric conductivity of gas sensor, help realizing the room temperature detection.The mixture solution of preparation can adopt to drip and method film forming on interdigital electrode such as is coated with, and processability is good, can prepare gas sensor easily, and having solved the tin ash gas sensor needs high temperature sintering usually, and processing is than complicated problems.
Description of drawings
Fig. 1 is the structural representation of gas sensor of the present invention;
Fig. 2 is the sem photograph of Graphene/stannic oxide nanometer compound;
Fig. 3 is the high resolving power transmission electron microscope picture of Graphene/stannic oxide nanometer compound;
Fig. 4 is the room temperature dynamic response curve of Graphene/stannic oxide nanometer composite gas sensor for ammonia;
Fig. 5 is Graphene/stannic oxide nanometer composite gas sensor for the room temperature response sensitivity of ammonia with the gas concentration change curve;
Fig. 6 is the repeated curve of Graphene/stannic oxide nanometer composite gas sensor for the response of 50 ppm ammonia room temperatures.
Embodiment
Further specify the present invention below in conjunction with accompanying drawing and embodiment.
With reference to Fig. 1; Graphene of the present invention/tin ash resistance type thin film gas sensor has ceramic matrix 1; Have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode 2; On interdigital gold electrode, be connected with lead-in wire 4, be coated with air-sensitive film 3 at ceramic matrix and interdigital gold electrode surfaces, this air-sensitive film is the nano-complex of Graphene and tin ash.
Embodiment 1:
(1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
(2) compound concentration is 0.01 mg/mL graphite oxide aqueous solution; Add two hydration stannous chloride and ureas then; The weight ratio of graphite oxide aqueous solution, two hydration stannous chloride and urea is 1:0.00225:0.01, and stirring and supersonic oscillations make abundant mixing, make precursor solution; Precursor solution is added in the water heating kettle to descend to react 2 hours at 80 ℃, make Graphene/stannic oxide nanometer complex solution;
(3) Graphene/stannic oxide nanometer complex solution with step (2) preparation drips the interdigital gold electrode surfaces with ceramic bases that is coated in step (1); 140 ℃ of following thermal treatments 0.5 hour, make Graphene/stannic oxide nanometer composite resistance film gas sensor.
Embodiment 2:
(1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
(2) compound concentration is 5 mg/mL graphite oxide aqueous solutions; Add two hydration stannous chloride and ureas then; The weight ratio of graphite oxide aqueous solution, two hydration stannous chloride and urea is 1:0.00225:0.005, and stirring and supersonic oscillations make abundant mixing, make precursor solution; Precursor solution is added in the water heating kettle to descend to react 12 hours at 100 ℃, make Graphene/stannic oxide nanometer complex solution;
(3) Graphene/stannic oxide nanometer complex solution with step (2) preparation drips the interdigital gold electrode surfaces with ceramic bases that is coated in step (1); 80 ℃ of following thermal treatments 3 hours, make Graphene/stannic oxide nanometer composite resistance film gas sensor.
Embodiment 3:
(1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
(2) compound concentration is 5 mg/mL graphite oxide aqueous solutions; Add two hydration stannous chloride and ureas then; The weight ratio of graphite oxide aqueous solution, two hydration stannous chloride and urea is 1:0.0225:0.025, and stirring and supersonic oscillations make abundant mixing, make precursor solution; Precursor solution is added in the water heating kettle to descend to react 12 hours at 120 ℃, make Graphene/stannic oxide nanometer complex solution;
(3) Graphene/stannic oxide nanometer complex solution with step (2) preparation drips the interdigital gold electrode surfaces with ceramic bases that is coated in step (1); 100 ℃ of following thermal treatments 2 hours, make Graphene/stannic oxide nanometer composite resistance film gas sensor.
Embodiment 4:
(1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
(2) compound concentration is 0. 1 mg/mL graphite oxide aqueous solutions; Add two hydration stannous chloride and ureas then; The weight ratio of graphite oxide aqueous solution, two hydration stannous chloride and urea is 1:0.1125:0.05, and stirring and supersonic oscillations make abundant mixing, make precursor solution; Precursor solution is added in the water heating kettle to descend to react 1 hour at 120 ℃, make Graphene/stannic oxide nanometer complex solution;
(3) Graphene/stannic oxide nanometer complex solution with step (2) preparation drips the interdigital gold electrode surfaces with ceramic bases that is coated in step (1); 100 ℃ of following thermal treatments 1 hour, make Graphene/stannic oxide nanometer composite resistance film gas sensor.
Embodiment 5:
(1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
(2) compound concentration is 0.01 mg/mL graphite oxide aqueous solution; Add two hydration stannous chloride and ureas then; The weight ratio of graphite oxide aqueous solution, two hydration stannous chloride and urea is 1:0.0225:0.02, and stirring and supersonic oscillations make abundant mixing, make precursor solution; Precursor solution is added in the water heating kettle to descend to react 8 hours at 120 ℃, make Graphene/stannic oxide nanometer complex solution;
(3) Graphene/stannic oxide nanometer complex solution with step (2) preparation drips the interdigital gold electrode surfaces with ceramic bases that is coated in step (1); 100 ℃ of following thermal treatments 2 hours, make Graphene/stannic oxide nanometer composite resistance film gas sensor.
The stereoscan photograph of the Graphene/stannic oxide nanometer compound of preparation is as shown in Figure 2; Can find out by Fig. 2; Be filled with between the graphene nano lamella in the compound and be arranged in petal-like stannic oxide nanometer lamella, it forms three-dimensional structure, and transmission electron microscope picture (Fig. 3) tightens the tin dioxide nano-particle of solid matter cloth for the nanometer sheet layer graphene; Can find out that the tin ash particle size is minimum, diameter is less than 5 nm.Graphene/stannic oxide nanometer compound that the electromicroscopic photograph explanation makes has meticulous 3-D nano, structure, and its specific surface area is very big, reaches 100 m through measuring 2/ g.
Graphene/stannic oxide nanometer composite resistance film the gas sensor of preparation is at room temperature seen Fig. 4 for the dynamic response curve of variable concentrations ammonia.Can find out that composite gas sensor all has quick response for the ammonia of variable concentrations, the response time is all less than 1 minute, and response has good reversibility.
Graphene/stannic oxide nanometer composite resistance film the gas sensor of preparation is at room temperature seen Fig. 5 for the response sensitivity curve of variable concentrations ammonia.Can find out that this sensor at room temperature has higher response sensitivity for low concentration ammonia, reach 16% for 50 ppm ammonias.
Graphene/stannic oxide nanometer composite resistance film the gas sensor of preparation is at room temperature seen Fig. 6 for the response repeatability curve of 50 ppm ammonias.Can find out and at room temperature pass through a plurality of loop tests of ammonia-nitrogen, its response curve shape is almost constant, shows that this sensor has good response repeatability.

Claims (2)

1. Graphene/stannic oxide nanometer composite resistance film gas sensor; It is characterized in that: it has ceramic matrix ⑴; Have many at ceramic matrix photomask surface and evaporation to interdigital gold electrode ⑵; On interdigital gold electrode, be connected with lead-in wire ⑷, be coated with air-sensitive film ⑶ at ceramic matrix and interdigital gold electrode surfaces, this air-sensitive film (3) is the nano-complex of Graphene and tin ash.
2. make the method for the described Graphene of claim 1/stannic oxide nanometer composite resistance film gas sensor, it is characterized in that may further comprise the steps:
(1) clean surface photoetching and evaporation have the ceramic substrate of interdigital gold electrode, dry for standby;
(2) compound concentration is 0.01 mg/mL ~ 5 mg/mL graphite oxide aqueous solutions; Add two hydration stannous chloride and ureas then; The weight ratio of graphite oxide aqueous solution, two hydration stannous chloride and urea is 1:0.00225 ~ 0.1125:0.005 ~ 0.05, and stirring and supersonic oscillations make abundant mixing, make precursor solution; Precursor solution is added in the water heating kettle to descend to react 1 ~ 12 hour at 80 ~ 120 ℃, make Graphene/stannic oxide nanometer complex solution;
(3) Graphene/stannic oxide nanometer complex solution with step (2) preparation drips the interdigital gold electrode surfaces with ceramic bases that is coated in step (1); 80~140 ℃ of following thermal treatments 0.5~3 hour, make Graphene/stannic oxide nanometer composite resistance film gas sensor.
CN2012100874321A 2012-03-29 2012-03-29 Graphene/ stannic oxide nanometer compounding resistance type film gas sensor and manufacturing method thereof Pending CN102636522A (en)

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Application publication date: 20120815