CN105092646A - Graphene/metal oxide composite film gas sensor and preparation method - Google Patents

Graphene/metal oxide composite film gas sensor and preparation method Download PDF

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CN105092646A
CN105092646A CN201510509623.6A CN201510509623A CN105092646A CN 105092646 A CN105092646 A CN 105092646A CN 201510509623 A CN201510509623 A CN 201510509623A CN 105092646 A CN105092646 A CN 105092646A
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graphene
metal oxide
film
particle
oxide particle
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CN105092646B (en
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太惠玲
叶宗标
郑伟健
刘春华
杜晓松
谢光忠
蒋亚东
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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Abstract

The invention discloses a graphene/metal oxide composite film gas sensor and a preparation method, belongs to the technical field of gas sensors of micro-electrical mechanicals, and aims to provide a sensor. Metal oxide nano particles are used as catalysis media, so that the chemical potential barrier of a graphene thin film to electron transferring of gas molecules, and the gas sensitive characteristic of the single graphene thin film is enhanced. According to the preparation method, a layer of nano-level metal oxide particles is deposited on an interdigital electrode preferentially based on the excellent gas sensitive characteristic of the graphene material, and then the graphene thin film layer is deposited; by a heating technology, a graphene/metal oxide composite film with a gas sensitive enhanced effect is obtained. The graphene/metal oxide composite film gas sensor is suitable for gas sensors and realizes high-sensitivity and high-selectivity detection on different types of gas.

Description

A kind of graphene/metal oxide composite membrane gas sensor and preparation method thereof
Technical field
The invention belongs to gas sensor and composite nano materials technical field, relate to a kind of graphene/metal oxide composite membrane gas sensor, particularly relate to a kind of gas sensor with support and catalytic effect be made based on Graphene, metal oxide composite Nano sensitive material.
Background technology
Along with the raising of health of people consciousness, the problem of room air pollution receives increasing concern.In recent years, along with production and life style modernization more, increasing work, entertainment and sports are all carried out in indoor, and such people had 80% even more time to spend in indoor average every day.Therefore, the relation of IAQ (indoor air quality) and health just seems closer.
Contaminants of chemical origin is the main matter of indoor pollution, and it generally comprises formaldehyde, carbon monoxide, benzene homologues, ammonia, Radon and its descendants and suspended particle etc.And the concentration of this pollutant is often lower, this brings difficulty to detection.For the detection of contaminants of chemical origin, the detection method of present main flow has: several conventional detection methods such as vapor-phase chromatography, electrochemical process, infra-red sepectrometry, phenol reagent method.Although these detection methods can detect the dusty gas of trace level, in testing process, there is shortcomings such as needing sampling, instrumentation is complicated, analysis time is long, expensive, power consumption is larger.And gas sensor is as one analysis means fast and effectively, have advantages such as can measuring in real time, volume is little, response is fast, price is low, power consumption is few, utilization gas sensor is that the remote sensing monitoring system of core devices can be monitored in real time the air pollutants in environment, managed.Given this, urgently a kind of sensitivity of research and development is higher, selectivity is better, stability is better, response speed gas sensor faster.
The main cause of current restriction gas sensor development has: the sensitivity of gas sensor is compared with factors such as low, selectivity is poor, power consumption is large, complicated process of preparation, price height, and the structure of the sensitive material that all of these factors taken together all adopts with gas sensor and gas sensor is relevant.Can say, the structure of sensitive material and sensor is that the basis of new gas sensor and even new gas sensor technology is with crucial.
Graphene, as a kind of new material, has been subject to warmly pursuing of all trades and professions researchist.Its huge specific surface area, high conductivity, extremely low intrinsic noise and to give and accept the characteristics such as change is extremely responsive to electronics, make it obtain extensive concern in sensor field.But research shows: because single grapheme material has the more weak intrinsic absorption affinity of gas molecule and indiscriminate response characterization of adsorption, make it be subject to fatefulue restriction in sensitivity and selectivity two.Therefore, the widespread consensus of present industry grapheme material and other functional materials is carried out compound to improve the gas sensitization characteristic of single grapheme material.
The application for a patent for invention being 201410166226.9 as application number discloses a kind of graphene-based tri compound thin film gas sensor and preparation method thereof, it is made up of tri compound film and substrate, tri compound film is by Graphene, metal or metal oxide nanoparticles, conducting polymer is composited, this application takes full advantage of the high-specific surface area of Graphene and nano particle, excellent electricity and physicochemical characteristics, and the air-sensitive response characteristic that conducting polymer is special, tri compound makes to form gain complementary mechanisms between different materials, enhance gas sensitization characteristic and the stability of system, be combined with the self-assembly process that sequence is good simultaneously, can be used for preparing high-sensitive room temperature probe gas sensor.
But, because Graphene has thermal polycondensation effect, namely Graphene will produce thermal polycondensation in thermal histories, single graphene-based film do not support in thermal histories node support and produce contraction even occur film division, thus the sensitivity reduced gas, cause the sensitivity of gas sensor lower.
Summary of the invention
Goal of the invention of the present invention is: for prior art Problems existing, graphene/metal oxide composite membrane gas sensor providing a kind of sensitivity higher and preparation method thereof.
To achieve these goals, the technical solution used in the present invention is:
A kind of graphene/metal oxide composite membrane gas sensor, comprise Sensitive Apparatus, described Sensitive Apparatus is provided with nanosize metal oxide particle film, has hole between the metal oxide particle of described nanosize metal oxide particle film; Described nanosize metal oxide particle film is provided with oxidation graphene film, described oxidation graphene film is reductive amination graphene oxide film, hydroxylation oxidation graphene film, carboxylated oxidation graphene film, fluoridize in oxidation graphene film and thin base oxidation graphene film one or more; On the contact interface of oxidation graphene film and nanosize metal oxide particle film, the functional group of oxidation graphene film and the metal oxide particle bonding of nanosize metal oxide particle film.
As preferred version of the present invention, described Sensitive Apparatus is interdigital electrode, described interdigital electrode is gold electrode or aluminium electrode, the interdigital spacing of described interdigital electrode is 20 μm-50 μm, the interdigital width of described interdigital electrode is 20 μm-50 μm, and the thickness of electrode of described interdigital electrode is 20nm-500nm.
As preferred version of the present invention, the metal oxide nano particles of described nanosize metal oxide particle film comprise in nano granular of zinc oxide, Nano granules of stannic oxide, nano oxidized tungsten particle, nano titania particle, nano indium oxide particle, nano manganese oxide particle and nano nickel oxide particles one or more.
As preferred version of the present invention, the particle diameter of the metal oxide nano particles of described nanosize metal oxide particle film is less than 150nm.
A preparation method for graphene/metal oxide composite membrane gas sensor, comprises the following steps:
Step one, cleaning interdigital electrode;
Step 2, preparation graphene oxide solution, nanosize metal oxide particle dispersion, and described graphene oxide solution is graphene oxide is amination graphene oxide, hydroxylation graphene oxide, carboxylated graphene oxide, Fluorinated graphene oxide, dredge in base graphene oxide one or more;
Step 3, prepare nanosize metal oxide particle film, by nanosize metal oxide particle dispersion by spin coating, gas blowout or drip to be coated with in process deposits to interdigital electrode and form nanosize metal oxide particle film;
Step 4, prepare graphene oxide film, by graphene oxide solution by spin coating, gas blowout or drip and be coated with process deposits in interdigital electrode, and form graphene oxide film on nanosize metal oxide particle film;
Step 5, heat the interdigital electrode depositing nanosize metal oxide particle film and graphene oxide film under the atmosphere of nitrogen or argon gas, graphene oxide film is heated and is reduced into oxidation graphene film.
As preferred version of the present invention, in step one, during cleaning interdigital electrode, acetone, ethanol, deionized water is used to carry out ultrasonic cleaning 9min-12min to interdigital electrode successively.
As preferred version of the present invention, the concentration of the nanosize metal oxide particle dispersion in step 2 is 0.01%-5%, in described nanosize metal oxide particle dispersion, the particle diameter of nanosize metal oxide particle is less than 150nm, the boiling point of described nanosize metal oxide particle dispersion is 100 ° of C, and the density of described nanosize metal oxide particle dispersion is 0.1mg/ml-5mg/ml.
As preferred version of the present invention, in step 5, the interdigital electrode depositing nanosize metal oxide particle film and graphene oxide film is put into nitrogen atmosphere stove or argon gas atmosphere stove, the flow of nitrogen or argon gas is 100mL/min-500mL/min, be heat 1min-5h under the environment of 100 DEG C-1500 DEG C in heating-up temperature, graphene oxide film is heated and is reduced into oxidation graphene film.
In sum, owing to have employed technique scheme, the invention has the beneficial effects as follows:
In the present invention, Sensitive Apparatus deposits nanosize metal oxide particle film from the bottom up successively, oxidation graphene film, nanosize metal oxide particle film on Sensitive Apparatus is formed by gas blowout nanosize metal oxide particle dispersion deposition, thus between the metal oxide particle of nanosize metal oxide particle film, hole is had, being convenient to sensitive gas to be measured enters bottom oxidation graphene film by this space, increase the contact area of sensitive gas to be measured and Graphene, give full play to the feature of Graphene upper surface and the two-sided effect of lower surface, improve the sensitivity of gas sensor, due to nanosize metal oxide particle film being provided with oxidation graphene film, the granularity of the metal oxide particle on nanosize metal oxide particle film reaches nanoscale, thus nanosize metal oxide particle film surface by with the oxygen effect in air and form oxonium ion chemisorbed layer, and different and form the oxonium ion (O of different chemical activity according to the semiconductor ability of metal oxide -2, O -, O 2 -deng), and the concentration of the oxonium ion of different chemical activity can be changed by heating, these oxonium ions will reduce the chemical potential barrier of gas molecule electron transfer as catalysis medium, thus enhancing Graphene responds the sensitivity of sensitive gas to be measured, improves the sensitivity of gas sensor, in addition, oxidation graphene film is by amination graphene oxide, hydroxylation graphene oxide, carboxylated graphene oxide, one or more in Fluorinated graphene oxide and thin base graphene oxide form through heat reduction, thus oxidation graphene film has corresponding structure of functional groups, the Graphene grid promoted in oxidation graphene film and the nano level metal oxide particle on nanosize metal oxide particle film are produced bonding action by these structure of functional groups, thus promote the speed of electron transfer, strengthen and accelerate the response of gas sensor to sensitive gas to be measured, improve sensitivity and the detection efficiency of gas sensor, in addition, nanosize metal oxide particle film is also provided with below oxidation graphene film, due to the thermal polycondensation effect of Graphene, thus when heat reduction graphene oxide film, metal oxide particle in nanosize metal oxide particle film can be used as the strong point of Graphene grid in oxidation graphene film, avoids graphene film to shrink in thermal histories and film division even occurs and reduces the sensitivity of gas sensor to sensitive gas to be measured.
Accompanying drawing explanation
Fig. 1 is the structural representation of gas sensor of the present invention;
Fig. 2 is that Fig. 1 exists the partial enlarged drawing at place;
Fig. 3 is that laminated film and single Graphene gas respond schematic diagram;
Fig. 4 is rGO/TiO 2with the response test figure of single rGO to 0.1-0.5ppm formaldehyde;
Fig. 5 is rGO/TiO 2with single rGO to 0.5ppm formaldehyde repeatability response test figure;
Fig. 6 is rGO/TiO 2with the selective response side view of single rGO to 1ppm variety classes gas;
Fig. 7 is rGO/TiO 2, and TiO 2/ rGO(Graphene is in lower floor, and titania is on upper strata) laminated film and single rGO be to the response test figure of 0.5ppm and 1pmm formaldehyde;
Wherein, Reference numeral is: 1-Sensitive Apparatus, 2-nanosize metal oxide particle film, 3-oxidation graphene film, 21-hole.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
embodiment 1
A kind of graphene/metal oxide composite membrane gas sensor, this gas sensor comprises Sensitive Apparatus, and this Sensitive Apparatus is interdigital electrode.This interdigital electrode is gold electrode or aluminium electrode, and the interdigital spacing of this interdigital electrode is 20 μm-50 μm, and the interdigital width of interdigital electrode is 20 μm-50 μm, and the thickness of electrode of interdigital electrode is 20 μm-500 μm.In the present embodiment, interdigital electrode selects gold electrode, and the interdigital spacing of interdigital electrode is 25 μm, and the interdigital width of interdigital electrode is 26 μm, and the thickness of electrode of interdigital electrode is 50nm.
This Sensitive Apparatus is provided with nanosize metal oxide particle film, the metal oxide nano particles of nanosize metal oxide particle film comprises nano granular of zinc oxide, Nano granules of stannic oxide, nano oxidized tungsten particle, nano titania particle, nano indium oxide particle, one or more in nano manganese oxide particle and nano nickel oxide particles, wherein nano granular of zinc oxide is that the particle diameter of particle reaches nano level zinc paste, Nano granules of stannic oxide is that the particle diameter of particle reaches nano level tin oxide, nano oxidized tungsten particle is that the particle diameter of particle reaches nano level tungsten oxide, nano titania particle is that the particle diameter of particle reaches nano level titanium dioxide, nano indium oxide particle is that the particle diameter of particle reaches nano level indium oxide, nano manganese oxide particle is that the particle diameter of particle reaches nano level manganese oxide, nano nickel oxide particles is that the particle diameter of particle reaches nano level nickel oxide.The nanosize metal oxide particle dispersion that this nanosize metal oxide particle film is 0.01%-5% by concentration deposits and forms, thus between the metal oxide particle of nanosize metal oxide particle film, have hole, and in this nanosize metal oxide particle dispersion, the particle diameter of metal oxide particle is less than 150nm.In the present embodiment, the metal oxide nano particles of nanosize metal oxide particle film selects nano granular of zinc oxide, and in nanosize metal oxide particle dispersion, the particle diameter of metal oxide particle is 80nm.
This nanosize metal oxide particle film is provided with oxidation graphene film, and this oxidation graphene film is formed through heat reduction by the graphene oxide film be deposited on nanosize metal oxide particle film.This oxidation graphene film is reductive amination graphene oxide film, hydroxylation oxidation graphene film, carboxylated oxidation graphene film, fluoridize in oxidation graphene film and thin base oxidation graphene film one or more, wherein reductive amination graphene oxide film refers to the film also deposited through heat reduction by amination graphene oxide, hydroxylation oxidation graphene film refers to the film also deposited through heat reduction by hydroxylation graphene oxide, carboxylated oxidation graphene film refers to the film also deposited through heat reduction by carboxylated graphene oxide, fluoridize oxidation graphene film and refer to the film also deposited through heat reduction by Fluorinated graphene oxide, dredge base oxidation graphene film and refer to the film also deposited through heat reduction by thin base graphene oxide.In the present embodiment, oxidation graphene film selects reductive amination graphene oxide film, the film namely also deposited through heat reduction by amination graphene oxide.
Because oxidation graphene film is formed through heat reduction by the graphene oxide film be deposited on nanosize metal oxide particle film, thus in the process of graphene oxide film heat reduction, the functional group of oxidation graphene film and the coating metal oxide particle bonding of nanosize metal oxide particle film, thus promote the speed of electron transfer, strengthen and accelerate the response of gas sensor to sensitive gas to be measured, improving sensitivity and the detection efficiency of gas sensor.
embodiment 2
A kind of graphene/metal oxide composite membrane gas sensor, this gas sensor comprises Sensitive Apparatus, and this Sensitive Apparatus is interdigital electrode.This interdigital electrode is gold electrode or aluminium electrode, and the interdigital spacing of this interdigital electrode is 20 μm-50 μm, and the interdigital width of interdigital electrode is 20 μm-50 μm, and the thickness of electrode of interdigital electrode is 20 μm-500 μm.In the present embodiment, interdigital electrode aluminium electrode, the interdigital spacing of interdigital electrode is 35 μm, and the interdigital width of interdigital electrode is 36 μm, and the thickness of electrode of interdigital electrode is 210nm.
This Sensitive Apparatus is provided with nanosize metal oxide particle film, the metal oxide nano particles of nanosize metal oxide particle film comprises nano granular of zinc oxide, Nano granules of stannic oxide, nano oxidized tungsten particle, nano titania particle, nano indium oxide particle, one or more in nano manganese oxide particle and nano nickel oxide particles, wherein nano granular of zinc oxide is that the particle diameter of particle reaches nano level zinc paste, Nano granules of stannic oxide is that the particle diameter of particle reaches nano level tin oxide, nano oxidized tungsten particle is that the particle diameter of particle reaches nano level tungsten oxide, nano titania particle is that the particle diameter of particle reaches nano level titanium dioxide, nano indium oxide particle is that the particle diameter of particle reaches nano level indium oxide, nano manganese oxide particle is that the particle diameter of particle reaches nano level manganese oxide, nano nickel oxide particles is that the particle diameter of particle reaches nano level nickel oxide.The nanosize metal oxide particle dispersion that this nanosize metal oxide particle film is 0.01%-5% by concentration deposits and forms, thus between the metal oxide particle of nanosize metal oxide particle film, have hole, and in this nanosize metal oxide particle dispersion, the particle diameter of metal oxide particle is less than 150nm.In the present embodiment, the metal oxide nano particles of nanosize metal oxide particle film selects Nano granules of stannic oxide, and in nanosize metal oxide particle dispersion, the particle diameter of metal oxide particle is 100nm.
This nanosize metal oxide particle film is provided with oxidation graphene film, and this oxidation graphene film is formed through heat reduction by the graphene oxide film be deposited on nanosize metal oxide particle film.This oxidation graphene film is reductive amination graphene oxide film, hydroxylation oxidation graphene film, carboxylated oxidation graphene film, fluoridize in oxidation graphene film and thin base oxidation graphene film one or more, wherein reductive amination graphene oxide film refers to the film also deposited through heat reduction by amination graphene oxide, hydroxylation oxidation graphene film refers to the film also deposited through heat reduction by hydroxylation graphene oxide, carboxylated oxidation graphene film refers to the film also deposited through heat reduction by carboxylated graphene oxide, fluoridize oxidation graphene film and refer to the film also deposited through heat reduction by Fluorinated graphene oxide, dredge base oxidation graphene film and refer to the film also deposited through heat reduction by thin base graphene oxide.In the present embodiment, oxidation graphene film selects hydroxylation oxidation graphene film, the film namely also deposited through heat reduction by hydroxylation graphene oxide.
Because oxidation graphene film is formed through heat reduction by the graphene oxide film be deposited on nanosize metal oxide particle film, thus in the process of graphene oxide film heat reduction, the functional group of oxidation graphene film and the coating metal oxide particle bonding of nanosize metal oxide particle film, thus promote the speed of electron transfer, strengthen and accelerate the response of gas sensor to sensitive gas to be measured, improving sensitivity and the detection efficiency of gas sensor.
embodiment 3
A kind of graphene/metal oxide composite membrane gas sensor, this gas sensor comprises Sensitive Apparatus, and this Sensitive Apparatus is interdigital electrode.This interdigital electrode is gold electrode or aluminium electrode, and the interdigital spacing of this interdigital electrode is 20 μm-50 μm, and the interdigital width of interdigital electrode is 20 μm-50 μm, and the thickness of electrode of interdigital electrode is 20 μm-500 μm.In the present embodiment, interdigital electrode aluminium electrode, the interdigital spacing of interdigital electrode is 45 μm, and the interdigital width of interdigital electrode is 46 μm, and the thickness of electrode of interdigital electrode is 430nm.
This Sensitive Apparatus is provided with nanosize metal oxide particle film, the metal oxide nano particles of nanosize metal oxide particle film comprises nano granular of zinc oxide, Nano granules of stannic oxide, nano oxidized tungsten particle, nano titania particle, nano indium oxide particle, one or more in nano manganese oxide particle and nano nickel oxide particles, wherein nano granular of zinc oxide is that the particle diameter of particle reaches nano level zinc paste, Nano granules of stannic oxide is that the particle diameter of particle reaches nano level tin oxide, nano oxidized tungsten particle is that the particle diameter of particle reaches nano level tungsten oxide, nano titania particle is that the particle diameter of particle reaches nano level titanium dioxide, nano indium oxide particle is that the particle diameter of particle reaches nano level indium oxide, nano manganese oxide particle is that the particle diameter of particle reaches nano level manganese oxide, nano nickel oxide particles is that the particle diameter of particle reaches nano level nickel oxide.The nanosize metal oxide particle dispersion that this nanosize metal oxide particle film is 0.01%-5% by concentration deposits and forms, thus between the metal oxide particle of nanosize metal oxide particle film, have hole, and in this nanosize metal oxide particle dispersion, the particle diameter of metal oxide particle is less than 150nm.In the present embodiment, the metal oxide nano particles of nanosize metal oxide particle film selects nano indium oxide particle, nano manganese oxide particle, and in nanosize metal oxide particle dispersion, the particle diameter of metal oxide particle is 130nm.
This nanosize metal oxide particle film is provided with oxidation graphene film, and this oxidation graphene film is formed through heat reduction by the graphene oxide film be deposited on nanosize metal oxide particle film.This oxidation graphene film is reductive amination graphene oxide film, hydroxylation oxidation graphene film, carboxylated oxidation graphene film, fluoridize in oxidation graphene film and thin base oxidation graphene film one or more, wherein reductive amination graphene oxide film refers to the film also deposited through heat reduction by amination graphene oxide, hydroxylation oxidation graphene film refers to the film also deposited through heat reduction by hydroxylation graphene oxide, carboxylated oxidation graphene film refers to the film also deposited through heat reduction by carboxylated graphene oxide, fluoridize oxidation graphene film and refer to the film also deposited through heat reduction by Fluorinated graphene oxide, dredge base oxidation graphene film and refer to the film also deposited through heat reduction by thin base graphene oxide.In the present embodiment, oxidation graphene film is selected carboxylated oxidation graphene film, is fluoridized oxidation graphene film, namely by the potpourri of carboxylated graphene oxide and Fluorinated graphene oxide through heat reduction and the film of deposition.
Because oxidation graphene film is formed through heat reduction by the graphene oxide film be deposited on nanosize metal oxide particle film, thus in the process of graphene oxide film heat reduction, the functional group of oxidation graphene film and the coating metal oxide particle bonding of nanosize metal oxide particle film, thus promote the speed of electron transfer, strengthen and accelerate the response of gas sensor to sensitive gas to be measured, improving sensitivity and the detection efficiency of gas sensor.
embodiment 4
A preparation method for graphene/metal oxide composite membrane gas sensor, comprises the following steps:
Step one, cleaning interdigital electrode;
When cleaning interdigital electrode, acetone, ethanol, deionized water is used to carry out ultrasonic cleaning 10min to interdigital electrode successively.
Step 2, preparation graphene oxide solution, nanosize metal oxide particle dispersion;
During preparation graphene oxide solution, the powdered graphite of 2g is added in 250mL beaker, then under cooling bath condition, in beaker, add 1g sodium nitrate successively, the 46mL concentrated sulphuric acid also fully stirs, in beaker, add the potassium permanganate of 6g and 92mL water again and stir 15min, the concentration finally continuing to add 80mL in beaker is the hydrogen peroxide of 3%, and obtains graphene oxide solution through centrifugal filtration.Graphene oxide in this step is amination graphene oxide, hydroxylation graphene oxide, carboxylated graphene oxide, Fluorinated graphene oxide, dredge in base graphene oxide one or more, in the present embodiment, graphene oxide is amination graphene oxide.
When preparing nanosize metal oxide particle dispersion, conventional dispersion liquid preparation method can be adopted, but need the concentration of nanosize metal oxide particle dispersion to be 0.01%-5%, in described nanosize metal oxide particle dispersion, the particle diameter of nanosize metal oxide particle is less than 150nm, the boiling point of described nanosize metal oxide particle dispersion is 100 ° of C, and the density of described nanosize metal oxide particle dispersion is 0.1mg/ml-5mg/ml.Wherein, metal oxide particle in nanosize metal oxide particle dispersion is one or more in nano granular of zinc oxide, Nano granules of stannic oxide, nano oxidized tungsten particle, nano titania particle, nano indium oxide particle, nano manganese oxide particle and nano nickel oxide particles, and the metal oxide particle in the present embodiment in nanosize metal oxide particle dispersion is nano titania particle.
Step 3, prepare nanosize metal oxide particle film, by nanosize metal oxide particle dispersion by spin coating, gas blowout or drip to be coated with in process deposits to interdigital electrode and form nanosize metal oxide particle film.In the present embodiment, the nano size Titania particles dispersion liquid of 1mL is deposited on interdigital electrode on the surface by gas blowout method.
Step 4, prepare graphene oxide film, by graphene oxide solution liquid by spin coating, gas blowout or drip and be coated with process deposits in interdigital electrode, and form graphene oxide film on nanosize metal oxide particle film.In the present embodiment, the graphene oxide solution liquid of 1mL is deposited on interdigital electrode on the surface by gas blowout method.
Step 5, heat the interdigital electrode depositing nanosize metal oxide particle film and graphene oxide film under the atmosphere of nitrogen or argon gas, graphene oxide film is heated and is reduced into oxidation graphene film.The interdigital electrode being about to deposit nanosize metal oxide particle film and graphene oxide film puts into nitrogen atmosphere stove or argon gas atmosphere stove, the flow of nitrogen or argon gas is 200mL/min, be heat 2h under the environment of 220 DEG C in heating-up temperature, graphene oxide film is heated and is reduced into oxidation graphene film.
embodiment 5
A preparation method for graphene/metal oxide composite membrane gas sensor, comprises the following steps:
Step one, cleaning interdigital electrode;
When cleaning interdigital electrode, acetone, ethanol, deionized water is used to carry out ultrasonic cleaning 11min to interdigital electrode successively.
Step 2, preparation graphene oxide solution, nanosize metal oxide particle dispersion;
During preparation graphene oxide solution, the powdered graphite of 4g is added in 250mL beaker, then under cooling bath condition, in beaker, add 2g sodium nitrate successively, the 42mL concentrated sulphuric acid also fully stirs, in beaker, add the potassium permanganate of 7g and 96mL water again and stir 17min, the concentration finally continuing to add 65mL in beaker is the hydrogen peroxide of 3%, and obtains graphene oxide solution through centrifugal filtration.Graphene oxide in this step is amination graphene oxide, hydroxylation graphene oxide, carboxylated graphene oxide, Fluorinated graphene oxide, dredge in base graphene oxide one or more, in the present embodiment, graphene oxide is amination graphene oxide.
When preparing nanosize metal oxide particle dispersion, conventional dispersion liquid preparation method can be adopted, but need the concentration of nanosize metal oxide particle dispersion to be 0.01%-5%, in described nanosize metal oxide particle dispersion, the particle diameter of nanosize metal oxide particle is less than 150nm, the boiling point of described nanosize metal oxide particle dispersion is 100 ° of C, and the density of described nanosize metal oxide particle dispersion is 0.1mg/ml-5mg/ml.Wherein, metal oxide particle in nanosize metal oxide particle dispersion is one or more in nano granular of zinc oxide, Nano granules of stannic oxide, nano oxidized tungsten particle, nano titania particle, nano indium oxide particle, nano manganese oxide particle and nano nickel oxide particles, and the metal oxide particle in the present embodiment in nanosize metal oxide particle dispersion is nano indium oxide particle.
Step 3, prepare nanosize metal oxide particle film, by nanosize metal oxide particle dispersion by spin coating, gas blowout or drip to be coated with in process deposits to interdigital electrode and form nanosize metal oxide particle film.In the present embodiment, the nanoscale indium particle dispersion of 1mL is deposited on interdigital electrode on the surface by gas blowout method.
Step 4, prepare graphene oxide film, by graphene oxide solution liquid by spin coating, gas blowout or drip and be coated with process deposits in interdigital electrode, and form graphene oxide film on nanosize metal oxide particle film.In the present embodiment, the graphene oxide solution liquid of 1mL is deposited on interdigital electrode on the surface by gas blowout method.
Step 5, heat the interdigital electrode depositing nanosize metal oxide particle film and graphene oxide film under the atmosphere of nitrogen or argon gas, graphene oxide film is heated and is reduced into oxidation graphene film.The interdigital electrode being about to deposit nanosize metal oxide particle film and graphene oxide film puts into nitrogen atmosphere stove or argon gas atmosphere stove, the flow of nitrogen or argon gas is 390mL/min, be heat 4.2h under the environment of 800 DEG C in heating-up temperature, graphene oxide film is heated and is reduced into oxidation graphene film.
embodiment 6
Performance test is carried out to gas sensor prepared by the method for embodiment 4, compound sensor is inserted in air-sensitive test chamber, formaldehyde gas under 500ml/min total gas couette under room temperature detection variable concentrations, and carry out performance comparison with the single graphene film sensor that obtains under same sample preparation method.
By the method that the application provides, as shown in 3 figure, the Nano titanium dioxide particle film of bottom is not only the effect that Graphene provides catalysis medium, it is also effect that Graphene provides support, make formaldehyde molecule not only in graphenic surface effect, by entering oxidation graphene film basal surface between the titanium dioxide nano-particle of porous and carrying out electro transfer, the effect strengthening the response of oxidation graphene film PARA FORMALDEHYDE PRILLS(91,95) gas can also be reached.As shown in Figures 4 and 5, compare single graphene film gas sensor, graphene/metal oxide composite membrane gas sensor, respectively in 0.1-0.5ppm variable concentrations and the reperformance test of 0.5ppm formaldehyde, has larger response and response recovery time faster, has larger sensitivity.Can be obtained by Fig. 6, compare single graphene film gas sensor, graphene/metal oxide composite membrane gas sensor PARA FORMALDEHYDE PRILLS(91,95) has more excellent selective response.In order to verify that Nano titanium dioxide particle film is to Graphene supporting role, same preparation method is utilized to prepare TiO 2/ rGO(Graphene is in lower floor, and titania is on upper strata) laminated film sensor.As shown in Figure 7, TiO 2/ rGO compares single stone rGO certain response gain, and this is due to TiO 2catalysis humidification cause; But rGO/TiO 2under same test condition, have larger response than the former two, this responds because formaldehyde gas molecular energy enters bottom Graphene.Therefore the supporting role of titania is also proven.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (8)

1. a graphene/metal oxide composite membrane gas sensor, comprise Sensitive Apparatus (1), it is characterized in that: described Sensitive Apparatus (1) is provided with nanosize metal oxide particle film (2) having hole (21) between the metal oxide particle of described nanosize metal oxide particle film (2); Described nanosize metal oxide particle film (2) is provided with oxidation graphene film (3), described oxidation graphene film (3) is reductive amination graphene oxide film (3), hydroxylation oxidation graphene film (3), carboxylated oxidation graphene film (3), fluoridize in oxidation graphene film (3) and thin base oxidation graphene film (3) one or more; On the contact interface of oxidation graphene film (3) with nanosize metal oxide particle film (2), the functional group of oxidation graphene film (3) and the metal oxide particle bonding of nanosize metal oxide particle film (2).
2. a kind of graphene/metal oxide composite membrane gas sensor as claimed in claim 1, it is characterized in that: described Sensitive Apparatus (1) is interdigital electrode, described interdigital electrode is gold electrode or aluminium electrode, the interdigital spacing of described interdigital electrode is 20 μm-50 μm, the interdigital width of described interdigital electrode is 20 μm-50 μm, and the thickness of electrode of described interdigital electrode is 20nm-500nm.
3. a kind of graphene/metal oxide composite membrane gas sensor as claimed in claim 1, is characterized in that: the metal oxide nano particles of described nanosize metal oxide particle film (2) comprise in nano granular of zinc oxide, Nano granules of stannic oxide, nano oxidized tungsten particle, nano titania particle, nano indium oxide particle, nano manganese oxide particle and nano nickel oxide particles one or more.
4. a kind of graphene/metal oxide composite membrane gas sensor as claimed in claim 3, is characterized in that: the particle diameter of the metal oxide nano particles of described nanosize metal oxide particle film (2) is less than 150nm.
5. a preparation method for graphene/metal oxide composite membrane gas sensor, is characterized in that, comprises the following steps:
Step one, cleaning interdigital electrode;
Step 2, preparation graphene oxide solution, nanosize metal oxide particle dispersion, and described graphene oxide solution is graphene oxide is amination graphene oxide, hydroxylation graphene oxide, carboxylated graphene oxide, Fluorinated graphene oxide, dredge in base graphene oxide one or more;
Step 3, prepare nanosize metal oxide particle film (2), by nanosize metal oxide particle dispersion by spin coating, gas blowout or drip to be coated with in process deposits to interdigital electrode and form nanosize metal oxide particle film (2);
Step 4, prepare graphene oxide film, by graphene oxide solution by spin coating, gas blowout or drip and be coated with process deposits in interdigital electrode, and form graphene oxide film on nanosize metal oxide particle film (2);
Step 5, heat the interdigital electrode depositing nanosize metal oxide particle film (2) and graphene oxide film under the atmosphere of nitrogen or argon gas, graphene oxide film is heated and is reduced into oxidation graphene film (3).
6. the preparation method of a kind of graphene/metal oxide composite membrane gas sensor as claimed in claim 5, it is characterized in that, in step one, during cleaning interdigital electrode, acetone, ethanol, deionized water is used to carry out ultrasonic cleaning 9min-12min to interdigital electrode successively.
7. the preparation method of a kind of graphene/metal oxide composite membrane gas sensor as claimed in claim 5, it is characterized in that, the concentration of the nanosize metal oxide particle dispersion in step 2 is 0.01%-5%, in described nanosize metal oxide particle dispersion, the particle diameter of nanosize metal oxide particle is less than 150nm, the boiling point of described nanosize metal oxide particle dispersion is 100 ° of C, and the density of described nanosize metal oxide particle dispersion is 0.1mg/ml-5mg/ml.
8. the preparation method of a kind of graphene/metal oxide composite membrane gas sensor as claimed in claim 5, it is characterized in that, in step 5, the interdigital electrode depositing nanosize metal oxide particle film (2) and graphene oxide film is put into nitrogen atmosphere stove or argon gas atmosphere stove, the flow of nitrogen or argon gas is 100mL/min-500mL/min, be heat 1min-5h under the environment of 100 DEG C-1500 DEG C in heating-up temperature, graphene oxide film is heated and is reduced into oxidation graphene film (3).
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