CN105259218A - Zinc oxide nanowire-graphene gas sensor and preparation method thereof - Google Patents
Zinc oxide nanowire-graphene gas sensor and preparation method thereof Download PDFInfo
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- CN105259218A CN105259218A CN201510716975.9A CN201510716975A CN105259218A CN 105259218 A CN105259218 A CN 105259218A CN 201510716975 A CN201510716975 A CN 201510716975A CN 105259218 A CN105259218 A CN 105259218A
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Abstract
The invention discloses a zinc oxide nanowire-graphene gas sensor and a preparation method thereof, and belongs to the technical field of gas detection. The gas sensor consists of a substrate, an interdigital electrode and a gas sensitive coating, wherein the gas sensitive coating is made of a zinc oxide nanowire-graphene composite material. The preparation process of the sensor comprises the following steps: (1) preparing the zinc oxide nanowire-graphene nano-composite material; (2) machining and preparing the interdigital electrode on the substrate by a micromachining method and covering the surface of the interdigital electrode with a layer of nano-composite material serving as the gas sensitive coating to form a sensing device. The lower detection limit of the gas sensor to ammonia gas under room temperature reaches 50 ppb; meanwhile, the gas senor is shorter in response time, higher in repeat stability and higher in gas selectivity. The gas sensor is suitable for performing high-sensitivity detection on the ammonia gas under the room temperature.
Description
Technical field
The present invention relates to a kind of gas sensor and preparation method thereof, be specifically related to a kind of zinc oxide nanowire-Graphene gas sensor and preparation method thereof, belong to gas detection technology field.
Background technology
Develop novel sensor that is highly sensitive and quick response, healthy, military and national defense of environmental monitoring, people etc. is had great importance.Complete at ambient temperature, to the high-sensitivity detection of ammonia, then there is very high environment protection.Along with the development of nanometer technology, the gas sensor based on nano material obtains incremental advances.Wherein metal oxide semiconductor nano-material and Graphene etc. have all been used for building gas sensor separately.
Wherein, Graphene, due to the two-dimensional nanostructure of uniqueness, has the advantage not available for a lot of conventional material: one is have large specific surface area, can provide passage for gas, thus improves the sensitivity of gas response; Two is at room temperature have good electric conductivity, greatly reduces the working temperature of gas sensing, can realize the gas sensing under room temperature; Three is the sizes greatly reducing sensor.But, single Graphene still also exists a series of bottleneck as sensor, comprises the shortcomings such as the low and selectivity of sensitivity is bad, is therefore necessary Graphene and other Material cladding, realize the integrated of material and function, give play to the advantage of bi-material.Zinc oxide nanowire is a kind of important direct band-gap semicondictor material, has larger specific surface area and good electric conductivity, is the ideal material being used as to build high sensor.By zinc oxide nanowire and Graphene compound, prepare the gas sensor based on zinc oxide nanowire-Graphene, significant for the sensing capabilities improving material.Also there is no relevant report in this respect at present.
Summary of the invention
The present invention is directed to the deficiency in above-mentioned prior art, provide a kind of zinc oxide nanowire-Graphene gas sensor and preparation method thereof, the gas sensor performance obtained, relative to Graphene gas sensor and zinc oxide nanowire gas sensor, has increased significantly.
A first aspect of the present invention, discloses a kind of zinc oxide nanowire-Graphene gas sensor, comprises substrate, interdigital electrode and air-sensitive coating; Interdigital electrode is positioned on substrate, and air-sensitive coating covers the surface of interdigital electrode; Air-sensitive coating is zinc oxide nanowire-graphene composite material.
Preferably, substrate is the one in silicon base, polymeric substrates, ceramic bases or sapphire substrates.
Preferably, interdigital electrode is obtained by miromaching, and the positive and negative electrode spacing of interdigital electrode is 300 ~ 800 μm, and the spacing of adjacent two interdigital electrodes is 100 ~ 500 μm.
Preferably, the mass percent of air-sensitive coating composition is: the zinc oxide nanowire of 5 ~ 50%, the Graphene of 50 ~ 95%.
A second aspect of the present invention, discloses the preparation method of above-mentioned gas sensor, carries out according to following steps:
Step 1, is dissolved in first part of solvent by graphene oxide, ultrasonic 15min obtains first part of solution;
Step 2, is dissolved in second part of solvent jointly by zinc oxide nanowire and surfactant, and ultrasonic 15min obtains second part of solution;
Step 3, under stirring, mixes second part of solution with first part of solution, Keep agitation 2h, then centrifuge washing 3 times, is finally placed in vacuum drying oven 50 DEG C of dry 24h, obtains zinc oxide nanowire-graphene oxide composite material;
Step 4, anneals zinc oxide nanowire-graphene oxide composite material, obtains zinc oxide nanowire-graphene composite material;
Step 5, makes dispersion liquid by zinc oxide nanowire-graphene composite material, dispersant liquid drop is added to interdigital electrode surface, forms described air-sensitive coating, test gas sensing capabilities after drying.
Preferably, the first solvent and the second solvent refer to: the one or any multiple composition among deionized water, DMF, DMA, methyl alcohol, ethanol or acetone.
Preferably, surfactant is the one among polyvinylpyrrolidone, lauryl sodium sulfate, neopelex, cetyl trimethyl ammonium bromide, ammonium citrate.
Preferably, stir as magnetic agitation or mechanical raking, stirring rate is 10 ~ 500rpm.
Preferably, dispersion liquid refers to: be added in the 3rd part of solvent with the concentration of 1 ~ 10mg/L by zinc oxide nanowire-graphene composite material, with 50 ~ 100KHz ultrasound wave process, 10 ~ 20min, zinc oxide nanowire-graphene composite material is dispersed in the 3rd part of solvent, thus obtains dispersion liquid.
Preferably, the 3rd part of solvent refers to: the one or any multiple composition among deionized water, DMF, DMA, methyl alcohol, ethanol or acetone.
Be described further below with reference to the technique effect of accompanying drawing to design of the present invention, instantiation and generation, to understand the present invention fully.The object providing these to illustrate only is to help to explain the present invention, should not be used for limiting the scope of claim of the present invention.
Accompanying drawing explanation
Fig. 1 is gas sensor configuration schematic diagram prepared by a preferred embodiment of the present invention;
Fig. 2 is the stereoscan photograph of zinc oxide nanowire-graphene composite material prepared by a preferred embodiment of the present invention;
Fig. 3 is that pure Graphene is at room temperature to the response curve of 50ppm concentration ammonia;
Fig. 4 is that zinc oxide nanowire-graphene composite material of preparing of a preferred embodiment of the present invention is at room temperature to the response curve of 50ppm concentration ammonia;
Fig. 5 is that the gas sensor prepared of a preferred embodiment of the present invention is at room temperature to the response curve of variable concentrations ammonia.
Embodiment
Below in conjunction with accompanying drawing, enforcement of the present invention is described in detail.The present embodiment is implemented under premised on technical scheme of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Jointly be dissolved in the deionized water of 30ml by zinc oxide nanowire 0.1g and polyvinylpyrrolidone 0.1g, ultrasonic 15min obtains first part of solution.Be dissolved in the deionized water of 30ml by Graphene 0.3g, ultrasonic 15min obtains second part of solution.Stir 1h by after the mixing of two kinds of solution, be centrifugally placed on 50 DEG C of dry 24h in vacuum drying oven for 3 times, obtain zinc oxide nanowire-graphene oxide composite material.
Zinc oxide nanowire-the graphene oxide composite material obtained is carried out the annealing under argon shield, annealing temperature is 300 DEG C, and annealing time is 30min, obtains zinc oxide nanowire-graphene composite material.With the concentration of 1mg/L, the powder of compound substance is joined in deionized water, with 40KHz ultrasonic process 10min, make compound substance in deionized water dispersed, thus obtain the dispersion liquid of zinc oxide nanowire-graphene composite material.
Adopt miromaching to prepare gold electrode, the spacing controlling positive and negative electrode is 800 μm, and the spacing of adjacent electrode is 300 μm.The dispersant liquid drop getting the zinc oxide nanowire-graphene composite material of 1 μ L is added to electrode surface, 200 DEG C of vacuum drying 1h, thus obtains zinc oxide nanowire-Graphene gas sensor.
Fig. 1 is sensor construction schematic diagram of the present invention, describes the sensing principle of zinc oxide nanowire-graphene composite material, realizes the response to ammonia by resistance variations when detecting compound substance and ammonia effect.
Fig. 2 is the stereoscan photograph of zinc oxide nanowire-graphene composite material, can see that zinc oxide nanowire evenly and be closely compounded on Graphene.
Fig. 3 is the response curve of pure Graphene to 50ppm concentration ammonia.Fig. 4 is the response curve of zinc oxide nanowire-graphene composite material to 50ppm concentration ammonia.Can be found by Fig. 3 and Fig. 4 contrast, after compound, the response of sensor to ammonia obviously strengthens.
Fig. 5 be zinc oxide nanowire-Graphene gas sensor to the response curve of variable concentrations ammonia, along with the increase of ammonia concentration, the response of gas sensor increases gradually, and minimum response concentration can reach 50ppb.
Embodiment 2
The mass percentage of zinc oxide nanowire in zinc oxide nanowire-graphene composite material, as embodiment 1, is reduced to 10% by 25% by step, and the obtained response of gas sensor to 50ppm concentration ammonia is reduced to 6.2%.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (10)
1. zinc oxide nanowire-Graphene gas sensor, is characterized in that, described gas sensor comprises substrate, interdigital electrode and air-sensitive coating; Described interdigital electrode is positioned on described substrate, and described air-sensitive coating covers the surface of described interdigital electrode; Described air-sensitive coating is zinc oxide nanowire-graphene composite material.
2. a kind of zinc oxide nanowire-Graphene gas sensor according to claim 1, is characterized in that, described substrate is the one in silicon base, polymeric substrates, ceramic bases or sapphire substrates.
3. a kind of zinc oxide nanowire-Graphene gas sensor according to claim 1, it is characterized in that, described interdigital electrode is obtained by miromaching, the positive and negative electrode spacing of described interdigital electrode is 300 ~ 800 μm, and the spacing of adjacent two described interdigital electrodes is 100 ~ 500 μm.
4. a kind of zinc oxide nanowire-Graphene gas sensor according to claim 1, is characterized in that, the mass percent of described air-sensitive coating composition is: the described zinc oxide nanowire of 5 ~ 50%, the described Graphene of 50 ~ 95%.
5. the preparation method of a kind of zinc oxide nanowire-Graphene gas sensor according to any one of claim 1-4, it is characterized in that, described preparation method carries out according to following steps:
Step 1, is dissolved in first part of solvent by graphene oxide, ultrasonic 15min obtains first part of solution;
Step 2, is dissolved in second part of solvent jointly by zinc oxide nanowire and surfactant, and ultrasonic 15min obtains second part of solution;
Step 3, under stirring, mixes described second part of solution with described first part of solution, Keep agitation 2h, then centrifuge washing 3 times, is finally placed in vacuum drying oven 50 DEG C of dry 24h, obtains zinc oxide nanowire-graphene oxide composite material;
Step 4, anneals described zinc oxide nanowire-graphene oxide composite material, obtains zinc oxide nanowire-graphene composite material;
Step 5, makes dispersion liquid by described zinc oxide nanowire-graphene composite material, described dispersant liquid drop is added to described interdigital electrode surface, forms described air-sensitive coating, test gas sensing capabilities after drying.
6. the preparation method of a kind of zinc oxide nanowire-Graphene gas sensor according to claim 5, it is characterized in that, described first part of solvent and described second part of solvent refer to: deionized water, N, one or any multiple composition among dinethylformamide, DMA, methyl alcohol, ethanol or acetone.
7. the preparation method of a kind of zinc oxide nanowire-Graphene gas sensor according to claim 5, it is characterized in that, described surfactant is the one among polyvinylpyrrolidone, lauryl sodium sulfate, neopelex, cetyl trimethyl ammonium bromide, ammonium citrate.
8. the preparation method of a kind of zinc oxide nanowire-Graphene gas sensor according to claim 5, is characterized in that, described stirring is magnetic agitation or mechanical raking, and stirring rate is 10 ~ 500rpm.
9. the preparation method of a kind of zinc oxide nanowire-Graphene gas sensor according to claim 5, it is characterized in that, described dispersion liquid refers to: be added in the 3rd part of solvent with the concentration of 1 ~ 10mg/L by described zinc oxide nanowire-graphene composite material, with 50 ~ 100KHz ultrasound wave process, 10 ~ 20min, described zinc oxide nanowire-graphene composite material is dispersed in described 3rd part of solvent, thus obtains described dispersion liquid.
10. the preparation method of a kind of zinc oxide nanowire-Graphene gas sensor according to claim 9, it is characterized in that, described 3rd part of solvent refers to: deionized water, N, one or any multiple composition among dinethylformamide, DMA, methyl alcohol, ethanol or acetone.
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