CN104569052B - Method for preparing graphene oxide sensor - Google Patents

Method for preparing graphene oxide sensor Download PDF

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CN104569052B
CN104569052B CN201410788111.3A CN201410788111A CN104569052B CN 104569052 B CN104569052 B CN 104569052B CN 201410788111 A CN201410788111 A CN 201410788111A CN 104569052 B CN104569052 B CN 104569052B
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graphene oxide
method preparing
oxide sensor
sensor according
mixed liquor
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CN104569052A (en
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万能
黄见秋
孙立涛
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Southeast University
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Southeast University
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Abstract

The invention provides a method for preparing a graphene oxide sensor. The method comprises the following specific steps: (1) dispersing graphene oxide in a solvent, and forming stable graphene oxide dispersion liquid; (2) performing surface functionalization treatment on a metal nanowire material; (3) adding the metal nanowire subjected to surface functionalization treatment in the step (2) into the graphene oxide dispersion liquid in the step (1), uniformly mixing so as to form a mixed solution of graphene oxide and metal nanowire; (4) carrying out stirring reaction on the mixed solution in the step (3) at the temperature of 30-200 DEG C for 1-300 minutes so as to form a graphene oxide coated metal nanowire structure, wherein a continuous current path is not formed between the metal nanowires; and (5) by taking the graphene oxide coated metal nanowire structure in the step (4) as a sensitive material of the sensor, preparing the graphene oxide sensor. The method contributes to improving the sensing characteristics of the device.

Description

A kind of method preparing graphene oxide sensor
Technical field
The present invention relates to a kind of method preparing graphene oxide sensor, more particularly, to a kind of using metal nanometer line and The method that graphene oxide composite material prepares senser element.Belong to the technical field of sophisticated semiconductor material preparation.
Background technology
It has been found that its more and more excellent performance after Graphene is found.Such as high intensity, height is led Electrically, high sensing sensitivity etc..As the important derivatives of Graphene, graphene oxide also receives and more and more weighs Depending on.Current research it has been shown that graphene oxide has excellent sensing characteristicses, its to vapor, ammonia, nitrogen dioxide, There is sensitive response in the multiple gases such as hydrogen sulfide.Among these especially with the sensitiveest to the response of vapor, its remolding sensitivity passes System vapor sensing (or humidity sensor) high two orders of magnitude.Graphene oxide derives to the high sensitivity characteristic of vapor The oxy radical that its surface is enriched.These oxy radicals and hydrone stronger interaction are that graphene oxide high-performance is wet The basis of degree sensor.In addition, being also possible to produce the high sensitivity to other gases through modified graphene oxide composite material Response.There is very high power of test such as through the graphene oxide after suitable reduction to nitrogen dioxide.
Although graphene oxide has excellent sensing capabilities, the traditional double being built using graphene oxide composite material is electric The senser element of pole structure has the shortcomings of electric leakage is larger, and in the case of low gas concentration, electric capacity is too little, sensing whirls stagnant big.These lack Point limits the manufacture of sensor and application based on graphene oxide.Solve these problems, need to improve the structure of device Or build new device architecture.Such as, researcher is had to have studied the senser element of top-bottom electrode structures and planar electrode structure Response characteristic, find that the former has preferable response characteristic.But the senser element of top-bottom electrode structures needs using complicated The ventilative upper electrode arrangement of technique preparation.Also researcher is had to have studied sensor nano wire being used as Top electrode.Due to Nano wire Top electrode has preferable ventilating performance, therefore can significantly improve the performance of device.Comprehensive current research situation It can be found that several researchers have proposed more method to lift the sensing characteristicses of sensor although having, but still have very Many problems need to solve further.Based on this research background, it is a kind of desirable for designing and preparing new device architecture, significantly carries The method of high device performance.
Content of the invention
The problem existing for prior art, the present invention provides a kind of method preparing graphene oxide sensor, uses Graphene oxide and metal nanometer line are raw material, and both are mixed to form the double-deck knot of graphene oxide coated metal nano wire Structure, and prepare graphene sensor, improve the sensitivity characteristic of device, and be conducive to fast device response and reduce device Whirl stagnant.
The technical scheme is that:A kind of method preparing graphene oxide sensor, comprises the following steps that:
(1) graphene oxide is scattered in solvent, forms stable graphene oxide dispersion;
(2) surface-functionalized process is carried out to metal nano wire material, make what metal nanometer line can be stable to be scattered in step (1) in the graphene oxide dispersion described in and affine with graphene oxide;
(3) take the metal nanometer line after surface-functionalized process in step (2), be added to the oxidation stone described in step (1) In black alkene dispersion liquid, mix homogeneously, form graphene oxide and metal nanometer line mixed liquor;
(4) by after the stirring reaction 1-300 minute at 30 DEG C -200 DEG C of the mixed liquor in step (3), formed with oxidation The mixed liquor of Graphene coated metal nano thread structure, described mixed liquor can prepare non-conductor thin film, namely described metal Do not form continuous current path between nano wire;
(5) using the mixed liquor with graphene oxide coated metal nano thread structure described in step (4) as sensor Sensitive material, prepare graphene oxide sensor.
Further, after the completion of the graphene oxide sensor preparation described in step (5), at post growth annealing Reason, described post growth annealing temperature is 100 DEG C -600 DEG C, and annealing time is 5 seconds -300 minutes.Increase metal nanometer line to substrate Adhesive capacity and nano wire between adhesive capacity.
Further, described in step (5), graphene oxide sensor includes:The dielectric substrate of bottom, is covered in insulation The electrode of substrate surface, is covered in the insulating barrier of electrode surface, and is covered in the sensitive material of surface of insulating layer, that is,:Band aerobic The mixed liquor of graphite alkene coated metal nano thread structure.
Further, the described graphene oxide being enclosed with metal nanometer line, using spraying process, spin-coating method or LB film Method, is covered in surface of insulating layer.
Further, if described insulating substrate material insulant, then directly use;If not insulant, then exist Its surface covers electrode after preparing dielectric isolation layer again.
Further, the material of described insulating barrier is silicon oxide, silicon nitride, Barium metatitanate. or barium strontium titanate.
Further, the lamella number of plies of graphene oxide described in step (1) is 1-20 layer, and it is micro- that lamella is smaller in size than 50 Rice;Metal nano linear diameter is less than 1 micron, and nanowire length is less than 50 microns.
Further, solvent described in step (1) be water, ethanol, benzene, toluene, hexamethylene, dimethyl sulfoxide, Ketocyclopentane, One of Ketohexamethylene, chloroform or two or more combinations.
Further, the structure of graphene oxide coated metal nano wire described in step (4), including:Graphene oxide In the middle of parcel nano wire, graphene oxide wraps up nano wire head and centre, and graphene oxide layer entirety coated metal is received Rice noodle.
Further, electrode described in step (5) is plane interdigital structure.
Beneficial effect:Using the present invention there is the preparation of suitable large area, process is simple, cost relatively low it is adaptable to multiple materials The advantages of material.
1., when two metal nanometer lines being coated with graphene oxide contact with each other, the interface of contact is metal-oxygen The sandwich of graphite alkene-metal.Wherein sensitive material remains as graphene oxide.Due to conventional plane electrode type sensing Device is typically in the form of interdigital electrode, and the Electric Field Distribution between interdigital electrode can affect the sensitivity of device.Actually pitch The most of electric field referring in electrode structure is all not passed through sensitive material, and the responsive type causing this structure reduces.And work as quick After adding metal nanometer line in sense material, the Electric Field Distribution between interdigital electrode can produce change.Nano wire can make electric field line more Plus trend towards being distributed in inside sensitive material.Therefore this structure is conducive to improving the sensitivity characteristic of device.
2. because sensitizing range is present in the place of two Nanowire contacts, the spacing of metal nanometer line conductor is little, when receiving Rice noodle has overall electric capacity during more contact point larger, can be convenient for measuring.
3. because sensitizing range is present in the place of two Nanowire contacts, its contact area is less, is conducive to quick device Part response and reduce device whirl stagnant.
4. metal nanometer line film layer structure is ventilating structure, and this structure is conducive to the diffusion of gas, is conducive to improving device The performance of part.
5. large area preparation can be carried out using this method, technique is relatively easy.
Brief description
Fig. 1:Prepare a kind of schematic diagram of package structure using graphene oxide and metal nanometer line.Wherein, 1:Metal is received Rice noodle;2:Graphene oxide sheet;3:Wrap the metal nanometer line of graphene oxide.The structure that is wrapped of metal nanometer line may There are multiple situation, such as I:In the middle of graphene oxide parcel nano wire;II graphene oxide parcel nano wire head and centre; III graphene oxide layer entirety coated metal nano wire.
Fig. 2:A kind of typical device junction composition.Wherein, 4:The metal nanometer line wrapping graphene oxide is in device table The sensitive layer that face is formed;5:Insulating barrier;6:Electrode;7:Dielectric substrate.
Fig. 3:The sectional view of device A-A '.Wherein, 4:The metal nanometer line wrapping graphene oxide is in device surface shape The sensitive layer becoming;5:Insulating barrier;6:Electrode;7:Dielectric substrate.
Fig. 4:Insulating substrate material is not insulant, then cover the device of electrode after dielectric isolation layer is prepared on its surface again Part structure chart.Wherein, 4:Wrap the sensitive layer that the metal nanometer line of graphene oxide is formed in device surface;5:Insulating barrier; 6:Electrode;7:Dielectric substrate;8:Dielectric isolation layer.
Specific embodiment
The present invention is further illustrated below in conjunction with the accompanying drawings.
A kind of method preparing graphene oxide sensor, comprises the following steps that:
(1) by the 0.2mg lamella number of plies be 10 layers, the graphene oxide of a size of 45 microns of lamella be scattered in the water of 10ml In, form stable graphene oxide dispersion;Wherein:Water could alternatively be water, ethanol, benzene, toluene, hexamethylene, dimethyl One of sulfoxide, Ketocyclopentane, Ketohexamethylene, chloroform or two or more combinations, no affect on this experimental result.Actual preparation When, in 1-20 layer, lamella is smaller in size than 50 microns to the lamella number of plies of graphene oxide.
(2) to a diameter of 0.8 micron, length be that 45 microns of nanowires of gold material carries out surface-functionalized process, process Method is as follows:Add TGA in nanowires of gold dispersion liquid, be sufficiently stirred for, so that dried nanowires of gold can be stablized Be scattered in the graphene oxide dispersion described in step (1) and affine with graphene oxide.When reality is selected, metal nano Linear diameter is less than 1 micron, and nanowire length is less than 50 microns.
Wherein:Nanowires of gold could alternatively be nano silver wire, copper nano-wire, Pt nanowires, palladium nanometer wire or sijna rice Line, for nano silver wire, adds polyvinyl alcohol, 50 degrees centigrade are sufficiently stirred in nanowire dispersion body.Other Nano wire can be with similar process.Every kind of nano wire needs, using different functionalized reagents, can select as needed.
(3) take the metal nanometer line after surface-functionalized process in 0.5mg step (2), be added to the oxygen described in step (1) In graphite alkene dispersion liquid, mix homogeneously, form graphene oxide and metal nanometer line mixed liquor, described mixed liquor can be prepared into To non-conductor thin film;
(4) by after the stirring reaction 100 minutes at 30 DEG C of the mixed liquor in step (3), form graphene oxide trapping gold Belong to the structure of nano wire;Wherein:Mixed liquor at 30 DEG C stirring reaction 300 minutes, at 200 DEG C stirring reaction 1 minute or At 100 DEG C, stirring reaction all can form the structure of graphene oxide coated metal nano wire for 80 minutes.Described graphene oxide The structure of coated metal nano wire, including:Graphene oxide parcel nano wire in the middle of, graphene oxide parcel nano wire head and Centre, and graphene oxide layer entirety coated metal nano wire;As shown in Figure 1.
(5) using the structure of the graphene oxide coated metal nano wire described in step (4) as sensor sensitive material, Prepare graphene oxide sensor.Specifically, as shown in Figure 2,3, graphene oxide sensor includes:The insulation lining of bottom Bottom 7, is covered in the electrode 6 of the plane interdigital structure of insulated substrate surface, is covered in the insulating barrier 5 of electrode surface, and is covered in The graphene oxide 4 being enclosed with metal nanometer line of surface of insulating layer.It is enclosed with the graphene oxide of metal nanometer line, using spray Coating, spin-coating method or LB embrane method, are covered in surface of insulating layer.
Wherein:If described insulating substrate material insulant, then directly use;If not insulant, then in its table Face covers electrode (as shown in Figure 4) again after preparing dielectric isolation layer 8.
The material of described insulating barrier 5 is silicon oxide, silicon nitride, Barium metatitanate. or barium strontium titanate.
As preferred embodiment:After the completion of graphene oxide sensor preparation described in step (5), after adopting Annealing process is processed, and described post growth annealing anneal at 80 DEG C 300 minutes, annealed 30 minutes or 600 at 100 DEG C Anneal 10 seconds at DEG C.Metal nanometer line all can be increased to the adhesion energy between the adhesive capacity of substrate and nano wire Power.
When two metal nanometer lines being coated with graphene oxide contact with each other, the interface of contact is metal-oxide The sandwich of Graphene-metal.Wherein sensitive material remains as graphene oxide.Due to conventional plane electrode type sensor Typically in the form of interdigital electrode, and the Electric Field Distribution between interdigital electrode can affect the sensitivity of device.Actually interdigital Most of electric field in electrode structure is all not passed through sensitive material, and the responsive type causing this structure reduces.And when sensitivity After adding metal nanometer line in material, the Electric Field Distribution between interdigital electrode can produce change.Nano wire can make electric field line more Trend towards being distributed in inside sensitive material.Therefore this structure is conducive to improving the sensitivity characteristic of device.
Although the present invention is disclosed above with preferred embodiment, so it is not limited to the present invention.The affiliated skill of the present invention Has usually intellectual, without departing from the spirit and scope of the present invention, when can be used for a variety of modifications and variations in art field.Cause This, protection scope of the present invention ought be defined depending on those as defined in claim.

Claims (10)

1. a kind of method preparing graphene oxide sensor it is characterised in that:Comprise the following steps that:
(1) graphene oxide is scattered in solvent, forms stable graphene oxide dispersion;
(2) surface-functionalized process is carried out to metal nano wire material, make what metal nanometer line can be stable to be scattered in step (1) institute In the graphene oxide dispersion stated and affine with graphene oxide;
(3) take the metal nanometer line after surface-functionalized process in step (2), be added to the graphene oxide described in step (1) In dispersion liquid, mix homogeneously, form graphene oxide and metal nanometer line mixed liquor;
(4) by after the stirring reaction 1-300 minute at 30 DEG C -200 DEG C of the mixed liquor in step (3), formed and carry graphite oxide The mixed liquor of alkene coated metal nano thread structure, described mixed liquor can prepare non-conductor thin film, namely metal nanometer line it Between do not form continuous current path;
(5) will be quick as sensor for the mixed liquor with graphene oxide coated metal nano thread structure described in step (4) Sense material, prepares graphene oxide sensor.
2. a kind of method preparing graphene oxide sensor according to claim 1 it is characterised in that:In step (5) After the completion of described graphene oxide sensor preparation, processed using post growth annealing, described post growth annealing temperature is 100 DEG C -600 DEG C, annealing time is 5 seconds -300 minutes.
3. a kind of method preparing graphene oxide sensor according to claim 1 it is characterised in that:In step (5) Described graphene oxide sensor includes:The dielectric substrate of bottom, is covered in the electrode of insulated substrate surface, is covered in electrode table The insulating barrier in face, and it is covered in the sensitive material of surface of insulating layer, that is,:With graphene oxide coated metal nano thread structure Mixed liquor.
4. a kind of method preparing graphene oxide sensor according to claim 3 it is characterised in that:Described it is enclosed with The graphene oxide of metal nanometer line, using spraying process, spin-coating method or LB embrane method, it is covered in surface of insulating layer.
5. a kind of method preparing graphene oxide sensor according to claim 3 it is characterised in that:Described insulation lining If bottom material insulant, then directly use;If not insulant, then cover again after dielectric isolation layer is prepared on its surface Electrode.
6. a kind of method preparing graphene oxide sensor according to claim 3 it is characterised in that:Described insulating barrier Material be silicon oxide, silicon nitride, Barium metatitanate. or barium strontium titanate.
7. a kind of method preparing graphene oxide sensor according to claim 1 it is characterised in that:In step (1) The lamella number of plies of described graphene oxide is 1-20 layer, and lamella is smaller in size than 50 microns;Metal nano linear diameter is less than 1 micron, Nanowire length is less than 50 microns.
8. a kind of method preparing graphene oxide sensor according to claim 1 it is characterised in that:In step (1) Described solvent is one of water, ethanol, benzene, toluene, hexamethylene, dimethyl sulfoxide, Ketocyclopentane, Ketohexamethylene, chloroform or two Plant above combination.
9. a kind of method preparing graphene oxide sensor according to claim 1 it is characterised in that:In step (4) The structure of described graphene oxide coated metal nano wire, including:In the middle of graphene oxide parcel nano wire, graphene oxide bag Wrap up in nano wire head and centre, and graphene oxide layer entirety coated metal nano wire.
10. a kind of method preparing graphene oxide sensor according to claim 3 it is characterised in that:In step (5) Described electrode is plane interdigital structure.
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