CN104569052A - Method for preparing graphene oxide sensor - Google Patents
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- CN104569052A CN104569052A CN201410788111.3A CN201410788111A CN104569052A CN 104569052 A CN104569052 A CN 104569052A CN 201410788111 A CN201410788111 A CN 201410788111A CN 104569052 A CN104569052 A CN 104569052A
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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
Technical field
The present invention relates to a kind of method preparing graphene oxide sensor, particularly relate to a kind of method using metal nanometer line and graphene oxide composite material to prepare senser element.Belong to technical field prepared by sophisticated semiconductor material.
Background technology
After Graphene is found, it is found that its increasing excellent performance.Such as high strength, high conductivity, high sensing sensitivity etc.As the important derivatives of Graphene, graphene oxide also receives increasing attention.There is responsive response in the multiple gases such as current research shows, graphene oxide has excellent sensing characteristics, and it is to water vapor, ammonia, nitrogen dioxide, sulfuretted hydrogen.This is wherein especially with the sensitiveest to the response of water vapor, its remolding sensitivity tradition water vapor sensing (or humidity sensor) high two orders of magnitude.The high sensitivity characteristic of graphene oxide to water vapor derives from the abundant oxy radical in its surface.The stronger interaction of these oxy radicals and hydrone is the basis of graphene oxide high-performance humidity sensor.In addition, the Old plant to other gases is also likely produced through the graphene oxide composite material of modification.Very high detectability is had to nitrogen dioxide such as through the graphene oxide after suitably reducing.
Although graphene oxide has excellent sensing capabilities, it is comparatively large that the senser element of the traditional double electrode structure using graphene oxide composite material to build has electric leakage, and in low gas concentration situation, electric capacity is too little, and sensing is whirled the stagnant shortcoming such as large.These shortcomings limit manufacture based on the sensor of graphene oxide and application.Address these problems, need the structure of improvement device or build new device architecture.Such as, there is researcher to have studied the response characteristic of the senser element of top-bottom electrode structures and planar electrode structure, find that the former has good response characteristic.But the senser element of top-bottom electrode structures needs the upper electrode arrangement using complicated technique preparation ventilative.Also researcher is had to have studied the sensor of use nano wire as top electrode.Because nano wire top electrode has good ventilating performance, the performance of device therefore can be significantly improved.Comprehensively current research situation can find, several researchers have proposed more method to promote the sensing characteristics of sensor although have, and still has a lot of problem to need to solve further.Based on this research background, it is a kind of desirable for designing and preparing new device architecture, significantly improves the method for device performance.
Summary of the invention
For prior art Problems existing, the invention provides a kind of method preparing graphene oxide sensor, graphene oxide and metal nanometer line is used to be raw material, both are mixed to form the double-decker of graphene oxide coated metal nano wire, and prepare graphene sensor, improve the sensitivity characteristic of device, and be conducive to fast device response and reduce whirling of device stagnant.
Technical scheme of the present invention is: a kind of method preparing graphene oxide sensor, and concrete steps are as follows:
(1) graphene oxide is scattered in solvent, forms stable graphene oxide dispersion;
(2) surface-functionalized process is carried out to metal nano wire material, to make in the graphene oxide dispersion being scattered in described in step (1) of metal nanometer line Absorbable organic halogens and affine with graphene oxide;
(3) get the metal nanometer line after surface-functionalized process in step (2), join in the graphene oxide dispersion described in step (1), mix, form graphene oxide and metal nanometer line mixed liquor;
(4) by the mixed liquor in step (3) at 30 DEG C-200 DEG C after stirring reaction 1-300 minute, form the mixed liquor with graphene oxide coated metal nano thread structure, described mixed liquor can prepare nonconductor film, does not also namely form continuous current path between described metal nanometer line;
(5) using the mixed liquor with graphene oxide coated metal nano thread structure described in step (4) as the sensitive material of sensor, prepare graphene oxide sensor.
Further, after prepared by the graphene oxide sensor described in step (5), adopt post growth annealing process, 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 the adhesive capacity between the adhesive capacity of substrate and nano wire.
Further, described in step (5), graphene oxide sensor comprises: the dielectric substrate of bottom, be covered in the electrode of insulated substrate surface, be covered in the insulation course of electrode surface, with the sensitive material being covered in surface of insulating layer, that is: with the mixed liquor of graphene oxide coated metal nano thread structure.
Further, described in be enclosed with the graphene oxide of metal nanometer line, use spraying process, spin-coating method or LB embrane method, be covered in surface of insulating layer.
Further, if described insulating substrate material insulating material, then directly use; If not insulating material, then coated electrode again after dielectric isolation layer is prepared on its surface.
Further, the material of described insulation course is monox, silicon nitride, barium titanate or barium strontium titanate.
Further, described in step (1), the lamella number of plies of graphene oxide is 1-20 layer, and lamella size is less than 50 microns; Metal nano linear diameter is less than 1 micron, and nanowire length is less than 50 microns.
Further, solvent described in step (1) is the one or more kinds of combinations in water, ethanol, benzene, toluene, cyclohexane, dimethyl sulfoxide (DMSO), cyclopentanone, cyclohexanone, chloroform.
Further, the structure of graphene oxide coated metal nano wire described in step (4), comprise: in the middle of graphene oxide parcel nano wire, graphene oxide parcel nano wire head and centre, and the overall coated metal nano wire of stannic oxide/graphene nano line.
Further, described in step (5), electrode is plane interdigital structure.
Beneficial effect: use the present invention to have the preparation of applicable large area, technique is simple, and cost is lower, is applicable to the advantages such as multiple material.
1., when the metal nanometer line that two are coated with graphene oxide contacts with each other, the interface of contact is the sandwich construction of metal-oxide Graphene-metal.Wherein sensitive material is still graphene oxide.Plane electrode type sensor due to routine generally adopts the form of interdigital electrode, and the Electric Field Distribution between interdigital electrode can affect the sensitivity of device.In fact the most of electric field in interdigitated electrode structure is not all through sensitive material, and the responsive type causing this structure reduces.And after adding metal nanometer line in sensitive material, the Electric Field Distribution between interdigital electrode can produce change.Nano wire can make electric field line more trend towards being distributed in sensitive material inside.Therefore this structure is conducive to the sensitivity characteristic improving device.
2. because sensitizing range is present in the place of two Nanowire contacts, the spacing of metal nanometer line conductor is little, and when nano wire has more contact point, the electric capacity of entirety is comparatively large, 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 fast device response and reduces whirling of device stagnant.
4. metal nanometer line film layer structure is ventilating structure, and this structure is conducive to the diffusion of gas, is conducive to the performance improving device.
5. use this method to carry out large area preparation, technique is relatively simple.
Accompanying drawing explanation
Fig. 1: use graphene oxide and metal nanometer line to prepare a kind of schematic diagram of package structure.Wherein, 1: metal nanometer line; 2: graphene oxide sheet; 3: the metal nanometer line wrapping graphene oxide.Being wrapped structure and may having multiple situation, such as I of metal nanometer line: in the middle of graphene oxide parcel nano wire; II graphene oxide parcel nano wire head and centre; The overall coated metal nano wire of II I stannic oxide/graphene nano line.
Fig. 2: a kind of typical device architecture figure.Wherein, 4: the sensitive layer that the metal nanometer line wrapping graphene oxide is formed at device surface; 5: insulation course; 6: electrode; 7: dielectric substrate.
Fig. 3: the sectional view of device A-A '.Wherein, 4: the sensitive layer that the metal nanometer line wrapping graphene oxide is formed at device surface; 5: insulation course; 6: electrode; 7: dielectric substrate.
Fig. 4: insulating substrate material is not insulating material, then the device architecture figure of coated electrode again after dielectric isolation layer is prepared on its surface.Wherein, 4: the sensitive layer that the metal nanometer line wrapping graphene oxide is formed at device surface; 5: insulation course; 6: electrode; 7: dielectric substrate; 8: dielectric isolation layer.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Prepare a method for graphene oxide sensor, concrete steps are as follows:
(1) be 10 layers by the 0.2mg lamella number of plies, the lamella graphene oxide that is of a size of 45 microns is scattered in the water of 10ml, forms stable graphene oxide dispersion; Wherein: water can replace with the one or more kinds of combinations in water, ethanol, benzene, toluene, cyclohexane, dimethyl sulfoxide (DMSO), cyclopentanone, cyclohexanone, chloroform, on this experimental result without impact.During actual preparation, the lamella number of plies of graphene oxide is at 1-20 layer, and lamella size is less than 50 microns.
(2) to diameter be 0.8 micron, length is that the nanowires of gold material of 45 microns carries out surface-functionalized process, disposal route is as follows: in nanowires of gold dispersion liquid, add mercaptoacetic acid, fully stir, to make in the graphene oxide dispersion being scattered in described in step (1) of dried nanowires of gold Absorbable organic halogens and affine with graphene oxide.Actual when selecting, metal nano linear diameter is less than 1 micron, and nanowire length is less than 50 microns.
Wherein: nanowires of gold can replace with nano silver wire, copper nano-wire, Pt nanowires, palladium nanometer wire or stannum nanowire, for nano silver wire, in nanowire dispersion body, add polyvinyl alcohol (PVA), 50 degrees centigrade fully stir.Other nano wires can similarly process.Often kind of nano wire needs to use different functionalized reagents, can select as required.
(3) metal nanometer line after surface-functionalized process in 0.5mg step (2) is got, join in the graphene oxide dispersion described in step (1), mix, form graphene oxide and metal nanometer line mixed liquor, described mixed liquor can prepare nonconductor film;
(4) stirring reaction at 30 DEG C of the mixed liquor in step (3), after 100 minutes, is formed the structure of graphene oxide coated metal 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 within 80 minutes, all can form the structure of graphene oxide coated metal nano wire.The structure of described graphene oxide coated metal nano wire, comprising: in the middle of graphene oxide parcel nano wire, graphene oxide parcel nano wire head and centre, and the overall coated metal nano wire of stannic oxide/graphene nano line; As shown in Figure 1.
(5) using the structure of the graphene oxide coated metal nano wire described in step (4) as the sensitive material of sensor, prepare graphene oxide sensor.Concrete, as shown in Figure 2,3, graphene oxide sensor comprises: the dielectric substrate 7 of bottom, is covered in the electrode 6 of the plane interdigital structure of insulated substrate surface, be covered in the insulation course 5 of electrode surface, and be covered in the graphene oxide 4 being enclosed with metal nanometer line of surface of insulating layer.Be enclosed with the graphene oxide of metal nanometer line, use spraying process, spin-coating method or LB embrane method, be covered in surface of insulating layer.
Wherein: if described insulating substrate material insulating material, then directly use; If not insulating material, then coated electrode (as shown in Figure 4) again after dielectric isolation layer 8 is prepared on its surface.
The material of described insulation course 5 is monox, silicon nitride, barium titanate or barium strontium titanate.
As preferred embodiment: after prepared by the graphene oxide sensor described in step (5), adopt post growth annealing process, described post growth annealing anneal 300 minutes, annealing 30 minutes or annealed for 10 seconds at 600 DEG C at 100 DEG C at 80 DEG C.The equal metal nanometer line that can increase is to the adhesive capacity between the adhesive capacity of substrate and nano wire.
When the metal nanometer line that two are coated with graphene oxide contacts with each other, the interface of contact is the sandwich construction of metal-oxide Graphene-metal.Wherein sensitive material is still graphene oxide.Plane electrode type sensor due to routine generally adopts the form of interdigital electrode, and the Electric Field Distribution between interdigital electrode can affect the sensitivity of device.In fact the most of electric field in interdigitated electrode structure is not all through sensitive material, and the responsive type causing this structure reduces.And after adding metal nanometer line in sensitive material, the Electric Field Distribution between interdigital electrode can produce change.Nano wire can make electric field line more trend towards being distributed in sensitive material inside.Therefore this structure is conducive to the sensitivity characteristic improving device.
Although the present invention with preferred embodiment disclose as above, so itself and be not used to limit the present invention.Persond having ordinary knowledge in the technical field of the present invention, without departing from the spirit and scope of the present invention, when being used for a variety of modifications and variations.Therefore, protection scope of the present invention is when being as the criterion depending on those as defined in claim.
Claims (10)
1. prepare a method for graphene oxide sensor, it is characterized in that: concrete steps are as follows:
(1) graphene oxide is scattered in solvent, forms stable graphene oxide dispersion;
(2) surface-functionalized process is carried out to metal nano wire material, to make in the graphene oxide dispersion being scattered in described in step (1) of metal nanometer line Absorbable organic halogens and affine with graphene oxide;
(3) get the metal nanometer line after surface-functionalized process in step (2), join in the graphene oxide dispersion described in step (1), mix, form graphene oxide and metal nanometer line mixed liquor;
(4) by the mixed liquor in step (3) at 30 DEG C-200 DEG C after stirring reaction 1-300 minute, form the mixed liquor with graphene oxide coated metal nano thread structure, described mixed liquor can prepare nonconductor film, does not also namely form continuous current path between metal nanometer line;
(5) using the mixed liquor with graphene oxide coated metal nano thread structure described in step (4) as the sensitive material of sensor, prepare graphene oxide sensor.
2. a kind of method preparing graphene oxide sensor according to claim 1, it is characterized in that: after prepared by the graphene oxide sensor described in step (5), adopt post growth annealing process, described post growth annealing temperature is 100 DEG C-600 DEG C, and annealing time is 5 seconds-300 minutes.
3. a kind of method preparing graphene oxide sensor according to claim 1, it is characterized in that: described in step (5), graphene oxide sensor comprises: the dielectric substrate of bottom, be covered in the electrode of insulated substrate surface, be covered in the insulation course of electrode surface, with the sensitive material being covered in surface of insulating layer, that is: with the mixed liquor of graphene oxide coated metal nano thread structure.
4. a kind of method preparing graphene oxide sensor according to claim 3, is characterized in that: described in be enclosed with the graphene oxide of metal nanometer line, use spraying process, spin-coating method or LB embrane method, be covered in surface of insulating layer.
5. a kind of method preparing graphene oxide sensor according to claim 3, is characterized in that: if described insulating substrate material insulating material, then directly use; If not insulating material, then coated electrode again after dielectric isolation layer is prepared on its surface.
6. a kind of method preparing graphene oxide sensor according to claim 3, is characterized in that: the material of described insulation course is monox, silicon nitride, barium titanate or barium strontium titanate.
7. a kind of method preparing graphene oxide sensor according to claim 1, is characterized in that: described in step (1), the lamella number of plies of graphene oxide is 1-20 layer, and lamella size is less than 50 microns; Metal nano linear diameter is less than 1 micron, and nanowire length is less than 50 microns.
8. a kind of method preparing graphene oxide sensor according to claim 1, is characterized in that: solvent described in step (1) is the one or more kinds of combinations in water, ethanol, benzene, toluene, cyclohexane, dimethyl sulfoxide (DMSO), cyclopentanone, cyclohexanone, chloroform.
9. a kind of method preparing graphene oxide sensor according to claim 1, it is characterized in that: the structure of graphene oxide coated metal nano wire described in step (4), comprise: in the middle of graphene oxide parcel nano wire, graphene oxide parcel nano wire head and centre, and the overall coated metal nano wire of stannic oxide/graphene nano line.
10. a kind of method preparing graphene oxide sensor according to claim 1, is characterized in that: described in step (5), electrode is plane interdigital structure.
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