CN105976941A - Preparation process for flexible aluminum-doped zinc oxide/graphene composite material - Google Patents
Preparation process for flexible aluminum-doped zinc oxide/graphene composite material Download PDFInfo
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- CN105976941A CN105976941A CN201610414434.5A CN201610414434A CN105976941A CN 105976941 A CN105976941 A CN 105976941A CN 201610414434 A CN201610414434 A CN 201610414434A CN 105976941 A CN105976941 A CN 105976941A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
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Abstract
The invention discloses a preparation process for a flexible aluminum-doped zinc oxide/graphene composite material. The preparation process comprises the specific steps of (1) preparing a graphene precursor liquid; (2) washing a substrate, wherein the substrate can be conductive glass, a silicon wafer and a glass slide; (3) preparing a ZnO seed layer; (4) preparing a graphene oxide thin film by a czochralski method for two times, and performing the czochralski method for 15min in each time; (5) performing reduction; and (6) preparing the composite material. According to the preparation process, one layer of the graphene oxide thin film is prepared on the glass substrate by the czochralski method; then the thin film is subjected to reduction by a chemical reduction method; the flexible aluminum-doped zinc oxide/graphene composite material is prepared by a hydrothermal method; the process is simple and feasible; the expensive indium tin oxide thin film is replaced; and the synthesized composite has relatively good appearance, high flexibility and quite high transmittance.
Description
Technical field
The present invention relates to Graphene metallic composite production field, particularly relate to a kind of flexible aluminium-doped zinc oxide
The preparation technology of/graphene composite material.
Background technology
Transparent conductive material is a kind of material possessing excellent electrical and optical performance, at solaode, liquid crystal
Display, touch screen and other field of photoelectric devices are widely used, main with electrically conducting transparent in these areas
Presented in thin film.The transparent conductive film commonly used at present is indium and tin oxide film, but indium resource is dilute
Few, membrane equipment is expensive, thin film cannot bending fold, therefore flexible electronics becomes main developing direction.
Summary of the invention
Present invention seek to address that the deficiencies in the prior art, and provide a kind of flexible aluminium-doped zinc oxide/Graphene multiple
The preparation technology of condensation material.
The present invention for achieving the above object, by the following technical solutions:
The preparation technology of a kind of flexible aluminium-doped zinc oxide/graphene composite material, concretely comprises the following steps:
(1) preparation of Graphene precursor liquid:
Graphite oxide is dissolved in ultra-pure water, is configured to the precursor liquid of 0.5-1.5mg/ml, stir 40min, super
90min is swung in acoustic shock, in triplicate, forms uniform suspension, is then centrifuged for 10min, and rotating speed is 9000r/min,
Repeat this process to produce to without precipitation, remove unstripped graphite oxide, then high frequency ultrasound concussion 90min,
To Graphene precursor liquid;
(2) substrate cleans:
With electro-conductive glass as substrate, first electro-conductive glass is cut into the square of 2 × 2cm, spirituous with dipping in
Surface cleaned by cotton swab, then puts it in glass container, adds acetone, and ultrasonic vibration washs 40min, it
After add ethanol, ultrasonic vibration washing 50min, in triplicate;Use H the most again2O2And H2SO4Mixing
Electro-conductive glass is soaked 30min by solution, washs 30min with distilled water ultrasonic vibration afterwards, is repeated 3 times;?
Rinse with distilled water and dehydrated alcohol afterwards, dry;
(3) preparation of ZnO kind layer:
Zinc acetate and the ethanolamine of equimolar amounts are dissolved in ethanol, are configured to the solution that concentration is 0.1mol/L,
Ultrasonic vibration 45min, stirs 90min, is sufficiently mixed;Pipette mixed solution with liquid-transfering gun and be spin-coated on conduction glass
On glass, rotary speed is 3000r/min, and spin-coating time is 25-30s, repeats spin coating 3 times, is allowed to distribution all
Even;Then electro-conductive glass is dried at 70 DEG C, puts in Muffle furnace after drying, 500 DEG C of calcinings
60-90min, heating rate is 5 DEG C/min;
(4) preparation of graphene oxide film:
The electro-conductive glass handled well is coated with diallyl dimethyl ammoniumchloride and the mixed solution of sodium chloride,
Glass is modified;Adding ammonia in the Graphene precursor liquid obtained, regulating its pH value is 10, ultrasonic
Concussion 90min;Electro-conductive glass is placed in Graphene precursor liquid, prepares graphene oxide film with czochralski method;
(5) reduction:
In the inner bag of water heating kettle, add hydrazine hydrate, put into the electro-conductive glass scribbling graphene film, seal, put
In baking oven, 80 DEG C of reduction 15h;
(6) preparation of composite:
In the acetic acid zinc solution that concentration is 10mmol/L, add aluminum nitrate, make the Al in solution3+: Zn2+'s
Mol ratio is 5-8:100, adds the hexamethylenetetramine with zinc acetate equimolar amounts afterwards, and stirring is sufficiently mixed,
It is 10 with the pH of ammonia regulation solution;Electro-conductive glass and solution are together put in water heating kettle, 90 DEG C of insulations
10h;Naturally cool to room temperature after having reacted, with distilled water and dehydrated alcohol cyclic washing, be vacuum dried,
Obtain flexible aluminium-doped zinc oxide/graphene composite material.
Described substrate can be silicon chip.
Described substrate can be microscope slide.
During described czochralski method prepares graphene oxide film, lifting twice altogether, lift 15min every time.
The inner bag of described water heating kettle is the material of politef.
The invention has the beneficial effects as follows: the present invention utilizes czochralski method to be prepared for one layer of graphite oxide on a glass substrate
Alkene thin film, reduces to it with chemical reduction method, and utilizes hydro-thermal method to be prepared for flexible aluminium-doped zinc oxide/stone
Ink alkene composite, this technique simple possible, instead of the indium and tin oxide film of costliness, the composite wood of synthesis
Material possesses preferable pattern and flexibility, and has the highest transmitance.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:
The preparation technology of a kind of flexible aluminium-doped zinc oxide/graphene composite material, concretely comprises the following steps:
(1) preparation of Graphene precursor liquid:
Graphite oxide is dissolved in ultra-pure water, is configured to the precursor liquid of 0.5mg/ml, stir 40min, ultrasonic
Concussion 90min, in triplicate, forms uniform suspension, is then centrifuged for 10min, and rotating speed is 9000r/min,
Repeat this process to produce to without precipitation, remove unstripped graphite oxide, then high frequency ultrasound concussion 90min,
To Graphene precursor liquid;
(2) substrate cleans:
With electro-conductive glass as substrate, first electro-conductive glass is cut into the square of 2 × 2cm, spirituous with dipping in
Surface cleaned by cotton swab, then puts it in glass container, adds acetone, and ultrasonic vibration washs 40min, it
After add ethanol, ultrasonic vibration washing 50min, in triplicate;Use H the most again2O2And H2SO4Mixing
Electro-conductive glass is soaked 30min by solution, washs 30min with distilled water ultrasonic vibration afterwards, is repeated 3 times;?
Rinse with distilled water and dehydrated alcohol afterwards, dry;
(3) preparation of ZnO kind layer:
Zinc acetate and the ethanolamine of equimolar amounts are dissolved in ethanol, are configured to the solution that concentration is 0.1mol/L,
Ultrasonic vibration 45min, stirs 90min, is sufficiently mixed;Pipette mixed solution with liquid-transfering gun and be spin-coated on conduction glass
On glass, rotary speed is 3000r/min, and spin-coating time is 25s, repeats spin coating 3 times, is allowed to be evenly distributed;
Then electro-conductive glass is dried at 70 DEG C, puts in Muffle furnace after drying, 500 DEG C of calcining 60min,
Heating rate is 5 DEG C/min;
(4) preparation of graphene oxide film:
The electro-conductive glass handled well is coated with diallyl dimethyl ammoniumchloride and the mixed solution of sodium chloride,
Glass is modified;Adding ammonia in the Graphene precursor liquid obtained, regulating its pH value is 10, ultrasonic
Concussion 90min;Electro-conductive glass is placed in Graphene precursor liquid, prepares graphene oxide film with czochralski method;
(5) reduction:
In the inner bag of water heating kettle, add hydrazine hydrate, put into the electro-conductive glass scribbling graphene film, seal, put
In baking oven, 80 DEG C of reduction 15h;
(6) preparation of composite:
In the acetic acid zinc solution that concentration is 10mmol/L, add aluminum nitrate, make the Al in solution3+: Zn2+'s
Mol ratio is 5:100, adds the hexamethylenetetramine with zinc acetate equimolar amounts afterwards, and stirring is sufficiently mixed,
It is 10 with the pH of ammonia regulation solution;Electro-conductive glass and solution are together put in water heating kettle, 90 DEG C of insulations
10h;Naturally cool to room temperature after having reacted, with distilled water and dehydrated alcohol cyclic washing, be vacuum dried,
Obtain flexible aluminium-doped zinc oxide/graphene composite material.
During described czochralski method prepares graphene oxide film, lifting twice altogether, lift 15min every time.
The inner bag of described water heating kettle is the material of politef.
Embodiment 2:
The preparation technology of a kind of flexible aluminium-doped zinc oxide/graphene composite material, concretely comprises the following steps:
(1) preparation of Graphene precursor liquid:
Graphite oxide is dissolved in ultra-pure water, is configured to the precursor liquid of 1.5mg/ml, stir 40min, ultrasonic
Concussion 90min, in triplicate, forms uniform suspension, is then centrifuged for 10min, and rotating speed is 9000r/min,
Repeat this process to produce to without precipitation, remove unstripped graphite oxide, then high frequency ultrasound concussion 90min,
To Graphene precursor liquid;
(2) substrate cleans:
With silicon chip as substrate, first silicon chip is cut into the square of 2 × 2cm, clean with dipping in spirituous cotton swab
Surface, then puts it in glass container, adds acetone, ultrasonic vibration washing 40min, adds afterwards
Ethanol, ultrasonic vibration washing 50min, in triplicate;Use H the most again2O2And H2SO4Mixed solution is by silicon
Sheet soaks 30min, washs 30min with distilled water ultrasonic vibration afterwards, is repeated 3 times;Finally with distilled water and
Dehydrated alcohol rinses, and dries;
(3) preparation of ZnO kind layer:
Zinc acetate and the ethanolamine of equimolar amounts are dissolved in ethanol, are configured to the solution that concentration is 0.1mol/L,
Ultrasonic vibration 45min, stirs 90min, is sufficiently mixed;Pipette mixed solution with liquid-transfering gun to be spin-coated on silicon chip,
Rotary speed is 3000r/min, and spin-coating time is 30s, repeats spin coating 3 times, is allowed to be evenly distributed;Then will
Silicon chip is dried at 70 DEG C, puts in Muffle furnace after drying, and 500 DEG C of calcining 90min, heating rate is
5℃/min;
(4) preparation of graphene oxide film:
The silicon chip handled well is coated with diallyl dimethyl ammoniumchloride and the mixed solution of sodium chloride, to silicon
Sheet is modified;Adding ammonia in the Graphene precursor liquid obtained, regulating its pH value is 10, ultrasonic vibration
90min;Silicon chip is placed in Graphene precursor liquid, prepares graphene oxide film with czochralski method;
(5) reduction:
In the inner bag of water heating kettle, add hydrazine hydrate, put into the silicon chip scribbling graphene film, seal, be placed in baking
In case, 80 DEG C of reduction 15h;
(6) preparation of composite:
In the acetic acid zinc solution that concentration is 10mmol/L, add aluminum nitrate, make the Al in solution3+: Zn2+'s
Mol ratio is 8:100, adds the hexamethylenetetramine with zinc acetate equimolar amounts afterwards, and stirring is sufficiently mixed,
It is 10 with the pH of ammonia regulation solution;Silicon chip and solution are together put in water heating kettle, 90 DEG C of insulation 10h;
Naturally cool to room temperature after having reacted, with distilled water and dehydrated alcohol cyclic washing, vacuum drying, obtain soft
Property aluminium-doped zinc oxide/graphene composite material.
During described czochralski method prepares graphene oxide film, lifting twice altogether, lift 15min every time.
The inner bag of described water heating kettle is the material of politef.
Embodiment 3:
The preparation technology of a kind of flexible aluminium-doped zinc oxide/graphene composite material, concretely comprises the following steps:
(1) preparation of Graphene precursor liquid:
Graphite oxide is dissolved in ultra-pure water, is configured to the precursor liquid of 1mg/ml, stir 40min, ultrasonic shake
Swinging 90min, in triplicate, form uniform suspension, be then centrifuged for 10min, rotating speed is 9000r/min,
Repeat this process to produce to without precipitation, remove unstripped graphite oxide, then high frequency ultrasound concussion 90min,
To Graphene precursor liquid;
(2) substrate cleans:
With microscope slide as substrate, first microscope slide is cut into the square of 2 × 2cm, with dipping in spirituous cotton swab
Cleaning surface, then put it in glass container, add acetone, ultrasonic vibration washs 40min, the most again
Adding ethanol, ultrasonic vibration washs 50min, in triplicate;Use H the most again2O2And H2SO4Mixed solution
Microscope slide is soaked 30min, washs 30min with distilled water ultrasonic vibration afterwards, be repeated 3 times;Finally with steaming
Distilled water and dehydrated alcohol rinse, and dry;
(3) preparation of ZnO kind layer:
Zinc acetate and the ethanolamine of equimolar amounts are dissolved in ethanol, are configured to the solution that concentration is 0.1mol/L,
Ultrasonic vibration 45min, stirs 90min, is sufficiently mixed;Pipette mixed solution with liquid-transfering gun and be spin-coated on microscope slide
On, rotary speed is 3000r/min, and spin-coating time is 28s, repeats spin coating 3 times, is allowed to be evenly distributed;So
After microscope slide is dried at 70 DEG C, put in Muffle furnace after drying, 500 DEG C calcining 80min, heat up
Speed is 5 DEG C/min;
(4) preparation of graphene oxide film:
The microscope slide handled well is coated with diallyl dimethyl ammoniumchloride and the mixed solution of sodium chloride, right
Microscope slide is modified;Adding ammonia in the Graphene precursor liquid obtained, regulating its pH value is 10, ultrasonic
Concussion 90min;Microscope slide is placed in Graphene precursor liquid, prepares graphene oxide film with czochralski method;
(5) reduction:
In the inner bag of water heating kettle, add hydrazine hydrate, put into the microscope slide scribbling graphene film, seal, be placed in
In baking oven, 80 DEG C of reduction 15h;
(6) preparation of composite:
In the acetic acid zinc solution that concentration is 10mmol/L, add aluminum nitrate, make the Al in solution3+: Zn2+'s
Mol ratio is 6:100, adds the hexamethylenetetramine with zinc acetate equimolar amounts afterwards, and stirring is sufficiently mixed,
It is 10 with the pH of ammonia regulation solution;Microscope slide and solution are together put in water heating kettle, 90 DEG C of insulation 10h;
Naturally cool to room temperature after having reacted, with distilled water and dehydrated alcohol cyclic washing, vacuum drying, obtain soft
Property aluminium-doped zinc oxide/graphene composite material.
During described czochralski method prepares graphene oxide film, lifting twice altogether, lift 15min every time.
The inner bag of described water heating kettle is the material of politef.
Above the present invention is exemplarily described, it is clear that the present invention implements and do not limited by aforesaid way
System, as long as have employed method design and the various improvement that carry out of technical scheme of the present invention, or the most improved directly
It is applied to other occasion, all within protection scope of the present invention.
Claims (5)
1. the preparation technology of flexible aluminium-doped zinc oxide/graphene composite material, it is characterised in that concrete
Step is:
(1) preparation of Graphene precursor liquid:
Graphite oxide is dissolved in ultra-pure water, is configured to the precursor liquid of 0.5-1.5mg/ml, stir 40min, super
90min is swung in acoustic shock, in triplicate, forms uniform suspension, is then centrifuged for 10min, and rotating speed is 9000r/min,
Repeat this process to produce to without precipitation, remove unstripped graphite oxide, then high frequency ultrasound concussion 90min,
To Graphene precursor liquid;
(2) substrate cleans:
With electro-conductive glass as substrate, first electro-conductive glass is cut into the square of 2 × 2cm, spirituous with dipping in
Surface cleaned by cotton swab, then puts it in glass container, adds acetone, and ultrasonic vibration washs 40min, it
After add ethanol, ultrasonic vibration washing 50min, in triplicate;Use H the most again2O2And H2SO4Mixing
Electro-conductive glass is soaked 30min by solution, washs 30min with distilled water ultrasonic vibration afterwards, is repeated 3 times;?
Rinse with distilled water and dehydrated alcohol afterwards, dry;
(3) preparation of ZnO kind layer:
Zinc acetate and the ethanolamine of equimolar amounts are dissolved in ethanol, are configured to the solution that concentration is 0.1mol/L,
Ultrasonic vibration 45min, stirs 90min, is sufficiently mixed;Pipette mixed solution with liquid-transfering gun and be spin-coated on conduction glass
On glass, rotary speed is 3000r/min, and spin-coating time is 25-30s, repeats spin coating 3 times, is allowed to distribution all
Even;Then electro-conductive glass is dried at 70 DEG C, puts in Muffle furnace after drying, 500 DEG C of calcinings
60-90min, heating rate is 5 DEG C/min;
(4) preparation of graphene oxide film:
The electro-conductive glass handled well is coated with diallyl dimethyl ammoniumchloride and the mixed solution of sodium chloride,
Glass is modified;Adding ammonia in the Graphene precursor liquid obtained, regulating its pH value is 10, ultrasonic
Concussion 90min;Electro-conductive glass is placed in Graphene precursor liquid, prepares graphene oxide film with czochralski method;
(5) reduction:
In the inner bag of water heating kettle, add hydrazine hydrate, put into the electro-conductive glass scribbling graphene film, seal, put
In baking oven, 80 DEG C of reduction 15h;
(6) preparation of composite:
In the acetic acid zinc solution that concentration is 10mmol/L, add aluminum nitrate, make the Al in solution3+: Zn2+'s
Mol ratio is 5-8:100, adds the hexamethylenetetramine with zinc acetate equimolar amounts afterwards, and stirring is sufficiently mixed,
It is 10 with the pH of ammonia regulation solution;Electro-conductive glass and solution are together put in water heating kettle, 90 DEG C of insulations
10h;Naturally cool to room temperature after having reacted, with distilled water and dehydrated alcohol cyclic washing, be vacuum dried,
Obtain flexible aluminium-doped zinc oxide/graphene composite material.
The preparation work of a kind of flexible aluminium-doped zinc oxide/graphene composite material the most according to claim 1
Skill, it is characterised in that described substrate can be silicon chip.
The preparation work of a kind of flexible aluminium-doped zinc oxide/graphene composite material the most according to claim 1
Skill, it is characterised in that described substrate can be microscope slide.
The preparation work of a kind of flexible aluminium-doped zinc oxide/graphene composite material the most according to claim 1
Skill, it is characterised in that during described czochralski method prepares graphene oxide film, lifting twice altogether, every time
Lifting 15min.
The preparation work of a kind of flexible aluminium-doped zinc oxide/graphene composite material the most according to claim 4
Skill, it is characterised in that the inner bag of described water heating kettle is the material of politef.
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Cited By (1)
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CN106542744A (en) * | 2016-10-28 | 2017-03-29 | 燕山大学 | A kind of preparation method of special appearance ZnO film |
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CN104183299A (en) * | 2013-05-23 | 2014-12-03 | 海洋王照明科技股份有限公司 | Flexible conductive graphene film and manufacturing method and application thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106542744A (en) * | 2016-10-28 | 2017-03-29 | 燕山大学 | A kind of preparation method of special appearance ZnO film |
CN106542744B (en) * | 2016-10-28 | 2019-03-22 | 燕山大学 | A kind of preparation method of special appearance ZnO film |
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Application publication date: 20160928 |