CN106835082A - The preparation method of the flexible self-supporting graphene film of metal nanoparticle doping - Google Patents
The preparation method of the flexible self-supporting graphene film of metal nanoparticle doping Download PDFInfo
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- CN106835082A CN106835082A CN201710017316.5A CN201710017316A CN106835082A CN 106835082 A CN106835082 A CN 106835082A CN 201710017316 A CN201710017316 A CN 201710017316A CN 106835082 A CN106835082 A CN 106835082A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a kind of preparation method of the flexible self-supporting graphene film of metal nanoparticle doping.Graphene and metal salt solution are mixed first, and mixed solution is titrated into the drying and forming-film in solid substrate.The film that will be obtained heats reduction in being put into aqueous ascorbic acid, obtains internal metal nano particle-doped flexible self-supporting graphene film.Graphene oxide water solution is titrated in solid substrate first, and drying and forming-film.Further by metal salt solution titration in graphene oxide membrane, heating reduction in aqueous ascorbic acid is put into after drying, obtains the flexible self-supporting graphene film of surface doping metal nanoparticle.The method is prepared simply, and reactions steps are few, easy to operate, simple to equipment, technological requirement, and raw material is cheap, low cost, is capable of achieving the preparation of the graphene film of internal metal nano particle-doped graphene film and surface doping metal nanoparticle.
Description
Technical field
The invention belongs to graphene composite material preparing technical field, it is soft that more particularly to a kind of metal nanoparticle adulterates
The preparation method of property self-supporting graphene film.
Background technology
Graphene is the carbon simple substance material of a kind of two-dimensional layer, monoatomic thickness, by sp2The carbon atom of hydridization is flat in two dimension
Ordered arrangement is formed on face.Since Graphene was found from 2004, because its unique monoatomic layer thickness and hydridization carbon are former
The dimensional plane structure that son is formed, mechanical performance high, excellent calorifics electric conductivity and special spectrochemical property and cause strong
Concern, and be applied to numerous areas, for example：Ultracapacitor, nano electrochemical, the storage of biological and chemical sensor and hydrogen
Deposit.
Metal nanoparticle and grapheme material are combined, the application of Graphene can be further expanded, improve its performance.
Preparation method metal nanoparticle being supported on graphene film has physical method and the major class of chemical method two.Physical is main
It is to be modified onto graphene film noble metal nano particles by methods such as sputtering method, gas evaporation method, vapour depositions, general system
Standby composite is all the graphene film of surface modification metal nanoparticle.The advantage of the method is to prepare simply, is had the disadvantage
Preparation condition is harsh, and the nanoparticle size for preparing is larger, and the particle size range of nano-particle is difficult to control to.Chemical method is main
It is to prepare the graphene film that metal nanoparticle is loaded by reducing growth method.It is general that graphene oxide sheet is first passed through into thermal reduction
Or electronation obtains redox graphene piece, then by redox graphene add metal salt solution in, by also
Former agent obtains the redox graphene material of surfaces of metal nanoparticles modification in graphenic surface in-situ reducing slaine
(Chem.Mater.2009,21,4796–4802).But the oxygen reduction fossil of surfaces of metal nanoparticles modification prepared by the method
Black alkene material is easy to nano-particle occur to come off and agglomeration.To solve this problem, can first by slaine and oxidation
Graphene is reduced obtain colloidal metal nano-particle and redox graphene respectively, and further graphenic surface is repaiied
Decorations come improve the affinity between metal nanoparticle and graphene film dispersiveness (J.Am.Chem.Soc., 2010,132,
7279–7281；Nanoscale.2010,2(12):2733).In a word, the metal nanoparticle that chemical method preparation is prepared at present is repaiied
The method of the redox graphene of decorations is complicated, and operating procedure is various, it usually needs the reduction of two steps is completed.And what is prepared is compound
Material is all the graphene film of surface modification metal nanoparticle, and internal metal nano particle-doped graphene film prepares relative
Research is less.Therefore, it is necessary to developing, one kind is simple to operate, step is few, prepares convenient method to realize surface and interior part
The preparation of not metal nano particle-doped graphene film.
The content of the invention
Technical problem：The present invention overcomes the problem that the graphene film for preparing doping metal particles in the prior art is present,
A kind of flexible self-supporting graphene film of the doping metal particles of high conductivity and preparation method thereof is provided.The method operation side
Just, prepare simply, reactions steps are few, simple to equipment, technological requirement, it is possible to achieve internal metal nano particle-doped graphite
The preparation of the graphene film of alkene film and surface doping metal nanoparticle.The Graphene of the metal nanoparticle doping of preparation
The amount of the metal nanoparticle of film size, thickness and doping is controllable, pliability is good, electric conductivity is high.
Technical scheme：A kind of preparation method of the flexible self-supporting graphene film of metal nanoparticle doping of the invention
It is first to be well mixed graphene oxide water solution and metal salt solution, and by mixed solution titration in plasma
Drying and forming-film in surface-treated solid substrate, the film that will be obtained heats reduction in being put into aqueous ascorbic acid, obtains
The flexible self-supporting graphene film of metal nanoparticle inside doping；
Or by graphene oxide water solution titration drying and forming-film in the solid substrate that plasma surface treatment is crossed, then
Graphene oxide membrane surface is further added dropwise metal salt solution, forms graphite oxide-slaine composite membrane, is put into after drying anti-bad
Hematic acid heated in water solution is reduced, and obtains surface doping metal nanoparticle flexible self-supporting graphene film；
The graphene film thickness of described metal nanoparticle doping is 50nm-10 μm, and electrical conductivity is 1x104~
1x105S/m, the size of metal nanoparticle is evenly distributed on graphene film inside or surface in 1nm -200nm.
Described graphene oxide water solution is the graphene oxide water solution for preparing with graphite as raw material, described
Graphene oxide water solution concentration be 0.2~3mg/ml.
The metal salt solution be one kind in nickel acetate, gold chloride, chloroplatinic acid, silver nitrate, tetrachloro-palladium acid sodium etc. or
It is various.
The concentration of described metal salt solution is 0.1~20wt.%, and the mass ratio of slaine and graphene oxide is 0.1
~10:1.
Described drying temperature is 50~100 DEG C, and the time is 0.5~5h.
Described aqueous ascorbic acid concentration is 0.1~10wt.%.
The temperature of described heating reduction is 60~120 DEG C, 1~5h of time.
Described ascorbic acid is 4~20 with the mass ratio of graphite oxide-slaine composite membrane:1.
Described metal salt solution is the mixed liquor of various metals salting liquid, realizes various metals nano-particle codope
The preparation of flexible self-supporting graphene film.
Beneficial effect：
(1) present invention is by simple titration graphene oxide solution and metal salt solution film forming, and is reduced by a step
Achieve that the flexible self-supporting graphene film of metal nanoparticle doping.Simple to operate, experimental procedure is few, to equipment, work
Skill is less demanding, low cost, is capable of achieving batch production.(2) by controlling the dropwise addition mode of metal salt solution, it is possible to achieve internal
The preparation of metal nano particle-doped graphene film and the graphene film of surface doping metal nanoparticle.Will metal
Salting liquid and graphene oxide are easily added dropwise film forming simultaneously, and reduction obtains internal metal nano particle-doped graphene film；
By the way that graphene oxide film forming is first added dropwise, then metal salt solution film forming is added dropwise, surface doping metal nanoparticle is obtained after reduction
Graphene film；(3) amount and species of the metal nanoparticle of the size of self-supporting graphene film, thickness and doping can
Control.The present invention can control the size of graphene film by controlling the size of solid substrate, by the use for controlling graphene oxide
The thickness of the controllable graphene film of amount；The amount of metal nanoparticle is controlled by the amount of the metal salt solution for controlling to add；
The species of the metal salt solution by controlling to add, is capable of achieving the flexible self-supporting Graphene of various metals nano-particle codope
The preparation of film；(4) the self-supporting graphene film the pliability good bending of 0~180 degree (be capable of achieving graphene film) for preparing, lead
It is electrically high that (electrical conductivity of graphene film is 1x104~1x105), and metal nanoparticle disperses in graphene film S/m
It is even, it is expected to be used for the aspects such as catalysis, SERS, flexible electronic, super capacitor, wearable sensing.
Brief description of the drawings
Fig. 1 is the IV curves of the flexible self-supporting graphene film of golden nanometer particle surface doping.
Specific embodiment
The feature that the invention is further illustrated by the following examples, but the invention is not limited in following examples.Foundation
Technology disclosed by the invention, it will be clear to the skilled person that metal can be realized completely with reference to prior art
The preparation of the flexible self-supporting graphene conductive film of nanoparticle doped.
The preparation method of the flexible self-supporting graphene film of metal nanoparticle doping of the invention comprises the following steps：
(1) according to improved Hummers methods (ACS Nano 4 (8):4806 (2010), Improved synthesis of
Graphene oxide), with graphite as raw material, prepare the graphene oxide water solution that concentration is 0.2~3mg/ml；Metal salt solution
The concentration of solution is 0.1~20wt.%.
(2) graphene oxide solution and metal salt solution are well mixed, the mass ratio of slaine and graphene oxide is
0.1~10:1.By mixed solution titration in the solid substrate that plasma surface treatment is crossed, and further take the photograph 50~100
0.5~5h is vacuum dried under family name's degree, graphene oxide film is obtained；
(3) film in solid substrate is put into the aqueous ascorbic acid that concentration is 0.1~10wt.%, Ran Hou
1~5h of reaction is carried out under 60~120 degrees Celsius, obtain being suspended in aqueous solution surface inside it is metal nano particle-doped from propping up
Support graphene film.
(4) repeatedly soaked with water, rinsed, room temperature is dried, that is, obtain internal metal nano particle-doped flexible self-supporting
Graphene film.
Embodiment 1：The preparation of the flexible self-supporting graphene conductive film of inside doping nickel nano particle
(1) according to improved Hummers methods (document ACS Nano 4 (8):4806 (2010), Improved
Synthesis of graphene oxide), with graphite as raw material, concentration is prepared for the graphene oxide of 0.5mg/ml is water-soluble
Liquid；Configuration concentration is the nickel acetate aqueous solution of 2mg/ml；
(2) graphene oxide solution and nickel acetate solution are well mixed, the mass ratio of nickel acetate and graphene oxide is
0.2:1.By mixed solution titration in the solid substrate that plasma surface treatment is crossed, and further vacuum at 60 c
0.5h is dried, graphene oxide film is obtained；
(3) graphene oxide film in substrate of glass is put into the aqueous ascorbic acid that concentration is 0.5wt.%,
1h is reacted under 95 degrees Celsius, obtains being suspended in the self-supporting graphene film of the inside doping golden nanometer particle of solution surface.
(4) film is transferred to pure water immersion, is rinsed, room temperature is dried, that is, prepare internal doping golden nanometer particle
Self-supporting graphene film.
Embodiment 2：The preparation of the flexible self-supporting graphene conductive film of surface doping gold rice corpuscles
(1) according to improved Hummers methods (ACS Nano 4 (8):4806 (2010), Improved synthesis of
Graphene oxide), with graphite as raw material, it is the graphene oxide water solution of 2mg/ml to prepare concentration；Configuration concentration is
The aqueous solution of chloraurate of 4mg/ml；
(2) graphene oxide water solution is uniformly titrated in the substrate of glass of plasma surface treatment, and further
1h is vacuum dried under 75 degrees Celsius, graphene oxide film is obtained；Further titration chlorauric acid solution is in graphene oxide membrane
On, the mass ratio of gold chloride and graphene oxide is 2:1.And 2h is vacuum dried at 60 c.
(3) film in substrate is put into the aqueous ascorbic acid that concentration is 1.5wt.%, is entered under 95 degrees Celsius
Row reaction 1h, obtains being suspended in the self-supporting graphene film of the surface doping golden nanometer particle of solution surface.
(4) film is transferred to pure water immersion, is rinsed, room temperature is dried, that is, prepare surface doping golden nanometer particle
Self-supporting graphene conductive film.
Embodiment 3：The preparation of the flexible self-supporting graphene conductive film of surface doping gold and platinum rice corpuscles
(1) according to improved Hummers methods, with graphite as raw material, it is the graphene oxide water of 1.5mg/ml to prepare concentration
Solution；Configuration concentration is the aqueous solution of chloraurate of 3mg/ml；Configuration concentration is the chloroplatinic acid aqueous solution of 3mg/ml；
(2) graphene oxide water solution is uniformly titrated in the substrate of glass of plasma surface treatment, and further
2h is vacuum dried under 75 degrees Celsius, graphene oxide film is obtained；Further titration gold chloride and platinum acid chloride solution are in oxidation
On graphene film, gold chloride, the mass ratio of chloroplatinic acid and graphene oxide is 1:1:1.And 1h is vacuum dried at 80 degrees celsius.
(3) film in substrate is put into the aqueous ascorbic acid that concentration is 1wt.%, is carried out under 90 degrees Celsius
Reaction 3h, obtains being suspended in the surface doping gold of solution surface and the self-supporting graphene film of nano platinum particle.
(4) film is transferred to pure water immersion, is rinsed, room temperature is dried, that is, prepare surface doping gold and platinum nanoparticle
The self-supporting graphene conductive film of son.
Claims (9)
1. the preparation method of the flexible self-supporting graphene film of a kind of metal nanoparticle doping, it is characterised in that first will
Graphene oxide water solution and metal salt solution are well mixed, and mixed solution titration is crossed in plasma surface treatment
Drying and forming-film in solid substrate, the film that will be obtained heats reduction in being put into aqueous ascorbic acid, obtains metal nanoparticle
The flexible self-supporting graphene film of inside doping；
Or by graphene oxide water solution titration drying and forming-film in the solid substrate that plasma surface treatment is crossed, then in oxidation
Graphene membrane surface is further added dropwise metal salt solution, forms graphite oxide-slaine composite membrane, and ascorbic acid is put into after drying
Heated in water solution is reduced, and obtains surface doping metal nanoparticle flexible self-supporting graphene film；
The graphene film thickness of described metal nanoparticle doping is 50nm-10 μm, and electrical conductivity is 1x104~1x105S/m,
The size of metal nanoparticle is evenly distributed on graphene film inside or surface in 1nm -200nm.
2. the preparation method of the flexible self-supporting graphene film of metal nanoparticle according to claim 1 doping, its
It is characterised by, described graphene oxide water solution is the graphene oxide water solution for preparing with graphite as raw material, described
Graphene oxide water solution concentration be 0.2~3mg/ml.
3. the preparation method of the flexible self-supporting graphene film of metal nanoparticle according to claim 1 doping, its
Be characterised by, the metal salt solution be one kind in nickel acetate, gold chloride, chloroplatinic acid, silver nitrate, tetrachloro-palladium acid sodium etc. or
It is various.
4. the preparation method of the flexible self-supporting graphene film for being adulterated according to the metal nanoparticle described in claim 1, it is special
Levy and be, the concentration of described metal salt solution is 0.1~20wt.%, the mass ratio of slaine and graphene oxide for 0.1~
10:1。
5. the preparation method of the flexible self-supporting graphene film of metal nanoparticle according to claim 1 doping, its
It is characterised by, described drying temperature is 50~100 DEG C, the time is 0.5~5h.
6. the preparation method of the flexible self-supporting graphene film of metal nanoparticle according to claim 1 doping, its
It is characterised by, described aqueous ascorbic acid concentration is 0.1~10wt.%.
7. the preparation method of the flexible self-supporting graphene film of metal nanoparticle according to claim 1 doping, its
It is characterised by：The temperature of described heating reduction is 60~120 DEG C, 1~5h of time.
8. the preparation method of the flexible self-supporting graphene film of metal nanoparticle according to claim 1 doping, its
It is characterised by：Described ascorbic acid is 4~20 with the mass ratio of graphite oxide-slaine composite membrane:1.
9. the preparation method of the flexible self-supporting graphene film of metal nanoparticle according to claim 1 doping, its
It is characterised by：Described metal salt solution is the mixed liquor of various metals salting liquid, realizes various metals nano-particle codope
Flexible self-supporting graphene film preparation.
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| CN107381558A (en) * | 2017-08-20 | 2017-11-24 | 长沙小新新能源科技有限公司 | The preparation method and high-electroconductivity graphene film of a kind of high-electroconductivity graphene film |
| CN107488824A (en) * | 2017-06-27 | 2017-12-19 | 深圳市远思达成科技有限公司 | A kind of preparation method of the bonding brass wire with graphene film |
| CN107523773A (en) * | 2017-06-27 | 2017-12-29 | 深圳市远思达成科技有限公司 | A kind of preparation method of the bonding filamentary silver with graphene film |
| CN107824220A (en) * | 2017-11-09 | 2018-03-23 | 东南大学 | The preparation method of golden nanometer particle graphene melamine sponge composite |
| CN108505023A (en) * | 2018-05-14 | 2018-09-07 | 陕西师范大学 | A kind of preparation method of self-supporting two-dimensional metallic film using protein welding |
| CN108840329A (en) * | 2018-07-10 | 2018-11-20 | 杭州高烯科技有限公司 | A kind of preparation method of the graphene-based ultrathin membrane of independent self-supporting |
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| CN112429722A (en) * | 2020-12-01 | 2021-03-02 | 武汉汉烯科技有限公司 | Nano metal particle doped graphene film and preparation method thereof |
| CN112582105A (en) * | 2020-11-24 | 2021-03-30 | 西安交通大学 | Preparation method of high-conductivity and internally continuous graphene hybrid film |
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| CN107523773A (en) * | 2017-06-27 | 2017-12-29 | 深圳市远思达成科技有限公司 | A kind of preparation method of the bonding filamentary silver with graphene film |
| CN107381558B (en) * | 2017-08-20 | 2019-06-25 | 江苏百年门地家居科技有限公司 | A kind of preparation method and high-electroconductivity graphene film of high-electroconductivity graphene film |
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| CN107824220A (en) * | 2017-11-09 | 2018-03-23 | 东南大学 | The preparation method of golden nanometer particle graphene melamine sponge composite |
| CN108505023A (en) * | 2018-05-14 | 2018-09-07 | 陕西师范大学 | A kind of preparation method of self-supporting two-dimensional metallic film using protein welding |
| CN108840329A (en) * | 2018-07-10 | 2018-11-20 | 杭州高烯科技有限公司 | A kind of preparation method of the graphene-based ultrathin membrane of independent self-supporting |
| CN108840329B (en) * | 2018-07-10 | 2020-07-07 | 杭州高烯科技有限公司 | Preparation method of independent self-supporting graphene-based ultrathin film |
| CN109269394A (en) * | 2018-10-26 | 2019-01-25 | 钟祥博谦信息科技有限公司 | It is a kind of using PDMS as conductive film of base material and preparation method thereof |
| CN109342484A (en) * | 2018-12-21 | 2019-02-15 | 四川聚创石墨烯科技有限公司 | A kind of doping graphene oxide attribute detection method |
| CN109965868A (en) * | 2019-04-08 | 2019-07-05 | 清华大学 | It is tatooed formula electrode preparation method and device based on multi-layer graphene |
| CN111455359A (en) * | 2020-04-28 | 2020-07-28 | 中国科学院兰州化学物理研究所 | Preparation method of gold-graphene composite coating on copper surface |
| CN112582105A (en) * | 2020-11-24 | 2021-03-30 | 西安交通大学 | Preparation method of high-conductivity and internally continuous graphene hybrid film |
| CN112582105B (en) * | 2020-11-24 | 2022-08-05 | 西安交通大学 | Preparation method of high-conductivity and internally continuous graphene hybrid film |
| CN112429722A (en) * | 2020-12-01 | 2021-03-02 | 武汉汉烯科技有限公司 | Nano metal particle doped graphene film and preparation method thereof |
| CN113567512A (en) * | 2021-07-20 | 2021-10-29 | 上海大学 | Carbon-based material sensor based on lithium ion doping and preparation method thereof |
| WO2023123559A1 (en) * | 2021-12-28 | 2023-07-06 | 陕西理工大学 | Graphene-loaded noble metal composite powder and preparation method therefor, and schottky device |
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