CN102557021B - Nanocomposite material preparation method based on graphene oxide autocatalysis - Google Patents
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Abstract
The invention discloses a nanocomposite material preparation method based on graphene oxide autocatalysis. The method comprises the following steps: 1, slowly adding a metal salt solution to a graphene oxide solution, and utilizing carboxyl groups and hydroxyl groups on the graphene oxide as nucleation sites of nanoparticle crystals; and 2, carrying out crystal growth on the nucleation sites on graphene oxide sheets through an autocatalysis process to form graphene sheets which are respectively attached with a layer of metal nanoparticles, and ultrafiltering or dialyzing to prepare the graphene nanocomposite material. The method which has the characteristics of simple and easily controlled technology, environmental protection, low cost, convenience for popularization and the like provides a feasible way for the industrialized production of the graphene composite material. The prepared graphene nanocomposite material which has the advantages of high specific surface area and good conductivity has important application values in electronic devices, energy storage, drug loading, biological detection and the like.
Description
Technical field
The present invention relates to a kind of preparation method of the nano composite material based on graphene oxide autocatalysis, take graphene oxide and metal-salt, as starting material single stage method, prepare graphene nanocomposite material, belong to nano material, functional materials technical field of chemistry.
Background technology
Graphene is up to now, in the world the material of the thinnest material-monatomic thickness.Not only have excellent electric property, quality is light, and thermal conductivity is good, and specific surface area is large, and Young's modulus and breaking tenacity also can compare favourably with carbon nanotube, but also has some unique performances, as quantum hall effect, quantum tunneling effect etc.Due to above unique nanostructure and excellent performance, Graphene can be applicable in many advanced material and device, as thin-film material, energy storage material, liquid crystal material, mechanical resonator etc.; Graphene is mono-layer graphite, and raw material is easy to get, so low price is expensive unlike carbon nanotube, therefore Graphene is expected to replace carbon nanotube to become the high quality filler of polymer-based carbon carbon nano-composite material.
The nano composite material of at present preparation based on Graphene is also few, is mainly because neither hydrophilic also oleophylic not of Graphene, and reactive behavior is not high.Make that it is carried out to modification ratio more difficult, thereby cause with other Material cladding also more difficult.Preparing now graphene nanocomposite material is mainly first to allow graphene oxide and other Material cladding, then graphene oxide reduction is wherein obtained to graphene nanocomposite material; Or with Graphene and other Material cladding of modification.
The graphene oxide that Liang etc. prepare Hummers method is scattered in and in water, carries out supersound process, and adds hydrazine hydrate under stirring action, makes the graphite oxide of partial reduction.Then in the graphite oxide dispersion liquid of partial reduction, add the acetone soln of epoxy resin/stiffening agent, and carry out supersound process, under agitation stoichiometric number hour.After reaction, at 60 ℃, be dried and make suitable shape, then at 250 ℃ of logical N
2situation under the 2h that anneals, unreduced graphite oxide is thoroughly reduced, thereby increases its electroconductibility.Finally obtain the matrix material of Graphene/epoxy resin, its electromagnetic shielding effect is less than or equal to 21 decibels, has substantially reached commercial applications requirement (20 decibels).
Watcharomne etc. have prepared Graphene/SiCh nano composite material with sol-gel method.By graphite oxide/SiO
2colloidal sol is applied on borosilicate glass, then dried sample is placed in to the container that is full of hydrazine hydrate steam and reduces, and finally obtains Graphene/SiO
2nano composite material.And increased 400 ℃ of its electric conductivitys of the sample of processing, this is because Sample consolidation causes the density in matrix of Graphene to increase, and has reduced the spacing between Graphene, has increased the path of conduction, thereby has increased electric conductivity.Graphite oxide/SiO
2the transmissivity of nano composite material is fine, through reduction after, due to " greying " thus cause transmissivity to reduce.The employing solution mixing methods such as Chao have been prepared the nano composite material of Pt, Pd, Au and Graphene.Be about to the precursor salts solution of precious metal (Pt, Pd, Au) and ethylene glycol and join in the graphite oxide aqueous solution after ultrasonic, at 100 ℃, react 6h, finally obtained Graphene/metal particle nano matrix material.They find that ethylene glycol can be used as the reductive agent of graphite oxide, and ethylene glycol is nontoxic, all harmless to human and environment, thereby have overcome the toxicity of conventional graphite oxide reductive agent hydrazine hydrate.Li etc. have also prepared Graphene/Pt nano composite material, and find that its catalytic effect for methanol oxidation is better than Pt/ Cabot graphitized carbon black.The photoactivation reduction methods such as Williams have obtained Graphene/TiO
2nano composite material.Graphite oxide is added by titanium isopropoxide and is hydrolyzed the TiO obtaining
2in ethanol colloid, and carry out supersound process, thereby obtain graphite oxide/TiO
2nano dispersion fluid; Under the irradiation of UV-light, graphite oxide is reduced again, finally obtained Graphene/TiO
2nano composite material.The Graphene can observe in matrix material by AFM is individual layer or bilayer.Without the graphite oxide/TiO of UV-irradiation
2resistance be 233 kilohms, after the UV-irradiation of 2h, the Graphene/TiO obtaining
2the resistance of nano composite material is 30.5 kilohms, and this is close to 1/8 of original resistance.
In sum, graphene composite material is due to unique nanostructure and excellent performance, is expected to become the advanced special type function materials such as electronic material that a class is new, thin-film material, energy storage material, liquid crystal material, catalytic material.Graphene nanocomposite material is the key areas of Graphene application, although the Progress in Nanocomposites of Graphene is slow.Along with deepening continuously of research, the nano composite material of Graphene will get more and more, and its Application Areas and application prospect are by boundless.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the nano composite material based on graphene oxide autocatalysis, the graphene nanocomposite material making is dispersed in the aqueous solution, there is unique nanostructure and excellent physicals, can be applicable to the aspects such as electron device, catalysis, energy storage and biological detection.
The preparation method of a kind of nano composite material based on graphene oxide autocatalysis provided by the invention, is specially:
First in graphene oxide solution, add slowly metal salt solution, utilize the nucleation site of the groups such as carboxyl on graphene oxide and hydroxyl as nanoparticle crystal;
On the nucleation site of method by autocatalysis on graphene oxide sheet, carry out crystal growth again, thereby form the graphene film that is attached with layer of metal nanoparticle, ultrafiltration or dialysis, prepare graphene nanocomposite material.
Describedly in graphene oxide solution, add slowly metal salt solution to carry out under magnetic agitation effect, drip off salts solution and stop stirring, room temperature is standing.
Described room temperature time of repose is 72 hours.
The catalytic carrier of described nano composite material is graphene oxide.
The application of sample order of described reaction process, dropwise joins metal salt solution in graphene oxide and goes.
Described metal salt solution and graphene oxide liquor capacity ratio are 0.1: 1-1: 1.
The concentration of described graphene oxide solution is greater than or equal to 0.5mg/mL.
Described graphene oxide solution pH value is slightly acidic and purity when high, and Solution Dispersion is good.
Described metal-salt is Silver Nitrate, hydrochloro-auric acid etc.
The concentration of described metal salt solution is 0.1M-0.01M.
In all building-up processes, do not add reductive agent and tensio-active agent.
All synthesis steps all carry out at room temperature.
Compared with prior art, beneficial effect of the present invention: the present invention utilizes the nucleation site that the groups such as carboxyl on graphene oxide and hydroxyl are nanoparticle crystal, method by autocatalysis is adhered to layer of metal nanoparticle on graphene oxide sheet, prepares graphene nanocomposite material.It is simple and easy to control that the method has technique, and environmental friendliness is with low cost and be convenient to the features such as popularization, for its suitability for industrialized production graphene composite material has supplied a feasible path.Stannic oxide/graphene nano matrix material specific surface area prepared by the present invention is high, and good conductivity, has important using value at aspects such as electron device, energy storage, medicine carrying and biological detection.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph one of the stannic oxide/graphene nano matrix material prepared of the embodiment of the present invention;
Fig. 2 is the scanning electron microscope (SEM) photograph two of the stannic oxide/graphene nano matrix material prepared of the embodiment of the present invention;
Fig. 3 is the atomic power Electronic Speculum figure mono-of embodiment of the present invention stannic oxide/graphene nano matrix material;
Fig. 4 is the atomic power Electronic Speculum figure bis-of embodiment of the present invention stannic oxide/graphene nano matrix material.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment, take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
1) preparation of graphene oxide:
In dry beaker, add 230mL, the vitriol oil of massfraction 98%, is cooled to 0 ℃ with ice-water bath, adds while stirring natural flake graphite (10g), NaNO
3(5g) and KMnO
4(30g).Control reacting liquid temperature at 10-15 ℃, stirring reaction certain hour; Then beaker is placed in to the water bath with thermostatic control of 35 ℃ of left and right, when question response temperature rises to 35 ℃ of left and right, continues to stir 30min; Finally in stirring, add deionized water, control reacting liquid temperature in 100 ℃, continue to stir 30min.After reaction solution being diluted to 1000mL with deionized water, add again appropriate massfraction 5%H
2o
2, filtered while hot, with massfraction 5%HCl and deionized water fully wash until in filtrate without SO
4 2-.(use BaCl
2solution detects), obtain the graphene oxide that purifying is crossed.
2) stannic oxide/graphene nano nano composite material is synthetic:
(a) get 100mL graphene oxide solution (0.5mg/mL) in clean vial;
(b) with the silver nitrate solution 100mL of dropper absorption 0.01M, under magnetic agitation effect, dropwise join above-mentioned graphene oxide solution, mix, be placed in room temperature 72 hours;
(c) nanoparticle in unnecessary unreacted ion and solution is removed in ultrafiltration or dialysis, prepares graphene nanocomposite material;
(d) adopt AFM, the means such as SEM are carried out performance characterization.
Embodiment 2
(a) get 100mL graphene oxide solution (0.5mg/mL) in clean vial;
(b) with the chlorauric acid solution 10mL of dropper absorption 0.1M, under magnetic agitation effect, dropwise join above-mentioned graphene oxide solution, mix, be placed in room temperature 72 hours;
(c) nanoparticle in unnecessary unreacted ion and solution is removed in ultrafiltration or dialysis, prepares graphene nanocomposite material;
(d) adopt AFM, the means such as SEM are carried out performance characterization.
Embodiment 3
(a) get 100mL graphene oxide solution (0.6mg/mL) in clean vial;
(b) with the silver nitrate solution 50mL of dropper absorption 0.05M, under magnetic agitation effect, dropwise join above-mentioned graphene oxide solution, mix, be placed in room temperature 72 hours;
(c) nanoparticle in unnecessary unreacted ion and solution is removed in ultrafiltration or dialysis, prepares graphene nanocomposite material;
(d) adopt AFM, the means such as SEM are carried out performance characterization.
The graphene nanocomposite material that above-described embodiment obtains, as Figure 1-4, Fig. 1, Fig. 2 are the scanning electron microscope (SEM) photograph of the stannic oxide/graphene nano matrix material prepared of the embodiment of the present invention; Fig. 3, Fig. 4 are the atomic power Electronic Speculum figure of embodiment of the present invention stannic oxide/graphene nano matrix material.
The present invention utilizes the nucleation site that the groups such as carboxyl on graphene oxide and hydroxyl are nanoparticle crystal, by the method for autocatalysis, adheres to layer of metal nanoparticle on graphene oxide sheet, prepares graphene nanocomposite material.Should be understood that, be more than the preferred embodiments of the present invention, and the present invention can also have other embodiment, such as the parameter of replacing in above-described embodiment, or does simple variation etc., and these are all easy to realize for a person skilled in the art.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.Those skilled in the art, read after foregoing, for multiple modification of the present invention and substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (6)
1. a preparation method for the nano composite material based on graphene oxide autocatalysis, is characterized in that:
First in graphene oxide solution, add slowly metal salt solution, utilize carboxyl on graphene oxide and the oh group nucleation site as nanoparticle crystal; The ratio of described metal salt solution and graphene oxide liquor capacity is 0.1: 1-1: 1, and the concentration of described metal salt solution is 0.1M-0.01M, the concentration of described graphene oxide solution is greater than or equal to 0.5mg/mL;
On the nucleation site of method by autocatalysis on graphene oxide sheet, carry out crystal growth again, from forming the graphene film that is attached with layer of metal nanoparticle, ultrafiltration or dialysis, prepare graphene nanocomposite material.
2. the preparation method of the nano composite material based on graphene oxide autocatalysis according to claim 1, it is characterized in that describedly in graphene oxide solution, adding slowly metal salt solution to carry out under magnetic agitation effect, drip off salts solution and stop stirring, room temperature is standing.
3. the preparation method of the nano composite material based on graphene oxide autocatalysis according to claim 2, is characterized in that described room temperature time of repose is 72 hours.
4. the preparation method of the nano composite material based on graphene oxide autocatalysis according to claim 1, is characterized in that described graphene oxide solution pH value is weakly acidic purity when high, and Solution Dispersion is good.
5. according to the preparation method of the nano composite material based on graphene oxide autocatalysis described in claim 1-4 any one, it is characterized in that described metal-salt is Silver Nitrate, or hydrochloro-auric acid.
6. the preparation method of the nano composite material based on graphene oxide autocatalysis according to claim 1, is characterized in that all synthesis steps all carry out at room temperature.
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| CN103014683B (en) * | 2012-12-11 | 2014-12-10 | 西安交通大学 | Preparation method of graphene-based nano-silver composite |
| CN103021574B (en) * | 2012-12-27 | 2016-01-13 | 上海交通大学 | A kind of Graphene/inorganic semiconductor composite film and preparation method thereof |
| CN103203460A (en) * | 2013-03-14 | 2013-07-17 | 东南大学 | Method for preparing grapheme-Ag nano-particle composite material |
| CN103408895A (en) * | 2013-04-18 | 2013-11-27 | 北京化工大学常州先进材料研究院 | Preparation method of graphene/epoxy resin composite material |
| CN103482614B (en) * | 2013-09-09 | 2015-11-11 | 东南大学 | A kind of preparation method of graphene-ZnO nanoparticle composite material |
| CN105251979B (en) * | 2015-09-29 | 2017-06-13 | 中国航空工业集团公司北京航空材料研究院 | A kind of method for preparing metal nanoparticle/graphene/carbon nano-tube material |
| CN106829947B (en) * | 2017-04-01 | 2019-04-19 | 盐城工学院 | A kind of nanocomposite and preparation method thereof |
| CN107032340A (en) * | 2017-05-22 | 2017-08-11 | 河北工程大学 | A kind of simple method for preparing of lanthanide oxide/stannic oxide/graphene nano composite |
| CN107858059A (en) * | 2017-11-21 | 2018-03-30 | 新化县中润化学科技有限公司 | A kind of graphene silver waterborne conductive coating compound and preparation method |
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