CN106057481A - Preparation method of graphene/zinc oxide nanocomposite and purpose thereof - Google Patents
Preparation method of graphene/zinc oxide nanocomposite and purpose thereof Download PDFInfo
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- CN106057481A CN106057481A CN201610659196.4A CN201610659196A CN106057481A CN 106057481 A CN106057481 A CN 106057481A CN 201610659196 A CN201610659196 A CN 201610659196A CN 106057481 A CN106057481 A CN 106057481A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to the nanocomposite field and especially relates to a preparation method of a graphene/zinc oxide nanocomposite and a purpose thereof. The preparation method of the graphene/zinc oxide nanocomposite comprises the following steps of (1) dissolving graphene oxide and nano-zinc oxide into an ethanol/benzyl alcohol mixed solvent, adding cetyl trimethyl ammonium bromide and a titanate coupling agent, and after an ultrasonic wave is dispersed, carrying out mechanical stirring so as to acquire a mixed liquor; (2) transferring the mixed liquor to a closed container, inletting a protection gas, and carrying out a reaction for 6-10 hs at 130-170 DEG C so as to acquire a reduction reaction liquid; and (3) naturally cooling the reduction reaction liquid to a room temperature, filtering, washing so that the liquid becomes neutral, drying in a vacuum mode and then crushing so as to acquire the graphene/zinc oxide nanocomposite, The preparation method is simple and easy to perform. The acquired graphene/zinc oxide nanocomposite fully combines a high theoretical capacity of the zinc oxide and high conductivity of the graphene and can be used as an electrode material to be applied to a super capacitor.
Description
Technical field
The present invention relates to field of nanocomposite materials, be specifically related to the system of a kind of Graphene/zinc oxide nanometer composite material
Preparation Method and application thereof.
Background technology
Inorganic material is distributed in graphene nanometer sheet surface make Graphene/inorganic nano composite material, Qi Zhongwu
The existence of machine nanoparticle can make the distance between graphene sheet layer increase to several nanometer, thus is greatly reduced graphene sheet layer
Between interaction, make the uniqueness of single-layer graphene be retained, usual chemical modification method is difficult to reach.Therefore,
Grapheme modified with inorganic nano-particle, it is provided that the new way that a tissue Graphene is reunited.From another perspective, graphite
Alkene/inorganic nano composite material, not only can keep the inherent character of Graphene and inorganic nano-particle simultaneously, and can produce
Raw synergism, is with a wide range of applications.
Metallic compound prepares composite from Graphene by different methods, is mainly used in ultracapacitor, lithium battery
In field, metallic compound includes metal-oxide, metal hydroxides, metal sulfide etc..Wherein zinc oxide/Graphene is multiple
The advantage that condensation material has zinc oxide and Graphene.Zinc oxide has the electricity of excellence, and optical chemical performance makes it at light
Electricity, solaode, Flied emission, the field such as air-sensitive has application prospect.The two-dimensional structure that Graphene is then made up of carbon atom,
Make it have the optics of excellence, transparency, mechanical elasticity, heat stability, the performance such as chemical stability.Built oxidation in the last few years
The research in zinc/graphene composite material field is increasingly paid attention to, and the most classical synthetic method is first in substrate
Then growth Graphene utilizes excusing from death spray pyrolysis, and the various means such as electrochemical deposition and Hydrothermal Synthesis grow on Graphene
Zinc oxide.But this kind of synthetic method, reactions steps is many, and required instrument and equipment is complicated.
Summary of the invention
The invention provides the preparation method and its usage of a kind of Graphene/zinc oxide nanometer composite material, described stone
The preparation method of ink alkene/zinc oxide nanometer composite material is simple, and technological parameter is easy to control, gained Graphene/zinc oxide nano
Nano composite material fully combines the higher theoretical capacity of zinc oxide and Graphene high conductivity.
The invention provides as realizing object above, the present invention is achieved by the following technical programs:
The preparation method of a kind of Graphene/zinc oxide nanometer composite material, comprises the following steps:
(1) graphene oxide, nano zine oxide are dissolved in ethanol/benzyl alcohol mixed solvent, add cetyl front three
Base ammonium bromide and titanate coupling agent, ultrasound wave dispersion 0.5h, then mechanical agitation 0.5h, obtain mixed liquor；
(2) mixed liquor is transferred in hermetic container, is passed through protective gas, at 130-170 DEG C, react 6-10h, must go back
Former reactant liquor；
(3) reduction reaction liquid being naturally cooled to room temperature, filter, washing, to neutral, pulverized after vacuum drying, is obtained graphite
Alkene/zinc oxide nanometer composite material.
Preferably, in described step (1), the mass ratio of graphene oxide and nano zine oxide is 1:8-2:11.
Preferably, in described step (1), the mass ratio of graphene oxide and titanate coupling agent is 10:1.
Preferably, the protective gas in described step (2) is nitrogen or argon.
Preferably, in described step (3), washing is washed for use dehydrated alcohol.
Graphene/zinc-oxide nano prepared by the preparation method of a kind of Graphene/zinc oxide nanometer composite material is combined
Material is as electrode material purposes in ultracapacitor.
The invention have the benefit that
1. in the present invention, the preparation method of Graphene/zinc oxide nanometer composite material is simple, and technological parameter is easy to control,
Using solvothermal method to prepare Graphene, energy consumption is low, can effectively reduce production cost, and gained Graphene/zinc-oxide nano is multiple
Condensation material fully combines the higher theoretical capacity of zinc oxide and Graphene high conductivity.
2. the titanate coupling agent that the present invention adds in reaction system, makes graphene oxide reduction grafting metatitanic acid the most simultaneously
Ester coupling agent molecule, under the synergism of cetyl trimethylammonium bromide, can improve the dispersibility of reaction system, make to be combined
The stability of material strengthens.
3. the Graphene that prepared by the present invention/zinc oxide nanometer composite material point chemical property is good, can be as ultracapacitor
Electrode material.
Detailed description of the invention
Further illustrate the technical solution of the present invention below in conjunction with specific embodiment, embodiment is not to be construed as right
The restriction of technical solution.
Embodiment 1:
The preparation method of a kind of Graphene/zinc oxide nanometer composite material, comprises the following steps:
(1) graphene oxide, nano zine oxide are dissolved in ethanol/benzyl alcohol mixed solvent, add cetyl front three
Base ammonium bromide and titanate coupling agent, ultrasound wave dispersion 0.5h, then mechanical agitation 0.5h, obtain mixed liquor；Wherein graphene oxide
Being 2:11 with the mass ratio of nano zine oxide, graphene oxide is 10:1 with the mass ratio of titanate coupling agent.
(2) mixed liquor is transferred in hermetic container, is passed through nitrogen protection, at 170 DEG C, react 6h, obtain reduction reaction
Liquid；
(3) reduction reaction liquid is naturally cooled to room temperature, filter, use absolute ethanol washing to neutral, after vacuum drying
Pulverize, obtain Graphene/zinc oxide nanometer composite material.
Embodiment 2:
The preparation method of a kind of Graphene/zinc oxide nanometer composite material, comprises the following steps:
(1) graphene oxide, nano zine oxide are dissolved in ethanol/benzyl alcohol mixed solvent, add cetyl front three
Base ammonium bromide and titanate coupling agent, ultrasound wave dispersion 0.5h, then mechanical agitation 0.5h, obtain mixed liquor；Wherein graphene oxide
Being 1:8 with the mass ratio of nano zine oxide, graphene oxide is 10:1 with the mass ratio of titanate coupling agent.
(2) mixed liquor is transferred in hermetic container, is passed through argon shield, at 130 DEG C, react 10h, obtain reduction reaction
Liquid；
(3) reduction reaction liquid is naturally cooled to room temperature, filter, use absolute ethanol washing to neutral, after vacuum drying
Pulverize, obtain Graphene/zinc oxide nanometer composite material.
Embodiment 3:
The preparation method of a kind of Graphene/zinc oxide nanometer composite material, comprises the following steps:
(1) graphene oxide, nano zine oxide are dissolved in ethanol/benzyl alcohol mixed solvent, add cetyl front three
Base ammonium bromide and titanate coupling agent, ultrasound wave dispersion 0.5h, then mechanical agitation 0.5h, obtain mixed liquor；Wherein graphene oxide
Being 1:7 with the mass ratio of nano zine oxide, graphene oxide is 10:1 with the mass ratio of titanate coupling agent.
(2) mixed liquor is transferred in hermetic container, is passed through nitrogen protection, at 150 DEG C, react 8h, obtain reduction reaction
Liquid；
(3) reduction reaction liquid is naturally cooled to room temperature, filter, use absolute ethanol washing to neutral, after vacuum drying
Pulverize, obtain Graphene/zinc oxide nanometer composite material.
Embodiment 4:
The preparation method of a kind of Graphene/zinc oxide nanometer composite material, comprises the following steps:
(1) graphene oxide, nano zine oxide are dissolved in ethanol/benzyl alcohol mixed solvent, add cetyl front three
Base ammonium bromide and titanate coupling agent, ultrasound wave dispersion 0.5h, then mechanical agitation 0.5h, obtain mixed liquor；Wherein graphene oxide
Being 1:6 with the mass ratio of nano zine oxide, graphene oxide is 10:1 with the mass ratio of titanate coupling agent.
(2) mixed liquor is transferred in hermetic container, is passed through argon shield, at 140 DEG C, react 9h, obtain reduction reaction
Liquid；
(3) reduction reaction liquid is naturally cooled to room temperature, filter, use absolute ethanol washing to neutral, after vacuum drying
Pulverize, obtain Graphene/zinc oxide nanometer composite material.
Embodiment 5:
The preparation method of a kind of Graphene/zinc oxide nanometer composite material, comprises the following steps:
(1) graphene oxide, nano zine oxide are dissolved in ethanol/benzyl alcohol mixed solvent, add cetyl front three
Base ammonium bromide and titanate coupling agent, ultrasound wave dispersion 0.5h, then mechanical agitation 0.5h, obtain mixed liquor；Wherein graphene oxide
Being 2:15 with the mass ratio of nano zine oxide, graphene oxide is 10:1 with the mass ratio of titanate coupling agent.
(2) mixed liquor is transferred in hermetic container, is passed through nitrogen protection, at 160 DEG C, react 7h, obtain reduction reaction
Liquid；
(3) reduction reaction liquid is naturally cooled to room temperature, filter, use absolute ethanol washing to neutral, after vacuum drying
Pulverize, obtain Graphene/zinc oxide nanometer composite material.
Embodiment 6:
The preparation method of a kind of Graphene/zinc oxide nanometer composite material, comprises the following steps:
(1) graphene oxide, nano zine oxide are dissolved in ethanol/benzyl alcohol mixed solvent, add cetyl front three
Base ammonium bromide and titanate coupling agent, ultrasound wave dispersion 0.5h, then mechanical agitation 0.5h, obtain mixed liquor；Wherein graphene oxide
Being 2:13 with the mass ratio of nano zine oxide, graphene oxide is 10:1 with the mass ratio of titanate coupling agent.
(2) mixed liquor is transferred in hermetic container, is passed through argon shield, at 155 DEG C, react 6h, obtain reduction reaction
Liquid；
(3) reduction reaction liquid is naturally cooled to room temperature, filter, use absolute ethanol washing to neutral, after vacuum drying
Pulverize, obtain Graphene/zinc oxide nanometer composite material.
It is more than the description to the embodiment of the present invention, by the described above to the disclosed embodiments, makes this area special
Industry technical staff is capable of or uses the present invention.Those skilled in the art are come by the multiple amendment to these embodiments
Saying and will be apparent from, generic principles defined herein can be in the situation without departing from the spirit or scope of the present invention
Under, realize in other embodiments.Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is intended to symbol
Close the widest scope consistent with principles disclosed herein and features of novelty.
Claims (6)
1. the preparation method of Graphene/zinc oxide nanometer composite material, it is characterised in that comprise the following steps:
(1) graphene oxide, nano zine oxide are dissolved in ethanol/benzyl alcohol mixed solvent, add cetyl trimethyl bromine
Change ammonium and titanate coupling agent, ultrasound wave dispersion 0.5h, then mechanical agitation 0.5h, obtain mixed liquor；
(2) mixed liquor is transferred in hermetic container, is passed through protective gas, at 130-170 DEG C, react 6-10h, must reduce anti-
Answer liquid；
(3) reduction reaction liquid being naturally cooled to room temperature, filter, washing, to neutral, pulverized after vacuum drying, is obtained Graphene/oxygen
Change zinc nano composite material.
The preparation method of Graphene/zinc oxide nanometer composite material the most according to claim 1, it is characterised in that described
In step (1), graphene oxide is 1:8-2:11 with the mass ratio of nano zine oxide.
The preparation method of Graphene/zinc oxide nanometer composite material the most according to claim 1, it is characterised in that described
In step (1), graphene oxide is 10:1 with the mass ratio of titanate coupling agent.
The preparation method of Graphene/zinc oxide nanometer composite material the most according to claim 1, it is characterised in that described
Protective gas in step (2) is nitrogen or argon.
The preparation method of Graphene/zinc oxide nanometer composite material the most according to claim 1, it is characterised in that described
In step (3), washing is for using dehydrated alcohol to wash.
6. according to prepared by the preparation method of the Graphene/zinc oxide nanometer composite material described in any one of claim 1-5
Graphene/zinc oxide nanometer composite material is as electrode material purposes in ultracapacitor.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107093521A (en) * | 2017-05-08 | 2017-08-25 | 华北电力大学（保定） | A kind of Ce/C composites, its preparation method and its application |
| CN108922792A (en) * | 2018-07-13 | 2018-11-30 | 黑龙江省科学院高技术研究院 | A kind of preparation method of graphene/ZnO/NiO composite material |
| CN108949102A (en) * | 2018-07-20 | 2018-12-07 | 青岛大学 | A kind of nano zine oxide/graphene composite material and preparation method thereof |
| CN109734056A (en) * | 2019-03-08 | 2019-05-10 | 上海理工大学 | Metal oxide/preparation method of fold rGO composite nano materials and the preparation method of fold nano-metal-oxide |
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| CN104076073A (en) * | 2014-07-10 | 2014-10-01 | 南京理工大学 | Short-bar-shaped nano-zinc oxide/graphene compound and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108922792A (en) * | 2018-07-13 | 2018-11-30 | 黑龙江省科学院高技术研究院 | A kind of preparation method of graphene/ZnO/NiO composite material |
| CN108949102A (en) * | 2018-07-20 | 2018-12-07 | 青岛大学 | A kind of nano zine oxide/graphene composite material and preparation method thereof |
| CN109734056A (en) * | 2019-03-08 | 2019-05-10 | 上海理工大学 | Metal oxide/preparation method of fold rGO composite nano materials and the preparation method of fold nano-metal-oxide |
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Application publication date: 20161026 |