CN106865529A - A kind of preparation method of the microwave radiation technology high-quality redox graphene of triggering mode - Google Patents
A kind of preparation method of the microwave radiation technology high-quality redox graphene of triggering mode Download PDFInfo
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- CN106865529A CN106865529A CN201710218841.3A CN201710218841A CN106865529A CN 106865529 A CN106865529 A CN 106865529A CN 201710218841 A CN201710218841 A CN 201710218841A CN 106865529 A CN106865529 A CN 106865529A
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a kind of preparation method of the high-quality redox graphene of microwave radiation technology, belong to technical field of graphene, it is poor with reduction effect in solving the problems, such as existing redox graphene technology of preparing.The preparation method of redox graphene of the invention includes：1) preparation of sheet graphene oxide thin layer；2) the Microwave-assisted Reduction graphene oxide of triggering mode；The method equipment is simple, the time is short, energy consumption is low, it is pollution-free, do not need atmosphere of inert gases protection, suitable low cost, the extensive graphene oxide for preparing high-quality.
Description
Technical field
The invention belongs to technical field of graphene, it is related to a kind of preparation of the high-quality redox graphene of microwave radiation technology
Method.
Background technology
Graphene has excellent electricity, optics, physics, chemistry and architectural characteristic, has a wide range of applications.To mesh
Before untill, conventional graphene preparation method has mechanical stripping method, chemical vapour deposition technique, silicon carbide epitaxial growth method, liquid phase
Peel off graphite method, graphene oxide reducing process.But, for the use in practice, can low cost, prepare high-quality on a large scale
Graphene it is critical that.In these methods, redox Graphene has low production cost, extensive preparation letter
Singly, the characteristics of yield is high, is a kind of effective ways for meeting above-mentioned requirements.At present, many approach can be used to prepare reduction
Graphene oxide, conventional method has high temperature reduction method, chemical reduction method etc..The chemistry examination used during chemical reduction method
Agent, such as hydrazine hydrate, sodium borohydride, phenylhydrazine and hydroquinones, easily pollute environment.Although high temperature reduction method will not be to environment
Pollute, but this process must be carried out under the high temperature conditions, be high energy consumption.Most of all, existing reduction side
Method cannot effectively remove the oxygen-containing functional group that graphene oxide contains, and reduction effect is poor, and the redox graphene of preparation is still
It is so highly unordered.Therefore, exploitation has low cost, the method for the large-scale redox graphene for preparing high-quality concurrently is
One problem in the urgent need to address.
The content of the invention
The invention provides a kind of preparation method (Fig. 1) of the high-quality redox graphene of microwave radiation technology, to solve
The problem of the reduction effect difference of the redox graphene for preparing in the prior art.The method is pollution-free, simple for process, energy
Consumption is low.
The technical scheme is that：
1) preparation of graphene oxide thin layer
Filter paper is soaked with 1% calcium chloride solution, graphene oxide solution is added dropwise on filter paper, sprawl it
Open；Then 1% calcium chloride solution is used to process the graphene oxide of drawout；Then by the filter paper with graphene oxide
Clean repeatedly in deionized water, dried in atmosphere after taking-up or 70 DEG C of baking oven in dry；Finally carefully remove thin layer
The graphene oxide of shape.
2) the high-quality redox graphene of microwave radiation technology
Triggering material and graphene oxide thin layer are put into container together, it is contacted, micro-wave oven is then put into the lump
In.Under conditions of microwave, by triggering the collective effect of agent and microwave, within the time of several seconds, graphene oxide
It is reduced.
Described graphene oxide is prepared by Hummer methods；
Described graphene oxide is individual layer, GO of the lateral dimension more than 10 microns；
Described micro-wave oven is common household microwave oven；
Described triggering material is including graphene oxide, Graphene powder, iron wire or the paper clip for reducing etc.；
Beneficial effects of the present invention are：
The inventive method is pollution-free, simple for process, energy consumption is low, good (Raman spectrum has clear obvious to reduction effect
Graphene characteristic peak), suitable low cost, the extensive redox graphene for preparing high-quality.
Brief description of the drawings
The Microwave-assisted Reduction graphene oxide schematic diagram of Fig. 1 triggering modes；
High-quality redox graphene thin layer (b) of Fig. 2 graphene oxides thin layer (a) and microwave radiation technology；
Fig. 3 highly oriented pyrolytic graphites (HOPG), the Graphene (MW-rGO) of chemical vapor deposition, the high-quality of microwave radiation technology
The x-ray photoelectron of redox graphene (MW-rGO), thermal annealing redox graphene (rGO) and graphene oxide (GO)
Power spectrum phenogram；
Fig. 4 highly oriented pyrolytic graphites, the Graphene of chemical vapor deposition, the high-quality reduction-oxidation graphite of microwave radiation technology
The Raman spectrogram of alkene, thermal annealing redox graphene and graphene oxide；
Fig. 5 highly oriented pyrolytic graphites, the Graphene of chemical vapor deposition, the high-quality reduction-oxidation graphite of microwave radiation technology
The Graphene domain and I of alkene, thermal annealing redox graphene and graphene oxide2D/IGEvolution comparison diagram；
The Raman spectrogram of the preparation of the high-quality redox graphene of the iron wire triggering of Fig. 6 microwave radiation technologies；
The Raman spectrogram of the preparation of the high-quality redox graphene of the paper clip triggering of Fig. 7 microwave radiation technologies；
Specific embodiment
In order to further illustrate the present invention, below in the way of accompanying drawing and combine example to the present invention provide high-quality also
The preparation of former graphene oxide is described in detail, but can not be understood as limiting the scope of the present invention.Following reality
Apply material and instrument employed in example be it is commercially available.Additionally, any method similar to described content or impartial and material
It is all applied in the inventive method.
With reference to the example implemented being described further.
Embodiment 1
1) preparation of graphene oxide thin layer
Filter paper is soaked with 1% calcium chloride solution, then graphene oxide solution is added dropwise on filter paper, sprawl it
Open；Then 1% calcium chloride solution is used to process the graphene oxide of drawout；Then by the filter paper with graphene oxide
Clean repeatedly in deionized water, dried in atmosphere after taking-up or 70 DEG C of baking oven in dry；Finally carefully remove thin layer
The graphene oxide of shape.Fig. 2 (a) is the graphene oxide thin layer for preparing.
2) prepared by the redox graphene of microwave radiation technology
The Graphene of triggering and graphene oxide thin layer are put into container together, it is contacted, is then put into the lump
In micro-wave oven.Under conditions of microwave, by triggering the collective effect of agent and microwave, within the time of several seconds, oxidation
Graphene is reduced.Fig. 2 (b) is the high-quality redox graphene of the microwave radiation technology for preparing.
Redox graphene in the embodiment of the present invention 1 is carried out into x-ray photoelectron power spectrum sign and Raman respectively
Spectral characterization, is as a result displayed on Fig. 3 and Fig. 4, and be extracted the intensity (I at 2D peaks in Raman spectrum2D) and G peaks intensity (IG)
Ratio as the equation of Graphene domain size (domain size), be as a result displayed in Fig. 5.
It is illustrated in figure 3 the high-quality oxygen reduction of highly oriented pyrolytic graphite, the Graphene of chemical vapor deposition, microwave radiation technology
The x-ray photoelectron power spectrum phenogram of graphite alkene, thermal annealing redox graphene and graphene oxide.Oxidation to reducing
For Graphene, the peak between 286 and 289eV generally belongs to epoxides, hydroxyl, carboxyl etc..In microwave radiation technology condition
In the x-ray photoelectron power spectrum of the high-quality redox graphene of lower preparation, the characteristic peak at 286.9eV disappears, and that shows
By after microwave reduction, the oxygen-containing functional group in GO is drastically reduced.Unlike graphene oxide and thermal annealing redox graphene
X-ray photoelectron power spectrum result with obvious oxygen-containing functional group characteristic peak, microwave radiation technology triggering agent reduction height
Result of the result of the x-ray photoelectron power spectrum of quality redox graphene closer to CVD-graphene and HOPG.Additionally,
The halfwidth of redox graphene, slightly larger than the Graphene and the halfwidth of highly oriented pyrolytic graphite of chemical vapor deposition, this
Show also there is a small amount of defect in redox graphene.
Highly oriented pyrolytic graphite, the Graphene of chemical vapor deposition, the high-quality reduction-oxidation of microwave radiation technology as shown in Figure 4
The Raman spectrogram of Graphene, thermal annealing redox graphene and graphene oxide.The appearance at precipitous and symmetrical 2D peaks, with
And all to show that the high-quality redox graphene and high-sequential Graphene of microwave radiation technology have similar at the D peaks for almost disappearing
Feature.Relative to rGO prepared by highly unordered thermal reduction, the high-quality redox graphene of microwave radiation technology has and chemistry
The similar Raman spectrum of Graphene of vapour deposition process growth, this explanation by the reduction-oxidation of this simple method preparation also
Graphene is high-quality.
We are extracted the intensity (I at 2D peaks in Raman spectrum as shown in Figure 52D) and G peaks intensity (IG) ratio conduct
The equation of Graphene domain size, and highly oriented pyrolytic graphite, chemical vapor deposition Graphene, thermal annealing reduction-oxidation graphite
The result of alkene and graphene oxide is contrasted.The Graphene domain size of the redox graphene prepared by microwave radiation technology
The domain adjoining dimensions of the Graphene grown with chemical vapour deposition technique, than graphene oxide and the reduction-oxidation graphite of thermal annealing
The Graphene domain size of alkene significantly increases many.This explanation is high by the redox graphene prepared after microwave reduction
Quality.
Embodiment 2
The preparation of the high-quality redox graphene of the iron wire triggering of microwave radiation technology, its concrete technical scheme and embodiment
1 is similar, and difference is that the Graphene in embodiment 1 is substituted for iron wire.The Raman spectrum of the Graphene of preparation such as Fig. 6 institutes
Show.
Embodiment 3
The preparation of the high-quality redox graphene of the paper clip triggering of microwave radiation technology, its concrete technical scheme and implementation
Example 1 is similar, and difference is that the Graphene in embodiment 1 is substituted for paper clip.The Raman spectrum of the Graphene of preparation is such as
Shown in Fig. 7.
Claims (7)
1. a kind of preparation method of the microwave radiation technology high-quality redox graphene of triggering mode is it is characterised in that it includes as follows
Step：
1) preparation of graphene oxide thin layer
Filter paper is soaked with 1% calcium chloride solution, graphene oxide solution is added dropwise on filter paper, make its drawout；Then
1% calcium chloride solution is added dropwise on the graphene oxide of drawout；Then by the filter paper with graphene oxide in deionization
Cleaned repeatedly in water, dried in atmosphere after taking-up or baking oven in dry；Finally remove the graphene oxide of lamelliform；
2) the high-quality redox graphene of microwave radiation technology
Triggering material and graphene oxide thin layer are put into container together, it is contacted, is then put into micro-wave oven in the lump,
Under conditions of microwave, by triggering the collective effect of material and microwave, within the time of several seconds, graphene oxide is gone back
It is former.
2. the preparation method of the microwave radiation technology high-quality redox graphene of a kind of triggering mode as described in right 1 is required,
It is characterized in that：Step 1) described in graphene oxide lateral dimension be more than 10 microns.
3. the preparation method of the microwave radiation technology high-quality redox graphene of a kind of triggering mode as described in right 1 is required,
It is characterized in that：Step 1) described in prepare graphene oxide thin layer be sheet or bulk.
4. the preparation method of the microwave radiation technology high-quality redox graphene of a kind of triggering mode as described in right 1 is required,
It is characterized in that：Step 1) described in graphene oxide solution be the scattered concentration of water more than 4mg/ml graphene oxide it is molten
Liquid.
5. the preparation method of the microwave radiation technology high-quality redox graphene of a kind of triggering mode as described in right 1 is required,
It is characterized in that：Step 1) described in graphene oxide be Hummer methods prepare graphene oxide.
6. the preparation method of the microwave radiation technology high-quality redox graphene of a kind of triggering mode as described in right 1 is required,
It is characterized in that：Step 1) described in calcium chloride solution concentration for mass fraction more than 0.5% calcium chloride solution.
7. the preparation method of the microwave radiation technology high-quality redox graphene of a kind of triggering mode as described in right 1 is required,
It is characterized in that：Step 2) described in triggering material including redox graphene, Graphene powder, iron wire or paper clip etc..
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Cited By (6)
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| CN108358191A (en) * | 2018-05-10 | 2018-08-03 | 郑州新世纪材料基因组工程研究院有限公司 | A kind of low defect graphene and preparation method thereof |
| CN108490015A (en) * | 2018-03-15 | 2018-09-04 | 中国科学院宁波材料技术与工程研究所 | A kind of determination method of oxygen-containing graphene reducing degree |
| CN110482535A (en) * | 2019-09-24 | 2019-11-22 | 大连海事大学 | A kind of method and device of liquid phase microwave plasma redox graphene |
| CN111441106A (en) * | 2020-05-07 | 2020-07-24 | 西安交通大学 | Method for preparing high-quality graphene fibers by high-energy microwave irradiation |
| CN112938957A (en) * | 2021-04-14 | 2021-06-11 | 新乡医学院 | Graphene oxide paper and preparation method thereof |
| CN113089371A (en) * | 2021-04-14 | 2021-07-09 | 新乡医学院 | Reduced graphene oxide paper and preparation method thereof |
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Cited By (6)
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| CN108490015A (en) * | 2018-03-15 | 2018-09-04 | 中国科学院宁波材料技术与工程研究所 | A kind of determination method of oxygen-containing graphene reducing degree |
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| CN111441106A (en) * | 2020-05-07 | 2020-07-24 | 西安交通大学 | Method for preparing high-quality graphene fibers by high-energy microwave irradiation |
| CN112938957A (en) * | 2021-04-14 | 2021-06-11 | 新乡医学院 | Graphene oxide paper and preparation method thereof |
| CN113089371A (en) * | 2021-04-14 | 2021-07-09 | 新乡医学院 | Reduced graphene oxide paper and preparation method thereof |
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Application publication date: 20170620 |