CN102583350B - Preparation method of graphene material - Google Patents
Preparation method of graphene material Download PDFInfo
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- CN102583350B CN102583350B CN2012100467880A CN201210046788A CN102583350B CN 102583350 B CN102583350 B CN 102583350B CN 2012100467880 A CN2012100467880 A CN 2012100467880A CN 201210046788 A CN201210046788 A CN 201210046788A CN 102583350 B CN102583350 B CN 102583350B
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Abstract
本发明公开了一种石墨烯材料的制备方法，将石墨粉末溶于有机溶剂或者水中，形成悬浮液，放入安装有齿轮组的容器中，齿轮低速，取出浆料，超声处理，进行高速离心使得未剥离撕裂的石墨颗粒和石墨片通过离心作用沉淀于离心管底部，而上层溶液即为单层石墨烯和多层石墨烯，最后对上层溶液进行浓缩、分离，可以获得石墨烯粉体或者稳定的石墨烯溶液。本发明利用齿轮组不停地转动同时搅拌石墨悬浮液，通过齿轮齿不停地啮合，不停地撕裂石墨片，克服了常规机械法引入缺陷多、产量低得缺点，能够高效、高质量地制备石墨烯。
The invention discloses a preparation method of a graphene material. Dissolving graphite powder in an organic solvent or water to form a suspension, putting it into a container equipped with a gear set, taking out the slurry at a low speed, ultrasonic treatment, and performing high-speed centrifugation The unstripped and torn graphite particles and graphite flakes are precipitated at the bottom of the centrifuge tube by centrifugation, and the upper layer solution is single-layer graphene and multi-layer graphene. Finally, the upper layer solution is concentrated and separated to obtain graphene powder Or a stable graphene solution. The present invention utilizes the gear set to continuously rotate and stir the graphite suspension at the same time, and the graphite sheets are continuously torn through the gear teeth, thereby overcoming the disadvantages of many defects introduced by the conventional mechanical method and low output, and can achieve high efficiency and high quality to prepare graphene.
Description
Technical field
The present invention relates to a kind of preparation method of grapheme material, belong to the novel nano-material field.
Background technology
The Graphene of Two-dimensional Carbon atomic crystal has good electricity leads and thermal conductivity and other Their Exotic Properties, and how preparing quickly and efficiently the Graphene of better quality and can conveniently applying is the emphasis direction that people explore this new function material.
Initial Graphene is torn and is found to exist from graphite block body by adhesive tape, constantly extends a lot of preparation methods.Comprise mechanically peel method, thermal expansion graphite method, chemical Vapor deposition process etc.But the method that exists at present also has shortcoming separately.For example, the adhesive tape method of Tearing needs repeatedly just can prepare the Graphene of trace, and the Graphene of processing on adhesive tape is cumbersome; Ball milled is because the shock of ball can will be introduced more defect in the Graphene two-dimensional surface; The time that chemical method etc. need to be grown is prepared, and chemical method needs number of chemical reagent.
Gear uses usually used as a kind of gearing, and in rotation, motion-work wheel and driven wheel ceaselessly mesh, and ceaselessly has frictional tear between wheel tooth.The mechanical means of Graphene can be torn out two-dimentional atomic crystal layer exactly effectively., for above characteristics, gear can be rotated as a kind of method that effectively prepares high-quality Graphene.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of grapheme material, the method, in conjunction with performance, the characteristics of Graphene, propose to utilize gear-driven engagement,, in conjunction with supersound process and high speed centrifugation, prepare Graphene.
The present invention adopts following technical scheme:
The preparation method of grapheme material is characterized in that comprising the following steps:
(1) powdered graphite is dissolved in organic solvent or water, forms suspension, then put into the container that gear unit is installed, gear, in low speed 1-800 rev/min rotation, rotates 0.5-30 hour, takes out slurry;
(2) step (1) slurry is carried out supersound process 0.5-2 hour, then high speed centrifugation, centrifugal rotational speed is at 1000-4000 rev/min, centrifugal more than 5 minutes, make the unstripped graphite granule of tearing and graphite flake be deposited in the centrifuge tube bottom by centrifugation, and upper solution is single-layer graphene and multi-layer graphene solution;
(3) upper solution after centrifugal in step (2) is concentrated, separating treatment, can obtain graphene powder or graphene solution.
The preparation method of described grapheme material is characterized in that: described Graphite Powder 99 is artificial synthetic graphite powder, natural graphite powder, high temperature pyrolysis Graphite Powder 99.
The preparation method of described grapheme material is characterized in that: described organic solvent is alcohol, acetone, dimethyl formamide, phenyl aldehyde.
The preparation method of described grapheme material is characterized in that: described gear unit is comprised of the gear of two or more quantity.
Beneficial effect of the present invention:
The present invention utilizes gear unit to gyrate and stirs simultaneously graphite suspension, by wheel tooth, ceaselessly meshes, and ceaselessly tears graphite flake, has overcome the conventional mechanical method and has introduced the shortcoming that defect is many, yield poorly, and can prepare efficiently, in high quality Graphene.
Description of drawings
Fig. 1 is gear unit schematic diagram used in the present invention.
Fig. 2 is the Graphene transmission electron microscope TEM photo that the present invention prepares.
Embodiment
Embodiment: Graphite Powder 99 and phenyl aldehyde are formed suspension according to the solubility of 2mg/ml, put into the container that gear unit is installed, gear rotational speed 50 right side of turning left, rotated 5 hours, takes out slurry, supersound process 0.5 hour, carry out high speed centrifugation, centrifugal rotational speed 4000 turns, 5 minutes, make the unstripped graphite granule of tearing and graphite flake be deposited in centrifuge tube or concentrator bowl bottom by centrifugation, and upper solution is single-layer graphene and multi-layer graphene solution.Graphene in the upper solution that obtains is carried out transmission electron microscope scanning, and Fig. 2 is the Graphene transmission electron microscope TEM photo of preparation.Fig. 1 is gear unit schematic diagram used in the present invention.
Claims (4)
1. the preparation method of a grapheme material is characterized in that comprising the following steps:
(1) powdered graphite is dissolved in organic solvent or water, forms suspension, then put into the container that gear unit is installed, gear, in low speed 1-800 rev/min rotation, rotates 0.5-30 hour, takes out slurry;
(2) step (1) slurry is carried out supersound process 0.5-2 hour, then high speed centrifugation, centrifugal rotational speed is at 1000-4000 rev/min, centrifugal more than 5 minutes, make the unstripped graphite granule of tearing and graphite flake be deposited in the centrifuge tube bottom by centrifugation, and upper solution is single-layer graphene and multi-layer graphene solution;
(3) upper solution after centrifugal in step (2) is concentrated, separating treatment, can obtain graphene powder or graphene solution.
2. the preparation method of grapheme material according to claim 1, it is characterized in that: described Graphite Powder 99 is artificial synthetic graphite powder, natural graphite powder, high temperature pyrolysis Graphite Powder 99.
3. the preparation method of grapheme material according to claim 1, it is characterized in that: described organic solvent is alcohol, acetone, dimethyl formamide, phenyl aldehyde.
4. the preparation method of grapheme material according to claim 1, it is characterized in that: described gear unit is comprised of the gear of two or more quantity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012100467880A CN102583350B (en) | 2012-02-28 | 2012-02-28 | Preparation method of graphene material |
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| CN2012100467880A CN102583350B (en) | 2012-02-28 | 2012-02-28 | Preparation method of graphene material |
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| CN102583350A CN102583350A (en) | 2012-07-18 |
| CN102583350B true CN102583350B (en) | 2013-11-20 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB201304770D0 (en) | 2013-03-15 | 2013-05-01 | Provost Fellows Foundation Scholars And The Other Members Of Board Of | A scalable process for producing exfoliated defect-free, non-oxidised 2-dimens ional materials in large quantities |
| TW201441147A (en) * | 2013-04-23 | 2014-11-01 | Enerage Inc | Graphene suspension solution and its preparation method |
| CN106365155A (en) * | 2015-07-20 | 2017-02-01 | 北京中科云腾科技有限公司 | Graphene and preparation method thereof |
| CN106542525B (en) * | 2016-10-27 | 2018-09-11 | 董兰田 | Continuous adhesive tape legal system takes stripping degumming and the packing method of graphene |
| WO2020175504A1 (en) * | 2019-02-28 | 2020-09-03 | 積水化学工業株式会社 | Flake graphite and manufacturing method therefor |
| CN114426271A (en) * | 2020-10-13 | 2022-05-03 | 中国石油化工股份有限公司 | Graphene and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7824651B2 (en) * | 2007-05-08 | 2010-11-02 | Nanotek Instruments, Inc. | Method of producing exfoliated graphite, flexible graphite, and nano-scaled graphene platelets |
| CN101671015B (en) * | 2009-10-13 | 2011-07-20 | 南昌航空大学 | Method of producing graphene |
| FR2962121B1 (en) * | 2009-11-03 | 2012-07-13 | Centre Nat Rech Scient | PREPARATION OF GRAPHENE BY MECHANICAL SLURRY OF GRAPHIC MATERIALS |
| CN101704520B (en) * | 2009-11-05 | 2012-05-23 | 华侨大学 | Method for producing graphene |
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