CN105692604A - Method for preparing powder graphene from gas phase plasma - Google Patents
Method for preparing powder graphene from gas phase plasma Download PDFInfo
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- CN105692604A CN105692604A CN201610172352.4A CN201610172352A CN105692604A CN 105692604 A CN105692604 A CN 105692604A CN 201610172352 A CN201610172352 A CN 201610172352A CN 105692604 A CN105692604 A CN 105692604A
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- graphite alkene
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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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a method for preparing powder graphene from gas phase plasma. The method comprises the following steps of (1) vacuumizing a plasma reaction chamber to be below 100 Pa; (2) leading a gas mixture of carbon source gas and inert gas into the plasma reaction chamber; (3) starting a plasma reaction at set temperature and under set pressure, and continuing leading the gas mixture and vacuumizing; (4) obtaining the powder graphene. The powder graphene obtained by adopting the preparation method has the advantages of high purity, good crystallinity and low defect density, and additionally, the method is suitable for continuous production.
Description
Technical field
The invention belongs to technical field of new material preparation, the preparation method relating to a kind of high-quality graphene, specifically a kind of technique utilizing gaseous plasma to prepare powdered graphite alkene。
Background technology
Graphene is a kind of laminated structure two-dimensional material being made up of monolayer or few layer carbon atom。Graphene has all shown excellent performance in a lot, and such as, Graphene only absorbs the light of 2.3%, and its light transmission is very good；The heat conductivity of Graphene is up to 5300W/m K, and in current known material, heat conductivity is the highest；Electron mobility under Graphene room temperature can more than 15000cm2/ V s, resistivity can be low to moderate 10 simultaneously-6Ω cm, lower than copper or silver, it is the minimum material of current resistivity；Additionally, Graphene is also current the hardest the thinnest material。Graphene is prepared into powder body and is more beneficial for the application of Graphene, as graphene powder macroscopic view is assembled into three-dimensional material or forms composite with other material, have broad application prospects。
From prior art, the preparation method of powdered graphite alkene is mainly oxidation-reduction method, liquid phase stripping method, biological material subsequent treatment method, and raw material is graphite or plant material。The Graphene that oxidation-reduction method obtains is difficult to reduce completely, the existence of oxygen functional group limits the performance of Graphene, in Raman spectrum test, defect peak is clearly, obtained Graphene defect more [the oxidation-reduction method preparation of Graphene and structural characterization are described, Chinese Journal of Inorganic Chemistry, 26,2083,2010]。Liquid phase stripping method is difficult to obtain the relatively thin grapheme material of the number of plies [the liquid phase preparation of Graphene and the research of transparent conductive film, master thesis, Institutes Of Technology Of Nanjing]。And Graphene purity that the method for biological material post processing obtains is generally poor, electric property differs more with the performance of ideal graphite alkene, and the application in electronic correlation field may be restricted。
Being above the graphene preparation method that current industry uses, according to above-mentioned analysis, the Graphene that these methods obtain is individually present some problems, as many in defect, sheet thickness, purity are high not。Therefore, at present the Graphene performance of batch production is not especially desirable, and neither be smooth especially in the application and development of downstream product based on the graphene powder material obtained at present。
Summary of the invention
Based on above-mentioned prior art, the present invention proposes a kind of method that gaseous plasma prepares powdered graphite alkene, and the Graphene crystalline quality that it obtains is good, purity is high, and the method for the present invention is suitable to continuous prodution。
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of gaseous plasma prepares the method for powdered graphite alkene, as follows:
1) plasma reaction chamber being evacuated to below 100Pa, oxygen very easily aoxidizes gained Graphene when plasma reaction, vacuum is evacuated to below 100Pa and can reduce the oxygen contained in the former chamber atmosphere impact on products obtained therefrom；
2) the mixing gas of carbon-source gas and noble gas being passed into plasma reaction chamber, the ratio of carbon-source gas is 1%-100%, and the ratio of carbon-source gas is according to preparing the requirement of Graphene productivity ratio and being adjusted according to equipment collection efficiency；
3) starting plasma reaction under design temperature and pressure and keep gas to pass into the operation with vacuum suction, the response time is controlled according to required Graphene yield；
4) powdered graphite alkene is obtained。
Preferably, step 2), carbon-source gas is one or more the mixing gases in methane, ethane, propane, butane, pentane, ethylene, propylene, butylene, acetylene, propine。
Preferably, step 2), noble gas is one or more the mixing gases in argon, nitrogen, helium, neon。
Preferably, step 3), reaction temperature is 0-1000 degree Celsius, and reaction pressure is 10-200Pa。
Preferably, step 3), plasma is produced by direct current or rf plasma source, plasma power 10-1000 watt。
Preferably, step 4), utilize the filter screen of airflow downstream directly to collect the powdered graphite alkene of generation。
The invention discloses a kind of method that gaseous plasma prepares powdered graphite alkene, carbon containing source of the gas and inertia source of the gas are passed in plasma cavity by it, make carbon containing source of the gas generate powdered graphite alkene material by plasma reaction in uniform temperature and air pressure range；The powdered graphite alkene generated carries to collecting zone then through air-flow and is collected。
The Graphene purity that the preparation method of powdered graphite alkene of the present invention obtains is high, Graphene good crystallinity, and defect concentration is low, and meanwhile, the inventive method is applicable to continuous prodution。
Accompanying drawing explanation
The transmission electron microscope photo of Fig. 1 is embodiment 1 acquisition Graphene。
Fig. 2 is the Raman test result figure of the obtained Graphene of embodiment 1。
Detailed description of the invention
The present invention is further illustrated below in conjunction with drawings and Examples。
Embodiment 1:
1) plasma reaction chamber is evacuated to 50Pa；
2) methane gas and argon oxygen mixture are passed into plasma reaction chamber with 1:5 ratio；
3) control reaction chamber temperature and be 400 degrees Celsius and pressure is 100Pa, plasma generator power setting is 1000 watts and starts plasma reactions；
4) the powdered graphite alkene of generation is directly collected at the filter screen utilizing airflow downstream。
The Graphene obtained utilizes transmission electron microscope to test as it is shown in figure 1, obtained Graphene has two-dimensional characteristics, and lateral dimension is more than 100 microns。The Raman test result of obtained Graphene is as in figure 2 it is shown, defect peak is less, and characteristic peak is obvious, illustrates that crystalline quality is high。
Embodiment 2:
1) plasma reaction chamber is evacuated to 10Pa；
2) ethane gas and nitrogen mixed gas are passed into plasma reaction chamber with 1:1 ratio；
3) keeping reaction chamber temperature is room temperature, and controlling reaction chamber pressure is 10Pa, is 200 watts by plasma generator power setting and starts plasma reaction；
4) the powdered graphite alkene of generation is directly collected at the filter screen utilizing airflow downstream。
Embodiment 3:
1) plasma reaction chamber is evacuated to 1Pa；
2) propyne gas and helium oxygen mixture are passed into plasma reaction chamber with 1:1 ratio；
3) control reaction chamber temperature be 1000 degrees Celsius, pressure be 200Pa, plasma generator power setting is 10 watts and starts plasma reactions；
4) the powdered graphite alkene of generation is directly collected at the filter screen utilizing airflow downstream。
Embodiment 4:
1) plasma reaction chamber is evacuated to 90Pa；
2) ethane gas and nitrogen mixed gas are passed into plasma reaction chamber with 1:1 ratio；
3) keeping reaction chamber temperature is 800 degrees Celsius, and controlling reaction chamber pressure is 180Pa, is 900 watts by plasma generator power setting and starts plasma reaction；
4) powdered graphite alkene is obtained。
Embodiment 5:
1) plasma reaction chamber is evacuated to 20Pa；
2) ethane gas and nitrogen mixed gas are passed into plasma reaction chamber with 1:1 ratio；
3) keeping reaction chamber temperature is 50 degrees Celsius, and controlling reaction chamber pressure is 80Pa, is 500 watts by plasma generator power setting and starts plasma reaction；
4) powdered graphite alkene is obtained。
Embodiment 6:
1) plasma reaction chamber is evacuated to 70Pa；
2) ethane gas and nitrogen mixed gas are passed into plasma reaction chamber with 1:1 ratio；
3) keeping reaction chamber temperature is 900 degrees Celsius, and controlling reaction chamber pressure is 30Pa, is 50 watts by plasma generator power setting and starts plasma reaction；
4) powdered graphite alkene is obtained。
It will be appreciated by those of ordinary skill in the art that above example is intended merely to the explanation present invention, and be not intended as limitation of the invention, as long as within the scope of the invention, the change of above example, deformation all will be dropped on protection scope of the present invention。
Claims (6)
1. the method that gaseous plasma prepares powdered graphite alkene, is characterized in that as follows:
1) plasma reaction chamber is evacuated to below 100Pa；
2) the mixing gas of carbon-source gas and noble gas is passed into plasma reaction chamber；
3) under design temperature and setting pressure, start plasma reaction and keep passing into and vacuum suction process of mixing gas；
4) powdered graphite alkene is obtained。
2. the method that gaseous plasma according to claim 1 prepares powdered graphite alkene, it is characterized in that: step 2), described carbon-source gas is one or more the mixing gases in methane, ethane, propane, butane, pentane, ethylene, propylene, butylene, acetylene, propine。
3. the method that gaseous plasma according to claim 1 prepares powdered graphite alkene, it is characterised in that: step 2), described noble gas is one or more the mixing gases in argon, nitrogen, helium, neon。
4. the method that gaseous plasma according to claim 1 prepares powdered graphite alkene, it is characterised in that: step 3), described design temperature is 0-1000 degree Celsius, sets pressure as 10-200Pa。
5. the method that the gaseous plasma according to claim 1 or 4 prepares powdered graphite alkene, it is characterised in that: step 3), described plasma is produced by direct current or rf plasma source, plasma power 10-1000 watt。
6. the method that the gaseous plasma according to claim 1 or 4 prepares powdered graphite alkene, it is characterised in that: step 4), utilize the filter screen of airflow downstream directly to collect the powdered graphite alkene of generation。
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| CN201610172352.4A CN105692604A (en) | 2016-03-24 | 2016-03-24 | Method for preparing powder graphene from gas phase plasma |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107058971A (en) * | 2017-04-10 | 2017-08-18 | 中国科学院重庆绿色智能技术研究院 | The preparation method and application of graphene composite material |
| CN109956462A (en) * | 2019-03-14 | 2019-07-02 | 北京航空航天大学 | Carbon nano-particle preparation system, carbon nano-particle aerosol generate system and method |
| CN110451496A (en) * | 2019-09-17 | 2019-11-15 | 北京石墨烯研究院 | A method of continuously high-volume preparing powder graphene |
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| CN103193224A (en) * | 2013-04-17 | 2013-07-10 | 苏州大学 | Method for preparing graphene film on nonmetallic substrate at low temperature |
| CN104010965A (en) * | 2011-09-30 | 2014-08-27 | Ppg工业俄亥俄公司 | Production of graphenic carbon particles utilizing hydrocarbon precursor materials |
| US20140248190A1 (en) * | 2010-10-15 | 2014-09-04 | Cedar Ridge Research, Llc | System for producing graphene in a magnetic field |
| CN104163418A (en) * | 2013-05-16 | 2014-11-26 | 中山大学 | Method for realizing controllable orientated growth of graphene and graphene prepared by using method |
| CN104961127A (en) * | 2015-07-23 | 2015-10-07 | 合肥开尔纳米能源科技股份有限公司 | Method for preparing nano graphene powder by plasma chemical vapor synthesis |
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2016
- 2016-03-24 CN CN201610172352.4A patent/CN105692604A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20140248190A1 (en) * | 2010-10-15 | 2014-09-04 | Cedar Ridge Research, Llc | System for producing graphene in a magnetic field |
| CN104010965A (en) * | 2011-09-30 | 2014-08-27 | Ppg工业俄亥俄公司 | Production of graphenic carbon particles utilizing hydrocarbon precursor materials |
| CN103101907A (en) * | 2011-11-15 | 2013-05-15 | 海洋王照明科技股份有限公司 | Graphene, and preparation method and application thereof |
| CN103193224A (en) * | 2013-04-17 | 2013-07-10 | 苏州大学 | Method for preparing graphene film on nonmetallic substrate at low temperature |
| CN104163418A (en) * | 2013-05-16 | 2014-11-26 | 中山大学 | Method for realizing controllable orientated growth of graphene and graphene prepared by using method |
| CN104961127A (en) * | 2015-07-23 | 2015-10-07 | 合肥开尔纳米能源科技股份有限公司 | Method for preparing nano graphene powder by plasma chemical vapor synthesis |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107058971A (en) * | 2017-04-10 | 2017-08-18 | 中国科学院重庆绿色智能技术研究院 | The preparation method and application of graphene composite material |
| CN109956462A (en) * | 2019-03-14 | 2019-07-02 | 北京航空航天大学 | Carbon nano-particle preparation system, carbon nano-particle aerosol generate system and method |
| CN110451496A (en) * | 2019-09-17 | 2019-11-15 | 北京石墨烯研究院 | A method of continuously high-volume preparing powder graphene |
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