CN103818899B - A kind of apparatus and method preparing graphene paper based on glow plasma positive column - Google Patents
A kind of apparatus and method preparing graphene paper based on glow plasma positive column Download PDFInfo
- Publication number
- CN103818899B CN103818899B CN201410049374.2A CN201410049374A CN103818899B CN 103818899 B CN103818899 B CN 103818899B CN 201410049374 A CN201410049374 A CN 201410049374A CN 103818899 B CN103818899 B CN 103818899B
- Authority
- CN
- China
- Prior art keywords
- paper
- chip bench
- graphene
- tapered electrode
- graphene oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a kind of apparatus and method preparing graphene paper based on glow plasma positive column.It comprises chip bench, quartz socket tube, silica tube, tapered electrode, high pressure negative electricity power supply, helium source of the gas; Chip bench, quartz socket tube and tapered electrode are arranged in silica tube; Chip bench can translation in silica tube; Chip bench embeds quartz socket tube; Tapered electrode cone-tip surface is to chip bench; Tapered electrode is connected with high pressure negative electricity power supply, chip bench ground connection; Silica tube one end open, the other end is connected with helium source of the gas.In preparation process, graphene oxide paper is fixed on chip bench, and between graphene oxide paper and tapered electrode, is formed the glow discharge plasma with positive column by high pressure.The present invention can realize the quick preparation of graphene paper at ambient pressure, and simply, environmental friendliness, capacity usage ratio is high, possesses extensive potentiality of amplifying application, is conducive to promoting the widespread use of graphene paper in multiple field for device and process.
Description
Technical field
The invention belongs to plasma body and technical field of nanometer material preparation, particularly relate to a kind of apparatus and method preparing graphene paper based on glow plasma positive column.
Background technology
Graphene is a kind of by sp
2the two-dimension nano materials that hydbridized carbon atoms arranges with hexagonal lattice, since Late Cambrian in 2004, has caused great interest and extensive concern with its peculiar performance.The flexible flexible materials that graphene paper is made up of multi-disc Graphene, has good electroconductibility, large specific surface area and excellent mechanical property, has broad application prospects in energy storage field.Such as, graphene paper can when without the need to when binding agent and conductive agent as collapsible ultracapacitor energy storage material.
At present, the preparation method of graphene paper mainly contains chemical reduction method (Haiqun Chen etc., Adv. Mater., 2008,20,3557 – 3561; H. Shin etc., Adv. Funct. Mater, 2009,19,1987-1992) and hot reducing method (H. C. Schniepp etc., Journal of Physical Chemistry B, 2006,110,8535-8539; Y. Zhu etc., ACS Nano, 2010,4,1227-1233; Patent CN 101901640 A).Wherein, chemical reduction method has the potentiality of scale operation graphene paper, but conventional reductive agent is as hydrazine or sodium borohydride, has chemical toxicity or explosivity, easily causes environmental pollution and be detrimental to health.Meanwhile, due to the use of reductive agent, easily in graphene paper, impurity is mixed.Compared with chemical reduction method, hot reducing method, without the need to reductive agent, realizes removal and the reduction of graphene oxide paper surface oxygen functional group by high temperature, and reaction environment is dry and there is not the problem introducing impurity.But the reaction process of hot reducing method needs certain high temperature usually, loss and the waste of energy can be caused while heating and cooling background gas.
Plasma body, as the 4th kind of form of material, is the strong tools of a kind of energy transformation and effectively utilization.Having at present utilizes multiple plasma source to carry out redox graphene to prepare the report of Graphene.Such as: microwave plasma source (Y. Zhu etc., Carbon, 2010,48,2118-2122; Z. Li etc., Journal of Materials Chemistry, 2010,20,4781-4783; Patent CN 102107870 A; Patent CN 102139873A), radio-frequency inductance coupling plasma (Q. Wang etc., Applied Physics Letters, 2012,101) and electron beam plasma (M. Baraket etc., Carbon, 2010,48,3382-3390) etc.In order to realize higher electron mean free path to obtain the abundant acceleration of electronics, above-mentioned plasma deoxidization process needs to carry out in the environment of low pressure or vacuum usually, and this materially increases complicacy and the preparation cost of equipment.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of apparatus and method preparing graphene paper based on glow plasma positive column are provided.
The device preparing graphene paper based on glow plasma positive column comprises: chip bench, quartz socket tube, silica tube, tapered electrode, high pressure negative electricity power supply and helium source of the gas; Chip bench, quartz socket tube and tapered electrode are arranged in silica tube; Chip bench can translation in silica tube; Chip bench embeds quartz socket tube; Tapered electrode cone-tip surface is to chip bench; Tapered electrode is connected with high pressure negative electricity power supply, chip bench ground connection; Silica tube one end open, the other end is connected with helium source of the gas.
Preferably, the material of described chip bench is conducting metal or graphite.
Preferably, there is gap between described quartz socket tube and silica tube.
Preferably, the material of described tapered electrode is conducting metal.
The method preparing graphene paper based on glow plasma positive column is as follows:
1), by graphene oxide paper be placed on chip bench surface, adopt quartz socket tube to be fixed, the distance arranging graphene oxide paper and tapered electrode cone point is 6 centimetres ~ 8 centimetres.
2), open helium source of the gas, in silica tube, pass into helium, wherein helium gas flow is 1 liter/min ~ 3 liters/min, continues 10 minutes.
3), keep helium gas flow constant, open high pressure negative electricity power supply, adjustment voltage to 10 kilovolt ~ 15 kilovolts, glow discharge plasma is produced between graphene oxide paper and tapered electrode cone point, form negative glow, then translation chip bench, the distance that adjustment graphene oxide paper and tapered electrode 4 bore point is 10.8 centimetres ~ 15 centimetres, while keeping negative glow to exist between graphene oxide paper and tapered electrode cone point, form positive column.
4), keep helium gas flow and voltage constant, continuous discharge 2 seconds ~ 5 seconds.
5), close high pressure negative electricity power supply, close helium source of the gas, obtain graphene paper.
Preferably, the preparation process of oxidized graphite paper is also comprised before the process per se:
It is the vitriol oil at room temperature Homogeneous phase mixing of 98% by natural graphite and mass concentration, wherein the ratio of the vitriol oil and natural graphite is 25 milliliters: 1 gram, potassium permanganate is added under condition of ice bath, wherein the quality of potassium permanganate is 3.5 times of natural graphite, in magnetic stirring apparatus, uniform stirring 30 minutes, is heated to 35 by gained mixture
oc and in magnetic stirring apparatus uniform stirring 2 hours, add deionized water and hydrogen peroxide, wherein the ratio of deionized water and natural graphite is 100 milliliters: 1 gram, the ratio of hydrogen peroxide and natural graphite is 8 milliliters: 1 gram, gained mixed solution carries out clean, finally by vacuum drying oven 35 by whizzer
ounder C condition, drying obtains graphite oxide powder.Deionized water is added obtained graphite oxide powder, wherein the ratio of graphite oxide powder and deionized water is 0.3 milligram: 1 milliliter, graphene oxide dispersion liquid in deionized water within 2 hours, is obtained by 300 watts of supersound process, the dispersion liquid of acquisition is carried out 24 hours vacuum filtrations by the millipore filtration of 0.22 micron pore size, last seasoning in atmosphere 6 hours, obtains graphene oxide paper at microporous membrane surface.
The beneficial effect that the present invention compared with prior art has:
1) this method can realize the fast restore of graphene oxide paper in 2 seconds ~ 5 seconds, and device and process simply, possess extensive potentiality of amplifying application.
2) compared to chemical reduction method, this method without the need to adding reductive agent, to human body and environment all without potential negative impact.
3) compared to chemical reduction method, this method is carried out in dry conditions, can not introduce impurity in the product.
4) compared to hot reducing method, this method, without the need to heating, utilizes the high-energy electron in plasma body to realize the reduction of graphene oxide paper, has higher energy utilization efficiency.
5) compared to microwave plasma, radio-frequency inductance coupling plasma and electron beam plasma method of reducing, this method can be carried out in atmospheric conditions, avoids the complex appts needed for lower pressure and operating device.
Based on the above-mentioned advantage of this method, quick, environmental protection and the less energy-consumption preparation of graphene paper can be realized by this method, be conducive to promoting the widespread use of this high-quality flexible materials of graphene paper at the energy, environment and electronic applications, and can huge economic benefits be produced.
Accompanying drawing explanation
Fig. 1 is device schematic diagram of the present invention.
In figure, chip bench 1, quartz socket tube 2, silica tube 3, tapered electrode 4, high pressure negative electricity power supply 5, helium source of the gas 6, negative glow 7, positive column 8.
Graphene paper scanning electron microscope (SEM) figure that Fig. 2 obtains for the embodiment of the present invention 1.
X-ray diffraction (XRD) spectrogram of the graphene oxide paper that Fig. 3 obtains for the embodiment of the present invention 1 and graphene paper.
X-ray electronic energy (XPS) spectrogram of the graphene oxide paper that Fig. 4 obtains for the embodiment of the present invention 1 and graphene paper.
The infrared spectra (FTIR) of the graphene oxide paper that Fig. 5 obtains for the present embodiment 1 and graphene paper detects figure.
Ultraviolet-visible light (UV-Vis) spectrogram of the graphene oxide paper that Fig. 6 obtains for the present embodiment 1 and graphene paper.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
As shown in Figure 1, the device preparing graphene paper based on glow plasma positive column comprises: comprise chip bench 1, quartz socket tube 2, silica tube 3, tapered electrode 4, high pressure negative electricity power supply 5 and helium source of the gas 6; Chip bench 1, quartz socket tube 2 and tapered electrode 4 are arranged in silica tube 3; Chip bench 1 can translation in silica tube 3; Chip bench 1 embeds quartz socket tube 2, and the graphene oxide paper on chip bench 1 surface is fixed by quartz socket tube 2; Tapered electrode 4 cone-tip surface is to graphene oxide paper; Tapered electrode 4 is connected with high pressure negative electricity power supply 5, chip bench 1 ground connection; Silica tube 3 one end open, the other end is connected with helium source of the gas 6.
The material selection conducting metal of chip bench or graphite, wherein there is gap between quartz socket tube and silica tube in the material selection conducting metal of tapered electrode.
The method preparing graphene paper based on glow plasma positive column is as follows:
1), by graphene oxide paper be placed on chip bench surface, adopt quartz socket tube to be fixed, the distance arranging graphene oxide paper and tapered electrode cone point is 6 centimetres ~ 8 centimetres.
2), open helium source of the gas, in silica tube, pass into helium, wherein helium gas flow is 1 liter/min ~ 3 liters/min, continues 10 minutes.
3), keep helium gas flow constant, open high pressure negative electricity power supply, adjustment voltage to 10 kilovolt ~ 15 kilovolts, glow discharge plasma is produced between graphene oxide paper and tapered electrode cone point, form negative glow, then translation chip bench, the distance that adjustment graphene oxide paper and tapered electrode 4 bore point is 10.8 centimetres ~ 15 centimetres, while keeping negative glow to exist between graphene oxide paper and tapered electrode cone point, form positive column.
4), keep helium gas flow and voltage constant, continuous discharge 2 seconds ~ 5 seconds.
5), close high pressure negative electricity power supply, close helium source of the gas, obtain graphene paper.
Also comprise the preparation process of oxidized graphite paper before the process per se:
It is the vitriol oil at room temperature Homogeneous phase mixing of 98% by natural graphite and mass concentration, wherein the ratio of the vitriol oil and natural graphite is 25 milliliters: 1 gram, potassium permanganate is added under condition of ice bath, wherein the quality of potassium permanganate is 3.5 times of natural graphite, in magnetic stirring apparatus, uniform stirring 30 minutes, is heated to 35 by gained mixture
oc and in magnetic stirring apparatus uniform stirring 2 hours, add deionized water and hydrogen peroxide, wherein the ratio of deionized water and natural graphite is 100 milliliters: 1 gram, the ratio of hydrogen peroxide and natural graphite is 8 milliliters: 1 gram, gained mixed solution carries out clean, finally by vacuum drying oven 35 by whizzer
ounder C condition, drying obtains graphite oxide powder.Deionized water is added obtained graphite oxide powder, wherein the ratio of graphite oxide powder and deionized water is 0.3 milligram: 1 milliliter, graphene oxide dispersion liquid in deionized water within 2 hours, is obtained by 300 watts of supersound process, the dispersion liquid of acquisition is carried out 24 hours vacuum filtrations by the millipore filtration of 0.22 micron pore size, last seasoning in atmosphere 6 hours, obtains graphene oxide paper at microporous membrane surface.
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.
Embodiment 1
1. be the vitriol oil at room temperature Homogeneous phase mixing of 98% by natural graphite and mass concentration, wherein the ratio of the vitriol oil and natural graphite is 25 milliliters: 1 gram, potassium permanganate is added under condition of ice bath, wherein the quality of potassium permanganate is 3.5 times of natural graphite, in magnetic stirring apparatus, uniform stirring 30 minutes, is heated to 35 by gained mixture
oc and in magnetic stirring apparatus uniform stirring 2 hours, add deionized water and hydrogen peroxide, wherein the ratio of deionized water and natural graphite is 100 milliliters: 1 gram, the ratio of hydrogen peroxide and natural graphite is 8 milliliters: 1 gram, gained mixed solution carries out clean, finally by vacuum drying oven 35 by whizzer
ounder C condition, drying obtains graphite oxide powder.Deionized water is added obtained graphite oxide powder, wherein the ratio of graphite oxide powder and deionized water is 0.3 milligram: 1 milliliter, graphene oxide dispersion liquid in deionized water within 2 hours, is obtained by 300 watts of supersound process, the dispersion liquid of acquisition is carried out 24 hours vacuum filtrations by the millipore filtration of 0.22 micron pore size, last seasoning in atmosphere 6 hours, obtains graphene oxide paper at microporous membrane surface.
2. graphene oxide paper is placed on chip bench 1 surface, adopts quartz socket tube 2 to be fixed, namely blocked the graphene oxide paper being placed on chip bench 1 surface by quartz socket tube 2.Be arranged in silica tube 3 by chip bench 1, quartz socket tube 2 and tapered electrode 4, tapered electrode 4 cone-tip surface is to chip bench 1.Tapered electrode 4 is connected with high pressure negative electricity power supply 5.By chip bench 1 ground connection.Silica tube 3 one end open, the other end is connected with helium source of the gas 6.
3. arranging the distance that graphene oxide paper and tapered electrode 4 bore point is 6 centimetres, and open helium source of the gas 6, toward silica tube 3 in, pass into helium, wherein helium gas flow is 1 liter/min, lasting 10 minutes.Keep helium gas flow constant, open high pressure negative electricity power supply 5, adjustment voltage to 10 kilovolt, bore between point in graphene oxide paper and tapered electrode 4 and produce glow discharge plasma, form negative glow 7, then translation chip bench 1, the distance that adjustment graphene oxide paper and tapered electrode 4 bore point is 10.8 centimetres, while graphene oxide paper and tapered electrode 4 are bored and to be kept negative glow 7 to exist between point, form positive column 8.Keep helium gas flow and voltage constant, continuous discharge 2 seconds.Close high pressure negative electricity power supply 5, close helium source of the gas 6, obtain graphene paper.
By above-mentioned steps, the reduction of graphene oxide paper can be realized, obtain the flexible Flexible graphene paper of sheet.Figure 2 shows that and embody typical graphene paper appearance structure by graphene paper scanning electron microscope (SEM) figure that the embodiment of the present invention 1 obtains.Figure 3 shows that X-ray diffraction (XRD) spectrogram of the graphene oxide paper that the embodiment of the present invention 1 obtains and graphene paper.Angle corresponding to the peak value of graphene oxide paper and graphene paper is respectively 10.2 degree and 22.7 degree, and corresponding graphene layer spacing is respectively 0.87nm and 0.39nm, and the reduction of interlamellar spacing confirms the elimination of oxygenated functional group.X-ray electronic energy (XPS) spectrogram of the graphene oxide paper that Fig. 4 obtains for the embodiment of the present invention 1 and graphene paper.By reduction, the C/O atomic ratio of graphene paper is 7.6:1, is significantly higher than the 2.2:1 of graphene paper.The infrared spectra (FTIR) of the graphene oxide paper that Fig. 5 obtains for the present embodiment 1 and graphene paper detects figure.Graphene oxide paper is at 1738cm
-1, 3413cm
-1, 1383cm
-1, 1228cm
-1and 1054cm
-1there is significant characteristic peak Deng position, shown the existence of the oxygenated functional groups such as C=O, O-H, C-O, through reduction after, these characteristic peaks in the infrared spectrogram of graphene paper or disappear or intensity significantly reduce, confirm reduction effect.Ultraviolet-visible light (UV-Vis) spectrogram of the graphene oxide paper that Fig. 6 obtains for the present embodiment 1 and graphene paper.The 264nm that the wavelength that characteristic peak is corresponding moves to graphene paper from the 230nm of graphene oxide paper, confirms reduction effect.
Embodiment 2
Repeat embodiment 1, its difference is only: the distance that initial setting up graphene oxide paper and tapered electrode 4 bore point is 7 centimetres, helium gas flow is 2 liters/min, the voltage of negative electricity high pressure is 12 kilovolts, after translation chip bench 1, the distance that adjustment graphene oxide paper and tapered electrode 4 bore point is 12 centimetres, continuous discharge 3.5 seconds.By above-mentioned steps, the graphene paper that C/O atomic ratio is 5.4:1 can be obtained.
Embodiment 3
Repeat embodiment 1, its difference is only: the distance that initial setting up graphene oxide paper and tapered electrode 4 bore point is 8 centimetres, helium gas flow is 3 liters/min, the voltage of negative electricity high pressure is 15 kilovolts, after translation chip bench 1, the distance that adjustment graphene oxide paper and tapered electrode 4 bore point is 15 centimetres, continuous discharge 5 seconds.By above-mentioned steps, the graphene paper that C/O atomic ratio is 6.1:1 can be obtained.
Obviously, the above embodiment of the present invention is only in order to example of the present invention is described, but not is to embodiments of the present invention or the restriction implementing material.In fact, along with the increase of service voltage, corresponding increase interelectrode distance can obtain the atmospheric pressure glow discharge plasma with positive column, embodiment can not enumerate at this.Allly belong to the row that apparent change that technical scheme of the present invention amplifies or variation are still in protection scope of the present invention.
Claims (5)
1. prepare a method for graphene paper, the device that the method uses comprises chip bench, quartz socket tube, silica tube, tapered electrode, high pressure negative electricity power supply and helium source of the gas; Chip bench, quartz socket tube and tapered electrode are arranged in silica tube; Chip bench can translation in silica tube; Chip bench embeds quartz socket tube; Tapered electrode cone-tip surface is to chip bench; Tapered electrode is connected with high pressure negative electricity power supply, chip bench ground connection; Silica tube one end open, the other end is connected with helium source of the gas, it is characterized in that the step of the method is as follows:
1), by graphene oxide paper be placed on chip bench surface, adopt quartz socket tube to be fixed, the distance arranging graphene oxide paper and tapered electrode cone point is 6 centimetres ~ 8 centimetres;
2), open helium source of the gas, in silica tube, pass into helium, wherein helium gas flow is 1 liter/min ~ 3 liters/min, continues 10 minutes;
3), keep helium gas flow constant, open high pressure negative electricity power supply, adjustment voltage to 10 kilovolt ~ 15 kilovolts, glow discharge plasma is produced between graphene oxide paper and tapered electrode cone point, form negative glow, then translation chip bench, the distance of adjustment graphene oxide paper and tapered electrode cone point is 10.8 centimetres ~ 15 centimetres, while keeping negative glow to exist between graphene oxide paper and tapered electrode cone point, form positive column;
4), keep helium gas flow and voltage constant, continuous discharge 2 seconds ~ 5 seconds;
5), close high pressure negative electricity power supply, close helium source of the gas, obtain graphene paper.
2. method according to claim 1, is characterized in that: the preparation process of described graphene oxide paper is as follows:
It is the vitriol oil at room temperature Homogeneous phase mixing of 98% by natural graphite and mass concentration, wherein the ratio of the vitriol oil and natural graphite is 25 milliliters: 1 gram, potassium permanganate is added under condition of ice bath, wherein the quality of potassium permanganate is 3.5 times of natural graphite, in magnetic stirring apparatus, uniform stirring 30 minutes, is heated to 35 by gained mixture
oc and in magnetic stirring apparatus uniform stirring 2 hours, add deionized water and hydrogen peroxide, wherein the ratio of deionized water and natural graphite is 100 milliliters: 1 gram, the ratio of hydrogen peroxide and natural graphite is 8 milliliters: 1 gram, gained mixed solution carries out clean, finally by vacuum drying oven 35 by whizzer
ounder C condition, drying obtains graphite oxide powder; Deionized water is added obtained graphite oxide powder, wherein the ratio of graphite oxide powder and deionized water is 0.3 milligram: 1 milliliter, graphene oxide dispersion liquid in deionized water within 2 hours, is obtained by 300 watts of supersound process, the dispersion liquid of acquisition is carried out 24 hours vacuum filtrations by the millipore filtration of 0.22 micron pore size, last seasoning in atmosphere 6 hours, obtains graphene oxide paper at microporous membrane surface.
3. a kind of method preparing graphene paper according to claim 1, is characterized in that: the material of described chip bench is conducting metal or graphite.
4. a kind of method preparing graphene paper according to claim 1, is characterized in that: there is gap between described quartz socket tube and silica tube.
5. a kind of method preparing graphene paper according to claim 1, is characterized in that: the material of described tapered electrode is conducting metal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410049374.2A CN103818899B (en) | 2014-02-12 | 2014-02-12 | A kind of apparatus and method preparing graphene paper based on glow plasma positive column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410049374.2A CN103818899B (en) | 2014-02-12 | 2014-02-12 | A kind of apparatus and method preparing graphene paper based on glow plasma positive column |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103818899A CN103818899A (en) | 2014-05-28 |
| CN103818899B true CN103818899B (en) | 2015-07-29 |
Family
ID=50754239
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410049374.2A Active CN103818899B (en) | 2014-02-12 | 2014-02-12 | A kind of apparatus and method preparing graphene paper based on glow plasma positive column |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103818899B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104671237B (en) * | 2015-02-04 | 2016-08-17 | 浙江大学 | A kind of devices and methods therefor preparing graphene film based on plasma |
| CN111302337B (en) * | 2020-04-05 | 2024-04-02 | 黑龙江工业学院 | Plasma contact type graphite purifying device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203070938U (en) * | 2012-11-20 | 2013-07-17 | 浙江大学 | Device used for preparing electrode of vertical graphene double electric layer capacitor at atmospheric pressure |
| CN103420363A (en) * | 2012-05-25 | 2013-12-04 | 海洋王照明科技股份有限公司 | Preparation method and application of graphene paper |
| CN203728584U (en) * | 2014-02-12 | 2014-07-23 | 浙江大学 | Device for preparing graphene paper based on glow plasma positive column |
-
2014
- 2014-02-12 CN CN201410049374.2A patent/CN103818899B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420363A (en) * | 2012-05-25 | 2013-12-04 | 海洋王照明科技股份有限公司 | Preparation method and application of graphene paper |
| CN203070938U (en) * | 2012-11-20 | 2013-07-17 | 浙江大学 | Device used for preparing electrode of vertical graphene double electric layer capacitor at atmospheric pressure |
| CN203728584U (en) * | 2014-02-12 | 2014-07-23 | 浙江大学 | Device for preparing graphene paper based on glow plasma positive column |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103818899A (en) | 2014-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Luo et al. | Synthesis of 3D-interconnected hierarchical porous carbon from heavy fraction of bio-oil using crayfish shell as the biological template for high-performance supercapacitors | |
| Li et al. | Synthesis, modification strategies and applications of coal-based carbon materials | |
| CN106517171B (en) | A kind of preparation method of graphene aerogel | |
| CN102942177B (en) | Method for preparing graphene sheet | |
| CN104401977A (en) | Preparation method of graphene aerogel and graphene-carbon nanotube aerogel | |
| CN109292760B (en) | Method for preparing graphene | |
| CN105417521B (en) | A kind of method for preparing the classifying porous charcoal nanometer sheet of ultracapacitor fluorenyl | |
| CN107298441A (en) | A kind of method that use waste biomass material prepares super capacitor material | |
| CN103787327A (en) | One-step preparation method of hollow spherical porous graphite for supercapacitor | |
| CN103613093B (en) | A kind of hydrogen reducing prepares the method for Graphene | |
| CN110148760B (en) | Porous carbon-carbon nanotube composite material and preparation method and application thereof | |
| CN108467021B (en) | Method for preparing nano black phosphorus by stripping black phosphorus with liquid nitrogen | |
| CN107746052A (en) | A kind of preparation method of the graphene aerogel of N doping | |
| CN103539106A (en) | Preparation method of carbon material | |
| CN109225182B (en) | Ultrathin silicon nanosheet photocatalyst and preparation method and application thereof | |
| CN106629685B (en) | A kind of three-dimensional graphene foam and preparation method thereof with multilevel structure | |
| CN102009976A (en) | Method for preparing graphene film | |
| CN203728584U (en) | Device for preparing graphene paper based on glow plasma positive column | |
| CN105271170A (en) | Preparation method of nano carbon and composite material of nano carbon | |
| CN103818899B (en) | A kind of apparatus and method preparing graphene paper based on glow plasma positive column | |
| CN102897756A (en) | Preparation method of graphene | |
| CN111099588B (en) | Controllable preparation method of biomass gel-based hierarchical pore ordered three-dimensional network structure carbon material | |
| CN111204741B (en) | Preparation method of three-dimensional graphene/carbon nanotube cross-linked composite material | |
| CN111204723A (en) | Method for efficiently preparing black phosphorus microcrystal with low energy consumption | |
| CN113135558B (en) | Photothermal material based on porous carbon spheres and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |