CN103818899A - Device and method for preparing graphene paper based on glow plasma positive column area - Google Patents
Device and method for preparing graphene paper based on glow plasma positive column area Download PDFInfo
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- CN103818899A CN103818899A CN201410049374.2A CN201410049374A CN103818899A CN 103818899 A CN103818899 A CN 103818899A CN 201410049374 A CN201410049374 A CN 201410049374A CN 103818899 A CN103818899 A CN 103818899A
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Abstract
The invention discloses a device and a method for preparing graphene paper based on a glow plasma positive column area. The device comprises a substrate platform, a quartz sleeve, a quartz tube, a conical electrode, a high-voltage negative power supply and a helium source, wherein the substrate platform, the quartz sleeve and the conical electrode are arranged in the quartz tube; the substrate platform can move horizontally in the quartz tube; the substrate platform is embedded into the quartz sleeve; the conical tip of the conical electrode faces the substrate platform; the conical electrode is connected with the high-voltage negative power supply; the substrate platform is grounded; one end of the quartz tube is open; the other end of the quartz tube is connected with the helium source. In a preparation process, oxidized graphene paper is fixed onto the substrate platform, and glow discharge plasmas with positive column areas are formed between the oxidized graphene paper and the conical electrode by high voltage. By the method and the device, the graphene paper can be prepared quickly under normal pressure; the device and the process are simple, environment-friendly, high in energy utilization rate, and favorable for promoting the wide application of the graphene paper in fields, and have the potential of enlarging application in large scales.
Description
Technical field
The invention belongs to plasma body and nano material preparing technical field, relate in particular to a kind of apparatus and method of preparing Graphene paper based on glow plasma positive column.
Background technology
Graphene is a kind of by sp
2the two-dimensional nano material that hydridization carbon atom is arranged with hexagonal lattice, since 2004 find first, has caused very big 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 good mechanical property, has broad application prospects in stored energy field.For example, Graphene paper can be as collapsible ultracapacitor energy storage material without binding agent and conductive agent in the situation that.
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 is detrimental to health.Meanwhile, due to the use of reductive agent, easily in Graphene paper, mix impurity.Compared with chemical reduction method, hot reducing method, without reductive agent, is realized removal and the reduction of graphene oxide paper surface oxygen functional group by high temperature, and reaction environment is dried and does not exist the problem of introducing impurity.But the reaction process of hot reducing method needs certain high temperature conventionally, can cause loss and the waste of energy in heating and cooling background gas.
Plasma body, as the 4th kind of form of material, is a kind of energy transformation and effective strong tools of utilizing.Have and utilize multiple plasma source to carry out the report that redox graphene is prepared Graphene at present.For example: 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 body (M. Baraket etc., Carbon, 2010,48,3382-3390) etc.In order to realize the abundant acceleration of higher electron mean free path with electron gain, above-mentioned plasma deoxidization process need to be carried out conventionally in the environment of low pressure or vacuum, and this has increased complicacy and the preparation cost of equipment to a great extent.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of apparatus and method of preparing Graphene paper based on glow plasma positive column are provided.
The device of 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 opening, the other end is connected with helium source of the gas.
Preferably, the material of described chip bench is conducting metal or graphite.
Preferably, between described quartz socket tube and silica tube, there is gap.
Preferably, the material of described tapered electrode is conducting metal.
The method of preparing Graphene paper based on glow plasma positive column is as follows:
1), graphene oxide paper is placed on to chip bench surface, adopt quartz socket tube to be fixed, graphene oxide paper and tapered electrode are set, and to bore sharp distance be 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, continue 10 minutes.
3), keep helium gas flow constant, open high pressure negative electricity power supply, adjust voltage to 10 kilovolt ~ 15 kilovolts, between graphene oxide paper and tapered electrode cone point, produce glow discharge plasma, form negative glow, then translation chip bench, it is 10.8 centimetres ~ 15 centimetres that adjustment graphene oxide paper and tapered electrode 4 are bored sharp distance, in keeping negative glow to exist, form positive column between graphene oxide paper and tapered electrode cone point.
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, before the method, also comprise the preparation process of oxidized graphite paper:
The vitriol oil that is 98% by natural graphite and mass concentration at room temperature evenly mixes, wherein the ratio of the vitriol oil and natural graphite is 25 milliliters: 1 gram, under condition of ice bath, add potassium permanganate, 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 by whizzer, finally by vacuum drying oven 35
othe dry graphite oxide powder that obtains under C condition.Deionized water is added to obtained graphite oxide powder, wherein the ratio of graphite oxide powder and deionized water is 0.3 milligram: 1 milliliter, within 2 hours, obtain the dispersion liquid of graphene oxide in deionized water by 300 watts of supersound process, the dispersion liquid of acquisition is carried out to 24 hours vacuum filtrations by the millipore filtration of 0.22 micron pore size, finally seasoning 6 hours in air, 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 are simple, possessed the potentiality of extensive amplification application.
2), than chemical reduction method, this method is without adding reductive agent, to human body and environment all without potential negative impact.
3) than chemical reduction method, this method is carried out under drying conditions, can in product, not introduce impurity.
4) than hot reducing method, this method is without heating, utilizes high-energy electron in plasma body to realize the reduction of graphene oxide paper, has higher energy utilization efficiency.
5) than microwave plasma, radio-frequency inductance coupling plasma and electron beam plasma deoxidization method, this method can be carried out under condition of normal pressure, has avoided low pressure condition required complex appts and operating device.
Based on the above-mentioned advantage of this method, by this method can realize Graphene paper fast, environmental protection and less energy-consumption preparation, be conducive to promote the widespread use of this high-quality flexible materials of Graphene paper at the energy, environment and electronic applications, and can produce huge economic benefits.
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.
The graphene oxide paper that Fig. 3 obtains for the embodiment of the present invention 1 and X-ray diffraction (XRD) spectrogram of Graphene paper.
The graphene oxide paper that Fig. 4 obtains for the embodiment of the present invention 1 and X-ray electronic energy (XPS) spectrogram of Graphene paper.
The graphene oxide paper that Fig. 5 obtains for the present embodiment 1 and the infrared spectra (FTIR) of Graphene paper detect figure.
The graphene oxide paper that Fig. 6 obtains for the present embodiment 1 and ultraviolet-visible light (UV-Vis) spectrogram of Graphene paper.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
As shown in Figure 1, the device of 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 be in the interior translation of 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 surfaces are 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 openings, the other end is connected with helium source of the gas 6.
Material selection conducting metal or the graphite of chip bench,, wherein there is gap between quartz socket tube and silica tube in the material selection conducting metal of tapered electrode.
The method of preparing Graphene paper based on glow plasma positive column is as follows:
1), graphene oxide paper is placed on to chip bench surface, adopt quartz socket tube to be fixed, graphene oxide paper and tapered electrode are set, and to bore sharp distance be 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, continue 10 minutes.
3), keep helium gas flow constant, open high pressure negative electricity power supply, adjust voltage to 10 kilovolt ~ 15 kilovolts, between graphene oxide paper and tapered electrode cone point, produce glow discharge plasma, form negative glow, then translation chip bench, it is 10.8 centimetres ~ 15 centimetres that adjustment graphene oxide paper and tapered electrode 4 are bored sharp distance, in keeping negative glow to exist, form positive column between graphene oxide paper and tapered electrode cone point.
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.
Before the method, also comprise the preparation process of oxidized graphite paper:
The vitriol oil that is 98% by natural graphite and mass concentration at room temperature evenly mixes, wherein the ratio of the vitriol oil and natural graphite is 25 milliliters: 1 gram, under condition of ice bath, add potassium permanganate, 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 by whizzer, finally by vacuum drying oven 35
othe dry graphite oxide powder that obtains under C condition.Deionized water is added to obtained graphite oxide powder, wherein the ratio of graphite oxide powder and deionized water is 0.3 milligram: 1 milliliter, within 2 hours, obtain the dispersion liquid of graphene oxide in deionized water by 300 watts of supersound process, the dispersion liquid of acquisition is carried out to 24 hours vacuum filtrations by the millipore filtration of 0.22 micron pore size, finally seasoning 6 hours in air, 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. the vitriol oil that is 98% by natural graphite and mass concentration at room temperature evenly mixes, wherein the ratio of the vitriol oil and natural graphite is 25 milliliters: 1 gram, under condition of ice bath, add potassium permanganate, 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 by whizzer, finally by vacuum drying oven 35
othe dry graphite oxide powder that obtains under C condition.Deionized water is added to obtained graphite oxide powder, wherein the ratio of graphite oxide powder and deionized water is 0.3 milligram: 1 milliliter, within 2 hours, obtain the dispersion liquid of graphene oxide in deionized water by 300 watts of supersound process, the dispersion liquid of acquisition is carried out to 24 hours vacuum filtrations by the millipore filtration of 0.22 micron pore size, finally seasoning 6 hours in air, obtains graphene oxide paper at microporous membrane surface.
2. graphene oxide paper is placed on to chip bench 1 surface, adopts quartz socket tube 2 to be fixed, block by quartz socket tube 2 the graphene oxide paper that is placed on chip bench 1 surface.Chip bench 1, quartz socket tube 2 and tapered electrode 4 are arranged in silica tube 3, and tapered electrode 4 cone-tip surfaces are 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 openings, the other end is connected with helium source of the gas 6.
3. graphene oxide paper and tapered electrode 4 are set, and to bore sharp distance be 6 centimetres, opens helium source of the gas 6, in silica tube 3, passes into helium, and wherein helium gas flow is 1 liter/min, continues 10 minutes.Keep helium gas flow constant, open high pressure negative electricity power supply 5, adjust voltage to 10 kilovolt, bore and between point, produce glow discharge plasma at graphene oxide paper and tapered electrode 4, form negative glow 7, then translation chip bench 1, it is 10.8 centimetres that adjustment graphene oxide paper and tapered electrode 4 are bored sharp distance, when graphene oxide paper and tapered electrode 4 are bored and 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, can realize the reduction of graphene oxide paper, obtain the flexible soft graphite alkene of sheet paper.Figure 2 shows that Graphene paper scanning electron microscope (SEM) figure that the embodiment of the present invention 1 obtains, embody typical Graphene paper appearance structure.Figure 3 shows that graphene oxide paper that the embodiment of the present invention 1 obtains and X-ray diffraction (XRD) spectrogram of Graphene paper.The peak value institute corresponding angle 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, the elimination that reduces to have confirmed oxygenated functional group of interlamellar spacing.The graphene oxide paper that Fig. 4 obtains for the embodiment of the present invention 1 and X-ray electronic energy (XPS) spectrogram of 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 graphene oxide paper that Fig. 5 obtains for the present embodiment 1 and the infrared spectra (FTIR) of Graphene paper detect 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, after reduction, these characteristic peaks in the infrared spectrogram of Graphene paper or disappearance or intensity significantly reduce, confirmed reduction effect.The graphene oxide paper that Fig. 6 obtains for the present embodiment 1 and ultraviolet-visible light (UV-Vis) spectrogram of Graphene paper.The 264nm that the wavelength that characteristic peak is corresponding moves to Graphene paper from the 230nm of graphene oxide paper, has confirmed reduction effect.
Repeat embodiment 1, its difference is only: it is 7 centimetres that initial setting up graphene oxide paper and tapered electrode 4 are bored sharp distance, helium gas flow is 2 liters/min, the voltage of negative electricity high pressure is 12 kilovolts, after translation chip bench 1, it is 12 centimetres that adjustment graphene oxide paper and tapered electrode 4 are bored sharp distance, continuous discharge 3.5 seconds.By above-mentioned steps, can obtain C/O atomic ratio is the Graphene paper of 5.4:1.
Repeat embodiment 1, its difference is only: it is 8 centimetres that initial setting up graphene oxide paper and tapered electrode 4 are bored sharp distance, helium gas flow is 3 liters/min, the voltage of negative electricity high pressure is 15 kilovolts, after translation chip bench 1, it is 15 centimetres that adjustment graphene oxide paper and tapered electrode 4 are bored sharp distance, continuous discharge 5 seconds.By above-mentioned steps, can obtain C/O atomic ratio is the Graphene paper of 6.1:1.
Obviously, the above embodiment of the present invention is only for example of the present invention is described, but not is the restriction to embodiments of the present invention or enforcement material.In fact, along with the increase of service voltage, can corresponding increase interelectrode distance obtain the atmospheric pressure glow discharge plasma with positive column, embodiment can not enumerate at this.Allly belong to apparent variation or the still row in protection scope of the present invention of variation that technical scheme of the present invention amplifies.
Claims (6)
1. a device of preparing Graphene paper based on glow plasma positive column, is characterized in that: comprise 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 opening, the other end is connected with helium source of the gas.
2. a kind of device of preparing Graphene paper based on glow plasma positive column according to claim 1, is characterized in that: the material of described chip bench is conducting metal or graphite.
3. a kind of device of preparing Graphene paper based on glow plasma positive column according to claim 1, is characterized in that: between described quartz socket tube and silica tube, have gap.
4. a kind of device of preparing Graphene paper based on glow plasma positive column according to claim 1, is characterized in that: the material of described tapered electrode is conducting metal.
5. prepare a method for Graphene paper, use device as claimed in claim 1, it is characterized in that its step is as follows:
1), graphene oxide paper is placed on to chip bench surface, adopt quartz socket tube to be fixed, graphene oxide paper and tapered electrode are set, and to bore sharp distance be 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, continue 10 minutes;
3), keep helium gas flow constant, open high pressure negative electricity power supply, adjust voltage to 10 kilovolt ~ 15 kilovolts, between graphene oxide paper and tapered electrode cone point, produce glow discharge plasma, form negative glow, then translation chip bench, it is 10.8 centimetres ~ 15 centimetres that adjustment graphene oxide paper and tapered electrode are bored sharp distance, in keeping negative glow to exist, form positive column between graphene oxide paper and tapered electrode cone point;
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.
6. method according to claim 5, is characterized in that: the preparation process of described oxidized graphite paper is as follows:
The vitriol oil that is 98% by natural graphite and mass concentration at room temperature evenly mixes, wherein the ratio of the vitriol oil and natural graphite is 25 milliliters: 1 gram, under condition of ice bath, add potassium permanganate, 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 by whizzer, finally by vacuum drying oven 35
oCthe dry graphite oxide powder that obtains under condition; Deionized water is added to obtained graphite oxide powder, wherein the ratio of graphite oxide powder and deionized water is 0.3 milligram: 1 milliliter, within 2 hours, obtain the dispersion liquid of graphene oxide in deionized water by 300 watts of supersound process, the dispersion liquid of acquisition is carried out to 24 hours vacuum filtrations by the millipore filtration of 0.22 micron pore size, finally seasoning 6 hours in air, obtains graphene oxide paper at microporous membrane surface.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104671237A (en) * | 2015-02-04 | 2015-06-03 | 浙江大学 | Device and method for preparing graphene film on basis of plasma |
| CN111302337A (en) * | 2020-04-05 | 2020-06-19 | 黑龙江工业学院 | Plasma contact type graphite purification device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104671237A (en) * | 2015-02-04 | 2015-06-03 | 浙江大学 | Device and method for preparing graphene film on basis of plasma |
| CN111302337A (en) * | 2020-04-05 | 2020-06-19 | 黑龙江工业学院 | Plasma contact type graphite purification device |
| CN111302337B (en) * | 2020-04-05 | 2024-04-02 | 黑龙江工业学院 | Plasma contact type graphite purifying device |
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