CN203728584U - Device for preparing graphene paper based on glow plasma positive column - Google Patents
Device for preparing graphene paper based on glow plasma positive column Download PDFInfo
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- CN203728584U CN203728584U CN201420063297.1U CN201420063297U CN203728584U CN 203728584 U CN203728584 U CN 203728584U CN 201420063297 U CN201420063297 U CN 201420063297U CN 203728584 U CN203728584 U CN 203728584U
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- graphene
- substrate table
- positive column
- chip bench
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 80
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000010453 quartz Substances 0.000 claims abstract description 26
- 239000001307 helium Substances 0.000 claims description 22
- 229910052734 helium Inorganic materials 0.000 claims description 22
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 21
- 239000000377 silicon dioxide Substances 0.000 claims description 20
- 230000005611 electricity Effects 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 15
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 230000003321 amplification Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract 7
- 210000002381 plasma Anatomy 0.000 abstract 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 12
- 230000009467 reduction Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229910021382 natural graphite Inorganic materials 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 231100000045 chemical toxicity Toxicity 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The utility model discloses a device for preparing graphene paper based on a glow plasma positive column. The device comprises a substrate table, a quartz sleeve, a quartz tube, a conical electrode, a high-voltage negative power supply and a helium-gas gas source, wherein the substrate table, the quartz sleeve and the conical electrode are arranged in the quartz tube; the substrate table can horizontally move in the quartz tube; the substrate table is embedded into the quartz sleeve; the conical tip surface of the conical electrode faces towards the substrate table; the conical electrode is connected with the high-voltage negative power supply; the substrate table is grounded; one end of the quartz tube is open, and the other end of the quartz tube is connected with the helium-gas gas source. In a preparation process, the graphene oxide paper is fixed on the substrate table, and glow discharge plasmas with a positive column are formed between the graphene oxide paper and the conical electrode by virtue of high voltage. The device disclosed by the utility model can realize rapid preparation of the graphene paper under the normal pressure, is simple in arrangement and process, environmental friendly, and high in energy utilization rate, has large-scale amplification application potential, and is beneficial to promoting the graphene paper to be widely applied in a plurality of fields.
Description
Technical field
The utility model belongs to plasma body and nano material preparing technical field, relates in particular to a kind of device 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 powerful tool 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 purpose of this utility model is to overcome the deficiencies in the prior art, and a kind of device of preparing Graphene paper based on glow plasma positive column is 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 beneficial effect that the utility model compared with prior art has:
1) this device can be realized 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 device is without adding reductive agent, to human body and environment all without potential negative impact.
3), than chemical reduction method, this device carries out under drying conditions, can in product, not introduce impurity.
4) than hot reducing method, this installs 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 device can carry out under condition of normal pressure, has avoided low pressure condition required complex appts and operating device.
Brief description of the drawings
Fig. 1 is device schematic diagram of the present utility model.
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 utility model embodiment 1.
The graphene oxide paper that Fig. 3 obtains for the utility model embodiment 1 and X-ray diffraction (XRD) spectrogram of Graphene paper.
The graphene oxide paper that Fig. 4 obtains for the utility model embodiment 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 utility model is described in further detail.
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.
Below in conjunction with specific embodiment, the utility model is further elaborated, but the utility model 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 utility model embodiment 1 obtains, embody typical Graphene paper appearance structure.Figure 3 shows that graphene oxide paper that the utility model embodiment 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 utility model embodiment 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.
Embodiment 2
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.
Embodiment 3
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, above-described embodiment of the present utility model is only for the utility model example is described, but not is the restriction to embodiment of the present utility model 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 domain of the present utility model of variation that the technical solution of the utility model amplifies.
Claims (4)
1. the 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. the 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. the 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. the 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420063297.1U CN203728584U (en) | 2014-02-12 | 2014-02-12 | Device for preparing graphene paper based on glow plasma positive column |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420063297.1U CN203728584U (en) | 2014-02-12 | 2014-02-12 | Device for preparing graphene paper based on glow plasma positive column |
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| Publication Number | Publication Date |
|---|---|
| CN203728584U true CN203728584U (en) | 2014-07-23 |
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| CN201420063297.1U Expired - Lifetime CN203728584U (en) | 2014-02-12 | 2014-02-12 | Device for preparing graphene paper based on glow plasma positive column |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818899A (en) * | 2014-02-12 | 2014-05-28 | 浙江大学 | Device and method for preparing graphene paper based on glow plasma positive column area |
| CN104671237A (en) * | 2015-02-04 | 2015-06-03 | 浙江大学 | Device and method for preparing graphene film on basis of plasma |
| CN113003567A (en) * | 2021-05-06 | 2021-06-22 | 哈尔滨工程大学 | Device and method for reducing graphene oxide |
-
2014
- 2014-02-12 CN CN201420063297.1U patent/CN203728584U/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818899A (en) * | 2014-02-12 | 2014-05-28 | 浙江大学 | Device and method for preparing graphene paper based on glow plasma positive column area |
| CN103818899B (en) * | 2014-02-12 | 2015-07-29 | 浙江大学 | A kind of apparatus and method preparing graphene paper based on glow plasma positive column |
| CN104671237A (en) * | 2015-02-04 | 2015-06-03 | 浙江大学 | Device and method for preparing graphene film on basis of plasma |
| CN113003567A (en) * | 2021-05-06 | 2021-06-22 | 哈尔滨工程大学 | Device and method for reducing graphene oxide |
| CN113003567B (en) * | 2021-05-06 | 2022-12-13 | 哈尔滨工程大学 | Device and method for reducing graphene oxide |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20140723 |