CN115636408B - Preparation method of graphene oxide - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 57
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 46
- 239000010439 graphite Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000007800 oxidant agent Substances 0.000 claims abstract description 24
- 230000001590 oxidative effect Effects 0.000 claims abstract description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 9
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 description 27
- 230000003647 oxidation Effects 0.000 description 22
- 238000009830 intercalation Methods 0.000 description 13
- 230000002687 intercalation Effects 0.000 description 13
- 239000000047 product Substances 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000000879 optical micrograph Methods 0.000 description 5
- -1 3 Chemical class 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 229920006337 unsaturated polyester resin Polymers 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
Abstract
The scheme discloses a preparation method of graphene oxide, which comprises the following steps: mixing graphite with concentrated sulfuric acid to obtain a mixture A, adding an expanding agent into the mixture A, vacuumizing, and reacting under a vacuum condition to obtain a mixture B; adding an oxidant into the mixture B, heating and vacuumizing, and reacting under a vacuum condition to obtain a mixture C; and carrying out suction filtration on the mixture C, and washing to obtain graphene oxide. The method accelerates the reaction rate through a vacuumizing process, reduces the consumption of the oxidant, and simultaneously prepares the graphene oxide with high stripping and large size.
Description
Technical Field
The invention relates to the technical field of two-dimensional material preparation, in particular to a preparation method of graphene oxide.
Background
Today, graphene oxide has demonstrated advantages in various fields, such as biomedical, flexible conductive films, liquid crystal optical materials, energy storage materials, and the like, and has been widely used. Increasing the lateral dimensions of graphene oxide can improve the related mechanics and liquid crystal performance of a macroscopic assembly structure assembled by graphene oxide sheets, and the market hopes to prepare large-sized graphene oxide because of the advantages of few nodes, few edge contacts, high orientation and the like. However, the graphene oxide produced in large scale is still prepared by adopting the traditional Hummers method, adding a large amount of potassium permanganate after premixing graphite and concentrated sulfuric acid, and respectively carrying out medium-temperature oxidation and hydration reaction. Longer oxidation times and larger amounts of oxidizing agent ensure stripping effects, but introduce more defect sites. Through the hydration and washing processes, the transverse size of the graphene oxide is greatly reduced under the action of water molecules and mechanical force, and the performance of a rear-end product is seriously affected. In addition, the use of a large amount of oxidizing agent causes not only an increase in the cost of use and post-treatment but also a problem of environmental pollution. Therefore, development of a preparation method of graphene oxide with low cost, high stripping and large size is urgently needed.
Graphene having a size of more than 50 μm is generally called large-sized graphene, and large-sized graphite is required as a raw material when large-sized graphene oxide is prepared by Hummers method. In CN113860295 'preparation of graphene oxide by large-particle-size crystalline flake graphite', large-particle-size graphite with the particle size of 45-325 μm is adopted, firstly, pre-intercalation is carried out on the large-particle-size crystalline flake graphite with concentrated sulfuric acid and hydrogen peroxide to obtain expanded graphite, the expanded graphite is added into a mixed acid solution of the concentrated sulfuric acid and phosphoric acid for protection reaction, and then the large-size graphene oxide is prepared through oxidation reaction and hydration stages. However, the use and discharge of phosphoric acid causes environmental pollution problems and increases the use and purification costs. In order to make the preparation method relatively green and environment-friendly, the CN107140632 'a preparation method of large-size graphene oxide sheets with high mechanical strength' adopts large-size crystalline flake graphite as a raw material, and prepares large-size graphene oxide by adding potassium persulfate and performing ultrasonic-assisted intercalation reaction. Although the oxidation and stripping efficiency is high, the method involves ultrasonic assistance, and the reduction of the size of graphene oxide to a certain extent is unavoidable. In order to introduce a new method for accelerating the reaction rate, in CN111925637 'a rapid curing unsaturated polyester resin for vacuum introduction', a compound accelerator E1 and the unsaturated polyester resin are introduced into a forming die for curing reaction under the condition of a vacuumizing process, so that the curing reaction rate between systems is greatly accelerated, bubbles in the reaction process are eliminated, the demolding time is shortened, and the cost is saved.
Disclosure of Invention
One purpose of the scheme is to provide a preparation method of graphene oxide, which accelerates the reaction rate through a vacuumizing process, reduces the consumption of an oxidant, and simultaneously prepares high-stripping large-size graphene oxide.
In order to achieve the above purpose, the scheme is as follows:
a method for preparing graphene oxide, comprising the following steps:
mixing graphite with concentrated sulfuric acid to obtain a mixture A, adding an expanding agent into the mixture A, vacuumizing, and reacting under a vacuum condition to obtain a mixture B;
adding an oxidant into the mixture B, heating and vacuumizing, and reacting under a vacuum condition to obtain a mixture C;
and carrying out suction filtration on the mixture C, and washing to obtain graphene oxide.
Preferably, the reaction temperature when the graphite is mixed with concentrated sulfuric acid to obtain the mixture A is 10-15 ℃.
Preferably, the mixture A is vacuumized after adding the expanding agent to reach a vacuum degree of-0.07 MPa to-0.1 MPa.
Preferably, in the step of reacting under vacuum to obtain the mixture B, the reaction time is 0.8-1.5 h; the reaction temperature is 15-20 ℃.
Preferably, the method further comprises: after the mixture B is obtained, the temperature of the mixture B is reduced to 0-5 ℃, and then an oxidant is added.
Preferably, in the step of reacting under vacuum to obtain the mixture C, the reaction time is 1.5 to 2.2 hours.
Preferably, the graphite is any one of flake graphite and expanded graphite, the mass percentage of carbon in the graphite is 95-99.99 wt%, and the particle size of the graphite is 50-200 meshes.
Preferably, the expanding agent is persulfate, the persulfate comprises one or two of sodium persulfate and potassium persulfate, and the dosage of the expanding agent is 5.0-8.0 times of that of graphite.
Preferably, the oxidant is potassium permanganate, and the dosage of the oxidant is 1.5-2.0 times of that of graphite.
The beneficial effects of this scheme are as follows:
1. the amount of the oxidant required by the traditional Hummers method is generally 4.0 times of that of graphite, compared with the traditional Hummers method, the amount of the oxidant used by the method is 2.0 times of that of the graphite, and the amount of the oxidant is reduced by 50%.
2. The length of the primary oxidation section in the traditional Hummers method needs to be reacted for 4 hours, and the method reduces the oxidation time to 2 hours through a vacuumizing process, so that the energy consumption and the cost are saved.
3. The average size of the graphene oxide prepared by the method is 90 mu m (D50), and the graphene oxide has the characteristics of uniformity and large size.
Drawings
In order to more clearly illustrate the practice of the present solution, the drawings that are required for the description of the embodiments will be briefly described below, it being apparent that the drawings in the following description are only some embodiments of the present solution and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an optical microscope image of graphene oxide prepared in example 1;
FIG. 2 is an optical microscope image of graphene oxide prepared in example 2;
FIG. 3 is an optical microscope image of graphene oxide prepared in example 3;
FIG. 4 is an optical microscope image of graphene oxide prepared in example 4;
FIG. 5 is an optical microscope image of graphene oxide prepared in example 5;
fig. 6 is a graph of the results of particle size analysis (see D50 particle size data).
Detailed Description
Embodiments of the present solution are described in further detail below. It is clear that the described embodiments are only some of the embodiments of the present solution, not an exhaustive list of all embodiments. It should be noted that, in the case of no conflict, the embodiments and features in the embodiments in the present solution may be combined with each other.
The stage1 state in the present application is a state in which an intercalator is present between all 2 adjacent graphene sheets.
Since the conventional Hummers method for preparing graphene oxide requires a large amount of oxidant to be added in the oxidation stage, the oxidation time is long. Excessive oxidation and crushing of the product are caused, and the transverse dimension of the graphene oxide is greatly reduced. The small-size graphene oxide not only reduces the yield of finished products, but also can influence the electric conductivity and the heat conductivity of the graphene.
The inventor of the application proposes that vacuum treatment processes are adopted in the pre-intercalation stage and the oxidation stage respectively, and because of the influence of vacuum degree, the interlayer spacing of the crystalline flake graphite is only more compact and attached, but the persulfate has chemical reaction under a concentrated acid system.
The inventor adopts vacuum-pumping technology in Hummers system in pre-intercalation stage and oxidation stage to prepare graphene oxide with low oxidation and large size.
Because the persulfate generates hydrogen sulfate and oxygen in a concentrated sulfuric acid system in the pre-intercalation stage, the removal of the oxygen can be accelerated by vacuumizing, the generated hydrogen sulfate is beneficial to forming graphitized intercalation in a stage1 state while the reaction rate is accelerated, the reaction is shown in a formula 1,
2S 2 O 8 2- +2H 2 O→4HSO 4 - +O 2 ∈ (reaction under concentrated acid environment) (1)
The vacuumizing process can promote the diffusion of the oxidant (high manganese anhydride) between layers during the oxidation stage, so that the utilization rate of the oxidant is improved, and the size reduction caused by long-time oxidation and stirring is avoided.
The reaction mechanism of the oxidation stage is shown in the formulas 2 and 3:
KMnO 4 +3H 2 SO 4 →k + +MnO 3 + +H 3 O + +3HSO 4 - (2)
MnO 3 + +MnO 4 - →Mn 2 O 7 (high manganese anhydride) (3)
According to the method, through carrying out vacuum reaction in the oxidation stage, the reaction rate can be increased, the reaction time can be shortened, meanwhile, the diffusion of the oxidant between graphite layers can be promoted, and the stripping and large-size characteristics of the graphene oxide are ensured while the consumption of the oxidant is small.
The method provided by the application reduces the oxidant consumption by 50% and the sulfuric acid consumption by 30% compared with the original Hummers method by adding a vacuumizing process in the pre-intercalation and oxidation stages. And the long preparation time of the original Hummers method and the possible influence of long-time mechanical force on the prepared graphene oxide size and the increased cost and energy consumption caused by using excessive oxidant are avoided.
The present application is illustrated by the following specific examples.
Example 1
Graphene oxide was prepared using a conventional Hummers method comprising the steps of:
1. premixing flake graphite with 100-150 meshes and concentrated sulfuric acid in a reaction kettle to obtain a mixture A, wherein the temperature is set to be 10 ℃;
2. slowly adding potassium permanganate with the dosage of 4.0 times of graphite into the mixture A in the step 1, slowly heating to 35 ℃, and oxidizing for 4 hours to obtain a mixture B;
3. and (3) slowly adding deionized water into the mixture B in the step (2), and then carrying out a suction filtration washing process to prepare the graphene oxide.
The prepared graphene oxide is placed under an optical microscope, the characterization is shown in fig. 1, a large number of thick sheets of the graphene oxide can be observed, the particle size is small, and the average size (D50) of the prepared product is about 20 mu m by measuring with a nanometer particle sizer.
Example 2
A preparation method of graphene oxide with low oxidation and large size, which comprises the following steps:
1. premixing flake graphite with 100-150 meshes and concentrated sulfuric acid in a reaction kettle to obtain a mixture A, wherein the temperature is set to be 10 ℃;
2. adding sodium persulfate with the dosage of 5.0 times of graphite into the mixture A in the step 1 to obtain a mixture B, carrying out vacuum reaction (vacuum degree-0.07 MPa) and keeping the temperature at 15 ℃ for intercalation time of 1h;
3. slowly adding potassium permanganate with the dosage of 2.0 times of graphite into the mixture B in the step 2 after releasing the vacuum to obtain a mixture C, slowly heating to 35 ℃, and continuously vacuumizing (the vacuum degree is-0.07 MPa) for oxidation reaction for 2 hours;
4. and (3) slowly adding deionized water into the mixture C in the step (3) after releasing vacuum, and carrying out a suction filtration washing process to prepare the graphene oxide.
The prepared graphene oxide is placed under an optical microscope, the characterization is shown in fig. 2, the size of the graphene oxide prepared by adding the pre-intercalation stage and vacuumizing reaction is obviously increased, and the average size (D50) of the prepared product measured by a nano-particle sizer is 75 mu m.
Example 3
A preparation method of graphene oxide with low oxidation, large size and high efficiency comprises the following steps:
1. premixing flake graphite with 100-150 meshes and concentrated sulfuric acid in a reaction kettle to obtain a mixture A, wherein the temperature is set to be 10 ℃;
2. adding potassium persulfate with the dosage of 5.0 times of graphite into the mixture A in the step 1 to obtain a mixture B, carrying out vacuum reaction (vacuum degree-0.1 MPa) and keeping the temperature at 15 ℃ for intercalation time of 1h;
3. slowly adding potassium permanganate with the dosage of 2.0 times of graphite into the mixture B in the step 2 after releasing the vacuum to obtain a mixture C, slowly heating to 35 ℃, and continuously vacuumizing (vacuum degree-0.1 MPa) for oxidation reaction for 2 hours;
4. and (3) slowly adding deionized water into the mixture C in the step (3) after releasing vacuum, and carrying out a suction filtration washing process to prepare the graphene oxide.
The prepared graphene oxide is placed under an optical microscope, the characterization is shown in fig. 3, after the vacuum degree is increased, the size of the prepared graphene oxide is further increased, and the average size (D50) of the prepared product is 85 μm as measured by a nano-particle sizer.
Example 4
A preparation method of graphene oxide with low oxidation, large size and high efficiency comprises the following steps:
1. premixing flake graphite with 100-150 meshes and concentrated sulfuric acid in a reaction kettle to obtain a mixture A, wherein the temperature is set to be 10 ℃;
2. adding potassium persulfate with the dosage of 8.0 times of graphite into the mixture A in the step 1 to obtain a mixture B, carrying out vacuum reaction (vacuum degree-0.1 MPa) and keeping the temperature at 15 ℃ for intercalation time of 1h;
3. slowly adding 1.5 times of graphite potassium permanganate into the mixture B in the step 2 after releasing the vacuum to obtain a mixture C, slowly heating to 35 ℃, and continuously vacuumizing (vacuum degree-0.1 MPa) for oxidation reaction for 2 hours;
4. and (3) slowly adding deionized water into the mixture C in the step (3) after releasing vacuum, and carrying out a suction filtration washing process to prepare the graphene oxide.
The prepared graphene oxide is placed under an optical microscope, the characterization is shown in fig. 4, the purposes of reducing cost can be achieved by further increasing the consumption of persulfate and reducing the consumption of potassium permanganate, and the dimensional change is found to be basically small. The average size (D50) of the product obtained was 88. Mu.m, as measured by a nanoparticle sizer.
Example 5
A preparation method of graphene oxide with low oxidation, large size and high efficiency comprises the following steps:
1. placing 100-150 mesh expandable graphite and concentrated sulfuric acid into a reaction kettle for premixing to obtain a mixture A, and setting the temperature to be 10 ℃;
2. adding potassium persulfate with the dosage of 8.0 times of graphite into the mixture A in the step 1 to obtain a mixture B, carrying out vacuum reaction (vacuum degree-0.1 MPa) and keeping the temperature at 15 ℃ for intercalation time of 1h;
3. slowly adding 1.5 times of graphite potassium permanganate into the mixture B in the step 2 after releasing the vacuum to obtain a mixture C, slowly heating to 35 ℃, and continuously vacuumizing (vacuum degree-0.1 MPa) for oxidation reaction for 2 hours;
4. and (3) slowly adding deionized water into the mixture C in the step (3) after releasing vacuum, and carrying out a suction filtration washing process to prepare the graphene oxide.
The prepared graphene oxide is placed under an optical microscope, the characterization is shown in fig. 5, and the stripping effect of the graphene oxide is better after the graphite raw material is replaced. The average size (D50) of the resulting product was 90um as measured by a nanoparticle sizer.
Compared with the prior art, the method can reduce the consumption of the oxidant and shorten the oxidation time through the vacuum pumping process in the pre-intercalation and oxidation stage, thereby obtaining the graphene oxide with large size and high stripping.
It should be understood that the foregoing examples of the present invention are provided merely for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention, and that various other changes and modifications may be made therein by one skilled in the art without departing from the spirit and scope of the present invention as defined by the appended claims.
Claims (8)
1. The preparation method of the graphene oxide is characterized by comprising the following steps of:
mixing graphite with concentrated sulfuric acid to obtain a mixture A, adding an expanding agent into the mixture A, vacuumizing, and reacting under vacuum condition to obtain a mixture B, wherein the vacuum degree is-0.07 MPa to-0.1 MPa, and the reaction temperature is 15-20 ℃;
adding an oxidant into the mixture B, heating and vacuumizing, and reacting under the vacuum condition to obtain a mixture C, wherein the vacuum degree is-0.07 MPa to-0.1 MPa;
and carrying out suction filtration on the mixture C, and washing to obtain graphene oxide.
2. The process according to claim 1, wherein the reaction temperature when the graphite is mixed with concentrated sulfuric acid to obtain the mixture a is 10 ℃ to 15 ℃.
3. The process according to claim 1, wherein the reaction time in the step of reacting under vacuum to obtain the mixture B is 0.8 to 1.5 hours.
4. The method of manufacturing according to claim 1, characterized in that the method further comprises:
after the mixture B is obtained, the temperature of the mixture B is reduced to 0-5 ℃, and then an oxidant is added.
5. The process according to claim 1, wherein the reaction time in the step of reacting under vacuum to obtain the mixture C is 1.5 to 2.2 hours.
6. The method according to claim 1, wherein the graphite is either of flake graphite and expanded graphite, the mass percentage of carbon in the graphite is 95 to 99.99wt%, and the particle size of the graphite is 50 to 200 mesh.
7. The method according to claim 1, wherein the expanding agent is persulfate, the persulfate comprises one or both of sodium persulfate and potassium persulfate, and the amount of the expanding agent is 5.0 to 8.0 times that of graphite.
8. The method according to claim 1, wherein the oxidizing agent is potassium permanganate, and the amount of the oxidizing agent is 1.5 to 2.0 times that of graphite.
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| CN101935035A (en) * | 2010-09-02 | 2011-01-05 | 中国科学院宁波材料技术与工程研究所 | Ultra-low temperature thermal expansion preparation method of high specific area graphene |
| CN102502611A (en) * | 2011-11-15 | 2012-06-20 | 东南大学 | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides |
| CN105197918A (en) * | 2015-10-12 | 2015-12-30 | 湖北工业大学 | High-quality graphene and quick preparation method thereof |
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| CN101935035A (en) * | 2010-09-02 | 2011-01-05 | 中国科学院宁波材料技术与工程研究所 | Ultra-low temperature thermal expansion preparation method of high specific area graphene |
| CN102502611A (en) * | 2011-11-15 | 2012-06-20 | 东南大学 | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides |
| CN105197918A (en) * | 2015-10-12 | 2015-12-30 | 湖北工业大学 | High-quality graphene and quick preparation method thereof |
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