CN106744873B - A kind of method of quick preparation small size graphene - Google Patents
A kind of method of quick preparation small size graphene Download PDFInfo
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- CN106744873B CN106744873B CN201611096485.4A CN201611096485A CN106744873B CN 106744873 B CN106744873 B CN 106744873B CN 201611096485 A CN201611096485 A CN 201611096485A CN 106744873 B CN106744873 B CN 106744873B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 155
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 89
- 239000010439 graphite Substances 0.000 claims abstract description 89
- 239000002245 particle Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract 2
- 238000003698 laser cutting Methods 0.000 claims abstract 2
- 238000003825 pressing Methods 0.000 claims abstract 2
- 238000005520 cutting process Methods 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- 230000002687 intercalation Effects 0.000 claims description 7
- 238000009830 intercalation Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 4
- 230000001629 suppression Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 238000009826 distribution Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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Abstract
一种快速制备小尺寸石墨烯的方法，本发明涉及一种制备小尺寸石墨烯的方法。本发明要解决现有小尺寸石墨烯的制备困难，生产成本高，污染环境严重的问题。方法：一、制备膨胀石墨；二、压制；三、激光切割；四、分散及干燥，得到粒径小于1μm的石墨烯。本发明用于一种快速制备小尺寸石墨烯的方法。
A method for rapidly preparing small-sized graphene, the present invention relates to a method for preparing small-sized graphene. The invention solves the problems of difficulty in preparation of existing small-sized graphene, high production cost and serious environmental pollution. Methods: 1. preparing expanded graphite; 2. pressing; 3. laser cutting; 4. dispersing and drying to obtain graphene with a particle size of less than 1 μm. The present invention is used for a method for rapidly preparing small-sized graphene.
Description
Technical field
The present invention relates to a kind of methods for preparing small size graphene.
Background technique
Graphene is referred to as " king of new material ", has ultra-thin, high-intensitive, high-termal conductivity, high conductivity, good light permeability
Etc. characteristics.Only one carbon atom thickness, is nature most thin material, stable structure, and intensity is higher by than best steel
Hundred times or more, thermal coefficient is up to 5300W/mk, is higher than carbon nanotube and diamond.Resistivity ratio copper or silver are lower, in the world
The smallest material of resistivity, translucency are up to 97.7%, almost light transmission.The method for preparing graphene at present mainly has chemical oxidation
Reduction method, vapour deposition process, liquid phase stripping method.Though chemistry redox method can realize prepared by magnanimity, due to caused by oxidation
Defect can not be restored completely, influence its electric conductivity.The graphene quality of vapour deposition process preparation is higher, but condition is more severe
It carves, higher cost, is not suitable for large-scale production.Liquid phase stripping method can be by graphite dispersion into specific solvent or surface-active
Energy in agent by ultrasonic wave prepares single-layer or multi-layer graphene, but dispersing agent subsequent processing is difficult.Above method preparation
Graphene size is both greater than 5 μm or more, and preparation graphene of the size less than 1 μm is highly difficult.Small size graphene synthetic fibers,
Antistatic material, electromagnetic wave absorption electrically conductive ink and battery conductive agent etc. have broad application prospects.
Summary of the invention
The invention solves the preparation of existing small size graphene difficulty, high production cost pollutes the serious problem of environment,
And provide a kind of method of quickly preparation small size graphene.
A kind of method of quick preparation small size graphene follows the steps below:
One, expanded graphite is prepared:
Using natural flake graphite as raw material, using chemical method intercalation, expansion, high magnification numbe expanded graphite is prepared；
The expansion multiple of the high magnification numbe expanded graphite is 200 times~500 times；
Two, it suppresses:
High magnification numbe expanded graphite is suppressed, the karbate impervious graphite with a thickness of 3mm~5mm is obtained；
Three, it is cut by laser:
Thickness direction using laser along karbate impervious graphite is cut, and cutting spacing is 1 μm~2 μm, after being cut
Graphite powder；
Four, disperse and dry:
Graphite powder after cutting is subjected to ultrasonic disperse, freeze-drying, obtains graphene of the partial size less than 1 μm.
Beneficial effects of the present invention:
It prepares in the method for graphene now, the graphene size of preparation prepares size less than 1 μm all at 5 μm or more
Graphene complex process.Advantage of the invention is that preparation method is environmentally protective, simple process, quality is stablized.First with
The expanded graphite of preparation is pressed into certain thickness graphite paper, and graphite paper has certain intensity, at this moment under vacuum using sharp
The high-energy of light cuts graphite paper, and maintains a certain distance, and weakens the Van der Waals force between the graphite flake cut down,
At this moment cavitation is carried out with ultrasonic wave again, removes graphite flake.
A kind of method of the present invention for quickly preparation small size graphene.
Detailed description of the invention
Fig. 1 is that graphene high-resolution of the partial size less than 1 μm prepared by embodiment one transmits photo；
Fig. 2 is graphene particle size distribution figure of the partial size less than 1 μm prepared by embodiment one.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it
Between any combination.
Specific embodiment 1: one kind described in present embodiment quickly preparation small size graphene method be according to
What lower step carried out:
One, expanded graphite is prepared:
Using natural flake graphite as raw material, using chemical method intercalation, expansion, high magnification numbe expanded graphite is prepared；
The expansion multiple of the high magnification numbe expanded graphite is 200 times~500 times；
Two, it suppresses:
High magnification numbe expanded graphite is suppressed, the karbate impervious graphite with a thickness of 3mm~5mm is obtained；
Three, it is cut by laser:
Thickness direction using laser along karbate impervious graphite is cut, and cutting spacing is 1 μm~2 μm, after being cut
Graphite powder；
Four, disperse and dry:
Graphite powder after cutting is subjected to ultrasonic disperse, freeze-drying, obtains graphene of the partial size less than 1 μm.
Present embodiment the utility model has the advantages that
It prepares in the method for graphene now, the graphene size of preparation prepares size less than 1 μm all at 5 μm or more
Graphene complex process.The advantage of present embodiment is that preparation method is environmentally protective, simple process, and quality is stablized.
It is pressed into certain thickness graphite paper first with the expanded graphite of preparation, graphite paper has certain intensity, at this moment in vacuum
The lower high-energy using laser cuts graphite paper, and maintains a certain distance, and makes the Van der Waals between the graphite flake cut down
Power weakens, and at this moment carries out cavitation with ultrasonic wave again, removes graphite flake.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: dispersion described in step 4
The dispersing agent used is deionized water.It is other same as the specific embodiment one.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two: institute in step 1
The partial size for the natural flake graphite stated is 50 mesh~300 mesh.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: institute in step 1
The expansion multiple for the high magnification numbe expanded graphite stated is 200 times.It is other identical as specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: institute in step 1
The expansion multiple for the high magnification numbe expanded graphite stated is 200 times~300 times.It is other identical as specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: in institute's step 1
The expansion multiple for the high magnification numbe expanded graphite stated is 300 times~400 times.It is other identical as specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: institute in step 1
The expansion multiple for the high magnification numbe expanded graphite stated is 400 times~500 times.It is other identical as specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: will in step 2
High magnification numbe expanded graphite is suppressed, and the karbate impervious graphite with a thickness of 2mm is obtained.It is other identical as specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: will be in step 2
High magnification numbe expanded graphite is suppressed, and the karbate impervious graphite with a thickness of 3mm is obtained.It is other identical as specific embodiment one to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine: will in step 2
High magnification numbe expanded graphite is suppressed, and the karbate impervious graphite with a thickness of 4mm is obtained.It is other identical as specific embodiment one to nine.
Specific embodiment 11: unlike one of present embodiment and specific embodiment one to ten: by high magnification numbe
Expanded graphite is suppressed, and the karbate impervious graphite with a thickness of 5mm is obtained.It is other identical as specific embodiment one to ten.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
The method that one kind described in the present embodiment quickly prepares small size graphene follows the steps below:
One, expanded graphite is prepared:
Using natural flake graphite as raw material, using chemical method intercalation, expansion, high magnification numbe expanded graphite is prepared；
The expansion multiple of the high magnification numbe expanded graphite is 200 times；
Two, it suppresses:
High magnification numbe expanded graphite is suppressed, the karbate impervious graphite with a thickness of 2mm is obtained；
Three, it is cut by laser:
Thickness direction using laser along karbate impervious graphite is cut, and cutting spacing is 1 μm~2 μm, after being cut
Graphite powder；
Four, disperse and dry:
Graphite powder after cutting is subjected to ultrasonic disperse, freeze-drying, obtains graphene of the partial size less than 1 μm；
The dispersing agent for dispersing to use described in step 4 is deionized water；
The partial size of natural flake graphite described in step 1 is 300 mesh.
Embodiment two:
The method that one kind described in the present embodiment quickly prepares small size graphene follows the steps below:
One, expanded graphite is prepared:
Using natural flake graphite as raw material, using chemical method intercalation, expansion, high magnification numbe expanded graphite is prepared；
The expansion multiple of the high magnification numbe expanded graphite is 200 times~300 times；
Two, it suppresses:
High magnification numbe expanded graphite is suppressed, the karbate impervious graphite with a thickness of 3mm is obtained；
Three, it is cut by laser:
Thickness direction using laser along karbate impervious graphite is cut, and cutting spacing is 1 μm~2 μm, after being cut
Graphite powder；
Four, disperse and dry:
Graphite powder after cutting is subjected to ultrasonic disperse, freeze-drying, obtains graphene of the partial size less than 1 μm；
The dispersing agent for dispersing to use described in step 4 is deionized water；
The partial size of natural flake graphite described in step 1 is 200 mesh.
Embodiment three:
The method that one kind described in the present embodiment quickly prepares small size graphene follows the steps below:
One, expanded graphite is prepared:
Using natural flake graphite as raw material, using chemical method intercalation, expansion, high magnification numbe expanded graphite is prepared；
The expansion multiple of the high magnification numbe expanded graphite is 300 times~400 times；
Two, it suppresses:
High magnification numbe expanded graphite is suppressed, the karbate impervious graphite with a thickness of 4mm is obtained；
Three, it is cut by laser:
Thickness direction using laser along karbate impervious graphite is cut, and cutting spacing is 1 μm~2 μm, after being cut
Graphite powder；
Four, disperse and dry:
Graphite powder after cutting is subjected to ultrasonic disperse, freeze-drying, obtains graphene of the partial size less than 1 μm；
The dispersing agent for dispersing to use described in step 4 is deionized water；
The partial size of natural flake graphite described in step 1 is 100 mesh.
Example IV:
The method that one kind described in the present embodiment quickly prepares small size graphene follows the steps below:
One, expanded graphite is prepared:
Using natural flake graphite as raw material, using chemical method intercalation, expansion, high magnification numbe expanded graphite is prepared；
The expansion multiple of the high magnification numbe expanded graphite is 400 times~500 times；
Two, it suppresses:
High magnification numbe expanded graphite is suppressed, the karbate impervious graphite with a thickness of 5mm is obtained；
Three, it is cut by laser:
Thickness direction using laser along karbate impervious graphite is cut, and cutting spacing is 1 μm~2 μm, after being cut
Graphite powder；
Four, disperse and dry:
Graphite powder after cutting is subjected to ultrasonic disperse, freeze-drying, obtains graphene of the partial size less than 1 μm；
The dispersing agent for dispersing to use described in step 4 is deionized water；
The partial size of natural flake graphite described in step 1 is 50 mesh~80 mesh.
Fig. 1 is that graphene high-resolution of the partial size less than 1 μm prepared by embodiment one transmits photo；As seen from the figure, graphene
The number of plies be 1-2 layers.
Fig. 2 is graphene particle size distribution figure of the partial size less than 1 μm prepared by embodiment one.For granularity corresponding to Fig. 2
Distribution table is as shown in table 1.By Fig. 2 and table 1 it is found that graphene size manufactured in the present embodiment is less than 1 μm, accumulation ratio is close
100%.
Table 1
Claims (7)
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318878A (en) * | 2013-06-27 | 2013-09-25 | 江南石墨烯研究院 | Preparation method and application of large size and shape ratio graphene microsheet |
| CN103601179A (en) * | 2013-11-19 | 2014-02-26 | 厦门凯纳石墨烯技术有限公司 | Preparation method of size controllable graphene nanoplatelets |
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| JP6195109B2 (en) * | 2013-11-22 | 2017-09-13 | 東海カーボン株式会社 | Method for producing graphene dispersion and method for producing graphene thin film |
| WO2015089142A1 (en) * | 2013-12-11 | 2015-06-18 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | Sub-micron laser patterning of graphene and 2d materials |
| KR102097292B1 (en) * | 2015-01-27 | 2020-04-06 | 한국전자통신연구원 | Method of fabricating electrode and capacitor comprising the electrode formed thereby |
| KR20160096374A (en) * | 2015-02-05 | 2016-08-16 | 이성균 | Layered Liquid Phase Pulsed Laser Ablation - Graphene, Phosphorus Manufacturing Method. |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318878A (en) * | 2013-06-27 | 2013-09-25 | 江南石墨烯研究院 | Preparation method and application of large size and shape ratio graphene microsheet |
| CN103601179A (en) * | 2013-11-19 | 2014-02-26 | 厦门凯纳石墨烯技术有限公司 | Preparation method of size controllable graphene nanoplatelets |
Non-Patent Citations (3)
| Title |
|---|
| Femtosecond laser induced micropatterning of graphene film;Golap Kalita et al;《Materials Letters》;20110224;第65卷;全文 |
| Microstructuring of Graphene Oxide Nanosheets Using Direct Laser Writing;Yong Zhou et al;《Advanced Materials》;20090903;第22卷;全文 |
| Nanoscale patterning of grapheme through femtosecond laser ablatin;R.Sahin et al;《Applied Physics Letters》;20140207;第104卷(第5期);第1页左栏第1段、右栏第3-4段 |
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