CN205328621U - Supersound and electric field synergism peel off device of graphite alkene fast - Google Patents
Supersound and electric field synergism peel off device of graphite alkene fast Download PDFInfo
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- CN205328621U CN205328621U CN201521138354.9U CN201521138354U CN205328621U CN 205328621 U CN205328621 U CN 205328621U CN 201521138354 U CN201521138354 U CN 201521138354U CN 205328621 U CN205328621 U CN 205328621U
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- graphite
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- graphite alkene
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- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 72
- 239000010439 graphite Substances 0.000 title claims abstract description 72
- 230000005684 electric field Effects 0.000 title claims abstract description 21
- -1 graphite alkene Chemical class 0.000 title abstract 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 115
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000003792 electrolyte Substances 0.000 claims abstract description 9
- 230000002195 synergetic effect Effects 0.000 claims description 14
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000004108 freeze drying Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 3
- 239000000138 intercalating agent Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000033116 oxidation-reduction process Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 description 2
- 235000011151 potassium sulphates Nutrition 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 229920005372 Plexiglas® Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The utility model provides a method of supersound and electric field synergism peel off device of graphite alkene fast, it relates to the device of peeling off graphite alkene fast, and it will solve current preparation graphite alkene the problem of the various defects of existence. The device is including ultrasonic device, graphite positive electrode, graphite negative electrode and container. The utility model discloses a high purity graphite piece or graphite cake are as the positive and negative electrode, and at the synergism of supersound with the electric field, the intercalator in the electrolyte gets into the surface that makes graphite alkene follow graphite block in the graphite electrode and peels off fast to the graphite alkene of peeling off is followed in further broken separation in the electrode. It obtains thin layer graphene to collect graphite alkene powder post -filtration, washing and freeze drying to the homogeneity and the dispersibility of graphite alkene are good. The utility model discloses a supersound and electric field synergism peel off device of graphite alkene fast, low to the facility request, device configuration is simple, and is with low costs, and the productivity is high, the industrialization production of being convenient for. The utility model discloses a preparation graphite alkene can be peeled off fast to the device under supersound and electric field are cooperateed with.
Description
Technical field
This utility model relates to the device of a kind of quick stripping Graphene。
Background technology
Graphene has the mechanical property of excellence, heat conductivility, electric conductivity and optical property, and in addition, Graphene also has the magnetic performance of excellence, (theoretical value reaches 2630m to the specific surface area of superelevation2/ g) and absorption property etc.。
Geim et al. by stick with adhesive tape the two sides of graphite flake carry out stickily tear repeatedly make graphite flake peel off and obtain Graphene。This technique is simple, and the Graphene quality prepared is higher, but the graphene sheet layer that the method is prepared is smaller, yields poorly, and is not suitable for large-scale production, is only applicable to Basic Experiment Study。CVD is to be positioned in the atmosphere of hydrocarbon gas to heat metallic matrix, Pintsch process generates carbon atom, and be deposited on metallic matrix and form Graphene, remove metallic matrix finally by chemical attack and obtain graphene film, CVD is generally adopted " etched the matrix method " and obtains Graphene, not only complicated process of preparation, waste resource, increase production cost, and contaminated environment, therefore how realizing the lossless transfer of growing substrate of Graphene, making matrix can be recycled is that CVD produces a Graphene difficult problem urgently to be resolved hurrily。Native graphite and strong acid and oxidizing species are reacted generation graphite oxide (GO) by oxidation-reduction method, graphene oxide (mono-layer graphite oxide) is prepared into through ultrasonic disperse, add reducing agent and remove the oxy radical on graphite oxide surface, such as carboxyl, epoxy radicals and hydroxyl, obtain Graphene。Oxidation-reduction method can prepare substantial amounts of Graphene with relatively low cost, becomes the most effective method preparing Graphene at present。But, adopt the Graphene that oxidation-reduction method produces, owing to being subject to the destruction of strong acid and strong oxidizer in intercalation process, easily and inevitably resulted in a large amount of defects of Graphene crystal structure, even if after strong reductant reducing agent, the prototype structure of Graphene can not be recovered completely, and be very easy to irreversible agglomeration, result in the excellent properties such as the specific surface area of Graphene and due high conductivity, high-termal conductivity, high light transmittance to have a greatly reduced quality, thus limit the Graphene application at energy storage field and accurate microelectronic etc.。The more important thing is, due to the use of strong acid and strong oxidizer, strong reductant etc., produce substantial amounts of waste liquid and waste gas, can cause serious environmental pollution in Graphene preparation process, this can bring the environmental protection cost of costliness to Producer。Epitaxial growth method is under fine vacuum and hot conditions, and heating SiC single crystal makes silicon atom evaporate, and remaining carbon atom carries out rearranging of structure in surface of SiC and obtains Graphene。The Graphene quality that epitaxial growth method is prepared is higher, but to be the working condition of Graphene strict for the shortcoming of the method, equipment requirements is higher, it is necessary to higher vacuum, adds production cost, and productivity is relatively low。And, during using SiC as substrate, the interaction of Graphene and SiC can affect the quality of Graphene。Therefore, epitaxial growth method is unfavorable for large-scale production Graphene。
Summary of the invention
This utility model is to solve the above-mentioned method preparing Graphene to there is the problem of various defect, and a kind of ultrasonic device quickly peeling off Graphene with electric field synergistic effect provided。
A kind of ultrasonic device quickly peeling off Graphene with electric field synergistic effect, it includes Vltrasonic device, graphite anelectrode, graphite negative electrode and container;Electrolyte filled by described container;Described Vltrasonic device, graphite anelectrode and graphite negative electrode are placed in container;Described Vltrasonic device is placed in the centre position of graphite anelectrode and graphite negative electrode。
This utility model adopts graphite block or graphite cake as positive and negative electrode, positive and negative electrode is placed in electrolyte solution, between positive and negative electrode, apply voltage and be controlled with voltage cyclelog, between graphite electrode, insert Vltrasonic device simultaneously, the cavitation effect that ultrasound wave produces accelerates the stripping effect of graphite block body, at the ultrasonic synergism with electric field, intercalator in electrolyte enters in graphite electrode and makes Graphene quickly peel off from the surface of graphite block body, and the broken apart Graphene peeled off from electrode further。Collect filter after Graphene powder, washing and lyophilization obtain thin graphene, and the uniformity of Graphene and favorable dispersibility。
The ultrasonic device quickly peeling off Graphene with electric field synergistic effect of this utility model, low for equipment requirements, device configuration is simple, and cost is low, and productivity is high, it is simple to industrialization produces。
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the ultrasonic device quickly peeling off Graphene with electric field synergistic effect in this utility model, and wherein 1 represents that Vltrasonic device, 2-1 represent that graphite anelectrode, 2-2 represent graphite negative electrode, 3 expression containers, 4 expression tanks, 5 expression voltage procedures controllers。
Detailed description of the invention
Detailed description of the invention one: shown in Fig. 1, a kind of ultrasonic device quickly peeling off Graphene with electric field synergistic effect, it includes Vltrasonic device 1, graphite anelectrode 2-1, graphite negative electrode 2-2 and container 3;Electrolyte filled by described container 3;Described Vltrasonic device 1, graphite anelectrode 2-1 and graphite negative electrode 2-2 are placed in container 3;Described Vltrasonic device 1 is placed on the sidewall of container 3。
Detailed description of the invention two: present embodiment and detailed description of the invention one the difference is that, described container 3 is plexiglass box。Other is identical with detailed description of the invention one。
Detailed description of the invention three: present embodiment and detailed description of the invention one the difference is that, described container 3 is placed in tank 4, and fills cooling water in tank 4。Other is identical with detailed description of the invention one。
Detailed description of the invention four: present embodiment and detailed description of the invention one the difference is that, described graphite anelectrode 2-1 is connected to the positive pole of voltage procedures controller 5, and described graphite negative electrode 2-2 is connected to the negative pole of voltage procedures controller 5。Other is identical with detailed description of the invention one。
Detailed description of the invention five: present embodiment and detailed description of the invention one the difference is that, what graphite anelectrode 2-1 and graphite negative electrode 2-2 adopted is quality purity is graphite block or the graphite cake of 85%-99.99%。Other is identical with detailed description of the invention one。
Detailed description of the invention six: present embodiment and detailed description of the invention one the difference is that, the spacing of graphite anelectrode 2-1 and graphite negative electrode 2-2 is 30~60mm。Other is identical with detailed description of the invention one。
Detailed description of the invention seven: present embodiment and detailed description of the invention one the difference is that, described electrolyte be in potassium sulfate solution, metabisulfite solution, dilute sulfuric acid, NaOH solution, KOH solution a kind of several arbitrarily than forming。Other is identical with detailed description of the invention one。
Detailed description of the invention eight: present embodiment and detailed description of the invention seven the difference is that, the mass percent concentration of described potassium sulfate solution is 10%~40%;The mass percent concentration of metabisulfite solution is 10%~40%;The mass percent concentration of dilute sulfuric acid is 5%~30%;The mass percent concentration of NaOH solution is 10%~20%;The mass percent concentration of KOH solution is 10%~20%。Other is identical with detailed description of the invention seven。
Adopt following example checking the beneficial effects of the utility model:
Embodiment:
Shown in Fig. 1, utilize and ultrasonic quickly peel off the method that the device of Graphene quickly peels off Graphene with electric field synergistic effect, sequentially include the following steps:
One, adopting the ultrasonic device quickly peeling off Graphene with electric field synergistic effect, fill cooling water in tank 4, Vltrasonic device 1, graphite anelectrode 2-1 and graphite negative electrode 2-2 are placed in container 3 and fill electrolyte, open voltage procedures controller 5;
Two, Vltrasonic device 1 applies ultrasound wave, controls the forward voltage of graphite anelectrode 2-1 and the backward voltage of graphite negative electrode 2-2 by voltage procedures controller 5 simultaneously, and the forward voltage time is 10min, and the backward voltage time is 20min;
Three, when voltage is zero, reaction terminates, filter electrolyte and collect precipitation, through washing and after lyophilization, obtaining Graphene, namely complete to utilize the ultrasonic device quickly peeling off Graphene with electric field synergistic effect quickly to peel off Graphene。
What in the present embodiment step one, graphite anelectrode 2-1 and graphite negative electrode 2-2 adopted is quality purity is the graphite block of more than 99.9%。In step one, the spacing of graphite anelectrode 2-1 and graphite negative electrode 2-2 is 30mm。In step one, electrolyte is mass percent concentration is the dilute sulfuric acid of 15%。Applying hyperacoustic frequency in step one is 20KHz, and ultrasonic power is 2KW。Step 2 applies between graphite anelectrode 2-1 and graphite negative electrode 2-2 5V voltage。
At the ultrasonic synergism with electric field in the present embodiment, Graphene is quickly peeled off from the surface of graphite electrode, and the broken apart Graphene peeled off from electrode further, and the productivity of Graphene is up to 99.8%, and uniformity and favorable dispersibility。
Claims (5)
1. the ultrasonic device quickly peeling off Graphene with electric field synergistic effect, it is characterised in that it includes Vltrasonic device (1), graphite anelectrode (2-1), graphite negative electrode (2-2) and container (3);Described container fills electrolyte in (3);Described Vltrasonic device (1), graphite anelectrode (2-1) and graphite negative electrode (2-2) are placed in container (3);Described Vltrasonic device (1) is placed on the sidewall of container (3)。
2. a kind of ultrasonic device quickly peeling off Graphene with electric field synergistic effect according to claim 1, it is characterised in that described container (3) is placed in tank (4), and fills cooling water in tank (4)。
3. a kind of ultrasonic device quickly peeling off Graphene with electric field synergistic effect according to claim 1, described graphite anelectrode (2-1) is connected to the positive pole of voltage procedures controller (5), and described graphite negative electrode (2-2) is connected to the negative pole of voltage procedures controller (5)。
4. a kind of ultrasonic device quickly peeling off Graphene with electric field synergistic effect according to claim 1, it is characterised in that what graphite anelectrode (2-1) and graphite negative electrode (2-2) adopted is quality purity is graphite block or the graphite cake of 85%-99.99%。
5. a kind of ultrasonic device quickly peeling off Graphene with electric field synergistic effect according to claim 1, it is characterised in that the spacing of graphite anelectrode (2-1) and graphite negative electrode (2-2) is 30~60mm。
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CN201521138354.9U CN205328621U (en) | 2015-12-31 | 2015-12-31 | Supersound and electric field synergism peel off device of graphite alkene fast |
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CN201521138354.9U CN205328621U (en) | 2015-12-31 | 2015-12-31 | Supersound and electric field synergism peel off device of graphite alkene fast |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107032336A (en) * | 2017-06-16 | 2017-08-11 | 成都新柯力化工科技有限公司 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
CN110698924A (en) * | 2019-10-14 | 2020-01-17 | 北京石墨烯技术研究院有限公司 | Graphene slurry, conductive ink and preparation method thereof |
-
2015
- 2015-12-31 CN CN201521138354.9U patent/CN205328621U/en active Active
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107032336A (en) * | 2017-06-16 | 2017-08-11 | 成都新柯力化工科技有限公司 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
CN107032336B (en) * | 2017-06-16 | 2018-03-13 | 成都新柯力化工科技有限公司 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
CN110698924A (en) * | 2019-10-14 | 2020-01-17 | 北京石墨烯技术研究院有限公司 | Graphene slurry, conductive ink and preparation method thereof |
CN110698924B (en) * | 2019-10-14 | 2022-08-09 | 北京石墨烯技术研究院有限公司 | Graphene slurry, conductive ink and preparation method thereof |
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Effective date of registration: 20170504 Address after: 154603 Heilongjiang city of Qitaihe Province New District baotailong Road No. 16 Patentee after: Qitaihe baotailong graphene New Material Co Ltd Address before: 154603 Heilongjiang city of Qitaihe Province New District baotailong Road No. 16 Co-patentee before: Ma Qing Patentee before: Jiao Yun |
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TR01 | Transfer of patent right |