CN102180461A - Preparation method of superconductive, thermally-conductive, ultrahigh-strength graphene composite film - Google Patents
Preparation method of superconductive, thermally-conductive, ultrahigh-strength graphene composite film Download PDFInfo
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- CN102180461A CN102180461A CN2011100273058A CN201110027305A CN102180461A CN 102180461 A CN102180461 A CN 102180461A CN 2011100273058 A CN2011100273058 A CN 2011100273058A CN 201110027305 A CN201110027305 A CN 201110027305A CN 102180461 A CN102180461 A CN 102180461A
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Abstract
The invention relates to a preparation method of a superconductive, thermally-conductive, ultrahigh-strength graphene composite film, which comprises the following steps: step 1, mixing 10%-80% by mass of nanometer graphene and 20%-90% by mass of liquid or powdery bridging carbon groups in a nitrogen-filling mixer at room temperature for 1-10 hours; step 2, pumping the mixed materials into a heating box by a vacuum pump, heating the materials to 100-500 DEG C for 1-20 hours; step 3, after heating, allowing the mixed materials to fall freely into a material distribution zone, uniformly spreading out the mixed materials by a scraper and a material-distributing roller, feeding the materials into a pre-press roller with a controlled pressure of 0.1-1.0 Mpa, pressing the materials tightly with several groups of press rollers so as to pull out a composite film with a thickness less than 100 microns; step 4, scanning the composite film line by line through a laser beam, an electron beam or an ion beam to allow the temperature of the scanned part of the composite film to be above 3000 DEG C so as to realize carbonization, graphitization, crystal growth, and the perfect combination of the molecular skeleton of nanometer graphene and the molecular skeleton of the bridging carbon groups; step 5, trimming the scanned composite film and rolling up. The invention has simple and compact steps, and can realize production with high efficiency by one continuous apparatus.
Description
Technical field
The present invention relates to the preparation method of a kind of superconduction, heat conduction, superstrength Graphene laminated film.
Background technology
Since single-layer graphene was successfully prepared in the laboratory, Graphene became the research focus in nano science field rapidly from Britain scientist in 2004.Graphene has the monolayer carbon atomic thickness, is a kind of novel carbonaceous material that bi-dimensional cellular shape crystalline network is arranged by carbon atom, is the essentially consist unit of every other dimension carbonaceous material.Its thickness has only 0.335nm, only be 200,000 of hair/, can be bundled into the soccerballene of zero dimension, be curled into the unidimensional carbon nanotube, be piled into three-dimensional graphite.
The appearance of Graphene has caused global research boom.It is not only in the known materials the thinnest a kind of, also very firmly hard; As simple substance, it is all faster than known conductor that it at room temperature transmits the speed of electronics.Graphene structure on atomic scale is very special, must just can describe with relativity quantum physics (relativistic quantumphysics).
Graphene-structured is highly stable, and up to now, the investigator does not find to have in the Graphene situation of carbon atom disappearance yet.Connection in the Graphene between each carbon atom is very pliable and tough, and when applying external mechanical force, the carbon atom face adapts to external force with regard to flexural deformation thereby carbon atom needn't be rearranged, and has also just kept Stability Analysis of Structures.
This stable crystalline network makes carbon atom have outstanding electroconductibility.Electronics in the Graphene when mobile, can or do not introduced foreign atom because of lattice imperfection scattering takes place in track.Because reactive force is very strong between atom, at normal temperatures, even carbon atom telescopes on every side, the interference that electronics is subjected in the Graphene is also very little.
Graphene has good mechanical, electricity, thermal property.It has highly stable structure.Each carbon atom is perfect in the Graphene lamella arranges, and when being subjected to external force, carbon atom can flexural deformation, need not rearrange, and has kept its structural stability.On the Graphene plane, the arrangement of carbon atom makes it very firmly hard, and tensile strength can reach 50-200GPa, and Young's modulus can reach 1TPa, is the material of preparing in the world at present with high specific strength.
Summary of the invention
The objective of the invention is to propose the preparation method of a kind of superconduction, heat conduction, superstrength Graphene laminated film.
Carboxylic-acid, amine, isocyanates, carbonyl class, hydroxy kind organic substance chemical property are active, the reaction of can building bridge, the present invention uses nano-graphene to mix with liquid or powder bridge formation carbon-based material, prepared a kind of superconduction, heat conduction, superstrength Graphene laminated film, its preparation methods steps is:
Fs mixes, and mass percent 10%-80% nano-graphene and 20%-90% liquid or powder bridge formation carbon back are put into mixing equipment respectively, charges into nitrogen protection then in this mixing equipment, at room temperature mixes 1-10 hour;
The subordinate phase heating is drawn onto mixed material in the heating container by vacuum pump through the mixing equipment baiting valve, behind reinforced the finishing, starts electrically heated., Heating temperature 100-500 ℃, 1-20 hour heat-up time;
The phase III film forming, the feed opening that will pass through heating container through the mixture of heating freely falls to the cloth district, then by scraper plate, distribute roll is evenly spread compound out, through transport tape mixture is delivered in the pony press, a control pressure 1-10 normal atmosphere is sent to next group pressure roller compacting through the graphite carbon base-material of precompressed through pressure roller, mixture through being compacted into film reaches final compression roll more successively, and mixture is suppressed the laminated film of thickness less than 0.1mm;
Quadravalence section scanning calorimeter is built bridge and is reacted, laminated film is sent to scanning area through compression roll, with laser beam, electron beam or ionic fluid laminated film is lined by line scan, the temperature that makes laminated film be scanned the position is higher than 3000 ℃, to realize carbonization, greying, long brilliant, build bridge and react, make the molecule frame perfect adaptation of the molecule frame and the bridge formation carbon back of nano-graphene, become superconduction, heat conduction, superstrength Graphene laminated film;
The five-stage rolling will be cut edge the back by the wrap-up rolling through the laminated film after the scanning, and wrap-up is installed the photoelectric error correction device in advance, to guarantee the planeness of rolling end face.
In above-mentioned preparation method, described liquid or powder bridge formation carbon back are at least two kinds in amine, carboxylic-acid, isocyanates, carbonyl class, the hydroxy kind organic substance, and ratio is the mole proportioning of reaction.
In above-mentioned preparation method, heating, film forming, the waste gas in scanning calorimeter bridge formation each stage of reaction are concentrated emission treatment through the off gas treatment pipeline by induced draft fan.
Preparation method's of the present invention outstanding advantage is: technology is simple, condition control easily, and realize dexterously building bridge between graphene molecules frame and carbon back molecule frame with energy-beam scanning energy regenerative form and react, good mechanical, electricity, thermal property that Graphene is had self are embodied in preparation method's of the present invention product one laminated film preferably.
Embodiment
Embodiment one:
The 100g nano-graphene is added that 900g mole proportioning is the loading hopper that 1: 1 quadrol and acetic acid are put into Graphene laminated film continuous machine respectively, in ribbon mixer, charge into nitrogen protection then, at room temperature mixed 10 hours; Mixed material is drawn onto in the heating container by vacuum pump through baiting valve, behind reinforced the finishing, starts electrically heated., 100 ℃ of Heating temperatures, 10 hours heat-up times; Mixture through heating freely falls to the cloth district through the feed opening of heating container, then by scraper plate, distribute roll is evenly spread compound out, through transport tape material is delivered in the pony press, 1 normal atmosphere of control pressure, graphite carbon base-material through precompressed is sent to next group pressure roller compacting through pressure roller, and the carbon back material web through being compacted into film reaches the laminated film that final compression roll (the 4th group of pressure roller) is suppressed mixture thickness 60um successively; Laminated film is sent to scanning area through compression roll, scan line by line with laser beam, electron beam or ionic fluid, make laminated film be scanned position temperature to 3500 ℃, carry out carbonization, greying, long brilliant, build bridge and react, make the molecule frame perfect adaptation of the molecule frame and the bridge formation carbon back of nano-graphene, become superconduction, heat conduction, superstrength Graphene laminated film; Laminated film after scanning is cut edge the back by the wrap-up rolling, and wrap-up is installed the photoelectric error correction device in advance, to guarantee the planeness of rolling end face; In the present embodiment, heating, film forming, the waste gas in scanning calorimeter bridge formation each stage of reaction are concentrated emission treatment through the off gas treatment pipeline by induced draft fan.
Off gas treatment pipeline in the Graphene laminated film continuous machine is concentrated emission treatment by induced draft fan.
Embodiment two:
The 100g nano-graphene is added that 900g mole proportioning is the loading hopper that 1: 1 ethanol and acetic acid are put into Graphene laminated film continuous machine respectively, in ribbon mixer, charge into nitrogen protection then, at room temperature mixed 10 hours; Mixed material is drawn onto in the heating container by vacuum pump through baiting valve, behind reinforced the finishing, starts electrically heated., 100 ℃ of Heating temperatures, 10 hours heat-up times; Carbon back mixture through heating freely falls to the cloth district through the feed opening of heating container, then by scraper plate, distribute roll is evenly spread compound out, through transport tape material is delivered in the pony press, 1 normal atmosphere of control pressure, graphite carbon base-material through precompressed is sent to next group pressure roller compacting through pressure roller, and the carbon back material web through being compacted into film reaches the laminated film that final compression roll (the 4th group of pressure roller) is suppressed mixture thickness 60um successively; Laminated film is sent to scanning area through compression roll, scan line by line with laser beam, electron beam or ionic fluid, make laminated film be scanned the position temperature and rise to 3500 ℃, carry out carbonization, greying, long brilliant, build bridge and react, make the molecule frame perfect adaptation of the molecule frame and the bridge formation carbon back of nano-graphene, become superconduction, heat conduction, superstrength Graphene laminated film; Laminated film after scanning is cut edge the back by the wrap-up rolling, and wrap-up is installed the photoelectric error correction device in advance, to guarantee the planeness of rolling end face; In the present embodiment, heating, film forming, the waste gas in scanning calorimeter bridge formation each stage of reaction are concentrated emission treatment through the off gas treatment pipeline by induced draft fan.
Embodiment three:
With 300g nano-graphene, 700g mole proportioning is the loading hopper that 1: 1 tolylene diisocyanate and quadrol are put into Graphene laminated film continuous machine respectively, charges into nitrogen protection then in ribbon mixer, at room temperature mixes 10 hours; Mixed material is drawn onto in the heating container by vacuum pump through baiting valve, behind reinforced the finishing, starts electrically heated., 500 ℃ of Heating temperatures, 20 hours heat-up times; Carbon back mixture through heating freely falls to the cloth district through the feed opening of heating container, then by scraper plate, distribute roll is evenly spread compound out, through transport tape material is delivered in the pony press, 10 normal atmosphere of pressure of control roll-in, graphite carbon base-material through precompressed is sent to next group pressure roller compacting through pressure roller, and the carbon back material web through being compacted into film reaches the laminated film that final compression roll (the 4th group of pressure roller) is suppressed mixture thickness 50um successively; Laminated film is sent to scanning area through compression roll, scan line by line on the laminated film to 3500 ℃ with laser beam, electron beam or ionic fluid, carry out carbonization, greying, long brilliant, build bridge and react, make the molecule frame perfect adaptation of the molecule frame and the bridge formation carbon back of nano-graphene, become superconduction, heat conduction, superstrength Graphene laminated film; Laminated film after scanning is cut edge the back by the wrap-up rolling, and wrap-up is installed the photoelectric error correction device in advance, to guarantee the planeness of rolling end face; In the present embodiment, heating, film forming, the waste gas in scanning calorimeter bridge formation each stage of reaction are concentrated emission treatment through the off gas treatment pipeline by induced draft fan.
Claims (3)
1. the preparation method of a superconduction, heat conduction, superstrength Graphene laminated film the steps include:
Fs mixes, and mass percent 10%-80% nano-graphene and 20%-90% liquid or powder bridge formation carbon back are put into mixing equipment respectively, charges into nitrogen protection then in this mixing equipment, at room temperature mixes 1-10 hour;
The subordinate phase heating is drawn onto mixed material in the heating container by vacuum pump through the mixing equipment baiting valve, behind reinforced the finishing, starts electrically heated., Heating temperature 100-500 ℃, 1-20 hour heat-up time;
The phase III film forming, the feed opening that will pass through heating container through the mixture of heating freely falls to the cloth district, then by scraper plate, distribute roll is evenly spread compound out, through transport tape mixture is delivered in the pony press, a control pressure 1-10 normal atmosphere is sent to next group pressure roller compacting through the graphite carbon base-material of precompressed through pressure roller, mixture through being compacted into film reaches final compression roll more successively, and mixture is suppressed the laminated film of thickness less than 0.1mm;
Quadravalence section scanning calorimeter is built bridge and is reacted, laminated film is sent to scanning area through compression roll, with laser beam, electron beam or ionic fluid laminated film is lined by line scan, the temperature that makes laminated film be scanned the position is higher than 3000 ℃, to realize carbonization, greying, long brilliant, build bridge and react, make the molecule frame perfect adaptation of the molecule frame and the bridge formation carbon back of nano-graphene, become superconduction, heat conduction, superstrength Graphene laminated film;
The five-stage rolling will be cut edge the back by the wrap-up rolling through the laminated film after the scanning, and wrap-up is installed the photoelectric error correction device in advance, to guarantee the planeness of rolling end face.
2. the preparation method of a kind of superconduction as claimed in claim 1, heat conduction, superstrength Graphene laminated film, it is characterized in that: described liquid or powder bridge formation carbon back are at least two kinds in amine, carboxylic-acid, isocyanates, carbonyl class, the hydroxy kind organic substance, and ratio is the mole proportioning of reaction.
3. the preparation method of a kind of superconduction as claimed in claim 1, heat conduction, superstrength Graphene laminated film is characterized in that: above-mentioned heating, film forming, the waste gas in scanning calorimeter bridge formation each stage of reaction are concentrated emission treatment through the off gas treatment pipeline by induced draft fan.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874795A (en) * | 2012-11-01 | 2013-01-16 | 哈尔滨工业大学 | Nano-carbon film based on nano-graphite sheet and preparation method thereof |
| CN102990765A (en) * | 2011-09-15 | 2013-03-27 | 上海安谱科学仪器有限公司 | Processing technology of high-temperature-resistant and long-life chromatographic gasket |
| CN109075293A (en) * | 2016-11-29 | 2018-12-21 | 株式会社Lg化学 | The diaphragm of carbonized graphite alkene layer comprising induced with laser and lithium-sulfur cell comprising the diaphragm |
| CN111180672A (en) * | 2020-01-19 | 2020-05-19 | 中南大学 | Protection method of alkali metal cathode, cathode prepared by protection method and application of cathode |
| CN111261833A (en) * | 2020-01-19 | 2020-06-09 | 中南大学 | Self-supporting lithium metal cathode and preparation and application thereof |
| CN114702030A (en) * | 2022-05-18 | 2022-07-05 | 山东大学 | Preparation method of ultrathin flexible graphene film |
-
2011
- 2011-01-26 CN CN2011100273058A patent/CN102180461A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102990765A (en) * | 2011-09-15 | 2013-03-27 | 上海安谱科学仪器有限公司 | Processing technology of high-temperature-resistant and long-life chromatographic gasket |
| CN102990765B (en) * | 2011-09-15 | 2014-12-10 | 上海安谱科学仪器有限公司 | Processing technology of high-temperature-resistant and long-life chromatographic gasket |
| CN102874795A (en) * | 2012-11-01 | 2013-01-16 | 哈尔滨工业大学 | Nano-carbon film based on nano-graphite sheet and preparation method thereof |
| CN109075293A (en) * | 2016-11-29 | 2018-12-21 | 株式会社Lg化学 | The diaphragm of carbonized graphite alkene layer comprising induced with laser and lithium-sulfur cell comprising the diaphragm |
| CN109075293B (en) * | 2016-11-29 | 2021-06-22 | 株式会社Lg化学 | Separator comprising laser-induced graphene carbide layer and lithium-sulfur battery comprising same |
| CN111180672A (en) * | 2020-01-19 | 2020-05-19 | 中南大学 | Protection method of alkali metal cathode, cathode prepared by protection method and application of cathode |
| CN111261833A (en) * | 2020-01-19 | 2020-06-09 | 中南大学 | Self-supporting lithium metal cathode and preparation and application thereof |
| CN111261833B (en) * | 2020-01-19 | 2021-06-22 | 中南大学 | Self-supporting lithium metal cathode and preparation and application thereof |
| CN114702030A (en) * | 2022-05-18 | 2022-07-05 | 山东大学 | Preparation method of ultrathin flexible graphene film |
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Application publication date: 20110914 |