CN105803587A - Tape casting method for preparing graphene fibers - Google Patents
Tape casting method for preparing graphene fibers Download PDFInfo
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- CN105803587A CN105803587A CN201510000110.2A CN201510000110A CN105803587A CN 105803587 A CN105803587 A CN 105803587A CN 201510000110 A CN201510000110 A CN 201510000110A CN 105803587 A CN105803587 A CN 105803587A
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 143
- 239000000835 fiber Substances 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 65
- 238000010345 tape casting Methods 0.000 title claims abstract description 24
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 44
- 239000010439 graphite Substances 0.000 claims abstract description 44
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000012530 fluid Substances 0.000 claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 10
- 239000010935 stainless steel Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 23
- 238000013019 agitation Methods 0.000 claims description 13
- 238000007766 curtain coating Methods 0.000 claims description 12
- 238000005266 casting Methods 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 5
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- 239000003093 cationic surfactant Substances 0.000 claims description 4
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- 239000002280 amphoteric surfactant Substances 0.000 claims description 3
- 239000003945 anionic surfactant Substances 0.000 claims description 3
- 238000007306 functionalization reaction Methods 0.000 claims description 3
- 239000002086 nanomaterial Substances 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 2
- 239000011229 interlayer Substances 0.000 abstract description 2
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- 238000003756 stirring Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 13
- 238000002360 preparation method Methods 0.000 description 12
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- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 2
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- 239000004917 carbon fiber Substances 0.000 description 2
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 2
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 1
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- 239000008117 stearic acid Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a tape casting method for preparing graphene fibers. The tape casting method includes the steps that vermiform expanded graphite, distilled water and a surfactant are mixed to be even according to the weight part ratio of (1-3):100:(0.01-1) to obtain a mixed solution, and the mixed solution is treated and concentrated through a liquid stirring and smashing machine to obtain graphite oxide colloidal liquid; the graphite oxide colloidal liquid is extruded and subjected to tape casting through a tape casting device to reach the surface of a polytetrafluoroethylene guiding band with a carved groove, and is dried to form graphite oxide stripes; the graphite oxide stripes are clamped and output through a stainless steel band, and rolled through pressure rollers in the period, air is then sprayed through a fluid nozzle for twisting and sprayed to the corresponding twisting point position with laser beams through a hole in the tail end of the nozzle, and the graphite oxide stripes are converted into the graphene fibers. According to the tape casting method, the operating process is easy and convenient, and following treating and cleaning are avoided; a large quantity of graphene fibers can be obtained, and next-step industrial application is convenient; the graphene fibers have the twist degree, interlayer bonding is compact, the outside and the inside are even in structure, and the mechanical performance is excellent.
Description
Technical field
The invention belongs to graphene oxide and grapheme material preparing technical field, be specifically related to a kind of the tape casting and prepare the Apparatus and method for of graphene fiber and yarn, described method is dry spinning method.
Background technology
Graphene is as the most basic construction unit of all material with carbon elements, there is real monoatomic layer thickness and strict two-dimensional structure, there is significantly high mechanical strength, elasticity, heat conductivity, electron mobility (100,000cm2 V-1 s-1) and quantum hall effect etc..Since British scientist An Delie Jim in 2010 and Ke Siteyanuowosainuo find that Graphene obtains Nobel Prize, Graphene research reaches unprecedented research climax, more and more studying discovery, Graphene can be used for field-effect transistor, high-frequency element, super microprocessor and single-molecule detection device etc..And be the three dimensional structure material that elementary cell is constituted by Graphene, such as thin film and bulk material, can be applicable to the field of functional materials such as controlled Breathable films, anisotropy ion-conducting material, ultracapacitor, lithium ion battery and energy catalysis.
Consider from practical application angle, nano-graphene material is changed in macrostructure material and is undoubtedly very valuable research direction.A main bugbear in Graphene research and application is effective assembling of Graphene macrostructure, and relatively successfully assembling at present is the thin film and the bulk that obtain three dimensional structure.In assembling the Graphene that macrostructure is one-dimentional structure;Graphene fiber is prepared although existing at present, but, owing to the dissolubility of Graphene itself is low and viscosity is poor, so being difficult to preparation high strength graphite alkene fiber.
At present, domestic and international researcher has prepared graphene fiber respectively through diverse ways.Zhejiang University is superb et al. and Chinese University of Science and Technology's Yu's book is grand et al. selects different precipitant to obtain graphene fiber by wet spinning-reduction two-step method.Beijing Institute of Technology Qu Liangti et al. obtains graphene fiber by high-temperature water thermal response in glass tubing.The bibliographical information of Qu Liangti etc., the open inside that graphene oxide solution is injected into of the document is equipped with in the capillary tube of copper wire, carry out the fiber of Hydrothermal Synthesis Graphene/copper wire, after cooling, copper wire is removed the Graphene micro-nano mitron obtaining hollow, Graphene micro-nano mitron prepared by the method has certain suppleness, but can not continuous prodution, can only obtain Graphene micro-nano mitron, graphene oxide doughnut can not be obtained, and the method subsequent treatment and remove impurity operation are all consuming time very long, have much room for improvement or develop new method.
In recent years, patent CN201180020978.9, for spinning the technique of graphene ribbon fiber, disclosed the method that CNT expands into graphene ribbon;201410016557.4, the method that CN201210001537.0(is prepared high-strength conductive graphene fiber by large-size graphene oxide sheet), CN201210001524.3(high-strength graphene ordered porous fibers and preparation method thereof), the preparation method of a CN201210017773.1(graphene fiber), CN201210001536.6(ion-enhanced graphene fiber and preparation method thereof), the preparation method of a CN201110441254.3(high strength macro graphene conductive fiber) etc. disclose different wet laid fiber preparation methoies;The preparation method of CN201310064816.6(Graphene/TiO2 fiber) disclose the technique that wet-layer preparation mixes titanium oxide;The method of CN201110098809.9(preparing grapheme/ceramic nanocrystalline particle composite material with electrospinning-hydrothemal method) method that discloses wet electrostatic spinning;CN200580000581.8(has the fine carbon fiber of various structures) disclose the performance of axially vertical fine carbon fiber;Therefore one can efficiently utilize existing, ripe, Traditional Industrialization equipment, and easy one-step method and low temperature, the method leniently preparing graphene fiber have to be developed, in order to better large-scale application.
Summary of the invention
The technical problem to be solved is in that in order to the preparation method needs overcoming employing wet-layer preparation graphene fiber in prior art dry the defect big, complex process that consumes energy, it is provided that a kind of method of dry process graphene fiber.The preparation method of the present invention is simple to operate, mild condition, and the cost of raw material is low;Utilizing the graphene fiber that method of the present invention prepares, even structure, mechanical performance is excellent, easy functionalization.
For solving above-mentioned technical problem, the present invention by the following technical solutions: a kind of the tape casting prepares the method for graphene fiber, and step is as follows:
A kind of the tape casting prepares the method for graphene fiber, and step is as follows:
(1) being that 1-3:100:0.01-1 mix homogeneously obtains mixed solution by vermiform expanded graphite, distilled water, surfactant according to weight part ratio, mixed solution processes through liquid agitation pulverizer, and obtaining concentration after concentrated is 20 ~ 25mg mL-1Graphite oxide colloidal solution;
(2) through casting apparatus, graphite oxide colloidal solution being extruded the curtain coating polytetrafluoro conduction band surface to cutting, drying machine drying and processing forms graphene oxide band;
(3) by graphene oxide band through stainless steel band clamping output, period rolls reality through the pressure roll of 1-5 ton, obtains thickness and is 16-100 μm, and width is the graphene oxide band of 0.1-0.5mm;
(4) graphene oxide band step (3) obtained sprays air twisting through fluid tip, and it is mapped to the twisting point position of correspondence through the hole of nozzle tail end with laser beam, graphite oxide fiber is transformed into graphene fiber, twisting synchronizes to increase the binding strength of graphene sheet layer, solve additive method and prepare the problem that the raising of Graphene composite fibre intensity is little, it is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Surfactant in described step (1) is cationic surfactant, anion surfactant or amphoteric surfactant, its cationic surfactant is quaternary ammonium salt cationic surfactant, is lecithin or glycine betaine if Dodecyl trimethyl ammonium chloride, anion surfactant are stearic acid or dodecylbenzene sodium sulfonate, amphoteric surfactant.
In described step (1), mixed solution processes 10-1000 minute through liquid agitation pulverizer, and the rotating speed of liquid agitation pulverizer is 10000-50000r/min.
The temperature that in described step (2), drying machine drying processes is 60-80 DEG C.
The laser beam that described step (4) adopts has effect of thermal reduction.
The laser beam that laser beam is 650nm, 80-1000 milliwatt 4 that described step (4) adopts is restrainted.
It is coated with plus nano functional particulate, nano functional solution/emulsion, nano material presoma emulsion/solution to the graphene oxide band top layer in step (3), prepares graphene oxide and the graphene fiber of functionalization.
Fluid tip injection air twister in described step (4) is the special nozzle of the sir jet spinning machines that cotton spinning enterprise uses and the device identical with its design principle.
Beneficial effects of the present invention: 1. the invention provides the dry-forming method of a kind of graphene oxide and graphene fiber, the method operating process is easy, existing Weaving device is utilized to be directly realized by the preparation of graphene fiber, through the corresponding ripe accessory of reasonably design and coupling, graphene fiber can be directly obtained, it is not necessary to subsequent treatment and remove impurity with pure graphene composite thin film;Graphene fiber can be obtained in a large number, in the scope of equipment license, it is possible to quickly prepare the graphene fiber up to a few myriametre length, and form specific package, it is simple to next step industrial applications;2. the construction material graphene oxide wide material sources utilized, cost is low, it is possible to a large amount of productions continuously;3. the graphene fiber that the present invention prepares has the twist, and graphene film interlayer is tightly combined, graphene fiber appearance and consistent internal structure, and mechanical performance is outstanding, flexible, flexible;4. the invention provides the tape casting and prepare the Apparatus and method for of graphene fiber and yarn, described method can before graphite oxide laminated film is cut coating nanometer functional material, obtain the composite graphite alkene fiber of in-situ modification containing equally distributed nano functional.
Figure of description
Fig. 1 is the machining sketch chart that the tape casting of the present invention prepares graphene fiber.
Fig. 2 is the machining sketch chart that the tape casting of the present invention prepares graphene fiber (MULTILAYER COMPOSITE).
Detailed description of the invention
For being best understood from the present invention, below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The present invention relates to a kind of curtain coating and prepare the device and method of graphene fiber and yarn, belong to graphene oxide and grapheme material preparing technical field.Described method is as follows: processed through liquid agitation pulverizer (mulser) that rotating speed is 50,000 turns by the mixed solution of vermiform expanded graphite 3 parts, distilled water 100 parts and 0.01 part of surfactant (dodecylbenzene sodium sulfonate), obtain graphite oxide colloidal solution, after concentrated, obtain 25mg mL-1Graphite oxide colloidal solution, this colloid extrudes curtain coating polytetrafluoro conduction band 2 surface to cutting through casting apparatus 1, drying machine 3 is drying and processing under 60 DEG C of conditions, then, band is through stainless steel band clamping output, period rolls reality through the pressure roll 4 of 5 tons, obtaining thickness is 16 μm, width is the graphene oxide band of 0.5mm, band sprays air twisting through fluid tip, four bundle 650nm simultaneously, the laser 5 of 300 milliwatts is mapped to the twisting point position of correspondence through the hole of nozzle tail end, graphite oxide fiber is transformed into graphene fiber, twisting synchronizes to increase the binding strength of graphene sheet layer, solve additive method and prepare the problem that the raising of graphene fiber intensity is little;It is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin 6 with the twist of certain package capacity.
Embodiment 2
The present invention relates to a kind of curtain coating and prepare the device and method of graphene fiber and yarn, belong to graphene oxide and grapheme material preparing technical field.Described method is as follows: processed through liquid agitation pulverizer (mulser) that rotating speed is 10,000 turns by the mixed solution of vermiform expanded graphite 1-3 part, distilled water 100 parts and 0.2 part of surfactant (glycine betaine), obtain graphite oxide colloidal solution, after concentrated, obtain 20mg mL-1Graphite oxide colloidal solution, this colloid extrudes the curtain coating polytetrafluoro conduction band surface to cutting, 80 DEG C of drying and processings of drying machine through casting apparatus, then, band is through stainless steel band clamping output, and period rolls reality through the pressure roll of 2 tons, obtaining thickness is 50 μm, and width is the graphene oxide band of 0.5mm.Band sprays air twisting through fluid tip, four bundle 650nm simultaneously, the laser of 400 milliwatts is mapped to the twisting point position of correspondence through the hole of nozzle tail end, graphite oxide fiber is transformed into graphene fiber, twisting synchronizes to increase the binding strength of graphene sheet layer, solves additive method and prepares the problem that the raising of graphene fiber intensity is little;It is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 3
The present invention relates to a kind of curtain coating and prepare the device and method of graphene fiber and yarn, belong to graphene oxide and grapheme material preparing technical field.Described method is as follows: processed through liquid agitation pulverizer (mulser) that rotating speed is 20,000 turns by the mixed solution of vermiform expanded graphite 1 part, distilled water 100 parts and 0.03 part of surfactant (Dodecyl trimethyl ammonium chloride), obtain graphite oxide colloidal solution, after concentrated, obtain 25mg mL-1Graphite oxide colloidal solution, this colloid extrudes the curtain coating polytetrafluoro conduction band surface to cutting through casting apparatus, 60-80 DEG C of drying and processing of drying machine, then, band is through stainless steel band clamping output, period rolls reality through the pressure roll of 1 ton, obtaining thickness is 16 μm, width is the graphene oxide band of 0.5mm, graphene oxide band sprays air twisting through fluid tip, four bundle 650nm simultaneously, the laser of 100 milliwatts is mapped to the twisting point position of correspondence through the hole of nozzle tail end, graphite oxide fiber is transformed into graphene fiber, twisting synchronizes to increase the binding strength of graphene sheet layer, solve additive method and prepare the problem that the raising of graphene fiber intensity is little;It is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 4
The present invention relates to a kind of the tape casting and prepare the device and method of graphene fiber and yarn, belong to graphene oxide and grapheme material preparing technical field.Described method is as follows: processed through liquid agitation pulverizer (mulser) that rotating speed is 50,000 turns by the mixed solution of vermiform expanded graphite 3 parts, distilled water 100 parts and cleaning tableware liquid detergent 0.01 part, obtain graphite oxide colloidal solution, after concentrated, obtain 25mg mL-1Graphite oxide colloidal solution, this colloid overlaps casting apparatus 1(as shown in Figure 2 through 3) extrude curtain coating polytetrafluoro conduction band 2 surface to cutting respectively, drying machine 3 is drying and processing under 60 DEG C of conditions, then, 3 bands are through stainless steel band clamping output, period rolls reality through the pressure roll 4 of 5 tons, obtaining thickness is 16 μm, width is the graphene oxide band of 0.5mm, graphene oxide band sprays air twisting through fluid tip, four bundle 650nm simultaneously, the laser 5 of 300 milliwatts is mapped to the twisting point position of correspondence through the hole of nozzle tail end, graphite oxide fiber is transformed into graphene fiber, twisting synchronizes to increase the binding strength of graphene sheet layer, solve additive method and prepare the problem that the raising of graphene fiber intensity is little;It is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin 6 with the twist of certain package capacity.
Embodiment 5
The tape casting of the present embodiment prepares the method for graphene fiber, and step is as follows:
(1) vermiform expanded graphite 1Kg, distilled water 100Kg, surfactant 0.01Kg mix homogeneously being obtained mixed solution, mixed solution processes 1000 minutes through the liquid agitation pulverizer that rotating speed is 10000r/min, and obtaining concentration after concentrated is 20mg mL-1Graphite oxide colloidal solution;
(2) through casting apparatus, graphite oxide colloidal solution being extruded the curtain coating polytetrafluoro conduction band surface to cutting, when 60 DEG C, drying machine drying and processing forms graphene oxide band;
(3) by graphene oxide band through stainless steel band clamping output, period rolls reality through the pressure roll of 1 ton, and obtaining thickness is 16 μm, and width is the graphene oxide band of 0.5mm;
(4) it is coated with plus nano functional particulate to the graphene oxide band top layer in step (3), graphene oxide band is sprayed air twisting through fluid tip, fluid tip injection air twister is the special nozzle of the sir jet spinning machines that cotton spinning enterprise uses and the device identical with its design principle, restraint 650nm with 4 simultaneously, 80 milliwatts and have reduction effect laser beam through the hole of nozzle tail end be mapped to correspondence twisting point position, graphite oxide fiber is transformed into graphene fiber, twisting synchronizes to increase the binding strength of graphene sheet layer, solve additive method and prepare the problem that the raising of Graphene composite fibre intensity is little, it is simultaneously outputting to coiling and molding device, it is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 6
The tape casting of the present embodiment prepares the method for graphene fiber, and step is as follows:
(1) vermiform expanded graphite 3Kg, distilled water 100Kg, surfactant (lecithin) 1Kg mix homogeneously are obtained mixed solution, mixed solution processes 10 minutes through the liquid agitation pulverizer that rotating speed is 50000r/min, and obtaining concentration after concentrated is 25mg mL-1Graphite oxide colloidal solution;
(2) through casting apparatus, graphite oxide colloidal solution being extruded the curtain coating polytetrafluoro conduction band surface to cutting, when 80 DEG C, drying machine drying and processing forms graphene oxide band;
(3) by graphene oxide band through stainless steel band clamping output, period rolls reality through the pressure roll of 5 tons, and obtaining thickness is 100 μm, and width is the graphene oxide band of 0.1mm;
(4) graphene oxide band step (3) obtained sprays air twisting through fluid tip, fluid tip injection air twister is the special nozzle of the sir jet spinning machines that cotton spinning enterprise uses and the device identical with its design principle, restraint 650nm with 4 simultaneously, 1000 milliwatts and have reduction effect laser beam through the hole of nozzle tail end be mapped to correspondence twisting point position, graphite oxide fiber is transformed into graphene fiber, twisting synchronizes to increase the binding strength of graphene sheet layer, solve additive method and prepare the problem that the raising of Graphene composite fibre intensity is little, it is simultaneously outputting to coiling and molding device, it is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 7
The tape casting of the present embodiment prepares the method for graphene fiber, and step is as follows:
(1) vermiform expanded graphite 2Kg, distilled water 100Kg, surfactant 0.05Kg mix homogeneously being obtained mixed solution, mixed solution processes 200 minutes through the liquid agitation pulverizer that rotating speed is 25000r/min, and obtaining concentration after concentrated is 24mg mL-1Graphite oxide colloidal solution;
(2) through casting apparatus, graphite oxide colloidal solution being extruded the curtain coating polytetrafluoro conduction band surface to cutting, when 60-80 DEG C, drying machine drying and processing forms graphene oxide band;
(3) by graphene oxide band through stainless steel band clamping output, period rolls reality through the pressure roll of 3 tons, and obtaining thickness is 50 μm, and width is the graphene oxide band of 0.2mm;
(4) graphene oxide band step (3) obtained sprays air twisting through fluid tip, fluid tip injection air twister is the special nozzle of the sir jet spinning machines that cotton spinning enterprise uses and the device identical with its design principle, restraint 650nm with 4 simultaneously, 500 milliwatts and have reduction effect laser beam through the hole of nozzle tail end be mapped to correspondence twisting point position, graphite oxide fiber is transformed into graphene fiber, twisting synchronizes to increase the binding strength of graphene sheet layer, solve additive method and prepare the problem that the raising of Graphene composite fibre intensity is little, it is simultaneously outputting to coiling and molding device, it is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Claims (7)
1. the method that a tape casting prepares graphene fiber, it is characterised in that step is as follows:
(1) being that 1-3:100:0.01-1 part mix homogeneously obtains mixed solution by vermiform expanded graphite, distilled water, surfactant according to weight part ratio, mixed solution processes through liquid agitation pulverizer, and obtaining concentration after concentrated is 20 ~ 25mg mL-1Graphite oxide colloidal solution;
(2) through casting apparatus, graphite oxide colloidal solution being extruded the curtain coating polytetrafluoro conduction band surface to cutting, drying machine drying and processing forms graphene oxide band;
(3) by graphene oxide band through stainless steel band clamping output, period rolls reality through the pressure roll of 1-5 ton, obtains thickness and is 16-100 μm, and width is the graphene oxide band of 0.1-0.5mm;
(4) graphene oxide band step (3) obtained sprays air twisting through fluid tip, and it is mapped to the twisting point position of correspondence through the hole of nozzle tail end with laser beam, graphene oxide band is transformed into graphene fiber, it is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin with the twist.
2. the method that the tape casting according to claim 1 prepares graphene fiber, it is characterised in that: the surfactant in described step (1) is cationic surfactant, anion surfactant or amphoteric surfactant.
3. the method that the tape casting according to claim 1 prepares graphene fiber, it is characterised in that: in described step (1), mixed solution processes 10-1000 minute through liquid agitation pulverizer, and the rotating speed of liquid agitation pulverizer is 10000-50000r/min.
4. the method that the tape casting according to claim 1 prepares graphene fiber, it is characterised in that: the temperature that in described step (2), drying machine drying processes is 60-80 DEG C.
5. the method that the tape casting according to claim 1 prepares graphene fiber, it is characterised in that: the laser beam that described step (4) adopts has effect of thermal reduction.
6. the method that the tape casting according to claim 1 prepares graphene fiber, it is characterised in that: the laser beam that laser beam is 650nm, 80-1000 milliwatt 4 that described step (4) adopts is restrainted.
7. the method that the tape casting according to any one in claim 1 ~ 6 prepares graphene fiber, it is characterized in that: be coated with plus nano functional particulate, nano functional solution/emulsion, nano material presoma emulsion/solution to the graphene oxide band top layer in step (3), prepare graphene oxide and the graphene fiber of functionalization.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107151835A (en) * | 2017-05-19 | 2017-09-12 | 杭州高烯科技有限公司 | A kind of Flexible graphene fiber and its continuous preparation method |
CN109750391A (en) * | 2019-02-12 | 2019-05-14 | 青岛大学 | A kind of positive pressure spin processes prepare the system and method for graphene fiber |
CN112458553A (en) * | 2020-10-29 | 2021-03-09 | 烟台泰和新材料股份有限公司 | High-performance carbon nano/MXene composite fiber and preparation method thereof |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0967423A2 (en) * | 1998-06-27 | 1999-12-29 | Sgl Technik Gmbh | Packing yarn of graphite and plastic sheet |
CN102115566A (en) * | 2011-01-06 | 2011-07-06 | 西安理工大学 | Preparation method for graphene oxide with high barrier property and polymer nanocomposite film |
CN103387225A (en) * | 2012-11-21 | 2013-11-13 | 厦门凯纳石墨烯技术有限公司 | Heat-conducting graphite membrane and preparation method |
CN103613927A (en) * | 2013-11-26 | 2014-03-05 | 哈尔滨工业大学 | Polyimide/fluorinated graphene composite film and preparation method thereof |
CN104003380A (en) * | 2014-06-09 | 2014-08-27 | 黑龙江奥星能源科技有限公司 | Preparation method of ultra-thin graphite paper and graphene oxide composited film |
-
2015
- 2015-01-02 CN CN201510000110.2A patent/CN105803587B/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0967423A2 (en) * | 1998-06-27 | 1999-12-29 | Sgl Technik Gmbh | Packing yarn of graphite and plastic sheet |
CN102115566A (en) * | 2011-01-06 | 2011-07-06 | 西安理工大学 | Preparation method for graphene oxide with high barrier property and polymer nanocomposite film |
CN103387225A (en) * | 2012-11-21 | 2013-11-13 | 厦门凯纳石墨烯技术有限公司 | Heat-conducting graphite membrane and preparation method |
CN103613927A (en) * | 2013-11-26 | 2014-03-05 | 哈尔滨工业大学 | Polyimide/fluorinated graphene composite film and preparation method thereof |
CN104003380A (en) * | 2014-06-09 | 2014-08-27 | 黑龙江奥星能源科技有限公司 | Preparation method of ultra-thin graphite paper and graphene oxide composited film |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107151835A (en) * | 2017-05-19 | 2017-09-12 | 杭州高烯科技有限公司 | A kind of Flexible graphene fiber and its continuous preparation method |
CN109750391A (en) * | 2019-02-12 | 2019-05-14 | 青岛大学 | A kind of positive pressure spin processes prepare the system and method for graphene fiber |
CN109750391B (en) * | 2019-02-12 | 2021-09-03 | 青岛大学 | System and method for preparing graphene fibers by positive pressure spinning method |
CN112458553A (en) * | 2020-10-29 | 2021-03-09 | 烟台泰和新材料股份有限公司 | High-performance carbon nano/MXene composite fiber and preparation method thereof |
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