CN105803587B - The method that the tape casting prepares graphene fiber - Google Patents
The method that the tape casting prepares graphene fiber Download PDFInfo
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- CN105803587B CN105803587B CN201510000110.2A CN201510000110A CN105803587B CN 105803587 B CN105803587 B CN 105803587B CN 201510000110 A CN201510000110 A CN 201510000110A CN 105803587 B CN105803587 B CN 105803587B
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- 239000000835 fiber Substances 0.000 title claims abstract description 88
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- -1 graphite alkene Chemical class 0.000 description 4
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- 238000007766 curtain coating Methods 0.000 description 3
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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
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
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- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 1
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Abstract
According to weight part ratio it is 13 by vermiform expanded graphite, distilled water, surfactant the invention discloses a kind of method that the tape casting prepares graphene fiber:100:0.01 1 it is well mixed obtain mixed solution, handled through liquid agitation pulverizer, obtain graphite oxide colloidal solution after concentration;Graphite oxide colloidal solution is extruded to the polytetrafluoro conduction band surface for being cast to cutting through casting apparatus, graphene oxide band is formed after drying;Graphene oxide band is clamped through stainless steel band and exported, and during which rolls reality through pressure roll, then through fluid tip injection air twisting, and is mapped to hole of the laser beam through nozzle tail end a corresponding twisting point position, graphene oxide band is transformed into graphene fiber.This method operating process is easy, it is not necessary to subsequent treatment and removal of impurities;Graphene fiber can be largely obtained, is easy to the industrial applications of next step;Graphene fiber has a twist, and Coating combination is close, appearance and consistent internal structure, and mechanical performance is outstanding.
Description
Technical field
The invention belongs to graphene oxide and grapheme material preparing technical field, specifically related to a kind of the tape casting prepares stone
The device and method of black alkene fiber and yarn, methods described is dry spinning method.
Background technology
Graphene as all carbon materials most basic construction unit, with real monoatomic layer thickness and strict two
Structure is tieed up, with very high mechanical strength, elasticity, thermal conductivity, electron mobility(100,000cm2· V-1·s-1)And amount
Sub- Hall effect etc..Obtained since British scientist An Delie Jim in 2010 and Ke Siteyanuowosainuo have found graphene
Since obtaining the Nobel Prize, graphene research reaches unprecedented research climax, and increasing research finds that graphene is available
In field-effect transistor, high-frequency element, super microprocessor and single-molecule detection device etc..And be made up of graphene for elementary cell
Three-dimensional structure material, such as film and bulk material can be applied to controllable Breathable filmses, anisotropy ion-conducting material, super
The field of functional materials such as capacitor, lithium ion battery and energy catalysis.
Consider from practical application angle, nano-graphene material is changed into macrostructure material undoubtedly very valuable
The research direction of value.A main bugbear in graphene research and application is effective assembling of graphene macrostructure, at present
Relatively successfully assembling is the film and bulk for obtaining three-dimensional structure.In the graphene side that assembling macrostructure is one-dimentional structure
Face;Although having prepared graphene fiber at present, because the solubility of graphene in itself is low and sticky difference, institute
To be difficult to prepare high strength graphite alkene fiber.
At present, domestic and international researcher has prepared graphene fiber by different methods respectively.Zhejiang University is high
Superfine people and Chinese University of Science and Technology's Yu's book is grand et al. has obtained graphite by wet spinning-reduction two-step method from different precipitating reagents
Alkene fiber.Beijing Institute of Technology Qu Liangti et al. in glass tube high temperature hydro-thermal reaction by having obtained graphene fiber.Qu Liang
The document report of body etc., the document, which is disclosed, is injected into graphene oxide solution in the internal capillary equipped with copper wire, enters water-filling
The fiber of thermal synthesis graphene/copper wire, copper wire is removed and obtains hollow graphene micro-nano mitron, prepared by this method after cooling
Graphene micro-nano mitron have certain suppleness, but be unable to continuous production, can only obtain graphene micro-nano mitron, it is impossible to
Obtain graphene oxide doughnut, and this method subsequent treatment and except miscellaneous operation takes very long, have much room for improvement or develop
New method.
In recent years, patent CN201180020978.9 was used for the technique for spinning graphene ribbon fiber, disclosed CNT
The method for expanding into graphene ribbon;201410016557.4、CN 201210001537.0(By large-size graphene oxide sheet system
The method of standby high-strength conductive graphene fiber)、CN201210001524.3(A kind of high-strength graphene ordered porous fibers and
Its preparation method)、CN201210017773.1(A kind of preparation method of graphene fiber)、CN201210001 536.6(It is a kind of
Ion-enhanced graphene fiber and preparation method thereof)、CN201110441254.3(A kind of high strength macro graphene conductive fiber
Preparation method)Etc. disclosing different wet laid fiber preparation methods;CN201310064 816.6(Graphene/TiO2 fibers
Preparation method)Disclose wet method and prepare the technique for mixing titanium oxide;CN201110098809.9(Electrospinning-hydro-thermal method prepares graphite
The method of the brilliant particulate composite of alkene/ceramic nano)The method for disclosing wet electrostatic spinning; CN200580000581.8(Tool
There is the fine carbon fiber of various structures)Disclose the performance of axially vertical fine carbon fiber;Therefore one kind can be efficiently using existing
Have, ripe, Traditional Industrialization equipment, easy one-step method and low temperature, the method for leniently preparing graphene fiber need out
Hair, so as to more preferable large-scale application.
The content of the invention
The technical problems to be solved by the invention are to prepare graphene fibre using wet method in the prior art to overcome
The preparation method of dimension needs drying to consume energy, and big, there is provided a kind of method of dry process graphene fiber for the defect of complex process.
The preparation method of the present invention is simple to operate, and mild condition, the cost of raw material is low;Prepared using method of the present invention
Graphene fiber, even structure, mechanical performance is excellent, easy functionalization.
In order to solve the above technical problems, the present invention uses following technical scheme:A kind of the tape casting prepares graphene fiber
Method, step is as follows:
A kind of method that the tape casting prepares graphene fiber, step is as follows:
(1)By vermiform expanded graphite, distilled water, surfactant according to weight part ratio be 1-3:100:0.01-1 is mixed
Close and uniformly obtain mixed solution, mixed solution is handled through liquid agitation pulverizer, the concentrated rear concentration that obtains is 20 ~ 25mg
mL-1Graphite oxide colloidal solution;
(2)Graphite oxide colloidal solution is extruded to the polytetrafluoro conduction band surface for being cast to cutting, drying machine through casting apparatus
Drying and processing formation graphene oxide band;
(3)Graphene oxide band is clamped through stainless steel band and exported, during which reality is rolled through 1-5 tons of pressure roll, obtains
Thickness is 16-100 μm, and width is 0.1-0.5mm graphene oxide band;
(4)By step(3)Obtained graphene oxide band is twisted through fluid tip injection air, and with laser beam through spray
The hole of mouth tail end is mapped to corresponding twisting point position, and graphite oxide fiber is transformed into graphene fiber, the synchronous increase graphite of twisting
The binding strength of alkene lamella, solves other method and prepares the problem of graphene composite fibre intensity improves little, export simultaneously
To coiling and molding device, the graphene fiber bobbin with the twist of certain package capacity is directly prepared into.
The step(1)In surfactant be cationic surfactant, anion surfactant or both sexes table
Face activating agent, its cationic surfactant is quaternary ammonium salt cationic surfactant, such as trimethyl chlorination
Ammonium, anion surfactant are stearic acid or neopelex, amphoteric surfactant are lecithin or glycine betaine.
The step(1)Middle mixed solution is handled 10-1000 minutes through liquid agitation pulverizer, liquid agitation pulverizer
Rotating speed is 10000-50000r/min.
The step(2)The temperature of middle drying machine drying processing is 60-80 DEG C.
The step(4)The laser beam of use has effects that thermal reduction.
The step(4)The laser beam used is 650nm, the beam of laser beam 4 of 80-1000 milliwatts.
To step(3)In graphene oxide band top layer apply plus nano functional particulate, nano functional solution/emulsion, receive
Rice material precursor emulsion/solution, prepares the graphene oxide and graphene fiber of functionalization.
The step(4)In fluid tip injection air twister be the special of sir jet spinning machines that cotton spinning enterprise is used
With nozzle and with its design principle identical device.
Beneficial effects of the present invention:1. the invention provides the dry process side of a kind of graphene oxide and graphene fiber
Method, this method operating process is easy, and the preparation of graphene fiber is directly realized by using existing Weaving device, through rational design and
The corresponding ripe accessory of matching, graphene fiber can be directly obtained with pure graphene composite thin film, it is not necessary to after
Continuous processing and removal of impurities;Graphene fiber can be largely obtained, in the range of equipment license, it is possible to quickly prepare up to tens of thousands of
The long graphene fiber of rice, and specific package is formed, it is easy to the industrial applications of next step;2. the construction material oxidation utilized
Graphene wide material sources, cost is low, largely can continuously produce;3. graphene fiber produced by the present invention has the twist, graphite
Alkene piece interlayer is tightly combined, and graphene fiber appearance and consistent internal structure, mechanical performance are outstanding, flexible, flexible;4.
Invention provides the device and method that the tape casting prepares graphene fiber and yarn, and methods described can be in graphite oxide laminated film
Coating nanometer functional material before cutting, obtains the composite graphite alkene fiber of the in-situ modification containing equally distributed nano functional.
Brief description of the drawings
Fig. 1 is the machining sketch chart that the tape casting of the present invention prepares graphene fiber.
Fig. 2 is that the tape casting of the present invention prepares graphene fiber(MULTILAYER COMPOSITE)Machining sketch chart.
Embodiment
To be best understood from the present invention, the present invention is described in further detail with reference to specific embodiment.
Embodiment 1
The present invention relates to the device and method that a kind of curtain coating prepares graphene fiber and yarn, belong to graphene oxide and stone
Black alkene technical field of material.Methods described is as follows:By vermiform 3 parts of expanded graphite, 100 parts of distilled water and surface-active
Agent(Neopelex)0.01 part of mixed solution is 50,000 turns of liquid agitation pulverizer through rotating speed(Mulser)Place
Reason, obtains graphite oxide colloidal solution, concentrated rear acquisition 25mgmL-1Graphite oxide colloidal solution, the colloid is squeezed through casting apparatus 1
Go out to be cast to the surface of polytetrafluoro conduction band 2 of cutting, the drying and processing under the conditions of 60 DEG C of drying machine 3, then, band is through stainless steel
Band clamping output, during which rolls reality through 5 tons of pressure roll 4, and it is 16 μm to obtain thickness, and width is 0.5mm graphene oxide bar
Band, band is twisted through fluid tip injection air, while four beam 650nm, hole of the laser 5 through nozzle tail end of 300 milliwatts is mapped to
Corresponding twisting point position, graphite oxide fiber is transformed into graphene fiber, the combination jail of the synchronous increase graphene sheet layer of twisting
Degree, solves other method and prepares the problem of graphene fiber intensity improves little;Coiling and molding device is output to simultaneously, directly
The graphene fiber bobbin 6 with the twist of certain package capacity is made.
Embodiment 2
The present invention relates to the device and method that a kind of curtain coating prepares graphene fiber and yarn, belong to graphene oxide and stone
Black alkene technical field of material.Methods described is as follows:Vermiform expanded graphite 1-3 parts, 100 parts of distilled water and surface are lived
Property agent(Glycine betaine)0.2 part of mixed solution is 10,000 turns of liquid agitation pulverizer through rotating speed(Mulser)Processing, is aoxidized
Graphite glue body fluid, 20 mgmL of concentrated rear acquisition-1Graphite oxide colloidal solution, the colloid is cast to quarter through casting apparatus extrusion
The polytetrafluoro conduction band surface of groove, 80 DEG C of drying and processings of drying machine, then, band are clamped through stainless steel band and exported, during which through 2 tons
Pressure roll roll reality, obtain thickness for 50 μm, width is 0.5mm graphene oxide band.Band sprays through fluid tip
Air is twisted, while four beam 650nm, hole of the laser through nozzle tail end of 400 milliwatts is mapped to corresponding twisting point position, aoxidizes stone
Black fiber is transformed into graphene fiber, and the binding strength of the synchronous increase graphene sheet layer of twisting solves other method and prepares stone
The problem of black alkene fibre strength improves little;Coiling and molding device is output to simultaneously, the band for being directly prepared into certain package capacity is twisted with the fingers
The graphene fiber bobbin of degree.
Embodiment 3
The present invention relates to the device and method that a kind of curtain coating prepares graphene fiber and yarn, belong to graphene oxide and stone
Black alkene technical field of material.Methods described is as follows:By vermiform 1 part of expanded graphite, 100 parts of distilled water and surface-active
Agent(DTAC)0.03 part of mixed solution is 20,000 turns of liquid agitation pulverizer through rotating speed(Mulser)
Processing, obtains graphite oxide colloidal solution, concentrated rear acquisition 25mgmL-1Graphite oxide colloidal solution, the colloid is through casting apparatus
Extrusion is cast to the polytetrafluoro conduction band surface of cutting, 60-80 DEG C of drying and processing of drying machine, and then, band is pressed from both sides through stainless steel band
Output is held, during which reality is rolled through 1 ton of pressure roll, it is 16 μm to obtain thickness, width is 0.5mm graphene oxide band, oxygen
Graphite alkene band is through fluid tip injection air twisting, while four beam 650nm, hole of the laser through nozzle tail end of 100 milliwatts
Corresponding twisting point position is mapped to, graphite oxide fiber is transformed into graphene fiber, the knot of the synchronous increase graphene sheet layer of twisting
Fastness is closed, other method is solved and prepares the problem of graphene fiber intensity improves little;Coiling and molding device is output to simultaneously,
It is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 4
The present invention relates to the device and method that a kind of the tape casting prepares graphene fiber and yarn, belong to graphene oxide and
Grapheme material preparing technical field.Methods described is as follows:By vermiform 3 parts of expanded graphite, 100 parts of distilled water and cleaning meal
The mixed solution that 0.01 part of tool liquid detergent is 50,000 turns of liquid agitation pulverizer through rotating speed(Mulser)Processing, is aoxidized
Graphite glue body fluid, concentrated rear acquisition 25mgmL-1Graphite oxide colloidal solution, the colloid is through 3 sets of casting apparatus 1(Such as Fig. 2 institutes
Show)Extrusion is cast to the surface of polytetrafluoro conduction band 2 of cutting respectively, the drying and processing under the conditions of 60 DEG C of drying machine 3, then, 3
Band is clamped through stainless steel band and exported, and during which rolls reality through 5 tons of pressure roll 4, and it is 16 μm to obtain thickness, and width is 0.5mm's
Graphene oxide band, graphene oxide band is twisted through fluid tip injection air, while four beam 650nm, and 300 milliwatts swash
Hole of the light 5 through nozzle tail end is mapped to corresponding twisting point position, and graphite oxide fiber is transformed into graphene fiber, and twisting is synchronous to be increased
Plus the binding strength of graphene sheet layer, solve other method and prepare the problem of graphene fiber intensity improves little;It is simultaneously defeated
Go out to coiling and molding device, be directly prepared into the graphene fiber bobbin 6 with the twist of certain package capacity.
Embodiment 5
The method that the tape casting of the present embodiment prepares graphene fiber, step is as follows:
(1)Vermiform expanded graphite 1Kg, the Kg of distilled water 100, the Kg of surfactant 0.01 are mixed
Solution is closed, mixed solution is handled 1000 minutes through rotating speed for 10000r/min liquid agitation pulverizer, concentrated rear acquisition is dense
Spend for 20mgmL-1Graphite oxide colloidal solution;
(2)Graphite oxide colloidal solution is extruded to the polytetrafluoro conduction band surface for being cast to cutting through casting apparatus, at 60 DEG C
Under the conditions of drying machine drying and processing formation graphene oxide band;
(3)Graphene oxide band is clamped through stainless steel band and exported, during which reality is rolled through 1 ton of pressure roll, obtains thickness
Spend for 16 μm, width is 0.5mm graphene oxide band;
(4)To step(3)In graphene oxide band top layer apply plus nano functional particulate, graphene oxide band is passed through
Fluid tip injection air twisting, fluid tip injection air twister is the special of the sir jet spinning machines that cotton spinning enterprise is used
Nozzle and with its design principle identical device, while with 4 beam 650nm, 80 milliwatts and the laser beam warp with reduction effect
The hole of nozzle tail end is mapped to corresponding twisting point position, and graphite oxide fiber is transformed into graphene fiber, the synchronous increase stone of twisting
The binding strength of black alkene lamella, solves other method and prepares the problem of graphene composite fibre intensity improves little, while defeated
Go out to coiling and molding device, be directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 6
The method that the tape casting of the present embodiment prepares graphene fiber, step is as follows:
(1)By the vermiform Kg of expanded graphite 3, distilled water 100Kg, surfactant(Lecithin)1Kg is well mixed
To mixed solution, mixed solution is handled 10 minutes through rotating speed for 50000r/min liquid agitation pulverizer, concentrated rear acquisition
Concentration is 25mgmL-1Graphite oxide colloidal solution;
(2)Graphite oxide colloidal solution is extruded to the polytetrafluoro conduction band surface for being cast to cutting through casting apparatus, at 80 DEG C
Under the conditions of drying machine drying and processing formation graphene oxide band;
(3)Graphene oxide band is clamped through stainless steel band and exported, during which reality is rolled through 5 tons of pressure roll, obtains thickness
Spend for 100 μm, width is 0.1mm graphene oxide band;
(4)By step(3)Obtained graphene oxide band is through fluid tip injection air twisting, and fluid tip injection is empty
Gas twister be the special nozzle of sir jet spinning machines that cotton spinning enterprise is used and with its design principle identical device, simultaneously
A corresponding twisting point position is mapped to 4 beam 650nm, 1000 milliwatts and with hole of the laser beam through nozzle tail end for reducing effect,
Graphite oxide fiber is transformed into graphene fiber, and the binding strength of the synchronous increase graphene sheet layer of twisting solves other method
The problem of graphene composite fibre intensity improves little is prepared, while being output to coiling and molding device, certain package is directly prepared into
The graphene fiber bobbin with the twist of capacity.
Embodiment 7
The method that the tape casting of the present embodiment prepares graphene fiber, step is as follows:
(1)The vermiform Kg of expanded graphite 2, the Kg of distilled water 100, the Kg of surfactant 0.05 are well mixed and obtained
Mixed solution, mixed solution is handled 200 minutes through rotating speed for 25000r/min liquid agitation pulverizer, and concentrated rear acquisition is dense
Spend for 24mgmL-1Graphite oxide colloidal solution;
(2)Graphite oxide colloidal solution is extruded to the polytetrafluoro conduction band surface for being cast to cutting through casting apparatus, at 60-80 DEG C
Under conditions of drying machine drying and processing formation graphene oxide band;
(3)Graphene oxide band is clamped through stainless steel band and exported, during which reality is rolled through 3 tons of pressure roll, obtains thickness
Spend for 50 μm, width is 0.2mm graphene oxide band;
(4)By step(3)Obtained graphene oxide band is through fluid tip injection air twisting, and fluid tip injection is empty
Gas twister be the special nozzle of sir jet spinning machines that cotton spinning enterprise is used and with its design principle identical device, simultaneously
A corresponding twisting point position, oxygen are mapped to 4 beam 650nm, 500 milliwatts and with hole of the laser beam through nozzle tail end for reducing effect
Graphite fiber is transformed into graphene fiber, and the binding strength of the synchronous increase graphene sheet layer of twisting solves other method system
The problem of standby graphene composite fibre intensity improves little, while being output to coiling and molding device, is directly prepared into certain package and holds
The graphene fiber bobbin with the twist of amount.
Claims (7)
1. a kind of method that the tape casting prepares graphene fiber, it is characterised in that step is as follows:
(1)By vermiform expanded graphite, distilled water, surfactant according to weight part ratio be 1-3:100:0.01-1 parts of mixing
Uniform to obtain mixed solution, mixed solution is handled through liquid agitation pulverizer, and the concentrated rear concentration that obtains is 20 ~ 25mgmL-1
Graphite oxide colloidal solution;
(2)Graphite oxide colloidal solution is extruded to the polytetrafluoro conduction band surface for being cast to cutting, the drying of drying machine through casting apparatus
Processing forms graphene oxide band;
(3)Graphene oxide band is clamped through stainless steel band and exported, during which reality is rolled through 1-5 tons of pressure roll, obtains thickness
For 16-100 μm, width is 0.1-0.5mm graphene oxide band;
(4)By step(3)Obtained graphene oxide band is twisted through fluid tip injection air, and with laser beam through nozzle tail
The hole at end is mapped to corresponding twisting point position, and graphene oxide band is transformed into graphene fiber, while being output 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 step(1)In
Surfactant be 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:The step(1)In
Mixed solution is handled 10-1000 minutes 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 step(2)In
The temperature of drying machine drying processing 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 step(4)Adopt
Laser beam has effects that thermal reduction.
6. the method that the tape casting according to claim 1 prepares graphene fiber, it is characterised in that:The step(4)Adopt
Laser beam is 650nm, the beam of laser beam 4 of 80-1000 milliwatts.
7. the method that the tape casting according to any one in claim 1 ~ 6 prepares graphene fiber, it is characterised in that:To
Step(3)In graphene oxide band top layer apply plus nano functional particulate, nano functional solution/emulsion, nano material forerunner
Precursor emulsion/solution, prepares the graphene oxide and graphene fiber of functionalization.
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CN109750391B (en) * | 2019-02-12 | 2021-09-03 | 青岛大学 | System and method for preparing graphene fibers by positive pressure spinning method |
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