CN107502995A - Graphene fiber and graphene fiber non-woven fabrics of a kind of fold and preparation method thereof - Google Patents
Graphene fiber and graphene fiber non-woven fabrics of a kind of fold and preparation method thereof Download PDFInfo
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- CN107502995A CN107502995A CN201710670077.3A CN201710670077A CN107502995A CN 107502995 A CN107502995 A CN 107502995A CN 201710670077 A CN201710670077 A CN 201710670077A CN 107502995 A CN107502995 A CN 107502995A
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- graphene
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/16—Chemical after-treatment of artificial filaments or the like during manufacture of carbon by physicochemical methods
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a kind of graphene fiber with pleated structure and graphene fiber non-woven fabrics and preparation method thereof, contain the micro-structural of a large amount of folds in the graphene fiber surface, and it can be used for forming more pleated structure graphene fiber non-woven fabrics, so that the specific surface area of non-woven fabrics is significantly increased, and graphene fiber and the connected network structure that is made up of fiber while there is higher electric conductivity and pliability, therefore can be applied as flexible electrode material in wearable energy storage device.
Description
Technical field
The present invention relates to graphene fiber and fabric, more particularly to a kind of graphite formed by the graphene film accumulation of fold
Alkene fiber and graphene fiber non-woven fabrics and preparation method thereof.
Background technology
Graphene fiber non-woven fabrics is a kind of new non-woven fabrics fabric (Nature being made up of graphene fiber
Communications, 2016,13684), due to realizing graphene fiber merging into each other in lap-joint so that this nothing
Spinning cloth material has the performances such as excellent conduction, heat conduction, so as to fully demonstrate the good characteristic of graphene on a macroscopic scale
(Science,2004,306:666-669).Have benefited from the highly conductive network structure that graphene fiber non-woven fabrics is presented, will
It has great application potential as the textile electrode of flexibility in the energy storage device such as capacitor and battery field.
Existing graphene fiber non-woven fabrics is flexible preferably, and electric conductivity is high, but forms the graphene fiber of non-woven fabrics
Surface micro-structure is less, in the electrode material as ultracapacitor because active surface area is smaller, significantly limit electricity
The specific capacitance value of container.If can be by special means in the substantial amounts of micro-structural of graphene fiber surface construction, significantly to increase
Add the specific surface area of fiber, the electric double layer capacitance with regard to graphene fiber non-woven fabrics electrode can be greatly promoted, obtain higher performance
Energy storage device.At present, the graphene fiber non-woven fabrics with multilevel hierarchy is not seen in report.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide the graphene fiber and graphene fibre of a kind of fold
Tie up non-woven fabrics and preparation method thereof.
The present invention is achieved through the following technical solutions:A kind of graphene fiber of fold, accumulated by the graphene film of fold
Form, the pleated structure of the graphene film has defective graphene film and formed under capillary forces.
A kind of preparation method of graphene fiber, comprises the following steps:
(1) continuous wet spinning is carried out by spinning solution of graphene oxide dispersion.
(2) obtained graphene oxide fiber is placed into more than 12h in room temperature, it is then true at a temperature of not higher than 80 DEG C
Sky dries 3h.
(3) fully dry graphene oxide fiber is immersed in the water heating kettle equipped with water and carries out hydro-thermal process, hydro-thermal
The temperature range of processing is 80-200 DEG C.
(4) graphene fiber formed by the graphene oxide sheet accumulation of fold is obtained after air drying.
Further, spinning solution is the aqueous solution or DMF solution of graphene oxide.Corresponding, spin
The coagulating bath that silk process uses is calcium chloride/water/alcohol mixeding liquid or ethyl acetate.
A kind of High-performance graphene fabric nonwoven cloth, mutually overlapped by graphene fiber and form network, at grid node
Graphene fiber mutually merges.
A kind of preparation method of High-performance graphene fabric nonwoven cloth, using high shear agitation machine by claim 2 step
Graphene fiber in rapid 3 after hydro-thermal process blends into the chopped fiber that length is 1-7mm in aqueous, is then sunk on filter screen
It is long-pending, obtain graphene fiber non-woven fabrics after air drying.
Further, the rotating speed of high shear agitation is 3000-8000rpm.
Further, this method also includes further being reduced dried graphene fiber non-woven fabrics.Reduction side
Method for reduced using chemical reducing agents such as hydroiodic acid, hydrazine hydrate, Vitamin C, sodium borohydrides or 100-3000 DEG C thermal reduction.
The present invention compared with prior art, has the advantages that:
(1) graphene fiber is formed by the graphene film accumulation of fold, significantly increases specific surface area, has bigger work
Property surface, is advantageous to its application in textile electrode.
(2) flexibility of graphene fiber non-woven fabrics is maintained while obtaining fiber surface multilevel hierarchy, can be worn in flexibility
Energy storage device field is worn to be with a wide range of applications.
(3) preparation method is simple, and the micro-structural of fiber surface can pass through the predrying temperature of fiber and hydro-thermal process temperature
Controllable adjustment is realized in change.
Brief description of the drawings
Fig. 1 is electron scanning micrograph of the fold graphene fiber under different amplification.
Fig. 2 is the forming process schematic diagram (a) and the scanning electron microscope (SEM) photograph in each stage (b~e) of fold graphene fiber;
Fig. 3 is schematic diagram (b) at the schematic diagram (a) and fusion of fold graphene fiber non-woven fabrics.
Embodiment
The present invention takes full advantage of the hydrophily of graphene oxide, makes graphene oxide molten by absorbing water after being immersed in water
Swollen effect assigns graphene sheet layer with certain free degree, is advantageous to the formation of pleated structure, and use the relatively low water of temperature
The structure that micro-structural is carried out to graphene fiber is heat-treated, energy consumption is low, and method is simple.In hydro-thermal process by graphite oxide
The reduction (removing of oxygenated functional group) of alkene lamella introduces defect in graphene sheet layer, there is provided what pleated structure was formed should
Power centrostigma.Graphene fiber spontaneously dries in atmosphere after hydro-thermal process, and the volatilization of the aqueous solvent contained in fiber forms huge
Big capillary force so that graphene sheet layer spontaneously produces fold, on graphene fiber surface and is internally formed micro-structural,
Dramatically increase the specific surface area of graphene fiber.Detailed process is as shown in Figure 2.
Above-mentioned fiber is mutually fused into network structure, forms pure graphene non-woven fabrics, as shown in figure 3, ensureing non-woven fabrics
The specific surface area of graphene fiber non-woven fabrics has been obviously improved while high conductivity.Based on features above, multistage of the invention
Pleated structure graphene fiber and graphene fiber non-woven fabrics can make energy storage device have high flexibility when as textile electrode
Excellent chemical property is obtained simultaneously, is hopeful to be applied in wearable electronic devices field.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment, belong to protection scope of the present invention.
Embodiment 1:
(1) graphene oxide/aqueous solution using concentration as 5mg/mL is spinning solution, calcium chloride/water/alcohol mixeding liquid (matter
Measure ratio 20:300:100) continuous wet spinning is carried out for coagulating bath.
(2) obtained graphene oxide fiber is placed into 12h in room temperature, is then dried in vacuo 3h at a temperature of 80 DEG C.
(3) fully dry graphene oxide fiber is immersed in the water heating kettle equipped with water and carries out hydro-thermal process, handled
Condition is 200 DEG C, 12h.
(4) more fold graphene fibers are obtained after air drying.
By above step, obtained graphene fiber has obvious pleated structure, fibre strength about 90MPa, conduction
Rate is 102S/m.
Embodiment 2:
(1) it is 5mg/mL graphene oxide/DMF solution for spinning solution using concentration, ethyl acetate is
Coagulating bath carries out continuous wet spinning.
(2) obtained graphene oxide fiber room temperature is placed into 14h, 60 DEG C of vacuum drying 3h.
(3) fully dry graphene oxide fiber is immersed in the water heating kettle equipped with water and carries out hydro-thermal process, handled
Condition is 150 DEG C, 12h.
(4) graphene fiber after hydro-thermal process is blended by growth with 3000rpm rotating speed using high shear agitation machine
The chopped fiber for 4mm is spent, and graphene fiber non-woven fabrics is obtained after filter deposited thereon, air drying.
By above step, obtained graphene fiber non-woven fabrics has multilevel hierarchy, graphene fiber rough surface, contained
There is the micro-structural of substantial amounts of fold and projection, specific surface area reaches 190m2/ g, conductance 80S/m, and the nonwoven cloth material is flexible
Preferably, tolerance is repeatedly bent and holding structure is stable.
Embodiment 3:
(1) graphene oxide water solution using concentration as 15mg/mL is dispersion liquid, and calcium chloride/water/alcohol mixeding liquid is solidifying
Gu bath carries out continuous wet spinning.
(2) obtained graphene oxide fiber room temperature is placed into 15h, 100 DEG C of vacuum drying 3h.
(3) fully dry graphene oxide fiber is immersed in the water heating kettle equipped with water and carries out hydro-thermal process, handled
Condition is 80 DEG C, 12h.
(4) graphene fiber after hydro-thermal process is blended into 5000rpm rotating speed using high shear agitation machine short
Fiber, and obtain the graphene fiber non-woven fabrics of multilevel hierarchy after filter deposited thereon, air drying.
(5) further electronation is carried out using hydrazine hydrate to dried graphene fiber non-woven fabrics.
By above step, obtained graphene fiber non-woven fabrics has multistage pleated structure, but due to being preheated in step 2
Drying temperature is too high, reduces the hydrophily of graphene fiber so that final graphene fiber surface folding degree is not high, fiber
Surface micro-structure is mostly to be distributed loose strip ridge projections.The specific surface area of non-woven fabrics is 63m2/ g, conductance 88S/m.
Embodiment 4:
Step 1-4 is with embodiment 1, without the further reduction of step 5.Gained graphene fiber non-woven fabrics has multistage
Pleated structure, conductance 1.2S/m.
Embodiment 5:
Step 1 is:It is 5mg/mL graphene oxide/DMF solution for spinning solution using concentration, acetic acid
Ethyl ester is that coagulating bath carries out continuous wet spinning.
Step 2-5 is the same as embodiment 2.
Two pieces of equal areas (~0.8cm are taken after obtaining more fold graphene non-woven fabrics2) non-woven fabrics as super capacitor
The positive and negative electrode of device, using filter paper as barrier film between two-stage, 1M H2SO4Solution is assembled into ultracapacitor as electrolyte.Through surveying
Examination, the ultracapacitor quality specific capacitance based on more fold graphene non-woven fabrics are up to 244F/g (current density 1A/g),
Area specific capacitance is up to 1060mF/cm2(current density 1mA/cm2), show higher electro-chemical activity.
Claims (7)
- A kind of 1. graphene fiber of fold, it is characterised in that formed by the graphene film accumulation of fold, the graphene film Pleated structure has defective graphene film and formed under capillary forces.
- 2. a kind of preparation method of graphene fiber, it is characterised in that comprise the following steps:(1) continuous wet spinning is carried out by spinning solution of graphene oxide dispersion.(2) obtained graphene oxide fiber is placed into more than 12h in room temperature, then vacuum is done at a temperature of not higher than 80 DEG C Dry 3h.(3) fully dry graphene oxide fiber is immersed in the water heating kettle equipped with water and carries out hydro-thermal process, hydro-thermal process Temperature range be 80-200 DEG C.(4) graphene fiber formed by the graphene oxide sheet accumulation of fold is obtained after air drying.
- 3. according to the method for claim 2, it is characterised in that spinning solution is the aqueous solution or N, N- diformazan of graphene oxide Base formamide solution.Corresponding, the coagulating bath that spinning process uses is calcium chloride/water/alcohol mixeding liquid or ethyl acetate.
- 4. a kind of High-performance graphene fabric nonwoven cloth, it is characterised in that as the graphene fiber phase lap described in claim 1 Connect to form network, the graphene fiber at grid node mutually merges.
- 5. a kind of preparation method of High-performance graphene fabric nonwoven cloth, it is characterised in that will be weighed using high shear agitation machine Profit requires that the graphene fiber in 2 steps 3 after hydro-thermal process blends into the chopped fiber that length is 1-7mm in aqueous, then Graphene fiber non-woven fabrics is obtained after filter deposited thereon, air drying.
- 6. according to the method for claim 5, it is characterised in that the rotating speed of high shear agitation is 3000-8000rpm.
- 7. according to the method for claim 5, it is characterised in that this method is also included dried graphene fiber nonwoven Cloth is further reduced.Restoring method is to be carried out using chemical reducing agents such as hydroiodic acid, hydrazine hydrate, Vitamin C, sodium borohydrides Reduction or 100-3000 DEG C of thermal reduction.
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CN201710670077.3A CN107502995B (en) | 2017-08-08 | 2017-08-08 | Graphene fiber and graphene fiber non-woven fabrics of a kind of fold and preparation method thereof |
PCT/CN2018/084334 WO2019029191A1 (en) | 2017-08-08 | 2018-04-25 | Draped graphene fiber and graphene fiber non-woven fabric and preparation method therefor |
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CN108707998A (en) * | 2018-04-11 | 2018-10-26 | 杭州牛墨科技有限公司 | Graphene fiber and graphene fiber non-woven fabrics of a kind of fold and preparation method thereof |
CN108708076A (en) * | 2018-04-09 | 2018-10-26 | 南京捷纳思新材料有限公司 | The method that wet spinning prepares core/shell polyurethane-carbon nanotube conducting non-woven fabrics |
CN108914251A (en) * | 2018-07-09 | 2018-11-30 | 杭州高烯科技有限公司 | A kind of azepine graphite fibre and preparation method thereof |
CN109267416A (en) * | 2018-09-21 | 2019-01-25 | 杭州高烯科技有限公司 | A kind of reduced graphene fibrous paper and preparation method thereof from fusion |
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CN113388905A (en) * | 2021-06-15 | 2021-09-14 | 广西大学 | Self-crimping preparation method and application of hollow graphene fiber |
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