CN105603581B - A kind of graphene fiber of quick response and preparation method thereof - Google Patents
A kind of graphene fiber of quick response and preparation method thereof Download PDFInfo
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- CN105603581B CN105603581B CN201610049310.1A CN201610049310A CN105603581B CN 105603581 B CN105603581 B CN 105603581B CN 201610049310 A CN201610049310 A CN 201610049310A CN 105603581 B CN105603581 B CN 105603581B
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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
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/42—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments
Abstract
The invention discloses a kind of graphene fiber of quick response and preparation method thereof.Method is：Graphene oxide membrane is warming up to 500 800 DEG C with 0.1 1 DEG C/min speed, it is incubated 0.5 2h, again 1,000 1300 DEG C are warming up to 13 DEG C/min speed, it is incubated 0.5 3h, then 2,000 3000 DEG C are warming up to 58 DEG C/min speed, are incubated 0.5 4h, obtain graphene film, uniformly obtain graphene fiber after winding again；The fiber can realize the quick response to 420 DEG C of high temperature 30 DEG C under safe voltage 0.5V 5V in very short time 1s 20s, graphene fiber can be wrapped on calandria, electric heating cloth use can also be woven into, overcome the shortcomings of traditional thermo electric material heating is slow, application voltage is high, it is excellent thermo electric material, possesses industrial prospect.
Description
Technical field
The present invention relates to a kind of graphene fiber of quick response and preparation method thereof.
Background technology
The strong Jims of Univ Manchester UK's peace moral in 2004 and Constantine Nuo Woxiao loves professor use micromechanics
Stripping method isolates two-dimensional graphene crystal first, and because the initiative experiment on two-dimensional graphene material obtains 2010
Year Nobel Prize in physics, thus grapheme material cause whole world scientists widely to be studied.Graphene has high disconnected
Resistance to spalling and Young's modulus, electric property are excellent.Graphene has conjugated structure, shows abundant chemical property, Ke Yitong
Different chemical reactions is crossed to carry out surface modification, obtains a series of chemical derivatives.Grapheme material has superelevation thermal conductivity,
Experiment value reaches 5000W/mK, can be as excellent thermo electric material.Traditional thermo electric material such as nichrome, cost height be present,
Density is big, quality weight, the shortcomings of yielding and processing technology complexity, is not suitable for irregular substrate, and grapheme material is soft
Good toughness, light weight, manufacture craft is simple, and the rate of heat addition is fast, and thermal response temperature is high, can be used for variously-shaped substrate, and
And can make can only human body heating fabric, for infrared therapeutic etc., be hopeful to substitute traditional thermo electric material extensive use.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided a kind of graphene fiber of quick response and its preparation
Method.
The purpose of the present invention is achieved through the following technical solutions：A kind of graphene fiber of quick response, the fibre
Double Archimedian screw structures to be made up of graphene nanometer sheet are tieed up, piece interlamellar spacing is 0.336nm, and the carbon-to-oxygen ratio of fiber is
52.66-98 XRD diffraction peaks are set to 26.4 °.
A kind of preparation method of the graphene fiber of quick response, it the step of it is as follows：
(1) graphene oxide membrane that thickness is 0.8~50 μm is prepared；
(2) 500-800 DEG C is warming up to 0.1-1 DEG C/min speed, is incubated 0.5-2h, then the speed with 1-3 DEG C/min
1000-1300 DEG C is warming up to, is incubated 0.5-3h, is then warming up to 2000-3000 DEG C with 5-8 DEG C/min speed, is incubated 0.5-
4h,；
(3) graphene film after step 3 is heat-treated is cut into graphene strips, graphene strips one end is fixed, the other end
It is connected with the rotor that rotating speed is 50-250 turns/min, after radially winding 1-5mim, obtains the graphene fiber of quick response.
Further, the aqueous solution of graphene oxide is passed through vacuum filtration by the graphene oxide membrane in the step (1)
One kind in the methods of method, spin-coating method, spraying process or plastic film mulch is prepared.
Further, the graphene oxide is obtained by native graphite chemical oxidation stripping method.
It is of the invention compared with traditional heating element heater nichrome etc., graphene fiber can be realized pair within a short period of time
The quick response of high temperature, reason are the thermal capacitance very littles of graphene, and thermal mass also very little, caused heat can not largely assemble and
The dissipation of heat is produced, after high-temperature process, substantial amounts of oxygen-containing functional group is removed, and conjugated structure is restored, and electric conductivity obtains
To very big raising.Further pass through winding so that the internal voids of graphene fiber are gradually extruded, and graphene fiber has
Close winding-structure, therefore resistance diminishes, so that graphene fiber has more preferable electrocaloric effect.In identical voltage
Under, heating rate and saturation temperature are all significantly increased.Can be real in very short time 1s-20s under safe voltage 0.5V-5V
Now to the quick response of 30 DEG C -420 DEG C of high temperature.Beneficial effect is：
1. the raw material of graphene is graphite, cost is cheap, and raw material is easy to get extensively.
2. the length and controlled diameter of graphene fiber, easily prepared.
3. the shortcomings that overcoming traditional thermo electric material fragility, arbitrarily it can bend and be attached on substrate.
4. compared with traditional thermo electric material, there is the rate of heat addition and rate of temperature fall of superelevation, the temperature-responsive of superelevation.
5. the operating voltage of graphene fiber is relatively low, it can be used for human body.
6. graphene fiber can with it is single use or be woven into fabric, used as electric heating cloth.
Brief description of the drawings
The SEM figures of Fig. 1 fibers；
Fig. 2 is the schematic diagram radially wound；
Fig. 3 is the gray-scale map of the Infrared Thermogram of graphene fiber.
Embodiment
As shown in figure 1, a kind of graphene fiber of quick response of the present invention, the fiber is to be made up of graphene nanometer sheet
Double Archimedian screw structures (structure refers to document Biscrolling Nanotube Sheets and Functional
Guests into Yarns), piece interlamellar spacing is 0.336nm, and the carbon-to-oxygen ratio of fiber is set to for 52.66, XRD diffraction peaks
26.5°。
A kind of preparation method of super stretchable highly conductive graphene fiber of the present invention, step are as follows：
(1) graphene oxide is obtained by native graphite chemical oxidation stripping method, prepares the oxidation that thickness is 0.8~50 μm
Graphene film；
(2) thickness prepared by step 1 is 0.8~50 μm of graphene oxide membrane, in the way of shown in 1~table of table 3
It is heat-treated, obtains graphene film.
(3) graphene film after step 2 is handled is cut into graphene strips, and graphene strips one end is fixed, the other end with
Rotating speed is that 80 turns/min rotor is connected, and radially (one end is fixed, and the other end constantly turns under rotor drive after winding 3min
It is dynamic, similar to making cord, as shown in Figure 2), the electric property for each product that different heat treatment mode obtains is shown in Table 1~table 3.
Graphene oxide membrane wherein in step (1) can be by the methods of vacuum filtration method, spin-coating method or spraying process
One kind be prepared.
Table 1
Table 2
Table 3
As can be seen that the electric heating property of this material is mainly by internal oxidation graphene film structure repair feelings from 1~table of table 3
Condition, i.e. functional group come off and high temperature under carbon conjugated structure reparation determine.
In table 1, by compare A1 B1 C1 D1 E1, A1 temperature is too low, is not enough to remove most of degradable official
It can roll into a ball, cause gas in second step pyroprocess largely quickly to produce, tear lamellar structure at high temperature；E1 temperature is too high, production
Angry body is too fast, can largely tear material internal structure, both can cause deterioration in material properties.Have only in B1, C1, D1 temperature
Under, functional group can slowly and thoroughly remove, to ensure material property.By compare C1 F1 G1 H1, F1 heating rates are too low,
Gas release is excessively slow；H1 temperature-rise periods are too fast, and gas release is too fast, tear material internal structure, are unfavorable for forming transmission
Passage.By compare C1 I1 J1 K1 L1 M1, I1 soaking times are too short, it is impossible to ensure the degraded of most of functional group；M1 is protected
Warm process is long, can absorb the tar inside stove, is unfavorable for the lifting of performance.J1, K1, L1 just avoid the above above-mentioned two
Kind unfavorable conditions
In table 2, by compare A2 B2 C2 D2 E2, A2 heating rates are too low, have a strong impact on electric heating property.E2 heating speed
Height is spent, graphene interlayer structure can be torn so that degradation.Have only under B2, C2, D2 programming rate, just can be capable
Not only ensure structure but also ensure the electric conductivity of graphene.By compare C2 F2 G2 H2, F2 temperature is too low so that stable function
Group can not be sufficiently disengaged from, and easily transition discharges gas during subsequently graphited, destroy internal structure；By compare C2
I2 J2 K2 L2 M2, I2 soaking times are too short, and stable functional group can not fully come off；M2 overlong times, graphene are easy
Tar adsorption, it is unfavorable for the lifting of graphene performance；And it can both ensure that stabilising functional group's was fully de- under the conditions of C2, J2, K2
Fall, and can avoids the puzzlement of tar.
In table 3, by compare A3 B3 C3 D3 E3, A3 heating rates are too low, and most stabilising functional group comes off excessively slow, no
Beneficial to the formation of conductive network；E3 temperature-rise periods are too fast, and gas release and high-temperature expansion are too fast, are easily destroyed structure.Only
In the case of B3, C3, D3, formation that the graphene of conductive network could be stablized, the structure on graphene could be repaired slowly.
By compare C3 F3 G3 H3 I3, F3 outlet temperatures are too low, graphene-structured repair it is not perfect enough, so various performances are all very
Difference；I3 outlet temperatures are too high, and graphene can be vaporized；Repairing for graphene-structured could both be ensured at a temperature of C3, G3, H3
It is multiple, it will not be vaporized again.By compare C3 J3 K3 L3 M3, J3 soaking times are too low, and graphene-structured can not be repaiied fully
Multiple, M3 soaking times are long, can also to adsorb the tar in body of heater, influence performance.
Claims (3)
- A kind of 1. preparation method of the graphene fiber of quick response, it is characterised in that it the step of it is as follows：（1）Prepare the graphene oxide membrane that thickness is 0.8 ~ 50 μm；（2）500-800 DEG C is warming up to 0.1-1 DEG C/min speed, is incubated 0.5-2h, then heat up with 1-3 DEG C/min speed To 1000-1300 DEG C, 0.5-3h is incubated, is then warming up to 2000-3000 DEG C with 5-8 DEG C/min speed, is incubated 0.5-4h；（3）Graphene film after step 2 is heat-treated is cut into graphene strips, and graphene strips one end is fixed, and the other end is with turning Speed is connected for 50-250 turns/min rotor, after radially winding the 1-5min times, obtains the graphene fiber of quick response.
- 2. according to the method for claim 1, it is characterised in that the step（1）In graphene oxide membrane will aoxidize stone The aqueous solution of black alkene is by vacuum filtration method, spin-coating method, and one kind in spraying process or plastic film mulch is prepared.
- 3. according to the method for claim 2, it is characterised in that the graphene oxide is shelled by native graphite chemical oxidation Obtained from method.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105657877B (en) * | 2016-01-25 | 2018-08-14 | 浙江大学 | Super stretchable graphene Electric radiant Heating Film of one kind and preparation method thereof |
| DE102018200236A1 (en) | 2018-01-09 | 2019-07-11 | Robert Bosch Gmbh | Process for producing graphene fibers, graphene fiber, yarn, electrical component and electrical conductor |
| DE102018218676A1 (en) | 2018-10-31 | 2020-04-30 | Robert Bosch Gmbh | Cable for a hand machine tool |
| DE102018222698A1 (en) | 2018-12-21 | 2020-06-25 | Robert Bosch Gmbh | Holding device for an electric motor |
| DE102019210211A1 (en) | 2019-07-10 | 2021-01-14 | Robert Bosch Gmbh | Process for the production of graphene fibers |
| DE102019219184A1 (en) | 2019-12-09 | 2021-06-10 | Robert Bosch Gmbh | Electrical conductor made of graphene and / or carbon nanotubes with coated joints |
| DE102021210974A1 (en) | 2021-09-30 | 2023-03-30 | Robert Bosch Gesellschaft mit beschränkter Haftung | Electrical machine and method for inserting at least one electrical conductor assembly into at least one slot of a stator or rotor for an electrical machine |
| DE102022203207A1 (en) | 2022-03-31 | 2023-10-05 | Robert Bosch Gesellschaft mit beschränkter Haftung | Process for producing a graphene film |
| CN115180620A (en) * | 2022-06-22 | 2022-10-14 | 山东利特纳米技术有限公司 | Preparation method of graphite film |
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