CN105603581A - Graphene fiber capable of achieving raid response and preparation method thereof - Google Patents
Graphene fiber capable of achieving raid response and preparation method thereof Download PDFInfo
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- CN105603581A CN105603581A CN201610049310.1A CN201610049310A CN105603581A CN 105603581 A CN105603581 A CN 105603581A CN 201610049310 A CN201610049310 A CN 201610049310A CN 105603581 A CN105603581 A CN 105603581A
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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 graphene fiber capable of achieving rapid response and a preparation method thereof. The method comprises the steps that a graphene oxide film is heated to 500-800 DEG C at the speed of 0.1-1 DEG C/min, the temperature is kept constant for 0.5-2 h, and then the graphene oxide film is heated to 1000-1300 DEG C at the speed of 1-3 DEG C/min, the temperature is kept constant for 0.5-3 h, then, the graphene oxide film is heated to 2000-3000 DEG C at the speed of 5-8 DEG C/min, the temperature is kept constant for 0.5-4 h, a graphene film is obtained, and the graphene fiber is obtained after uniform winding. The fiber can achieve rapid response under the high temperature of 30-420 DEG C within a short period of time of 1-20 s under the safety voltage of 0.5-5 V, the graphene fiber can be wound around a heating body and can also be woven into an electric heating cloth for use, the defects that a traditional electric heating material is slow in temperature rise, high in applied voltage and the like are overcome, and the graphene fiber is the good electric heating material and has the industrial prospect.
Description
Technical field
The present invention relates to graphene fiber of a kind of quick response and preparation method thereof.
Background technology
Within 2004, Univ Manchester UK's peace moral is strong. and Jim and Constantine. professor Nuo Woxiaoluofu adopt micro-Mechanical stripping method is isolated two-dimentional Graphene crystal first, and because starting on two-dimentional grapheme materialProperty experiment obtains the Nobel Prize in physics of 2010, and grapheme material causes that whole world scientists is wide thusGeneral research. Graphene has high fracture strength and Young's modulus, electric property excellence. Graphene has altogetherYoke structure, shows abundant chemical property, can carry out finishing by different chemical reactions,Obtain a series of chemical derivatives. Grapheme material has excessive heat conductance, and experiment value reaches 5000W/mK,Can be used as excellent thermo electric material. Traditional electrical hot material, as nichrome, exists cost high, and density is large,Quality weight, the shortcomings such as yielding and processing technology complexity, are not suitable for irregular substrate, and Graphene materialMaterial pliability is good, and quality is light, and manufacture craft is simple, and the rate of heat addition is fast, and thermal response temperature is high, can be forThe substrate of various shapes, and can make can only human body heating fabric, for infrared therapeutic etc., is hopefulSubstitute the extensive use of traditional electrical hot material.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of quick response graphene fiber andIts preparation method.
The object of the invention is to be achieved through the following technical solutions: a kind of graphene fiber of quick response,Described fiber is the two Archimedian screw structures that are made up of graphene nanometer sheet, and sheet interlayer spacing is 0.336nm,The carbon-to-oxygen ratio of fiber is 52.66-98, and XRD diffraction peak is set to 26.4 °.
A preparation method for the graphene fiber of quick response, its step is as follows:
(1) prepare the graphene oxide film that thickness is 0.8～50 μ m;
(2) be warmed up to 500-800 DEG C with the speed of 0.1-1 DEG C/min, insulation 0.5-2h, then with 1-3 DEG C/minSpeed be warmed up to 1000-1300 DEG C, insulation 0.5-3h, be then warmed up to the speed of 5-8 DEG C/min2000-3000 DEG C, insulation 0.5-4h;
(3) graphene film after step 3 heat treatment is cut into graphene strips, graphene strips one end is fixed,The other end is connected with the rotor that rotating speed is turn/min of 50-250, radially reels after 1-5mim, obtains fastThe graphene fiber of response.
Further, the graphene oxide film in described step (1) passes through the aqueous solution of graphene oxide trueEmpty suction method, spin-coating method, the one in the methods such as spraying process or plastic film mulch prepares.
Further, described graphene oxide obtains by native graphite chemical oxidation stripping method.
The present invention is compared with traditional heating element heater nichrome etc., and graphene fiber can within a short period of timeRealize the quick response to high temperature, reason is that the thermal capacitance of Graphene is very little, and thermal mass is also very little, producesHeat can not assemble in a large number and produce the dissipation of heat, after high-temperature process, a large amount of oxygen-containing functional groups are removed,Conjugated structure is restored, and electric conductivity is greatly improved. Further, by reeling, make GrapheneThe internal voids of fiber is extruded gradually, and graphene fiber has winding-structure closely, therefore resistance decreasing,Thereby make graphene fiber there is better electrocaloric effect. Under identical voltage, heating rate and saturatedTemperature is all significantly increased. Under safe voltage 0.5V-5V, can in very short time 1s-20s, realize heightThe quick response that temperature is 30 DEG C-420 DEG C. Beneficial effect is:
1. the raw material of Graphene is graphite, with low cost, and raw material is extensively easy to get.
2. the length of graphene fiber and diameter are controlled, are easy to preparation.
3. overcome the shortcoming of traditional electrical hot material fragility, can bend arbitrarily and be attached on substrate.
4. compared with traditional electrical hot material, there is the rate of heat addition and the rate of temperature fall of superelevation, the temperature-responsive of superelevation.
5. the operating voltage of graphene fiber is lower, can be for human body.
6. graphene fiber can single use or is woven into fabric, uses as electric heating cloth.
Brief description of the drawings
The SEM figure of Fig. 1 fiber;
Fig. 2 is the schematic diagram of radially reeling;
Fig. 3 is the gray-scale map of the Infrared Thermogram of graphene fiber.
Detailed description of the invention
As shown in Figure 1, the graphene fiber of a kind of quick response of the present invention, described fiber is by graphene nano(structure can bibliography BiscrollingNanotubeSheetsand for two Archimedian screw structures of sheet compositionFunctionalGuestsintoYarns), sheet interlayer spacing is 0.336nm, and the carbon-to-oxygen ratio of fiber is 52.66, XRDDiffraction peak is set to 26.5 °.
The preparation method of the graphene fiber of a kind of super stretchable high conduction of the present invention, step is as follows:
(1) obtain graphene oxide by native graphite chemical oxidation stripping method, preparing thickness is 0.8～50 μ mGraphene oxide film;
(2) thickness of being prepared by step 1 is the graphene oxide film of 0.8～50 μ m, according to table 1～table 3Shown mode is heat-treated, and obtains graphene film.
(3) graphene film after treatment step 2 is cut into graphene strips, graphene strips one end is fixed,The other end is connected with the rotor that rotating speed is 80 turn/min, radially reel after 3min (one end is fixed, anotherEnd constantly rotates under rotor drives, and is similar to and makes cord, and as shown in Figure 2), different heat treatment mode obtainsThe electric property of each product in table 1～table 3.
Wherein the graphene oxide film in step (1) can pass through vacuum filtration method, spin-coating method or spraying process etc.One in method prepares.
Table 1
Table 2
Table 3
From table 1～table 3, can find out, the electric heating property of this material is mainly by internal oxidation graphene film structureReparation situation, functional group come off and high temperature under carbon conjugated structure reparation determine.
In table 1, by A1 relatively B1 C1 D1 E1, the temperature of A1 is too low, is not enough to remove easily most ofThe functional group of degraded, causes a large amount of generations fast of gas in second step pyroprocess, at high temperature tears lamellaStructure; E1 excess Temperature, produces gas too fast, can tear in a large number material internal structure, both can makeDeterioration in material properties. Have only at B1, C1, D1 temperature, functional group can slowly and thoroughly remove, to protectBarrier material property. By C1 relatively F1 G1 H1, F1 heating rate is too low, air release is too slow;H1 temperature-rise period is too fast, and air release is too fast, tears material internal structure, is unfavorable for forming transmission channel.By C1 relatively I1 J1 K1 L1 M1, I1 temperature retention time is too short, can not ensure the degraded of most of functional group;M1 insulating process is long, can absorb the tar of stove the inside, is unfavorable for the lifting of performance. J1, K1, L1Above above-mentioned two kinds of unfavorable conditions are just in time avoided
In table 2, by A2 relatively B2 C2 D2 E2, A2 heating rate is too low, has a strong impact on electric heating property.E2 programming rate is too high, can tear Graphene interlayer structure, makes degradation. Have B2, C2, D2 onlyProgramming rate under, just can be capable not only ensured structure but also ensured the electric conductivity of Graphene. By comparingC2 F2 G2 H2, F2 temperature is too low, and stable functional group can not fully be departed from, follow-up graphitedIn process, easily transition discharges gas, destroys internal structure; By C2 relatively I2 J2 K2 L2 M2, I2 protectsThe temperature time is too short, and stable functional group can not fully come off; M2 overlong time, the easy tar adsorption of Graphene,Be unfavorable for the lifting of Graphene performance; And under C2, J2, K2 condition, both can ensure stabilising functional group fullyCome off, can avoid again the puzzlement of tar.
In table 3, by A3 relatively B3 C3 D3 E3, A3 heating rate is too low, stabilising functional group comes offExcessively slow, be unfavorable for the formation of conductive network; E3 temperature-rise period is too fast, air release and high-temperature expansion mistakeHurry up, easily destroy structure. Only have in the situation of B3, C3, D3, the Graphene of conductive network could be stablizedFormation, the structure on Graphene could be repaired slowly. By C3 relatively F3 G3 H3 I3, F3 terminalTemperature is too low, and graphene-structured reparation is perfect not, so various performance is all very poor; I3 outlet temperature is too high,Graphene can be vaporized; At the temperature of C3, G3, H3, could both ensure the reparation of graphene-structured, again notCan be vaporized. By C3 relatively J3 K3 L3 M3, J3 temperature retention time is too low, graphene-structured can not be filledDivide and repair, M3 temperature retention time is long, also can make to adsorb the tar in body of heater, affects performance.
Claims (4)
1. the graphene fiber responding fast, is characterized in that, described fiber is for to be rolled up by graphene sheet layerAround the two Archimedian screw structures that form, sheet interlayer spacing is 0.336nm, and the carbon-to-oxygen ratio of fiber is 52.66-98,XRD diffraction peak is set to 26.4 °.
2. a preparation method for the graphene fiber responding fast, is characterized in that, its step is as follows:
(1) prepare the graphene oxide film that thickness is 0.8～50 μ m;
(2) be warmed up to 500-800 DEG C with the speed of 0.1-1 DEG C/min, insulation 0.5-2h, then with 1-3 DEG C/minSpeed be warmed up to 1000-1300 DEG C, insulation 0.5-3h, be then warmed up to the speed of 5-8 DEG C/min2000-3000 DEG C, insulation 0.5-4h;
(3) graphene film after step 3 heat treatment is cut into graphene strips, graphene strips one end is fixed,The other end is connected with the rotor that rotating speed is turn/min of 50-250, radially reels after the 1-5min time, obtains fastThe graphene fiber of speed response.
3. method according to claim 2, is characterized in that, the graphite oxide in described step (1)The aqueous solution of graphene oxide is passed through vacuum filtration method, spin-coating method, the methods such as spraying process or plastic film mulch by alkene filmIn one prepare.
4. method according to claim 3, is characterized in that, described graphene oxide passes through native graphiteChemical oxidation stripping method obtains.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105657877A (en) * | 2016-01-25 | 2016-06-08 | 浙江大学 | Super-stretchable graphene electro-thermal film 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 |
| WO2021004692A1 (en) | 2019-07-10 | 2021-01-14 | Robert Bosch Gmbh | Method for producing graphene fibres |
| WO2021115669A1 (en) | 2019-12-09 | 2021-06-17 | Robert Bosch Gmbh | Electrical conductor made of graphene and/or carbon nanotubes having coated joints |
| 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 |
| 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 |
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| CN104085143A (en) * | 2014-05-29 | 2014-10-08 | 深圳市铭晶科技有限公司 | Preparation method of composite heat conduction graphene film and composite heat conduction graphene film |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105657877A (en) * | 2016-01-25 | 2016-06-08 | 浙江大学 | Super-stretchable graphene electro-thermal film 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 |
| US11939703B2 (en) | 2019-07-10 | 2024-03-26 | Robert Bosch Gmbh | Method for producing graphene fibres |
| WO2021004692A1 (en) | 2019-07-10 | 2021-01-14 | Robert Bosch Gmbh | Method for producing graphene fibres |
| WO2021115669A1 (en) | 2019-12-09 | 2021-06-17 | Robert Bosch Gmbh | Electrical conductor made of graphene and/or carbon nanotubes having coated joints |
| US11875913B2 (en) | 2019-12-09 | 2024-01-16 | Robert Bosch Gmbh | Electrical conductor made of graphene and/or carbon nanotubes having 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 |
| WO2023052116A1 (en) | 2021-09-30 | 2023-04-06 | Robert Bosch Gmbh | Electric machine and method for placing at least one electrical composite conductor into at least one groove of a stator or rotor for an electric machine |
| DE102022203207A1 (en) | 2022-03-31 | 2023-10-05 | Robert Bosch Gesellschaft mit beschränkter Haftung | Process for producing a graphene film |
| WO2023186456A1 (en) | 2022-03-31 | 2023-10-05 | Robert Bosch Gmbh | Method 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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Effective date of registration: 20190905 Address after: 313199 Room 830, 8th Floor, Changxing World Trade Building, 1278 Mingzhu Road, Changxing Economic Development Zone, Huzhou City, Zhejiang Province Patentee after: Changxin de Technology Co., Ltd. Address before: 310058 Xihu District, Zhejiang, Yuhang Tong Road, No. 866, No. Patentee before: Zhejiang University |