CN103320881B - A kind of device and method of preparing skin-core structure conductive carbon nanotube composite fibre - Google Patents
A kind of device and method of preparing skin-core structure conductive carbon nanotube composite fibre Download PDFInfo
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- CN103320881B CN103320881B CN201310299160.6A CN201310299160A CN103320881B CN 103320881 B CN103320881 B CN 103320881B CN 201310299160 A CN201310299160 A CN 201310299160A CN 103320881 B CN103320881 B CN 103320881B
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Abstract
The invention discloses a kind of device and method of preparing skin-core structure conductive carbon nanotube composite fibre. Described device comprises bobbin I, is provided with the container of perforation, heater, feed carrier and bobbin II, and described bobbin I and bobbin II are all connected with speed control motor. Described method be first by from bobbin I extract out carbon nano-tube fibre by boring a hole through container, being fixed on after heater and feed carrier in bobbin II successively, then the conductive polymer solution of preparation is added in container, open speed control motor, make carbon nano-tube fibre at the uniform velocity to pass through conductive polymer solution, and open heater simultaneously, make the composite fiber rapid solidification forming; Finally make the composite fibre after solidifying be collected in bobbin II through feed carrier. The prepared composite fibre of the present invention has the operability of common yarn, the requirement of the subsequent treatment process such as can meet stretching, weave, and applicable scale.
Description
Technical field
The present invention relates to a kind of device and method of preparing skin-core structure conductive carbon nanotube composite fibre, specifically, relate toA kind of system of the skin-core structure conductive carbon nanotube composite fibre taking carbon nano-tube fibre as sandwich layer, taking conducting polymer as cortexStandby device and method.
Background technology
CNT was found to start just to become the focus of scientific research from 1991, its research now related to chemistry, physics,Multiple fields such as biology, microelectronics, materialogy. CNT is a kind of typical monodimension nanometer material, is divided into single wall carbon and receivesMitron and multi-walled carbon nano-tubes, be by single or multiple lift graphite linings structure around center by curling form seamless of certain helical angleNanoscale pipe, it has mechanical characteristic and unique electrical properties of high strength, ultralight amount. In order to realize carbon nanometerPipe is in the application of every field, CNT must be compounded to form to the material of macro-scale through assembling or with other materials,Wherein carbon nano-tube fibre technology is one of tool potentiality and the significant direction of achievement.
The preparation method of carbon nano-tube fibre has dry spinning method, direct spinning and wet spinning process at present. Dry method is spunSilk method is first to adopt chemical vapour deposition technique to grow even grade carbon nano pipe array of micron order, then extracts out from arrayThe carbon nano-tube film of certain width, is then twisted fiber by twisting technology, and this method is called again two-step method. Direct SpinningSilk method is directly to prepare carbon nano-tube fibre by twisting in the process of High Temperature Gas phase reaction synthesizing continuous carbon nanometer tube, claims againFor one-step method. Wet spinning is that carbon nanotube dust and high polymer are mixed into dispersion liquid, then through being pressed through coagulating bathOr utilize electrospinning process preparation, carbon nano-tube fibre phosphorus content prepared by this method is lower, and mechanics and electrical propertyCan be all poor compared with first two method.
The carbon nano-tube fibre intensity (being greater than 500MPa) that dry spinning and direct spinning method obtain and pliability all can be withCurrent commercial natural fiber or chemical fibre compare favourably, and its excellent electric conductivity has more been given carbon nano-tube fibre in intelligenceThe using value of textile field. Because carbon nano-tube fibre diameter is at 5 μ m～20 μ m, single-root carbon nano-tube fiber is heldThe maximum pull being subject to is only tens lis of oxen, and even several lis of oxen, and fiber surface CNT wearability is poor, and is not suitable forDirectly weave, thereby by carbon nano-tube fibre and the compound necessary condition that becomes further application carbon nano-tube fibre of polymer.As the preparation method of the high-performance carbon nanotube fiber of mentioning in Chinese patent CN101967699B, this method is to adoptDry spinning is prepared in the process of carbon nano-tube fibre the carbon nano-tube film extracting in array with heat curing-type polyamic acid/N-Methyl pyrrolidone solution impregnation forms carbon nano tube/polyamide 6 amino acid composite fibre after twisting, and it is cured to processingEnd form becomes nanometer tube/polyimide composite fiber. The diameter of this composite fibre does not have too large compared with carbon nano-tube fibre diameterChange, in composite fibre, the percent by volume of polyimides is only below 5%, and polyimide polymer reticulates structure dispersionIn composite fibre.
Summary of the invention
For the existing the problems referred to above of prior art and application demand, the object of this invention is to provide one and prepare skin-core structureThe device and method of conductive carbon nanotube composite fibre.
For achieving the above object, the technical solution used in the present invention is as follows:
Prepare a device for skin-core structure conductive carbon nanotube composite fibre, comprise bobbin I, be provided with perforation container, addHot charging is put, feed carrier and bobbin II, the fiber of being extracted out by bobbin I successively through being provided with perforation container, heater andFeed carrier is fixed in bobbin II, and described bobbin I and bobbin II are all connected with speed control motor.
As a kind of preferred version, described bobbin I, the container that is provided with perforation, heater, feed carrier and bobbin IIVertical arrangement from bottom to top successively, described perforation is arranged on the center of container bottom.
The diameter of described perforation is preferably 30 μ m～100 μ m.
The material of described container is the corrosion-resistant plastics such as stainless steel, glass or polytetrafluoroethylene (PTFE).
Described container and heater can be one or more groups.
Use said apparatus to prepare the method for skin-core structure conductive carbon nanotube composite fibre, comprise the steps:
A) preparation conductive polymer solution, for subsequent use;
B) by from bobbin I extract out carbon nano-tube fibre by boring a hole through container, successively after heater and feed carrierBe fixed in bobbin II;
C) conductive polymer solution of step a) being prepared adds in container, opens speed control motor, makes carbon nano-tube fibre with evenSpeed process conductive polymer solution, and open heater simultaneously, make the composite fiber rapid solidification forming;
D) composite fibre after making to solidify is collected in bobbin II through feed carrier.
The mass percent concentration of described conductive polymer solution is recommended to be greater than 1%, is preferably 5%～10%.
Described conductive polymer solution is by polyvinyl alcohol, polyacrylonitrile, polyurethane, nylon, polyester, cellulose, silkwormAt least one in silk and water, dimethyl formamide, dimethylacetylamide, formamide, formic acid, carrene, three chloromethanesAt least one in alkane, acetone, methyl alcohol, ethylene bromide base triphenyl squama (being called again Schweizer reagent) is formulated.
Also can be suitable in described conductive polymer solution add nano-metal particle (for example: nano-Ag particles) to improveThe electric conductivity of composite fibre.
As a kind of preferred version, c), the degree of depth of controlling the conductive polymer solution in container remains at 5mm to step,And control carbon nano-tube fibre and at the uniform velocity pass through conductive polymer solution with the speed of 0.5mm/s～1mm/s, and control the thermal treatment zoneThe temperature in territory is 60～80 DEG C.
Described carbon nano-tube fibre can be that one-step method is directly spinned and obtains by chemical vapour deposition (CVD), can be also two-step methodBy being carried out to dry spinning preparation, carbon nano pipe array obtains; Described carbon nano-tube fibre can be single-root carbon nano-tube fibreDimension can be also the plying carbon nano-tube fibre after many twisting.
Skin-core structure conductive carbon nanotube composite fibre of the present invention is a kind of taking carbon nano-tube fibre as sandwich layer, to conduct electricityPolymer is the skin-core structure composite fibre of cortex.
Compared with prior art, the present invention has following beneficial effect:
The volume percent content that 1, can make polymeric skin is more than 5%, and the diameter of composite fibre exceedes 10 μ m'sSkin-core structure conductive carbon nanotube composite fibre.
2, the surface uniform of prepared skin-core structure conductive carbon nanotube composite fibre is smooth, without filoplume, has excellent resistingFrictional behaviour.
3, the tensile break strength of prepared skin-core structure conductive carbon nanotube composite fibre is higher than 50cN, at length directionOn electrical conductivity be not less than 500S/cm, there is the operability of common yarn, the subsequent treatment work such as can meet stretching, weaveThe requirement of skill.
4, preparation facilities is simple, and preparation technology is easy to operate, can realize continuous production, and manufacturing cycle is short, is applicable to scale.
Brief description of the drawings
Fig. 1 is a kind of structural representation of preparing skin-core structure conductive carbon nanotube composite fibre device that embodiment 1 provides;
Fig. 2 is the structural representation of the prepared skin-core structure conductive carbon nanotube composite fibre of embodiment 1;
Fig. 3 is a kind of structural representation of preparing skin-core structure conductive carbon nanotube composite fibre device that embodiment 2 provides;
Fig. 4 is the structural representation of the prepared skin-core structure conductive carbon nanotube composite fibre of embodiment 2.
In figure: 1, bobbin I; 2, container; 21, perforation; 22, conductive polymer solution; 3, heater; 4, leadYarn feeding device; 5, bobbin II; 6, speed control motor; A, carbon nano-tube fibre; B, composite fibre; A, sandwich layer; B, cortex;B1, the first cortex; B2, the second cortex.
Detailed description of the invention
Below in conjunction with specific embodiments and the drawings, further set forth the present invention. Should be understood that these embodiment are only for illustrating thisInvention but not limit the scope of the invention.
As shown in figures 1 and 3: a kind of device of preparing skin-core structure conductive carbon nanotube composite fibre of the present invention,Comprise bobbin I 1, be provided with container 2, heater 3, feed carrier 4 and the bobbin II 5 of perforation, extracted out by bobbin I 1Fiber is successively through being provided with the container 2 of perforation, being fixed in bobbin II 5 after heater 3 and feed carrier 4 successively,Described bobbin I 1 and bobbin II 5 are all connected with speed control motor 6.
As a kind of preferred version, described bobbin I 1, the container 2 that is provided with perforation, heater 3, feed carrier 4 andBobbin II 5 vertical arrangement from bottom to top successively, described perforation 21 is arranged on the bottom centre position of container 2; Described appearanceDevice 2 and heater 3 can be one group the composite fibre of preparation single skin cored structure (example as shown in Figure 1, for) orMany groups (example as shown in Figure 2, has the composite fibre of the multilayer skin-core structure of different polymeric skins for preparation).
The diameter of described perforation 21 is preferably 30 μ m～100 μ m, to guarantee being no matter single-root carbon nano-tube fiber or manyPlying carbon nano-tube fibre after twisting all can pass this hole by friction free, and can ensure the conductive polymer solution 22 in containerCan from this hole, not ooze out due to surface tension effects.
The material of described container 2 will be used the material that can not corroded by splendid attire conductive polymer solution 22 wherein, Ke YiweiThe corrosion-resistant plastics such as stainless steel, glass or polytetrafluoroethylene (PTFE).
Use said apparatus to prepare the method for skin-core structure conductive carbon nanotube composite fibre, comprise the steps:
A) preparation conductive polymer solution, for subsequent use;
B) by from bobbin I extract out carbon nano-tube fibre by boring a hole through container, successively after heater and feed carrierBe fixed in bobbin II;
C) conductive polymer solution of step a) being prepared adds in container, opens speed control motor, makes carbon nano-tube fibre with evenSpeed process conductive polymer solution, and open heater simultaneously, make the composite fiber rapid solidification forming;
D) composite fibre after making to solidify is collected in bobbin II through feed carrier.
The mass percent concentration of described conductive polymer solution is recommended to be greater than 1%, is preferably 5%～10%; Described leadsElectric polymer solution is at least one by polyvinyl alcohol, polyacrylonitrile, polyurethane, nylon, polyester, cellulose, silkPlant and water, dimethyl formamide, dimethylacetylamide, formamide, formic acid, carrene, chloroform, acetone, firstAt least one in alcohol, ethylene bromide base triphenyl squama (being called again Schweizer reagent) is formulated; Described conduction is poly-Also can be suitable in compound solution add nano-metal particle (for example: nano-Ag particles) to improve the electric conductivity of composite fibre.
As a kind of preferred version, c), the degree of depth of controlling the conductive polymer solution in container remains at 5mm to step,And control carbon nano-tube fibre and at the uniform velocity pass through conductive polymer solution with the speed of 0.5mm/s～1mm/s, and control the thermal treatment zoneThe temperature in territory is 60～80 DEG C.
Described carbon nano-tube fibre can be that one-step method is directly spinned and obtains by chemical vapour deposition (CVD), can be also two-step methodBy being carried out to dry spinning preparation, carbon nano pipe array obtains; Described carbon nano-tube fibre can be single-root carbon nano-tube fibreDimension can be also the plying carbon nano-tube fibre after many twisting.
Skin-core structure conductive carbon nanotube composite fibre of the present invention is a kind of taking carbon nano-tube fibre as sandwich layer, to conduct electricityPolymer is the skin-core structure composite fibre of cortex, and the volume percent content of polymeric skin is more than 5%, and composite fibreDiameter exceed 10 μ m.
Embodiment 1: prepare polyvinyl alcohol/CNT single skin cored structure composite fibre
A, 5g polyvinyl alcohol is dissolved in deionized water, is mixed with mass percent concentration and is 10% polyvinyl alcohol water solution;
B, use Fig. 1 shown device, the head end that diameter is about to the carbon nano-tube fibre a of 30 μ m takes out from bobbin I 1,, then after heater 3 and feed carrier 4, be fixed in bobbin II 5 successively through container 2 by perforation 21;
C, the polyvinyl alcohol water solution that step a) is prepared add in container 2, and control polyvinyl alcohol water solution 22 whereinThe degree of depth be always 5mm, open speed control motor 6 make carbon nano-tube fibre a with the speed of 0.5mm/s at the uniform velocity through being contained inPolyvinyl alcohol water solution 22 in container 2; Open heater 3, the temperature of controlling heating region is 60～80 DEG C simultaneously,Make the carbon nano tube composite fibre rapid curing being infiltrated by polyvinyl alcohol water solution; Make the composite fibre b process guide after solidifyingDevice 4 is collected in bobbin II 5.
Fig. 2 is the structural representation of prepared composite fibre, as seen from Figure 2: prepared composite fibre is individual layer core-skinStructure: carbon nano-tube fibre layer is sandwich layer A, conductive polymer coating (polyvinyl alcohol layer) is cortex B.
Embodiment 2: prepare polyurethane/polyvinyl alcohol/carbon nanotube multilayer skin-core structure composite fibre
A, 2.5g polyvinyl alcohol is dissolved in deionized water, is mixed with mass percent concentration and is 5% polyvinyl alcohol water solution;2.5g polyurethane is dissolved in dimethyl formamide, is mixed with mass percent concentration and is 5% polyurethane dimethyl formamideSolution;
B, use Fig. 3 shown device, the head end that diameter is about to the carbon nano-tube fibre a of 30 μ m takes out from bobbin I 1,After passing first group of container 2 and heater 3 by perforation 21, pass second group of container 2 ' and heater 3 ' by perforation 21 ' again,Then be fixed in bobbin II 5 through feed carrier 4;
C, the polyvinyl alcohol water solution that step a) is prepared add the polyurethane dimethyl methyl of a) preparing in container 2 and by stepAmide solution adds in container 2 ', and it is molten to control respectively splendid attire polyvinyl alcohol water solution and polyurethane dimethyl formamide whereinThe degree of depth of liquid is always 5mm, opens speed control motor 6 and makes carbon nano-tube fibre a at the uniform velocity pass through and contain successively with the speed of 1mm/sBe contained in polyvinyl alcohol water solution and the heater 3 in container 2 and be contained in polyurethane dimethyl formamide in container 2 ' moltenLiquid and heater 3 ' (temperature that all needs to control heating region is 60～80 DEG C); Composite fibre b process after solidifying is ledYarn feeding device 4 is collected in bobbin II 5.
Fig. 4 is the structural representation of prepared composite fibre, as seen from Figure 4: prepared composite fibre is multilayer core-skinStructure: carbon nano-tube fibre layer is sandwich layer A, polyvinyl alcohol layer is the first cortex B1, layer of polyurethane is the second cortex B2.
Embodiment 3: polyurethane/polyvinyl alcohol/carbon nanotube multilayer skin-core structure composite fibre of nano-Ag particles is added in preparation
The difference of the present embodiment embodiment 2 is only: at preparation polyvinyl alcohol water solution and polyurethane dimethyl formamideWhen solution, all add 10mg nano-Ag particles simultaneously and adopt magnetic stirring apparatus and have children outside the state plan concussion method that nano particle is evenly dividedBe dispersed in solution. All the other operate all with identical described in embodiment 2.
The prepared composite fibre of the present embodiment is also multilayer skin-core structure: carbon nano-tube fibre layer is sandwich layer A, containing Nano SilverThe polyvinyl alcohol layer of particle is the first cortex B1, is the second cortex B2 containing the layer of polyurethane of nano-Ag particles.
Finally be necessary described herein: above embodiment is only for doing to say in further detail to technical scheme of the present inventionBright, can not be interpreted as limiting the scope of the invention; Those skilled in the art's foregoing according to the present invention is madeSome nonessential improvement and adjust and all belong to protection scope of the present invention.
Claims (8)
1. a device of preparing skin-core structure conductive carbon nanotube composite fibre, is characterized in that: comprise bobbin I, be provided withContainer, heater, feed carrier and the bobbin II of perforation, the fiber of being extracted out by bobbin I is successively through being provided with the appearance of perforationDevice, heater and feed carrier are fixed in bobbin II, and described bobbin I and bobbin II are all connected with speed control motor; InstituteThe bobbin I of stating, the container that is provided with perforation, heater, feed carrier and bobbin II vertical arrangement from bottom to top successively, instituteThe perforation of stating is arranged on the center of container bottom; The diameter of described perforation is 30 μ m～100 μ m.
2. device as claimed in claim 1, is characterized in that: the material of described container is stainless steel, glass or corrosion resistantErosion plastics.
3. device as claimed in claim 1, is characterized in that: described container and heater are one or more groups.
4. right to use requires device described in 1 to prepare a method for skin-core structure conductive carbon nanotube composite fibre, its featureBe, comprise the steps:
A) preparation conductive polymer solution, for subsequent use;
B) by from bobbin I extract out carbon nano-tube fibre by boring a hole through container, successively after heater and feed carrierBe fixed in bobbin II;
C) conductive polymer solution of step a) being prepared adds in container, opens speed control motor, makes carbon nano-tube fibre with evenSpeed process conductive polymer solution, and open heater simultaneously, make the composite fiber rapid solidification forming;
D) composite fibre after making to solidify is collected in bobbin II through feed carrier.
5. method as claimed in claim 4, is characterized in that: described conductive polymer solution is by polyvinyl alcohol, poly-At least one in acrylonitrile, polyurethane, nylon, polyester, cellulose, silk and water, dimethyl formamide, dimethylIn acetamide, formamide, formic acid, carrene, chloroform, acetone, methyl alcohol, ethylene bromide base triphenyl squama extremelyFew a kind of formulated, the mass percent concentration of described conductive polymer solution is greater than 1%.
6. method as claimed in claim 5, is characterized in that: in described conductive polymer solution, be added with nano metalParticle.
7. method as claimed in claim 4, is characterized in that: step c), is controlled conductive polymer solution in containerThe degree of depth remains at 5mm, and controls carbon nano-tube fibre and at the uniform velocity pass through conducting polymer with the speed of 0.5mm/s～1mm/sThing solution, and the temperature of control heating region is 60～80 DEG C.
8. method as claimed in claim 4, is characterized in that: described carbon nano-tube fibre is single-root carbon nano-tube fiberOr plying carbon nano-tube fibre after many twisting.
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| CN105541149B (en) * | 2015-12-08 | 2018-01-09 | 余姚市交通规划设计研究院 | A kind of modification for bituminous pavement top is the same as the compound fine fibre of core and application |
| CN106676679A (en) * | 2016-11-08 | 2017-05-17 | 江南大学 | Preparation method of polylactic acid conductive fibers |
| JP6666866B2 (en) * | 2017-02-17 | 2020-03-18 | 矢崎総業株式会社 | Method for producing carbon nanotube twisted electric wire |
| CN109545574B (en) * | 2017-09-22 | 2020-09-22 | 中国科学院物理研究所 | Preparation method and device of carbon nano tube/conductive polymer composite material |
| CN109735953B (en) * | 2018-07-06 | 2021-12-07 | 东华大学 | Preparation method and application of TPE/PANI (thermoplastic elastomer)/skin-core structure elastic conductive fiber |
| CN113005544B (en) * | 2021-02-02 | 2022-08-05 | 华中科技大学 | Manufacturing method of filament outlet and photoelectric chip integrated fiber and fabric |
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Patent Citations (5)
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| DE557554C (en) * | 1930-02-01 | 1932-08-25 | Fritz Ehrlich | Method and device for the production of artificial threads |
| US4118212A (en) * | 1976-11-30 | 1978-10-03 | Siemens Aktiengesellschaft | Double crucible system for the production of light conducting fibers |
| US4473617A (en) * | 1981-01-15 | 1984-09-25 | Akzo Nv | Synthetical technical multifilament yarn and a process for the manufacture thereof |
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| CN203382872U (en) * | 2013-07-16 | 2014-01-08 | 上海工程技术大学 | Device for preparing conductive carbon nanotube composite fiber with skin-core structure |
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