CN103850114A - Method for electro-enhancement of carbon nano tube fiber - Google Patents
Method for electro-enhancement of carbon nano tube fiber Download PDFInfo
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- CN103850114A CN103850114A CN201210513599.XA CN201210513599A CN103850114A CN 103850114 A CN103850114 A CN 103850114A CN 201210513599 A CN201210513599 A CN 201210513599A CN 103850114 A CN103850114 A CN 103850114A
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Abstract
The invention discloses a method for electro-enhancement of a carbon nano tube fiber. The method comprises the following steps: (1) fully infiltrating the carbon nano tube fiber by using a thermosetting resin precursor diluent; and (2) galvanizing the infiltrated carbon nano tube fiber, so that thermosetting resin is quickly cross-linked and solidified, so as to prepare a high-strength fiber. Compared with a traditional unprocessed carbon nano tube fiber, the high-strength fiber has the advantages that the strength and the modulus are respectively improved by over 125% and 150%, and achieve 2.25GPa and 100GPa. By adopting the method disclosed by the invention, improvement of the mechanical property of the fiber can be achieved within a few minutes, and is much quicker than that of a traditional thermosetting treatment mode. Therefore, the carbon nano tube fiber can be enhanced when spinning of the carbon nano tube fiber is enhanced, and meanwhile, the method also has the characteristics of being simple to operate, convenient and quick, outstanding in effect and the like, and has a large-scale application prospect.
Description
Technical field
The present invention relates to a kind of high-performance fiber preparation method, relate in particular to a kind of method of quick enhancing carbon nano-tube fibre of current induced.
Background technology
Carbon nano-tube fibre is that a large amount of CNTs are assembled most important one in the macroscopic form obtaining.Within 2002, from carbon nano pipe array, extract first fiber out by Fan Shoushan group of Tsing-Hua University, just to develop rapidly be a very great-hearted research direction of tool to carbon nano-tube fibre afterwards, shown huge application potential in prepare composite such as Aero-Space, bulletproof equipment, sports apparatuses.The preparation method of the current carbon nano-tube fibre having developed mainly contains array reel off raw silk from cocoons method, solution spinning and unsteady chemical vapor deposition (CVD) spin processes.Array spin processes is on can the basis of spinning carbon nano pipe array, prepares carbon nano-tube fibre by reeling off raw silk from cocoons, twist, infiltrate the dry spinning process such as enhancing.Solution spinning is first carbon nanotube dust to be dispersed into and to have certain density homogeneous solution, then simulates traditional solution spining technology, is injected into silk obtains by liquid phase.The developer the earliest of unsteady CVD direct spinning is the Windle group of univ cambridge uk, and this method is to have technical scale most to prepare one of method of carbon nano-tube fibre potentiality.
Compared with carbon fibre material, carbon nano-tube fibre, as a kind of novel high performance fibre material, has more self-growth advantage.First, the TENSILE STRENGTH of carbon nano-tube fibre can meet the requirement of most of structural members to mechanics of materials intensity more than can having stablized and reaching 1.0 GPa.And compared with the theoretical strength value of CNT, the intensity of carbon nano-tube fibre also has the very large rising space.Secondly, carbon nano-tube fibre has high toughness, can not affect its mechanical property through bending, knotting repeatedly, can be effective to contact, bending, the stressed position such as irregular, and effectively solve the problems such as the fragility of common carbon fibre reinforced composite is excessive, boundary strength is not high.Finally, high energy absorption capability when the great elongation at break of carbon nano-tube fibre and low strain thereof, may make it in acquisition ample scopes for abilities, field such as the high energy-absorbing of needs, high strength, as bullet-proof vest and mechanical shockproof parts etc.
But macroscopic carbon nanotube fiber is to be assembled by the CNT tube bank of microcosmic, fibrous inside exists a large amount of cavities, and carbon pipe bulk density is not high.This loose internal structure not only affects the mechanical property of fiber, and simultaneously its conductive capability is also far below the theoretical value of single-root carbon nano-tube.Therefore improve fibrous inner structure, reduce the distance between fibrous inside cavity and carbon pipe, increase its CONTACT WITH FRICTION, become the key that improves carbon nano-tube fibre mechanics and electric property.At present existing a few thing focuses on that the mechanics of carbon nano-tube fibre strengthens, if (patent publication No. are CN101967699A) such as Zhao Jingna is at the inner heat curing-type polyamic acid of introducing of carbon nano-tube fibre, after solidifying 1 h again in 150-240 DEG C, fiber loudness can be increased to 2.06 GPa.The mode that this method is filled high strength thermosetting type resin in carbon nano-tube fibre prepare in high performance carbon nanofiber significant.More than but hot environment is toasted 1 h, power consumption and consuming time, this legal system realizes continued operation for high-performance carbon nanotube fiber difficulty or ease in addition.In addition as (Nanoscale such as Meng Fancheng, 2012,4,7464 – 7468. Carbon nanotube fibers for electrochemical applications:effect of enhanced interfaces by an acid treatment) process carbon nano-tube fibre by concentrated acid, cause the fine and close contraction in fiber top layer, and then fiber reinforcement 52% is reached to 1.5 GPa.The advantage of this method is simple to operate, but red fuming nitric acid (RFNA) danger is high, and reaches and strengthen that effect is consuming time also long (is generally 2 h).(the ACS Nano such as the Kai Liu of Tsing-Hua University, 2010,4,5827 – 5834. Scratch-Resistant, Highly Conductive, and High-Strength Carbon Nanotube-Based Composite Yarns) by spun array carbon nano-tube fibre is crossed to PVA solution, then in the high temperature furnace of 150 DEG C, baking is dry, and the intensity of fiber is increased to 2.0 GPa.The equipment that this method needs is more complicated, and will pass through equally high-temperature baking process, when consumption energy consumption.So it is very necessary exploring a kind of method that effectively also can realize fast continuous enhancing carbon nano-tube fibre.
Summary of the invention
The object of the present invention is to provide a kind of electricity to cause the method that strengthens carbon nano-tube fibre, it is simple to operate, convenient and swift, and successful, can in the process of spinning, realize fortifying fibre rapidly, continuously simultaneously, thereby overcome deficiency of the prior art.
For achieving the above object, the technical solution used in the present invention comprises:
Electricity causes a method that strengthens carbon nano-tube fibre, comprising:
(1) fully infiltrate carbon nano-tube fibre with thermosetting resin presoma dilution;
(2) in the carbon nano-tube fibre after infiltration, pass to electric current, cause thermosetting resin Quick cross-linking to solidify, make high strength fibre.
Further, the preparation technology of described carbon nano-tube fibre comprises any one in array spin processes, solution spinning and chemical meteorology deposition spin processes.
In the preparation technology of described carbon nano-tube fibre, CNT used comprises Single Walled Carbon Nanotube and/or multi-walled carbon nano-tubes.
Described thermosetting resin comprises any one or the two or more combinations in unsaturated polyester resin, phenolic resins and thermosetting epoxy resin, and described unsaturated polyester resin comprises that span carrys out amide resin (BMI), but is not limited to this.
As one of embodiment preferably, the concentration of described thermosetting resin presoma dilution is 0.1wt%～50wt%.
Diluent in described thermosetting resin presoma dilution comprises in DMF, NMP, ethanol, acetone, chloroform, dimethyl sulfoxide (DMSO), dichloroethanes and ethyl acetate any one or two or more combinations, but is not limited to this.
Particularly, the operation in step (1), carbon nano-tube fibre being infiltrated is in the spinning process of carbon nano-tube fibre or has spun and carried out afterwards.
In step (1), infiltrate the mode of processing and comprise immersion way and/or spraying method, but also two or more modes are successively carried out.
As one of embodiment preferably, described size of current is 1 mA～20 mA.
In described high strength fibre, the volume percent content of thermosetting resin is below 10%, and overall phosphorus content is below 90wt%, and the diameter of single-stranded fiber is at 3-50 μ m.
Compare to prior art, the present invention at least has following remarkable advantage: the present invention only need be in the time of fibre spinning an additional constant-current supply, flow through fiber number minute with a certain size electric current, can improve 125% and 150% by maximum the strength and modulus of fiber, reach respectively 2.25 GPa and 100 GPa; The present invention, compared with conventional carbon nanotube fiber reinforcement mode, also has rapidly, continuously, equipment is very simple, and the advantage such as easy and simple to handle, has scale and prepare prospect.
For making the practicality of substantive distinguishing features of the present invention and institute's tool thereof be easier to understand, be that some specific embodiments are described in further detail technical scheme of the present invention below in conjunction with accompanying drawing.But the following description about embodiment and explanation do not constitute any limitation protection domain of the present invention; those of ordinary skill in the art are according to these embodiment institute work energy, method or structural equivalent transformation or alternative, within all belonging to protection scope of the present invention.
Brief description of the drawings
Fig. 1 is the implementation process schematic diagram of the present invention's one better specific embodiments;
Fig. 2 is the scanning electron microscope (SEM) photograph of pure nano-carbon tube fiber sample in the embodiment of the present invention 1;
Fig. 3 is the mechanical stretch curve that in the embodiment of the present invention 1, pure nano-carbon tube fiber and BMI resinous electricity cause the carbon nano-tube fibre after enhancing;
Fig. 4 is the stretching fracture stereoscan photograph that in the embodiment of the present invention 1, BMI resinous electricity causes the carbon nano-tube fibre after enhancing;
Fig. 5 is that in the embodiment of the present invention 3, BMI resin infiltrates after carbon nano-tube fibre, with the fibre strength variation after 4 mA intensifying current fiber different times;
Fig. 6 is that in the embodiment of the present invention 1, BMI resin infiltrates after carbon nano-tube fibre, with the fibre strength variation after 5 mA intensifying current fiber different times;
Fig. 7 is that in the embodiment of the present invention 2, BMI resin infiltrates after carbon nano-tube fibre, with the fibre strength variation after 6 mA intensifying current fiber different times.
Detailed description of the invention
The present invention aims to provide a kind of electricity and causes the method that strengthens carbon nano-tube fibre, consults Fig. 1, and it comprises following steps:
A. prepare carbon nano-tube fibre;
B. prepare thermosetting resin presoma dilution;
C. fully infiltrate carbon nano-tube fibre with described thermosetting resin presoma dilution;
D. in the carbon nano-tube fibre after infiltration, pass to and set big or small electric current, cause resin Quick cross-linking to solidify, make high strength fibre.
Further, the carbon nano-tube fibre in step a can be the carbon nano-tube fibre preparing by array spin processes or solution spinning or chemical meteorology deposition spin processes, but is not limited to this.
Further, aforementioned CNT comprises Single Walled Carbon Nanotube, multi-walled carbon nano-tubes or their mixing.
Further, aforementioned hot thermosetting resin comprises BMI (span carrys out amide resin), phenolic resins, and at least one in epoxy resin and other unsaturated polyester resins etc., but be not limited to this.
Further, the mass concentration of aforementioned hot thermosetting resin presoma dilution is 0.1%～50%.
Further, in step c, infiltrate the processing time and comprise that, in fibre spinning process or after having spun, the way of contact of fiber and resin dilution comprises immersion way or spraying method, but also two or more modes are successively carried out.
Further, the size of current scope adopting in steps d is 1 mA～20 mA.
Further, the volume percent content of thermosetting resin in final high strength fibre is below 10%, and overall phosphorus content is more than 90%, and the diameter of single-stranded fiber is at 3～50 μ m.
Further combined with some embodiment, the present invention is described in more detail below:
embodiment 1
From pulling out film spinning carbon nano pipe array, after the fixed film other end, by High Rotation Speed (500 rpm) array, film is twisted and prepared carbon nano-tube fibre.The twist triangle zone of this carbon nano-tube fibre is unsettled fixes the BMI/DMF dilution that a mass fraction is 25wt%, the carbon nano-tube fibre that spins infiltrates after this drop, successively by two smooth electrodes, interelectrode distance is 14 cm, additional constant-current supply, setting is 5 mA by the size of current of carbon nano-tube fibre, finally collects carbon nano-tube fibre, and it collects the speed of reeling is 7 cm/min.
In this process, directly as shown in Figure 2, its intensity is 1.0 GPa left and right to the spun carbon nano-tube fibre sample that does not infiltrate resin, modulus approximately 40 GPa.
Carbon nano-tube fibre enters the constant current district taking copper cash as two ends after going out resin infiltrate, and this stage passes to 5 mA stable electrical and flows through carbon nano-tube fibre (following be called for short " fiber "), and the time of the electric current section of passing by is about 2 min.As shown in Figure 3, after galvanization, the more former beginning and end infiltration of the intensity of fiber fibre strength has improved 110%, reaches 2.1 GPa, and modulus has improved 140%, reaches 97 GPa.And this electricity causes enhancing only 2 min consuming time, speed is fast, successful, and can realize continuous production High Strength Carbon Nanotubes fiber (also can be described as high strength fibre) in spinning process.In addition, by extending conduction time, also can be further by high strength fibre intensity enhancing to 2.25 GPa, modulus is brought up to 100 GPa above (seeing Fig. 6).
Fig. 4 shows that BMI resin is curing on carbon nano-tube fibre surface, and the CNT in high strength fibre is bonded together each other firmly.When tension failure, a large amount of carbon pipes fractures, only have little CNT slippage, thus this electricity to cause high strength fibre fracture after enhancing simply neat.
embodiment 2
With the CVD method carbon nano-tube aeroge that floats, in high temperature furnace pipe exit, CNT aeroge is twisted, strengthen and collect, the speed of wherein twisting and collecting is respectively 1000 rpm and 14 cm/min.In the method after carbon nano-tube fibre plug for outlet, allow its BMI/DMF liquid bath that is 25wt% by a mass fraction.After fiber liquid outlet groove liquid level, pass through successively again two electrodes, electrode spacing 14 cm, size of current is 6 mA, again the fiber after strengthening is twisted simultaneously and is collected afterwards.
In this process, 6 mA electric currents have kept the only 1 min time during by fiber, and the strength and modulus of fiber is just increased to respectively 2.0 GPa and 94 GPa.
embodiment 3
From pulling out film spinning carbon nano pipe array, after the fixed film other end, by High Rotation Speed (100 rpm) array, film is twisted to be prepared into fiber.The BMI/NMP dilution liquid bath that first this fiber is 20wt% through a mass fraction, after fiber liquid outlet groove liquid level, by two smooth electrodes, interelectrode distance is 14 cm successively, additional constant-current supply, setting is 4 mA by the size of current of fiber.Finally collect fiber, the speed that its collecting terminal is reeled is 1.4 cm/min.
In this process, the logical 4 mA current times of fiber that infiltrate after resin are 10 min, and the fibre strength obtaining is 1.93 GPa, and modulus is 89 GPa.
The variation trends of fiber after Fig. 5～Fig. 7 represents respectively and passes to 4,5,6 mA electric current different times in the carbon nano-tube fibre after resin infiltrates.Wherein after 4 mA electric current approximately 10 min, the intensity of fiber can reach 1.93 GPa, extends conduction time, and the intensity of fiber slightly promotes, and after 120 min, intensity is stabilized in 2.0 GPa left and right substantially.And more than 5 mA, 6 mA electric currents can be increased to 2.0 GPa by the intensity of fiber fast in 2 min, maximum intensity reaches 2.25 GPa.For large intensifying current fiber experiment; although time expand fiber intensity slightly decline again (this may be because heavy current cause fibrous inner structure local failure); but actual enhancing in operation only need shorten conduction time; this also prepare demand with scale and requiring of increasing work efficiency consistent, i.e. in the short time, reach optimum efficiency.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned example embodiment, and in the situation that not deviating from spirit of the present invention or essential characteristic, can realize the present invention with other concrete form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, is therefore intended to all changes that drop in the implication and the scope that are equal to important document of claim to include in the present invention.Any Reference numeral in claim should be considered as limiting related claim.
In addition, be to be understood that, although this description is described according to embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should make description as a whole, and the technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (10)
1. electricity causes a method that strengthens carbon nano-tube fibre, it is characterized in that, comprising:
(1) fully infiltrate carbon nano-tube fibre with thermosetting resin presoma dilution;
(2) in the carbon nano-tube fibre after infiltration, pass to electric current, cause thermosetting resin Quick cross-linking to solidify, make high strength fibre.
2. electricity according to claim 1 causes the method that strengthens carbon nano-tube fibre, it is characterized in that, the preparation technology of described carbon nano-tube fibre comprises any one in array spin processes, solution spinning and chemical meteorology deposition spin processes.
3. electricity according to claim 2 causes the method that strengthens carbon nano-tube fibre, it is characterized in that, in the preparation technology of described carbon nano-tube fibre, CNT used comprises Single Walled Carbon Nanotube and/or multi-walled carbon nano-tubes.
4. electricity according to claim 1 causes the method that strengthens carbon nano-tube fibre, it is characterized in that, described thermosetting resin comprises any one or the two or more combinations in unsaturated polyester resin, phenolic resins and thermosetting epoxy resin, and described unsaturated polyester resin comprises that span carrys out amide resin.
5. electricity according to claim 1 causes the method that strengthens carbon nano-tube fibre, it is characterized in that, the concentration of described thermosetting resin presoma dilution is 0.1wt%～50wt%.
6. electricity causes the method that strengthens carbon nano-tube fibre according to claim 1 or 5, it is characterized in that, the diluent in described thermosetting resin presoma dilution comprises in DMF, NMP, ethanol, acetone, chloroform, dimethyl sulfoxide (DMSO), dichloroethanes and ethyl acetate any one or two or more combinations.
7. electricity according to claim 1 causes the method that strengthens carbon nano-tube fibre, it is characterized in that, the operation in step (1), carbon nano-tube fibre being infiltrated is in the spinning process of carbon nano-tube fibre or has spun and carried out afterwards.
8. cause according to the electricity described in claim 1 or 7 method that strengthens carbon nano-tube fibre, it is characterized in that, in step (1), infiltrate the mode of processing and comprise immersion way and/or spraying method.
9. electricity according to claim 1 causes the method that strengthens carbon nano-tube fibre, it is characterized in that, described size of current is 1 mA～20 mA.
10. electricity according to claim 1 causes the method that strengthens carbon nano-tube fibre, it is characterized in that, in described high strength fibre, the volume percent content of thermosetting resin is below 10%, and overall phosphorus content is below 90wt%, and the diameter of single-stranded fiber is at 3-50 μ m.
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| CN105256530A (en) * | 2015-12-02 | 2016-01-20 | 南京科技职业学院 | Preparation method of carbon nanotube fibers with high tensile strength |
| CN106521971A (en) * | 2016-08-25 | 2017-03-22 | 北京浩运盛跃新材料科技有限公司 | Method for improving performance of carbon nanotube fibers |
| CN108656652A (en) * | 2017-03-30 | 2018-10-16 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon nano-tube fibre composite material and preparation method |
| CN110373894A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | High-performance carbon nanotube/metal composite conductive fiber and preparation method thereof |
| CN110799592A (en) * | 2019-09-06 | 2020-02-14 | 深圳烯湾科技有限公司 | Carbon nanotube fiber composite material and preparation method thereof |
| CN111101371A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | High-performance carbon nanotube/carbon composite fiber and rapid preparation method thereof |
| CN111304799A (en) * | 2020-04-10 | 2020-06-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Argon-free self-protection method for high-temperature electric heating of carbon nanotube fiber and application thereof |
| CN112359441A (en) * | 2020-12-02 | 2021-02-12 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | High-orientation carbon nano tube composite fiber, and preparation method and system thereof |
| CN112941680A (en) * | 2021-01-28 | 2021-06-11 | 华侨大学 | Preparation method of carbon nanotube fiber-loaded nano iron oxide composite material |
| CN114411407A (en) * | 2022-01-29 | 2022-04-29 | 深圳市绿自然生物降解科技有限公司 | PBAT carbon nanotube fiber and method for reinforcing carbon nanotube fiber |
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| CN105256530A (en) * | 2015-12-02 | 2016-01-20 | 南京科技职业学院 | Preparation method of carbon nanotube fibers with high tensile strength |
| CN106521971A (en) * | 2016-08-25 | 2017-03-22 | 北京浩运盛跃新材料科技有限公司 | Method for improving performance of carbon nanotube fibers |
| CN108656652B (en) * | 2017-03-30 | 2021-01-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon nanotube fiber composite material and preparation method thereof |
| CN108656652A (en) * | 2017-03-30 | 2018-10-16 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon nano-tube fibre composite material and preparation method |
| CN110373894A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | High-performance carbon nanotube/metal composite conductive fiber and preparation method thereof |
| CN111101371B (en) * | 2018-10-25 | 2022-07-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | High-performance carbon nanotube/carbon composite fiber and rapid preparation method thereof |
| CN111101371A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | High-performance carbon nanotube/carbon composite fiber and rapid preparation method thereof |
| WO2021042384A1 (en) * | 2019-09-06 | 2021-03-11 | 深圳烯湾科技有限公司 | Carbon nanotube fiber composite material and preparation method therefor |
| CN110799592A (en) * | 2019-09-06 | 2020-02-14 | 深圳烯湾科技有限公司 | Carbon nanotube fiber composite material and preparation method thereof |
| CN111304799A (en) * | 2020-04-10 | 2020-06-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Argon-free self-protection method for high-temperature electric heating of carbon nanotube fiber and application thereof |
| CN112359441A (en) * | 2020-12-02 | 2021-02-12 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | High-orientation carbon nano tube composite fiber, and preparation method and system thereof |
| CN112941680A (en) * | 2021-01-28 | 2021-06-11 | 华侨大学 | Preparation method of carbon nanotube fiber-loaded nano iron oxide composite material |
| CN112941680B (en) * | 2021-01-28 | 2022-09-30 | 华侨大学 | Preparation method of carbon nanotube fiber-loaded nano iron oxide composite material |
| CN114411407A (en) * | 2022-01-29 | 2022-04-29 | 深圳市绿自然生物降解科技有限公司 | PBAT carbon nanotube fiber and method for reinforcing carbon nanotube fiber |
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