CN103850114B - The method of electroluminescent enhancing carbon nano-tube fibre - Google Patents
The method of electroluminescent enhancing carbon nano-tube fibre Download PDFInfo
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- CN103850114B CN103850114B CN201210513599.XA CN201210513599A CN103850114B CN 103850114 B CN103850114 B CN 103850114B CN 201210513599 A CN201210513599 A CN 201210513599A CN 103850114 B CN103850114 B CN 103850114B
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Abstract
The invention discloses a kind of method of electroluminescent enhancing carbon nano-tube fibre, comprising: (1) fully infiltrates carbon nano-tube fibre with thermosetting resin presoma dilution; (2) pass to electric current in the carbon nano-tube fibre after infiltration, cause thermosetting resin Quick cross-linking to solidify, obtained high strength fibre.This high strength fibre improves respectively compared with the strength and modulus of its original untreatment carbon nanotube fibers and exceedes 125% and 150%, reaches 2.25GPa and 100GPa.The present invention only can realize the raising of fibrous mechanical property within a few minutes, far faster than traditional heat cure processing mode, strengthens while thus can realizing carbon nano-tube fibre spinning to it.Meanwhile, the features such as the present invention also has simple to operate, convenient and swift, remarkably productive, have scale application prospect.
Description
Technical field
The present invention relates to a kind of high-performance fiber preparation method, particularly relate 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 CNT assembles most important one in the macroscopic form obtained.Within 2002, from carbon nano pipe array, extract fiber out first by Fan Shoushan group of Tsing-Hua University, carbon nano-tube fibre just develops rapidly is afterwards a very great-hearted research direction of tool, shows huge application potential in the fields such as composite such as Aero-Space, bulletproof equipment, sports apparatuses.The preparation method of the current carbon nano-tube fibre developed mainly contains array and to reel off raw silk from cocoons method, solution spinning and floating chemical vapor deposition (CVD) spin processes.Array spin processes is can on the basis of spinning carbon nano pipe array, and by reeling off raw silk from cocoons, twisting, infiltrate, the dry spinning process such as enhancing prepare carbon nano-tube fibre.Solution spinning first carbon nanotube dust is dispersed into have certain density homogeneous solution, then simulates conventional solution spining technology, be injected into silk and obtain by liquid phase.The developer the earliest of floating CVD direct spinning is the Windle group of univ cambridge uk, and this method has 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 have been stablized and reached more than 1.0GPa, can meet the requirement of most of structural member to mechanics of materials intensity.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 repeatedly bending, knotting, contact, bending, the stressed position such as irregular can be effective to, and the problem such as the fragility effectively solving usual 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 dynamic 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 restrained by the CNT of microcosmic to assemble, fibrous inside also exists a large amount of cavity, and carbon pipe bulk density is not high.This loose internal structure not only affects the mechanical property of fiber, and its conductive capability is also far below the theoretical value of single-root carbon nano-tube simultaneously.Therefore improve fibrous inner structure, reduce the distance between fibrous inside cavity and carbon pipe, increase its CONTACT WITH FRICTION, become the key improving carbon nano-tube fibre mechanics and electric property.Existing a few thing focuses on that the mechanics of carbon nano-tube fibre strengthens at present, as (patent publication No. are CN101967699A) such as Zhao Jingna introduces heat curing-type polyamic acid in carbon nano-tube fibre inside, solidify in 150-240 DEG C again after 1h, fiber loudness can be increased to 2.06GPa.This method mode of filling high strength thermosetting resin in carbon nano-tube fibre prepare in high performance carbon nanofiber significant.But hot environment baking more than 1h, 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.Carbonnanotubefibersforelectrochemicalapplications: effectofenhancedinterfacesbyanacidtreatment) by concentrated acid process carbon nano-tube fibre, cause fiber sheath densification to be shunk, and then fiber reinforcement 52% is reached 1.5GPa.The advantage of this method is simple to operate, but red fuming nitric acid (RFNA) danger is high, and reaches enhancing effect consuming time also longer (being generally 2h).(the ACSNano such as the KaiLiu of Tsing-Hua University, 2010,4,5827 – 5834.Scratch-Resistant, HighlyConductive, andHigh-StrengthCarbonNanotube-BasedCompositeYarns) by spun for array carbon nano-tube fibre is crossed PVA solution, then in the high temperature furnace of 150 DEG C, baking is dry, and the intensity of fiber is increased to 2.0GPa.The equipment that this method needs is more complicated, and equally will through high-temperature baking process, during consumption energy consumption.So it is very necessary for exploring a kind of method that effectively also can realize strengthening continuously carbon nano-tube fibre fast.
Summary of the invention
The object of the present invention is to provide a kind of method of electroluminescent enhancing carbon nano-tube fibre, it is simple to operate, convenient and swift, and successful, fortifying fibre rapidly, continuously can be realized in the process of spinning simultaneously, thus overcome deficiency of the prior art.
For achieving the above object, the technical solution used in the present invention comprises:
A method for electroluminescent enhancing carbon nano-tube fibre, comprising:
(1) fully carbon nano-tube fibre is infiltrated with thermosetting resin presoma dilution;
(2) pass to electric current in the carbon nano-tube fibre after infiltration, cause thermosetting resin Quick cross-linking to solidify, obtained 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.
CNT used in the preparation technology of described carbon nano-tube fibre comprises Single Walled Carbon Nanotube and/or multi-walled carbon nano-tubes.
Described thermosetting resin comprises any one or two or more combinations in unsaturated polyester resin, phenolic resins and thermosetting epoxy resin, and described unsaturated polyester resin comprises span and carrys out amide resin (BMI), but is not limited thereto.
As preferably one of embodiment, the concentration of described thermosetting resin presoma dilution is 0.1wt% ~ 50wt%.
Diluent in described thermosetting resin presoma dilution to comprise in DMF, NMP, ethanol, acetone, chloroform, dimethyl sulfoxide (DMSO), dichloroethanes and ethyl acetate any one or two or more combinations, but is not limited thereto.
Specifically, the operation infiltrated carbon nano-tube fibre in step (1) carries out in the spinning process of carbon nano-tube fibre or after having spun.
The mode infiltrating process in step (1) comprises immersion way and/or spraying method, but also two or more modes are successively carried out.
As preferably one of embodiment, described size of current is 1mA ~ 20mA.
In described high strength fibre, the volume percent content of thermosetting resin is below 10%, and overall phosphorus content is at below 90wt%, and the diameter of single-stranded fiber is at 3-50 μm.
Compare to prior art, the present invention at least has following remarkable advantage: the present invention only need when fibre spinning an additional constant-current supply, flow through fiber number minute with a certain size electric current, by maximum for the strength and modulus of fiber raising 125% and 150%, 2.25GPa and 100GPa can be reached respectively; The advantages such as the present invention, compared with conventional carbon nanotube fibers enhancement method, also has rapidly, continuously, equipment is very simple, easy and simple to handle, have scale and prepare prospect.
Being easier to for making the practicality of substantive distinguishing features of the present invention and institute's tool thereof understand, below in conjunction with accompanying drawing and some specific embodiments, technical scheme of the present invention being described in further detail.But the following description about embodiment and explanation do not constitute any limitation scope; those of ordinary skill in the art are according to these embodiment institute work energy, method or structural equivalent transformations or substitute, and all belong within protection scope of the present invention.
Accompanying drawing explanation
Fig. 1 is the implementation process schematic diagram of the better specific embodiments of the present invention one;
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 of the carbon nano-tube fibre in the embodiment of the present invention 1 after pure nano-carbon tube fiber and the electroluminescent enhancing of BMI resin;
Fig. 4 is the stretching fracture stereoscan photograph of the carbon nano-tube fibre in the embodiment of the present invention 1 after the electroluminescent enhancing of BMI resin;
Fig. 5 is after in the embodiment of the present invention 3, BMI resin infiltrates carbon nano-tube fibre, with the fibre strength change after 4mA intensifying current fiber different time;
Fig. 6 is after in the embodiment of the present invention 1, BMI resin infiltrates carbon nano-tube fibre, with the fibre strength change after 5mA intensifying current fiber different time;
Fig. 7 is after in the embodiment of the present invention 2, BMI resin infiltrates carbon nano-tube fibre, with the fibre strength change after 6mA intensifying current fiber different time.
Detailed description of the invention
The present invention aims to provide a kind of method of electroluminescent enhancing carbon nano-tube fibre, and consult Fig. 1, it comprises following steps:
A. carbon nano-tube fibre is prepared;
B. thermosetting resin presoma dilution is prepared;
C. fully carbon nano-tube fibre is infiltrated with described thermosetting resin presoma dilution;
D. pass to the electric current of setting size in the carbon nano-tube fibre after infiltration, cause resin Quick cross-linking to solidify, obtained high strength fibre.
Further, the carbon nano-tube fibre in step a can be the carbon nano-tube fibre prepared by array spin processes or solution spinning or chemical meteorology deposition spin processes, but is not limited thereto.
Further, foregoing carbon nanotubes comprises Single Walled Carbon Nanotube, multi-walled carbon nano-tubes or their mixing.
Further, foregoing thermosetting resins comprises BMI (span carrys out amide resin), phenolic resins, at least one in epoxy resin and other unsaturated polyester resins etc., but is not limited thereto.
Further, the mass concentration of foregoing thermosetting resins presoma dilution is 0.1% ~ 50%.
Further, infiltrating the processing time in step c comprises in fibre spinning process or after having spun, and the way of contact of fiber and resins dilute liquid comprises immersion way or spraying method, but also two or more modes are successively carried out.
Further, the size of current scope adopted in steps d is 1mA ~ 20mA.
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 μm.
Further combined with some embodiments, the present invention is described in more detail below:
embodiment 1
From film can be pulled out spinning carbon nano pipe array, by High Rotation Speed (500rpm) array, twisting is carried out to film after the fixed film other end and prepare 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%, after the carbon nano-tube fibre that spins infiltrates this drop, successively by two smooth electrodes, interelectrode distance is 14cm, additional constant-current supply, setting is 5mA by the size of current of carbon nano-tube fibre, finally collects carbon nano-tube fibre, and its speed of collecting winding is 7cm/min.
In this process, directly as shown in Figure 2, its intensity is about 1.0GPa to the spun carbon nano-tube fibre sample not infiltrating resin, and modulus is about 40GPa.
It is the constant current district at two ends that carbon nano-tube fibre enters after going out resin infiltrate with copper cash, and this stage passes to 5mA stable electrical and flows through carbon nano-tube fibre (following be called for short " fiber "), and the time of electric current section of passing by is about 2min.As shown in Figure 3, after galvanization, the more original non-wetting fibre intensity of the intensity of fiber improves 110%, and reach 2.1GPa, modulus improves 140%, reaches 97GPa.And this electroluminescent enhancing only 2min 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 extend conduction time, also can further by high strength fibre intensity enhancing to 2.25GPa, modulus brings up to more than 100GPa (see Fig. 6).
Fig. 4 shows BMI resin and solidifies on carbon nano-tube fibre surface, and the CNT in high strength fibre is bonded together each other firmly.During tension failure, a large amount of carbon pipe fracture, only have little CNT slippage, the high strength fibre fracture thus after this electroluminescent enhancing is simply neat.
embodiment 2
With floating CVD carbon nano-tube aeroge, twist carbon nanotube aerogel in high temperature furnace pipe exit, strengthen and collect, the speed of wherein twisting and collecting is respectively 1000rpm and 14cm/min.In the method after carbon nano-tube fibre plug for outlet, it is allowed to be the BMI/DMF liquid bath of 25wt% by a mass fraction.Again successively by two electrodes after fiber liquid outlet groove liquid level, electrode spacing 14cm, size of current is 6mA, twists simultaneously and collects again afterwards to the fiber after enhancing.
In this process, 6mA electric current is by maintaining the only 1min time during fiber, the strength and modulus of fiber is just increased to 2.0GPa and 94GPa respectively.
embodiment 3
From film can be pulled out spinning carbon nano pipe array, twist to be prepared into fiber to film by High Rotation Speed (100rpm) array after the fixed film other end.First this fiber is the BMI/NMP dilution liquid bath of 20wt% through a mass fraction, and after fiber liquid outlet groove liquid level, successively by two smooth electrodes, interelectrode distance is 14cm, additional constant-current supply, and setting by the size of current of fiber is 4mA.Finally collect fiber, the speed of its collecting terminal winding is 1.4cm/min.
In this process, it is 10min that the fiber infiltrated after resin leads to 4mA current time, and the fibre strength obtained is 1.93GPa, and modulus is 89GPa.
Fig. 5 ~ Fig. 7 represents respectively in the carbon nano-tube fibre after resin infiltrates and passes to 4,5, the variation trends of fiber after 6mA electric current different time.After wherein 4mA electric current is about 10min, the intensity of fiber can reach 1.93GPa, and extend conduction time, the intensity of fiber slightly promotes, and after 120min, intensity is basically stable at about 2.0GPa.And the intensity of fiber can be increased to more than 2.0GPa fast by 5mA, 6mA electric current in 2min, maximum intensity reaches 2.25GPa.Big current fortifying fibre is tested; although time expand, the intensity of fiber slightly declined (this may be because heavy current cause fibrous inner structure local failure) again; but actual enhancing in operation only need shorten conduction time; this also prepares demand with scale consistent with the requirement of increasing work efficiency, and namely reaches optimum efficiency in the short time.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.Any Reference numeral in claim should be considered as the claim involved by limiting.
In addition, be to be understood that, although this description is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should by description integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (8)
1. a method for electroluminescent enhancing carbon nano-tube fibre, is characterized in that, comprising:
(1), in the spinning process of carbon nano-tube fibre or after having spun, fully carbon nano-tube fibre is infiltrated with thermosetting resin presoma dilution;
(2) pass to the electric current of 1mA ~ 20mA in the carbon nano-tube fibre after infiltration, cause thermosetting resin Quick cross-linking to solidify, obtained high strength fibre.
2. the method for electroluminescent enhancing carbon nano-tube fibre according to claim 1, is characterized in that, the preparation technology of described carbon nano-tube fibre comprise in array spin processes, solution spinning and chemical vapour deposition (CVD) spin processes any one.
3. the method for electroluminescent enhancing carbon nano-tube fibre according to claim 2, it is characterized in that, CNT used in the preparation technology of described carbon nano-tube fibre comprises Single Walled Carbon Nanotube and/or multi-walled carbon nano-tubes.
4. the method for electroluminescent enhancing carbon nano-tube fibre according to claim 1, it is characterized in that, described thermosetting resin comprises any one or two or more combinations in unsaturated polyester resin, phenolic resins and thermosetting epoxy resin, and described unsaturated polyester resin comprises span and carrys out amide resin.
5. the method for electroluminescent enhancing carbon nano-tube fibre according to claim 1, is characterized in that, the concentration of described thermosetting resin presoma dilution is 0.1wt% ~ 50wt%.
6. the method for electroluminescent enhancing carbon nano-tube fibre according to claim 1 or 5, it is characterized in that, the diluent in described thermosetting resin presoma dilution to comprise in DMF, NMP, ethanol, acetone, chloroform, dimethyl sulfoxide (DMSO), dichloroethanes and ethyl acetate any one or two or more combinations.
7. the method for electroluminescent enhancing carbon nano-tube fibre according to claim 1, is characterized in that, the mode infiltrating process in step (1) comprises immersion way and/or spraying method.
8. the method for electroluminescent enhancing carbon nano-tube fibre according to claim 1, 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 at below 90wt%, and the diameter of single-stranded fiber is at 3 ~ 50 μm.
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| CN105256530B (en) * | 2015-12-02 | 2017-08-25 | 南京科技职业学院 | A kind of preparation method of high-tensile carbon nano-tube fibre |
| 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 |
| 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 |
| 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 |
| CN111304799B (en) * | 2020-04-10 | 2022-05-31 | 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 |
| CN112359441B (en) * | 2020-12-02 | 2022-11-08 | 江西省纳米技术研究院 | High-orientation carbon nano tube composite fiber, and preparation method and system thereof |
| 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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