CN103276593A - Method for enhancing carbon nano tube fiber by utilizing fluorine-removing cross-linking reaction - Google Patents
Method for enhancing carbon nano tube fiber by utilizing fluorine-removing cross-linking reaction Download PDFInfo
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Abstract
The invention discloses a method for enhancing a carbon nano tube fiber by utilizing fluorine-removing cross-linking reaction. The method comprises the following steps of: after the carbon nano tube fiber is fluorinated, sufficiently immersing the carbon nano tube fiber in a fluorine-removing reaction solution until a fluorine-removing reaction is finished, wherein the fluorine-removing solution contains an electron donor reagent and an organic solvent; or after the carbon nano tube fiber is fluorinated, sufficiently immersing the carbon nano tube fiber into the organic solvent and irradiating by ultraviolet light until the fluorine-removing reaction is finished; and continually improving the whole mechanical property of the carbon nano tube fiber. According to the method disclosed by the invention, in a fluorine-removing reaction process, a covalent bond is introduced between the surface of one carbon nano tube and the surface of the other carbon nano tube to combine, namely the bonding force between interfaces of the carbon nano tubes is improved, so that the effect of enhancing the fiber is improved. The method disclosed by the invention is simple in process and low in cost, and can easily realize large-scale implementation; and other enhancing materials do not need to be introduced and the property of the carbon nano tube fiber can be sufficiently remained.
Description
Technical field
The present invention relates to a kind of preparation method who strengthens carbon nano-tube fibre, particularly a kind of utilization and go the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, belong to field of nanometer material technology.
Background technology
CNT is paid close attention to after being found in 1991 widely, it is the accurate one-dimentional structure characteristics that the unit constitutes with carbon atom hexagonal wire side, makes its Young's modulus up to 1TPa, and TENSILE STRENGTH surpasses 100GPa, elongation at break reaches 15%～30%, considerably beyond common fibrous material.In addition, the high thermal conductivity of CNT, good electrology characteristic, good chemical stability, high-specific surface area etc. all make it have huge application potential aspect a lot.Yet want to give full play to the superior function of CNT, it must be assembled into macrostructure, as fiber, silk ribbon, film etc.At present, carbon nano-tube fibre is becoming a research direction that has very much vigor, is that the composite that matrix or enhancing system are equipped with will represent application potential in fields such as Aero-Space, shellproof equipment, sports apparatuses with the carbon nano-tube fibre.
Carbon nano-tube fibre preparation method commonly used mainly comprises the dry spinning method, direct spinning and wet spinning process.All there is following shortcoming in the fiber of these method preparations: because carbon nano tube surface is smooth, the interface between the CNT does not have the combination of chemical bond, thus slippage takes place easily, thus make the mechanical property of carbon nano-tube fibre not reach perfect performance.Thereby the mechanical property that how to improve the interface interaction fortifying fibre of CNT is it really drops into the emphasis problem that engineering is used.
At present, the enhancing carbon nano-tube fibre method of bibliographical information mainly comprises two parts.A kind of is that fiber is combined the preparation composite with other materials, comprises compound with polymer or inorganic body etc.This method often need be carried out functionalized modification at CNT, easily makes its structure destroy to some extent thereby mechanical performance is strengthened limited, also will restrict the application of this kind fiber in addition with the input of the research and development preparation of the organic or inorganic body of fiber composite.Another kind method is improved the aftertreatment technology of fiber, comprises twisting, or passes through the fibre denseization of surface tension driving, and utilizes traditional high-temperature heat treatment process to improve material with carbon element performance etc.For example, the intensity of the carbon nano-tube fibre by dry spinning method preparation is very big apart from its theoretical strength still deviation, and this mainly with in the fiber exists a large amount of defectives such as pore structure relevant, and twisting can obviously improve the mechanical property of carbon nano-tube fibre.Again for example, make carbon nano-tube fibre can make the thickness of fiber reduce several magnitude by the drop of ethanol, thereby make its densification improve mechanical property.Then, though preceding method is simple to operate, only be the improvement to the fibrous physics form, so the performance enhancing is also limited.
Summary of the invention
The object of the present invention is to provide a kind of utilization to go the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, it utilizes the enhancing of sloughing carbon pipe that fluorine element produces and the realization of the cross-linked structure between carbon pipe fiber on the carbon fluoride nano-tube surface, thereby overcomes deficiency of the prior art.
For achieving the above object, the present invention has adopted following technical scheme:
A kind of utilization goes the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, comprising:
The carbon fluoride nano-tube fiber is fully flooded in removing the fluorine reaction solution, and until finishing the fluorine reaction, the described fluorine reaction solution that goes comprises electron donor reagent and organic solvent; Perhaps,
With the carbon fluoride nano-tube fiber in organic solvent fully in the dipping and be aided with UV-irradiation, until finishing the fluorine reaction.
As one of embodiment preferred comparatively, the preparation technology of described carbon fluoride nano-tube fiber comprises: be greater than or equal in temperature under 25 ℃ the condition, carbon nano-tube fibre is placed more than the reaction atmosphere reaction 5min that contains fluorine gas, obtain target product.
As one of embodiment preferred comparatively, the preparation technology of described carbon fluoride nano-tube fiber comprises: be under 25 ℃～500 ℃ the condition in temperature, place the reaction atmosphere of mainly being formed by fluorine gas and inert gas to react 5min～600min carbon nano-tube fibre, obtain target product.
Preferably, to comprise volume ratio be 1: 1 fluorine gas and inert gas to described reaction atmosphere.
Described inert gas can include but not limited to nitrogen, argon gas or helium etc.
As one of embodiment preferred comparatively, the described fluorine reaction solution that goes comprises 0.01wt%-5wt% electron donor reagent.
Described electron donor reagent can include but not limited to N, N-dimethyl-p-phenylenediamine or four thio rich tile alkene etc.
Described organic solvent can include but not limited to ethanol, acetone, oxolane, pyrrolidones or N, dinethylformamide etc.
As one of embodiment preferred comparatively, this method comprises: the carbon fluoride nano-tube fiber is taken out after going the fluorine reaction solution to soak into 1～30min, and drying obtains the enhanced carbon nanotube fiber.
As one of embodiment preferred comparatively, this method comprises: the carbon fluoride nano-tube fiber impregnation in organic solvent, is taken out behind 1～30min, and drying obtains the enhanced carbon nanotube fiber.And be that 200～400nm, power are the UV-irradiation 5～60min of 5～100 milliwatts with wavelength, obtain the enhanced carbon nanotube fiber.
One more specifically among the embodiment, aforementioned ultraviolet light wavelength can be 280nm, and power can be 5 milliwatts.
As one of embodiment preferred comparatively, this method comprises: drive the carbon fluoride nano-tube fiber by draw-gear, make the carbon fluoride nano-tube fiber from remove fluorine reaction solution or organic solvent by and obtain fully to soak into.
Compared with prior art, the present invention has following advantage at least:
1. after the present invention handles the TENSILE STRENGTH of carbon nano-tube fibre (following abbreviation " fiber ") is improved largely, compare untreated fibers, intensity can be increased to the about 160% of original TENSILE STRENGTH, comprehensive mechanical performance also makes moderate progress simultaneously;
Though 2. the present invention needs earlier fiber to be fluoridized, the fluorine reaction of going subsequently can be sloughed fluorine, can not cause obvious destruction to fiber form, and the pattern of fiber and other performances still can be preserved;
3. do not introduce other reinforcing materials among the present invention, the fiber sample that finally obtains still only is made up of CNT, and it has still kept high-specific surface area and low-density original characteristics to compare composite;
4. the present invention need not to develop other reinforcing materials, does not also need complicated chemical modification, only needs that fiber is fluoridized the back solution-treated in tube furnace and gets final product, and equipment is simple, and operation is easily grasped, and is fit to heavy industrialization and uses.
Description of drawings
Fig. 1 is the infrared spectrum of carbon nano-tube fibre after fluoridizing the back and removing fluorine in the embodiment of the invention 1, wherein show, the carbon fluoride nano-tube fiber has the very significantly characteristic peak of C-F chemical bond, shown through fluoridizing the back carbon nano-tube fibre and successfully inserted fluorine element, and the intensity at C-F peak sharply weakens after the past, fluorine was crosslinked, fluorine element almost disappears, and has illustrated to fluoridize and go the success of fluorine reaction to carry out.
Fig. 2 A and Fig. 2 B are respectively that carbon nano-tube fibre is being fluoridized and removed the sem photograph of fluorine after crosslinked in the embodiment of the invention 1, can see, experience goes the carbon nano-tube fibre diameter after fluorine is handled to reduce to some extent, and surface structure does not have tangible destruction to change, the fibre structure that still is kept perfectly.
Fig. 3 is that carbon nano-tube fibre is being fluoridized and removed the tensile strength curve figure of fluorine after crosslinked in the embodiment of the invention 1, show original carbon nano-tube fibre (namely, pristine fibre among the figure) and the fortifying fibre that finally obtains (namely, fiber among the figure after first method is removed fluorine) mechanical property, the carbon nano-tube fibre of strengthen handling as can be seen is than pristine fibre and only be significantly improved through the TENSILE STRENGTH of fiber that organic solvent was handled (that is, among the figure only through the fiber of solvent processing).
The specific embodiment
As previously mentioned, in view of deficiency of the prior art, the present invention aims to provide a kind of new method that strengthens carbon nano-tube fibre, it comprises: by carbon nano tube surface being fluoridized and utilizing chemical reaction to make it fluorine subsequently, utilize carbon pipe and the cross-linked structure between the carbon pipe of going to produce in the fluorine process to strengthen carbon nano-tube fibre.
As comparatively one of embodiment preferred of the present invention, can at first utilize the gaseous mixture that contains fluorine element gas as fluorization agent in this method, under certain temperature and pressure directly and carbon nano-tube fibre carry out fluorination reaction;
Subsequently can be with the organic solution (for example, ethanol) that contains electron donor reagent (for example, N, N-dimethyl-p-phenylenediamine) or also can go fluorine reaction to fluoridizing fiber with the ultra violet lamp fiber; After past fluorine reaction, namely can improve the mechanical property of carbon nano-tube fibre integral body.
Among the present invention, owing to go between CNT and carbon nano tube surface, to introduce covalent bonds in the fluorine course of reaction, namely improved the adhesion between the CNT interface, thereby played the effect of fortifying fibre.
The inventive method is simply effective, need not to introduce other reinforcing materials, can fully keep the character of carbon nano-tube fibre self.
Below in conjunction with some preferred embodiments technical scheme of the present invention is described further.Should be understood that these embodiment only are used for explanation the present invention, but not limit the scope of the invention.
Embodiment 1 present embodiment relates to soaking with solution and goes fluorine crosslinked to strengthen the technology of carbon nano-tube fibre, and it comprises the steps:
(1) at high temperature carbon nano-tube fibre is carried out fluorination treatment: get on the reaction boat that one section carbon nano-tube fibre is fixed on corronil, place tubular react furnace, it is 150 degrees centigrade that temperature is set, reaction tube is evacuated to vacuum 10～20Pa, stop to vacuumize, the fluorine gas that feeding mixes in advance and the mist of nitrogen, the mixed volume ratio is 1: 10, gas flow is 50ppm, and the reaction time is 10min.
(2) the fluorine reaction solution is removed in preparation: be N with solute, the N-dimethyl-p-phenylenediamine fully is dissolved in the ethanol, and the mass concentration of solute in solution is 0.5wt%;
(3) go the fluorine crosslinking Treatment to fluoridizing fiber: will fluoridize fiber in the solution of above-mentioned preparation, and take out the carbon nano-tube fibre that oven dry can be enhanced after 2 minutes.
Embodiment 2 present embodiments relate to ultraviolet irradiation and go fluorine crosslinked to strengthen the technology of carbon nano-tube fibre, comprise the steps:
(1) at high temperature carbon nano-tube fibre is carried out fluorination treatment: get on the reaction boat that one section carbon nano-tube fibre is fixed on corronil, place tubular react furnace, it is 150 degrees centigrade that temperature is set, reaction tube is evacuated to vacuum 10～20Pa, stop to vacuumize, the fluorine gas that feeding mixes in advance and the mist of nitrogen, the mixed volume ratio is 1: 10, gas flow is 50ppm, and the reaction time is 10min.
(2) go the fluorine crosslinking Treatment to fluoridizing fiber: will fluoridize fiber and be immersed in the alcohol solvent, be the ultra violet lamp 25 minutes of 280nm with wavelength, and uviol lamp power is 5 milliwatts, takes out the carbon nano-tube fibre that can be enhanced after the oven dry.
It is pointed out that above-described embodiment only is explanation technical conceive of the present invention and characteristics, its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit essence is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (10)
1. a utilization goes the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, it is characterized in that, comprising:
The carbon fluoride nano-tube fiber is fully flooded in removing the fluorine reaction solution, and until finishing the fluorine reaction, the described fluorine reaction solution that goes comprises electron donor reagent and organic solvent; Perhaps,
With the carbon fluoride nano-tube fiber in organic solvent fully in the dipping and be aided with UV-irradiation, until finishing the fluorine reaction.
2. utilization according to claim 1 goes the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, it is characterized in that, the preparation technology of described carbon fluoride nano-tube fiber comprises: be greater than or equal in temperature under 25 ℃ the condition, carbon nano-tube fibre is placed more than the reaction atmosphere reaction 5min that contains fluorine gas, obtain target product.
3. utilization according to claim 2 goes the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, it is characterized in that, the preparation technology of described carbon fluoride nano-tube fiber comprises: be under 25 ℃～500 ℃ the condition in temperature, place the reaction atmosphere of mainly being formed by fluorine gas and inert gas to react 5min～600min carbon nano-tube fibre, obtain target product.
4. go the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre according to claim 2 or 3 described utilizations, it is characterized in that, it is 1: 1 fluorine gas and inert gas that described reaction atmosphere comprises volume ratio.
5. go the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre according to claim 2 or 3 described utilizations, it is characterized in that described inert gas comprises nitrogen, argon gas or helium.
6. utilization according to claim 1 goes the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, it is characterized in that, the described fluorine reaction solution that goes comprises 0.01wt%-5wt% electron donor reagent, and described electron donor reagent comprises N, N-dimethyl-p-phenylenediamine or four thio rich tile alkene.
7. go the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre according to claim 1 or 6 described utilizations, it is characterized in that described organic solvent comprises ethanol, acetone, oxolane, pyrrolidones or N, dinethylformamide.
8. utilization according to claim 1 goes the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, it is characterized in that, this method comprises: the carbon fluoride nano-tube fiber is taken out after going the fluorine reaction solution to soak into 1～30min, and drying obtains the enhanced carbon nanotube fiber.
9. utilization according to claim 1 goes the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, it is characterized in that, this method comprises: the carbon fluoride nano-tube fiber impregnation in organic solvent, is taken out behind 1～30min, and drying obtains the enhanced carbon nanotube fiber.And be that 200～400nm, power are the UV-irradiation 5～60min of 5～100 milliwatts with wavelength, obtain the enhanced carbon nanotube fiber.
10. utilization according to claim 1 goes the fluorine cross-linking reaction to strengthen the method for carbon nano-tube fibre, it is characterized in that, this method comprises: drive the carbon fluoride nano-tube fiber by draw-gear, make the carbon fluoride nano-tube fiber pass through and obtain fully to soak into from remove fluorine reaction solution or organic solvent.
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| JP2016204254A (en) * | 2015-04-22 | 2016-12-08 | ステラケミファ株式会社 | Crosslinked structure of carbon material and method for manufacturing the same |
| CN106592215A (en) * | 2016-12-19 | 2017-04-26 | 曲阜师范大学 | Method for preparing fluorine content- and dimension-adjustable carbon fluoride fibers |
| CN107163912A (en) * | 2017-06-13 | 2017-09-15 | 四川大学 | A kind of MWCNTSWave absorbing agent, its preparation method and absorbing material |
| CN108928809A (en) * | 2017-05-22 | 2018-12-04 | 天津大学 | The fluorine carbon ratio of carbon fluoride nano-tube regulates and controls method |
| CN109231184A (en) * | 2018-11-13 | 2019-01-18 | 广州百思创科技有限公司 | A kind of multi-functional conductive carbon nanotube and its preparation method and application |
| CN109295550A (en) * | 2018-09-21 | 2019-02-01 | 武汉大学苏州研究院 | A kind of high intensity, high elastic modulus, the carbon fiber material of good malleability and preparation method |
| CN109411752A (en) * | 2017-08-15 | 2019-03-01 | 天津大学 | A method of carbon fluoride nano-tube is prepared by Fluorine source of fluorine gas |
| CN109599535A (en) * | 2017-09-30 | 2019-04-09 | 天津大学 | Carbon fluoride nano-tube/carbon nanotube sponge composite material and preparation method for lithium-sulphur cell positive electrode |
| US11220433B2 (en) * | 2015-06-23 | 2022-01-11 | Indiana University Research And Technology Corporation | Process for modification of carbon surfaces |
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| JP2016204254A (en) * | 2015-04-22 | 2016-12-08 | ステラケミファ株式会社 | Crosslinked structure of carbon material and method for manufacturing the same |
| US11220433B2 (en) * | 2015-06-23 | 2022-01-11 | Indiana University Research And Technology Corporation | Process for modification of carbon surfaces |
| CN106592215A (en) * | 2016-12-19 | 2017-04-26 | 曲阜师范大学 | Method for preparing fluorine content- and dimension-adjustable carbon fluoride fibers |
| CN108928809A (en) * | 2017-05-22 | 2018-12-04 | 天津大学 | The fluorine carbon ratio of carbon fluoride nano-tube regulates and controls method |
| CN107163912B (en) * | 2017-06-13 | 2019-08-20 | 四川大学 | A kind of MWCNTSWave absorbing agent, preparation method and absorbing material |
| CN107163912A (en) * | 2017-06-13 | 2017-09-15 | 四川大学 | A kind of MWCNTSWave absorbing agent, its preparation method and absorbing material |
| CN109411752A (en) * | 2017-08-15 | 2019-03-01 | 天津大学 | A method of carbon fluoride nano-tube is prepared by Fluorine source of fluorine gas |
| CN109599535A (en) * | 2017-09-30 | 2019-04-09 | 天津大学 | Carbon fluoride nano-tube/carbon nanotube sponge composite material and preparation method for lithium-sulphur cell positive electrode |
| CN109599535B (en) * | 2017-09-30 | 2021-06-04 | 天津大学 | Fluorinated carbon nanotube/carbon nanotube sponge composite material for lithium-sulfur battery anode and preparation method thereof |
| CN109295550B (en) * | 2018-09-21 | 2021-02-02 | 武汉大学苏州研究院 | Carbon nanotube fiber material with high strength, high elastic modulus and excellent ductility and preparation method thereof |
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