CN106012537A - Method for preparing wear-resistant conductive fibers - Google Patents
Method for preparing wear-resistant conductive fibers Download PDFInfo
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- CN106012537A CN106012537A CN201610352567.4A CN201610352567A CN106012537A CN 106012537 A CN106012537 A CN 106012537A CN 201610352567 A CN201610352567 A CN 201610352567A CN 106012537 A CN106012537 A CN 106012537A
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- Prior art keywords
- wear
- resistant conductive
- conductive fiber
- carbon nano
- preparation
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Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
- D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention provides a method for preparing wear-resistant conductive fibers. The method is characterized by comprising the following steps: soaking carbon nano tube yarns in a resin, and preparing carbon nano tube composite fibers; performing one-time or multiple cycle cryogenic treatment on the carbon nano tube composite fibers in a stretching state, thereby obtaining the wear-resistant conductive fibers. According to the invention, with the adoption of cryogenic treatment, the overall mechanical property and electrical properties of a carbon nano tube fiber-reinforced resin composite material can be obviously improved on premise of improving the wear resistance of the carbon nano tube fibers. Moreover, the process method is simple and convenient to operate, the production cost of the modified process is reduced, and the method has obvious economic benefits and social benefits and also has good industrial application prospects.
Description
Technical field
The present invention relates to the preparation method of a kind of wear-resistant conductive fiber, belong to high-performance fiber modification field.
Background technology
CNT yarn be at present the gentliest, the fibrous material that the strongest, plasticity is maximum, its development has greatly promoted ultra-fine fibre
Dimension and the development of a new generation's structure function composite.And it also has chemical resistance, high temperature resistant, molten and excellence
Electric conductivity, but, due to the anti-wear performance of its weakness, the extensively application of CNT yarn have received restriction greatly.
Due to the network structure of CNT, the electric conductivity of its excellence is increasingly favored by conductive fiber.And lead
The wearability of electricity fiber, research is relatively fewer at present, is concentrated mainly on coating modified.The carbon carbon structure of CNT yarn,
Chemical property presents inertia relatively, will necessarily bring damage to fiber so coating modified.At present, " similar compatibility " it is typically based on
Principle, selects suitable resin to be combined with it, thus increases certain anti-wear performance.
Subzero treatment is also known as super low temperature or super sub-cold treatment, and it is the extension of conventional cold treatment.Cryogenic treatment process
Being generally considered to be using liquid nitrogen as deep cooling medium, be contained in by treated sample in certain container, different materials is special by it
Fixed temperature lowering curve, controls rate of temperature fall, sample drops to liquid nitrogen temperature, held for some time lentamente, then presses heating curve,
It is slowly raised to the processing procedure of room temperature.This technique is not only mainly used in ferrous material and alloy thereof, nonferrous materials
And alloy etc., metal tools can be made in abrasive wear resistant weld deposit, corrosion and wear resistance, minimizing internal stress and the stability improving material
Etc. aspect all demonstrate a certain degree of improvement.
Cryogenics application, generally using liquid nitrogen as low-temperature receiver, utilizes its phase transformation (gasification) heat absorption to obtain low temperature environment.Nitrogen
Gas is one of main composition in air, nonpoisonous and tasteless, thus the application environmental sound of cryogenics, belong to green manufacturing
Technology category.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of wear-resistant conductive fiber, utilizes at deep cooling
Reason, and then improve the Optical instrument between CNT yarn and resin matrix interface, improve the anti-wear performance of carbon nano-tube fibre.
In order to solve above-mentioned technical problem, the invention provides the preparation method of a kind of wear-resistant conductive fiber, its feature exists
In, including: CNT yarn is immersed in resin, makes carbon nano tube composite fibre；Described CNT is combined
Fiber carries out single or multiple cyclic cryogenic treatment in a stretched state, obtains wear-resistant conductive fiber.
Preferably, the percentage elongation of described extended state is 1%-5%.
Preferably, the treatment temperature of described subzero treatment is-90 DEG C to-200 DEG C, the process time be 3 hours-15 little
Time.
Preferably, the cooling method of described subzero treatment uses programme-control borehole cooling, or be directly placed into-90 DEG C to-
The mode of cooling suddenly under the ultra-low temperature surroundings of 200 DEG C；Process of rising again uses temperature programmed control, or employing is placed directly in room temperature environment
Under the mode risen again.
Preferably, described subzero treatment includes: is put in a stretched state by carbon nano tube composite fibre and has deep cooling
In the deep cold treatment apparatus of medium, it is airtight, it is that 0.5 DEG C/min-10 DEG C/min cools to-90 DEG C to-200 with cooling rate
DEG C, the process time is 3 hours-15 hours, rises again after room temperature with 0.5 DEG C/min-5 DEG C/min of speed, is disposed.
Preferably, described CNT yarn is single cotton sewing thread on cop or multi-wall carbon nano-tube cotton sewing thread on cop.
Preferably, described resin is thermosetting or thermoplastic resin.
It is highly preferred that described resin is epoxy resin, polyvinyl alcohol resin, polyurethane resin or polyamide.
Preferably, before being immersed in resin by CNT yarn, first diluent is used to be diluted resin.
Preferably, the viscosity of described resin controls between 100-300mPa.s.
Preferably, described diluent is reactive diluent or non-activated thinner, and described reactive diluent is preferably
At least one in acrylic glycidyl ether, phenyl glycidyl ether and ethylene glycol bis glycidyl ether；Described is nonactive
Diluent is preferably at least one in ethanol, benzene, ethanol, acetone, butanol or dibutyl ester.
Preferably, the diameter 10 of described CNT yarn～500 microns.
Preferably, described soak time is 0.5 hour-5 hours.
CNT yarn in the present invention can be adopted as direct spinning, array reels off raw silk from cocoons weaving or thin film twisting
The conventional methods such as method are made.
Compared with prior art, the invention has the beneficial effects as follows:
1, carbon nano tube composite fibre is carried out subzero treatment, carbon nano tube composite fibre by the present invention in a stretched state
Crocking resistance and tensile property are significantly improved, and have given full play to the potentiality of carbon fiber material.
2, the present invention uses carbon nano-tube fibre as conductive fiber, has given full play to the network conduction that CNT is excellent
Performance, conductive effect is more significantly.
3, the present invention passes through subzero treatment, makes CNT yarn and resin adhering to each other tightly, improves fiber
Electric conductivity and wearability.This wear-resistant conductive fiber has widely in electronic textile, electromagnetic shielding, intelligent wearable field
Application prospect.
4, the cryogenic treatment process process of the present invention and deep cold treatment apparatus simple in construction, with other modification process phases
Ratio, more saves the energy and production cost, has good development prospect.
5, subzero treatment technology of the present invention is using liquid nitrogen as low-temperature receiver, utilizes its phase transformation (gasification) heat absorption to obtain low temperature
Environment, nonpoisonous and tasteless, environmental friendliness, belong to green manufacture technology category.
6, due to the fact that employing subzero treatment, can be under the abrasion resistance properties premise improving carbon nano-tube fibre, can
Significantly improve carbon nano-tube fibre and strengthen the overall mechanical property of resin composite materials and electric property, and process is simple,
Easy to operate, reduce the production cost of modified technique, there is significant economic benefit and social benefit, having good industry should
Use prospect.
Accompanying drawing explanation
Fig. 1 is the preparation facilities schematic diagram of wear-resistant conductive fiber.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Viscosity in the present invention uses rotating cylinder viscometer test.
Percentage elongation in the present invention refers to the percentage ratio of length that sample extends and original length.
The preparation facilities of the wear-resistant conductive fiber below used is as it is shown in figure 1, the preparation of described wear-resistant conductive fiber fills
Put and include electric rotating machine 1, CNT yarn 2, sley point 3, first heater 4, water bath 5, container 6, second add hot charging
Put 7 and deep cold treatment apparatus 8.Container 6 is located in water bath 5, and water bath 5 is located in first heater 4, CNT yarn
2 under the driving of electric rotating machine 1, after secondary heating mechanism 7 heats, carries out in sley point 3 imports equipped with the container 6 of resin
Immersion treatment.
Embodiment 1: the preparation method of multi-walled carbon nano-tubes-polyvinyl alcohol subzero treatment wear-resistant conductive fiber
(1) by polyvinyl alcohol (degree of polymerization 1750, alcoholysis degree 98%) dilute with water, the mass ratio of polyethylene alcohol and water is
1: 16, obtain the poly-vinyl alcohol solution of 200 milliliters, in the container 6 of the preparation facilities loading wear-resistant conductive fiber, be stirred well to
Uniform state, viscosity is 30MPa.s.
(2) by multi-wall carbon nano-tube cotton sewing thread on cop (diameter 100 microns) 2 under the driving of electric rotating machine 1, import through sley point 3
Container 6 is immersed in poly-vinyl alcohol solution, and water bath 5 temperature controls at 70 DEG C, and the boot speed of CNT yarn is 20r/
Min, 1 hour persistent period, after taking-up, 100 DEG C of drying in secondary heating mechanism 7, obtain carbon nano tube composite fibre；
(3) described carbon nano tube composite fibre is carried out under the extended state that percentage elongation is 2% at 5 circulation deep coolings
Reason, described subzero treatment includes: is put in a stretched state by carbon nano tube composite fibre and has the deep of deep cooling medium liquid nitrogen
In the container of cold treatment equipment 8 (SLX-30), container cover is closely closed, in order to avoid low temperature liquid nitrogen is revealed, affect temperature controlled standard
Really property and treatment effect, arranges cryogenic treatment process parameter such as table 1, controls cooling rate and cools to cold insulation temperature, cold insulation one section
After time, control speed is risen again after room temperature, is disposed, obtains wear-resistant conductive fiber.
Table 1 Deep Cryogenic Treatment table
After being disposed, after the ambient temperature of container reaches room temperature, fiber can't be taken out the most from container with hands,
Use special equipment.Multi-walled carbon nano-tubes-the polyvinyl alcohol composite fiber of subzero treatment to be removed is risen again the most naturally
During to room temperature, i.e. complete processing procedure.
Multi-walled carbon nano-tubes-polyvinyl alcohol conductive fiber through subzero treatment compares the conduction of multi-wall carbon nano-tube cotton sewing thread on cop
Property is by 4 × 103S/m brings up to 4.4 × 103S/m, improves 10%；Wearability is brought up to fracture in 360 seconds by fracture in 160 seconds, carries
High by 125%；Hot strength is brought up to 200Mpa by 120MPa, improves 66.7%.
The preparation of embodiment 2 multi-walled carbon nano-tubes-epoxy resin subzero treatment wear-resistant conductive fiber
(1) epoxy resin (E51) and firming agent (R-871) being mixed, the mass ratio of epoxy resin and firming agent is 5:
1, obtain the epoxy resin solution of 200 milliliters, in the container 6 of the preparation facilities loading wear-resistant conductive fiber, be stirred well to all
Even state, viscosity is 30MPa.s.
(2) by multi-wall carbon nano-tube cotton sewing thread on cop (diameter 100 microns) 2 under the driving of electric rotating machine 1, import through sley point 3
Container 6 is immersed in epoxy resin solution, and water bath 5 temperature controls at 70 DEG C, and the boot speed of CNT yarn is 20r/
Min, 1.5 hours persistent period, after taking-up, 100 DEG C of drying in secondary heating mechanism 7, obtain carbon nano tube composite fibre；
(3) described carbon nano tube composite fibre is carried out under the extended state that percentage elongation is 3% 1 subzero treatment,
Described subzero treatment includes: is put in a stretched state by carbon nano tube composite fibre and has at the deep cooling of deep cooling medium liquid nitrogen
In the container of reason equipment 8 (SLX-30), container cover is closely closed, in order to avoid low temperature liquid nitrogen is revealed, affect temperature controlled accuracy
And treatment effect, cryogenic treatment process parameter such as table 2 is set, controls cooling rate and cool to cold insulation temperature, cold insulation a period of time
After, control speed is risen again after room temperature, is disposed, obtains wear-resistant conductive fiber.
Table 2 Deep Cryogenic Treatment table
| Cooling rate (DEG C/min) | Cold insulation temperature/DEG C | Cold insulation time/(h) | Rise again mode | Deep cooling medium |
| 3 | -180 | 14 | Automatically rise again | Liquid nitrogen |
After being disposed, after container ambient temperature reaches room temperature, fiber can't be taken out the most from container with hands, use
Special equipment.Multi-walled carbon nano-tubes-the epoxy resin composite fiber of subzero treatment to be removed is risen again the most naturally
During room temperature, i.e. complete processing procedure
The multi-walled carbon nano-tubes of subzero treatment-epoxy resin conduction fiber compare the electric conductivity of multi-wall carbon nano-tube cotton sewing thread on cop by
4×103S/m brings up to 4.5 × 103S/m, improves 12.5%；Wearability is brought up to fracture in 280 seconds by fracture in 160 seconds, improves
75%；Hot strength is brought up to 220Mpa by 120MPa, improves 83.3%.
The preparation method of embodiment 3 SWCNs-polyvinyl alcohol subzero treatment wear-resistant conductive fiber
(1) polyvinyl alcohol (degree of polymerization 1750, alcoholysis degree 98%) deionized water is diluted, the quality of polyethylene alcohol and water
Ratio is 1: 16, obtains the epoxy resin solution of 200 milliliters, in the container 6 of the preparation facilities loading wear-resistant conductive fiber, fully
Being stirred until homogeneous state, viscosity is 30MPa.s.
(2) by single cotton sewing thread on cop (diameter 30 microns) 2 under the driving of electric rotating machine 1, import through sley point 3 and hold
Device 6 is immersed in poly-vinyl alcohol solution, and water bath 5 temperature controls at 70 DEG C, and the boot speed of CNT yarn is 20r/
Min, 1 hour persistent period, after taking-up, 60-110 DEG C of drying in secondary heating mechanism 7, obtains carbon nano tube composite fibre；
(3) described carbon nano tube composite fibre is carried out under the extended state that percentage elongation is 5% at 5 circulation deep coolings
Reason, described subzero treatment includes: is put in a stretched state by carbon nano tube composite fibre and has the deep of deep cooling medium liquid nitrogen
In the container of cold treatment equipment 8 (SLX-30), container cover is closely closed, in order to avoid low temperature liquid nitrogen is revealed, affect temperature controlled standard
Really property and treatment effect, arranges cryogenic treatment process parameter such as table 3, controls cooling rate and cools to cold insulation temperature, cold insulation one section
After time, control speed is risen again after room temperature, is disposed, obtains wear-resistant conductive fiber.
Table 3 Deep Cryogenic Treatment table
| Cooling rate (DEG C/min) | Cold insulation temperature/DEG C | Cold insulation time/(h) | Rise again mode | Deep cooling medium |
| 1 | -195 | 12 | Automatically rise again | Liquid nitrogen |
After being disposed, after container ambient temperature reaches room temperature, fiber can't be taken out the most from container with hands, use
Special equipment.SWCN-the polyvinyl alcohol composite fiber of subzero treatment to be removed is risen again the most naturally
During room temperature, i.e. complete processing procedure.
SWCN-polyvinyl alcohol conductive fiber through subzero treatment compares the conduction of single cotton sewing thread on cop
Property is by 1.2 × 104S/m brings up to 1.5 × 104S/m, improves 25%；Wearability is brought up to fracture in 263 seconds by fracture in 106 seconds,
Improve 148%；Hot strength is brought up to 516Mpa by 300MPa, improves 72%.
Claims (10)
1. the preparation method of a wear-resistant conductive fiber, it is characterised in that including: CNT yarn is immersed in resin,
Make carbon nano tube composite fibre；Described carbon nano tube composite fibre is carried out in a stretched state single or multiple circulation deep
Cold treatment, obtains wear-resistant conductive fiber.
2. the preparation method of wear-resistant conductive fiber as claimed in claim 1, it is characterised in that the elongation of described extended state
Rate is 1%-5%.
3. the preparation method of wear-resistant conductive fiber as claimed in claim 1, it is characterised in that the process of described subzero treatment
Temperature is-90 DEG C to-200 DEG C, and the process time is 3 hours-15 hours.
4. the preparation method of wear-resistant conductive fiber as claimed in claim 1, it is characterised in that the cooling of described subzero treatment
Mode uses programme-control borehole cooling, or is directly placed under the ultra-low temperature surroundings of-90 DEG C to-200 DEG C the mode of cooling suddenly；Return
Temperature process uses temperature programmed control, or employing is placed directly in the mode risen again under room temperature environment.
5. the preparation method of wear-resistant conductive fiber as claimed in claim 1, it is characterised in that described subzero treatment includes:
Carbon nano tube composite fibre is put in a stretched state in the deep cold treatment apparatus with deep cooling medium, it is airtight, with fall
Temperature speed is that 0.5 DEG C/min-10 DEG C/min cools to-90 DEG C to-200 DEG C, and the process time is 3 hours-15 hours, with speed
0.5 DEG C/min-5 DEG C/min rises again after room temperature, is disposed.
6. the preparation method of wear-resistant conductive fiber as claimed in claim 1, it is characterised in that described CNT yarn is
Single cotton sewing thread on cop or multi-wall carbon nano-tube cotton sewing thread on cop.
7. the preparation method of wear-resistant conductive fiber as claimed in claim 1, it is characterised in that CNT yarn is being soaked
Before in resin, first diluent is used to be diluted resin.
8. the preparation method of wear-resistant conductive fiber as claimed in claim 1, it is characterised in that the viscosity of described resin controls
Between 100-300mPa.s.
9. the preparation method of wear-resistant conductive fiber as claimed in claim 1, it is characterised in that described CNT yarn
Diameter 10～500 microns.
10. the preparation method of wear-resistant conductive fiber as claimed in claim 1, it is characterised in that described soak time is 0.5
Hours-5 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610352567.4A CN106012537B (en) | 2016-05-25 | 2016-05-25 | A kind of preparation method of wear-resistant conductive fiber |
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| CN201610352567.4A CN106012537B (en) | 2016-05-25 | 2016-05-25 | A kind of preparation method of wear-resistant conductive fiber |
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| CN106012537A true CN106012537A (en) | 2016-10-12 |
| CN106012537B CN106012537B (en) | 2018-05-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110184550A (en) * | 2019-07-08 | 2019-08-30 | 南昌航空大学 | A kind of cryogenic treating process of continuous filament reinforced metallic matrix composite |
| CN111379170A (en) * | 2018-12-27 | 2020-07-07 | 苏州迪塔杉针织有限公司 | Preparation method of coating liquid for enhancing wear resistance of textile fiber yarns |
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| US5865913A (en) * | 1995-06-19 | 1999-02-02 | 300 Below, Inc. | Deep cryogenic tempering process based on flashing liquid nitrogen through a dispersal system |
| CN103590233A (en) * | 2013-11-01 | 2014-02-19 | 东华大学 | Method for interfacial modification of carbon fiber by cryogenic treatment |
| WO2014204517A2 (en) * | 2013-03-16 | 2014-12-24 | Mcclung Guy L | Cryogenic treatments & systems, materials made with them & methods for using them |
| CN104231296A (en) * | 2014-09-15 | 2014-12-24 | 东华大学 | Method for modifying carbon fiber composite material by cryogenic treatment |
-
2016
- 2016-05-25 CN CN201610352567.4A patent/CN106012537B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5865913A (en) * | 1995-06-19 | 1999-02-02 | 300 Below, Inc. | Deep cryogenic tempering process based on flashing liquid nitrogen through a dispersal system |
| WO2014204517A2 (en) * | 2013-03-16 | 2014-12-24 | Mcclung Guy L | Cryogenic treatments & systems, materials made with them & methods for using them |
| CN103590233A (en) * | 2013-11-01 | 2014-02-19 | 东华大学 | Method for interfacial modification of carbon fiber by cryogenic treatment |
| CN104231296A (en) * | 2014-09-15 | 2014-12-24 | 东华大学 | Method for modifying carbon fiber composite material by cryogenic treatment |
Non-Patent Citations (2)
| Title |
|---|
| DAE-WEON KIM 等: ""Improvement of Carbon Nanotubes using Cryogenic Treatment"", 《JAPANESE JOURNAL OF APPLIED PHYSICS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111379170A (en) * | 2018-12-27 | 2020-07-07 | 苏州迪塔杉针织有限公司 | Preparation method of coating liquid for enhancing wear resistance of textile fiber yarns |
| CN110184550A (en) * | 2019-07-08 | 2019-08-30 | 南昌航空大学 | A kind of cryogenic treating process of continuous filament reinforced metallic matrix composite |
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