CN104164784A - Preparation method of composite fiber with high thermal conductivity through coating graphene on chemical fiber surface - Google Patents
Preparation method of composite fiber with high thermal conductivity through coating graphene on chemical fiber surface Download PDFInfo
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Abstract
The invention discloses a preparation method of a composite fiber with a high thermal conductivity through coating graphene on the chemical fiber surface. The preparation method comprises the following steps: (1) preparing a pretreatment liquid, carrying out a pretreatment on the fiber surface including deoiling, roughening, sensitizing, and activating; (2) preparing a silver electroplating solution, carrying out silver electroplating on the fiber surface; (3) soaking the silver-coated fibers on a sulfhydrylated graphene solution to assemble a layer of graphene on the fiber surface; (4) taking out the fibers, and drying so as to obtain the coated composite fibers. The prepared composite fiber has the advantages of high thermal conductivity, high mechanical strength, and excellent tensile performance due to the chemical fiber substrate; and the thermal conductivity of the glass fiber is enhanced by taking graphene as the coating material.
Description
Technical field
The present invention relates to a kind of method that Graphene is coated in to the high heat conduction composite fiber of chemical fibre surface making, utilize Graphene to be coated in chemical fibre surface as enhanced thermal conduction material.
Background technology
At present along with electronics technology constantly develops rapidly, high power battery is also more and more as the parts of energy body, so having the material of high heat conduction and radiating efficiency receives much concern, how to improve the heat conduction and heat radiation rate of heat sink material, dwindle its occupied space, the rigidity, the hardness that increase material are the problems that Heat Conduction Material field is paid close attention to always.
Chinese patent CN102560712A discloses a kind of high heat conduction composite fiber and manufacture method thereof in 2012-07-11, and this high heat conduction composite fiber is by fiber bodies, and the high heat conduction diaphragm of bar shaped being blended in fiber bodies forms.Described high heat conduction diaphragm is high conductive graphite diaphragm or Graphene diaphragm.The preparation method of this composite fibre is: the high heat conduction diaphragm of making bar shaped; The liquid fiber base material of fusing and high heat conduction diaphragm are mixed; Fiber base material is carried out to wire drawing processing, solidify rear formation composite fibre.Another preparation method of this composite fibre is: the high heat conduction diaphragm of making bar shaped; By high heat conduction diaphragm and the fiber base material of bar shaped, press close to operation or be mutually wound around; Improve environment temperature, make fiber base material fusing, after solidifying, mix with the high heat conduction diaphragm of bar shaped, form composite fibre.
Graphene is a kind of new material of the individual layer laminated structure consisting of carbon atom.It is a kind of two-dimensional material of only having a carbon atom thickness.2004, the physicist An Deliehaimu of Univ Manchester UK and Constantine Nuo Woxiaoluofu successfully isolated Graphene, and confirm that it can individualism in experiment from graphite.Graphene is the material for world resistivity minimum.Therefore because its resistivity is extremely low, the speed of electron transfer is exceedingly fast, and is expected to can be used to that development is thinner, conduction speed electronic component of new generation or transistor faster.Because Graphene is in fact a kind of transparent, good conductor, be also applicable to for manufacturing transparent touch screen, tabula rasa or even solar cell.
Chemical fibre fibrous insulation performance is good, corrosion resistance is good, mechanical strength is high, as packing material, can strengthen crushing resistance, pull resistance, the impact resistance of base material.The packing material of utilization and high power battery outer packing plates, can increase its mechanical performance greatly.
Chemical silvering is that people develop one of chemical plating method the earliest, comes from ancient silver mirror reaction, so far existing century-old history.Different from galvanoplastic, the coating that chemical silvering forms not is the electronics that provides by outside as reductant self-catalyzed deposition, but forms by the chemical reaction between reductant and metal ion solution.Although Electroless Silver Plating was employed over 50 years.
Chemical silvering is actual is redox reaction.Oxidation solution is generally comprised of silver nitrate and ammoniacal liquor, because the aqueous solution of silver nitrate is unstable, easily decomposes, and generates the Ag2O precipitation of brown.Therefore in liquor argenti nitratis ophthalmicus, drip a small amount of ammoniacal liquor during dosing, separate out Ag2O precipitation, continue to drip ammoniacal liquor and form silver ammonia complex and Ag2O is dissolved, Ag (NH3) 2OH further forms Ag (NH3) 2OH complexing body with product NH4NO3 again.Reaction equation is as follows:
In reduction reaction, conventional reductant is mainly glucose, sucrose, formaldehyde, tartrate etc.The present invention adopts glucose as reductant, and its reaction is as follows:
Summary of the invention
For the above-mentioned deficiency of prior art, according to embodiments of the invention, be desirable to provide a kind of composite fibre that is coated in fiberglass surfacing by Graphene, it has compared with high-heat conductive efficency, has certain mechanical strength, can be used as packing material; And propose Graphene to be coated in the method that chemical fibre surface makes high heat conduction composite fiber, utilize Graphene to be coated in chemical fibre surface as enhanced thermal conduction material.
According to embodiment, a kind of method that Graphene is coated in to chemical fibre surface making composite fibre that technical solution of the present invention provides, comprises the steps:
(1) oil removing: the ethanolic solution that is 180-240ml/L by volumetric concentration, as solvent, is removed the oil stain on chemical fibre surface, and the processing time is 10-20min, after oil removing, cleans and dry chemical fibre with deionized water;
(2) alligatoring: according to different chemical fibres, the chemical fibre after oil removing is immersed in the sodium hydroxide solution of 70-90g/L, at 70-85 ℃ of temperature, processes 10-25min, clean with deionized water;
(3) sensitization: utilize dissolving with hydrochloric acid stannous chloride, until completely dissolved, then add deionized water to be mixed with the sensitizing solution of 10-30g/L, and add a small amount of tin grain in sensitizing solution; Chemical fibre after alligatoring is immersed in sensitizing solution, take out after at room temperature processing 10-20min, with buck, clean, then clean with deionized water.In order to prevent divalent tin ion oxidation, in sensitizing solution, add a small amount of tin grain; With buck cleaning, being beneficial to two valency tin ions is hydrolyzed.
(4) activation: the liquor argenti nitratis ophthalmicus that compound concentration is 0.5-3g/L, drip ammoniacal liquor and occur reddish brown precipitation, continue to drip until precipitation disappears, add deionized water and be mixed with activating solution to 100-300ml; Chemical fibre after sensitization is processed is immersed in activating solution, take out after processing 5-20min under room temperature, with deionized water, wash and dry;
(5) chemical silvering: slowly add ammoniacal liquor in the liquor argenti nitratis ophthalmicus that is 5-10g/L in concentration and stir, until precipitation disappears, adding concentration is the NaOH of 2-4g/L, there is precipitation, slowly add again ammoniacal liquor and stir, until precipitation just disappears, being mixed with oxidation solution; By glucose deionized water dissolving, be mixed with the reducing solution that concentration is 10-20g/L; Chemical fibre through pre-treatment is placed in reducing solution, oxidation solution is dripped in reducing solution, ultrasonic processing 10-20min, after question response is complete, takes out chemical fibre, with deionized water, cleans and dries;
(6) apply: the ethanolic solution of silver-plated chemical fibre being put into the sulfhydrylation Graphene of 1-5%, fully reaction in reactor, the combination between sulfydryl and silver ion obtains the chemical fibre that Graphene applies after sulfhydrylation Graphene is coated in to silver-plated chemical fibre surface.
According to an embodiment, the present invention is aforementioned to be coated in Graphene in the method that chemical fibre surface makes composite fibre, and chemical fibre is terylene, polypropylene fibre or polyamide fibre.
According to an embodiment, the present invention is aforementioned to be coated in Graphene in the method that chemical fibre surface makes composite fibre, in step (4)-(5), and the concentration <2% of ammoniacal liquor.
The chief component of the composite fibre making according to the inventive method is sulfhydrylation Graphene, silver and chemical fibre, first fiber is carried out to surface treatment, carries out chemical silvering, and sulfhydrylation Graphene and silver plated fiber are in the combination of fiber surface afterwards.This composite fibre has high-heat conductive efficency and high mechanical properties simultaneously, and chemical fibre has superior stretch-proof performance as base, and selects Graphene as the thermal conductivity of coating material reinforcing glass fiber.
The present invention, by form a layer graphene coating at fiber surface, has improved the heat conduction and heat radiation efficiency of fiber effectively.
It is base material that the composite fibre that the present invention makes be take terylene, polyamide fibre, polypropylene fiber, and composite not only has toughness and the intensity of fiber, and has possessed on this basis good heat conductivility.
The composite fibre that the present invention makes can be used as the filler of injected plastics material, increases the mechanical performance of sheet material, bulk.Experiment showed, that the composite fibre that the present invention makes has better heat conduction and heat radiation performance compared to common fiber, and can keep original mechanical performance.
The composite fibre that the present invention makes has that preparation is simple, heat transfer efficiency is high, and mechanical strength is high, high temperature resistant, the advantage of corrosion resistance, can be widely used in the filler of Heat Conduction Material on market, with heat conductivility and the mechanical strength of reinforcing material.
Accompanying drawing explanation
Fig. 1 is the graphene coated afterwards surperficial SEM figure of polyster fibre.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, further set forth the present invention.These embodiment are interpreted as only for the present invention is described, is not used in and limits the scope of the invention.After having read the content of the present invention's record, those skilled in the art can make various changes or modifications the present invention, and these equivalences change and modification falls into the scope of the claims in the present invention equally.
Embodiment 1
Graphene is coated in to the method that PET fiber surface is made highly heat-conductive material
1, pre-treatment process
(1) oil removing: the ethanolic solution that is 200ml/L by volumetric concentration, as solvent, is removed the oil stain on terylene surface, and the processing time is 15min, after oil removing, cleans and dry terylene with deionized water;
(2) alligatoring: the terylene after oil removing is immersed in the sodium hydroxide solution of 80g/L, at 80 ℃ of temperature, processes 15min, clean with deionized water;
(3) sensitization: utilize dissolving with hydrochloric acid stannous chloride, until completely dissolved, then add deionized water to be mixed with the sensitizing solution of 15g/L, and add a small amount of tin grain in sensitizing solution; Terylene after alligatoring is immersed in sensitizing solution, take out after at room temperature processing 15min, with buck, clean, then clean with deionized water.In order to prevent divalent tin ion oxidation, in sensitizing solution, add a small amount of tin grain; With buck cleaning, being beneficial to two valency tin ions is hydrolyzed.
(4) activation: the liquor argenti nitratis ophthalmicus that compound concentration is 0.5-3g/L, drip ammoniacal liquor and occur reddish brown precipitation, continue to drip until precipitation disappears, add deionized water and be mixed with activating solution to 200ml; Terylene after sensitization is processed is immersed in activating solution, take out after processing 10min under room temperature, with deionized water, wash and dry.
2, Electroless Silver Plating
(1) oxidation solution preparation: first the 8g silver nitrate weighing up is dissolved in 1L deionized water, slowly add ammoniacal liquor (concentration <2%) and stir, until precipitation disappears, then add 2.5g NaOH, there is precipitation, slowly add again ammoniacal liquor and stir, until precipitation just disappears.
(2) reducing solution preparation: by the 15g/L glucose deionized water dissolving preparing.
(3) terylene through pre-treatment is placed in reducing solution, oxidation solution is dripped in reducing solution, ultrasonic processing 15min, after question response is complete, takes out terylene, and, oven dry clean with deionized water obtains chemical silvering terylene.
3, Graphene coating processes:
(1) sulfhydrylation Graphene-ethanolic solution that configuration concentration is 1%;
(2) 3g chemical silvering terylene is put into polytetrafluoroethylene (PTFE) reactor, the sulfhydrylation Graphene-ethanolic solution that adds 80ml to configure, puts into 60 ℃ of reflection 2h of baking oven;
(3) take out terylene, dry and obtain the graphene coated terylene in surface.Surface after polyster fibre is graphene coated as shown in Figure 1.
According to usual method, measure mechanical performance and the heat conductivility that terylene and embodiment 1 make the graphene coated terylene in surface, result is as following table 1-2:
The contrast of table 1. mechanical performance
| Sample | Fracture strength (cN/dtex) | Extension at break (%) |
| Terylene | 4.6 | 27.36 |
| The terylene that Graphene applies | 3.9 | 20.39 |
The contrast of table 2. heat conductivility
| Sample | Thermal conductivity factor (W/m ℃) | Specific heat capacity J/g.k |
| Terylene | 0.35 | 2.01 |
| Graphene applies terylene | 0.42 | 2.22 |
Embodiment 2
Graphene is coated in to the method that polypropylene fiber surface makes highly heat-conductive material
1, pre-treatment process
(1) oil removing: the ethanolic solution that is 220ml/L by volumetric concentration, as solvent, is removed the oil stain on polypropylene fibre surface, and the processing time is 15min, after oil removing, cleans and dry polypropylene fibre with deionized water;
(2) alligatoring: the polypropylene fibre after oil removing is immersed in the sodium hydroxide solution of 90g/L, at 85 ℃ of temperature, processes 20min, clean with deionized water;
(3) sensitization: utilize dissolving with hydrochloric acid stannous chloride, until completely dissolved, then add deionized water to be mixed with the sensitizing solution of 20g/L, and add a small amount of tin grain in sensitizing solution; Polypropylene fibre after alligatoring is immersed in sensitizing solution, take out after at room temperature processing 15min, with buck, clean, then clean with deionized water.In order to prevent divalent tin ion oxidation, in sensitizing solution, add a small amount of tin grain; With buck cleaning, being beneficial to two valency tin ions is hydrolyzed.
(4) activation: the liquor argenti nitratis ophthalmicus that compound concentration is 0.5-3g/L, drip ammoniacal liquor and occur reddish brown precipitation, continue to drip until precipitation disappears, add deionized water and be mixed with activating solution to 250ml; Polypropylene fibre after sensitization is processed is immersed in activating solution, take out after processing 15min under room temperature, with deionized water, wash and dry;
2, Electroless Silver Plating
(1) oxidation solution preparation: first the 5g silver nitrate weighing up is dissolved in 1L deionized water, slowly add ammoniacal liquor (concentration <2%) and stir, until precipitation disappears, then add 2.5g NaOH, there is precipitation, slowly add again ammoniacal liquor and stir, until precipitation just disappears.
(2) reducing solution preparation: by the 15g/L glucose deionized water dissolving preparing.
(3) polypropylene fibre through pre-treatment is placed in reducing solution, oxidation solution is dripped in reducing solution, ultrasonic processing 15min, after question response is complete, takes out fiber, and, oven dry clean with deionized water obtains chemical silvering polypropylene fibre.
3, Graphene coating processes:
(1) sulfhydrylation Graphene-ethanolic solution that configuration concentration is 2%;
(2) the silver-plated polypropylene fibre of 3g is put into polytetrafluoroethylene (PTFE) reactor, the sulfhydrylation Graphene-ethanolic solution that adds 80ml to configure, puts into 60 ℃ of reflection 2h of baking oven;
(3) take out polypropylene fibre, dry and obtain the graphene coated polypropylene fibre in surface.
According to usual method, measure mechanical performance and the heat conductivility that polypropylene fibre and embodiment 1 make the graphene coated polypropylene fibre in surface, result is as following table 3-4:
The contrast of table 3. mechanical performance
| Sample | Fracture strength (cN/dtex) | Extension at break (%) |
| Polypropylene fibre | 3.6 | 32.12 |
| Graphene applies polypropylene fibre | 2.9 | 24.38 |
The contrast of table 4. heat conductivility
| Sample | Thermal conductivity factor (W/m ℃) | Specific heat capacity J/g.k |
| Polypropylene fibre | 0.22 | 1.92 |
| Graphene applies polypropylene fibre | 0.31 | 2.11 |
Embodiment 3
Graphene is coated in to the method that nylon fibre surface makes highly heat-conductive material
1, pre-treatment process
(1) oil removing: the ethanolic solution that is 200ml/L by volumetric concentration, as solvent, is removed the oil stain on polyamide fibre surface, and the processing time is 15min, after oil removing, cleans and dry polyamide fibre with deionized water;
(2) alligatoring: the polyamide fibre after oil removing is immersed in the sodium hydroxide solution of 80g/L, at 80 ℃ of temperature, processes 15min, clean with deionized water;
(3) sensitization: utilize dissolving with hydrochloric acid stannous chloride, until completely dissolved, then add deionized water to be mixed with the sensitizing solution of 20g/L, and add a small amount of tin grain in sensitizing solution; Polyamide fibre after alligatoring is immersed in sensitizing solution, take out after at room temperature processing 15min, with buck, clean, then clean with deionized water.In order to prevent divalent tin ion oxidation, in sensitizing solution, add a small amount of tin grain; With buck cleaning, being beneficial to two valency tin ions is hydrolyzed.
(4) activation: the liquor argenti nitratis ophthalmicus that compound concentration is 0.5-3g/L, drip ammoniacal liquor and occur reddish brown precipitation, continue to drip until precipitation disappears, add deionized water and be mixed with activating solution to 250ml; Polyamide fibre after sensitization is processed is immersed in activating solution, take out after processing 15min under room temperature, with deionized water, wash and dry;
2, Electroless Silver Plating
(1) oxidation solution preparation: first the 10g silver nitrate weighing up is dissolved in 1L deionized water, slowly add ammoniacal liquor (concentration <2%) and stir, until precipitation disappears, then add 2.5g NaOH, there is precipitation, slowly add again ammoniacal liquor and stir, until precipitation just disappears.
(2) reducing solution preparation: by the 15g/L glucose deionized water dissolving preparing.
(3) polyamide fibre through pre-treatment is placed in reducing solution, oxidation solution is dripped in reducing solution, ultrasonic processing 15min, after question response is complete, takes out polyamide fibre, and, oven dry clean with deionized water obtains chemical silvering polyamide fibre.
3, Graphene coating processes:
(1) sulfhydrylation Graphene-ethanolic solution that configuration concentration is 1.5%;
(2) the silver-plated polyamide fibre of 3g is put into polytetrafluoroethylene (PTFE) reactor, the sulfhydrylation Graphene-ethanolic solution that adds 80ml to configure, puts into 60 ℃ of reflection 2h of baking oven;
(3) take out fiber, dry and obtain the graphene coated polyamide fibre in surface.
According to usual method, measure mechanical performance and the heat conductivility that polyamide fibre and embodiment 1 make the graphene coated polyamide fibre in surface, result is as following table 5-6:
The contrast of table 5. mechanical performance
| Sample | Fracture strength (cN/dtex) | Extension at break (%) |
| Polyamide fibre | 4.35 | 32.21 |
| Graphene applies polyamide fibre | 3.92 | 27.63 |
The contrast of table 6. heat conductivility
| Sample | Thermal conductivity factor (W/m ℃) | Specific heat capacity J/g.k |
| Polyamide fibre | 0.25 | 1.67 |
| Graphene applies polyamide fibre | 0.32 | 1.93 |
Claims (4)
1. Graphene is coated in to the method that chemical fibre surface makes composite fibre, it is characterized in that, comprise the steps:
(1) oil removing: the ethanolic solution that is 180-240ml/L by volumetric concentration, as solvent, is removed the oil stain on chemical fibre surface, and the processing time is 10-20min, after oil removing, cleans and dry chemical fibre with deionized water;
(2) alligatoring: according to different chemical fibres, the chemical fibre after oil removing is immersed in the sodium hydroxide solution of 70-90g/L, at 70-85 ℃ of temperature, processes 10-25min, clean with deionized water;
(3) sensitization: utilize dissolving with hydrochloric acid stannous chloride, until completely dissolved, then add deionized water to be mixed with the sensitizing solution of 10-30g/L, and add a small amount of tin grain in sensitizing solution; Chemical fibre after alligatoring is immersed in sensitizing solution, take out after at room temperature processing 10-20min, with buck, clean, then clean with deionized water;
(4) activation: the liquor argenti nitratis ophthalmicus that compound concentration is 0.5-3g/L, drip ammoniacal liquor and occur reddish brown precipitation, continue to drip until precipitation disappears, add deionized water and be mixed with activating solution to 100-300ml; Chemical fibre after sensitization is processed is immersed in activating solution, take out after processing 5-20min under room temperature, with deionized water, wash and dry;
(5) chemical silvering: slowly add ammoniacal liquor in the liquor argenti nitratis ophthalmicus that is 5-10g/L in concentration and stir, until precipitation disappears, adding concentration is the NaOH of 2-4g/L, there is precipitation, slowly add again ammoniacal liquor and stir, until precipitation just disappears, being mixed with oxidation solution; By glucose deionized water dissolving, be mixed with the reducing solution that concentration is 10-20g/L; Chemical fibre through pre-treatment is placed in reducing solution, oxidation solution is dripped in reducing solution, ultrasonic processing 10-20min, after question response is complete, takes out chemical fibre, with deionized water, cleans and dries;
(6) apply: the ethanolic solution of silver-plated chemical fibre being put into the sulfhydrylation Graphene of 1-5%, fully reaction in reactor, the combination between sulfydryl and silver ion obtains the chemical fibre that Graphene applies after sulfhydrylation Graphene is coated in to silver-plated chemical fibre surface.
2. the method that Graphene is coated in to chemical fibre surface making composite fibre according to claim 1, is characterized in that, chemical fibre is terylene, polypropylene fibre or polyamide fibre.
3. the method that Graphene is coated in to chemical fibre surface making composite fibre according to claim 1, is characterized in that, in step (4)-(5), and the concentration <2% of ammoniacal liquor.
4. the composite fibre that in claim 1-3, the method described in any one makes.
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| CN104611786A (en) * | 2015-02-03 | 2015-05-13 | 广东泰宝医疗科技股份有限公司 | Method for preparing persistent inhibition carbon fiber dressing |
| CN105821663A (en) * | 2016-05-10 | 2016-08-03 | 北京创新爱尚家科技股份有限公司 | Conductive graphene fiber and production method and system |
| CN106758179A (en) * | 2017-01-16 | 2017-05-31 | 苏州泰克银纤维科技有限公司 | A kind of silver-coating method of polyamide fibre DTY fiber |
| CN107032799A (en) * | 2017-05-18 | 2017-08-11 | 成都新柯力化工科技有限公司 | A kind of pantograph pan graphene reinforcing glass fiber and preparation method |
| CN108774890A (en) * | 2018-06-29 | 2018-11-09 | 杭州白熊科技有限公司 | Temperature self controlled electrically-heated fiber of organic PTC based on graphene and its preparation method and application |
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| CN107032799A (en) * | 2017-05-18 | 2017-08-11 | 成都新柯力化工科技有限公司 | A kind of pantograph pan graphene reinforcing glass fiber and preparation method |
| CN107032799B (en) * | 2017-05-18 | 2019-06-11 | 海安县中祥线业有限公司 | A kind of pantograph pan graphene reinforcing glass fiber and preparation method |
| CN108774890A (en) * | 2018-06-29 | 2018-11-09 | 杭州白熊科技有限公司 | Temperature self controlled electrically-heated fiber of organic PTC based on graphene and its preparation method and application |
| CN114892394A (en) * | 2022-06-08 | 2022-08-12 | 深圳市乐清合兴电子有限公司 | Multilayer conductive cloth and manufacturing method thereof |
| CN114892394B (en) * | 2022-06-08 | 2023-09-22 | 深圳市乐清合兴电子有限公司 | Multilayer conductive cloth and manufacturing method thereof |
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