CN103881298A - Thermosetting resin composite material with electricity and heat conduction functions, and preparation method thereof - Google Patents
Thermosetting resin composite material with electricity and heat conduction functions, and preparation method thereof Download PDFInfo
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- CN103881298A CN103881298A CN201210558250.8A CN201210558250A CN103881298A CN 103881298 A CN103881298 A CN 103881298A CN 201210558250 A CN201210558250 A CN 201210558250A CN 103881298 A CN103881298 A CN 103881298A
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- thermosetting resin
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Abstract
The invention discloses a thermosetting resin composite material with electricity and heat conduction functions, and a preparation method thereof. The thermosetting resin composite material with electricity and heat conduction functions includes a continuous carbon fiber (a), a graphite nanosheet (b) and a thermosetting resin (c). The thermosetting resin can be one or more of epoxy resin, unsaturated polyester, and polyurethane or polyimide. The composite material concretely comprises, by mass, 10-65 parts of the continuous carbon fiber, 5-20 parts of the graphite nanosheet and 30-85 parts of the thermosetting resin. The preparation method of the composite material comprises the following steps: mixing the graphite nanosheet or expandable graphite with a thermosetting resin liquid prepolymer composition to prepare a dipping liquid, dipping the continuous carbon fiber in the dipping liquid to make the continuous carbon fiber attached with the dipping liquid, and adopting a pultrusion technology, a winding technology or a molding technology to prepare the composite material. The composite material has enhanced mechanical properties in a three-dimensional direction, has excellent heat and electricity conduction properties, and has balanced comprehensive properties.
Description
One, technical field
The present invention relates to conductive and heat-conductive functional composite material and preparation method thereof, particularly thermosetting resin conductive and heat-conductive functional composite material and preparation method thereof, belongs to functional composite material field.
Two, background technology
Carbon fiber has the excellent properties such as the low and thermal expansivity of high specific strength, high ratio modulus, high temperature resistant, conduction, heat conduction, density is little, is with a wide range of applications in fields such as spaceship, aerospacecraft, man-made satellite, automobile ships, building and machineries.Continuous carbon fibre/thermosetting resin polymer composites can be in a big way adjusting function as required, be the most promising novel texture functional materials at present.
Carbon fiber only presents obvious enhancing, conduction and conduction effect in fiber direction to matrix material conventionally, therefore the anisotropy of continuous carbon fibre/polymer composites is very outstanding, its excellent physical and mechanical property all concentrates on fiber direction, and horizontal without fiber reinforcement, heat conduction, electric action at matrix material, horizontal mechanical strength, heat-conductivity conducting poor performance, therefore transverse mechanical intensity, mechanical moduli, shock resistance, electroconductibility and the thermal conductivity etc. of matrix material are all lower, large with longitudinal direction difference.For the Application Areas of the shape goods such as flat board, tubing or section bar and many complicated applied forces, this is obvious deficiency and the shortcoming of current continuous carbon fibre/polymer composites, particularly pultrusion composite materials.
Three, summary of the invention
The object of the invention is to provide thermosetting resin conductive and heat-conductive functional composite material that a kind of over-all properties is more excellent and preparation method thereof.
The technical solution that realizes the object of the invention is: a kind of thermosetting resin conductive and heat-conductive functional composite material, comprises (a) continuous carbon fibre, (b) nano graphite sheet and (c) thermosetting resin.
The thermosetting resin that thermosetting resin conductive and heat-conductive functional composite material of the present invention adopts can be one or more in epoxy resin, unsaturated polyester, urethane or polyimide.
In thermosetting resin conductive and heat-conductive functional composite material of the present invention, continuous carbon fibre 10~65 mass parts, nano graphite sheet 5~20 mass parts, thermosetting resin 30~85 mass parts.
The preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention can be: comprise the following steps successively:
(1) expansible black lead is expanded and makes expanded graphite and expanded graphite is peeled off and made nano graphite sheet, or expansible black lead is expanded and makes expanded graphite;
(2) liquid to nano graphite sheet and thermosetting resin pre-polymerization composition is mixed and is made into the compound dipping solution of nano graphite sheet-thermosetting resin, or liquid to expanded graphite and thermosetting resin pre-polymerization composition is mixed and is made into the compound dipping solution of nano graphite sheet-thermosetting resin;
(3) continuous carbon fibre is immersed to the compound dipping solution of nano graphite sheet-thermosetting resin, make continuous carbon fibre enclose the compound dipping solution of nano graphite sheet-thermosetting resin;
(4) the continuous carbon fibre set of enclosing the compound dipping solution of nano graphite sheet-thermosetting resin is formed to specified shape aggregate;
(5) the specified shape aggregate of formation is solidified and obtains matrix material.
Between (1) step described in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention and (2) step, can increase that expanded graphite carries out surface modification treatment step or nano graphite sheet carries out surface modification treatment step.
Thermosetting resin 95~70 mass parts in compound dipping solution described in (2) step described in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention, nano graphite sheet 5~30 mass parts.
(3) continuous carbon fibre that step adopts described in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention is the continuous carbon fibre after surface modification preferably.
The method that described in (4) step described in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention, the continuous carbon fibre set of enclosing the compound dipping solution of nano graphite sheet-thermosetting resin is formed to specified shape aggregate can be pultrude process, winding process or mould pressing process.
The thermosetting resin adopting in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention can be one or more in epoxy resin, unsaturated polyester, urethane or polyimide.
Compared with prior art, the present invention has significant advantage.Continuous carbon fibre is the one dimension reinforcement of high-strength and high-modulus, and graphite nanosheets (expanded graphite recombination process can become graphite nanosheets) is the two-dimentional reinforcement of high-strength and high-modulus, and they are electrical conductor and heat conductor both.Continuous carbon fibre only has excellent reinforced effects and electrical and thermal conductivity performance in its carbon fiber direction, and in the resin matrix of graphite nanosheets disperse between continuous carbon fibre, direction (or claiming another two-dimensional directional) in vertical carbon fiber direction presents enhancement and electrical and thermal conductivity performance, therefore composite materials property of the present invention, conductivity and heat conductivility are all more excellent and more balanced on three-dimensional, can bring into play better the excellent properties of continuous carbon fibre composite material than current continuous carbon fibre/same with thermosetting compound material, meet better high-tech sector for material lightweight, high-strength, the demand of multifunction, can be in aerospace, automobile ships, mechanical industry, mining industry, the fields such as electronic appliance obtain better application.
Four, embodiment
The hot thermosetting resin conductive and heat-conductive of the present invention functional composite material, comprises (a) continuous carbon fibre, (b) nano graphite sheet and (c) thermosetting resin.
The thermosetting resin that thermosetting resin conductive and heat-conductive functional composite material of the present invention adopts is one or more in epoxy resin, unsaturated polyester, urethane or polyimide.
In thermosetting resin conductive and heat-conductive functional composite material of the present invention, continuous carbon fibre 10~65 mass parts, nano graphite sheet 5~20 mass parts, thermosetting resin 30~85 mass parts.
The preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention can be: comprise the following steps successively:
(1) expansible black lead is expanded and makes expanded graphite and expanded graphite is peeled off and made nano graphite sheet, or expansible black lead is expanded and makes expanded graphite;
(2) liquid to nano graphite sheet and thermosetting resin pre-polymerization composition is mixed and is made into the compound dipping solution of nano graphite sheet-thermosetting resin, or liquid to expanded graphite and thermosetting resin pre-polymerization composition is mixed and is made into the compound dipping solution of nano graphite sheet-thermosetting resin;
(3) continuous carbon fibre is immersed to the compound dipping solution of nano graphite sheet-thermosetting resin, make continuous carbon fibre enclose the compound dipping solution of nano graphite sheet-thermosetting resin;
(4) the continuous carbon fibre set of enclosing the compound dipping solution of nano graphite sheet-thermosetting resin is formed to specified shape aggregate;
(5) the specified shape aggregate of formation is solidified and obtains matrix material.
The liquid pre-polymerization composition of thermosetting resin described in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention, refer to the fluid composition that thermosetting resin prepolymer and solidifying agent (or linking agent), reaction promoter (as promotor, initiator, catalyzer, promotor etc.), solvent and other additives (as filler, pigment, fire retardant etc.) etc. mix, its under proper condition (as being heated or other) be solidified into solid polymer (as epoxy resin, unsaturated polyester, urethane or polyimide).Such as, the liquid form mixt of epoxy prepolymer and solidifying agent (as fatty amine curing agent, aromatic amine curing agent, acid anhydride type curing agent etc.), promotor (as DMP-30); The liquid form mixt of unsaturated polyester prepolymer and linking agent (as vinylbenzene), initiator (as dibenzoyl peroxide etc.), promotor (as cobalt naphthenate) etc.; The liquid form mixt of isocyanate-monomer and polyvalent alcohol monomer (as polyester polyol or polyether glycol), catalyzer (as tertiary amines, organic tin etc.) etc.; Deng.
Between (1) step described in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention and (2) step, can increase that expanded graphite carries out surface modification treatment step or nano graphite sheet carries out surface modification treatment step, can improve like this expanded graphite or nano graphite sheet and be combined with the interface of thermosetting resin, make the performance of thermosetting resin conductive and heat-conductive functional composite material of the present invention better.
Thermosetting resin 95~70 mass parts in compound dipping solution described in (2) step described in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention, nano graphite sheet 5~30 mass parts.
(3) continuous carbon fibre that step adopts described in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention is the continuous carbon fibre after surface modification preferably, can improve like this continuous carbon fibre and be combined with the interface of thermosetting resin, make the performance of thermosetting resin conductive and heat-conductive functional composite material of the present invention better.
The method that described in (4) step described in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention, the continuous carbon fibre set of enclosing the compound dipping solution of nano graphite sheet-thermosetting resin is formed to specified shape aggregate can be pultrude process, winding process or mould pressing process.
The thermosetting resin adopting in the preparation method of thermosetting resin conductive and heat-conductive functional composite material of the present invention is one or more in epoxy resin, unsaturated polyester, urethane or polyimide.
Embodiment 1 adopts epoxy resin E-51, solidifying agent MeHHPA to be mixed in proportion and adds appropriate altax P-30 to be made into the liquid pre-polymerization composition of epoxy resin.Then expanded graphite is sneaked into the liquid pre-polymerization composition mixing of epoxy resin and be made into the compound dipping solution of nano graphite sheet-epoxy resin, expanded graphite massfraction is 15%.Continuous carbon fibre is immersed to the compound dipping solution of nano graphite sheet-epoxy resin, make continuous carbon fibre enclose the compound dipping solution of nano graphite sheet-epoxy resin, adopt pultrude process set to form block aggregate the continuous carbon fibre of enclosing the compound dipping solution of nano graphite sheet-epoxy resin, finally be heated to 100 ℃ from room temperature temperature programming gradually, make the block aggregate forming fully solidify and obtain matrix material (continuous carbon fibre massfraction 35%).The tensile strength 1.35GPa of block matrix material, tensile modulus 125GPa, electric conductivity 25S/cm, thermal conductivity 2.6W/mK.
Embodiment 2 adopts P61972 unsaturated polyester, dibenzoyl peroxide and promotor cobalt naphthenate to be mixed in proportion and is made into the liquid pre-polymerization composition of unsaturated polyester.Expanded graphite is peeled off and become nano graphite sheet by ultrasonic wave, nano graphite sheet is sneaked into the liquid pre-polymerization composition mixing of unsaturated polyester and be made into the compound dipping solution of nano graphite sheet-unsaturated polyester, expanded graphite massfraction is 25%.Surface treatment continuous carbon fibre is immersed to the compound dipping solution of nano graphite sheet-unsaturated polyester, make continuous carbon fibre enclose the compound dipping solution of nano graphite sheet-unsaturated polyester, adopt winding process set to form block aggregate the continuous carbon fibre of enclosing the compound dipping solution of nano graphite sheet-unsaturated polyester, finally be heated to 60 ℃ from room temperature temperature programming gradually, make the block aggregate forming fully solidify and obtain matrix material (continuous carbon fibre massfraction 45%).The tensile strength 1.42GPa of block matrix material, tensile modulus 138GPa, electric conductivity 31S/cm, thermal conductivity 3.3W/mK.
Embodiment 3 adopts poly methylene poly phenyl poly isocyanate and polyether glycol 4110 to be mixed in proportion and adds the sub-tin of octoate catalyst to be made into the liquid pre-polymerization composition of urethane.Expanded graphite is peeled off and become nano graphite sheet by ultrasonic wave, nano graphite sheet is sneaked into the liquid pre-polymerization composition mixing of urethane and be made into the compound dipping solution of nano graphite sheet-urethane, nano graphite sheet massfraction is 10%.Surface treatment continuous carbon fibre is immersed to the compound dipping solution of nano graphite sheet-urethane, make continuous carbon fibre enclose the compound dipping solution of nano graphite sheet-urethane, adopt mould pressing process set to form block aggregate the continuous carbon fibre of enclosing the compound dipping solution of nano graphite sheet-urethane, finally be heated to 60 ℃ from room temperature temperature programming gradually, make the block aggregate forming fully solidify and obtain matrix material (continuous carbon fibre massfraction 50%).The tensile strength 1.78GPa of block matrix material, tensile modulus 147GPa, electric conductivity 36S/cm, thermal conductivity 3.8W/mK.
The dimethyl sulphoxide solution mixing that expanded graphite is sneaked into polyamic acid by embodiment 4 is made into the compound dipping solution of nano graphite sheet-polyamic acid, and nano graphite sheet massfraction is 35%.Surface treatment continuous carbon fibre is immersed to the compound dipping solution of nano graphite sheet-polyamic acid, make continuous carbon fibre enclose the compound dipping solution of nano graphite sheet-polyamic acid, adopt pultrude process set to form block aggregate the continuous carbon fibre of enclosing the compound dipping solution of nano graphite sheet-polyamic acid, heat drying is removed dimethyl sulfoxide solvent, finally heat up and be heated to 350 ℃ of cyclodehydrations, make the block aggregate forming fully solidify and obtain polyimide-based composite material (continuous carbon fibre 65%).The tensile strength 1.85GPa of block matrix material, tensile modulus 158GPa, electric conductivity 44S/cm, thermal conductivity 4.3W/mK.
Claims (9)
1. a thermosetting resin conductive and heat-conductive functional composite material, is characterized in that: comprise (a) continuous carbon fibre, (b) nano graphite sheet and (c) thermosetting resin.
2. thermosetting resin conductive and heat-conductive functional composite material according to claim 1, is characterized in that: thermosetting resin is one or more in epoxy resin, unsaturated polyester, urethane or polyimide.
3. according to thermosetting resin conductive and heat-conductive functional composite material described in claim 1 or 2, it is characterized in that: continuous carbon fibre 10~65 mass parts, nano graphite sheet 5~20 mass parts, thermosetting resin 30~85 mass parts.
4. according to a preparation method for thermosetting resin conductive and heat-conductive functional composite material described in claim 1~3 any one, it is characterized in that: comprise the following steps successively:
(1) expansible black lead is expanded and makes expanded graphite and expanded graphite is peeled off and made nano graphite sheet, or expansible black lead is expanded and makes expanded graphite;
(2) liquid to nano graphite sheet and thermosetting resin pre-polymerization composition is mixed and is made into the compound dipping solution of nano graphite sheet-thermosetting resin, or liquid to expanded graphite and thermosetting resin pre-polymerization composition is mixed and is made into the compound dipping solution of nano graphite sheet-thermosetting resin;
(3) continuous carbon fibre is immersed to the compound dipping solution of nano graphite sheet-thermosetting resin, make continuous carbon fibre enclose the compound dipping solution of nano graphite sheet-thermosetting resin;
(4) the continuous carbon fibre set of enclosing the compound dipping solution of nano graphite sheet-thermosetting resin is formed to specified shape aggregate;
(5) the specified shape aggregate of formation is solidified and obtains matrix material.
5. the preparation method of thermosetting resin conductive and heat-conductive functional composite material according to claim 4, is characterized in that: between (1) step and (2) step, increase that expanded graphite carries out surface modification treatment step or nano graphite sheet carries out surface modification treatment step.
6. according to the preparation method of thermosetting resin conductive and heat-conductive functional composite material described in claim 4 or 5, it is characterized in that: thermosetting resin 95~70 mass parts in compound dipping solution described in (2) step, nano graphite sheet 5~30 mass parts.
7. according to the preparation method of thermosetting resin conductive and heat-conductive functional composite material described in claim 4~6 any one, it is characterized in that: (3) continuous carbon fibre that step adopts is the continuous carbon fibre after surface modification.
8. according to the preparation method of thermosetting resin conductive and heat-conductive functional composite material described in claim 4~7 any one, it is characterized in that: the method that described in (4) step, the continuous carbon fibre set of enclosing the compound dipping solution of nano graphite sheet-thermosetting resin is formed to specified shape aggregate is pultrude process, winding process or mould pressing process.
9. according to the preparation method of thermosetting resin conductive and heat-conductive functional composite material described in claim 4~8 any one, it is characterized in that: thermosetting resin is one or more in epoxy resin, unsaturated polyester, urethane or polyimide.
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CN104387727A (en) * | 2014-11-21 | 2015-03-04 | 芜湖市宝艺游乐科技设备有限公司 | Expanded graphite modified epoxy resin composite material and preparation method thereof |
CN105199317A (en) * | 2015-09-17 | 2015-12-30 | 吉林化工学院 | Method for preparing high-tenacity high-strength epoxy-resin-based conductive composite |
CN106336618A (en) * | 2016-09-12 | 2017-01-18 | 中电科芜湖钻石飞机制造有限公司 | High-heat-conductivity carbon fiber composite material and preparation method thereof |
CN106898409A (en) * | 2017-04-21 | 2017-06-27 | 广东国利先进复合材料研发有限公司 | A kind of conductive plate and preparation method thereof |
CN109135512A (en) * | 2018-09-03 | 2019-01-04 | 武汉掌声科技有限责任公司 | A kind of building template release coating |
CN109281157A (en) * | 2018-11-23 | 2019-01-29 | 南昌航空大学 | Graphene nanometer sheet-multi-walled carbon nanotube sizing agent modified carbon fiber method |
CN109504036A (en) * | 2018-11-16 | 2019-03-22 | 南昌航空大学 | A kind of micro-nano graphite flake epoxy resin-matrix/modified carbon fiber composite material and preparation method |
CN111395001A (en) * | 2020-03-30 | 2020-07-10 | 联新(开平)高性能纤维有限公司 | Conductive dipping solution, preparation method and application thereof, dipped cord and preparation method and application thereof |
CN114530278A (en) * | 2022-03-22 | 2022-05-24 | 合肥中南光电有限公司 | Conductive slurry for HJT battery and production process thereof |
CN114874605A (en) * | 2022-05-09 | 2022-08-09 | 上海大学 | Continuous carbon fiber reinforced thermosetting resin prepreg filament and preparation method and application thereof |
CN115011073A (en) * | 2022-07-07 | 2022-09-06 | Oppo广东移动通信有限公司 | Fiber reinforced plastic, preparation method thereof, electronic equipment structural member and electronic equipment |
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Cited By (12)
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CN104387727A (en) * | 2014-11-21 | 2015-03-04 | 芜湖市宝艺游乐科技设备有限公司 | Expanded graphite modified epoxy resin composite material and preparation method thereof |
CN105199317A (en) * | 2015-09-17 | 2015-12-30 | 吉林化工学院 | Method for preparing high-tenacity high-strength epoxy-resin-based conductive composite |
CN106336618A (en) * | 2016-09-12 | 2017-01-18 | 中电科芜湖钻石飞机制造有限公司 | High-heat-conductivity carbon fiber composite material and preparation method thereof |
CN106898409A (en) * | 2017-04-21 | 2017-06-27 | 广东国利先进复合材料研发有限公司 | A kind of conductive plate and preparation method thereof |
CN109135512A (en) * | 2018-09-03 | 2019-01-04 | 武汉掌声科技有限责任公司 | A kind of building template release coating |
CN109504036A (en) * | 2018-11-16 | 2019-03-22 | 南昌航空大学 | A kind of micro-nano graphite flake epoxy resin-matrix/modified carbon fiber composite material and preparation method |
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CN109281157A (en) * | 2018-11-23 | 2019-01-29 | 南昌航空大学 | Graphene nanometer sheet-multi-walled carbon nanotube sizing agent modified carbon fiber method |
CN111395001A (en) * | 2020-03-30 | 2020-07-10 | 联新(开平)高性能纤维有限公司 | Conductive dipping solution, preparation method and application thereof, dipped cord and preparation method and application thereof |
CN114530278A (en) * | 2022-03-22 | 2022-05-24 | 合肥中南光电有限公司 | Conductive slurry for HJT battery and production process thereof |
CN114874605A (en) * | 2022-05-09 | 2022-08-09 | 上海大学 | Continuous carbon fiber reinforced thermosetting resin prepreg filament and preparation method and application thereof |
CN115011073A (en) * | 2022-07-07 | 2022-09-06 | Oppo广东移动通信有限公司 | Fiber reinforced plastic, preparation method thereof, electronic equipment structural member and electronic equipment |
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Application publication date: 20140625 |