CN106589809B - A kind of preparation method of carbon fiber/epoxy resin composite material - Google Patents

A kind of preparation method of carbon fiber/epoxy resin composite material Download PDF

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CN106589809B
CN106589809B CN201510680957.XA CN201510680957A CN106589809B CN 106589809 B CN106589809 B CN 106589809B CN 201510680957 A CN201510680957 A CN 201510680957A CN 106589809 B CN106589809 B CN 106589809B
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carbon fiber
epoxy resin
carbon
minutes
preparation
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CN106589809A (en
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徐凯
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Zhangjiagang Shunchen Machinery Co Ltd
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Zhangjiagang Shunchen Machinery Co Ltd
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Abstract

, the preparation of carbon fiber this application discloses a kind of preparation methods of carbon fiber/epoxy resin composite material, comprising: (1);(2), the surface treatment of carbon fiber;(3), the carbon fiber of surface treatment is dried in vacuo.(4), at 40~50 DEG C blending epoxy and curing agent and stir 30~40 minutes;(5), carbon fiber and diluent are added in the mixture of epoxy resin and curing agent agitation grinding 30 minutes, the mass ratio of the carbon fiber and epoxy resin is (5~20): 100;(6), it is added acetone ultrasonic disperse 10~30 minutes at 50~70 DEG C;(7), under vacuum condition, 50~70 DEG C is heated to and is stirred simultaneously vacuum defoamation 6~8 hours, target product is obtained.In technical solution of the present invention, the raw material sources of carbon fiber are abundant, and preparation cost is low, and composite material obtained is lighter, have high intensity, high temperature resistant, high thermal conductivity characteristic, can be used for field of aerospace.

Description

A kind of preparation method of carbon fiber/epoxy resin composite material
Technical field
The application belongs to technical field of electronic devices, more particularly to a kind of system of carbon fiber/epoxy resin composite material Preparation Method, the heat dissipation for electronic device.
Background technique
The connection procedure of electronic equipment and heat dissipation equipment is the interfacial contact of solid and solid, realizes that contact heat-exchanging is very much The approach of electronic radiation.
Microcosmic rough two surfaces contact is not complete enough, causes contact surface to generate contact resistance, is present in bumps Air between uneven gap has very big influence to the conducting power of heat dissipation, because air is the non-conductor of heat.Even and if In two surfaces of solids these gaps can not also eliminated using biggish pressure, and some electronic components are unbearable larger Pressure, will result in bigger gap in this way, the serious heat for hindering electronic component be also conducted to cooling fin.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of carbon fiber/epoxy resin composite material, existing to overcome Deficiency in technology.
To achieve the above object, the invention provides the following technical scheme:
The embodiment of the present application discloses a kind of preparation method of carbon fiber/epoxy resin composite material, comprising:
(1), the preparation of carbon fiber;
(2), it the surface treatment of carbon fiber: carbon fiber is put into aoxidize 3~5 hours in 65~68% concentrated nitric acid takes Out, with distilled water repeated flushing;
(3), the carbon fiber of surface treatment is dried in vacuo.
(4), at 40~50 DEG C blending epoxy and curing agent and stir 30~40 minutes;
(5), carbon fiber and diluent are added in the mixture of epoxy resin and curing agent agitation grinding 30 minutes, institute The mass ratio for stating carbon fiber and epoxy resin is (5~20): 100;
(6), it is added acetone ultrasonic disperse 10~30 minutes at 50~70 DEG C;
(7), under vacuum condition, 50~70 DEG C is heated to and is stirred simultaneously vacuum defoamation 6~8 hours, target product is obtained.
Preferably, in the preparation method of above-mentioned carbon fiber/epoxy resin composite material, in the step (1), carbon fiber The preparation method of dimension includes: to mix the PVP of the PAN of 8.9%wt and 1%wt, and the DMF of 90%wt is added, magnetic agitation 3 small When, clear solution is obtained, ‰ nickel acetate of 1wt is added, stirring is until form the spinning precursor solution of green transparent, presoma Solution obtains PAN/PVP/ nickel acetate composite nano fiber by electrostatic spinning technique, and PAN/PVP/ nickel acetate composite Nano is fine Dimension is heat-treated 2h under 275 DEG C of air atmospheres, and heating rate is 1 DEG C/min, is subsequently transferred in tube furnace, 2 are put into boiler tube The PVP of times PAN/PVP/ nickel acetate composite nano fiber quality, under an argon atmosphere, 900 DEG C are heat-treated 120 minutes, are divided The carbon nanotube of level structure/nickel carbon fiber composite carbon material, carbon nanotube/nickel carbon fiber composite carbon material of hierarchical structure with Potassium hydroxide reacts 30 minutes under 250 degree, then is warming up to 750 degree of 1 hours of reaction, and under an argon atmosphere, heating is fast for reaction Rate is 5 DEG C/min, carbon nanotube/nickel carbon fiber composite carbon material of the hierarchical structure after being activated, the classification knot after activation The carbon nanotube of structure/nickel carbon fiber composite carbon material is put into the nitric acid solution of 7M, is removed nickel, is obtained the carbon of hierarchical structure Pipe/carbon fiber complex carbon material.
Preferably, in the preparation method of above-mentioned carbon fiber/epoxy resin composite material, the epoxy resin is to shrink One or more of glycerol ether type epoxy resins, glycidyl ester epoxy resin and linear aliphatic epoxy resin Mixture.
Preferably, in the preparation method of above-mentioned carbon fiber/epoxy resin composite material, the curing agent is polyamide Resin.
Compared with the prior art, the advantages of the present invention are as follows: the raw material sources of carbon fiber are abundant, and preparation cost is low, is obtained The composite material obtained is lighter, has high intensity, high temperature resistant, high thermal conductivity characteristic, can be used for field of aerospace.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
In the present embodiment, the preparation method of carbon fiber/epoxy resin composite material, comprising:
(1), the preparation of carbon fiber:
The PVP (1,000,000---1,500,000g/mol) of the PAN (150,000g/mol) and 1%wt of 8.9%wt are mixed It closes, the DMF (n,N-Dimethylformamide) of 90%wt is added, 3 hours of magnetic agitation, obtains clear solution, adds 1wt ‰ Nickel acetate, stirring is until form the spinning precursor solution of green transparent.Precursor solution is obtained by electrostatic spinning technique PAN/PVP/ nickel acetate composite nano fiber.PAN/PVP/ nickel acetate composite nano fiber is heat-treated under 275 DEG C of air atmospheres 2h, heating rate are 1 DEG C/min.It is subsequently transferred in tube furnace, it is fine that 2 times of PAN/PVP/ nickel acetate composite Nanos is put into boiler tube The PVP for tieing up quality, under argon gas (99.99%) atmosphere, 900 DEG C are heat-treated 120 minutes, obtain the carbon nanotube of hierarchical structure/ Nickel carbon fiber composite carbon material.The carbon nanotube of hierarchical structure/nickel carbon fiber composite carbon material and potassium hydroxide (mass ratio 1: 5) it is reacted 30 minutes under 250 degree, then is warming up to 750 degree of 1 hours of reaction, reacted under an argon atmosphere, heating rate 5 DEG C/min, carbon nanotube/nickel carbon fiber composite carbon material of the hierarchical structure after being activated.Hierarchical structure after activation Carbon nanotube/nickel carbon fiber composite carbon material is put into the nitric acid solution of 7M, is removed nickel, is obtained carbon pipe/carbon of hierarchical structure Fiber composite carbon material
(2), the surface treatment of carbon fiber:
Carbon fiber is put into 65~68% concentrated nitric acid to aoxidize 3 hours and be taken out, with distilled water repeated flushing.
(3), the carbon fiber of surface treatment is dried in vacuo.
(4), at 40 DEG C blending epoxy and curing agent and stir 30 minutes;
(5), carbon fiber and diluent are added in the mixture of epoxy resin and curing agent agitation grinding 30 minutes, carbon The mass ratio of fiber and epoxy resin is 1:20;
(6), it is added acetone ultrasonic disperse 10 minutes at 50 DEG C;
(7), under vacuum condition, 70 DEG C is heated to and is stirred simultaneously vacuum defoamation 6 hours, target product is obtained.
Microcosmic surface SEM test, heating conduction test and interface contact heat resistance is carried out to target product respectively to test, Known to:
(1), nano copper particle is evenly distributed, and contacts with each other to form thermally conductive network chain each other.
(2), the thermal coefficient of target product reaches 0.66W (m.K);
(3), when interfacial contact pressure is 1MPa, thermal contact resistance 26.53mm2K/W。
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.

Claims (3)

1. a kind of preparation method of carbon fiber/epoxy resin composite material characterized by comprising
(1), the preparation of carbon fiber: the PVP of the PAN of 8.9%wt and 1%wt is mixed, the DMF of 90%wt, magnetic agitation 3 is added A hour, clear solution is obtained, add ‰ nickel acetate of 1wt, spinning precursor solution of the stirring up to forming green transparent is preceding Liquid solution is driven by electrostatic spinning technique, obtains PAN/PVP/ nickel acetate composite nano fiber, PAN/PVP/ nickel acetate is compound to be received Rice fiber is heat-treated 2h under 275 DEG C of air atmospheres, and heating rate is 1 DEG C/min, is subsequently transferred in tube furnace, puts in boiler tube Enter the PVP of 2 times of PAN/PVP/ nickel acetate composite nano fiber quality, under an argon atmosphere, 900 DEG C are heat-treated 120 minutes, obtain The carbon nanotube of hierarchical structure/nickel carbon fiber composite carbon material, carbon nanotube/nickel carbon fiber composite carbon material of hierarchical structure It is reacted under 250 degree 30 minutes with potassium hydroxide, then is warming up to 750 degree of 1 hours of reaction, reaction under an argon atmosphere, heats up Rate is 5 DEG C/min, carbon nanotube/nickel carbon fiber composite carbon material of the hierarchical structure after being activated, the classification after activation The carbon nanotube of structure/nickel carbon fiber composite carbon material is put into the nitric acid solution of 7M, is removed nickel, is obtained hierarchical structure Carbon pipe/carbon fiber complex carbon material;
(2), the surface treatment of carbon fiber: carbon fiber is put into 65~68% concentrated nitric acid to aoxidize 3~5 hours and is taken out, used Distilled water repeated flushing;
(3), the carbon fiber of surface treatment is dried in vacuo;
(4), at 40~50 DEG C blending epoxy and curing agent and stir 30~40 minutes;
(5), carbon fiber and diluent are added in the mixture of epoxy resin and curing agent agitation grinding 30 minutes, the carbon The mass ratio of fiber and epoxy resin is (5~20): 100;
(6), it is added acetone ultrasonic disperse 10~30 minutes at 50~70 DEG C;
(7), under vacuum condition, 50~70 DEG C is heated to and is stirred simultaneously vacuum defoamation 6~8 hours, target product is obtained.
2. the preparation method of carbon fiber/epoxy resin composite material according to claim 1, it is characterised in that: the ring Oxygen resin is in glycidyl ether type epoxy resin, glycidyl ester epoxy resin and linear aliphatic epoxy resin One or more of mixtures.
3. the preparation method of carbon fiber/epoxy resin composite material according to claim 1, it is characterised in that: described solid Agent is polyamide.
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Publication number Priority date Publication date Assignee Title
CN107189356A (en) * 2017-07-07 2017-09-22 合肥新意境材料有限责任公司 A kind of carbon fiber epoxy resin composite material of modified pitch toughness reinforcing and preparation method thereof
CN109233203A (en) * 2018-08-29 2019-01-18 佛山皖和新能源科技有限公司 A kind of hydroelectric installation carbon fibre reinforced composite
CN110818306B (en) * 2019-11-21 2020-08-18 四川大学 Reinforcing and toughening agent for concrete and preparation method and application thereof
CN113858720B (en) * 2021-09-30 2023-10-03 深圳雷木新材料科技有限公司 Carbon fiber composite board and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1563557A (en) * 2004-04-05 2005-01-12 华南理工大学 Fiber sheet plate and usage
CN102153833A (en) * 2010-09-20 2011-08-17 青岛科技大学 Carbon fiber (powder)/epoxy resin composite material used for rapid prototyping die
CN103602042A (en) * 2013-10-31 2014-02-26 中科院广州化学有限公司 Liquid crystal epoxy resin - carbon fiber composite material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1563557A (en) * 2004-04-05 2005-01-12 华南理工大学 Fiber sheet plate and usage
CN102153833A (en) * 2010-09-20 2011-08-17 青岛科技大学 Carbon fiber (powder)/epoxy resin composite material used for rapid prototyping die
CN103602042A (en) * 2013-10-31 2014-02-26 中科院广州化学有限公司 Liquid crystal epoxy resin - carbon fiber composite material and preparation method thereof

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