CN106589807B - A kind of preparation method of carbon fiber/nano-copper/epoxy resin composite material - Google Patents
A kind of preparation method of carbon fiber/nano-copper/epoxy resin composite material Download PDFInfo
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- CN106589807B CN106589807B CN201510680390.6A CN201510680390A CN106589807B CN 106589807 B CN106589807 B CN 106589807B CN 201510680390 A CN201510680390 A CN 201510680390A CN 106589807 B CN106589807 B CN 106589807B
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Abstract
, the preparation of carbon fiber this application discloses a kind of preparation methods of carbon fiber/nano-copper/epoxy resin composite material, comprising: (1)；(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, with distilled water repeated flushing；(3), the carbon fiber of surface treatment is dried in vacuo；(4), nano-copper/epoxy resin composite material is prepared；(5), carbon fiber, nano-copper/epoxy resin composite material and diluent are mixed and is fully ground；(6), acetone is added at 40~50 DEG C to carry out ultrasonic disperse 15~20 minutes；(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
Technical field
The application belongs to technical field of electronic devices, more particularly to a kind of carbon fiber/Nanometer Copper/epoxy resin composite wood
The preparation method of material, 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 method of carbon fiber/nano-copper/epoxy resin composite material, with gram
Take deficiency in the prior art.
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/nano-copper/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), nano-copper/epoxy resin composite material is prepared；
(5), carbon fiber, nano-copper/epoxy resin composite material and diluent are mixed and is fully ground；
(6), acetone is added at 40~50 DEG C to carry out ultrasonic disperse 15~20 minutes；
(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 above-mentioned carbon fiber/nano-copper/epoxy resin composite material preparation method, the step (1)
In, the preparation method of carbon fiber includes: to mix the PVP of the PAN of 8.9%wt and 1%wt, the DMF of 90%wt is added, magnetic force stirs
3 hours are mixed, clear solution is obtained, add ‰ nickel acetate of 1wt, stirring is until the spinning presoma for forming green transparent is molten
Liquid, precursor solution obtain PAN/PVP/ nickel acetate composite nano fiber by electrostatic spinning technique, and PAN/PVP/ nickel acetate is multiple
It closes nanofiber and is heat-treated 2h under 275 DEG C of air atmospheres, heating rate is 1 DEG C/min, is subsequently transferred in tube furnace, boiler tube
In be put into 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 carbon nanotube/nickel carbon fiber composite carbon material of hierarchical structure, carbon nanotube/nickel carbon fiber composite carbon of hierarchical structure
Material reacts 30 minutes with potassium hydroxide under 250 degree, then is warming up to 750 degree of 1 hours of reaction, reacts under an argon atmosphere,
Heating rate is 5 DEG C/min, carbon nanotube/nickel carbon fiber composite carbon material of the hierarchical structure after being activated, after activation
The carbon nanotube of hierarchical structure/nickel carbon fiber composite carbon material is put into the nitric acid solution of 7M, and nickel is removed, and obtains classification knot
Carbon pipe/carbon fiber complex carbon material of structure.
Preferably, in above-mentioned carbon fiber/nano-copper/epoxy resin composite material preparation method, the step (4)
In, the preparation method of nano-copper/epoxy resin composite material includes:
(1), epoxy resin and curing agent are mixed 30~80 minutes at 40 DEG C~60 DEG C；
(2), nano copper particle is prepared:
Step 1: preparing CuSO4Aqueous solution；
Step 2: to CuSO4Polyvinylpyrrolidone is added in aqueous solution, ultrasonic 30min~50min obtains polyethylene
Than pyrrolidone/CuSO4Mixed aqueous solution；
Step 3: at room temperature mixing hydrazine hydrate with distilled water, hydrazine hydrate solution is obtained；
Step 4: preparing NaOH solution；
Step 5: by polyvinylpyrrolidone/CuSO4Mixed aqueous solution, hydrazine hydrate solution and NaOH solution mixing,
Temperature be 65 DEG C~75 DEG C and revolving speed be 250r/min~350r/min under conditions of stir 20min~25min, then using steaming
Distilled water filtering and washing 2h~3h, then be 0.08MPa~0.09MPa in vacuum degree and be dried in vacuo 2h~4h under room temperature, it obtains
To nano copper particle；
(3), nano copper particle and diluent are added in the mixture of epoxy resin and curing agent, it is ultrasonic at 50 DEG C
The mass ratio of dispersion 10 minutes, the epoxy resin and nano copper particle is 1:(0.5~0.8)；
(4), under vacuum condition, 60 DEG C~70 DEG C is heated to and is stirred simultaneously vacuum defoamation 6~8 hours, target is obtained and produces
Product.
Preferably, in above-mentioned carbon fiber/nano-copper/epoxy resin composite material preparation method, the asphalt mixtures modified by epoxy resin
Rouge is one of glycidyl ether type epoxy resin, glycidyl ester epoxy resin and linear aliphatic epoxy resin
Or several mixture.
Preferably, in above-mentioned carbon fiber/nano-copper/epoxy resin composite material preparation method, the curing agent
For polyamide.
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, carbon fiber/nano-copper/epoxy resin composite material preparation method, comprising:
(1), the preparation of carbon fiber, comprising: the PVP of the PAN of 8.9%wt and 1%wt is mixed, the DMF of 90%wt is added,
3 hours of magnetic agitation, clear solution is obtained, add ‰ nickel acetate of 1wt, stirring is until form the spinning forerunner of green transparent
Liquid solution, precursor solution obtain PAN/PVP/ nickel acetate composite nano fiber, PAN/PVP/ acetic acid by electrostatic spinning technique
Nickel composite nano 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,
The PVP of 2 times of PAN/PVP/ nickel acetate composite nano fiber quality is put into boiler tube, under an argon atmosphere, 900 DEG C of heat treatments 120
Minute, obtain carbon nanotube/nickel carbon fiber composite carbon material of hierarchical structure, carbon nanotube/nickel carbon fiber of hierarchical structure
Complex carbon material reacts 30 minutes with potassium hydroxide under 250 degree, then is warming up to 750 degree of 1 hours of reaction, reacts in argon gas gas
Under atmosphere, heating rate is 5 DEG C/min, and carbon nanotube/nickel carbon fiber composite carbon material of the hierarchical structure after being activated is living
The carbon nanotube of hierarchical structure after change/nickel carbon fiber composite carbon material is put into the nitric acid solution of 7M, is removed nickel, is obtained
Carbon pipe/carbon fiber complex carbon material of hierarchical structure；
(2), the surface treatment of carbon fiber: carbon fiber is put into 68% concentrated nitric acid to aoxidize 3 hours and is taken out, with distillation
Water repeated flushing；
(3), the carbon fiber of surface treatment is dried in vacuo；
(4), nano-copper/epoxy resin composite material is prepared, comprising steps of
A, epoxy resin and curing agent are mixed 30 minutes at 40 DEG C；
B, nano copper particle is prepared:
Step 1: preparing CuSO4Aqueous solution；
Step 2: to CuSO4Polyvinylpyrrolidone is added in aqueous solution, ultrasonic 30min~50min obtains polyethylene
Than pyrrolidone/CuSO4Mixed aqueous solution；
Step 3: at room temperature mixing hydrazine hydrate with distilled water, hydrazine hydrate solution is obtained；
Step 4: preparing NaOH solution；
Step 5: by polyvinylpyrrolidone/CuSO4Mixed aqueous solution, hydrazine hydrate solution and NaOH solution mixing,
Temperature be 65 DEG C DEG C and revolving speed be 250r/min under conditions of stir 20min, then use distilled water filtering and washing 3h, then true
Reciprocal of duty cycle is 0.08MPa and is dried in vacuo 4h under room temperature, obtains nano copper particle；
C, nano copper particle and diluent are added in the mixture of epoxy resin and curing agent, the ultrasound point at 50 DEG C
It dissipates 10 minutes, the mass ratio of the epoxy resin and nano copper particle is 1:0.5；
D, under vacuum condition, 60 DEG C is heated to and is stirred simultaneously vacuum defoamation 6 hours, target product is obtained.
(5), carbon fiber, nano-copper/epoxy resin composite material and diluent are mixed and is fully ground；
(6), acetone is added at 50 DEG C to carry out ultrasonic disperse 15 minutes；
(7), under vacuum condition, 50 DEG C is heated to and is stirred simultaneously vacuum defoamation 6 hours, target product is obtained.
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 (4)
1. a kind of preparation method of carbon fiber/nano-copper/epoxy resin composite material characterized by comprising
(1), the PVP of the PAN of 8.9%wt and 1%wt is mixed, the DMF of 90%wt, magnetic agitation 3 is added by the preparation of carbon fiber
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), nano-copper/epoxy resin composite material is prepared；
(5), carbon fiber, nano-copper/epoxy resin composite material and diluent are mixed and is fully ground；
(6), acetone is added at 40~50 DEG C to carry out ultrasonic disperse 15~20 minutes；
(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/nano-copper/epoxy resin composite material according to claim 1, it is characterised in that:
In the step (4), the preparation method of nano-copper/epoxy resin composite material includes:
(1), epoxy resin and curing agent are mixed 30~80 minutes at 40 DEG C~60 DEG C；
(2), nano copper particle is prepared:
Step 1: preparing CuSO4Aqueous solution；
Step 2: to CuSO4Polyvinylpyrrolidone is added in aqueous solution, ultrasonic 30min~50min obtains polyvinyl pyrrole
Alkanone/CuSO4Mixed aqueous solution；
Step 3: at room temperature mixing hydrazine hydrate with distilled water, hydrazine hydrate solution is obtained；
Step 4: preparing NaOH solution；
Step 5: by polyvinylpyrrolidone/CuSO4Mixed aqueous solution, hydrazine hydrate solution and NaOH solution mixing, in temperature
20min~25min is stirred under conditions of being 250r/min~350r/min for 65 DEG C~75 DEG C and revolving speed, then uses distilled water
Filtering and washing 2h~3h, then be 0.08MPa~0.09MPa in vacuum degree and be dried in vacuo 2h~4h under room temperature, it is received
Rice copper particle；
(3), nano copper particle and diluent are added in the mixture of epoxy resin and curing agent, the ultrasonic disperse at 50 DEG C
10 minutes, the mass ratio of the epoxy resin and nano copper particle was 1:(0.5~0.8)；
(4), under vacuum condition, 60 DEG C~70 DEG C is heated to and is stirred simultaneously vacuum defoamation 6~8 hours, target product is obtained.
3. the preparation method of carbon fiber/nano-copper/epoxy resin composite material according to claim 2, it is characterised in that:
The epoxy resin is glycidyl ether type epoxy resin, glycidyl ester epoxy resin and linear aliphatic class asphalt mixtures modified by epoxy resin
The mixture of one or more of rouge.
4. the preparation method of carbon fiber/nano-copper/epoxy resin composite material according to claim 2, it is characterised in that:
The curing agent is polyamide.
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| CN107685151A (en) * | 2017-08-28 | 2018-02-13 | 江西赣大材料技术研究有限公司 | A kind of preparation method of the compound antibacterial solid sols of nanometer of copper epoxy |
| CN107964118B (en) * | 2017-12-17 | 2019-05-21 | 王南南 | A kind of preparation method of epoxy resin composite conducting material special-purpose nanometer carbon fiber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033379A (en) * | 2006-03-10 | 2007-09-12 | 国家淀粉及化学投资控股公司 | Anisotropic conductive adhesive |
| CN103396576A (en) * | 2006-08-07 | 2013-11-20 | 东丽株式会社 | Prepreg and carbon fiber-reinforced composite material |
| CN104625085A (en) * | 2015-01-23 | 2015-05-20 | 中国矿业大学 | Method for simply and stably preparing micro-nano hollow copper |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033379A (en) * | 2006-03-10 | 2007-09-12 | 国家淀粉及化学投资控股公司 | Anisotropic conductive adhesive |
| CN103396576A (en) * | 2006-08-07 | 2013-11-20 | 东丽株式会社 | Prepreg and carbon fiber-reinforced composite material |
| CN104625085A (en) * | 2015-01-23 | 2015-05-20 | 中国矿业大学 | Method for simply and stably preparing micro-nano hollow copper |
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