CN106589807A - Preparation method of carbon fiber/nano-copper/epoxy resin composite material - Google Patents
Preparation method of carbon fiber/nano-copper/epoxy resin composite material Download PDFInfo
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- CN106589807A CN106589807A CN201510680390.6A CN201510680390A CN106589807A CN 106589807 A CN106589807 A CN 106589807A CN 201510680390 A CN201510680390 A CN 201510680390A CN 106589807 A CN106589807 A CN 106589807A
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Abstract
The invention discloses a preparation method of a carbon fiber/nano-copper/epoxy resin composite material. The preparation method comprises steps as follows: (1), carbon fibers are prepared; (2), surface treatment of the carbon fibers is performed and comprises following steps: the carbon fibers are placed in concentrated nitric acid with the concentration being 65%-68% and oxidized for 3-5 h, and then the carbon fibers are taken out and repeatedly washed with distilled water; (3), the carbon fibers after the surface treatment are subjected to vacuum drying; (4), a nano-copper/epoxy resin composite material is prepared; (5), the carbon fibers, the nano-copper/epoxy resin composite material and a diluent are mixed and sufficiently ground; (6), acetone is added at the temperature of 40-50 DEG C, and a mixture is subjected to ultrasonic dispersion for 15-20 min; (7), under the vacuum condition, the mixture is heated to 50-70 DEG C, stirred and subjected to vacuum defoaming for 6-8 h, and a target product is obtained. According to the technical scheme, raw materials of the carbon fibers have abundant sources, the preparation cost is low, and the obtained composite material is lighter, has the characteristics of high strength, high temperature resistance and high thermal conductivity and can be applied to the field of aviation and space.
Description
Technical field
The application belongs to technical field of electronic devices, more particularly to a kind of carbon fiber/Nanometer Copper/epoxy resin
The preparation method of composite, for the radiating of electronic device.
Background technology
Electronic equipment and the interracial contact that the connection procedure of heat dissipation equipment is solid and solid, realize that contact is changed
Heat is the approach of many electronic radiations.
Rough two surfaces contact on microcosmic not enough completely, causes contact surface to produce contact resistance, deposits
It is that air between uneven gap has very big impact to the conducting power for radiating, because air is
The non-conductor of heat.And in two surfaces of solids these spaces cannot also eliminated even with larger pressure,
And some electronic devices and components cannot bear larger pressure, so will result in bigger gap, also will
It is serious to hinder the heat of electronic devices and components to be conducted to fin.
The content of the invention
It is an object of the invention to provide a kind of preparation side of carbon fiber/nano-copper/epoxy resin composite material
Method, to overcome deficiency of the prior art.
For achieving the above object, the present invention provides following technical scheme：
The embodiment of the present application discloses a kind of preparation method of carbon fiber/nano-copper/epoxy resin composite material, bag
Include：
(1), the preparation of carbon fiber；
(2), the surface treatment of carbon fiber：Carbon fiber is put in 65～68% red fuming nitric acid (RFNA) and aoxidize 3～5
Hour is taken out, and is rinsed repeatedly with distilled water；
(3), the carbon fiber to being surface-treated is vacuum dried；
(4), nano-copper/epoxy resin composite material is prepared；
(5), the mixing of carbon fiber, nano-copper/epoxy resin composite material and diluent is fully ground；
(6), acetone is added to carry out ultrasonic disperse 15～20 minutes at 40～50 DEG C；
(7), under vacuum condition, 50～70 DEG C are heated to and are stirred simultaneously vacuum defoamation 6～8 hours, obtained
Target product.
Preferably, it is described in the preparation method of above-mentioned carbon fiber/nano-copper/epoxy resin composite material
In step (1), the preparation method of carbon fiber includes：By the PVP of the PAN of 8.9%wt and 1%wt
Mixing, adds the DMF of 90%wt, 3 hours of magnetic agitation to obtain clear solution, add 1wt ‰
Nickel acetate, stirring is until form the spinning precursor solution of green transparent, precursor solution passes through Static Spinning
Silk technology, obtains PAN/PVP/ nickel acetate composite nano fibers, PAN/PVP/ nickel acetate composite nano fibers
2h is heat-treated under 275 DEG C of air atmospheres, heating rate is 1 DEG C/min, in being subsequently transferred to tube furnace,
The PVP of 2 times of PAN/PVP/ nickel acetate composite nano fiber quality is put in boiler tube, under an argon atmosphere,
900 DEG C are heat-treated 120 minutes, obtain the CNT/nickel carbon fiber composite material with carbon element of hierarchy, point
The CNT of level structure/nickel carbon fiber composite material with carbon element reacts 30 minutes with potassium hydroxide under 250 degree,
750 degree of reactions, 1 hour is warmed up to again, and under an argon atmosphere, heating rate is 5 DEG C/min, is obtained for reaction
The CNT of the hierarchy to after activation/nickel carbon fiber composite material with carbon element, the hierarchy after activation
CNT/nickel carbon fiber composite material with carbon element is put in the salpeter solution of 7M, removes nickel, is classified
Carbon pipe/carbon fiber the complex carbon material of structure.
Preferably, it is described in the preparation method of above-mentioned carbon fiber/nano-copper/epoxy resin composite material
In 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 one, preparation CuSO4The aqueous solution；
Step 2, to CuSO4Add PVP in the aqueous solution, ultrasonic 30min～50min,
Obtain PVP/CuSO4Mixed aqueous solution；
Hydrazine hydrate is mixed with distilled water under step 3, room temperature, obtains hydrazine hydrate solution；
Step 4, preparation NaOH solution；
Step 5, by PVP/CuSO4Mixed aqueous solution, hydrazine hydrate solution and NaOH are molten
Liquid mixes, and stirs under conditions of temperature is 65 DEG C～75 DEG C and rotating speed is 250r/min～350r/min
20min～25min, then using distilled water filtering and washing 2h～3h, then vacuum be 0.08MPa～
2h～4h is vacuum dried under 0.09MPa and room temperature condition, nano copper particle is obtained；
(3), nano copper particle and diluent are added in the mixture of epoxy resin and curing agent,
Ultrasonic disperse 10 minutes at 50 DEG C, the epoxy resin is 1 with the mass ratio of nano copper particle:(0.5～0.8)；
(4), under vacuum condition, 60 DEG C～70 DEG C are heated to and are stirred simultaneously vacuum defoamation 6～8 hours, obtained
Obtain target product.
Preferably, it is described in the preparation method of above-mentioned carbon fiber/nano-copper/epoxy resin composite material
Epoxy resin is glycidyl ether type epoxy resin, glycidyl ester epoxy resin and linear aliphatic
The mixture of one or more in based epoxy resin.
Preferably, it is described in the preparation method of above-mentioned carbon fiber/nano-copper/epoxy resin composite material
Curing agent is polyamide.
Compared with prior art, it is an advantage of the current invention that：The abundant raw material source of carbon fiber, is prepared into
This is low, and the composite for being obtained is lighter, with high intensity, high temperature resistant, high heat conduction characteristic, can
For field of aerospace.
Specific embodiment
The present invention is described further by the following example：According to following embodiments, can be more preferably geographical
The solution present invention.However, as it will be easily appreciated by one skilled in the art that the specific material described by embodiment
The present invention is merely to illustrate than, process conditions and its result, and should not also without limitation on claims
In the present invention described in detail.
In the present embodiment, the preparation method of carbon fiber/nano-copper/epoxy resin composite material, including：
(1), the preparation of carbon fiber, including：The PVP of the PAN of 8.9%wt and 1%wt is mixed,
The DMF of 90%wt, 3 hours of magnetic agitation is added to obtain clear solution, add the vinegar of 1wt ‰
Sour nickel, stirring is until form the spinning precursor solution of green transparent, precursor solution passes through electrostatic spinning
Technology, obtains PAN/PVP/ nickel acetate composite nano fibers, and PAN/PVP/ nickel acetate composite nano fibers exist
2h is heat-treated under 275 DEG C of air atmospheres, heating rate is 1 DEG C/min, in being subsequently transferred to tube furnace, stove
The PVP of 2 times of PAN/PVP/ nickel acetate composite nano fiber quality is put in pipe, under an argon atmosphere,
900 DEG C are heat-treated 120 minutes, obtain the CNT/nickel carbon fiber composite material with carbon element of hierarchy, point
The CNT of level structure/nickel carbon fiber composite material with carbon element reacts 30 minutes with potassium hydroxide under 250 degree,
750 degree of reactions, 1 hour is warmed up to again, and under an argon atmosphere, heating rate is 5 DEG C/min, is obtained for reaction
The CNT of the hierarchy to after activation/nickel carbon fiber composite material with carbon element, the hierarchy after activation
CNT/nickel carbon fiber composite material with carbon element is put in the salpeter solution of 7M, removes nickel, is classified
Carbon pipe/carbon fiber the complex carbon material of structure；
(2), the surface treatment of carbon fiber：Carbon fiber is put in 68% red fuming nitric acid (RFNA) and aoxidize 3 hours
Take out, rinsed repeatedly with distilled water；
(3), the carbon fiber to being surface-treated is vacuum dried；
(4), nano-copper/epoxy resin composite material is prepared, including step：
A, epoxy resin and curing agent are mixed 30 minutes at 40 DEG C；
B, prepare nano copper particle：
Step one, preparation CuSO4The aqueous solution；
Step 2, to CuSO4Add PVP in the aqueous solution, ultrasonic 30min～50min,
Obtain PVP/CuSO4Mixed aqueous solution；
Hydrazine hydrate is mixed with distilled water under step 3, room temperature, obtains hydrazine hydrate solution；
Step 4, preparation NaOH solution；
Step 5, by PVP/CuSO4Mixed aqueous solution, hydrazine hydrate solution and NaOH are molten
Liquid mixes, and under conditions of temperature is 65 DEG C DEG C and rotating speed is 250r/min 20min is stirred, and then uses
Distilled water filtering and washing 3h, then 4h is vacuum dried in the case where vacuum is 0.08MPa and room temperature condition, obtain
To nano copper particle；
C, nano copper particle and diluent are added in the mixture of epoxy resin and curing agent, at 50 DEG C
Lower ultrasonic disperse 10 minutes, the epoxy resin is 1 with the mass ratio of nano copper particle:0.5；
Under d, vacuum condition, it is heated to 60 DEG C and is stirred simultaneously vacuum defoamation 6 hours, obtains target product.
(5), the mixing of carbon fiber, nano-copper/epoxy resin composite material and diluent is fully ground；
(6), acetone is added to carry out ultrasonic disperse 15 minutes at 50 DEG C；
(7), under vacuum condition, 50 DEG C are heated to and are stirred simultaneously vacuum defoamation 6 hours, obtain target
Product.
Finally, in addition it is also necessary to explanation, term " including ", "comprising" or its any other variant meaning
Covering including for nonexcludability so that process, method, article including a series of key elements or
Equipment not only includes those key elements, but also including other key elements being not expressly set out, or also wrap
Include the key element intrinsic for this process, method, article or equipment.
Claims (5)
1. a kind of preparation method of carbon fiber/nano-copper/epoxy resin composite material, it is characterised in that bag
Include：
(1), the preparation of carbon fiber；
(2), the surface treatment of carbon fiber：Carbon fiber is put in 65～68% red fuming nitric acid (RFNA) and aoxidize 3～5
Hour is taken out, and is rinsed repeatedly with distilled water；
(3), the carbon fiber to being surface-treated is vacuum dried；
(4), nano-copper/epoxy resin composite material is prepared；
(5), the mixing of carbon fiber, nano-copper/epoxy resin composite material and diluent is fully ground；
(6), acetone is added to carry out ultrasonic disperse 15～20 minutes at 40～50 DEG C；
(7), under vacuum condition, 50～70 DEG C are heated to and are stirred simultaneously vacuum defoamation 6～8 hours, obtained
Target product.
2. the preparation method of carbon fiber/nano-copper/epoxy resin composite material according to claim 1,
It is characterized in that：In the step (1), the preparation method of carbon fiber includes：By the PAN of 8.9%wt
Mix with the PVP of 1%wt, add the DMF of 90%wt, 3 hours of magnetic agitation to obtain
Bright solution, adds the nickel acetates of 1wt ‰, stirs up to the spinning precursor solution for forming green transparent,
Precursor solution obtains PAN/PVP/ nickel acetate composite nano fibers by electrostatic spinning technique,
PAN/PVP/ nickel acetates composite nano fiber is heat-treated 2h under 275 DEG C of air atmospheres, and heating rate is 1 DEG C
/ min, in being subsequently transferred to tube furnace, is put into 2 times of PAN/PVP/ nickel acetate composite nano fibers in boiler tube
The PVP of quality, under an argon atmosphere, 900 DEG C are heat-treated 120 minutes, obtain the carbon nanometer of hierarchy
Pipe/nickel carbon fiber composite material with carbon element, the CNT/nickel carbon fiber composite material with carbon element of hierarchy and hydrogen-oxygen
Change potassium to react 30 minutes under 250 degree, then be warmed up to 750 degree of reactions, 1 hour, react in argon gas gas
Under atmosphere, heating rate is 5 DEG C/min, and the CNT/nickel carbon fiber of the hierarchy after being activated is answered
Material with carbon element is closed, the CNT/nickel carbon fiber composite material with carbon element of the hierarchy after activation puts into 7M's
In salpeter solution, nickel is removed, obtain the carbon pipe/carbon fiber complex carbon material of hierarchy.
3. the preparation method of carbon fiber/nano-copper/epoxy resin composite material according to claim 1,
It is characterized 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 one, preparation CuSO4The aqueous solution；
Step 2, to CuSO4Add PVP in the aqueous solution, ultrasonic 30min～50min,
Obtain PVP/CuSO4Mixed aqueous solution；
Hydrazine hydrate is mixed with distilled water under step 3, room temperature, obtains hydrazine hydrate solution；
Step 4, preparation NaOH solution；
Step 5, by PVP/CuSO4Mixed aqueous solution, hydrazine hydrate solution and NaOH are molten
Liquid mixes, and stirs under conditions of temperature is 65 DEG C～75 DEG C and rotating speed is 250r/min～350r/min
20min～25min, then using distilled water filtering and washing 2h～3h, then vacuum be 0.08MPa～
2h～4h is vacuum dried under 0.09MPa and room temperature condition, nano copper particle is obtained；
(3), nano copper particle and diluent are added in the mixture of epoxy resin and curing agent,
Ultrasonic disperse 10 minutes at 50 DEG C, the epoxy resin is 1 with the mass ratio of nano copper particle:(0.5～0.8)；
(4), under vacuum condition, 60 DEG C～70 DEG C are heated to and are stirred simultaneously vacuum defoamation 6～8 hours, obtained
Obtain target product.
4. the preparation method of carbon fiber/nano-copper/epoxy resin composite material according to claim 3,
It is characterized in that：The epoxy resin is glycidyl ether type epoxy resin, glycidol esters asphalt mixtures modified by epoxy resin
The mixture of one or more in fat and linear aliphatic epoxy resin.
5. the preparation method of carbon fiber/nano-copper/epoxy resin composite material according to claim 3,
It is characterized in that：The curing agent is polyamide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107964118A (en) * | 2017-12-17 | 2018-04-27 | 李巧珍 | 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 |
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| 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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2015
- 2015-10-19 CN CN201510680390.6A patent/CN106589807B/en active Active
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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107964118A (en) * | 2017-12-17 | 2018-04-27 | 李巧珍 | A kind of preparation method of epoxy resin composite conducting material special-purpose nanometer carbon fiber |
| 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 |
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