CN107553996A - A kind of heat-conductive composite material of multilayer fibre reinforced and preparation method thereof - Google Patents
A kind of heat-conductive composite material of multilayer fibre reinforced and preparation method thereof Download PDFInfo
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- CN107553996A CN107553996A CN201610517225.3A CN201610517225A CN107553996A CN 107553996 A CN107553996 A CN 107553996A CN 201610517225 A CN201610517225 A CN 201610517225A CN 107553996 A CN107553996 A CN 107553996A
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- 239000000463 material Substances 0.000 claims description 5
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
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- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of heat-conductive composite material of multilayer fibre reinforced and preparation method thereof, the heat-conductive composite material of the multilayer fibre reinforced is made up of semi-solid preparation thermal conductive adhesive composition and multilayer carbon fibre reinforcement, the number of plies of multilayer carbon fiber is more than 2 layers, semi-solid preparation thermal conductive adhesive composition is by epoxy resin, curing agent, heat filling, anti-current glue filler and dispersant composition, the mass ratio of epoxy resin and curing agent is 100: 10~100, the mass fraction of heat filling is 10~50, the mass fraction of anti-current glue filler is 10~30, the mass fraction of dispersant is 1~5.The heat-conductive composite material of the present invention uses multilayer carbon fibre reinforced cloth, in addition to as forming skeleton, also advantageously improves heat conductivility；Natural graphite flakes are aligned, not only increase the thermal conductivity of heat-conductive composite material, while also reduce production cost, of the invention method is simple, is applicable to manufacture on a large scale.
Description
Technical field
The present invention relates to a kind of heat-conductive composite material of multilayer fibre reinforced and preparation method thereof, refer in particular to it is a kind of have lead
Heat-conductive composite material of heat and adhesive property and preparation method thereof.
Background technology
Heat dissipation problem turns into the bottleneck for limiting numerous industry developments.Especially as integrated technology in electronics industry and assembling skill
The continuous renewal development of art, electronic component and electronic equipment small, integrated and densification, working frequency are anxious
Increase severely plus, now heat caused by electronic equipment accumulates rapidly, at a temperature of use environment, for ensure electronic component it is long when
Between high reliability normal work, propose higher and higher requirement for the heat conductivility of adhesive for playing cementation.
Epoxy resin is the macromolecule matrix for being commonly used for heat conduction stick, and it has excellent physical and mechanical properties and caking property
Can, while solidification temperature scope is wide, crosslink density is easily controllable, and solidification process does not produce small molecule by-product, thus shrinkage factor
It is low.But epoxy resin still has its weak point while many excellent properties be present, as thermal conductivity factor is low, only 0.2W/
Mk, heat conductivility is poor, greatly limit its application in high-tech sector.Significantly improve leading for adhesive
Hot, main path is exactly the filling heat conduction component into polymer, and such as patent CN 102719210A, to describe a kind of ultralow temperature exhausted
Edge heat conduction adhesive, heat filling are made up of metal powder and nonmetallic heat conductive powder, and the thermal conductive adhesive thermal conductivity factor of preparation is
Improve, but be no more than 1W/mk, and also add the weight of heat-conducting glue, being not suitable for Aeronautics and Astronautics etc. has special want to weight
The field asked uses.Patent CN201110346213.6 describes a kind of BN as heat filling, the epoxy half of glass-fiber-fabric enhancing
Cured sheets and its manufacture method, thermal conductivity factor can reach 3.5W/mk, be the thermally conductive sheets of individual layer glass-fiber-fabric enhancing, in microwave tube
In use, heat conductivility can't reach requirement on constant power pipe.
The unique sheet crystal structure of natural flake graphite, the characteristics of causing its heat conductivility that anisotropy is presented, i.e.,
High-termal conductivity along graphite flake layer direction and the low heat conductivity perpendicular to graphite flake layer direction.In its face thermal conductivity 140~
500W/mk, and interlayer direction thermal conductivity is only 3~10W/mk or so.
Asphalt base carbon fiber is a kind of using coal asphalt or petroleum asphalt as special type of the phosphorus content made of raw material more than 92%
Fiber, there is the excellent combination property such as high intensity, high-modulus, high heat conduction, corrosion-resistant, can be widely applied to Aero-Space, state
The fields such as anti-, industry.The heat conductivility of asphalt base carbon fiber is very excellent, and thermal conductivity is in 100~1000W/mk, even more
It is high.Japanese Unexamined Patent Publication 2010-53224 data describes one kind fibre reinforced, BN, Al2O3Epoxy half as heat filling is solid
5.0W/mk can be arrived by changing piece and its manufacture method, thermal conductivity factor.
The content of the invention
It is high it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of thermal conductivity factor, while have excellent
The heat-conductive composite material of stick performance, the heat-conductive composite material is by semi-solid preparation thermal conductive adhesive composition and multilayer fibre reinforced
Material forms, and the number of plies of multilayer carbon fiber is more than 2 layers, and semi-solid preparation thermal conductive adhesive composition is by epoxy resin, curing agent, heat conduction
The mass ratio of filler, anti-current glue filler and dispersant composition, epoxy resin and curing agent is 100: 10~100, heat filling
Mass fraction be 10~50, the mass fraction of anti-current glue filler is 10~30, and the mass fraction of dispersant is 1~5.
Described carbon fibre reinforcement is asphalt base carbon fiber, is to spin asphalt or coal tar asphalt through melting
Silk, solidification, carbonization and other processes, finally made of 1600 DEG C~3000 DEG C high-temperature process and graphitization, a diameter of the 5 of carbon fiber
~10um, the length of carbon fiber is 20~25mm.
Described heat filling is natural flake graphite, and thermal conductivity is about 60~220W/mk, material diameter scope is 0.15~
0.55mm。
Described anti-current glue filler is one or both of kaolin and preparing spherical SiO 2 mixture, and particle size range is
1~3um.
Described dispersant is anionic dispersing agents.
Described epoxy resin is in liquid bisphenol A types epoxy resin, solid-state bisphenol A type epoxy resin fat, phenolic resin
One or two mixing, curing agent are the mixing of one or both of organoborane amine, dicyandiamide, modified anhydride.
It is a further object to provide a kind of preparation method of the heat-conductive composite material of multilayer fibre reinforced, bag
Include following steps：
(1) preparation of carbon fibre reinforced cloth：By 80~90g/m2Carbon fiber is weighed, with the multiple washing and filtering of 95% alcohol
And 60 DEG C of drying in vacuum drying chamber, copied with short net tilting wet method and network structure is made, be immersed in water miscible phenolic aldehyde ring
In the binding agent of oxygen tree fat and Polyamine Type curing agent composition, after 120 DEG C predrying, then under 180 DEG C, 10~15MPa pressure
Compacting 5~10 seconds, handled 3 minutes at 150 DEG C afterwards, carbon fibre reinforced cloth is made；
(2) preparation of semi-solid preparation thermal conductive adhesive mixture：Epoxy resin and curing agent are weighed in proportion, after stirring
Heat filling, anti-current jelly and dispersant are added, is again stirring for after being well mixed, carries out vacuum defoamation；
(3) preparation of the heat-conductive composite material of multilayer fibre reinforced：One layer of demoulding is sprayed in the mould bottom surface customized
Agent, the thick semi-solid preparation thermal conductive adhesive mixtures of one layer of 0.1~0.4mm are poured into, with orientation compression roll along parallel to mould base
The direction extruding adhesive mixture at bottom, makes graphite flakes be arranged parallel to the direction of mold base, then after extrusion mixed
Laminate spreads one layer of carbon fibre reinforced cloth prepared, and it is gluing then to pour into the thick semi-solid preparation heat conduction of one layer of 0.1~0.4mm again
Agent composition, the step of repetition above, after the completion of last layer of semi-solid preparation thermal conductive adhesive mixture is suppressed, in 100~180
DEG C dry 2~4 hours, that is, the heat-conductive composite material of multilayer fibre reinforced is made；
(4) cutting and use of heat-conductive composite material：The plane aligned perpendicular to graphite, carried out by the width used
Cutting, the heat-conductive composite material needed is made, in use, being put by graphite flake in heat-conductive composite material perpendicular to the direction of bonding plane
Put among two bonding planes, at 150~210 DEG C, heating 30~120min solidifications.
The excellent effect of the present invention is：
Using multilayer carbon fibre reinforced cloth, in addition to as heat-conductive composite material forming skeleton, can also further improve
Heat conductivility；Natural graphite flakes are aligned, while effectively solving device heat dissipation problem, also reduces and is produced into
This, of the invention method is simple, is applicable to manufacture on a large scale.
Brief description of the drawings：
Fig. 1 is a kind of preparation flow figure of the heat-conductive composite material of multilayer fibre reinforced.
Fig. 2 is a kind of heat-conductive composite material structural representation of multilayer fibre reinforced, wherein 1 is multilayer fibre reinforced
Heat-conductive composite material, 11 be semi-solid preparation thermal conductive adhesive composition, and 12 be carbon fibre reinforced cloth, and 2 be anti-current glue filler, and 3 are
Epoxy resin cure sizing material, 4 be crystalline flake graphite, and 5 be the mould for scribbling remover, and 6 be orientation compression roll.
Fig. 3 is that a kind of heat-conductive composite material of multilayer fibre reinforced uses schematic diagram, wherein 1 is multilayer fibre reinforced
Heat-conductive composite material, 2 for bonding matrix.
Embodiment
Epoxy resin involved in the present invention, curing agent, dispersant are bought from Wuxi Ren Ze chemical products Co., Ltd,
Crystalline flake graphite purchase is limited from the source carbon graphite material of Shenzhen's crystalline substance from Qingdao Jin Tao graphite Co., Ltd, carbon fibre material purchase
Company, anti-current glue filler are bought from Chemical Reagent Co., Ltd., Sinopharm Group.
The invention will be further described with reference to embodiments, but the implementation of the present invention is not limited to this.
Embodiment 1
(1) preparation of carbon fibre reinforced cloth：By 80g/m2Weigh carbon fiber, with the multiple washing and filtering of 95% alcohol and
60 DEG C of drying, are copied with short net tilting wet method and network structure are made, be immersed in water miscible epoxy novolac tree in vacuum drying chamber
In the binding agent of fat and Polyamine Type curing agent composition, after 120 DEG C predrying, then suppressed 10 seconds under 180 DEG C, 10MPa pressure
Clock, handled 3 minutes at 150 DEG C afterwards, carbon fibre reinforced cloth is made；
(2) preparation of semi-solid preparation thermal conductive adhesive mixture：Weigh 40g liquid bisphenols A types epoxy resin and 4g organic borons
Amine hardener, 5g 0.55mm 3 μm of natural flake graphite, 5g kaolin and 0.6g dispersants are stirring evenly and then adding into, then
It is secondary be uniformly mixed after, carry out vacuum defoamation；
(3) preparation of the heat-conductive composite material of multilayer fibre reinforced：One layer of demoulding is sprayed in the mould bottom surface customized
Agent, the thick semi-solid preparation thermal conductive adhesive mixtures of one layer of 0.4mm are poured into, adhesive is extruded along the direction parallel to mold base
Mixture, one layer of carbon fibre reinforced cloth prepared is then spread above mixture after extrusion, then pours into one layer of 0.4mm again
Thick semi-solid preparation thermal conductive adhesive mixture, the step of repetition above, in last layer of semi-solid preparation thermal conductive adhesive mixture pressure
After the completion of system, dried in 140 DEG C 3 hours, that is, the heat-conductive composite material of multilayer fibre reinforced is made；
(4) cutting and use of heat-conductive composite material：The plane aligned perpendicular to graphite, carried out by the width used
Cutting, the heat-conductive composite material needed is made, in use, by graphite flake in thermally conductive sheet composite perpendicular to the direction of bonding plane
It is placed among two bonding planes, at 180 DEG C, heating 90min solidifications.
Embodiment 2
(1) preparation of carbon fibre reinforced cloth：By 90g/m2Weigh carbon fiber, with the multiple washing and filtering of 95% alcohol and
60 DEG C of drying, are copied with short net tilting wet method and network structure are made, be immersed in water miscible epoxy novolac tree in vacuum drying chamber
In the binding agent of fat and Polyamine Type curing agent composition, after 120 DEG C predrying, then suppressed 5 seconds under 180 DEG C, 15MPa pressure
Clock, handled 3 minutes at 150 DEG C afterwards, carbon fibre reinforced cloth is made；
(2) preparation of semi-solid preparation thermal conductive adhesive mixture：Weigh 20g liquid bisphenol A types epoxy resin, 20g Solid Doubles
Phenol A types epoxy resin and 40g modified anhydride curing agent, are stirring evenly and then adding into 3 μm of 20g 0.55mm natural flake graphites, 8g
Silica and 2g dispersants, be again stirring for it is well mixed after, carry out vacuum defoamation；
(3) preparation of the heat-conductive composite material of multilayer fibre reinforced：One layer of demoulding is sprayed in the mould bottom surface customized
Agent, the thick semi-solid preparation thermal conductive adhesive mixtures of one layer of 0.3mm are poured into, adhesive is extruded along the direction parallel to mold base
Mixture, one layer of carbon fibre reinforced cloth prepared is then spread above mixture after extrusion, then pours into one layer of 0.3mm again
Thick semi-solid preparation thermal conductive adhesive mixture, the step of repetition above, in last layer of semi-solid preparation thermal conductive adhesive mixture pressure
After the completion of system, dried in 100 DEG C 2 hours, that is, the heat-conductive composite material of multilayer fibre reinforced is made；
(4) cutting and use of heat-conductive composite material：The plane aligned perpendicular to graphite, carried out by the width used
Cutting, the heat-conductive composite material needed is made, in use, being put by graphite flake in heat-conductive composite material perpendicular to the direction of bonding plane
Put among two bonding planes, at 150 DEG C, heating 120min solidifications.
Embodiment 3
(1) preparation of carbon fibre reinforced cloth：By 85g/m2Weigh carbon fiber, with the multiple washing and filtering of 95% alcohol and
60 DEG C of drying, are copied with short net tilting wet method and network structure are made, be immersed in water miscible epoxy novolac tree in vacuum drying chamber
In the binding agent of fat and Polyamine Type curing agent composition, after 120 DEG C predrying, then suppressed 8 seconds under 180 DEG C, 12MPa pressure
Clock, handled 3 minutes at 150 DEG C afterwards, carbon fibre reinforced cloth is made；
(2) preparation of semi-solid preparation thermal conductive adhesive mixture：Weigh 30g liquid bisphenol A types epoxy resin, 10g phenolic aldehyde rings
Oxygen tree fat and 4g dicy-curing agents, be stirring evenly and then adding into 10g 0.15mm natural flake graphites, 1 μm of 4g kaolin and
1g dispersants, it is again stirring for after being well mixed, carries out vacuum defoamation；
(3) preparation of the heat-conductive composite material of multilayer fibre reinforced：One layer of demoulding is sprayed in the mould bottom surface customized
Agent, the thick semi-solid preparation thermal conductive adhesive mixtures of one layer of 0.1mm are poured into, adhesive is extruded along the direction parallel to mold base
Mixture, one layer of carbon fibre reinforced cloth prepared is then spread above mixture after extrusion, then pours into one layer of 0.1mm again
Thick semi-solid preparation thermal conductive adhesive mixture, the step of repetition above, in last layer of semi-solid preparation thermal conductive adhesive mixture pressure
After the completion of system, dried in 180 DEG C 4 hours, that is, the heat-conductive composite material of multilayer fibre reinforced is made；
(4) cutting and use of heat-conductive composite material：The plane aligned perpendicular to graphite, carried out by the width used
Cutting, the heat-conductive composite material needed is made, in use, being put by graphite flake in heat-conductive composite material perpendicular to the direction of bonding plane
Put among two bonding planes, at 210 DEG C, heating 30min solidifications.
Embodiment 4
(1) preparation of carbon fibre reinforced cloth：By 80g/m2Weigh carbon fiber, with the multiple washing and filtering of 95% alcohol and
60 DEG C of drying, are copied with short net tilting wet method and network structure are made, be immersed in water miscible epoxy novolac tree in vacuum drying chamber
In the binding agent of fat and Polyamine Type curing agent composition, after 120 DEG C predrying, then suppressed 10 seconds under 180 DEG C, 15MPa pressure
Clock, handled 3 minutes at 150 DEG C afterwards, carbon fibre reinforced cloth is made；
(2) preparation of semi-solid preparation thermal conductive adhesive mixture：Weigh 30g liquid bisphenol A types epoxy resin, 10g Solid Doubles
Phenol A types epoxy resin and 20g modified anhydrides, 3g dicy-curing agents, it is stirring evenly and then adding into the natural scale stones of 15g 0.25mm
Ink, 12g1 μm of silica and 0.4g dispersants, it is again stirring for after being well mixed, carries out vacuum defoamation；
(3) preparation of the heat-conductive composite material of multilayer fibre reinforced：One layer of demoulding is sprayed in the mould bottom surface customized
Agent, the thick semi-solid preparation thermal conductive adhesive mixtures of one layer of 0.2mm are poured into, adhesive is extruded along the direction parallel to mold base
Mixture, one layer of carbon fibre reinforced cloth prepared is then spread above mixture after extrusion, then pours into one layer of 0.2mm again
Thick semi-solid preparation thermal conductive adhesive mixture, the step of repetition above, in last layer of semi-solid preparation thermal conductive adhesive mixture pressure
After the completion of system, dried in 150 DEG C 2 hours, that is, the heat-conductive composite material of multilayer fibre reinforced is made；
(4) cutting and use of heat-conductive composite material：The plane aligned perpendicular to graphite, carried out by the width used
Cutting, the heat-conductive composite material needed is made, in use, being put by graphite flake in heat-conductive composite material perpendicular to the direction of bonding plane
Put among two bonding planes, at 180 DEG C, heating 60min solidifications.
Embodiment 5
(1) preparation of carbon fibre reinforced cloth：By 88g/m2Weigh carbon fiber, with the multiple washing and filtering of 95% alcohol and
60 DEG C of drying, are copied with short net tilting wet method and network structure are made, be immersed in water miscible epoxy novolac tree in vacuum drying chamber
In the binding agent of fat and Polyamine Type curing agent composition, after 120 DEG C predrying, then suppressed 6 seconds under 180 DEG C, 13MPa pressure
Clock, handled 3 minutes at 150 DEG C afterwards, carbon fibre reinforced cloth is made；
(2) preparation of semi-solid preparation thermal conductive adhesive mixture：Weigh 20g liquid bisphenol A types epoxy resin, 20g phenolic aldehyde rings
Oxygen tree fat and 3g organoborane amines, 2g dicyandiamide agents, it is stirring evenly and then adding into 10g 0.40mm natural flake graphites, 2 μm of 8g
Silica and 0.4g dispersants, it is again stirring for after being well mixed, carries out vacuum defoamation；
(3) preparation of the heat-conductive composite material of multilayer fibre reinforced：One layer of demoulding is sprayed in the mould bottom surface customized
Agent, the thick semi-solid preparation thermal conductive adhesive mixtures of one layer of 0.3mm are poured into, adhesive is extruded along the direction parallel to mold base
Mixture, one layer of carbon fibre reinforced cloth prepared is then spread above mixture after extrusion, then pours into one layer of 0.3mm again
Thick semi-solid preparation thermal conductive adhesive mixture, the step of repetition above, in last layer of semi-solid preparation thermal conductive adhesive mixture pressure
After the completion of system, dried in 170 DEG C 3 hours, that is, the heat-conductive composite material of multilayer fibre reinforced is made；
(4) cutting and use of heat-conductive composite material：The plane aligned perpendicular to graphite, carried out by the width used
Cutting, the heat-conductive composite material needed is made, in use, being put by graphite flake in heat-conductive composite material perpendicular to the direction of bonding plane
Put among two bonding planes, at 200 DEG C, heating 60min solidifications.
Claims (7)
1. a kind of heat-conductive composite material of multilayer fibre reinforced, it is characterised in that described heat-conductive composite material is by semi-solid preparation
Thermal conductive adhesive composition and multilayer carbon fibre reinforcement composition, the number of plies of multilayer carbon fiber are more than 2 layers, semi-solid preparation heat-conducting glue
Adhesive composition is made up of epoxy resin, curing agent, heat filling, anti-current glue filler and dispersant, epoxy resin and solidification
The mass ratio of agent is 100: 10~100, and the mass fraction of heat filling is 10~50, the mass fraction of anti-current glue filler for 10~
30, the mass fraction of dispersant is 1~5.
A kind of 2. heat-conductive composite material of multilayer fibre reinforced according to claim 1, it is characterised in that described carbon
Fibre reinforced materials is asphalt base carbon fiber, is through works such as melt spinning, solidification, carbonizations by asphalt or coal tar asphalt
Sequence, finally made of 1600 DEG C~3000 DEG C high-temperature process and graphitization, a diameter of 5~10um of carbon fiber, carbon fiber
Length is 20~25mm.
3. the heat-conductive composite material of a kind of multilayer fibre reinforced according to claim 1, it is characterised in that described leads
Hot filler is natural flake graphite, and thermal conductivity is about 60~220W/mk, and particle size range is 0.15~0.55mm.
4. the heat-conductive composite material of a kind of multilayer fibre reinforced according to claim 1, it is characterised in that described is anti-
Gummosis filler is one or both of kaolin and preparing spherical SiO 2 mixture, and particle size range is 1~3um.
A kind of 5. heat-conductive composite material of multilayer fibre reinforced according to claim 1, it is characterised in that described point
Powder is anionic dispersing agents.
A kind of 6. heat-conductive composite material of multilayer fibre reinforced according to claim 1, it is characterised in that described ring
Oxygen tree fat is the mixing of one or both of liquid bisphenol A types epoxy resin, solid-state bisphenol A type epoxy resin fat, phenolic resin, Gu
Agent is the mixing of one or both of organoborane amine, dicyandiamide, modified anhydride.
7. a kind of heat-conductive composite material of multilayer fibre reinforced, it is characterised in that described preparation method is according to the following steps
Carry out：
(1) preparation of carbon fibre reinforced cloth：By 80~90g/m2Weigh carbon fiber, with the multiple washing and filtering of 95% alcohol and
60 DEG C of drying, are copied with short net tilting wet method and network structure are made, be immersed in water miscible epoxy novolac tree in vacuum drying chamber
In the binding agent of fat and Polyamine Type curing agent composition, after 120 DEG C predrying, then 5 are suppressed under 180 DEG C, 10~15MPa pressure
~10 seconds, handled 3 minutes at 150 DEG C afterwards, carbon fibre reinforced cloth is made；
(2) preparation of semi-solid preparation thermal conductive adhesive mixture：Epoxy resin and curing agent are weighed in proportion, are stirring evenly and then adding into
Heat filling, anti-current jelly and dispersant, it is again stirring for after being well mixed, carries out vacuum defoamation；
(3) preparation of the heat-conductive composite material of multilayer fibre reinforced：One layer of releasing agent is sprayed in the mould bottom surface customized, is fallen
Enter the thick semi-solid preparation thermal conductive adhesive mixture of one layer of 0.1~0.4mm, with orientation compression roll along the side parallel to mold base
To extruding adhesive mixture, graphite flakes are made to be arranged parallel to the direction of mold base, then on mixture after extrusion
Face spreads one layer of carbon fibre reinforced cloth prepared, then pours into the thick semi-solid preparation thermal conductive adhesive mixing of one layer of 0.1~0.4mm again
Thing, the step of repetition above, after the completion of last layer of semi-solid preparation thermal conductive adhesive mixture is suppressed, dry 2 in 100~180 DEG C
~4 hours, that is, the heat-conductive composite material of multilayer fibre reinforced is made.
(4) cutting and use of heat-conductive composite material：The plane aligned perpendicular to graphite, is cut by the width used
Cut, the heat-conductive composite material needed is made, in use, being placed by graphite flake in heat-conductive composite material perpendicular to the direction of bonding plane
Among two bonding planes, at 150~210 DEG C, heating 30~120min solidifications.
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| CN115416376A (en) * | 2022-09-29 | 2022-12-02 | 上海昌海船舶技术有限公司 | High-temperature-resistant high-strength heat-insulating cushion block and preparation method thereof |
| CN117135871A (en) * | 2023-01-30 | 2023-11-28 | 荣耀终端有限公司 | Composite material part, processing method thereof, part and electronic equipment |
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