CN109651810A - A kind of poly heat-conductive composite material and preparation method thereof - Google Patents
A kind of poly heat-conductive composite material and preparation method thereof Download PDFInfo
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- CN109651810A CN109651810A CN201811583087.4A CN201811583087A CN109651810A CN 109651810 A CN109651810 A CN 109651810A CN 201811583087 A CN201811583087 A CN 201811583087A CN 109651810 A CN109651810 A CN 109651810A
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Abstract
The present invention relates to a kind of poly heat-conductive composite materials and preparation method thereof, the composite material is using poly as matrix, with the redox graphene (frGO) of surface functionalization and multi-walled carbon nanotube (MWCNTs) for heat filling.Preparation method includes: that above-mentioned carbon material is dispersed in polymer solution to obtain compound poly solution, and then solution is coated on substrate, after solvent volatilization completely to obtain the final product.The present invention has high temperature resistant, and high-intensitive and good heating conduction is suitable for the fields such as Electronic Packaging, hot industry heat dissipation equipment, circuit board, has wide practical prospect.
Description
Technical field
The invention belongs to Heat Conduction Material field, in particular to a kind of poly heat-conductive composite material and
Preparation method.
Background technique
Thermal-conductive polymer matrix composites have been widely used at present aerospace, electronic and electrical industry, industrial equipment,
The fields such as heat dissipation product.Currently, 95% or more electronic package substrate, cooling fin are thermal-conductive polymer matrix composites.And
With the development of electronics technology, high power, highly integrated electronic device can generate more heats, if these heats cannot
It removes, the performance of component will be impacted in time, or even failure.But traditional thermal-conductive polymer matrix composites are such as poly-
Propylene (PP), epoxy resin, polymethyl methacrylate (PMMA) etc., since its working limit temperature is low, under higher temperature just
It is bad to will appear dimensional stability, physical and chemical performance declines phenomenon, is not able to satisfy high power, highly integrated electronic component pair increasingly
The requirement of radiating condition.Therefore, exploitation heat-resistant polymer base heat-conductive composite material is the weight that Heat Conduction Material develops at present
Want direction.
Due to the structural particularity of high molecular material, thermal coefficient is generally all very low, between 0.1~0.4W/mK.It is general
And practical method is that heat filling is added in polymeric matrix, prepares thermal-conductive polymer matrix composites.Patent
Boron nitride nanometer disk is added in poly-vinyl alcohol solution by CN106009445B, and the thermally conductive composite wood of polyvinyl alcohol has been prepared
Material, but the heat resistance of this material is lower.Before patent CN104592950B is by preparing graphene and polymer composites
Body is driven, and the composite material heating conduction for the preparation that is carbonized, is graphitized to it improves obviously, but the mechanical property of material is serious
Decline.
Therefore, a kind of new there is still a need for developing to solve heat dissipation problem under high power, highly integrated electrical hot conditions
Heat-conductive composite material.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of poly heat-conductive composite material and
Preparation method, the material have many advantages, such as high temperature resistant, high intensity, high thermal conductivity, easily molded processing, can will be highly integrated, high
The amount of heat that electronic components of high power generates removes, and maintains good dimensional stability, and physical and chemical performance is not in
It is decreased obviously, there is very wide, practical prospect.
The present invention provides a kind of poly heat-conductive composite materials, and the composite material is with poly- isophthalic
Two formyl m-phenylene diamine (MPD)s are matrix, are to lead with the redox graphene frGO of surface functionalization and multi-walled carbon nanotube MWCNTs
Hot filler.
The poly is copolymerized by phenyl-diformyl with m-phenylene diamine (MPD).
The redox graphene frGO of the surface functionalization is and right by surface of graphene oxide Grafted oligomers
Graphene oxide is restored and is obtained.
The oligomer is obtained by the gavaculine polycondensation of purity > 99%.
The reduction is using ethylenediamine, hydrazine hydrate or vitamin C reduction, preferably hydrazine hydrate.
In the composite material mass fraction of poly be 95~99.5wt%, frGO with
The total mass fraction of MWCNTs is 0.5~5wt%.
The mass ratio of the frGO and MWCNTs is 2:1~10:1.
The poly heat-conductive composite material with a thickness of 20~100 μm.
The present invention also provides a kind of preparation methods of poly heat-conductive composite material, comprising:
The redox graphene frGO of surface functionalization and multi-walled carbon nanotube MWCNTs is added to phenyl-diformyl between gathering
In m-phenylenediamine solution, at a temperature of 80~120 DEG C stir 12~for 24 hours, obtain poly composite solution；It will
Obtained composite solution salivation is coated on substrate, is completely dried to obtain poly heat-conductive composite material.
The frGO and MWCNTs 3~6h of ultrasonic disperse, preferably 5h in a solvent in advance.
The solvent that the composite solution uses is selected from DMAC N,N' dimethyl acetamide, N,N-dimethylformamide, N- methyl pyrrole
One or more of pyrrolidone, preferably n,N-dimethylacetamide.
The solid content of the poly is 12~16wt%, preferably 14wt%.
The drying temperature be 80~120 DEG C, drying time be 12~for 24 hours.
The present invention obtains the reduction-oxidation graphite of surface functionalization by preparing graphene oxide, and by certain method
Alkene then utilizes " π-is pi-conjugated " effect, by multi-walled carbon nanotube " fixation " on the redox graphene of surface functionalization,
Obtain composite heat-conducting particle.It then adds it in poly matrix, between being gathered after coating is dry
Phenyl-diformyl m-phenylene diamine (MPD) base heat-conductive composite material.
Beneficial effect
The present invention passes through the poly- isophthalic two that is added to the redox graphene of surface functionalization and multi-walled carbon nanotube
Poly heat-conductive composite material is prepared in formyl m-phenylene diamine (MPD) polymeric matrix.Graphene is due to it
High high fever thermal coefficient (5000W/mK), can be used as conductive particle and is obviously improved poly base
The heating conduction of body, and carbon nanotube not only excellent thermal conductivity, while its significant draw ratio can be in graphene nanometer sheet
Interlayer plays the role of " thermally conductive bridge ", forms three dimentional heat conduction network in composite system, utilizes redox graphene
The heating conduction of poly composite material is promoted with the synergistic effect of multi-wall carbon tube.
The polymer matrix composite heat conducting material used in the past is compared, the special chemistry knot of poly
Structure imparts its outstanding high temperature resistance, excellent mechanical property, outstanding high temperature dimensional stability；The present invention has preparation
Simple process, physical and chemical performance are excellent, the advantages that can be mass-produced, suitable for high-power, highly integrated electric heat dissipation
In system, it is suitable for the fields such as Electronic Packaging, hot industry heat dissipation equipment, circuit board, there is very wide, practical prospect.
Detailed description of the invention
Fig. 1 is the graphene TEM figure prepared, and wherein a is graphene oxide；B is the reduction-oxidation graphite of surface functionalization
Alkene.
Fig. 2 is that the redox graphene of surface functionalization and the compound particle TEM of multi-wall carbon tube scheme.
Fig. 3 be oligomer polymer, graphene oxide, surface functionalization redox graphene infrared spectrum.
Fig. 4 is the cross section SEM figure of poly heat-conductive composite material of the present invention.
Fig. 5 is the thermally conductive schematic diagram of poly heat-conductive composite material of the present invention.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
1. dispersing 0.4g graphene oxide in 40ml n,N-dimethylacetamide, ultrasonic 3h；
2. 0.685g gavaculine is added in 40ml n,N-dimethylacetamide, reacted under the conditions of 130 DEG C
24h；Then scattered graphene oxide solution is added in above-mentioned solution, the reaction was continued 20h；It is eventually adding 1ml hydration
Hydrazine filters and dry after reacting 4h, obtains functionalized redox graphene.
3. by the functionalized redox graphene of preparation and multi-walled carbon nanotube by the mass ratio of 2:1 in N, N- diformazan
Ultrasonic disperse 3h in yl acetamide is subsequently added in poly slurry, prepared composite solution
Solid content is 12%, and the mass fraction of carbon material (i.e. functionalized redox graphene and multi-walled carbon nanotube) is 0.5%.
4. composite solution is coated on substrate, drying for 24 hours, it is thermally conductive multiple to obtain poly at 80 DEG C
Condensation material.The specimen size of 2mm*2mm is made for thermal coefficient in test surfaces, the specimen size of 5mm*5mm is used for test surfaces
To thermal coefficient.Thermal coefficient in the face of obtained composite material are as follows: 3.17W/mK.
Embodiment 2
1. dispersing 0.4g graphene oxide in 40ml n,N-dimethylacetamide, ultrasonic 3h；
2. 0.685g gavaculine is added in 40ml n,N-dimethylacetamide, reacted under the conditions of 130 DEG C
24h；Then scattered graphene oxide solution is added in above-mentioned solution, the reaction was continued 20h；It is eventually adding 1ml hydration
Hydrazine filters and dry after reacting 4h, obtains functionalized redox graphene.
3. by the functionalized redox graphene of preparation and multi-walled carbon nanotube by the mass ratio of 4:1 in N, N- diformazan
Ultrasonic disperse 6h in yl acetamide is subsequently added in poly slurry, prepared composite solution
Solid content is 14%, and the mass fraction of carbon material (i.e. functionalized redox graphene and multi-walled carbon nanotube) is 1%.
4. composite solution is coated on substrate, dry 16h, it is thermally conductive to obtain poly at 100 DEG C
Composite material.The specimen size of 2mm*2mm is made for thermal coefficient in test surfaces, the specimen size of 5mm*5mm is for testing
Towards thermal coefficient.Thermal coefficient in the face of obtained composite material are as follows: 5.43W/mK.
Embodiment 3
1. dispersing 0.4g graphene oxide in 40ml n,N-dimethylacetamide, ultrasonic 3h；
2. 0.685g gavaculine is added in 40ml n,N-dimethylacetamide, reacted under the conditions of 130 DEG C
24h；Then scattered graphene oxide solution is added in above-mentioned solution, the reaction was continued 20h；It is eventually adding 1ml hydration
Hydrazine filters and dry after reacting 4h, obtains functionalized redox graphene.
3. by the functionalized redox graphene of preparation and multi-walled carbon nanotube by the mass ratio of 6:1 in N, N- diformazan
Ultrasonic disperse 4h in yl acetamide is subsequently added in poly slurry, prepared composite solution
Solid content is 16%, and the mass fraction of carbon material (i.e. functionalized redox graphene and multi-walled carbon nanotube) is 2%.
4. composite solution is coated on substrate, dry 20h, it is thermally conductive multiple to obtain poly at 90 DEG C
Condensation material.The specimen size of 2mm*2mm is made for thermal coefficient in test surfaces, the specimen size of 5mm*5mm is used for test surfaces
To thermal coefficient.Thermal coefficient in the face of obtained composite material are as follows: 6.17W/mK.
Embodiment 4
1. dispersing 0.4g graphene oxide in 40ml n,N-dimethylacetamide, ultrasonic 3h；
2. 0.685g gavaculine is added in 40ml n,N-dimethylacetamide, reacted under the conditions of 130 DEG C
24h；Then scattered graphene oxide solution is added in above-mentioned solution, the reaction was continued 20h；It is eventually adding 1ml hydration
Hydrazine filters and dry after reacting 4h, obtains functionalized redox graphene.
3. by the functionalized redox graphene of preparation and multi-walled carbon nanotube by the mass ratio of 8:1 in N, N- diformazan
Ultrasonic disperse 5h in yl acetamide is subsequently added in poly slurry, prepared composite solution
Solid content is 13%, and the mass fraction of carbon material (i.e. functionalized redox graphene and multi-walled carbon nanotube) is 4%.
4. composite solution is coated on substrate, dry 15h, it is thermally conductive to obtain poly at 110 DEG C
Composite material.The specimen size of 2mm*2mm is made for thermal coefficient in test surfaces, the specimen size of 5mm*5mm is for testing
Towards thermal coefficient.Thermal coefficient in the face of obtained composite material are as follows: 8.18W/mK.
Embodiment 5
1. dispersing 0.4g graphene oxide in 40ml n,N-dimethylacetamide, ultrasonic 3h；
2. 0.685g gavaculine is added in 40ml n,N-dimethylacetamide, reacted under the conditions of 130 DEG C
24h；Then scattered graphene oxide solution is added in above-mentioned solution, the reaction was continued 20h；It is eventually adding 1ml hydration
Hydrazine filters and dry after reacting 4h, obtains functionalized redox graphene.
3. by the functionalized redox graphene of preparation and multi-walled carbon nanotube by the mass ratio of 10:1 in N, N- bis-
Ultrasonic disperse 3h in methylacetamide is subsequently added in poly slurry, prepared composite solution
Solid content be 14%, the mass fraction of carbon material (i.e. functionalized redox graphene and multi-walled carbon nanotube) is 5%.
4. composite solution is coated on substrate, dry 18h, it is thermally conductive to obtain poly at 100 DEG C
Composite material.The specimen size of 2mm*2mm is made for thermal coefficient in test surfaces, the specimen size of 5mm*5mm is for testing
Towards thermal coefficient.Thermal coefficient in the face of obtained composite material are as follows: 8.76W/mK.
As shown in Figure 1, for graphene oxide (Fig. 1 a) after surface grafting restores, surface becomes more coarse (Fig. 1 b),
This is because oligomer causes with surface of graphene oxide functional group reactions.
As shown in Figure 2, due to the pi-conjugated effect of π-, multi-wall carbon tube can be by firmly " fixation " in functionalized oxygen reduction
Graphite alkene surface, will not occur apparent agglomeration.
From the figure 3, it may be seen that occur N-H on functionalized redox graphene (frGO) infrared spectrum, and C=O, the peak C-N,
Show that oligomer is successfully grafted to redox graphene surface.
As shown in Figure 4, FGC-0 section is smooth, and after frGO and MWCNTs is added, FGC-0.5 and FGC-2 section becomes
It obtains coarse；In FGC-0.5 (white arrow MWCNTs, black arrow frGO), MWCNTs is uniformly distributed；It is (white in FGC-2
Line is heat conduction network) in, frGO and MWCNTs form three dimentional heat conduction network, and it is compound to improve poly
The heating conduction of material.
Fig. 5 is pure poly material (left figure) and the thermally conductive composite wood of poly
Expect the thermal conduction mechanism schematic diagram of (right figure).For pure poly, since thermal coefficient itself is low, heat is not
Heat build-up can be conducted and then caused in inside in time；And for poly heat-conductive composite material, frGO
Three dimentional heat conduction network is capable of forming in polymer matrix body with MWCNTs, heat can be transmitted in matrix and be removed in time.
Claims (9)
1. a kind of poly heat-conductive composite material, it is characterised in that: the composite material is with poly- isophthalic two
Formyl m-phenylene diamine (MPD) is matrix, is thermally conductive with the redox graphene frGO of surface functionalization and multi-walled carbon nanotube MWCNTs
Filler.
2. a kind of heat-conductive composite material according to claim 1, it is characterised in that: the reduction-oxidation of the surface functionalization
Graphene frGO restores graphene oxide and is obtained by surface of graphene oxide Grafted oligomers.
3. a kind of heat-conductive composite material according to claim 2, it is characterised in that: the oligomer is by purity >'s 99%
Gavaculine polycondensation obtains.
4. a kind of heat-conductive composite material according to claim 2, it is characterised in that: the reduction is using ethylenediamine, hydration
Hydrazine or vitamin C reduction.
5. a kind of heat-conductive composite material according to claim 1, it is characterised in that: poly- isophthalic diformazan in the composite material
The mass fraction of acyl m-phenylene diamine (MPD) is that the total mass fraction of 95~99.5wt%, frGO and MWCNTs are 0.5~5wt%.
6. a kind of heat-conductive composite material according to claim 1 or 5, it is characterised in that: the matter of the frGO and MWCNTs
Amount is than being 2:1~10:1.
7. a kind of preparation method of poly heat-conductive composite material, comprising:
The redox graphene frGO of surface functionalization and multi-walled carbon nanotube MWCNTs is added to phenyl-diformyl isophthalic between gathering
In diamine solution, at a temperature of 80~120 DEG C stir 12~for 24 hours, obtain poly composite solution；It will obtain
Composite solution salivation be coated on substrate on, be completely dried to obtain poly heat-conductive composite material.
8. a kind of preparation method of heat-conductive composite material according to claim 7, it is characterised in that: the composite solution is adopted
Solvent is selected from one or more of DMAC N,N' dimethyl acetamide, N,N-dimethylformamide, N-Methyl pyrrolidone；It is poly-
The solid content of mpd-i is 12~16wt%.
9. a kind of preparation method of heat-conductive composite material according to claim 7, it is characterised in that: the drying temperature is
80~120 DEG C, drying time be 12~for 24 hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130092234A (en) * | 2012-02-10 | 2013-08-20 | 금오공과대학교 산학협력단 | Aramid composites reinforced with mixed carbon nanomaterials of graphene and carbon nanotube and process for producing the same |
| KR20130100467A (en) * | 2012-03-02 | 2013-09-11 | 이성균 | CNT Graphene Meta Aramid Composition |
| CN108993178A (en) * | 2018-07-27 | 2018-12-14 | 天津工业大学 | A kind of preparation method of high throughput high temperature resistant composite nanometer filtering film |
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2018
- 2018-12-24 CN CN201811583087.4A patent/CN109651810B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130092234A (en) * | 2012-02-10 | 2013-08-20 | 금오공과대학교 산학협력단 | Aramid composites reinforced with mixed carbon nanomaterials of graphene and carbon nanotube and process for producing the same |
| KR20130100467A (en) * | 2012-03-02 | 2013-09-11 | 이성균 | CNT Graphene Meta Aramid Composition |
| CN108993178A (en) * | 2018-07-27 | 2018-12-14 | 天津工业大学 | A kind of preparation method of high throughput high temperature resistant composite nanometer filtering film |
Non-Patent Citations (1)
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| 欧忠星等: ""功能化改性还原氧化石墨烯-碳纳米管/热塑性聚氨酯复合材料膜的制备及性能"", 《复合材料学报》 * |
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