CN107501861A - A kind of composite heat interfacial material based on graphene and preparation method thereof - Google Patents
A kind of composite heat interfacial material based on graphene and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of composite heat interfacial material based on graphene and preparation method thereof, it is related to thermal interfacial material technical field, solve the problems, such as that graphene bad dispersibility in the epoxy and interface resistance are larger, so as to improve the thermal conductivity of epoxy resin-base material, this method improves the dispersity of graphene in the base by carrying out surface modification to graphene oxide；And graphene and nano-Ag particles is can be uniformly dispersed in matrix material using seasoning is stirred under vacuum, solve the reunion settlement issues commonly mixed；Also, molten condition occurs during composite heat cure in nano-Ag particles, connected with this to strengthen between graphene layer, form the Heat transmission approach of 3 D stereo network.The present invention can make graphene oxide fine dispersion be not susceptible to gather in matrix material, while improve the thermal conductivity of epoxy resin-base material.
Description
Technical field
The present invention relates to thermal interfacial material technical field, and in particular to a kind of composite heat interfacial material based on graphene and
Its preparation method.
Background technology
In recent years, electronics industry has obtained rapid development with energy technology, and these development are greatly enhanced diode, crystalline substance
The performance of the electronic device such as body pipe and LED component, is also made that tremendous contribution for energy management.But then, one it is serious
Heat dissipation problem also engender.As in the electronics industry, electronic equipment and device were towards microminaturization, height in the last few years
The direction rapid development of power, High Density Packaging, the heat power consumption that this can certainly increase the inside of electronic equipment and device are close
Degree, causes equipments and devices internal system temperature to steeply rise, and eventually limits the performance of electronic equipment and device and makes
Use the life-span.Obviously, the necessary condition that effective heat management has turned into electronics and energy industry develops.Research is found, with electronics
The gradual microminaturization of device, the interface resistance between solid-solid interface, which has become, restricts the main of dissipation from electronic devices
One of factor, greatly hinder the heat transfer property between solid.To solve the heat transfer problem between solid-solid interface, hot interface material
Material has been widely used for hole, the groove between filling interface between solid-solid interface, builds new heat transmission passage, from
And between solving the problems, such as interface to a certain extent due to incomplete contact between and caused by heat transfer property it is relatively low.At present, in the market
Conventional thermal interfacial material mainly has heat conductive pad, thermally conductive grease, thermally conductive gel etc., and this kind of thermal interfacial material is mostly in asphalt mixtures modified by epoxy resin
Added in the matrix materials such as fat, silicones made of the of a relatively high fillers of thermal conductivity such as aluminium nitride, boron nitride, ceramics, although
The thermal conductivity of matrix material improves after addition packing material, and generally in 0.5~2W/mK, but this numerical value is still
The radiating requirements of electronic equipment can not be met.In addition, the performance of these polymer thermal interface materials can raise with the temperature of thermal source
Severe degradation, the problems such as causing the aging, failure, seepage of boundary material, so as to can further influence electricity are lengthened with the time for exposure
The reliability of sub- equipment and life-span.Therefore, the filler of high heat conductance is added in the matrix materials such as epoxy resin, carrys out hot high fever circle
The overall thermal conductivity of plane materiel material is still current study hotspot problem.
The content of the invention
In view of the shortcomings of the prior art, the technical problem to be solved in the present invention is that how to solve graphene in the epoxy
Bad dispersibility and the problem of larger interface resistance, improve dispersiveness of the graphene in matrix material and strengthen graphene
Interlayer conducts heat, so as to improve the thermal conductivity of epoxy resin-base material.
For above-mentioned technical problem, technical scheme provided by the invention is：A kind of composite heat interfacial material based on graphene
The preparation method of material, comprises the following steps：
Step 1, modified graphene oxide is prepared, it is specifically as follows step by step：
（1）By coupling agent and organic solvent in proportion 1:5 ~ 10 mixings obtain mixed liquor；
（2）Graphene oxide after vacuum drying is added in the mixed liquor and is uniformly mixing to obtain graphene oxide and is mixed
Liquid；
（3）The graphene oxide liquid mixture is heated under vacuo to react to obtain functional graphene oxide feed liquid；
（4）The functional graphene oxide feed liquid through and washing, filter, being dried to obtain modified graphene oxide；
Step 2, the composite heat interfacial material of graphene and epoxy resin is prepared, it is specifically as follows step by step：
（1）Epoxy resin and curing agent are added in organic solvent and mixed and obtains mixed liquor；
（2）The graphene oxide of the modification is added in the mixed liquor, and adds organic solvent diluting agitation grinding and obtains
To graphene oxide liquid mixture；
（3）Ultrasonic disperse is carried out to the graphene oxide liquid mixture；
（4）The graphene oxide liquid mixture after ultrasonic disperse is heated and is slowly stirred under vacuo, vacuum defoamation 5 ~
15min；
Step 3, the composite heat interfacial material based on graphene is prepared, it is specifically as follows step by step：
（1）Dried nano-Ag particles are added to the composite heat interfacial material of the graphene and epoxy resin, and addition has
Solvent agitation grinding obtains mixed liquor；
（2）Ultrasonic disperse is carried out to the mixed liquor；
（3）The mixed liquor after ultrasonic disperse is heated and is slowly stirred under vacuo, 5 ~ 15min of vacuum defoamation；
（4）The mixed liquor after vacuum defoamation is injected into mould, heating is solidified to obtain based on the compound of graphene
Thermal interfacial material.
The organic solvent is acetone, espeleton, ether, expoxy propane, hexamethylene, cyclohexanone, toluene, toluene hexamethylene
At least one of ketone；
The step 1 is step by step（3）The reaction temperature of middle graphene oxide and the mixed liquor is 40-80 DEG C, the reaction time
For 2-12 hours；
The step 1 is step by step（1）With the step 2 step by step（1）Described in mixing temperature be 40
DEG C, it is 30min to mix the time；
The step 2 is step by step（3）With the step 3 step by step（2）Described in ultrasonic disperse temperature be for 40 DEG C,
The ultrasonic disperse time is 20min；
The step 2 is step by step（4）With the step 3 step by step（3）Described in vacuum defoamation using be stirred under vacuum
Machine, the heating under vacuum temperature are 60 DEG C, and the aspiration rate of vacuum is 0.1-2L/s；
The step 3 is step by step（4）In solidification temperature be followed successively by 90 DEG C, 120 DEG C, 150 DEG C, 180 DEG C, hardening time point
Wei not be 1 ~ 2 hour.
The present invention also provides a kind of composite heat interfacial material based on graphene, by above-mentioned compound thermal circle based on graphene
The preparation method of plane materiel material is made, and its component composition is in parts by weight：
5 ~ 10 parts of graphene oxide,
30 ~ 40 parts of nano-Ag particles,
100 parts of epoxy resin,
1 ~ 5 part of curing agent,
1 ~ 5 part of coupling agent.
The epoxy resin refers to liquid bisphenol A type epoxy resin；Further, the model of the bisphenol A type epoxy resin
For at least one of E-42, E-44, E-51；
The curing agent is at least one of aromatic polyamine, acid anhydrides, imidazole curing agent；
The coupling agent is silane coupler or titanate coupling agent；
The average grain diameter of the nano-Ag particles is 50 ~ 100nm；
The thickness of the graphene oxide is 0.55 ~ 1.2nm.
The present invention compared with prior art, has the advantages that：
1. by being modified processing to graphene oxide, the compatibility of graphene oxide and matrix material is improved, can be good
It is dispersed in matrix material well, is not susceptible to gather.
2. by doping nano-Ag particles to graphene and epoxy resin composite heat interfacial material, utilizing nano silver particles
The molten condition occurred in hot setting is connected between graphene layer to strengthen, and forms the Heat transmission approach of 3 D stereo network,
Reduce the interface resistance of composite inner.
Brief description of the drawings
Fig. 1 is the preparation flow figure of graphene and epoxy resin composite heat interfacial material；
Fig. 2 is the preparation flow figure of the composite heat interfacial material based on graphene.
Embodiment
Below by the invention will be further described in conjunction with the accompanying drawings and embodiments, but it is not limitation of the present invention.
Fig. 1 to Fig. 2 shows the preparation method of the composite heat interfacial material based on graphene, comprises the following steps：
Step 1, modified graphene oxide is prepared, it is specifically as follows step by step：
（1）By coupling agent and organic solvent in proportion 1:5 ~ 10 mixings obtain mixed liquor；
（2）Graphene oxide after vacuum drying is added in the mixed liquor and is uniformly mixing to obtain graphene oxide and is mixed
Liquid；
（3）The graphene oxide liquid mixture is heated under vacuo to react to obtain functional graphene oxide feed liquid；
（4）The functional graphene oxide feed liquid through and washing, filter, being dried to obtain modified graphene oxide；
Step 2, the composite heat interfacial material of graphene and epoxy resin is prepared, it is specifically as follows step by step：
（1）Epoxy resin and curing agent are added in organic solvent and mixed and obtains mixed liquor；
（2）The graphene oxide of the modification is added in the mixed liquor, and adds organic solvent diluting agitation grinding and obtains
To graphene oxide liquid mixture；
（3）Ultrasonic disperse is carried out to the graphene oxide liquid mixture；
（4）The graphene oxide liquid mixture after ultrasonic disperse is heated and is slowly stirred under vacuo, vacuum defoamation 5 ~
15min；
Step 3, the composite heat interfacial material based on graphene is prepared, it is specifically as follows step by step：
（1）Dried nano-Ag particles are added to the composite heat interfacial material of the graphene and epoxy resin, and addition has
Solvent agitation grinding obtains mixed liquor；
（2）Ultrasonic disperse is carried out to the mixed liquor；
（3）The mixed liquor after ultrasonic disperse is heated and is slowly stirred under vacuo, 5 ~ 15min of vacuum defoamation；
（4）The mixed liquor after vacuum defoamation is injected into mould, heating is solidified to obtain based on the compound of graphene
Thermal interfacial material.
The organic solvent is acetone, espeleton, ether, expoxy propane, hexamethylene, cyclohexanone, toluene, toluene hexamethylene
At least one of ketone；
The step 1 is step by step（3）The reaction temperature of middle graphene oxide and the mixed liquor is 40-80 DEG C, the reaction time
For 2-12 hours；
The step 1 is step by step（1）With the step 2 step by step（1）Described in mixing temperature be 40
DEG C, it is 30min to mix the time；
The step 2 is step by step（3）With the step 3 step by step（2）Described in ultrasonic disperse temperature be for 40 DEG C,
The ultrasonic disperse time is 20min；
The step 2 is step by step（4）With the step 3 step by step（3）Described in vacuum defoamation using be stirred under vacuum
Machine, the heating under vacuum temperature are 60 DEG C, and the aspiration rate of vacuum is 0.1-2L/s；
The step 3 is step by step（4）In solidification temperature be followed successively by 90 DEG C, 120 DEG C, 150 DEG C, 180 DEG C, hardening time point
Wei not be 1 ~ 2 hour.
Embodiment 1：
In order that graphene can be better dispersed in epoxy resin, graphene oxide is modified using coupling agent.Will
1g silane resin acceptor kh-550s and 30g acetone carry out mixing 30min；Graphene oxide after 5g is dried in vacuo adds
Into above-mentioned mixed liquor；Above-mentioned mixed liquor is heated under vacuo to 80 DEG C, and reaction obtains functional graphene oxide after 4 hours
Feed liquid；Above-mentioned feed liquid through and washing, filter, being dried to obtain modified graphene oxide.
100g epoxy resin E-42 and 1g m-phenylene diamine (MPD) resin curing agents are added in 100g acetone and mixed
30min；The modified graphene oxides of 2g are added in above-mentioned mixing liquid, and add 150g acetone in 40 DEG C of dilution stirrings
30min；To above-mentioned mixed liquor at 40 DEG C ultrasonic disperse 20min；Mixed liquor after ultrasonic disperse is put into de-airing mixer,
Regulation vacuum suction speed is 0.5L/s and is heated to 60 DEG C, is slowly stirred and vacuum defoamation 10min, obtains graphene and epoxy
Resin compounded thermal interfacial material.
The dried nano-Ag particles of 30g are added to the above-mentioned graphenes prepared of 80g and epoxy resin compound thermal circle
In plane materiel material, and add 50g acetone and stir and grind 30min；To above-mentioned mixing liquid at 40 DEG C ultrasonic disperse 20min；Will
Mixed liquor after ultrasonic disperse is put into de-airing mixer, and regulation vacuum suction speed is 0.5L/s and is heated to 60 DEG C, slowly
Simultaneously vacuum defoamation 10min is stirred, obtains the composite heat interfacial material based on graphene；Above-mentioned composite fluid material is injected into mould
Elevated cure is carried out in tool, hot setting temperature is followed successively by 90 DEG C, 120 DEG C, 150 DEG C, 180 DEG C, and hardening time is respectively 1 small
When.
Embodiment 2：
In order that graphene can be better dispersed in epoxy resin, graphene oxide is modified using coupling agent.Will
5g silane resin acceptor kh-550s and 30g acetone carry out mixing 30min；Graphene oxide after 10g is dried in vacuo adds
Enter into above-mentioned mixed liquor；Above-mentioned mixed liquor is heated under vacuo to 80 DEG C, and reaction obtains functional graphene oxide after 4 hours
Feed liquid；Above-mentioned feed liquid through and washing, filter, being dried to obtain modified graphene oxide.
100g epoxy resin E-42 and 5g m-phenylene diamine (MPD) resin curing agents are added in 100g acetone and mixed
30min；The modified graphene oxides of 3g are added in above-mentioned mixing liquid, and add 150g acetone in 40 DEG C of dilution stirrings
30min；To above-mentioned mixed liquor at 40 DEG C ultrasonic disperse 20min；Mixed liquor after ultrasonic disperse is put into de-airing mixer,
Regulation vacuum suction speed is 0.5L/s and is heated to 60 DEG C, is slowly stirred and vacuum defoamation 10min, obtains graphene and epoxy
Resin compounded thermal interfacial material.
The dried nano-Ag particles of 40g are added to the above-mentioned graphenes prepared of 80g and epoxy resin compound thermal circle
In plane materiel material, and add 50g acetone and stir and grind 30min；To above-mentioned mixing liquid at 40 DEG C ultrasonic disperse 20min；Will
Mixed liquor after ultrasonic disperse is put into de-airing mixer, and regulation vacuum suction speed is 0.5L/s and is heated to 60 DEG C, slowly
Simultaneously vacuum defoamation 10min is stirred, obtains the composite heat interfacial material based on graphene；Above-mentioned composite fluid material is injected into mould
Elevated cure is carried out in tool, hot setting temperature is followed successively by 90 DEG C, 120 DEG C, 150 DEG C, 180 DEG C, and hardening time is respectively 1 small
When.
The interface resistance of composite inner can be further reduced using technical scheme, is improved again so as to overall
The heat conductivility of condensation material.
Embodiments of the present invention are made that with detailed description above in association with drawings and examples, but the present invention is not limited to
Described embodiment.To those skilled in the art, without departing from the principles and spirit of the present invention, it is right
These embodiments carry out various change, modification, replacement and modification and still fallen within protection scope of the present invention.
Claims (10)
- A kind of 1. preparation method of the composite heat interfacial material based on graphene, it is characterised in that：Comprise the following steps：Step 1, modified graphene oxide is prepared, it is specifically as follows step by step：（1）By coupling agent and organic solvent in proportion 1:5 ~ 10 mixings obtain mixed liquor；（2）Graphene oxide after vacuum drying is added in the mixed liquor and is uniformly mixing to obtain graphene oxide and is mixed Liquid；（3）The graphene oxide liquid mixture is heated under vacuo to react to obtain functional graphene oxide feed liquid；（4）The functional graphene oxide feed liquid through and washing, filter, being dried to obtain modified graphene oxide；Step 2, the composite heat interfacial material of graphene and epoxy resin is prepared, it is specifically as follows step by step：（1）Epoxy resin and curing agent are added in organic solvent and mixed and obtains mixed liquor；（2）The graphene oxide of the modification is added in the mixed liquor, and adds organic solvent diluting agitation grinding and obtains To graphene oxide liquid mixture；（3）Ultrasonic disperse is carried out to the graphene oxide liquid mixture；（4）The graphene oxide liquid mixture after ultrasonic disperse is heated and is slowly stirred under vacuo, vacuum defoamation 5 ~ 15min；Step 3, the composite heat interfacial material based on graphene is prepared, it is specifically as follows step by step：（1）Dried nano-Ag particles are added to the composite heat interfacial material of the graphene and epoxy resin, and addition has Solvent agitation grinding obtains mixed liquor；（2）Ultrasonic disperse is carried out to the mixed liquor；（3）The mixed liquor after ultrasonic disperse is heated and is slowly stirred under vacuo, 5 ~ 15min of vacuum defoamation；（4）The mixed liquor after vacuum defoamation is injected into mould, heating is solidified to obtain based on the compound of graphene Thermal interfacial material.
- 2. the preparation method of the composite heat interfacial material according to claim 1 based on graphene, it is characterised in that：It is described Organic solvent is at least one in acetone, espeleton, ether, expoxy propane, hexamethylene, cyclohexanone, toluene, toluene cyclohexanone Kind.
- 3. the preparation method of the composite heat interfacial material according to claim 1 or 2 based on graphene, it is characterised in that：The step 1 is step by step（3）The reaction temperature of middle graphene oxide and the mixed liquor is 40-80 DEG C, the reaction time For 2-12 hours；The step 1 is step by step（1）With the step 2 step by step（1）Described in mixing temperature be 40 DEG C, it is 30min to mix the time；The step 2 is step by step（3）With the step 3 step by step（2）Described in ultrasonic disperse temperature be for 40 DEG C, The ultrasonic disperse time is 20min；The step 2 is step by step（4）With the step 3 step by step（3）Described in vacuum defoamation using be stirred under vacuum Machine, the heating under vacuum temperature are 60 DEG C, and the aspiration rate of vacuum is 0.1-2L/s；The step 3 is step by step（4）In solidification temperature be followed successively by 90 DEG C, 120 DEG C, 150 DEG C, 180 DEG C, hardening time point Wei not be 1 ~ 2 hour.
- 4. it is based on graphite made of a kind of preparation method of composite heat interfacial material based on graphene as described in claim 1 The composite heat interfacial material of alkene, it is characterised in that：Its component forms：5 ~ 10 parts of graphene oxide,30 ~ 40 parts of nano-Ag particles,100 parts of epoxy resin,1 ~ 5 part of curing agent,1 ~ 5 part of coupling agent.
- 5. the composite heat interfacial material according to claim 4 based on graphene, it is characterised in that：The epoxy resin is Refer to liquid bisphenol A type epoxy resin.
- 6. the composite heat interfacial material according to claim 5 based on graphene, it is characterised in that：The bisphenol-A type ring At least one of model E-42, E-44, E-51 of oxygen tree fat.
- 7. the composite heat interfacial material according to claim 4 based on graphene, it is characterised in that：The curing agent is virtue At least one of fragrant race's polyamines, acid anhydrides, imidazole curing agent.
- 8. the composite heat interfacial material according to claim 4 based on graphene, it is characterised in that：The coupling agent is silicon Alkane coupling agent or titanate coupling agent.
- 9. the composite heat interfacial material based on graphene according to any one of claim 4 to 8, it is characterised in that：It is described The average grain diameter of nano-Ag particles is 50 ~ 100nm.
- 10. the composite heat interfacial material based on graphene according to any one of claim 4 to 8, it is characterised in that：It is described The thickness of graphene oxide is 0.55 ~ 1.2nm.
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| CN110117376A (en) * | 2018-02-06 | 2019-08-13 | 中国科学院深圳先进技术研究院 | Compound cutan and preparation method thereof |
| CN110204867A (en) * | 2019-06-20 | 2019-09-06 | 西北工业大学 | A kind of three-dimensional silver-graphene hydridization foam/epoxy resin electromagnetic shielding composite material and preparation method thereof |
| CN113088037A (en) * | 2021-04-13 | 2021-07-09 | 珠海昌意新材料科技有限公司 | Heat dissipation material with high heat conductivity coefficient and high radiation coefficient and preparation method thereof |
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Application publication date: 20171222 |