CN108659466A - A kind of epoxy resin composite material and its preparation method and application - Google Patents
A kind of epoxy resin composite material and its preparation method and application Download PDFInfo
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- CN108659466A CN108659466A CN201810420081.9A CN201810420081A CN108659466A CN 108659466 A CN108659466 A CN 108659466A CN 201810420081 A CN201810420081 A CN 201810420081A CN 108659466 A CN108659466 A CN 108659466A
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- epoxy resin
- graphene
- composite material
- resin composite
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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
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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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
- C08K7/00—Use of ingredients characterised by shape
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
Abstract
The invention belongs to polymeric material field, it is related to a kind of epoxy resin composite material and its preparation method and application.Epoxy resin composite material provided by the invention includes graphene, curing agent and epoxy resin, and the mass ratio of the graphene, curing agent and epoxy resin is 0.33~8:10~50:100.The present invention is modified epoxy resin using graphene, and the excellent heat conductivility of graphene is utilized, and graphene dispersion forms heat conduction network, improve the heat conductivility of epoxy resin composite material in epoxy resin-base.The present invention controls the ratio of graphene and epoxy resin in above range, is conducive to keep graphene fully dispersed in the epoxy, and then is conducive to improve the heat conductivility of epoxy resin.
Description
Technical field
The present invention relates to polymeric material fields, and in particular to a kind of epoxy resin composite material and preparation method thereof and answers
With.
Background technology
Epoxy resin is with caking property is good, have a wide range of application, chemistry and spatial stability performance are good, mechanical property is good, processing
The features such as simple for process, is just being widely used in the fields such as production and living and national defence.To improve the object of epoxy resin composite material
Reason and chemical property, are increasingly paid close attention to the research that epoxy resin is modified by domestic and international researcher.But existing skill
The thermal conductivity of modified epoxy is still undesirable in art, cannot be satisfied the demand of people.
Invention content
The present invention provides a kind of epoxy resin composite materials and its preparation method and application.Asphalt mixtures modified by epoxy resin provided by the invention
Resin composite material thermal conductivity is good, and thermal coefficient is 0.331~0.414W/ (m*K).
The present invention provides a kind of epoxy resin composite material, including graphene, curing agent and epoxy resin, the graphite
The mass ratio of alkene, curing agent and epoxy resin is 0.33~8:10~50:100.
Preferably, the epoxy resin is 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters;The curing agent
For amine curing agent.
Preferably, the graphene is the graphene of two-dimensional layered structure.
The present invention provides the preparation methods of epoxy resin composite material described in above-mentioned technical proposal, include the following steps:
(1) graphene and low boiling point organic solvent are mixed, carries out ultrasonic disperse, obtain dispersion slurries;
(2) the dispersion slurries obtained to the step (1) heat, and the low boiling point organic solvent in dispersion slurries is made to steam
Hair obtains homogenization graphene;The temperature of the heating is 65~85 DEG C;
(3) it after mixing the homogenization graphene that the step (2) obtains with epoxy resin and curing agent, carries out successively true
Empty deaeration and curing molding, obtain epoxy resin composite material.
Preferably, low boiling point organic solvent is acetone in the step (1).
Preferably, the power of ultrasonic disperse is 280~320W in the step (1), time of the ultrasonic disperse is 1~
3h。
Preferably, the time heated in the step (2) is 16~20h;The volume of the organic solvent be 100~
200mL。
Preferably, the pressure of vacuum defoamation is 10~100Pa in the step (3).
Preferably, the temperature of curing molding is 60~150 DEG C in the step (3).
The present invention also provides rings described in epoxy resin composite material described in above-mentioned technical proposal or above-mentioned technical proposal
Application of the epoxy resin composite material that the preparation method of epoxy resin composite material is prepared in electronic package material.
Epoxy resin composite material provided by the invention includes graphene, curing agent and epoxy resin, and the graphene is consolidated
The mass ratio of agent and epoxy resin is 0.33~8:10~50:100.The present invention changes epoxy resin using graphene
Property, the excellent heat conductivility of graphene is utilized, graphene dispersion forms heat conduction network in epoxy resin-base, improves
The heat conductivility of epoxy resin composite material.The present invention controls the ratio of graphene, curing agent and epoxy resin in above-mentioned model
It encloses, is conducive to keep graphene fully dispersed in the epoxy, and then be conducive to improve the heat conductivility of epoxy resin.Embodiment
The result shows that, the thermal coefficient of epoxy resin composite material provided by the invention is 0.331~0.414W/ (m*K).
Description of the drawings
The epoxy resin composite material that Fig. 1 is prepared for the embodiment of the present invention 1 retouches electron microscope.
Specific implementation mode
The present invention provides a kind of epoxy resin composite material, including graphene, curing agent and epoxy resin, the graphite
The mass ratio of alkene, curing agent and epoxy resin is 0.33~8:10~50:100.
In the present invention, unless otherwise specified, each raw material component is commercial goods well known to those skilled in the art.
Epoxy resin composite material provided by the invention includes graphene, curing agent and epoxy resin.In the present invention, institute
The mass ratio for stating graphene, curing agent and epoxy resin is 0.33~8:10~50:100, preferably 0.5~5:15~45:
100, further preferably 1~4:20~40:100, more preferably 2~3:25~35:100.The present invention is using graphene to ring
Oxygen resin is modified, and the excellent heat conductivility of graphene is utilized, and graphene dispersion forms heat conduction in epoxy resin-base
Network improves the heat conductivility of epoxy resin composite material.The present invention controls the ratio of graphene and epoxy resin upper
Range is stated, is conducive to keep graphene fully dispersed in the epoxy, and then is conducive to improve the heat conductivility of epoxy resin.
In the present invention, the graphene is preferably the graphene of two-dimensional layered structure;The curing agent is preferably amine
Class curing agent, further preferably HDMA curing agent;The epoxy resin is preferably 4,5- 7-oxa-bicyclo[4.1.0-1,2- dioctyl phthalate two
Ethylene oxidic ester.
The present invention provides the preparation methods of epoxy resin composite material described in above-mentioned technical proposal, include the following steps:
(1) graphene and low boiling point organic solvent are mixed, carries out ultrasonic disperse, obtain dispersion slurries;
(2) the dispersion slurries obtained to the step (1) heat, and the low boiling point organic solvent in dispersion slurries is made to steam
Hair obtains homogenization graphene;The temperature of the heating is 65~80 DEG C;
(3) it after mixing the homogenization graphene that the step (2) obtains with epoxy resin and curing agent, carries out successively true
Empty deaeration and curing molding, obtain epoxy resin composite material.
The present invention mixes graphene and low boiling point organic solvent, carries out ultrasonic disperse, obtains dispersion slurries.
In the present invention, the quality of the graphene and the volume ratio of low boiling point organic solvent are preferably 0.8~14mg:
1mL, further preferably 1~13mg:1mL, more preferably 4~10mg:1mL.
In the present invention, the low boiling point organic solvent is preferably acetone.
In the present invention, the power of the ultrasonic disperse is preferably 280~320W, further preferably 300W;It is described super
The time of sound dispersion is preferably 1~3h, further preferably 1.5~2.5h.The present invention is conducive to make dispersion by ultrasonic disperse
The uniform particle sizesization of graphene in slurries.
The present invention heats obtained dispersion slurries, so that the low boiling point organic solvent in dispersion slurries is evaporated, obtains
Homogenize graphene.
In the present invention, the temperature of the heating is 65~85 DEG C, preferably 70~80 DEG C;The time of the heating is preferred
For 16~20h, further preferably 17~19h.In the present invention, the volume of the low boiling point organic solvent be preferably 100~
200mL, further preferably 120~180mL, more preferably 140~160mL.
The present invention is preferably stirred the dispersion slurries while heating.The present invention preferably by stirring at
It manages to improve the evaporation rate of low boiling point organic solvent.
The present invention evaporates low boiling point organic solvent by heat treatment, is conducive to that the uniform stone of particle size dispersion is prepared
Black alkene, and then be conducive to that graphene is enable to be well dispersed in epoxy resin-base, improve leading for epoxy resin composite material
Hot property.In the present invention, the homogenization graphene is preferably the uniform graphene powder of particle size dispersion.
After obtaining homogenization graphene, after the present invention mixes the homogenization graphene, epoxy resin and curing agent, according to
Secondary progress vacuum defoamation and curing molding, obtain epoxy resin composite material.
The present invention will homogenize graphene and be mixed with epoxy resin and curing agent, obtain mixed liquor.In the present invention, institute
The mode for stating mixing is preferably stirred, and the rotating speed of the stirring is preferably 700~900rpm, further preferably 750~
850rpm, more preferably 800rpm;The time being stirred is preferably 20~40min, further preferably 25~
35min, more preferably 30min.
The present invention preferably first mixes homogenization graphene with epoxy resin, is then mixed again with curing agent.
Present invention preferably employs above-mentioned hybrid mode, be conducive to graphene and epoxy resin being sufficiently mixed.
After the mixing, mixed liquor is carried out vacuum defoamation by the present invention, obtains deaeration feed liquid.
In the present invention, the pressure of the vacuum defoamation is preferably 10~100Pa, further preferably 20~80Pa, more
Preferably 40~60Pa;The time of the vacuum defoamation is preferably 40~80min, further preferably 50~70min, more preferably
It is still more preferably 60min for 55~65min.The present invention is preferably by the pressure of vacuum defoamation and time control in above-mentioned model
In enclosing, be conducive to remove in the bubble in mixed liquor, and then make graphene being capable of the company of being formed in epoxy resin-base
Continuous network structure improves the thermal conductivity of epoxy resin composite material.
After the vacuum defoamation, the present invention carries out curing molding to the deaeration feed liquid, obtains epoxy resin composite material.
In the present invention, the temperature of the curing molding is preferably 60~150 DEG C, further preferably 70~140 DEG C, more
Preferably 80~130 DEG C, be still more preferably 90~120 DEG C, most preferably 100~110 DEG C;The time of the curing molding
Preferably 1~4h, further preferably 2~3h.The present invention preferably controls the temperature and time of curing molding in above range
It is interior, be conducive under the action of curing agent, epoxy resin and graphene be made to be cured.
The preparation method of epoxy resin composite material provided by the invention is simple, easily operated, and can be prepared and lead
Hot good epoxy resin composite material.
The present invention also provides made described in epoxy resin composite material described in above-mentioned technical proposal or above-mentioned technical proposal
Application of the epoxy resin composite material that Preparation Method is prepared as electronic package material.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.
Embodiment 1
The graphene of 0.125g is added in the organic solvent-acetone of 150mL and carries out ultrasonic disperse, the ultrasonic disperse time
For 2h, dispersion slurries are obtained.Dispersion slurries are subjected to mechanical agitation in heating, heating temperature is 80 DEG C, and heating time is
18h so that after organic solvent volatilization completely therein, stop heating, obtain homogenization graphene.
The TDE-85 types epoxy resin of 25g is added to while stirring in above-mentioned obtained homogenization graphene, is stirred
Amine curing agent 12.5g is added while stirring after uniformly, continues after stirring evenly, vacuum defoamation is put into air dry oven,
Cure 3h at 120 DEG C, makes its curing molding to get to epoxy resin composite material.
Embodiment 2
The graphene of 0.25g is added in the organic solvent-acetone of 150mL and carries out ultrasonic disperse, the ultrasonic disperse time is
2h obtains dispersion slurries.Dispersion slurries are subjected to mechanical agitation in heating, heating temperature is 80 DEG C, heating time 18h,
So that after organic solvent volatilization completely therein, stop heating, obtains homogenization graphene.
The TDE-85 types epoxy resin of 25g is added to while stirring in above-mentioned obtained homogenization graphene, is stirred
Curing agent 12.5g is added while stirring after uniformly, continues after stirring evenly, vacuum defoamation is put into air dry oven, 120 DEG C
Lower solidification 3h makes its curing molding to get to epoxy resin composite material.
Embodiment 3
The graphene of the two-dimensional layered structure of 0.75g is added in the organic solvent-acetone of 150mL and carries out ultrasonic disperse,
The ultrasonic disperse time is 2h, obtains dispersion slurries.Dispersion slurries are subjected to mechanical agitation in heating, heating temperature is 80 DEG C,
Heating time is 18h so that after organic solvent volatilization completely therein, stops heating, obtains homogenization graphene.
The TDE-85 types epoxy resin of 25g is added to while stirring in above-mentioned obtained homogenization graphene, is stirred
Curing agent 12.5g is added while stirring after uniformly, continues after stirring evenly, vacuum defoamation is put into air dry oven, 120 DEG C
Lower solidification 3h makes its curing molding to get to epoxy resin composite material.
Embodiment 4
The graphene of the two-dimensional layered structure of 1.25g is added in the organic solvent-acetone of 150mL and carries out ultrasonic disperse,
The ultrasonic disperse time is 2h, obtains dispersion slurries.Dispersion slurries are subjected to mechanical agitation in heating, heating temperature is 80 DEG C,
Heating time is 18h so that after organic solvent volatilization completely therein, stops heating, obtains homogenization graphene.
The TDE-85 types epoxy resin of 25g is added to while stirring in above-mentioned obtained homogenization graphene, is stirred
Curing agent 12.5g is added while stirring after uniformly, continues after stirring evenly, vacuum defoamation is put into air dry oven, 120 DEG C
Lower solidification 3h makes its curing molding to get to epoxy resin composite material.
Embodiment 5
The graphene of the two-dimensional layered structure of 1.97g is added in the organic solvent-acetone of 150mL and carries out ultrasonic disperse,
The ultrasonic disperse time is 2h, obtains dispersion slurries.Dispersion slurries are subjected to mechanical agitation in heating, heating temperature is 80 DEG C,
Heating time is 18h so that after organic solvent volatilization completely therein, stops heating, obtains homogenization graphene.
The TDE-85 types epoxy resin of 25g is added to while stirring in above-mentioned obtained homogenization graphene, is stirred
Curing agent 12.5g is added while stirring after uniformly, continues after stirring evenly, vacuum defoamation is put into air dry oven, 120 DEG C
Lower solidification 3h makes its curing molding to get to epoxy resin composite material.
Comparative example 1
It is tested according to the method for embodiment 1, difference lies in graphene is not added, is directly added in the epoxy solid
Agent.
The structure for the epoxy resin composite material that embodiment 1 is prepared is scanned electron microscope analysis, as a result such as Fig. 1 institutes
Show.By Fig. 1 test results it is found that graphene can be dispersed in asphalt mixtures modified by epoxy resin in epoxy resin composite material provided by the invention
In aliphatic radical body.
The heat conductivility for the epoxy resin composite material that Examples 1 to 5 and comparative example 1 are prepared is tested.It adopts
Test the thermal coefficient of epoxy resin composite material at room temperature with NETZSCH heat transfer analysis instrument.During the test, asphalt mixtures modified by epoxy resin
The disk of a diameter of 12.7mm of resin composite material sample, one end are irradiated by laser pulse, are received and are risen in the other end of sample
Warm signal.Test result is as shown in table 1.
The thermal coefficient of 1 Examples 1 to 5 epoxy resin composite material of table
By 1 test result of table it is found that the thermal coefficient of epoxy resin composite material provided by the invention be 0.331~
0.414W/ (m*K), heat conductivility is preferable.
By the way that the thermal coefficient of the embodiment of the present invention 1 and comparative example 1 is compared it is found that asphalt mixtures modified by epoxy resin provided by the invention
Resin composite material have better heat conductivility, the present invention in graphene for improve epoxy resin composite material thermal conductivity have
It plays an important role.
As seen from the above embodiment, epoxy resin composite material provided by the invention has preferable heat conductivility, heat conduction
Coefficient reaches as high as 0.414W/ (m*K).
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of epoxy resin composite material, including graphene, curing agent and epoxy resin, the graphene, curing agent and ring
The mass ratio of oxygen resin is 0.33~8:10~50:100.
2. epoxy resin composite material according to claim 1, which is characterized in that the epoxy resin is 4,5- epoxide rings
Hexane -1,2- dicarboxylic acid diglycidyl esters;The curing agent is amine curing agent.
3. epoxy resin composite material according to claim 1, which is characterized in that the graphene is two-dimensional layered structure
Graphene.
4. a kind of preparation method of any one of claims 1 to 3 epoxy resin composite material, includes the following steps:
(1) graphene and low boiling point organic solvent are mixed, carries out ultrasonic disperse, obtain dispersion slurries;
(2) the dispersion slurries obtained to the step (1) heat, and the low boiling point organic solvent in dispersion slurries is made to evaporate,
Obtain homogenization graphene;The temperature of the heating is 65~85 DEG C;
(3) after mixing the homogenization graphene that the step (2) obtains with epoxy resin and curing agent, it is de- that vacuum is carried out successively
Bubble and curing molding, obtain epoxy resin composite material.
5. preparation method according to claim 4, which is characterized in that low boiling point organic solvent is third in the step (1)
Ketone.
6. preparation method according to claim 4 or 5, which is characterized in that the power of ultrasonic disperse is in the step (1)
The time of 280~320W, the ultrasonic disperse are 1~3h.
7. preparation method according to claim 4, which is characterized in that the time heated in the step (2) is 16~
20h;The volume of the low boiling point organic solvent is 100~200mL.
8. preparation method according to claim 4, which is characterized in that the pressure of vacuum defoamation is 10 in the step (3)
~100Pa.
9. the preparation method according to claim 4 or 8, which is characterized in that the temperature of curing molding is in the step (3)
60~150 DEG C.
10. any one of any one of claims 1 to 3 epoxy resin composite material or claim 4~9 the preparation side
Application of the epoxy resin composite material that method is prepared as electronic package material.
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Cited By (4)
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CN109694552A (en) * | 2018-12-17 | 2019-04-30 | 湖南艾华集团股份有限公司 | A kind of lithium battery encapsulation material and preparation method thereof |
CN110204861A (en) * | 2019-05-13 | 2019-09-06 | 广东墨睿科技有限公司 | A kind of graphene composite material and preparation method of excellent thermal conductivity |
CN113980426A (en) * | 2021-10-21 | 2022-01-28 | 浙江工业大学 | Modified graphene toughened epoxy resin heat-resistant composite material and preparation method thereof |
CN115011072A (en) * | 2022-07-08 | 2022-09-06 | 安徽宇航派蒙健康科技股份有限公司 | Epoxy resin composite heat conducting fin and preparation method thereof |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109694552A (en) * | 2018-12-17 | 2019-04-30 | 湖南艾华集团股份有限公司 | A kind of lithium battery encapsulation material and preparation method thereof |
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CN115011072A (en) * | 2022-07-08 | 2022-09-06 | 安徽宇航派蒙健康科技股份有限公司 | Epoxy resin composite heat conducting fin and preparation method thereof |
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Application publication date: 20181016 |