CN104610706B - A kind of bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material and preparation method thereof - Google Patents
A kind of bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of bitter earth nano crystalline substance coated graphite alkene epoxy resin composite material and preparation method thereof, in epoxy resin-base, have for existing Graphene filler that heat conductivity is low, shortcoming without electrical insulating property, it is provided that the epoxy resin composite material of a kind of low conductivity high thermal conductivity.The present invention by dispersed for bitter earth nano crystalline substance coated graphite alkene composite in the epoxy and curing molding, utilize the insulating properties of magnesium oxide, and combining magnesium oxide and the good heat conductivity of Graphene, the electric conductivity effectively reducing epoxy resin also improves its heat conductivility；And the dispersibility that bitter earth nano crystalline substance coated graphite alkene composite is in the epoxy is preferably, can play good heat conductivility in the case of addition is less.The bitter earth nano crystalline substance coated graphite alkene epoxy resin composite material that the present invention prepares has huge application prospect in electronic package material field.
Description
Technical field
The present invention relates to the epoxy resin composite material of a kind of low conductivity high thermal conductivity, be specifically related to a kind of bitter earth nano crystalline substance bag
Cover graphene-epoxy resin composite material and preparation method thereof.
Background technology
Along with developing rapidly of China's economic construction, various circuit devcies are constantly along integrated, the trend development of miniaturization, thus
The problem caused is that electronic devices and components the most easily produce substantial amounts of heat, and have a strong impact on circuit devcie work can
By property, stability and service life etc..Therefore, in the encapsulation field of electronic devices and components, need to develop the electricity of new high thermal conductivity
Sub-encapsulating material, guides environment in time by work used heat and is not trapped in device interior.Epoxy resin is to use in electronic package material
One of plastic that amount is maximum, for improving the thermal conductivity of epoxy resin electronic package material, generally adds height in matrix resin
The inorganic filler of heat conductivity, such as graphite, carbon fiber, carborundum, boron nitride, aluminium oxide, silver and other metal or inorganic non-
Metal packing.These fillers have higher heat conductivity, form heat conduction network, can be effectively improved base in epoxy resin-base
The heat conductivity of body.But, in order to reach high thermal conductivity coefficient, filler must be imitated when high filler loading capacity in the preferable heat conduction of competence exertion
Really, resin-encapsulated drawing abillity and mechanical property deterioration are caused.
In recent years, to be gradually used as heat filling polymer-based to strengthen for carbon nanomaterial (such as CNT, Graphene)
The heat conductivity of body.The heat conductivity of SWCN is 6000W/m K, and the heat conductivity of multi-walled carbon nano-tubes is 3000
W/m·K；And the heat conductivity of Graphene is also up to more than 5000W/m K, and heat conduction direction is two dimension, therefore by above-mentioned carbon
Nano material has the strongest advantage as heat filling.But, the filler of these high thermal conductivity coefficients has the electric conductivity of excellence,
It is filled in resin matrix the electrical conductivity that improve matrix, it is impossible to well meet the encapsulating material requirement to electrical insulation properties.
Therefore, how to reduce the electrical conductivity of resin matrix that Graphene is filled, and improve the heat conductivility of composite, will be at electronic seal
Package material field has huge application prospect.
Summary of the invention
It is an object of the invention to provide epoxy resin composite material of a kind of low conductivity high thermal conductivity and preparation method thereof, described
Composite have high thermal conductivity can and good electrical insulation properties, have huge application in high heat insulator field
Prospect.
For achieving the above object, the technical solution used in the present invention is:
A kind of bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material, with epoxy resin, bitter earth nano crystalline substance coated graphite
Alkene composite, firming agent and organic solvent are that raw material is prepared from, and epoxy resin is combined with bitter earth nano crystalline substance coated graphite alkene
The mass ratio of material is (10～1000): 1, and the addition of firming agent is the 5～50% of epoxy resin quality, bitter earth nano crystalline substance bag
The solid-liquid ratio covering graphene composite material and organic solvent is (5～20): 1mg/ml.
According to such scheme, described epoxy resin is bisphenol A-type E-51 or bisphenol A-type E-44 or bisphenol F type resin.
According to such scheme, the preparation method of described bitter earth nano crystalline substance coated graphite alkene composite is: added by graphite oxide
In deionized water, ultrasonic disperse 0.5～2h, obtain graphene oxide solution；In gained graphene oxide solution, add solvable
Property magnesium salt, be warming up to 60～100 DEG C under agitation, be then added dropwise over alkaline solution, and be heated to reflux 4～12h, reaction
Carry out sucking filtration after completing, the filtrate obtained is dried at 60～100 DEG C, obtain magnesium hydroxide cladding graphene oxide taupe
Solid；The beige solid obtained is added in deionized water, ultrasonic disperse 0.5～2h, then it is added thereto to reducing agent, stirring
Under the conditions of mixing, be heated to reflux 6～24h at 60～100 DEG C after, through sucking filtration, drying, obtain magnesium hydroxide cladding reduced graphene greyish black
Color solid；By the grey black solid that obtains under inert gas shielding, calcine 2～5h through 500～700 DEG C, obtain described magnesium oxide and receive
The brilliant coated graphite alkene composite of rice.
According to such scheme, described solubility magnesium salt is (1～30) with the mass ratio of graphite oxide: 1；Described graphene oxide solution is dense
Degree is 0.5～5mg/ml；Described solubility magnesium salt is magnesium sulfate, magnesium chloride, magnesium nitrate or their hydrate；Alkaline aqueous solution
For sodium hydroxide, potassium hydroxide or ammonia, hydroxide ion and the magnesium ion in solubility magnesium salt in the alkaline solution added
Mol ratio is (2～4): 1；Described reducing agent is sodium borohydride, ethylenediamine or hydrazine hydrate, reducing agent and magnesium hydroxide cladding oxidation stone
The mass ratio of ink alkene is (1～30): 1.
According to such scheme, the concentration of described ammonia is 28wt%, and density is 0.89g/ml；Sodium hydroxide or potassium hydroxide dense
Degree is 10～50mg/ml.
According to such scheme, described firming agent is 1-ethyl imidazol(e), 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole, 593 solid
Agent or methyl tetrahydrophthalic anhydride.
According to such scheme, described organic solvent is ethanol, acetone, oxolane or chloroform.
The preparation method of above-mentioned a kind of bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material, it is characterised in that include with
Lower step: joining in organic solvent by bitter earth nano crystalline substance coated graphite alkene composite, ultrasonic disperse 0.5～2h must disperse
Liquid, more successively epoxy resin and firming agent are added in dispersion liquid, first at 70～90 DEG C of ultrasonic disperse 0.5～2h, the most by force
Power stirring 0.5～3h, forms bitter earth nano crystalline substance coated graphite alkene composite homodisperse epoxy resin liquid；Then, incite somebody to action
After carrying out vacuum outgas bubble to epoxy resin liquid, cast on stainless steel mould, and under conditions of room temperature to 150 DEG C solidify 12～
48h, obtains described bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material after the last demoulding.
Compared with prior art, the invention have the benefit that
1) bitter earth nano crystalline substance coated graphite alkene composite utilizes the insulating properties of magnesium oxide, and magnesium oxide is coated on Graphene
Surface, improves the insulating properties of this composite；In combination with magnesium oxide and the heat conductivility of Graphene, make this composite table
Reveal good heat conductivity.Described bitter earth nano crystalline substance coated graphite alkene composite is applied to epoxy resin, can obviously reduce
The electric conductivity of epoxy resin also improves its heat conductivility.
2) bitter earth nano crystalline substance coated graphite alkene composite improves Graphene dispersibility in the epoxy, can improve composite wood
Material mechanical property and form effective heat conduction network, make bitter earth nano crystalline substance coated graphite alkene composite less at addition
In the case of can show good insulation heat-conducting property.
3) crystalline substance coated graphite alkene-epoxy resin composite material preparation method is simple, efficiency is high, low cost, work for described bitter earth nano
Industry metaplasia is produced and is had a high potential, and products obtained therefrom has good heat conductivility and excellent insulating properties.
Detailed description of the invention
In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, but present disclosure is not only
It is confined to the following examples.
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is carried out
Further describe.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to limit this
Invention.
Embodiment 1
A kind of bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material, is prepared from by following steps:
1) 100mg graphite oxide is added in 100ml deionized water, ultrasonic disperse 1h, it is thus achieved that graphene oxide solution, then
It is added thereto to 2g Magnesium dichloride hexahydrate (0.01mol), is under agitation warming up to 80 DEG C, is added dropwise over 40ml hydrogen-oxygen wherein
Change sodium solution (20mg/ml), and be heated to reflux 12h, after having reacted, after having reacted, carry out sucking filtration, the filtration that will obtain
Thing is dried at 80 DEG C, obtains magnesium hydroxide cladding graphene oxide beige solid；Take 100mg magnesium hydroxide cladding graphite oxide
Alkene adds in the deionized water of 100ml, and ultrasonic disperse 1h is subsequently adding the sodium borohydride of 1g, under agitation, at 80 DEG C
After being heated to reflux 6h, through sucking filtration, dry at 80 DEG C, obtain magnesium hydroxide cladding reduced graphene grey black solid.Again by hydroxide
Magnesium cladding reduced graphene under nitrogen protection, is calcined 3h through 600 DEG C, is obtained bitter earth nano crystalline substance coated graphite alkene composite.
2) take 800mg bitter earth nano crystalline substance coated graphite alkene composite and join (5mg/ml) in 160ml ethanol, ultrasonic point
Scattered 0.5h obtains dispersion liquid, adds 800g bisphenol A-type E-51 epoxy resin and 40g 2-ethyl-4-methylimidazole to dispersion successively
In liquid, first at 70 DEG C of ultrasonic disperse 0.5h, and then machinery strong stirring 0.5h, form bitter earth nano crystalline substance coated graphite alkene multiple
Condensation material homodisperse epoxy resin liquid.Then, after the epoxy resin liquid obtained is carried out vacuum outgas bubble, cast in stainless
In steel mold, and solidify 12h at ambient temperature, obtain described bitter earth nano crystalline substance coated graphite alkene-epoxy resin after the demoulding and be combined
Material.
Bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material that the present embodiment prepares is carried out heat conduction and electric conductivity is surveyed
Examination, its heat conductivity is 0.2012W/m K, and electrical conductivity is 2.8 × 10-13S·cm-1。
Embodiment 2
A kind of bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material, is prepared from by following steps:
1) 240mg graphite oxide is joined in 480ml deionized water, ultrasonic disperse 0.5h, it is thus achieved that graphene oxide solution
(0.5mg/ml), then it is added thereto to 240mg magnesium sulfate (0.002mol), is under agitation warming up to 60 DEG C, the most dropwise
Add 33ml potassium hydroxide solution (10mg/ml), and be heated to reflux 4h, after having reacted, carry out sucking filtration, the filtration that will obtain
Thing is dried at 60 DEG C, obtains magnesium hydroxide cladding graphene oxide beige solid；Take 200mg magnesium hydroxide cladding graphite oxide
Alkene adds in the deionized water of 400ml, and ultrasonic disperse 0.5h is subsequently adding 200mg ethylenediamine, under agitation,
After 60 DEG C are heated to reflux 6h, through sucking filtration, dry at 60 DEG C, obtain magnesium hydroxide cladding reduced graphene grey black solid.Again by hydrogen
Magnesium oxide cladding reduced graphene, under argon shield, is calcined 5h through 500 DEG C, is obtained bitter earth nano crystalline substance coated graphite alkene composite wood
Material.
2) take 500mg bitter earth nano crystalline substance coated graphite alkene composite and join (10mg/ml) in 50ml acetone, ultrasonic
Dispersion 1h obtains dispersion liquid, adds in dispersion liquid by 593 firming agent of 10g bisphenol A-type E-44 epoxy resin and 3g successively,
First at 80 DEG C of ultrasonic disperse 1h, and then machinery strong stirring 1h, form bitter earth nano crystalline substance coated graphite alkene composite equal
Even scattered epoxy resin liquid.Then, will obtain after epoxy resin liquid carries out vacuum outgas bubble, casting on stainless steel mould,
And under the conditions of 80 DEG C, solidify 24h, described bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material after the demoulding.
Bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material that the present embodiment prepares is carried out heat conduction and electric conductivity is surveyed
Examination, its heat conductivity is 0.3584W/m K, and electrical conductivity is 1.6 × 10-10S·cm-1。
Embodiment 3
A kind of bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material, is prepared from by following steps:
1) 2.5g graphite oxide is added in 500ml deionized water, ultrasonic disperse 2h, it is thus achieved that graphene oxide solution (5mg/ml),
Be added thereto to 75g magnesium nitrate hexahydrate again, be under agitation warming up to 100 DEG C, be added dropwise over wherein 79ml ammonia (28wt%,
Density is 0.89g/ml), and it is heated to reflux 12h, carry out sucking filtration after having reacted, the filtrate obtained dried at 100 DEG C,
Obtain magnesium hydroxide cladding graphene oxide beige solid；Take 2.5g magnesium hydroxide cladding graphene oxide add 500ml go from
In sub-water, ultrasonic disperse 2h, be subsequently adding the hydrazine hydrate of 75g, under agitation, be heated to reflux 24h at 100 DEG C after, through taking out
Filter, dry at 100 DEG C, obtain magnesium hydroxide cladding reduced graphene grey black solid；Again magnesium hydroxide is coated with reduced graphene to exist
Under nitrogen protection, calcine 2h through 700 DEG C, obtain bitter earth nano crystalline substance coated graphite alkene composite.
2) take 1.2g bitter earth nano crystalline substance coated graphite alkene composite and join (20mg/ml) in 60ml oxolane, super
Sound dispersion 2h obtains dispersion liquid, 12g bisphenol A-type E-51 epoxy resin and 6g methyl tetrahydrophthalic anhydride is solidified successively
Agent is added in dispersion liquid, first at 90 DEG C of ultrasonic disperse 2h, and then strong stirring 3h, forms bitter earth nano crystalline substance cladding stone
Ink alkene composite homodisperse epoxy resin liquid.Then, after the epoxy resin liquid obtained is carried out vacuum outgas bubble, casting
On stainless steel mould, and at a temperature of 150 DEG C, solidify 48h, after the demoulding, obtain described bitter earth nano crystalline substance coated graphite alkene-epoxy
Resin composite materials.
Bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material that the present embodiment prepares is carried out heat conduction and electric conductivity is surveyed
Examination, its heat conductivity is 0.4842W/m K, and electrical conductivity is 6.4 × 10-9S·cm-1。
The each raw material that the present invention relates to and bound value thereof, interval value can realize the present invention, the technological parameter of the present invention (as
Temperature, time etc.) lower limit value and interval value can realize the present invention, embodiment numerous to list herein.
Claims (8)
1. bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material, it is characterised in that with epoxy resin, magnesium oxide
Nanocrystalline coated graphite alkene composite, firming agent and organic solvent are that raw material is prepared from, and epoxy resin is brilliant with bitter earth nano
The mass ratio of coated graphite alkene composite is (10～1000): 1, and the addition of firming agent is the 5～50% of epoxy resin quality,
Bitter earth nano crystalline substance coated graphite alkene composite is (5～20): 1mg/ml with the solid-liquid ratio of organic solvent.
Bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material the most according to claim 1, it is characterised in that institute
State epoxy resin be bisphenol A-type E-51, bisphenol A-type E-44 or bisphenol F type resin.
Bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material the most according to claim 1, it is characterised in that institute
The preparation method stating bitter earth nano crystalline substance coated graphite alkene composite is: joined by graphite oxide in deionized water, ultrasonic point
Dissipate 0.5～2h, obtain graphene oxide solution；In gained graphene oxide solution, add solubility magnesium salt, under agitation
It is warming up to 60～100 DEG C, is then added dropwise over alkaline solution, and is heated to reflux 4～12h, after having reacted, carry out sucking filtration, will
The filtrate arrived is dried at 60～100 DEG C, obtains magnesium hydroxide cladding graphene oxide beige solid；The taupe that will obtain
Solid adds in deionized water, ultrasonic disperse 0.5～2h, then is added thereto to reducing agent, under agitation, at 60～100 DEG C
After being heated to reflux 6～24h, through sucking filtration, drying, obtain magnesium hydroxide cladding reduced graphene grey black solid；Greyish black by obtain
Color solid, under inert gas shielding, calcines 2～5h through 500～700 DEG C, obtains described bitter earth nano crystalline substance coated graphite alkene and is combined
Material.
Bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material the most according to claim 3, it is characterised in that institute
The mass ratio stating solubility magnesium salt and graphite oxide is (1～30): 1；Graphene oxide solution concentration is 0.5～5mg/ml；Soluble magnesium
Salt is magnesium sulfate, magnesium chloride, magnesium nitrate or their hydrate；Alkaline aqueous solution is sodium hydroxide, potassium hydroxide or ammonia,
In the alkaline solution added, hydroxide ion is (2～4) with the mol ratio of the magnesium ion in solubility magnesium salt: 1；Reducing agent is boron hydrogen
Changing sodium, ethylenediamine or hydrazine hydrate, reducing agent is (1～30) with the mass ratio of magnesium hydroxide cladding graphene oxide: 1.
Bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material the most according to claim 4, it is characterised in that institute
The concentration that concentration is 28wt%, sodium hydroxide or potassium hydroxide stating ammonia is 10～50mg/ml.
Bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material the most according to claim 1, it is characterised in that institute
Stating firming agent is 1-ethyl imidazol(e), 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole, 593 firming agent or methyl tetrahydrochysene O-phthalic
Anhydride.
Bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material the most according to claim 1, it is characterised in that institute
Stating organic solvent is ethanol, acetone, oxolane or chloroform.
8. the preparation method of the bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material described in any one of claim 1～7,
It is characterized in that, comprise the following steps: bitter earth nano crystalline substance coated graphite alkene composite is joined in organic solvent, ultrasonic
Dispersion 0.5～2h obtains dispersion liquid, then adds in dispersion liquid by epoxy resin and firming agent successively, first at 70～90 DEG C ultrasonic point
Scattered 0.5～2h, then strong stirring 0.5～3h, form the bitter earth nano crystalline substance coated graphite homodisperse epoxy of alkene composite
Resin liquid；Then, after the epoxy resin liquid obtained is carried out vacuum outgas bubble, cast on stainless steel mould, and in room temperature extremely
Solidify 12～48h under conditions of 150 DEG C, after the demoulding, obtain described bitter earth nano crystalline substance coated graphite alkene-epoxy resin composite material.
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| CN104861910B (en) * | 2015-05-20 | 2017-04-05 | 北京化工大学 | A kind of graphene coated inorganic filler epoxy resin compound adhesive and preparation method thereof |
| CN105504231A (en) * | 2016-01-22 | 2016-04-20 | 武汉理工大学 | High-weather-resistance epoxy resin for composite material |
| CN106084662B (en) * | 2016-06-22 | 2018-10-16 | 苏交科集团股份有限公司 | A kind of epoxy resin composite material of anti-ultraviolet ageing and preparation method thereof |
| CN106117518A (en) * | 2016-06-22 | 2016-11-16 | 柳州市强威锻造厂 | A kind of imidazoles epoxy resin cure formula |
| CN106496632A (en) * | 2016-10-14 | 2017-03-15 | 复旦大学 | A kind of preparation method of magnesium oxide Graphene composite heat-conducting insulating packing |
| CN106496634A (en) * | 2016-10-14 | 2017-03-15 | 复旦大学 | A kind of preparation method of magnesium hydroxide Graphene composite heat-conducting insulating packing |
| CN107129660A (en) | 2017-05-12 | 2017-09-05 | 深圳市华星光电技术有限公司 | LED encapsulation material and preparation method |
| CN107524934A (en) * | 2017-10-18 | 2017-12-29 | 安徽建筑大学 | A kind of AC light-emitting diode lamp tool |
| CN108276615B (en) * | 2017-12-29 | 2020-05-19 | 华中科技大学 | High-thermal-conductivity layered graphene composite material and preparation method thereof |
| CN111393795B (en) * | 2019-11-19 | 2023-10-13 | 浙江工业大学 | Three-dimensional heat-conducting insulating epoxy resin composite material and preparation method thereof |
| CN113629350B (en) * | 2021-08-06 | 2022-07-12 | 江苏正力新能电池技术有限公司 | Power battery heat-conducting coating diaphragm and preparation method thereof |
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| CN102286189B (en) * | 2011-06-24 | 2012-11-21 | 中国科学院理化技术研究所 | Method for preparing graphene oxide/epoxide resin nano composite material |
| KR20110089835A (en) * | 2011-07-13 | 2011-08-09 | 이재환 | High density nano coating compositions |
| CN102921376A (en) * | 2012-11-27 | 2013-02-13 | 武汉工程大学 | Magnesium hydroxide/graphene compound adsorbing material for phosphorus-containing wastewater treatment as well as preparation method and application thereof |
| KR20140086581A (en) * | 2012-12-28 | 2014-07-08 | 삼성전기주식회사 | Resin composition with enhanced heat-releasing property, heat-releasing film, insulating film, and prepreg |
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