CN104610706A - Magnesium oxide nanocrystalline coated graphene-epoxy resin composite material and preparation method thereof - Google Patents
Magnesium oxide nanocrystalline coated graphene-epoxy resin composite material and preparation method thereof Download PDFInfo
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- CN104610706A CN104610706A CN201410825902.9A CN201410825902A CN104610706A CN 104610706 A CN104610706 A CN 104610706A CN 201410825902 A CN201410825902 A CN 201410825902A CN 104610706 A CN104610706 A CN 104610706A
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Abstract
The invention discloses a magnesium oxide nanocrystalline coated graphene-epoxy resin composite material and a preparation method thereof, aims to avoid the defects that the existing graphene packing in an epoxy resin matrix is low in heat conductivity coefficient and has no electrical insulating property, and provides an epoxy resin composite material with low electrical conductivity and high thermal conductivity. According to the preparation method disclosed by the invention, the magnesium oxide nanocrystalline coated graphene composite material is uniformly dispersed into epoxy resin and solidified and molded, the insulating property of magnesium oxide as well as the good thermal conductivity of magnesium oxide and graphene can be utilized to effectively reduce the electrical conductivity of epoxy resin and improve the heat conducting property of epoxy resin; furthermore, the dispersity of the magnesium oxide nanocrystalline coated graphene composite material is good in epoxy resin, so that the heat conductivity is good when the additive amount is low. The magnesium oxide nanocrystalline coated graphene-epoxy resin composite material prepared according to the preparation method disclosed by the invention has a huge application prospect in the electronic packaging material field.
Description
Technical field
The present invention relates to a kind of epoxy resin composite material of low conductivity high thermal conductivity, be specifically related to brilliant coating graphite alkene-epoxy resin composite material of a kind of bitter earth nano and preparation method thereof.
Background technology
Along with the develop rapidly of China's economic construction, various circuit devcie is constantly along integrated, microminiaturized trend development, the problem caused thus is that electronic devices and components easily produce a large amount of heats in the course of the work, and has a strong impact on reliability, the stability and work-ing life etc. of circuit devcie work.Therefore, in the encapsulation field of electronic devices and components, need the electronic package material developing new high thermal conductivity, lead work used heat environment and be not trapped in device interior in time.Epoxy resin is one of plastics that in electronic package material, consumption is maximum, for improving the thermal conductivity of epoxy resin electronic package material, usually in matrix resin, the mineral filler of high thermal conductivity coefficient is added, as graphite, carbon fiber, silicon carbide, boron nitride, aluminum oxide, silver and other metal or inorganic non-metallic filler.These fillers have higher thermal conductivity, form heat conduction network in epoxy resin-base, effectively can improve the thermal conductivity of matrix.But, in order to reach high thermal conductivity coefficient, filler must when high filler loading capacity the good heat-conducting effect of competence exertion, cause resin package Drawing abillity and mechanical property deterioration.
In recent years, carbon nanomaterial (as carbon nanotube, Graphene) is used as heat conductive filler gradually to strengthen the thermal conductivity of macromolecule matrix.The thermal conductivity of Single Walled Carbon Nanotube is 6000W/mK, and the thermal conductivity of multi-walled carbon nano-tubes is 3000W/mK; And the thermal conductivity of Graphene is also up to more than 5000W/mK, and heat conduction direction is two dimension, therefore above-mentioned carbon nanomaterial is had very strong advantage as heat conductive filler.But the filler of these high thermal conductivity coefficients has excellent electroconductibility, is filled in resin matrix the specific conductivity that improve matrix, is not well positioned to meet the requirement of packaged material to electrical insulation properties.Therefore, how to reduce the specific conductivity of the resin matrix that Graphene is filled, and improve the heat conductivility of matrix material, by electronic package material field, there is huge application prospect.
Summary of the invention
The object of the present invention is to provide epoxy resin composite material of a kind of low conductivity high thermal conductivity and preparation method thereof, described matrix material has high thermal conductivity energy and good electrical insulation properties, has huge application prospect in high thermal insulating material field.
For achieving the above object, the technical solution used in the present invention is:
The brilliant coating graphite alkene-epoxy resin composite material of a kind of bitter earth nano, with epoxy resin, bitter earth nano brilliant coating graphite alkene matrix material, solidifying agent and organic solvent for raw material is prepared from, the mass ratio of epoxy resin and bitter earth nano brilliant coating graphite alkene matrix material is (10 ~ 1000): 1, the addition of solidifying agent is 5 ~ 50% of epoxy resin quality, and the solid-liquid ratio of the brilliant coating graphite alkene matrix material of bitter earth nano 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 brilliant coating graphite alkene matrix material is: joined by graphite oxide in deionized water, ultrasonic disperse 0.5 ~ 2h, obtains graphene oxide solution; To in gained graphene oxide solution, add solubility magnesium salts, be warming up to 60 ~ 100 DEG C under agitation, then dropwise basic solution is added, and reflux 4 ~ 12h, carry out suction filtration after having reacted, the filtrate obtained is dried at 60 ~ 100 DEG C, obtain the coated graphene oxide beige solid of magnesium hydroxide; The beige solid obtained is added in deionized water, ultrasonic disperse 0.5 ~ 2h, then add reductive agent wherein, under agitation, after 60 ~ 100 DEG C of reflux 6 ~ 24h, through suction filtration, oven dry, obtain magnesium hydroxide coated reduced graphene grey black solid; By the grey black solid that obtains under protection of inert gas, through 500 ~ 700 DEG C of calcining 2 ~ 5h, obtain described bitter earth nano brilliant coating graphite alkene matrix material.
According to such scheme, the mass ratio of described solubility magnesium salts and graphite oxide is (1 ~ 30): 1; Described graphene oxide solution concentration is 0.5 ~ 5mg/ml; Described solubility magnesium salts is magnesium sulfate, magnesium chloride, magnesium nitrate or their hydrate; Alkaline aqueous solution is sodium hydroxide, potassium hydroxide or ammoniacal liquor, and the mol ratio of the magnesium ion in the basic solution added in hydroxide ion and solubility magnesium salts is (2 ~ 4): 1; Described reductive agent is sodium borohydride, quadrol or hydrazine hydrate, and the mass ratio of reductive agent and the coated graphene oxide of magnesium hydroxide is (1 ~ 30): 1.
According to such scheme, the concentration of described ammoniacal liquor is 28wt%, and density is 0.89g/ml; The concentration of sodium hydroxide or potassium hydroxide is 10 ~ 50mg/ml.
According to such scheme, described solidifying agent is 1-ethyl imidazol(e), 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole, 593 solidifying agent or methyl tetrahydrophthalic anhydride.
According to such scheme, described organic solvent is ethanol, acetone, tetrahydrofuran (THF) or chloroform.
The preparation method of the brilliant coating graphite alkene-epoxy resin composite material of above-mentioned a kind of bitter earth nano, it is characterized in that, comprise the following steps: bitter earth nano brilliant coating graphite alkene matrix material is joined in organic solvent, ultrasonic disperse 0.5 ~ 2h obtains dispersion liquid, successively epoxy resin and solidifying agent are added in dispersion liquid again, first at 70 ~ 90 DEG C of ultrasonic disperse 0.5 ~ 2h, then strong stirring 0.5 ~ 3h, forms the homodisperse epoxy resin liquid of the brilliant coating graphite alkene matrix material of bitter earth nano; Then, will obtain after epoxy resin liquid carries out vacuum outgas bubble, casting on stainless steel mould, and under the condition of room temperature to 150 DEG C solidification 12 ~ 48h, obtain the brilliant coating graphite alkene-epoxy resin composite material of described bitter earth nano after finally demould.
Compared with prior art, beneficial effect of the present invention is:
1) bitter earth nano brilliant coating graphite alkene matrix material utilizes magnesian insulating property, magnesium oxide is coated on the surface of Graphene, improves the insulating property of this matrix material; Simultaneously in conjunction with the heat conductivility of magnesium oxide and Graphene, this composite material exhibits is made to go out good thermal conductivity.Described bitter earth nano brilliant coating graphite alkene matrix material is applied to epoxy resin, obviously can reduces the conductivity of epoxy resin and improve its heat conductivility.
2) to improve Graphene dispersed in the epoxy for bitter earth nano brilliant coating graphite alkene matrix material, the mechanical property of matrix material can be improved and form effective heat conduction network, making bitter earth nano brilliant coating graphite alkene matrix material can show good insulation heat-conducting property when addition is less.
3) alkene-epoxy resin composite material preparation method is simple, efficiency is high, cost is low, industrial production potential is huge for described bitter earth nano brilliant coating graphite, and products obtained therefrom has good heat conductivility and excellent insulating property.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
The brilliant coating graphite alkene-epoxy resin composite material of a kind of bitter earth nano, is prepared from by following steps:
1) 100mg graphite oxide is added in 100ml deionized water, ultrasonic disperse 1h, obtain graphene oxide solution, then add 2g Magnesium dichloride hexahydrate (0.01mol) wherein, be under agitation warming up to 80 DEG C, dropwise add 40ml sodium hydroxide solution (20mg/ml) wherein, and reflux 12h, after having reacted, after having reacted, carry out suction filtration, the filtrate obtained is dried at 80 DEG C, obtains the coated graphene oxide beige solid of magnesium hydroxide; Getting the coated graphene oxide of 100mg magnesium hydroxide adds in the deionized water of 100ml, ultrasonic disperse 1h, then adds the sodium borohydride of 1g, under agitation, after 80 DEG C of reflux 6h, through suction filtration, dry at 80 DEG C, obtain magnesium hydroxide coated reduced graphene grey black solid.Again by coated for magnesium hydroxide reduced graphene under nitrogen protection, through 600 DEG C of calcining 3h, obtain bitter earth nano brilliant coating graphite alkene matrix material.
2) get 800mg bitter earth nano brilliant coating graphite alkene matrix material and join (5mg/ml) in 160ml ethanol, ultrasonic disperse 0.5h obtains dispersion liquid, successively 800g bisphenol A-type E-51 epoxy resin and 40g 2-ethyl-4-methylimidazole are added in dispersion liquid, first at 70 DEG C of ultrasonic disperse 0.5h, and then mechanical strong stirring 0.5h, forms the homodisperse epoxy resin liquid of the brilliant coating graphite alkene matrix material of bitter earth nano.Then, after the epoxy resin liquid obtained is carried out vacuum outgas bubble, cast on stainless steel mould, and solidify 12h at ambient temperature, after the demoulding, obtain the brilliant coating graphite alkene-epoxy resin composite material of described bitter earth nano.
Brilliant for bitter earth nano obtained for the present embodiment coating graphite alkene-epoxy resin composite material is carried out heat conduction and conducting performance test, and its thermal conductivity is 0.2012W/mK, and specific conductivity is 2.8 × 10
-13scm
-1.
Embodiment 2
The brilliant coating graphite alkene-epoxy resin composite material of a kind of bitter earth nano, is prepared from by following steps:
1) 240mg graphite oxide is joined in 480ml deionized water, ultrasonic disperse 0.5h, obtain graphene oxide solution (0.5mg/ml), add 240mg magnesium sulfate (0.002mol) more wherein, under agitation be warming up to 60 DEG C, dropwise add 33ml potassium hydroxide solution (10mg/ml) wherein, and reflux 4h, suction filtration is carried out after having reacted, the filtrate obtained is dried at 60 DEG C, obtains the coated graphene oxide beige solid of magnesium hydroxide; Getting the coated graphene oxide of 200mg magnesium hydroxide adds in the deionized water of 400ml, ultrasonic disperse 0.5h, then adds 200mg quadrol, under agitation, after 60 DEG C of reflux 6h, through suction filtration, dry at 60 DEG C, obtain magnesium hydroxide coated reduced graphene grey black solid.Again by coated for magnesium hydroxide reduced graphene under argon shield, through 500 DEG C of calcining 5h, obtain bitter earth nano brilliant coating graphite alkene matrix material.
2) get 500mg bitter earth nano brilliant coating graphite alkene matrix material and join (10mg/ml) in 50ml acetone, ultrasonic disperse 1h obtains dispersion liquid, successively 593 solidifying agent of 10g bisphenol A-type E-44 epoxy resin and 3g are added in dispersion liquid, first at 80 DEG C of ultrasonic disperse 1h, and then mechanical strong stirring 1h, forms the homodisperse epoxy resin liquid of the brilliant coating graphite alkene matrix material of bitter earth nano.Then, will obtain after epoxy resin liquid carries out vacuum outgas bubble, casting on stainless steel mould, and solidify 24h under 80 DEG C of conditions, the brilliant coating graphite alkene-epoxy resin composite material of described bitter earth nano after the demoulding.
Brilliant for bitter earth nano obtained for the present embodiment coating graphite alkene-epoxy resin composite material is carried out heat conduction and conducting performance test, and its thermal conductivity is 0.3584W/mK, and specific conductivity is 1.6 × 10
-10scm
-1.
Embodiment 3
The brilliant coating graphite alkene-epoxy resin composite material of a kind of bitter earth nano, is prepared from by following steps:
1) 2.5g graphite oxide is added in 500ml deionized water, ultrasonic disperse 2h, obtain graphene oxide solution (5mg/ml), then add 75g magnesium nitrate hexahydrate wherein, be under agitation warming up to 100 DEG C, dropwise add 79ml ammoniacal liquor (28wt% wherein, density is 0.89g/ml), and reflux 12h, carry out suction filtration after having reacted, the filtrate obtained is dried at 100 DEG C, obtains the coated graphene oxide beige solid of magnesium hydroxide; Getting the coated graphene oxide of 2.5g magnesium hydroxide adds in the deionized water of 500ml, ultrasonic disperse 2h, then adds the hydrazine hydrate of 75g, under agitation, at 100 DEG C after reflux 24h, through suction filtration, dry at 100 DEG C, obtain magnesium hydroxide coated reduced graphene grey black solid; Again by coated for magnesium hydroxide reduced graphene under nitrogen protection, through 700 DEG C of calcining 2h, obtain bitter earth nano brilliant coating graphite alkene matrix material.
2) get 1.2g bitter earth nano brilliant coating graphite alkene matrix material and join (20mg/ml) in 60ml tetrahydrofuran (THF), ultrasonic disperse 2h obtains dispersion liquid, successively 12g bisphenol A-type E-51 epoxy resin and 6g methyl tetrahydrophthalic anhydride solidifying agent are added in dispersion liquid, first at 90 DEG C of ultrasonic disperse 2h, and then strong stirring 3h, forms the homodisperse epoxy resin liquid of the brilliant coating graphite alkene matrix material of bitter earth nano.Then, after the epoxy resin liquid obtained is carried out vacuum outgas bubble, cast on stainless steel mould, and solidify 48h at 150 DEG C of temperature, after the demoulding, obtain the brilliant coating graphite alkene-epoxy resin composite material of described bitter earth nano.
Brilliant for bitter earth nano obtained for the present embodiment coating graphite alkene-epoxy resin composite material is carried out heat conduction and conducting performance test, and its thermal conductivity is 0.4842W/mK, and specific conductivity is 6.4 × 10
-9scm
-1.
The each raw material that the present invention relates to and bound value thereof, interval value can realize the present invention, and lower limit value and the interval value of processing parameter of the present invention (as temperature, time etc.) can realize the present invention, do not enumerate embodiment at this.
Claims (8)
1. the brilliant coating graphite alkene-epoxy resin composite material of bitter earth nano, it is characterized in that, with epoxy resin, bitter earth nano brilliant coating graphite alkene matrix material, solidifying agent and organic solvent for raw material is prepared from, the mass ratio of epoxy resin and bitter earth nano brilliant coating graphite alkene matrix material is (10 ~ 1000): 1, the addition of solidifying agent is 5 ~ 50% of epoxy resin quality, and the solid-liquid ratio of the brilliant coating graphite alkene matrix material of bitter earth nano and organic solvent is (5 ~ 20): 1mg/ml.
2. matrix material according to claim 1, is characterized in that, described epoxy resin is bisphenol A-type E-51, bisphenol A-type E-44 or bisphenol F type resin.
3. matrix material according to claim 1, is characterized in that, the preparation method of described bitter earth nano brilliant coating graphite alkene matrix material is: joined by graphite oxide in deionized water, ultrasonic disperse 0.5 ~ 2h, obtains graphene oxide solution; To in gained graphene oxide solution, add solubility magnesium salts, be warming up to 60 ~ 100 DEG C under agitation, then dropwise basic solution is added, and reflux 4 ~ 12h, carry out suction filtration after having reacted, the filtrate obtained is dried at 60 ~ 100 DEG C, obtain the coated graphene oxide beige solid of magnesium hydroxide; The beige solid obtained is added in deionized water, ultrasonic disperse 0.5 ~ 2h, then add reductive agent wherein, under agitation, after 60 ~ 100 DEG C of reflux 6 ~ 24h, through suction filtration, oven dry, obtain magnesium hydroxide coated reduced graphene grey black solid; By the grey black solid that obtains under protection of inert gas, through 500 ~ 700 DEG C of calcining 2 ~ 5h, obtain described bitter earth nano brilliant coating graphite alkene matrix material.
4. matrix material according to claim 3, is characterized in that, the mass ratio of described solubility magnesium salts and graphite oxide is (1 ~ 30): 1; Graphene oxide solution concentration is 0.5 ~ 5mg/ml; Solubility magnesium salts is magnesium sulfate, magnesium chloride, magnesium nitrate or their hydrate; Alkaline aqueous solution is sodium hydroxide, potassium hydroxide or ammoniacal liquor, and the mol ratio of the magnesium ion in the basic solution added in hydroxide ion and solubility magnesium salts is (2 ~ 4): 1; Reductive agent is sodium borohydride, quadrol or hydrazine hydrate, and the mass ratio of reductive agent and the coated graphene oxide of magnesium hydroxide is (1 ~ 30): 1.
5. matrix material according to claim 4, is characterized in that, the concentration of described ammoniacal liquor is 28wt%, and the concentration of sodium hydroxide or potassium hydroxide is 10 ~ 50mg/ml.
6. matrix material according to claim 1, is characterized in that, described solidifying agent is 1-ethyl imidazol(e), 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole, 593 solidifying agent or methyl tetrahydrophthalic anhydride.
7. matrix material according to claim 1, is characterized in that, described organic solvent is ethanol, acetone, tetrahydrofuran (THF) or chloroform.
8. the preparation method of the brilliant coating graphite alkene-epoxy resin composite material of the bitter earth nano described in any one of claim 1 ~ 7, it is characterized in that, comprise the following steps: bitter earth nano brilliant coating graphite alkene matrix material is joined in organic solvent, ultrasonic disperse 0.5 ~ 2h obtains dispersion liquid, successively epoxy resin and solidifying agent are added in dispersion liquid again, first at 70 ~ 90 DEG C of ultrasonic disperse 0.5 ~ 2h, then strong stirring 0.5 ~ 3h, forms the homodisperse epoxy resin liquid of the brilliant coating graphite alkene matrix material of bitter earth nano; Then, after the epoxy resin liquid obtained is carried out vacuum outgas bubble, cast on stainless steel mould, and under the condition of room temperature to 150 DEG C solidification 12 ~ 48h, after the demoulding the described brilliant coating graphite alkene-epoxy resin composite material of bitter earth nano.
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| 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 |
| CN106084662A (en) * | 2016-06-22 | 2016-11-09 | 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 |
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| 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 |
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| CN108276615A (en) * | 2017-12-29 | 2018-07-13 | 华中科技大学 | A kind of high heat conduction stratiform graphene composite material and preparation method |
| 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 |
| CN111393795A (en) * | 2019-11-19 | 2020-07-10 | 浙江工业大学 | Three-dimensional heat-conducting insulating epoxy resin composite material and preparation method thereof |
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