CN102532606A - Modified aluminum nitride filled epoxy resin composite material - Google Patents
Modified aluminum nitride filled epoxy resin composite material Download PDFInfo
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- CN102532606A CN102532606A CN201010623954XA CN201010623954A CN102532606A CN 102532606 A CN102532606 A CN 102532606A CN 201010623954X A CN201010623954X A CN 201010623954XA CN 201010623954 A CN201010623954 A CN 201010623954A CN 102532606 A CN102532606 A CN 102532606A
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Abstract
The invention discloses a heat-conducting insulated modified superfine aluminum nitride filled epoxy resin composite material. The composite material is prepared by doping superfine aluminum nitride powder which is subjected to plasma organic polymerization (with pyrrole and acrylic acid) into epoxy resin, and performing processes of vacuum degassing, vacuum filling and the like. The composite material has high heat conductivity, insulating property and mechanical properties, can be applied in the fields requiring materials such as electronic packaging materials, integrated circuits and the like to have high heat conductivity and insulating property.
Description
Technical field
The invention belongs to field of compound material.Specifically, the present invention relates to a kind of heat conduction, the good modification aluminium nitride AlN filling epoxy resin matrix material of insulating property.This material (77K) under normal temperature, low temperature has the good mechanical performance.
Background technology
Epoxy resin matrix material structured material and the insulating material done commonly used can both seen its trace on a lot of devices, like the baseplate material of electron device, superconducting magnet insulation system, large-scale integrated circuit etc.Therefore epoxy resin should have heat conduction, insulate, has the function of certain mechanical strength.Have research with aluminum nitride particle as strongthener, epoxy resin (E-51) is as polymeric matrix, aluminum nitride particle mixes the back thermal conductivity can reach 0.46W.m
-1.K
-1, and still can keep the epoxy resin specific inductivity; Also there is document to adopt titanate coupling agent to handle aluminium nitride powder, preparation aluminium nitride AlN epoxy resin composite material, and mention aluminium nitride AlN massfraction 10～20% o'clock, shock strength is better.Obviously, the performance of aluminium nitride AlN composite epoxy resin material is better, uses more extensive.Based on the demand, the inventor intends and proposes a kind of modification aluminium nitride AlN composite epoxy resin material.
Chinese invention patent " a kind of magnetic seed material " has been set forth the way of plasma polymerization magneticsubstance has been carried out modification, has obtained a kind of and the stronger magneticsubstance of organism avidity.The inventor uses for reference this method, adopts the method for plasma polymerization that the superfine aluminium nitride particle is carried out modification, adopts vacuum perfusion process to prepare aluminium nitride AlN filling epoxy resin matrix material.
Summary of the invention
The purpose of this invention is to provide a kind of modification aluminum nitride particle and preparation method thereof.
Another object of the present invention provides good modification aluminium nitride AlN filling epoxy resin matrix material of a kind of heat conduction, insulating property and preparation method thereof.
Modification aluminum nitride particle according to the invention is that the polymeric film by aluminum nitride particle and particle surface constitutes.
Wherein, said polymeric film is vinylformic acid (C
2H
4O
2) or pyrroles (C
2H
5N) film; Preferred pyrroles (C
2H
5N) film.
Because a little less than acrylic acid volatility, experiment finds that the material total amount that is deposited on particle surface behind the plasma polymerization is less, the infrared figure peak of the superfine aluminium nitride powder that plasma polymerization is acrylic acid modified is not obvious; The aluminium nitride AlN filling epoxy resin composite material strength of polymeric acrylic acid modification also is not so good as pyrrole polymerization modification aluminium nitride AlN prepared composite material, the therefore preferred pyrroles (C of said polymeric film in addition
2H
5N) film.
The granularity of said aluminum nitride particle is a micron order; Generally can adopt commercial aluminium nitride AlN micron powder, its general size is a few to tens of microns; Modification aluminum nitride particle according to the invention can adopt this area method preparation commonly used, preferably adopts the preparation of plasma polymerization method.The thickness of said polymeric film is generally nano level.
The synoptic diagram of said plasma polymerization method equipment therefor is seen shown in Figure 1, specifically carries out as follows: the superfine aluminium nitride about 0.5g is placed in the glass bend pipe reaction chamber, guarantee that each several part is airtight after, open vacuum air pump, open radio-frequency power supply.When reaction indoor gas color was white in color, the expression plasma film coating apparatus was in proper working order.Below the about 30pa of reaction tubes internal pressure this moment.Unscrew the monomeric under meter of connection, make flow of monomer at 10～20ml/min.Magneton in the reaction tubes rotates under the magnetic stirring apparatus effect, thereby the powder that is modified is fully contacted with reaction tubes interpolymer steam.40-150min is carried out in reaction, about generally about 1h.
Wherein, monomer is vinylformic acid or pyrroles, and this monomer is generally volatile liquid, under the effect of sucking pump pump, and lower pressure of plasma film coating apparatus inner sustain, monomer became and evaporated into gas more easily this moment.Thereby control monomeric flow through the adjustments of gas under meter, make monomer be coated on the powder surface that is modified equably.Behind the plasma organic polymer, the polymkeric substance that polar group is arranged that monomer polymerization forms firmly covers the superfine aluminium nitride surface.
The present invention also provides good modification aluminium nitride AlN filling epoxy resin matrix material of a kind of heat conduction, insulating property and preparation method thereof.
Modification aluminium nitride AlN filling epoxy resin matrix material of the present invention mainly is made up of epoxy resin and the above-mentioned modification aluminium nitride powder that wherein is mingled with;
The mass ratio of said epoxy resin and modification aluminium nitride AlN is: 2～11: 1; If when modification aluminium nitride AlN content continues to increase, the powder layering can occur in the epoxy resin composite material, be helpless to the raising of performance.According to experimental result, preferred 5: 1 of the mass ratio of said epoxy resin and modification aluminium nitride AlN.
In addition, said matrix material also comprises toughner and solidifying agent.
Wherein, said epoxy resin is this area various epoxy resin commonly used; Be preferably bisphenol F epoxy resin (diglycidylether Bisphenol F);
Said toughner is epoxy resin toughner commonly used, like DOP, DBP, TCP, TPP etc.; The preferred IPBE of the present invention i.e. (2-glycidyl-3-n-butoxy)-1-propyl ether.
Solidifying agent also can be selected epoxy resin solidifying agent commonly used for use, is main body like aliphatic amide, aliphatic cyclic amine, aromatic amine, polymeric amide, acid anhydrides, resene, tertiary amine etc. with the phenyl ring, has the molecule of flexible side-chains; Preferred DETD (diethyl toluene diamine), perhaps DMTD (diformazan sulfenyl tolylene diamine).
Preferably, said matrix material comprises following component: epoxy resin massfraction 45～55%, solidifying agent massfraction 15～25%, toughner massfraction 10～20%; Modified superfine aluminium nitride AlN massfraction 5～20%.
Preferred, said toughner massfraction 10～20%, solidifying agent massfraction 20%, resin 50% remain and are the modified superfine aluminium nitride AlN.
The present invention also provides the preparation method of above-mentioned modification aluminium nitride AlN filling epoxy resin matrix material.
The preparation method of described modification aluminium nitride AlN filling epoxy resin matrix material is:
1) modified superfine aluminium nitride AlN and solidifying agent, toughner, epoxy resin are mixed by proportioning, mixture is carried out vacuum outgas handle; Said vacuum outgas is preferably carried out as follows: under the vacuum state, and 20～60 ℃, the degassing 1～3h;
2) inject mould, heat up and solidify the demoulding then.
For reaching the purpose of mixing, said mixing can adopt this area method commonly used to carry out, like mechanical stirring, ultra-sonic dispersion etc.; Preferably carry out mechanical stirring earlier, and then ultra-sonic dispersion; Adopt the mechanical stirring mode roughly to mix earlier, the macrobead of reuniting is broken up; After treating that machinery stirs, adopt UW to mix again, with a small amount of not small-particle mixing of mixing, it is more even that component is mixed.Wherein, the kind of mechanical stirring and ultra-sonic dispersion and parameter can rule of thumb be selected by those skilled in the art.
Said injection mould preferably carries out under vacuum; The resin that the present invention adopts is a normal temperature current downflow property resin preferably, is convenient to very much carry out priming by vacuum after the vacuum outgas.The technology of priming by vacuum is poured into down compared with normal pressure, because priming by vacuum can not make resin dissolve into some air once more, the material bubble that makes like this is few.
Said vacuum outgas can be removed lower-boiling impurity that is mixed with in the resin etc.; Preferably can be employed in 30 ℃ of temperature, the following vacuum outgas 1h of vacuum tightness 30Pa achieves the goal.
When it should be noted that carrying out vacuum outgas handles, temperature should be moderate.Too high height is prone to cause the resin premature setting rotten, and it is slow to cross in the low resin impurity effusion speed, and general 20～60 ℃, more than the degassing 1h, until not or till not little bubble overflows.
Wherein, said epoxy resin massfraction 45～55%, solidifying agent massfraction 15～25%, toughner massfraction 10～20%; Modified superfine aluminium nitride AlN massfraction 5～20%.
Preferably, said toughner massfraction 10～20%, solidifying agent massfraction 20%, resin 50% remain and are the modified superfine aluminium nitride AlN.
Said toughner is epoxy resin toughner commonly used, like DOP, DBP, TCP, TPP etc.; The preferred IPBE of the present invention i.e. (2-glycidyl-3-n-butoxy)-1-propyl ether.
Solidifying agent also can be selected epoxy resin solidifying agent commonly used for use, like aliphatic amide, aliphatic cyclic amine, aromatic amine, polymeric amide, acid anhydrides, resene, tertiary amine etc.; Preferred DETD (diethyl toluene diamine), perhaps DMTD (diformazan sulfenyl tolylene diamine).
Used resin is this area various epoxy resin commonly used; Be preferably bisphenol F epoxy resin (diglycidylether Bisphenol F);
Step 2) said intensification need be confirmed according to the kind of epoxy resin and used solidifying agent, is generally 20～180 ℃; The present invention preferably keeps 10～15h at 80～110 ℃, and 120～150 ℃ keep 8～15h then, to accomplish solidification process.
In addition, carry out step 2) before, before soon resin dosing equipment will get into mould, use acetone and clean mould.Coat releasing agent then, wipe clean with gauze behind the 10min and coat releasing agent again, 3 times repeatedly.
The perfusion front mold places 40-60 ℃ of left and right sides baking oven to spend the night.
Concrete, the preparation method of modification aluminium nitride AlN filling epoxy resin matrix material according to the invention can carry out as follows:
1) adopt the method for plasma polymerization that superfine aluminium nitride is carried out modification, polymerization single polymerization monomer can be vinylformic acid (C
2H
4O
2) or pyrroles (C
2H
5N);
2) the modified superfine aluminium nitride AlN is mixed by proportioning with solidifying agent, toughner, resin.Carrying out vacuum outgas behind mechanical stirring, the ultra-sonic dispersion handles.To remove lower-boiling impurity that is mixed with in the resin etc.;
3) the resin priming by vacuum after will outgasing gets into the mould that is of a size of 180mm * 62mm * 4mm.Temperature programming removes mould and can obtain modification aluminium nitride AlN filling epoxy resin matrix material after solidifying.
Compare with existing aluminium nitride composite material, modified superfine aluminium nitride AlN filling epoxy resin matrix material of the present invention has following characteristic:
1) whole mixed with resin objects system is at filling process medium viscosity little (less than 600mPaS), and flowability is strong.Be convenient to carry out priming by vacuum;
2) solidification process is: 80～110 ℃ keep 10～15h, and 120～150 ℃ keep 8～15h then, can accomplish solidification process;
3) effectively improved the thermal conductivity of modification aluminium nitride AlN filling epoxy resin matrix material through the plasma polymerization modification, because the ligation of modified layer, the thermal vibration of aluminum nitride particle can more effectively be propagated in matrix; Toughner massfraction 10～20%, solidifying agent about 20%, resin about 50%, modified superfine aluminium nitride powder content were from 5～15% o'clock; Mechanical property significantly improves about 1.6～2.5 times under this matrix material normal temperature; Tensile strength reaches as high as 364Mpa; Improve about 1.7～2.4 times under liquid nitrogen (77k) temperature, low temperature stretched intensity reaches as high as 529Mpa.This matrix material thermal conductivity increases by 2～3 times than virgin resin, and thermal conductivity can reach 0.73Wm-1K-1, exceeds 2～3 times of virgin resin.
4) this series different components proportioning matrix material specific inductivity improves 15～25% than virgin resin, and insulation effect improves.
Description of drawings
Fig. 1 is a plasma organic polymer device synoptic diagram.A: vacuum fan interface; B: the monomer import that plasma polymerization is used; C: radio-frequency power supply; D: ruhmkorff coil; E: magnetic stirring apparatus; F: glass evacuated reaction tubes; G: magneton is used to stir powder.
Fig. 2 is the stereoscan photograph of modified superfine aluminium nitride AlN.
Fig. 3 is a plasma organic polymer pyrroles modified superfine aluminium nitride AlN infared spectrum.
Embodiment
Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.Specialize like nothing, the used material of the present invention is commercial.
Embodiment 1
The modification PREPARATION OF ALUMINUM NITRIDE POWDER that the present invention is used:
Concrete equipment is seen Fig. 1; The preparation process is referring to one Chinese patent application 200710117668.4, specifically preparation as follows: the superfine aluminium nitride about 0.5g is placed in the glass bend pipe reaction chamber F, guarantee that each several part is airtight after; Open vacuum fan, open radio-frequency power supply C.When the gas color was white in color in the reaction chamber F, the expression plasma film coating apparatus was in proper working order.Below the about 30pa of reaction tubes internal pressure this moment.Open the monomer import B that plasma polymerization is used, unscrew the monomeric under meter of connection, make flow of monomer at 10～20ml/min.Magneton G in the reaction tubes rotates under magnetic stirring apparatus E effect, fully contacts with reaction tubes interpolymer steam thereby make by aluminium nitride powder.60min is carried out in reaction.
In general, the above-mentioned reaction times can be decided according to the effect of actual plated film, and fast if grain color changes, proved response is fast, and the then short plated film time is just enough; If the aluminum nitride particle colour-change is slow, then need prolong the above-mentioned processing of plated film effluxion.The plasma modification can improve the wetting ability of aluminum nitride particle, and said hydrophilic raising has utilized following experiment showed, under identical plasma polymerization condition; Monocrystalline silicon piece is carried out modification, then little water droplet is dropped on the modification silicon chip, through microscopic examination water droplet and eyeglass contact angle; The result is for to reach more than 150 ° through silicon chip surface contact angle after the modification; Obviously, the material wetting ability effectively improves, in like manner; Behind the plasma polymerization of similarity condition, the wetting ability of modification aluminum nitride particle also improves greatly.
In addition, strength of joint is big between polymeric film and the aluminium nitride AlN matrix, and after handling with alcohol immersion and sonic oscillation, examination of infrared spectrum shows that also the position at organism peak, intensity do not have considerable change.
The particulate stereoscan photograph that obtains is seen Fig. 2;
When monomer was the pyrroles, its infared spectrum was seen Fig. 3.
Embodiment 2
Prepare modified superfine aluminium nitride AlN filling epoxy resin matrix material of the present invention by following step:
1) mould of 180mm * 62mm * 4mm is cleaned with acetone, smear releasing agent after, put in the baking oven 60 ℃ and spend the night for use.
2) taking by weighing resin DGEBF (diglycidylether Bisphenol F) 55g, solidifying agent DETD (diethyl toluene diamine) 20g, toughner IPBE{ (2-glycidyl-3-n-butoxy)-1-propyl ether } 15g, plasma polymerization pyrroles modified superfine aluminium nitride powder 10g be mixed in the 250ml Erlenmeyer flask, and vacuum outgas does not have bubble to emerge in resin.
3) vacuum perfusion process pours into said mould with above-mentioned resin, place baking oven after, 80 ℃ kept 10 hours, 120 ℃ kept 8 hours.Finish the back furnace cooling and take out this material.
Test result shows that the flexural strength of this matrix material is that 312MPa (normal temperature), thermal conductivity are 0.65Wm-1K
-1(normal temperature), specific inductivity are 3.35 (pure epoxy resin is 3.13).
Embodiment 3
Prepare modified superfine aluminium nitride AlN filling epoxy resin matrix material of the present invention by following step:
1) mould of 180mm * 62mm * 4mm is cleaned with acetone, smear releasing agent after, put in the baking oven 60 ℃ and spend the night for use.
2) taking by weighing resin DGEBF (diglycidylether Bisphenol F) 45g, solidifying agent DETD (diethyl toluene diamine) 25g, toughner IPBE{ (2-glycidyl-3-n-butoxy)-1-propyl ether } 10g, the acrylic acid modified superfine aluminium nitride powder 20g of plasma polymerization be mixed in the 250ml Erlenmeyer flask, and vacuum outgas does not have bubble to emerge in resin.
3) vacuum perfusion process pours into said mould with above-mentioned resin, place baking oven after, 90 ℃ kept 12 hours, 140 ℃ kept 15 hours.Finish the back furnace cooling and take out this material.
Test result shows, the flexural strength 320MPa of this matrix material (normal temperature), thermal conductivity 0.59Wm-1K-1 (normal temperature), specific inductivity 3.48.
Embodiment 4
Prepare modified superfine aluminium nitride AlN filling epoxy resin matrix material of the present invention by following step:
1) mould of 180mm * 62mm * 4mm is cleaned with acetone, smear releasing agent after, put in the baking oven 60 ℃ and spend the night for use.
2) taking by weighing resin DGEBF (diglycidylether Bisphenol F) 50g, solidifying agent DMTD (diformazan sulfenyl tolylene diamine) 20g, toughner IPBE{ (2-glycidyl-3-n-butoxy)-1-propyl ether } 20g, plasma polymerization pyrroles modified superfine aluminium nitride powder 10g be mixed in the 250ml Erlenmeyer flask, and vacuum outgas does not have bubble to emerge in resin.
3) vacuum perfusion process pours into said mould with above-mentioned resin, places baking oven, and 100 ℃ kept 12 hours, and 120 ℃ kept 12 hours.Finish the back furnace cooling and take out this material.
Test result shows, the flexural strength 364MPa of this matrix material (normal temperature), thermal conductivity 0.73Wm-1K-1 (normal temperature), specific inductivity 3.61.
Claims (10)
1. a modification aluminum nitride particle is characterized in that, is that the polymeric film by aluminum nitride particle and particle surface constitutes.
2. modification aluminum nitride particle as claimed in claim 1 is characterized in that, said polymeric film is vinylformic acid or pyrroles's film; Preferred pyrroles's film.
3. modification aluminum nitride particle as claimed in claim 1 is characterized in that, said modification aluminum nitride particle is prepared by the plasma polymerization method.
4. the matrix material like the arbitrary described modification aluminium nitride AlN filling epoxy resin of claim 1-3 is characterized in that, mainly is made up of epoxy resin and the above-mentioned modification aluminium nitride powder that wherein is mingled with; The mass ratio of said epoxy resin and modification aluminium nitride AlN is: 2～11: 1; Preferred 5: 1.
5. matrix material as claimed in claim 4 is characterized in that said matrix material also comprises toughner and solidifying agent.
6. matrix material as claimed in claim 5 is characterized in that, said epoxy resin is bisphenol F epoxy resin; Said toughner is one or more among DOP, DBP, TCP, the TPP, preferred IPBE; Said solidifying agent is one or more in aliphatic amide, aliphatic cyclic amine, aromatic amine, polymeric amide, acid anhydrides, resene, the tertiary amine, preferred DETD or DMTD.
7. like claim 5 or 6 described matrix materials, it is characterized in that said matrix material comprises following component: epoxy resin massfraction 45～55%, solidifying agent massfraction 15～25%, toughner massfraction 10～20%; Modified superfine aluminium nitride AlN massfraction 5～20%.
8. like claim 5 or 6 described matrix materials, it is characterized in that said matrix material comprises following component:, said toughner massfraction 10～20%, solidifying agent massfraction 20%, resin 50% remain and are the modified superfine aluminium nitride AlN.
9. like the preparation method of the arbitrary described matrix material of claim 4-8, it is characterized in that, may further comprise the steps:
1) modified superfine aluminium nitride AlN and solidifying agent, toughner, resin are mixed by proportioning, mixture is carried out vacuum outgas handle; Said vacuum outgas is preferably carried out as follows: under the vacuum state, and 20～60 ℃, the degassing 1～3h;
2) inject mould, heat up and solidify the demoulding then.
10. preparation method as claimed in claim 9 is characterized in that, said injection mould carries out under vacuum; Said intensification is solidified and carried out as follows: keep 10～15h at 80～110 ℃, 120～150 ℃ keep 8～15h then.
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Cited By (6)
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| CN102982981A (en) * | 2012-12-04 | 2013-03-20 | 江苏亚威变压器有限公司 | Epoxy resin insulating transformer |
| CN104403272A (en) * | 2014-11-21 | 2015-03-11 | 芜湖市宝艺游乐科技设备有限公司 | Modified aluminum nitride powder toughened epoxy resin composite material and manufacture method thereof |
| CN105694369A (en) * | 2016-04-06 | 2016-06-22 | 东华大学 | High-heat conductivity epoxy composite material and preparation method thereof |
| CN104262971B (en) * | 2014-08-28 | 2017-09-26 | 华南理工大学 | A kind of high heat conduction heat vulcanized silicone rubber composite and preparation method thereof |
| CN109535649A (en) * | 2018-10-23 | 2019-03-29 | 华北电力大学 | A kind of filler modified method and system of aluminium nitride for electrician's epoxy resin |
| CN111886216A (en) * | 2018-03-22 | 2020-11-03 | 3M创新有限公司 | Modified aluminum nitride particles and method for preparing same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102982981A (en) * | 2012-12-04 | 2013-03-20 | 江苏亚威变压器有限公司 | Epoxy resin insulating transformer |
| CN104262971B (en) * | 2014-08-28 | 2017-09-26 | 华南理工大学 | A kind of high heat conduction heat vulcanized silicone rubber composite and preparation method thereof |
| CN104403272A (en) * | 2014-11-21 | 2015-03-11 | 芜湖市宝艺游乐科技设备有限公司 | Modified aluminum nitride powder toughened epoxy resin composite material and manufacture method thereof |
| CN105694369A (en) * | 2016-04-06 | 2016-06-22 | 东华大学 | High-heat conductivity epoxy composite material and preparation method thereof |
| CN105694369B (en) * | 2016-04-06 | 2019-02-26 | 东华大学 | A kind of high thermal conductivity epoxy composite material and preparation method thereof |
| CN111886216A (en) * | 2018-03-22 | 2020-11-03 | 3M创新有限公司 | Modified aluminum nitride particles and method for preparing same |
| US11492495B2 (en) | 2018-03-22 | 2022-11-08 | 3M Innovative Properties Company | Modified aluminum nitride particles and methods of making the same |
| CN109535649A (en) * | 2018-10-23 | 2019-03-29 | 华北电力大学 | A kind of filler modified method and system of aluminium nitride for electrician's epoxy resin |
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