CN106832792A - A kind of insulated type epoxy resin composite material high of copper-clad plate silicon nitride comprising and preparation method thereof - Google Patents
A kind of insulated type epoxy resin composite material high of copper-clad plate silicon nitride comprising and preparation method thereof Download PDFInfo
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- CN106832792A CN106832792A CN201611255971.6A CN201611255971A CN106832792A CN 106832792 A CN106832792 A CN 106832792A CN 201611255971 A CN201611255971 A CN 201611255971A CN 106832792 A CN106832792 A CN 106832792A
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- epoxy resin
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- copper
- aluminium nitride
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
- C08L63/04—Epoxynovolacs
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/05—Polymer mixtures characterised by other features containing polymer components which can react with one another
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Abstract
The invention discloses a kind of insulated type epoxy resin composite material high of copper-clad plate silicon nitride comprising, and its preparation technology, characterized in that, with bisphenol A-type novolac epoxy resin, 2 methylimidazoles, silica, aluminium nitride, graphene oxide, ethylenediamine, PTS, dibutyl tin laurate, multi-walled carbon nano-tubes, calcium carbonate crystal whisker, benzyl dimethylamine, aluminum oxide, silicon nitride, antimony oxide etc. as raw material.The present invention carries out hydroxylating treatment with aluminium nitride as function phase to it, there is synergy between silica, obtains high-heat conductivity aluminium nitride ceramics, assigns resin good heat conductivility.Graphene oxide radius-thickness ratio is big, heat conduction master batch is formed after thermal reduction and forms thermal conducting path in the composite, it is carried out amino modified；The method for passing through chemical modification with poly- MTES (PTS), organosilicon is introduced into epoxy resin, and chemical modification epoxy resin product has excellent tensile strength and elongation at break, heat endurance.
Description
Technical field
The present invention relates to field of compound material, and in particular to a kind of insulated type epoxy resin high of copper-clad plate silicon nitride comprising
Composite, and its preparation technology.
Background technology
Copper-clad laminate abbreviation copper-clad plate, is electricity mainly for the manufacture of printed circuit board, telecommunications and instrument and meter
The basic material of sub- industry.The matrix resin of current copper-clad plate is based on bisphenol-type epoxy resin, but its heat resistance is poor, dielectric
Constant and dielectric loss are higher, it is impossible to meet the requirement of the high performance copper clad laminate used under high frequency condition.
Appoint section secret in its master thesis《The development of high-performance epoxy resin base copper-clad plate》In one text, with novolac
Resin is curing agent, with bisphenol A-type novolac epoxy resin and isocyanate modified epoxy resin as matrix resin, with silica
It is filler.Accelerator 2-methylimidazole, hard resin are dissolved in solvent butanone, 4-8h is stirred and cure, is blended into
Resin adhesive liquid, adds powder filler, makes its dispersed with high-shearing dispersion emulsifying machine, is prepared for glue.Glue is uniformly applied
It is put on E- glass fabrics, 5-8min is baked in 170 DEG C of high temperature ovens, takes out cooling and obtain prepreg；Will be partly solid
Change piece superposition and two sides is coated with Copper Foil, be placed in vacuum laminator and heat, pressurize, be pressed into copper-clad plate.But there is thermal conductivity
Can be not enough.
The content of the invention
The present invention solves the technical problem of a kind of insulated type epoxy resin high of copper-clad plate silicon nitride comprising of offer
Composite and its preparation technology, according to the technique prepare thermal conductivity of composite materials is high, good insulation preformance.
The technical problems to be solved by the invention are realized using following technical scheme：
Bisphenol A-type novolac epoxy resin 35-53,2-methylimidazole 8-13, silica 9-16, aluminium nitride 5-12, graphite oxide
Alkene 6-10, ethylenediamine 7-10, PTS 3-6, dibutyl tin laurate 2-4, multi-walled carbon nano-tubes 5-9, calcium carbonate crystal whisker 5-8,
Carboxyl terminated liquid polybutadiene rubber 3-5, benzyl dimethylamine 2-4, aluminum oxide 3-6, silicon nitride 4-7, antimony oxide 5-8, butanone,
KH550, ethanol, DMF, distilled water, appropriate NaOH solution.
A kind of preparation method of the insulated type epoxy resin composite material high of copper-clad plate silicon nitride comprising, it is characterised in that
Carry out according to the following steps：
A. in aluminium nitride 1:5-10 adds NaOH solution, is heated to 80-90 DEG C of stirring 1-2h, and centrifugation, alcohol are washed 3-5 times, 60-
2-4h is dried at 70 DEG C, hydroxylating aluminium nitride is obtained；1:3-5 adds silica, KH550, the ultrasonic disperse 3- at 50-60 DEG C
4h, alcohol is washed 3-5 times, is placed in Muffle furnace and is warmed up to 450-550 DEG C of insulation 1-2h, and 1700-1900 is warming up in nitrogen atmosphere
DEG C sintering 2-3h, be cooled to room temperature, grind；
B. in graphene oxide 1:3-5 adds DMF, mixes with ethylenediamine, ultrasonically treated 1-2h, and 3- is reacted at 110-130 DEG C
6h, filtering, alcohol wash water are washed 3-5 times, 70-90 DEG C of drying, are mixed with PTS, are warming up to 75-95 DEG C and are stirred, and 1:2-5 is added dropwise two
Dibutyl tin laurate, distilled water, isothermal reaction 3-5h add multi-walled carbon nano-tubes, sonic oscillation 1-2h；
C. calcium carbonate crystal whisker is dried into 2-3h, 1 at 110-130 DEG C:2-4 adds KH550, stirs, and pours into surface plate
In, after standing 5-10h at room temperature, 3-4h is vacuum dried at 110-130 DEG C, obtain surface modified calcium carbonate whisker；
D. bisphenol A-type novolac epoxy resin, carboxyl terminated liquid polybutadiene rubber, benzyl dimethylamine are mixed, is put into oil bath
In, the lower heating of stirring is warming up to 130-140 DEG C of reaction 3-4h, is down to room temperature, adds 2-4 times of acetone, stirs, and adds
Aluminum oxide, silicon nitride, antimony oxide, stir 3-5h, stand-by；
E. 2-methylimidazole is dissolved in butanone, is mixed with resulting material in a, b, c, d, stirred, be heated to 85-95
DEG C curing 4-8h, 2-4h is dried in 50-60 DEG C of vacuum drying oven, the deaeration 1-2h in 80-90 DEG C of vacuum drying chamber is down to room
Temperature, pours into mould, is put into platen-press and obtains composite in 120-200 DEG C of curing reaction 1-2h, natural cooling, the demoulding.
Reaction mechanism of the invention is as follows：
（1）Using hydridization filler aluminium nitride as function phase, hydroxylating treatment is carried out to its surface, add silica, the two is deposited
In synergy, the dense sintering of aluminium nitride ceramics, the high-ratio surface of aluminium nitride powder is promoted also to promote its densification process,
The aluminium nitride ceramics with high heat conductance is obtained, the good heat conduction of resin and processing characteristics is assigned, and excellent dielectric and resistance
Combustion performance.
（2）Graphene oxide has radius-thickness ratio high, heat conduction master batch is formed after thermal reduction and forms heat conduction in the composite
Path, is carried out amino modified with ethylenediamine to it, is successfully accessed amino, can significantly improve the calorifics and mechanical property of epoxy resin
Energy.
（3）The method for passing through chemical modification with poly- MTES (PTS), is prepared for silicon-modified epoxy tree
Fat, hydrolysate and the hydroxyl in epoxy resin of PTS react, and organosilicon are introduced into epoxy resin, chemical modification epoxy
Resin product has excellent tensile strength and elongation at break, heat endurance.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
The insulated type epoxy resin composite material high of a kind of copper-clad plate silicon nitride comprising, by the raw material of following weight parts (g)
It is obtained：
Bisphenol A-type novolac epoxy resin 53,2-methylimidazole 13, silica 16, aluminium nitride 12, graphene oxide 10, second two
Amine 10, PTS 6, dibutyl tin laurate 4, multi-walled carbon nano-tubes 9, calcium carbonate crystal whisker 8, carboxyl terminated liquid polybutadiene rubber
5, benzyl dimethylamine 4, aluminum oxide 6, silicon nitride 7, antimony oxide 8, butanone, KH550, ethanol, DMF, distilled water, NaOH solution are fitted
Amount.
A kind of preparation method of the insulated type epoxy resin composite material high of copper-clad plate silicon nitride comprising, it is characterised in that
Carry out according to the following steps：
A. in aluminium nitride 1:10 add NaOH solution, are heated to 80-90 DEG C of stirring 1h, and centrifugation, alcohol are washed at 3 times, 60-70 DEG C
2h is dried, hydroxylating aluminium nitride is obtained；1:5 add silica, KH550, the ultrasonic disperse 3h at 50-60 DEG C, alcohol to wash 3 times, put
In 450-550 DEG C of insulation 2h is warmed up in Muffle furnace, 1700-1900 DEG C of sintering 3h is warming up in nitrogen atmosphere, is cooled to room
Temperature, grinds；
B. in graphene oxide 1:5 add DMF, mix with ethylenediamine, ultrasonically treated 1h, and 3h, mistake are reacted at 110-130 DEG C
Filter, alcohol wash water are washed 3 times, and 80-90 DEG C of drying mixes with PTS, is warming up to 85-95 DEG C and stirs, and 1:5 are added dropwise tin dilaurate two
Butyl tin, distilled water, isothermal reaction 3h add multi-walled carbon nano-tubes, sonic oscillation 2h；
C. calcium carbonate crystal whisker is dried into 2h, 1 at 120-130 DEG C:4 add KH550, stir, and pour into surface plate, room
After the lower standing 5h of temperature, 3h is vacuum dried at 120-130 DEG C, obtains surface modified calcium carbonate whisker；
D. bisphenol A-type novolac epoxy resin, carboxyl terminated liquid polybutadiene rubber, benzyl dimethylamine are mixed, is put into oil bath
In, the lower heating of stirring is warming up to 130-140 DEG C of reaction 3h, is down to room temperature, adds 4 times of acetone, stirs, and adds oxidation
Aluminium, silicon nitride, antimony oxide, stir 3h, stand-by；
E. 2-methylimidazole is dissolved in butanone, is mixed with resulting material in a, b, c, d, stirred, be heated to 85-95
DEG C curing 6h, 4h is dried in 50-60 DEG C of vacuum drying oven, the deaeration 2h in 80-90 DEG C of vacuum drying chamber is down to room temperature,
Enter mould, be put into platen-press and obtain composite in 160-180 DEG C of curing reaction 2h, natural cooling, the demoulding.
Claims (2)
1. the insulated type epoxy resin composite material high of a kind of copper-clad plate silicon nitride comprising, it is characterised in that by following weight parts
Raw material be obtained：
Bisphenol A-type novolac epoxy resin 35-53,2-methylimidazole 8-13, silica 9-16, aluminium nitride 5-12, graphite oxide
Alkene 6-10, ethylenediamine 7-10, PTS 3-6, dibutyl tin laurate 2-4, multi-walled carbon nano-tubes 5-9, calcium carbonate crystal whisker 5-8,
Carboxyl terminated liquid polybutadiene rubber 3-5, benzyl dimethylamine 2-4, aluminum oxide 3-6, silicon nitride 4-7, antimony oxide 5-8, butanone,
KH550, ethanol, DMF, distilled water, appropriate NaOH solution.
2. the preparation of the insulated type epoxy resin composite material high of a kind of copper-clad plate silicon nitride comprising according to claim 1
Method, it is characterised in that carry out according to the following steps：
A. in aluminium nitride 1:5-10 adds NaOH solution, is heated to 80-90 DEG C of stirring 1-2h, and centrifugation, alcohol are washed 3-5 times, 60-
2-4h is dried at 70 DEG C, hydroxylating aluminium nitride is obtained；1:3-5 adds silica, KH550, the ultrasonic disperse 3- at 50-60 DEG C
4h, alcohol is washed 3-5 times, is placed in Muffle furnace and is warmed up to 450-550 DEG C of insulation 1-2h, and 1700-1900 is warming up in nitrogen atmosphere
DEG C sintering 2-3h, be cooled to room temperature, grind；
B. in graphene oxide 1:3-5 adds DMF, mixes with ethylenediamine, ultrasonically treated 1-2h, and 3- is reacted at 110-130 DEG C
6h, filtering, alcohol wash water are washed 3-5 times, 70-90 DEG C of drying, are mixed with PTS, are warming up to 75-95 DEG C and are stirred, and 1:2-5 is added dropwise two
Dibutyl tin laurate, distilled water, isothermal reaction 3-5h add multi-walled carbon nano-tubes, sonic oscillation 1-2h；
C. calcium carbonate crystal whisker is dried into 2-3h, 1 at 110-130 DEG C:2-4 adds KH550, stirs, and pours into surface plate
In, after standing 5-10h at room temperature, 3-4h is vacuum dried at 110-130 DEG C, obtain surface modified calcium carbonate whisker；
D. bisphenol A-type novolac epoxy resin, carboxyl terminated liquid polybutadiene rubber, benzyl dimethylamine are mixed, is put into oil bath
In, the lower heating of stirring is warming up to 130-140 DEG C of reaction 3-4h, is down to room temperature, adds 2-4 times of acetone, stirs, and adds
Aluminum oxide, silicon nitride, antimony oxide, stir 3-5h, stand-by；
E. 2-methylimidazole is dissolved in butanone, is mixed with resulting material in a, b, c, d, stirred, be heated to 85-95
DEG C curing 4-8h, 2-4h is dried in 50-60 DEG C of vacuum drying oven, the deaeration 1-2h in 80-90 DEG C of vacuum drying chamber is down to room
Temperature, pours into mould, is put into platen-press and obtains composite in 120-200 DEG C of curing reaction 1-2h, natural cooling, the demoulding.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611255971.6A CN106832792A (en) | 2016-12-30 | 2016-12-30 | A kind of insulated type epoxy resin composite material high of copper-clad plate silicon nitride comprising and preparation method thereof |
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| CN201611255971.6A CN106832792A (en) | 2016-12-30 | 2016-12-30 | A kind of insulated type epoxy resin composite material high of copper-clad plate silicon nitride comprising and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286582A (en) * | 2017-06-15 | 2017-10-24 | 铜陵安博电路板有限公司 | A kind of PCB heat conductive insulating baseplate materials of alumina carbon nanotube composite strengthening and preparation method thereof |
| CN108047654A (en) * | 2017-12-27 | 2018-05-18 | 福州大学 | Epoxy resin composite material being modified using graphene oxide-ceramic powder-liquid polyisoprene rubber and preparation method thereof |
| CN108314778A (en) * | 2018-02-28 | 2018-07-24 | 南方科技大学 | A kind of modified epoxy resin composite and preparation method thereof |
| CN114393891A (en) * | 2022-03-10 | 2022-04-26 | 康熹智能科技（东莞）有限公司 | High-thermal-conductivity copper-clad plate and preparation method thereof |
| CN114717500A (en) * | 2022-03-30 | 2022-07-08 | 青岛靓塔钢结构有限公司 | Processing technology of galvanized single-tube tower |
| CN115926381A (en) * | 2023-02-01 | 2023-04-07 | 江苏耀鸿电子有限公司 | Silicon dioxide filled epoxy resin copper-clad plate and preparation method thereof |
| CN116618647A (en) * | 2023-07-21 | 2023-08-22 | 安徽诺星航空科技有限公司 | Molybdenum-copper alloy composite material and preparation process thereof |
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| CN103214795A (en) * | 2013-04-07 | 2013-07-24 | 西安科技大学 | Composition of high-insulation heat conduction copper-clad plate and preparation method thereof |
| CN103694644A (en) * | 2013-12-30 | 2014-04-02 | 景旺电子科技(龙川)有限公司 | Epoxy resin composition, metal-based copper-clad plate and manufacturing method thereof |
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2016
- 2016-12-30 CN CN201611255971.6A patent/CN106832792A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103214795A (en) * | 2013-04-07 | 2013-07-24 | 西安科技大学 | Composition of high-insulation heat conduction copper-clad plate and preparation method thereof |
| CN103694644A (en) * | 2013-12-30 | 2014-04-02 | 景旺电子科技(龙川)有限公司 | Epoxy resin composition, metal-based copper-clad plate and manufacturing method thereof |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286582A (en) * | 2017-06-15 | 2017-10-24 | 铜陵安博电路板有限公司 | A kind of PCB heat conductive insulating baseplate materials of alumina carbon nanotube composite strengthening and preparation method thereof |
| CN108047654A (en) * | 2017-12-27 | 2018-05-18 | 福州大学 | Epoxy resin composite material being modified using graphene oxide-ceramic powder-liquid polyisoprene rubber and preparation method thereof |
| CN108314778A (en) * | 2018-02-28 | 2018-07-24 | 南方科技大学 | A kind of modified epoxy resin composite and preparation method thereof |
| CN108314778B (en) * | 2018-02-28 | 2021-01-05 | 南方科技大学 | Modified epoxy resin composite material and preparation method thereof |
| CN114393891A (en) * | 2022-03-10 | 2022-04-26 | 康熹智能科技（东莞）有限公司 | High-thermal-conductivity copper-clad plate and preparation method thereof |
| CN114393891B (en) * | 2022-03-10 | 2023-10-20 | 江苏高驰新材料科技有限公司 | High-heat-conductivity copper-clad plate and preparation method thereof |
| CN114717500A (en) * | 2022-03-30 | 2022-07-08 | 青岛靓塔钢结构有限公司 | Processing technology of galvanized single-tube tower |
| CN114717500B (en) * | 2022-03-30 | 2023-12-01 | 青岛靓塔钢结构有限公司 | Zinc-plating single-tube tower processing technology |
| CN115926381A (en) * | 2023-02-01 | 2023-04-07 | 江苏耀鸿电子有限公司 | Silicon dioxide filled epoxy resin copper-clad plate and preparation method thereof |
| CN116618647A (en) * | 2023-07-21 | 2023-08-22 | 安徽诺星航空科技有限公司 | Molybdenum-copper alloy composite material and preparation process thereof |
| CN116618647B (en) * | 2023-07-21 | 2023-10-13 | 安徽诺星航空科技有限公司 | Molybdenum-copper alloy composite material and preparation process thereof |
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