CN105199318B - A kind of preparation method of resin base heat-conductive copper-clad plate - Google Patents
A kind of preparation method of resin base heat-conductive copper-clad plate Download PDFInfo
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- CN105199318B CN105199318B CN201510615340.XA CN201510615340A CN105199318B CN 105199318 B CN105199318 B CN 105199318B CN 201510615340 A CN201510615340 A CN 201510615340A CN 105199318 B CN105199318 B CN 105199318B
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Abstract
The present invention relates to a kind of preparation method of resin base heat-conductive copper-clad plate, the preparation method includes the preparation of glue, resin coating, folds and accompany and suppress, wherein the raw material used in the preparation of the glue is：Isocyanate-based epoxy resin, o-cresol aldehyde type epoxy resin, the methylimidazole of 2 ethyl 4, dicyandiamide, bortz powder, golden red stone flour, lithium hydroxide, toluene diphenyl phosphate, montmorillonite, vermiculite, antimony oxide, alkenyl succinic acid copper, benzophenone, silica, dimethyldichlorosilane and solvent.A kind of preparation method of resin base heat-conductive copper-clad plate provided by the invention, the copper-clad plate prepared by this method have good thermal conductivity and thermal shock resistance.
Description
Technical field
The invention belongs to field of electronic materials, more particularly to a kind of preparation method of resin base heat-conductive copper-clad plate.
Background technology
Now, heat-conductive copper-clad plate answering in fields such as LED illumination, LED television, power supply board, motor vehicle assembly, frequency-variable modules
Risen with just gradual.Heat-conductive copper-clad plate be while electrical insulating property is retained on improve its capacity of heat transmission, usual heat-conductive copper-clad plate
Heat conduction metal-based copper-clad plate and the major class of resin base heat-conductive copper-clad plate two can be divided into.Wherein with heat conduction in resin base heat-conductive copper-clad plate
The use of CEM-3 resin base copper-clad plates is most.Heat conduction CEM-3 resin base copper-clad plates, there is higher intensity, good insulating properties
Energy and excellent processability, while its thermal conductivity is compared with higher than common CEM-3 resins base copper-clad plate.However, with LED illumination
Use power increasing Deng field, and the application of frequency-variable module is more and more wider, the heat conduction to resin base heat-conductive copper-clad plate
Performance proposes higher requirement, so not only can further improve the heat-sinking capability of product, reduces the aging of product, while also rise
To the effect of energy-conservation and the service life for extending product.
The content of the invention
Technical problems to be solved are：For at least one to solve the above problems, there is provided a kind of resin base heat conduction is covered
The preparation method of copper coin.
Technical scheme：In order to solve the above problems, the invention provides a kind of preparation method of resin base heat-conductive copper-clad plate,
The step of preparation method, is as follows：
（1）The preparation of glue：Each raw material is weighed according to constant weight number：Isocyanate-based epoxy resin, o-cresol
Aldehyde type epoxy resin, 2-ethyl-4-methylimidazole, dicyandiamide, bortz powder, golden red stone flour, lithium hydroxide, toluene phosphoric acid hexichol
Ester, montmorillonite, vermiculite, antimony oxide, alkenyl succinic acid copper, benzophenone, silica, dimethyldichlorosilane and molten
Agent；Bortz powder in raw material, golden red stone flour, montmorillonite, vermiculite, antimony oxide and silica are put into ball mill,
250 mesh sieves are crossed after 3 ~ 10h of ball milling, are then mixed evenly with remaining raw material, it is standby；
（2）Resin is coated with：Glass-fiber-fabric is immersed into step（1）In in prepared glue, be then dried to prepreg；
（3）It is folded to match somebody with somebody：By step（2）In obtained prepreg carry out mutually folded being assigned to certain predetermined thickness；
（4）Compacting：By step（3）The middle prepreg after folded match somebody with somebody is overlapped with copper foil, so and is placed in vacuum hotpressing
In machine, required copper-clad plate is pressed into.
Further, the step（1）In each raw material be according to parts by weight：Isocyanate-based 45 ~ 70 parts of epoxy resin,
50 ~ 80 parts of o-cresol aldehyde type epoxy resin, 1 ~ 4 part of 2-ethyl-4-methylimidazole, 35 ~ 60 parts of dicyandiamide, bortz powder 2 ~ 12
Part, 1 ~ 8 part of golden red stone flour, 2 ~ 6 parts of lithium hydroxide, 4 ~ 15 parts of toluene diphenyl phosphate, 2 ~ 10 parts of montmorillonite, 1 ~ 7 part of vermiculite, three
Aoxidize 2 ~ 9 parts of two antimony, 1 ~ 6 part of alkenyl succinic acid copper, 1 ~ 5 part of benzophenone, 2 ~ 6 parts of silica, dimethyldichlorosilane 2 ~ 8
20 ~ 40 parts of part and solvent.
Further, the step（1）In each raw material be according to parts by weight：Isocyanate-based 45 ~ 60 parts of epoxy resin,
65 ~ 80 parts of o-cresol aldehyde type epoxy resin, 2 ~ 4 parts of 2-ethyl-4-methylimidazole, 40 ~ 60 parts of dicyandiamide, bortz powder 4 ~ 12
Part, 3 ~ 8 parts of golden red stone flour, 4 ~ 6 parts of lithium hydroxide, 6 ~ 15 parts of toluene diphenyl phosphate, 5 ~ 10 parts of montmorillonite, 3 ~ 7 parts of vermiculite, three
Aoxidize 2 ~ 7 parts of two antimony, 1 ~ 5 part of alkenyl succinic acid copper, 1 ~ 4 part of benzophenone, 2 ~ 5 parts of silica, dimethyldichlorosilane 2 ~ 6
20 ~ 35 parts of part and solvent.
Further, the step（1）In each raw material be according to parts by weight：Isocyanate-based 54 parts of epoxy resin,
70 parts of o-cresol aldehyde type epoxy resin, 3 parts of 2-ethyl-4-methylimidazole, 52 parts of dicyandiamide, 8 parts of bortz powder, golden red stone flour
6 parts, 5 parts of lithium hydroxide, 12 parts of toluene diphenyl phosphate, 7 parts of montmorillonite, 5 parts of vermiculite, 4 parts of antimony oxide, alkenyl succinic acid
28 parts of 2 parts of copper, 3 parts of benzophenone, 4 parts of silica, 3 parts of dimethyldichlorosilane and solvent.
Further, the solvent is at least one of acetone, propane diols, ethylene glycol monomethyl ether and dimethylbenzene.
Further, the step（3）Described in prepreg to carry out the mutually folded predetermined thickness matched somebody with somebody be 20 ~ 120um.
Further, the step（4）Described in condition in vacuum hotpressing machine be：210 DEG C of press temperature, 35MPa
Pressing pressure.
The invention has the advantages that：The thermal conductivity of copper-clad plate prepared by the present invention is 1.5 ~ 2.1 W/（m•k）,
It is significantly higher than commercially available epoxy resin copper-clad plate, illustrates that the copper-clad plate prepared by the present invention has good thermal conductivity, in addition, surveys
Resistance to sudden heating prepared by the test result display present invention is more preferably.
Embodiment
For a further understanding of the present invention, invention preferred embodiment is described with reference to embodiment, but should
Work as understanding, these descriptions are simply further explanation the features and advantages of the present invention, rather than the limit to the claims in the present invention
System.
Embodiment 1
A kind of preparation method of resin base heat-conductive copper-clad plate, it is characterised in that as follows the step of the preparation method：
（1）The preparation of glue：Each raw material is weighed according to constant weight number：Isocyanate-based 45 parts of epoxy resin, adjacent first
50 parts of base phenol aldehyde type epoxy resin, 1 part of 2-ethyl-4-methylimidazole, 35 parts of dicyandiamide, 2 parts of bortz powder, 1 part of golden red stone flour,
2 parts of lithium hydroxide, 4 parts of toluene diphenyl phosphate, 2 parts of montmorillonite, 1 part of vermiculite, 2 parts of antimony oxide, alkenyl succinic acid copper 1
Part, 1 part of benzophenone, 2 parts of silica, 2 parts of dimethyldichlorosilane and 20 parts of acetone solvent；By the diamond in raw material
In powder, golden red stone flour, montmorillonite, vermiculite, antimony oxide and silica input ball mill, 250 mesh sieves are crossed after ball milling 3h, so
It is mixed evenly afterwards with remaining raw material, it is standby；
（2）Resin is coated with：Glass-fiber-fabric is immersed into step（1）In in prepared glue, be then dried to prepreg；
（3）It is folded to match somebody with somebody：By step（2）In obtained prepreg carry out mutually folded being assigned to 20um thickness；
（4）Compacting：By step（3）The middle prepreg after folded match somebody with somebody is overlapped with copper foil, so and is placed in vacuum hotpressing
In machine, required copper-clad plate is pressed under 210 DEG C of press temperature, 35MPa pressing pressure.
Embodiment 2
A kind of preparation method of resin base heat-conductive copper-clad plate, it is characterised in that as follows the step of the preparation method：
（1）The preparation of glue：Each raw material is weighed according to constant weight number：Isocyanate-based 70 parts of epoxy resin, adjacent first
80 parts of base phenol aldehyde type epoxy resin, 4 parts of 2-ethyl-4-methylimidazole, 60 parts of dicyandiamide, 12 parts of bortz powder, golden red stone flour 8
Part, 6 parts of lithium hydroxide, 15 parts of toluene diphenyl phosphate, 10 parts of montmorillonite, 7 parts of vermiculite, 9 parts of antimony oxide, alkenyl succinic acid
40 parts of 6 parts of copper, 5 parts of benzophenone, 6 parts of silica, 8 parts of dimethyldichlorosilane and propylene glycol solvent；By the gold in raw material
In emery, golden red stone flour, montmorillonite, vermiculite, antimony oxide and silica input ball mill, 250 mesh are crossed after ball milling 10h
Sieve, is then mixed evenly with remaining raw material, standby；
（2）Resin is coated with：Glass-fiber-fabric is immersed into step（1）In in prepared glue, be then dried to prepreg；
（3）It is folded to match somebody with somebody：By step（2）In obtained prepreg carry out mutually folded being assigned to 120um thickness；
（4）Compacting：By step（3）The middle prepreg after folded match somebody with somebody is overlapped with copper foil, so and is placed in vacuum hotpressing
In machine, required copper-clad plate is pressed under 210 DEG C of press temperature, 35MPa pressing pressure.
Embodiment 3
A kind of preparation method of resin base heat-conductive copper-clad plate, it is characterised in that as follows the step of the preparation method：
（1）The preparation of glue：Each raw material is weighed according to constant weight number：Isocyanate-based 58 parts of epoxy resin, adjacent first
65 parts of base phenol aldehyde type epoxy resin, 3 parts of 2-ethyl-4-methylimidazole, 47 parts of dicyandiamide, 7 parts of bortz powder, 4 parts of golden red stone flour,
4 parts of lithium hydroxide, 10 parts of toluene diphenyl phosphate, 6 parts of montmorillonite, 4 parts of vermiculite, 5 parts of antimony oxide, alkenyl succinic acid copper 3
Part, 3 parts of benzophenone, 4 parts of silica, 5 parts of dimethyldichlorosilane and 30 parts of ethylene glycol monomethyl ether solvent；By the gold in raw material
In emery, golden red stone flour, montmorillonite, vermiculite, antimony oxide and silica input ball mill, 250 mesh are crossed after ball milling 6h
Sieve, is then mixed evenly with remaining raw material, standby；
（2）Resin is coated with：Glass-fiber-fabric is immersed into step（1）In in prepared glue, be then dried to prepreg；
（3）It is folded to match somebody with somebody：By step（2）In obtained prepreg carry out mutually folded being assigned to 70um thickness；
（4）Compacting：By step（3）The middle prepreg after folded match somebody with somebody is overlapped with copper foil, so and is placed in vacuum hotpressing
In machine, required copper-clad plate is pressed under 210 DEG C of press temperature, 35MPa pressing pressure.
Embodiment 4
A kind of preparation method of resin base heat-conductive copper-clad plate, it is characterised in that as follows the step of the preparation method：
（1）The preparation of glue：Each raw material is weighed according to constant weight number：Isocyanate-based 54 parts of epoxy resin, adjacent first
70 parts of base phenol aldehyde type epoxy resin, 3 parts of 2-ethyl-4-methylimidazole, 52 parts of dicyandiamide, 8 parts of bortz powder, 6 parts of golden red stone flour,
5 parts of lithium hydroxide, 12 parts of toluene diphenyl phosphate, 7 parts of montmorillonite, 5 parts of vermiculite, 4 parts of antimony oxide, alkenyl succinic acid copper 2
Part, 3 parts of benzophenone, 4 parts of silica, 3 parts of dimethyldichlorosilane and 28 parts of xylene solvent；By the diamond in raw material
In powder, golden red stone flour, montmorillonite, vermiculite, antimony oxide and silica input ball mill, 250 mesh sieves are crossed after ball milling 8h, so
It is mixed evenly afterwards with remaining raw material, it is standby；
（2）Resin is coated with：Glass-fiber-fabric is immersed into step（1）In in prepared glue, be then dried to prepreg；
（3）It is folded to match somebody with somebody：By step（2）In obtained prepreg carry out mutually folded being assigned to 8um thickness；
（4）Compacting：By step（3）The middle prepreg after folded match somebody with somebody is overlapped with copper foil, so and is placed in vacuum hotpressing
In machine, required copper-clad plate is pressed under 210 DEG C of press temperature, 35MPa pressing pressure.
Embodiment 5
A kind of preparation method of resin base heat-conductive copper-clad plate, it is characterised in that as follows the step of the preparation method：
（1）The preparation of glue：Each raw material is weighed according to constant weight number：Isocyanate-based 60 parts of epoxy resin, adjacent first
65 parts of base phenol aldehyde type epoxy resin, 2 parts of 2-ethyl-4-methylimidazole, 40 parts of dicyandiamide, 4 parts of bortz powder, 3 parts of golden red stone flour,
4 parts of lithium hydroxide, 6 parts of toluene diphenyl phosphate, 5 parts of montmorillonite, 3 parts of vermiculite, 7 parts of antimony oxide, alkenyl succinic acid copper 5
Part, 4 parts of benzophenone, 5 parts of silica, 6 parts of dimethyldichlorosilane and 35 parts of propylene glycol solvent；By the diamond in raw material
In powder, golden red stone flour, montmorillonite, vermiculite, antimony oxide and silica input ball mill, 250 mesh sieves are crossed after ball milling 7h, so
It is mixed evenly afterwards with remaining raw material, it is standby；
（2）Resin is coated with：Glass-fiber-fabric is immersed into step（1）In in prepared glue, be then dried to prepreg；
（3）It is folded to match somebody with somebody：By step（2）In obtained prepreg carry out mutually folded being assigned to 60um thickness；
（4）Compacting：By step（3）The middle prepreg after folded match somebody with somebody is overlapped with copper foil, so and is placed in vacuum hotpressing
In machine, required copper-clad plate is pressed under 210 DEG C of press temperature, 35MPa pressing pressure.
Performance test
Following table is to use ASTM-D5470 as the performance test of the copper-clad plate prepared by above example, wherein heat conductivility
Method.In order to embody the performance of the copper-clad plate prepared by the present invention, surveyed as a comparison case with commercially available epoxy resin copper-clad plate
Examination compares, and test result refers to following table：
As can be seen here, the thermal conductivity of the copper-clad plate prepared by the present invention is 1.5 ~ 2.1 W/（m•k）, it is significantly higher than commercially available
Epoxy resin copper-clad plate, illustrate that the copper-clad plate prepared by the present invention has good thermal conductivity, in addition, test result shows this hair
Bright prepared resistance to sudden heating is more preferably.
Claims (6)
1. a kind of preparation method of resin base heat-conductive copper-clad plate, it is characterised in that as follows the step of the preparation method：
（1）The preparation of glue：Each raw material is weighed according to constant weight number：Isocyanate-based 45 ~ 70 parts of epoxy resin, adjacent methyl
50 ~ 80 parts of phenol aldehyde type epoxy resin, 1 ~ 4 part of 2-ethyl-4-methylimidazole, 35 ~ 60 parts of dicyandiamide, 2 ~ 12 parts of bortz powder, gold
Red 1 ~ 8 part of stone flour, 2 ~ 6 parts of lithium hydroxide, 4 ~ 15 parts of toluene diphenyl phosphate, 2 ~ 10 parts of montmorillonite, 1 ~ 7 part of vermiculite, three oxidations
Two 2 ~ 9 parts of antimony, 1 ~ 6 part of alkenyl succinic acid copper, 1 ~ 5 part of benzophenone, 2 ~ 6 parts of silica, 2 ~ 8 parts of dimethyldichlorosilane and
20 ~ 40 parts of solvent；Bortz powder in raw material, golden red stone flour, montmorillonite, vermiculite, antimony oxide and silica are put into
In ball mill, 250 mesh sieves are crossed after 3 ~ 10h of ball milling, are then mixed evenly with remaining raw material, it is standby；
（2）Resin is coated with：Glass-fiber-fabric is immersed into step（1）In in prepared glue, be then dried to prepreg；
（3）It is folded to match somebody with somebody：By step（2）In obtained prepreg carry out mutually folded being assigned to certain predetermined thickness；
（4）Compacting：By step（3）The middle prepreg after folded match somebody with somebody is overlapped with copper foil, so and is placed in vacuum hotpressing machine,
It is pressed into required copper-clad plate.
A kind of 2. preparation method of resin base heat-conductive copper-clad plate according to claim 1, it is characterised in that the step（1）
In each raw material be according to parts by weight：Isocyanate-based 45 ~ 60 parts of epoxy resin, 65 ~ 80 parts of o-cresol aldehyde type epoxy resin,
2 ~ 4 parts of 2-ethyl-4-methylimidazole, 40 ~ 60 parts of dicyandiamide, 4 ~ 12 parts of bortz powder, 3 ~ 8 parts of golden red stone flour, lithium hydroxide 4 ~ 6
Part, 6 ~ 15 parts of toluene diphenyl phosphate, 5 ~ 10 parts of montmorillonite, 3 ~ 7 parts of vermiculite, 2 ~ 7 parts of antimony oxide, alkenyl succinic acid copper 1 ~
20 ~ 35 parts of 5 parts, 1 ~ 4 part of benzophenone, 2 ~ 5 parts of silica, 2 ~ 6 parts of dimethyldichlorosilane and solvent.
A kind of 3. preparation method of resin base heat-conductive copper-clad plate according to claim 1, it is characterised in that the step（1）
In each raw material be according to parts by weight：Isocyanate-based 54 parts of epoxy resin, 70 parts of o-cresol aldehyde type epoxy resin, 2- second
3 parts of base -4-methylimidazole, 52 parts of dicyandiamide, 8 parts of bortz powder, 6 parts of golden red stone flour, 5 parts of lithium hydroxide, toluene phosphoric acid hexichol
12 parts of ester, 7 parts of montmorillonite, 5 parts of vermiculite, 4 parts of antimony oxide, 2 parts of alkenyl succinic acid copper, 3 parts of benzophenone, silica 4
28 parts of part, 3 parts of dimethyldichlorosilane and solvent.
4. the preparation method of a kind of resin base heat-conductive copper-clad plate according to claim 1, it is characterised in that the solvent is
At least one of acetone, propane diols, ethylene glycol monomethyl ether and dimethylbenzene.
A kind of 5. preparation method of resin base heat-conductive copper-clad plate according to any one of Claims 1-4, it is characterised in that institute
State step（3）Described in prepreg to carry out the mutually folded predetermined thickness matched somebody with somebody be 20 ~ 120um.
A kind of 6. preparation method of resin base heat-conductive copper-clad plate according to any one of Claims 1-4, it is characterised in that institute
State step（4）Described in condition in vacuum hotpressing machine be：210 DEG C of press temperature, 35MPa pressing pressure.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510615340.XA CN105199318B (en) | 2015-09-24 | 2015-09-24 | A kind of preparation method of resin base heat-conductive copper-clad plate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510615340.XA CN105199318B (en) | 2015-09-24 | 2015-09-24 | A kind of preparation method of resin base heat-conductive copper-clad plate |
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| CN105199318A CN105199318A (en) | 2015-12-30 |
| CN105199318B true CN105199318B (en) | 2017-12-26 |
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| CN102911479B (en) * | 2012-11-14 | 2015-01-07 | 江苏华海诚科新材料有限公司 | High heat conduction epoxy resin composition applicable to fully wrapped devices and preparation method |
| CN103694644B (en) * | 2013-12-30 | 2015-11-04 | 景旺电子科技(龙川)有限公司 | A kind of composition epoxy resin, metal-based copper-clad plate and preparation method thereof |
| CN104448718B (en) * | 2014-12-08 | 2017-02-22 | 陕西生益科技有限公司 | Resin composition and application thereof |
| CN104760368B (en) * | 2015-04-14 | 2016-08-24 | 东华大学 | A kind of Study of Epoxy-Imide Resin matrix copper-clad laminate and preparation method thereof |
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