CN105199318A - Preparation method of resin-based heat conduction copper-clad plate - Google Patents
Preparation method of resin-based heat conduction copper-clad plate Download PDFInfo
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- CN105199318A CN105199318A CN201510615340.XA CN201510615340A CN105199318A CN 105199318 A CN105199318 A CN 105199318A CN 201510615340 A CN201510615340 A CN 201510615340A CN 105199318 A CN105199318 A CN 105199318A
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Abstract
The invention relates to a preparation method of a resin-based heat conduction copper-clad plate. The preparation method includes the steps of adhesive liquid preparing, resin coating, overlying and pressing. Raw materials used in adhesive liquid preparing comprise isocyanate epoxy resin, o-cresol-formaldehyde epoxy resin, 2-ethyl-4-methylimidazole, dicyandiamide, diamond powder, rutile powder, lithium hydroxide, cresyl diphenyl phosphate, montmorillonite, vermiculite, antimonous oxide, alkenyl succinic acid copper, benzophenone, silica, dimethyldichlorosilance and solvent. By means of the preparation method for the resin-based heat conduction copper-clad plate, the prepared copper-clad plate has good thermal conductance and thermal shock resistance.
Description
Technical field
The invention belongs to field of electronic materials, particularly relate to a kind of preparation method of resin base heat-conductive copper-clad plate.
Background technology
Now, heat-conductive copper-clad plate rises just gradually in the application in the fields such as LED illumination, LED television, power supply board, motor vehicle assembly, frequency-variable module.Heat-conductive copper-clad plate be retaining electrical insulating property while on improve its capacity of heat transmission, usual heat-conductive copper-clad plate can be divided into the large class of heat conduction metal-based copper-clad plate and resin base heat-conductive copper-clad plate two.Wherein maximum with the use of heat conduction CEM-3 resin base copper-clad plate in resin base heat-conductive copper-clad plate.The copper-clad plate of heat conduction CEM-3 resin base, has higher intensity, good insulating property and excellent processibility, and its thermal conductivity is comparatively higher than the copper-clad plate of common CEM-3 resin base simultaneously.But, along with the use power in the fields such as LED illumination is increasing, and the application of frequency-variable module is more and more wider, the heat conductivility of resin base heat-conductive copper-clad plate is had higher requirement, so not only can further improve the heat-sinking capability of product, reduce the aging of product, also play effect that the is energy-conservation and work-ing life of prolongation product simultaneously.
Summary of the invention
The technical problem solved is: in order at least one solved the problem, and provides a kind of preparation method of resin base heat-conductive copper-clad plate.
Technical scheme: in order to solve the problem, the invention provides a kind of preparation method of resin base heat-conductive copper-clad plate, the step of this preparation method is as follows:
(1) preparation of glue: take each raw material according to certainweight number: isocyanate-based epoxy resin, o-cresol aldehyde type epoxy resin, 2-ethyl-4-methylimidazole, Dyhard RU 100, bortz powder, golden red stone flour, lithium hydroxide, toluene diphenyl phosphate, polynite, vermiculite, antimonous oxide, alkenyl succinic acid copper, benzophenone, silicon-dioxide, dimethyldichlorosilane(DMCS) and solvent; Bortz powder in raw material, golden red stone flour, polynite, vermiculite, antimonous oxide and silicon-dioxide are dropped in ball mill, after ball milling 3 ~ 10h, cross 250 mesh sieves, then carry out mixing and stirring with remaining raw material, for subsequent use;
(2) resin-coated: glass-fiber-fabric to be immersed in glue prepared in step (1), be then dried to prepreg;
(3) foldedly to join: the prepreg obtained in step (2) is carried out mutually foldedly be assigned to certain pre-determined thickness;
(4) suppress: the prepreg in step (3) after folded joining is carried out superimposed with Copper Foil, right be placed in vacuum hotpressing machine, be pressed into required copper-clad plate.
Further, in described step (1), each raw material according to parts by weight is: isocyanate-based epoxy resin 45 ~ 70 parts, o-cresol aldehyde type epoxy resin 50 ~ 80 parts, 2-ethyl-4-methylimidazole 1 ~ 4 part, Dyhard RU 100 35 ~ 60 parts, bortz powder 2 ~ 12 parts, golden red stone flour 1 ~ 8 part, lithium hydroxide 2 ~ 6 parts, toluene diphenyl phosphate 4 ~ 15 parts, polynite 2 ~ 10 parts, vermiculite 1 ~ 7 part, antimonous oxide 2 ~ 9 parts, alkenyl succinic acid copper 1 ~ 6 part, benzophenone 1 ~ 5 part, silicon-dioxide 2 ~ 6 parts, dimethyldichlorosilane(DMCS) 2 ~ 8 parts and solvent 20 ~ 40 parts.
Further, in described step (1), each raw material according to parts by weight is: isocyanate-based epoxy resin 45 ~ 60 parts, o-cresol aldehyde type epoxy resin 65 ~ 80 parts, 2-ethyl-4-methylimidazole 2 ~ 4 parts, Dyhard RU 100 40 ~ 60 parts, bortz powder 4 ~ 12 parts, golden red stone flour 3 ~ 8 parts, lithium hydroxide 4 ~ 6 parts, toluene diphenyl phosphate 6 ~ 15 parts, polynite 5 ~ 10 parts, vermiculite 3 ~ 7 parts, antimonous oxide 2 ~ 7 parts, alkenyl succinic acid copper 1 ~ 5 part, benzophenone 1 ~ 4 part, silicon-dioxide 2 ~ 5 parts, dimethyldichlorosilane(DMCS) 2 ~ 6 parts and solvent 20 ~ 35 parts.
Further, in described step (1), each raw material according to parts by weight is: isocyanate-based epoxy resin 54 parts, o-cresol aldehyde type epoxy resin 70 parts, 2-ethyl-4-methylimidazole 3 parts, Dyhard RU 100 52 parts, bortz powder 8 parts, golden red stone flour 6 parts, lithium hydroxide 5 parts, toluene diphenyl phosphate 12 parts, polynite 7 parts, vermiculite 5 parts, antimonous oxide 4 parts, alkenyl succinic acid copper 2 parts, benzophenone 3 parts, silicon-dioxide 4 parts, dimethyldichlorosilane(DMCS) 3 parts and solvent 28 parts.
Further, described solvent is at least one in acetone, propylene glycol, ethylene glycol monomethyl ether and dimethylbenzene.
Further, prepreg described in described step (3) carries out folded pre-determined thickness of joining mutually is 20 ~ 120um.
Further, the condition in vacuum hotpressing machine described in described step (4) is: the press temperature of 210 DEG C, the pressing pressure of 35MPa.
The present invention has following beneficial effect: the thermal conductivity of the copper-clad plate prepared by the present invention is 1.5 ~ 2.1W/(mk), be 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, the resistance to sudden heating that shows prepared by the present invention of test result is better.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, invention preferred embodiment is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
Embodiment 1
A preparation method for resin base heat-conductive copper-clad plate, is characterized in that the step of this preparation method is as follows:
(1) preparation of glue: take each raw material according to certainweight number: isocyanate-based epoxy resin 45 parts, o-cresol aldehyde type epoxy resin 50 parts, 2-ethyl-4-methylimidazole 1 part, Dyhard RU 100 35 parts, bortz powder 2 parts, golden red stone flour 1 part, lithium hydroxide 2 parts, toluene diphenyl phosphate 4 parts, polynite 2 parts, vermiculite 1 part, antimonous oxide 2 parts, alkenyl succinic acid copper 1 part, benzophenone 1 part, silicon-dioxide 2 parts, dimethyldichlorosilane(DMCS) 2 parts and acetone solvent 20 parts; Bortz powder in raw material, golden red stone flour, polynite, vermiculite, antimonous oxide and silicon-dioxide are dropped in ball mill, after ball milling 3h, cross 250 mesh sieves, then carry out mixing and stirring with remaining raw material, for subsequent use;
(2) resin-coated: glass-fiber-fabric to be immersed in glue prepared in step (1), be then dried to prepreg;
(3) foldedly to join: the prepreg obtained in step (2) is carried out mutually folded to be assigned to 20um thick;
(4) suppress: the prepreg in step (3) after folded joining is carried out superimposed with Copper Foil, right be placed in vacuum hotpressing machine, in the press temperature of 210 DEG C, under the pressing pressure of 35MPa, be pressed into required copper-clad plate.
Embodiment 2
A preparation method for resin base heat-conductive copper-clad plate, is characterized in that the step of this preparation method is as follows:
(1) preparation of glue: take each raw material according to certainweight number: isocyanate-based epoxy resin 70 parts, o-cresol aldehyde type epoxy resin 80 parts, 2-ethyl-4-methylimidazole 4 parts, Dyhard RU 100 60 parts, bortz powder 12 parts, golden red stone flour 8 parts, lithium hydroxide 6 parts, toluene diphenyl phosphate 15 parts, polynite 10 parts, vermiculite 7 parts, antimonous oxide 9 parts, alkenyl succinic acid copper 6 parts, benzophenone 5 parts, silicon-dioxide 6 parts, dimethyldichlorosilane(DMCS) 8 parts and propylene glycol solvent 40 parts, bortz powder in raw material, golden red stone flour, polynite, vermiculite, antimonous oxide and silicon-dioxide are dropped in ball mill, after ball milling 10h, cross 250 mesh sieves, then carry out mixing and stirring with remaining raw material, for subsequent use,
(2) resin-coated: glass-fiber-fabric to be immersed in glue prepared in step (1), be then dried to prepreg;
(3) foldedly to join: the prepreg obtained in step (2) is carried out mutually folded to be assigned to 120um thick;
(4) suppress: the prepreg in step (3) after folded joining is carried out superimposed with Copper Foil, right be placed in vacuum hotpressing machine, in the press temperature of 210 DEG C, under the pressing pressure of 35MPa, be pressed into required copper-clad plate.
Embodiment 3
A preparation method for resin base heat-conductive copper-clad plate, is characterized in that the step of this preparation method is as follows:
(1) preparation of glue: take each raw material according to certainweight number: isocyanate-based epoxy resin 58 parts, o-cresol aldehyde type epoxy resin 65 parts, 2-ethyl-4-methylimidazole 3 parts, Dyhard RU 100 47 parts, bortz powder 7 parts, golden red stone flour 4 parts, lithium hydroxide 4 parts, toluene diphenyl phosphate 10 parts, polynite 6 parts, vermiculite 4 parts, antimonous oxide 5 parts, alkenyl succinic acid copper 3 parts, benzophenone 3 parts, silicon-dioxide 4 parts, dimethyldichlorosilane(DMCS) 5 parts and ethylene glycol monomethyl ether solvent 30 parts, bortz powder in raw material, golden red stone flour, polynite, vermiculite, antimonous oxide and silicon-dioxide are dropped in ball mill, after ball milling 6h, cross 250 mesh sieves, then carry out mixing and stirring with remaining raw material, for subsequent use,
(2) resin-coated: glass-fiber-fabric to be immersed in glue prepared in step (1), be then dried to prepreg;
(3) foldedly to join: the prepreg obtained in step (2) is carried out mutually folded to be assigned to 70um thick;
(4) suppress: the prepreg in step (3) after folded joining is carried out superimposed with Copper Foil, right be placed in vacuum hotpressing machine, in the press temperature of 210 DEG C, under the pressing pressure of 35MPa, be pressed into required copper-clad plate.
Embodiment 4
A preparation method for resin base heat-conductive copper-clad plate, is characterized in that the step of this preparation method is as follows:
(1) preparation of glue: take each raw material according to certainweight number: isocyanate-based epoxy resin 54 parts, o-cresol aldehyde type epoxy resin 70 parts, 2-ethyl-4-methylimidazole 3 parts, Dyhard RU 100 52 parts, bortz powder 8 parts, golden red stone flour 6 parts, lithium hydroxide 5 parts, toluene diphenyl phosphate 12 parts, polynite 7 parts, vermiculite 5 parts, antimonous oxide 4 parts, alkenyl succinic acid copper 2 parts, benzophenone 3 parts, silicon-dioxide 4 parts, dimethyldichlorosilane(DMCS) 3 parts and xylene solvent 28 parts, bortz powder in raw material, golden red stone flour, polynite, vermiculite, antimonous oxide and silicon-dioxide are dropped in ball mill, after ball milling 8h, cross 250 mesh sieves, then carry out mixing and stirring with remaining raw material, for subsequent use,
(2) resin-coated: glass-fiber-fabric to be immersed in glue prepared in step (1), be then dried to prepreg;
(3) foldedly to join: the prepreg obtained in step (2) is carried out mutually folded to be assigned to 8um thick;
(4) suppress: the prepreg in step (3) after folded joining is carried out superimposed with Copper Foil, right be placed in vacuum hotpressing machine, in the press temperature of 210 DEG C, under the pressing pressure of 35MPa, be pressed into required copper-clad plate.
Embodiment 5
A preparation method for resin base heat-conductive copper-clad plate, is characterized in that the step of this preparation method is as follows:
(1) preparation of glue: take each raw material according to certainweight number: isocyanate-based epoxy resin 60 parts, o-cresol aldehyde type epoxy resin 65 parts, 2-ethyl-4-methylimidazole 2 parts, Dyhard RU 100 40 parts, bortz powder 4 parts, golden red stone flour 3 parts, lithium hydroxide 4 parts, toluene diphenyl phosphate 6 parts, polynite 5 parts, vermiculite 3 parts, antimonous oxide 7 parts, alkenyl succinic acid copper 5 parts, benzophenone 4 parts, silicon-dioxide 5 parts, dimethyldichlorosilane(DMCS) 6 parts and propylene glycol solvent 35 parts, bortz powder in raw material, golden red stone flour, polynite, vermiculite, antimonous oxide and silicon-dioxide are dropped in ball mill, after ball milling 7h, cross 250 mesh sieves, then carry out mixing and stirring with remaining raw material, for subsequent use,
(2) resin-coated: glass-fiber-fabric to be immersed in glue prepared in step (1), be then dried to prepreg;
(3) foldedly to join: the prepreg obtained in step (2) is carried out mutually folded to be assigned to 60um thick;
(4) suppress: the prepreg in step (3) after folded joining is carried out superimposed with Copper Foil, right be placed in vacuum hotpressing machine, in the press temperature of 210 DEG C, under the pressing pressure of 35MPa, be pressed into required copper-clad plate.
Performance test
Following table is the performance test of the copper-clad plate prepared by above embodiment, and wherein heat conductivility adopts ASTM-D5470 method.In order to embody the performance of the copper-clad plate prepared by the present invention, carry out test comparison as a comparison case with commercially available epoxy resin copper-clad plate, 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 ~ 2.1W/(mk), be 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, the resistance to sudden heating that shows prepared by the present invention of test result is better.
Claims (7)
1. a preparation method for resin base heat-conductive copper-clad plate, is characterized in that the step of this preparation method is as follows:
(1) preparation of glue: take each raw material according to certainweight number: isocyanate-based epoxy resin, o-cresol aldehyde type epoxy resin, 2-ethyl-4-methylimidazole, Dyhard RU 100, bortz powder, golden red stone flour, lithium hydroxide, toluene diphenyl phosphate, polynite, vermiculite, antimonous oxide, alkenyl succinic acid copper, benzophenone, silicon-dioxide, dimethyldichlorosilane(DMCS) and solvent; Bortz powder in raw material, golden red stone flour, polynite, vermiculite, antimonous oxide and silicon-dioxide are dropped in ball mill, after ball milling 3 ~ 10h, cross 250 mesh sieves, then carry out mixing and stirring with remaining raw material, for subsequent use;
(2) resin-coated: glass-fiber-fabric to be immersed in glue prepared in step (1), be then dried to prepreg;
(3) foldedly to join: the prepreg obtained in step (2) is carried out mutually foldedly be assigned to certain pre-determined thickness;
(4) suppress: the prepreg in step (3) after folded joining is carried out superimposed with Copper Foil, right be placed in vacuum hotpressing machine, be pressed into required copper-clad plate.
2. the preparation method of a kind of resin base heat-conductive copper-clad plate according to claim 1, it is characterized in that in described step (1), each raw material according to parts by weight is: isocyanate-based epoxy resin 45 ~ 70 parts, o-cresol aldehyde type epoxy resin 50 ~ 80 parts, 2-ethyl-4-methylimidazole 1 ~ 4 part, Dyhard RU 100 35 ~ 60 parts, bortz powder 2 ~ 12 parts, golden red stone flour 1 ~ 8 part, lithium hydroxide 2 ~ 6 parts, toluene diphenyl phosphate 4 ~ 15 parts, polynite 2 ~ 10 parts, vermiculite 1 ~ 7 part, antimonous oxide 2 ~ 9 parts, alkenyl succinic acid copper 1 ~ 6 part, benzophenone 1 ~ 5 part, silicon-dioxide 2 ~ 6 parts, dimethyldichlorosilane(DMCS) 2 ~ 8 parts and solvent 20 ~ 40 parts.
3. the preparation method of a kind of resin base heat-conductive copper-clad plate according to claim 1, it is characterized in that in described step (1), each raw material according to parts by weight is: isocyanate-based epoxy resin 45 ~ 60 parts, o-cresol aldehyde type epoxy resin 65 ~ 80 parts, 2-ethyl-4-methylimidazole 2 ~ 4 parts, Dyhard RU 100 40 ~ 60 parts, bortz powder 4 ~ 12 parts, golden red stone flour 3 ~ 8 parts, lithium hydroxide 4 ~ 6 parts, toluene diphenyl phosphate 6 ~ 15 parts, polynite 5 ~ 10 parts, vermiculite 3 ~ 7 parts, antimonous oxide 2 ~ 7 parts, alkenyl succinic acid copper 1 ~ 5 part, benzophenone 1 ~ 4 part, silicon-dioxide 2 ~ 5 parts, dimethyldichlorosilane(DMCS) 2 ~ 6 parts and solvent 20 ~ 35 parts.
4. the preparation method of a kind of resin base heat-conductive copper-clad plate according to claim 1, it is characterized in that in described step (1), each raw material according to parts by weight is: isocyanate-based epoxy resin 54 parts, o-cresol aldehyde type epoxy resin 70 parts, 2-ethyl-4-methylimidazole 3 parts, Dyhard RU 100 52 parts, bortz powder 8 parts, golden red stone flour 6 parts, lithium hydroxide 5 parts, toluene diphenyl phosphate 12 parts, polynite 7 parts, vermiculite 5 parts, antimonous oxide 4 parts, alkenyl succinic acid copper 2 parts, benzophenone 3 parts, silicon-dioxide 4 parts, dimethyldichlorosilane(DMCS) 3 parts and solvent 28 parts.
5. the preparation method of a kind of resin base heat-conductive copper-clad plate according to claim 1, is characterized in that described solvent is at least one in acetone, propylene glycol, ethylene glycol monomethyl ether and dimethylbenzene.
6. the preparation method of a kind of resin base heat-conductive copper-clad plate according to any one of claim 1 to 5, it is characterized in that prepreg described in described step (3) carries out folded pre-determined thickness of joining mutually is 20 ~ 120um.
7. the preparation method of a kind of resin base heat-conductive copper-clad plate according to any one of claim 1 to 5, is characterized in that the condition in vacuum hotpressing machine described in described step (4) is: the press temperature of 210 DEG C, the pressing pressure of 35MPa.
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| 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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| 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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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911479A (en) * | 2012-11-14 | 2013-02-06 | 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 |
| 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 |
| CN104448718A (en) * | 2014-12-08 | 2015-03-25 | 陕西生益科技有限公司 | Resin composition and application thereof |
| CN104760368A (en) * | 2015-04-14 | 2015-07-08 | 东华大学 | Epoxy-imide resin-based copper-clad plate and preparation method thereof |
-
2015
- 2015-09-24 CN CN201510615340.XA patent/CN105199318B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911479A (en) * | 2012-11-14 | 2013-02-06 | 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 |
| 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 |
| CN104448718A (en) * | 2014-12-08 | 2015-03-25 | 陕西生益科技有限公司 | Resin composition and application thereof |
| CN104760368A (en) * | 2015-04-14 | 2015-07-08 | 东华大学 | Epoxy-imide resin-based copper-clad plate and preparation method thereof |
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| CN105199318B (en) | 2017-12-26 |
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