CN102775731B - Glue solution for preparing FR-4 (fiberglass board) copper-clad plate and preparation method - Google Patents
Glue solution for preparing FR-4 (fiberglass board) copper-clad plate and preparation method Download PDFInfo
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- CN102775731B CN102775731B CN201210240380.7A CN201210240380A CN102775731B CN 102775731 B CN102775731 B CN 102775731B CN 201210240380 A CN201210240380 A CN 201210240380A CN 102775731 B CN102775731 B CN 102775731B
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Abstract
The invention relates to glue solution for preparing an FR-4 (fiberglass board) copper-clad plate. The glue solution is characterized by comprising the following materials in parts by weight: 35-45 parts of high bromide epoxy resin, 10-20 parts of o-cresol novolac epoxy resin or phenol phenolic epoxy resin, 10-20 parts of E-type difunctional epoxy resin E-44 or E-51, 5-15 parts of tetraphenyl glycidyl ether based ethane, 15-25 parts of bisphenol A-type lacquer resin, 0.06-0.1 parts of 2-phenylimidazole, 20-30 parts of silicon dioxide powder of which the particle size is 3-5 microns, and 53-80 parts of propylene glycol methyl ether acetate. Compared with the traditional FR-4 copper-clad plate, the performance of the FR-4 copper-clad plate prepared from the glue solution disclosed by the invention according to a conventional process is greatly improved.
Description
[technical field]
The present invention relates to a kind of glue for the preparation of low thermal coefficient of expansion FR-4 copper-clad plate.
[background technology]
The preparation technology of FR-4 type copper-clad laminate (referred to as FR-4 copper-clad plate) mainly draws together following 3 steps: the configuration of (1) glue; (2) preparation of prepreg: increase material (comprising glasscloth, paper substrate, matrix material etc.) and use the glue of step (1) gained to carry out impregnation, baking to obtain prepreg (3) compacting on spreadometer: the prepreg of by dimensional requirement, prepreg being sheared out desired size; The prepreg of pressing the desired size of the superimposed corresponding number of product thickness, is covered with electrolytic copper foil, in press, suppresses.
The Tg of traditional FR-4 copper-clad plate is about 130 DEG C, and the Z axis coefficient of expansion is 280-320ppm/ DEG C (after Tg), and 50-260 DEG C of deformation ratio minimum is 4%; For high density packaging technique, traditional FR-4 copper-clad plate manifests the deficiency in its performance gradually; Along with the slimming of electric equipment products, multifunction, integrated development, the number of plies of pcb board is more and more, aligning accuracy requires also more and more higher, when components and parts welding, need stand thermal shocking repeatedly, therefore, the Z axis thermal expansivity of reduction FR-4 type copper-clad laminate becomes the exploitation direction of more paying close attention in copper-clad plate field.
[summary of the invention]
The technical problem to be solved in the present invention is to provide a kind of glue for the preparation of FR-4 copper-clad plate, and it can improve the performance of FR-4 copper-clad plate significantly.
Above-mentioned technical problem is achieved through the following technical solutions:
For the preparation of a glue for FR-4 copper-clad plate, it is characterized in that, made by following raw material by weight ratio:
High Bromine epoxy Resin, 35-45 part; Study On O-cresol Epoxy Resin or phenol novolac epoxy resins, 10-20 part; E type difunctional epoxy resin E-44 or E-51,10-20 part; Tetraphenyl glycidyl ether ethane, 5-15 part; Bisphenol A-type lacquer resins, 15-25 part; 2-phenylimidazole, 0.06-0.1 part; The silicon dioxide powder of particle diameter 3-5 μ m, 20-30 part; 1-Methoxy-2-propyl acetate, 53-80 part.
Further scheme is that described glue is made up of following raw material by weight ratio:
High Bromine epoxy Resin, 40 parts; Study On O-cresol Epoxy Resin, 15 parts; E type difunctional epoxy resin E-44,10 parts; Tetraphenyl glycidyl ether ethane, 10 parts; Bisphenol A-type lacquer resins, 25 parts; 2-phenylimidazole, 0.1 part; 30 parts of the silicon dioxide powders of particle diameter 3-5 μ m; 1-Methoxy-2-propyl acetate, 70 parts.
Further scheme is that described glue is made up of following raw material by weight ratio:
High Bromine epoxy Resin, 35 parts; Phenol novolac epoxy resins, 10 parts; E type difunctional epoxy resin E-44,20 parts; Tetraphenyl glycidyl ether ethane, 15 parts; Bisphenol A-type lacquer resins, 20 parts; 2-phenylimidazole, 0.08 part; The silicon dioxide powder of particle diameter 3-5 μ m, 25 parts; 1-Methoxy-2-propyl acetate, 53 parts.
Further scheme is that described glue is made up of following raw material by weight ratio:
High Bromine epoxy Resin, 45 parts; Study On O-cresol Epoxy Resin, 20 parts; E type difunctional epoxy resin E-51,15 parts; Tetraphenyl glycidyl ether ethane, 5 parts; Bisphenol A-type lacquer resins, 15 parts; 2-phenylimidazole, 0.06 part; The silicon dioxide powder of particle diameter 3-5 μ m, 20 parts; 1-Methoxy-2-propyl acetate, 80 parts.
Above-mentioned glue makes to prepare with the following method, and method specifically comprises the following steps:
(201), take raw material by above-mentioned weight part proportioning: High Bromine epoxy Resin, Study On O-cresol Epoxy Resin or phenol novolac epoxy resins, E type difunctional epoxy resin E-44 or E-51, tetraphenyl glycidyl ether ethane, bisphenol A-type lacquer resins, 2-phenylimidazole, the silicon dioxide powder of particle diameter 3-5 μ m, 1-Methoxy-2-propyl acetate;
(202), dissolve 2-phenylimidazole with part 1-Methoxy-2-propyl acetate, the weight ratio of described diol segment methyl ether acetate and 2-phenylimidazole is 5-10;
(203), by High Bromine epoxy Resin, Study On O-cresol Epoxy Resin or phenol novolac epoxy resins, dihydroxyphenyl propane lacquer resins, E type difunctional epoxy resin E-44 or E-51, tetraphenyl glycidyl ether ethane, joins in remaining 1-Methoxy-2-propyl acetate, is stirred to completely and dissolves;
(204), the gains of step (202) are mixed with the gains of step (203), then add silicon dioxide powder, stir slaking 8h, obtain required glue.
Effect of the present invention:
According to experiment test, use glue of the present invention, and according to the conventional preparation flow of FR-4 copper-clad plate (preparation of prepreg, compacting), the FR-4 copper-clad plate making, its parameter is: Tg is 170 DEG C-180 DEG C, the Z axis coefficient of expansion is less than 220ppm/ DEG C (after Tg), and 50-260 DEG C of deformation ratio is less than 3%.Visible, use the prepared FR-4 copper-clad plate of glue of the present invention, with respect to traditional FR-4 copper-clad plate, performance is greatly improved.
The chemical formula of above-mentioned High Bromine epoxy Resin is:
Study On O-cresol Epoxy Resin:
Phenol novolac epoxy resins:
The chemical formula of above-mentioned E type difunctional epoxy resin E-44 is:
The chemical formula of above-mentioned bisphenol A-type lacquer resins is:
The chemical formula of above-mentioned 2-phenylimidazole is:
The chemical formula of 1-Methoxy-2-propyl acetate is:
[embodiment]
Embodiment mono-
One, glue preparation
(1) glue is to be made up of following raw material by weight ratio:
High Bromine epoxy Resin, 40 parts; Study On O-cresol Epoxy Resin, 15 parts; E type difunctional epoxy resin E-44,10 parts; Tetraphenyl glycidyl ether ethane, 10 parts; Bisphenol A-type lacquer resins, 25 parts; 2-phenylimidazole, 0.1 part; 30 parts of the silicon dioxide powders of particle diameter 3-5 μ m; 1-Methoxy-2-propyl acetate, 70 parts;
(2) preparation process, comprises the following steps:
(201), take raw material by above-mentioned weight part proportioning: High Bromine epoxy Resin, Study On O-cresol Epoxy Resin, E type difunctional epoxy resin E-44, tetraphenyl glycidyl ether ethane, bisphenol A-type lacquer resins, 2-phenylimidazole, the silicon dioxide powder of particle diameter 3-5 μ m, 1-Methoxy-2-propyl acetate;
(202), dissolve 2-phenylimidazole with part 1-Methoxy-2-propyl acetate, the weight ratio of described diol segment methyl ether acetate and 2-phenylimidazole is 10;
(203), by High Bromine epoxy Resin, Study On O-cresol Epoxy Resin, dihydroxyphenyl propane lacquer resins, E type difunctional epoxy resin E-44, tetraphenyl glycidyl ether ethane, joins in remaining 1-Methoxy-2-propyl acetate, is stirred to completely and dissolves;
(204), the gains of step (202) are mixed with the gains of step (203), then add silicon dioxide powder, stir slaking 8h, obtain required glue;
Two, the preparation of prepreg: adopt 7628 woven fiber glass, on fall shaft hlue spreader, first use the glue of step 1 gained to carry out in the baking oven of fall shaft hlue spreader, toasting after impregnation, the speed of the operation of 7628 woven fiber glass is 2.5m/min, the temperature of baking oven is 180 DEG C, show that prepreg (select by the routine that is set to of speed and temperature, as long as guarantee that the parameter of prepreg is within following product standard: gelation time GT:70-90s/171 DEG C, indicated weight: 3.67-3.73/m2, RF:18-22%; Those skilled in the art can regulate the speed and temperature flexibly);
Three, compacting:
By dimensional requirement, prepreg is sheared out the prepreg of desired size; By the prepreg of the desired size of the superimposed corresponding number of product thickness (if thickness is that 1.6mm needs 8 prepregs), be covered with electrolytic copper foil, in press, suppress, wherein, and press temperature: 200 DEG C/2h, pressure: vacuum press 40kg/cm
2, make required FR-4 copper-clad plate.
Extract wherein two FR-4 copper-clad plates and test, test data is in table 1.
Table 1
| Test event | Model 1 | Model 2 |
| Tg℃ | 170 | 173 |
| Z axis rate of expansion (after Tg) ppm/ DEG C | 205 | 195 |
| 50-260 DEG C of deformation ratio % | 2.2 | 2.5 |
Embodiment bis-
One, glue preparation
(1) glue is to be made up of following raw material by weight ratio:
High Bromine epoxy Resin, 35 parts; Phenol novolac epoxy resins, 10 parts; E type difunctional epoxy resin E-44,20 parts; Tetraphenyl glycidyl ether ethane, 15 parts; Bisphenol A-type lacquer resins, 20 parts; 2-phenylimidazole, 0.08 part; The silicon dioxide powder of particle diameter 3-5 μ m, 25 parts; 1-Methoxy-2-propyl acetate, 53 parts;
(2) preparation process, comprises the following steps:
(201), take raw material by above-mentioned weight part proportioning: High Bromine epoxy Resin, phenol novolac epoxy resins, E type difunctional epoxy resin E-44, tetraphenyl glycidyl ether ethane, bisphenol A-type lacquer resins, 2-phenylimidazole, the silicon dioxide powder of particle diameter 3-5 μ m, 1-Methoxy-2-propyl acetate;
(202), dissolve 2-phenylimidazole with part 1-Methoxy-2-propyl acetate, the weight ratio of described diol segment methyl ether acetate and 2-phenylimidazole is 5;
(203), by High Bromine epoxy Resin, phenol novolac epoxy resins, dihydroxyphenyl propane lacquer resins, E type difunctional epoxy resin E-44, tetraphenyl glycidyl ether ethane, joins in remaining 1-Methoxy-2-propyl acetate, is stirred to completely and dissolves;
(204), the gains of step (202) are mixed with the gains of step (203), then add silicon dioxide powder, stir slaking 8h, obtain required glue;
Two, the preparation of prepreg: referring to embodiment mono-
Three, compacting:
By dimensional requirement, prepreg is sheared out the prepreg of desired size; By the prepreg of the desired size of the superimposed corresponding number of product thickness (if thickness is that 1.6mm needs 8 prepregs), be covered with electrolytic copper foil, in press, suppress, wherein, and press temperature: 200 DEG C/2h, pressure: vacuum press 40kg/cm
2; The parameter of baking oven is set to conventional selection, under those skilled in the art's grasp, can adjust flexibly; Make required FR-4 copper-clad plate.
Extract wherein two FR-4 copper-clad plates and test, test data is in table 2.
Table 2
| Test event | Model 3 | Model 4 |
| Tg℃ | 180 | 175 |
| Z axis rate of expansion (after Tg) ppm/ DEG C | 210 | 212 |
| 50-260 DEG C of deformation ratio % | 2.1 | 2.5 |
Embodiment tri-
One, glue preparation
(1) glue is to be made up of following raw material by weight ratio:
High Bromine epoxy Resin, 45 parts; Study On O-cresol Epoxy Resin, 20 parts; E type difunctional epoxy resin E-51,15 parts; Tetraphenyl glycidyl ether ethane, 5 parts; Bisphenol A-type lacquer resins, 15 parts; 2-phenylimidazole, 0.06 part; The silicon dioxide powder of particle diameter 3-5 μ m, 20 parts; 1-Methoxy-2-propyl acetate, 80 parts;
(2) preparation process, comprises the following steps:
(201), take raw material by above-mentioned weight part proportioning: High Bromine epoxy Resin, Study On O-cresol Epoxy Resin, E type difunctional epoxy resin E-51, tetraphenyl glycidyl ether ethane, bisphenol A-type lacquer resins, 2-phenylimidazole, the silicon dioxide powder of particle diameter 3-5 μ m, 1-Methoxy-2-propyl acetate;
(202), dissolve 2-phenylimidazole with part 1-Methoxy-2-propyl acetate, the weight ratio of described diol segment methyl ether acetate and 2-phenylimidazole is 7;
(203), by High Bromine epoxy Resin, Study On O-cresol Epoxy Resin, dihydroxyphenyl propane lacquer resins, E type difunctional epoxy resin E-51, tetraphenyl glycidyl ether ethane, joins in remaining 1-Methoxy-2-propyl acetate, is stirred to completely and dissolves;
(204), the gains of step (202) are mixed with the gains of step (203), then add silicon dioxide powder, stir slaking 8h, obtain required glue;
Two, the preparation of prepreg: referring to embodiment mono-
Three, compacting:
By dimensional requirement, prepreg is sheared out the prepreg of desired size; By the prepreg of the desired size of the superimposed corresponding number of product thickness (if thickness is that 1.6mm needs 8 prepregs), be covered with electrolytic copper foil, in press, suppress, wherein, and press temperature: 200 DEG C/2h, pressure: vacuum press 40kg/cm
2, make required FR-4 copper-clad plate.
Extract wherein two FR-4 copper-clad plates and test, test data is in table 3.
Table 3
| Test event | Model 5 | Model 6 |
| Tg℃ | 178 | 180 |
| Z axis rate of expansion (after Tg) ppm/ DEG C | 220 | 215 |
| 50-260 DEG C of deformation ratio % | 2.8 | 2.6 |
Embodiment tetra-
One, glue preparation
(1) glue is to be made up of following raw material by weight ratio:
High Bromine epoxy Resin, 38 parts; Phenol novolac epoxy resins, 17 parts; E type difunctional epoxy resin E-51,18 parts; Tetraphenyl glycidyl ether ethane, 12 parts; Bisphenol A-type lacquer resins, 21 parts; 2-phenylimidazole, 0.07 part; The silicon dioxide powder of particle diameter 3-5 μ m, 26 parts; 1-Methoxy-2-propyl acetate, 75 parts;
(2) preparation process, comprises the following steps:
(201), take raw material by above-mentioned weight part proportioning: High Bromine epoxy Resin, phenol novolac epoxy resins, E type difunctional epoxy resin E-51, tetraphenyl glycidyl ether ethane, bisphenol A-type lacquer resins, 2-phenylimidazole, the silicon dioxide powder of particle diameter 3-5 μ m, 1-Methoxy-2-propyl acetate;
(202), dissolve 2-phenylimidazole with part 1-Methoxy-2-propyl acetate, the weight ratio of described diol segment methyl ether acetate and 2-phenylimidazole is 8;
(203), by High Bromine epoxy Resin, phenol novolac epoxy resins, dihydroxyphenyl propane lacquer resins, E type difunctional epoxy resin E-51, tetraphenyl glycidyl ether ethane, joins in remaining 1-Methoxy-2-propyl acetate, is stirred to completely and dissolves;
(204), the gains of step (202) are mixed with the gains of step (203), then add silicon dioxide powder, stir slaking 8h, obtain required glue;
Two, the preparation of prepreg: referring to embodiment mono-
Three, compacting:
By dimensional requirement, prepreg is sheared out the prepreg of desired size; By the prepreg of the desired size of the superimposed corresponding number of product thickness (if thickness is that 1.6mm needs 8 prepregs), be covered with electrolytic copper foil, in press, suppress, wherein, and press temperature: 200 DEG C/2h, pressure: vacuum press 40kg/cm
2, make required FR-4 copper-clad plate.
Extract wherein two FR-4 copper-clad plates and test, test data is in table 4.
Table 4
| Test event | Model 7 | Model 8 |
| Tg℃ | 180 | 177 |
| Z axis rate of expansion (after Tg) ppm/ DEG C | 210 | 197 |
| 50-260 DEG C of deformation ratio % | 2.7 | 2.6 |
The present invention is not limited to above-described embodiment, based on simple replacement above-described embodiment, that do not make creative work, should belong to the scope that the present invention discloses.
Claims (5)
1. for the preparation of a glue for FR-4 copper-clad plate, it is characterized in that, made by following raw material by weight ratio:
High Bromine epoxy Resin, 35-45 part; Study On O-cresol Epoxy Resin or phenol novolac epoxy resins, 10-20 part; E type difunctional epoxy resin E-44 or E-51,10-20 part; Tetraphenyl glycidyl ether ethane, 5-15 part; Bisphenol A-type lacquer resins, 15-25 part; 2-phenylimidazole, 0.06-0.1 part; The silicon dioxide powder of particle diameter 3-5 μ m, 20-30 part; 1-Methoxy-2-propyl acetate, 53-80 part.
2. glue according to claim 1, is characterized in that, is made up of following raw material by weight ratio:
High Bromine epoxy Resin, 40 parts; Study On O-cresol Epoxy Resin, 15 parts; E type difunctional epoxy resin E-44,10 parts; Tetraphenyl glycidyl ether ethane, 10 parts; Bisphenol A-type lacquer resins, 25 parts; 2-phenylimidazole, 0.1 part; 30 parts of the silicon dioxide powders of particle diameter 3-5 μ m; 1-Methoxy-2-propyl acetate, 70 parts.
3. glue according to claim 1, is characterized in that, is made up of following raw material by weight ratio:
High Bromine epoxy Resin, 35 parts; Phenol novolac epoxy resins, 10 parts; E type difunctional epoxy resin E-44,20 parts; Tetraphenyl glycidyl ether ethane, 15 parts; Bisphenol A-type lacquer resins, 20 parts; 2-phenylimidazole, 0.08 part; The silicon dioxide powder of particle diameter 3-5 μ m, 25 parts; 1-Methoxy-2-propyl acetate, 53 parts.
4. glue according to claim 1, is characterized in that, is made up of following raw material by weight ratio:
High Bromine epoxy Resin, 45 parts; Study On O-cresol Epoxy Resin, 20 parts; E type difunctional epoxy resin E-51,15 parts; Tetraphenyl glycidyl ether ethane, 5 parts; Bisphenol A-type lacquer resins, 15 parts; 2-phenylimidazole, 0.06 part; The silicon dioxide powder of particle diameter 3-5 μ m, 20 parts; 1-Methoxy-2-propyl acetate, 80 parts.
5. prepare the method for claim 1 to the glue described in claim 4 any one, it is characterized in that, comprise the following steps:
(201), take raw material by above-mentioned weight part proportioning: High Bromine epoxy Resin, Study On O-cresol Epoxy Resin or phenol novolac epoxy resins, E type difunctional epoxy resin E-44 or E-51, tetraphenyl glycidyl ether ethane, bisphenol A-type lacquer resins, 2-phenylimidazole, the silicon dioxide powder of particle diameter 3-5 μ m, 1-Methoxy-2-propyl acetate;
(202), dissolve 2-phenylimidazole with part 1-Methoxy-2-propyl acetate, the weight ratio of described part 1-Methoxy-2-propyl acetate and 2-phenylimidazole is 5-10;
(203), by High Bromine epoxy Resin, Study On O-cresol Epoxy Resin or phenol novolac epoxy resins, dihydroxyphenyl propane lacquer resins, E type difunctional epoxy resin E-44 or E-51, tetraphenyl glycidyl ether ethane, joins in remaining 1-Methoxy-2-propyl acetate, is stirred to completely and dissolves;
(204), the gains of step (202) are mixed with the gains of step (203), then add silicon dioxide powder, stir slaking 8h, obtain required glue.
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| CN105199619B (en) * | 2015-09-21 | 2017-08-08 | 金安国纪科技（珠海）有限公司 | Aluminum-based copper-clad plate high-heat-conductivity glue membrane preparation method |
| CN108300145A (en) * | 2017-09-05 | 2018-07-20 | 湖州加成金属涂料有限公司 | A kind of zinc-plated base material powdery paints and preparation method |
| CN109836778B (en) * | 2019-02-26 | 2021-05-28 | 金安国纪科技（杭州）有限公司 | Epoxy resin composition, preparation method and application thereof |
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| CN101921458A (en) * | 2010-08-05 | 2010-12-22 | 宏昌电子材料股份有限公司 | Unleaded epoxy resin composite for printed circuit copper clad laminate |
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| CN101921458A (en) * | 2010-08-05 | 2010-12-22 | 宏昌电子材料股份有限公司 | Unleaded epoxy resin composite for printed circuit copper clad laminate |
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