CN105419231B - The copper-clad plate and pcb board of a kind of resin combination and its making - Google Patents
The copper-clad plate and pcb board of a kind of resin combination and its making Download PDFInfo
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- CN105419231B CN105419231B CN201510851763.1A CN201510851763A CN105419231B CN 105419231 B CN105419231 B CN 105419231B CN 201510851763 A CN201510851763 A CN 201510851763A CN 105419231 B CN105419231 B CN 105419231B
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Abstract
The present invention relates to printed-board technology field, more particularly to a kind of resin combination, by weight, including 20~25 parts of phosphorous epoxy resin, 10~15 parts of brominated epoxy resin, 10~20 parts of cycloaliphatic epoxy resin, 25~30 parts of acid anhydrides, 10~15 parts of phosphorus-containing phenolic aldehyde, 5~15 parts of boehmite；Wherein, 100~200g/eq of epoxide equivalent scope of the cycloaliphatic epoxy resin；The present invention by ordinary epoxy resin system introduce cycloaliphatic epoxy resin and by with anhydride-cured, excellent anti-creep track property and heat resistance can be obtained, system is set to reach flame-retardancy requirements by bromine, phosphorus cooperative mode simultaneously, and introduce the more preferable boehmite filler materials of a small amount of heat resistance, filling aluminium hydrate need not be added, it is to avoid the defect of mass filler addition；The invention further relates to the copper-clad plate that the resin combination makes, its CTI >=600V, heat-resist, alkali resistance is excellent, reach flame-retardancy requirements；And the pcb board that the resin combination makes.
Description
Technical field
The present invention relates to printed-board technology field, more particularly to a kind of resin combination and the height using its making
CTI copper-clad plates and pcb board.
Background technology
Copper-clad plate is widely used in various electronics, electric product as the insulating substrate of printed circuit board, with people
Increasingly pay attention to electronics, the security reliability of electric product, the security reliability of copper-clad plate is accordingly proposed higher and higher
It is required that, wherein proof tracking is exactly a significant reliability index of copper-clad plate, and the copper-clad plate of proof tracking difference is
The potential risk that electronics, electric product fire are produced.The Capability index of the anti creepage trace on insulating materials surface is referred to as comparing
Creepage trace index CTI (Comparative Tracking Idex), refers to that material surface is able to take 50 drop electrolyte
The maximum voltage value of (0.1% aqueous ammonium chloride solution) without forming tracking, it weighs the exhausted of material to a certain extent
Edge security performance, this value is higher, and proof tracking is better, and the insulating properties for representing material is better, therefore, high CTI products into
For electronics industry research and development trend.
Copper-clad plate must improve its proof tracking, i.e., just can guarantee that its security reliability with higher CTI values, at present
The CTI values of common copper-clad plate are general in 175-250V, and for traditional high CTI copper-clad plate, though its CTI can reach 400V
More than, but the preparation method of traditional high CTI copper-clad plates realizes by addition filling aluminium hydrate；Such a method is in system
Making copper-clad plate of the CTI values more than 600V needs to add substantial amounts of filling aluminium hydrate, and the filler of high content easily causes sheet material
Processability declines, heat resistance and alkali resistance are reduced.In view of the above-mentioned problems, be badly in need of a kind of new resin combination has height to be made
The copper-clad plate of CTI values, to solve the above problems.
The content of the invention
For above-mentioned the deficiencies in the prior art, an object of the present invention is the provision of a kind of resin combination, can use
The copper-clad plate with high CTI value is made；
The second object of the present invention is to provide a kind of high CTI copper-clad plates made using above-mentioned resin combination, used
Its phase ratio creepage tracking index of the copper-clad plate of resin combination preparation is high, heat-resist, alkali resistance is excellent and can reach fire-retardant want
Ask.
The third object of the present invention is to provide a kind of pcb board made using above-mentioned resin combination.
To achieve these goals, technical scheme is as follows：
A kind of resin combination, by weight, including 20~25 parts of phosphorous epoxy resin, brominated epoxy resin 10~15
Part, 10~20 parts of cycloaliphatic epoxy resin, 25~30 parts of acid anhydrides, 10~15 parts of phosphorus-containing phenolic aldehyde, 5~15 parts of boehmite；Wherein, institute
The epoxide equivalent for stating phosphorous epoxy resin is 250~450g/eq, phosphorus content 1%~4%；The epoxy of the brominated epoxy resin
300~500g/eq of equivalent weight range, bromine content 15%~50%；The epoxide equivalent of the cycloaliphatic epoxy resin be 100~
200g/eq, the phosphorus content 5%~15% of the phosphorus-containing phenolic aldehyde.
Compared to the resin combination of prior art, wherein used ordinary epoxy resin is due to containing substantial amounts of benzene
Ring, causes to introduce cycloaliphatic epoxy resin in the poor performances such as the obtained anti creepage trace of copper-clad plate, the present invention, it synthesizes former
Reason is different from glycidol type epoxy resin, and the epoxy radicals in its molecule is the double bond epoxidation using unsaturated lipid cycle compound
Formed, industrial is typically by the alicyclic olefin compound containing two double bonds passes through peroxide (such as peracetic acid)
Oxidation formation epoxidation alicyclic olefin compound；Therefore, there is no phenyl ring and hydroxyl in the molecular structure of cycloaliphatic epoxy resin
Cl is free of in base, and building-up process—、Na+Plasma；Itself it is not in addition polymer, but is acted on anhydride curing agent
The polymer of the three-dimensional structure of excellent performance can be generated afterwards；The copper-clad plate made using the resin combination of the present invention, its
Good electrical property, especially anti creepage trace performance.
It is preferred that the acid anhydrides is tung oil acid anhydride, alkylene succinic anhydride, methyl hexahydrophthalic acid anhydride, hydrogenating methyl
One in carbic anhydride, glutaric anhydride, poly- azelaic acid acid anhydride, poly- icosane diacid anhydride, styrene-maleic anhydride copolymer
Plant or several mixtures.
It is preferred that the structural formula of the styrene-maleic anhydride copolymer is as follows：
It is preferred that percentage, in addition to curing accelerator 0.01%~0.1%；Specifically, the solidification promotees
Enter agent for 2-methylimidazole, 1- methylimidazoles, 2-ethyl-4-methylimidazole, 1- fluoro ethyls -2-ethyl-4-methylimidazole, 2- benzene
One or more of mixtures in base imidazoles, 2- undecyl imidazoles, 2- phenyl -4-methylimidazole；Its effect is to make resin group
Compound has suitable curing rate, while making resin combination have suitable molding time, it is ensured that filling out between boundary layer
Fill effect and adhesion strength.
A kind of copper-clad plate prepared using resin combination as described above.
A kind of preparation method of copper-clad plate as described above, comprises the following steps：
It is well mixed after weighing each component in the resin combination by formula ratio first, adds solvent and be made into resin glue
Liquid；
Then reinforcing material is immersed in resin adhesive liquid, rear drying removes solvent, obtains prepreg；
The prepreg of gained is covered with metal foil, is laminated, the copper-clad plate is produced.
It is preferred that the solvent is acetone, butanone, cyclohexanone, hexamethylene, glycol monoethyl ether, triglyme, first
One or more of mixtures in benzene, dimethylbenzene, N,N-dimethylformamide；For dissolving in acid anhydrides and resin combination
Other materials etc., makes resin combination have suitable viscosity.
It is preferred that the solid content in the resin adhesive liquid is 20%~50%.
A kind of pcb board prepared using resin combination as described above.
A kind of electronic product prepared using resin combination as described above.
Compared to prior art, resin combination of the invention in ordinary epoxy resin system by introducing aliphatic ring
Oxygen tree fat, and being obtained by it with anhydride-cured, the copper-clad plate made using invention resin composition can obtain excellent resistance to
Creepage trace characteristic and heat resistance, while invention resin composition makes system reach fire-retardant want by bromine, phosphorus cooperative mode
Ask, and introduce the more preferable boehmite filler materials of a small amount of heat resistance, without adding filling aluminium hydrate, it is to avoid conventional method is because a large amount of
Filling aluminium hydrate is added, and brings the problems such as product processability, heat resistance and alkali resistance decline；
The copper-clad plate prepared using the resin combination its CTI >=600V, heat-resist, alkali resistance is excellent, it is fire-retardant to reach
It is required that；And without substantial amounts of filling aluminium hydrate is added in the copper-clad plate, so as to avoid conventional method because of a large amount of addition hydrogen-oxygens
Change the poor sheet fabrication that brings of Al filler, heat resistance and alkali resistance can not be up to standard etc. technical problem；Thus, the copper-clad plate with
Greatly improved when making printed circuit board (PCB) and using the security reliability on electronic product.
Embodiment
The embodiment to the present invention is described in further detail below.
Embodiment 1
A kind of resin combination, by total weight parts be 100 parts (not including curing accelerator) based on, including：Phosphorous asphalt mixtures modified by epoxy resin
20 parts of fat (DOW Chemical, XZ92530), 15 parts of brominated epoxy resin (big Japanese ink company, Epiclon153-60M), alicyclic ring
20 parts of race's epoxy resin (DOW Chemical, ERL-4221D), 25 parts of acid anhydrides (Cray Willie, SMAEF-40), phosphorus-containing phenolic aldehyde (SHINA
Chemistry, LC-950) 15 parts, 5 parts of boehmite；Curing accelerator (2-methylimidazole) is additionally included, percentage is,
For the 0.05% of resin combination gross weight.
Above-mentioned resin combination is applied to make copper-clad plate, its preparation method comprises the following steps：
First, each components by weight percent of the resin combination is weighed by formula ratio, and be mixed it is uniform, then to the mixture
Middle addition 2-methylimidazole and appropriate acetone are made into resin adhesive liquid, and solid content is 30% wherein in resin adhesive liquid；
Secondly, will it is well mixed after resin adhesive liquid be coated on E-glass cloth, after in an oven 155 DEG C toast 5 points
Clock removes solvent and obtains prepreg；
Then, 8 prepregs are stacked, 18 μ electrolytic copper foil is respectively covered up and down, in vacuum press middle level
Pressure, lamination is 190 DEG C, 90 minutes, and copper-clad plate is made；
Finally obtained copper-clad plate is detected, detection performance is as shown in table 1.
Embodiment 2
A kind of resin combination, by total weight parts be 100 parts based on (not including curing accelerator), including：Phosphorous asphalt mixtures modified by epoxy resin
23 parts of fat (DOW Chemical, XZ92530), 12 parts of brominated epoxy resin (big Japanese ink company, Epiclon153-60M), alicyclic ring
15 parts of race's epoxy resin (DOW Chemical, ERL-4221D), 27 parts of acid anhydrides (Cray Willie, SMAEF-40), phosphorus-containing phenolic aldehyde (SHINA
Chemistry, LC-950) 13 parts, 10 parts of boehmite；In addition, also including curing accelerator (2- phenylimidazoles), percentage
To account for the 0.1% of resin combination gross weight.
Above-mentioned resin combination is applied to make copper-clad plate, its preparation method comprises the following steps：
First, weigh each component of the resin combination by formula ratio, and by said components it is well mixed after, thereto plus
Enter 2- phenylimidazoles and solvent (mixture of dimethylbenzene and toluene) is made into resin adhesive liquid, wherein solid content is in resin adhesive liquid
40%；
Secondly, will it is well mixed after resin adhesive liquid be coated on E-glass cloth, after in an oven 155 DEG C toast 5 points
Clock removes solvent and obtains prepreg；
Then, 8 prepregs are stacked, 18 μ electrolytic copper foil is respectively covered up and down, in vacuum press middle level
Pressure, lamination is 190 DEG C, 90 minutes, and copper-clad plate is made；
Finally obtained copper-clad plate is detected, detection performance is as shown in table 1.
Embodiment 3
A kind of resin combination, is (not include curing accelerator in this 100 parts) based on 100 parts by total weight parts, including：Contain
25 parts of phosphorus epoxy resin (DOW Chemical, XZ92530), brominated epoxy resin (big Japanese ink company, Epiclon153-60M)
10 parts, 10 parts of cycloaliphatic epoxy resin (DOW Chemical, ERL-4221D), 30 parts of acid anhydrides (Cray Willie, SMAEF-40) is phosphorous
10 parts of phenolic aldehyde (SHINA chemistry, LC-950), 15 parts of boehmite；In addition, also including curing accelerator (1- methylimidazoles), by weight
Percentage meter is measured, is the 0.01% of resin combination gross weight.
Above-mentioned resin combination is applied to make copper-clad plate, its preparation method comprises the following steps：
First, weigh each component of the resin combination by formula ratio, and by said components it is well mixed after thereto plus
Enter 1- methylimidazoles and solvent cyclohexanone is made into resin adhesive liquid, solid content is 50% wherein in resin adhesive liquid；
Secondly, will it is well mixed after resin adhesive liquid be coated on E-glass cloth, after in an oven 155 DEG C toast 5 points
Clock removes solvent and obtains prepreg；
Then, 8 prepregs are stacked, 18 μ electrolytic copper foil is respectively covered up and down, in vacuum press middle level
Pressure, lamination is 190 DEG C, 90 minutes, and copper-clad plate is made；
Finally obtained copper-clad plate is detected, detection performance is as shown in table 1.
Comparative example 1
A kind of resin combination, be 100 parts (in this 100 parts do not include curing accelerator) by total weight parts based on, including：Bromine
Change 45 parts of epoxy resin (DOW Chemical, DER530), 13 parts of bisphenol A epoxide resin (HEXION, Epikote1001), hydroxide
40 parts of Al filler, 2 parts of dicyandiamide；In addition, also including curing accelerator (2-methylimidazole), percentage is, for tree
The 0.01% of oil/fat composition gross weight.
Above-mentioned resin combination is applied to make copper-clad plate, its preparation method comprises the following steps：
First, weigh each component of the resin combination by formula ratio, and by said components it is well mixed after thereto plus
Enter 2-methylimidazole and solvent acetone is made into resin adhesive liquid, solid content is 30% wherein in resin adhesive liquid；
Secondly, will it is well mixed after resin adhesive liquid be coated on E-glass cloth, after in an oven 155 DEG C toast 5 points
Clock removes solvent and obtains prepreg；
Then, 8 prepregs are stacked, 18 μ electrolytic copper foil is respectively covered up and down, in vacuum press middle level
Pressure, lamination is 190 DEG C, 90 minutes, and copper-clad plate is made；
Finally obtained copper-clad plate is detected, detection performance is as shown in table 1.
Comparative example 2
A kind of resin combination, by total weight parts be 100 parts (not including curing accelerator) based on, including：Phosphorous asphalt mixtures modified by epoxy resin
45 parts of fat (DOW Chemical, XZ92530), 13 parts of bisphenol A epoxide resin (HEXION, Epikote1001), filling aluminium hydrate 40
Part, 2 parts of dicyandiamide；In addition, also including curing accelerator (1- methylimidazoles), percentage is that resin combination is total
The 0.05% of weight.
Above-mentioned resin combination is applied to make copper-clad plate, its preparation method comprises the following steps：
First, each component of the resin combination is weighed by formula ratio, and is mixed uniformly, then is added into composition
1- methylimidazoles and solvent cyclohexanone are made into resin adhesive liquid, and solid content is 40% wherein in resin adhesive liquid；
Secondly, will it is well mixed after resin adhesive liquid be coated on E-glass cloth, after in an oven 155 DEG C toast 5 points
Clock removes solvent and obtains prepreg；
Then, 8 prepregs are stacked, 18 μ electrolytic copper foil is respectively covered up and down, in vacuum press middle level
Pressure, lamination is 190 DEG C, 90 minutes, and copper-clad plate is made；
Finally obtained copper-clad plate is detected, detection performance is as shown in table 1.
Table 1
From table 1 from the point of view of the Comparative result of embodiment and comparative example, meet at the same time high phase ratio creepage tracking index (>
On the premise of 600V), three embodiments can be tested by alkali resistance, and two comparative examples can not be tested by alkali resistance；From
From the point of view of several Heat-tolerant indexes such as thermal shock number of times, resistance to immersed solder time, Td, the test result of embodiment is obviously higher than contrast
Example, copper-clad plate its phase ratio creepage tracking index (the CTI) >=600V for illustrating prepared by the resin combination proposed by the invention,
Heat-resist, alkali resistance is excellent, reach flame-retardancy requirements.
Embodiment 4
A kind of pcb board of the copper-clad plate containing obtained by embodiment 2.
Embodiment 5
A kind of electronic product of the copper-clad plate containing obtained by embodiment 2.
Above-described embodiment, simply presently preferred embodiments of the present invention, not for limiting the scope of the present invention, thus it is all with this
The equivalent change or modification that construction, feature and principle described in invention claim are done, all should be included in right of the present invention will
Within the scope of asking.
Claims (10)
1. a kind of resin combination, it is characterised in that：By weight, including 20~25 parts of phosphorous epoxy resin, brominated epoxy
10~15 parts of resin, 10~20 parts of cycloaliphatic epoxy resin, 25~30 parts of acid anhydrides, 10~15 parts of phosphorus-containing phenolic aldehyde, boehmite 5~15
Part；Wherein, the epoxide equivalent of the cycloaliphatic epoxy resin is 100~200g/eq.
2. resin combination according to claim 1, it is characterised in that：The acid anhydrides is tung oil acid anhydride, alkylene fourth two
Acid anhydrides, methyl hexahydrophthalic acid anhydride, hydrogenating methyl carbic anhydride, glutaric anhydride, poly- azelaic acid acid anhydride, poly- icosane diacid
One or more of mixtures in acid anhydrides, styrene-maleic anhydride copolymer.
3. resin combination according to claim 2, it is characterised in that：The knot of the styrene-maleic anhydride copolymer
Structure formula is as follows：。
4. resin combination according to claim 1, it is characterised in that：The epoxide equivalent of the phosphorous epoxy resin is
250~450g/eq, phosphorus content 1%~4%；The phosphorus content 5%~15% of the phosphorus-containing phenolic aldehyde, the brominated epoxy resin
Epoxide equivalent is 300~500g/eq, bromine content 15%~50%.
5. resin combination according to claim 1, it is characterised in that：Percentage, in addition to solidification promote
Agent 0.01%~0.1%.
6. resin combination according to claim 5, it is characterised in that：The curing accelerator is 2-methylimidazole, 1-
Methylimidazole, 2-ethyl-4-methylimidazole, 1- fluoro ethyls -2-ethyl-4-methylimidazole, 2- phenylimidazoles, 2- undecyl miaows
One or more of mixtures in azoles, 2- phenyl -4-methylimidazole.
7. copper-clad plate prepared by a kind of resin combination using as described in any one of claim 1~6.
8. a kind of preparation method of copper-clad plate as claimed in claim 7, it is characterised in that comprise the following steps：First by matching somebody with somebody
Side's amount is well mixed after weighing each component in the resin combination, adds curing accelerator and solvent is made into resin adhesive liquid；
Then reinforcing material is immersed in resin adhesive liquid, rear drying removes solvent, obtains prepreg；
The prepreg of gained is covered with metal foil, is laminated, the copper-clad plate is produced.
9. the preparation method of copper-clad plate according to claim 8, it is characterised in that：The solvent is acetone, butanone, hexamethylene
One kind or several in ketone, hexamethylene, glycol monoethyl ether, triglyme, toluene, dimethylbenzene, N,N-dimethylformamide
The mixture planted.
10. pcb board prepared by a kind of resin combination using as described in any one of claim 1~6.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510851763.1A CN105419231B (en) | 2015-11-27 | 2015-11-27 | The copper-clad plate and pcb board of a kind of resin combination and its making |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510851763.1A CN105419231B (en) | 2015-11-27 | 2015-11-27 | The copper-clad plate and pcb board of a kind of resin combination and its making |
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| CN105419231A CN105419231A (en) | 2016-03-23 |
| CN105419231B true CN105419231B (en) | 2017-11-03 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106496936A (en) * | 2016-10-20 | 2017-03-15 | 蓝星（成都）新材料有限公司 | A kind of benzoxazine resins and preparation method thereof |
| CN107793702B (en) * | 2017-09-12 | 2020-09-08 | 广东生益科技股份有限公司 | Resin composition and adhesive film and covering film made of same |
| CN117229596A (en) * | 2023-09-04 | 2023-12-15 | 忠信世纪电子材料(始兴)有限公司 | High heat-resistant copper-clad plate and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1833001A (en) * | 2003-06-06 | 2006-09-13 | 陶氏环球技术公司 | Curable flame retardant epoxy resin compositions |
| CN102093670A (en) * | 2010-12-23 | 2011-06-15 | 广东生益科技股份有限公司 | Halogen-free flame retardant epoxy resin composition and copper clad plate prepared from same |
| CN104371320A (en) * | 2014-11-11 | 2015-02-25 | 广东生益科技股份有限公司 | Thermosetting resin composition and prepreg and laminate prepared therefrom |
-
2015
- 2015-11-27 CN CN201510851763.1A patent/CN105419231B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1833001A (en) * | 2003-06-06 | 2006-09-13 | 陶氏环球技术公司 | Curable flame retardant epoxy resin compositions |
| CN102093670A (en) * | 2010-12-23 | 2011-06-15 | 广东生益科技股份有限公司 | Halogen-free flame retardant epoxy resin composition and copper clad plate prepared from same |
| CN104371320A (en) * | 2014-11-11 | 2015-02-25 | 广东生益科技股份有限公司 | Thermosetting resin composition and prepreg and laminate prepared therefrom |
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