CN106751533A - A kind of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material and preparation method thereof - Google Patents
A kind of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material and preparation method thereof Download PDFInfo
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- CN106751533A CN106751533A CN201611096874.7A CN201611096874A CN106751533A CN 106751533 A CN106751533 A CN 106751533A CN 201611096874 A CN201611096874 A CN 201611096874A CN 106751533 A CN106751533 A CN 106751533A
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F259/00—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00
- C08F259/08—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00 on to polymers containing fluorine
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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
- C08L2201/08—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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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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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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses a kind of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material, it is made from the following raw materials in parts by weight：1080 glass-fiber-fabrics 32 34, E-51 epoxy resin 40 42, phenolic resin 29 30,4 ethyl imidazol(e)s 0.3 0.4, CNT 20 22, vinylidene hexafluoropropylene copolymer 2.3 2.6, butadiene 25 30, appropriate hydrogasoline, nickel naphthenate 0.01 0.02, triisobutyl aluminium 0.4 0.5, BFEE 0.7 0.8, micron order zinc oxide 2.3 2.6, LiFePO4 1 1.3, zinc diamyldithiocarbamate 1.3 1.5.By the present invention in that with micron order zinc oxide, LiFePO4, zinc diamyldithiocarbamate, material anti-light aging and heat aging are improve, also with good antibiotic property and wearability.
Description
Technical field
It is multiple the present invention relates to printed circuit board (PCB) prepreg technical field, more particularly to a kind of anti-aging epoxy resin glass-fiber-fabric
Close printed circuit board material and preparation method thereof.
Background technology
Printed circuit board (PCB) is the critical piece in electronic product, and its q＆r is heavy to closing for electronic product
Will.Epoxy prepreg (Epoxy Prepreg) is the main raw material(s) for producing printed circuit board (PCB) at present.Storage is aging will be to epoxy
The performance of prepreg produces significant impact, and then has influence on the quality of printed circuit board (PCB).And the wet-heat resisting of printed circuit board (PCB) is old
Change performance and directly influence the reliability of electronic product, characterize and improve its moisture-resistant heat aging performance have to electronics industry it is important
Meaning.Herein by various research meanses are combined, epoxy prepreg chemical and physical features in ageing process is stored are have studied
Change, so as to establish the aging quality supervision system of storage of epoxy prepreg, and be successfully applied to electronics industry.
By comparing the methods such as differential scanning calorimetry (DSC), middle infrared spectrum (Mid-IR) and near infrared spectrum (NIR), NIR is found
Can be very good to characterize the functional group's change before and after epoxy prepreg solidification.NIR results show 4530cm-1The epoxy peak at place and
4620cm-1Phenyl ring peak there is good resolution ratio and the overlap without other absworption peaks to disturb.Constant temperature at 100 DEG C of epoxy prepreg
The NIR tracking results of solidification show that keep uniform consumption in solidification process epoxide group, phenyl ring peak intensity is held essentially constant.
And then it is aging using NIR to have studied storage of the epoxy prepreg under different temperatures and humidity, find with storage temperature and aging
The increase of time, explanation NIR is accordingly increased to respect to curing degree aging to the storage of epoxy prepreg can be carried out effectively
Monitoring.Corresponding with solidification conversion ratio increase, the processing viscosity of epoxy prepreg is with storage aging temperature and the increase of time
Significantly improve, gel time accordingly shortens.Epoxy prepreg after dynamic mechanical analysis (DMA) discovery storage is aging occurs in that two
Individual glass transition temperature, binding time differentiates light scattering (TRSL) and the means such as petrographic microscope (OM), it was demonstrated that storage is always
Epoxy prepreg there occurs phase separation during change.Further improved by introducing amphipathic oligomeric silane coupling agent herein
The interface performance of resin and glass in printed circuit board (PCB), so as to improve reliability of the printed circuit board (PCB) in hygrothermal environment.Adopt
Synthesize a kind of amphipathic oligomeric silane coupling agent with silane coupler and octyl phenyl polyglycol ether, by gel chromatography
(GPC), the test specification such as IR, gas chromatography mass spectrometry chromatograph (GC-MS) its epoxy prepreg processing characteristics is not influenceed substantially.
The result of contact angle test shows that amphipathic coupling agent can significantly reduce contact angle of the resin to glass in epoxy prepreg.
Water absorption test finds, although the equilibrium water absorption of epoxy prepreg slightly rises after solidification, due to the work of amphipathic coupling agent
With the water suction of its interface is substantially suppressed.Circuit malfunction test, the test result of ESEM/energy disperse spectroscopy (SEM/EDX) are said
Bright, amphipathic oligomeric silane coupling agent can suppress the generation of conductive anodic filament (CAF) failure under hygrothermal environment, and then improve electricity
The reliability of road plate.In addition, compared with circuit malfunction is tested, interface water suction analysis can easily and effectively evaluate printed circuit board (PCB)
Resistance to CAF performances.
《Aging and printed circuit board (PCB) the hydrothermal aging research of storage of epoxy prepreg》The printed circuit board (PCB) that one text is obtained
Water resistance be improved, but epoxy resin property is more crisp, the caking property with glass surface is bad, by vibrations can peel off,
The stability in use of circuit board is influenceed, it is necessary to improve, in addition it is also necessary to improve the ageing resistance of circuit board.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of anti-aging epoxy resin glass-fiber-fabric is combined
Printed circuit board material and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material, is made from the following raw materials in parts by weight：1080 glass
Fine cloth 32-34, E-51 epoxy resin 40-42, phenolic resin 29-30,4- ethyl imidazol(e) 0.3-0.4, CNT 20-22, partially
It is viton copolymers 2.3-2.6, butadiene 25-30, appropriate hydrogasoline, nickel naphthenate 0.01-0.02, three different
Butyl aluminium 0.4-0.5, BFEE 0.7-0.8, micron order zinc oxide 2.3-2.6, LiFePO4 1-1.3, diamyl two
Zinc thiocarbamate 1.3-1.5.
The preparation method of the anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material, comprises the following steps：
（1）By in butadiene addition hydrogasoline, the solution of 100-105g/L is configured to, adds CNT, stirred,
Be put into water bath with thermostatic control, be heated to 75-78 DEG C, add vinylidene fluoride-hexafluoropropylene copolymer, nickel naphthenate, triisobutyl aluminium,
BFEE reacts 10-15 minutes, obtains glue；
（2）1080 glass-fiber-fabrics are immersed into above-mentioned glue vibrations stirring reaction 2-2.3 hours, 1080 glass-fiber-fabrics are taken out, is put into self-styled
Bag, is irradiated, and absorbed dose of radiation is 68-78kGy, obtains modified 1080 glass-fiber-fabrics；
（3）By E-51 epoxy resin, phenolic resin, it is well mixed, adds other residual components and be well mixed, obtains resin
Glue is coated with modified 1080 glass-fiber-fabrics, and resin glue is 1.9-2 with the weight ratio of glass-fiber-fabric:1, processed at 168-170 DEG C
4-5 minutes, obtain final product.
It is an advantage of the invention that：The present invention is changed using vinylidene fluoride-hexafluoropropylene copolymer, butadiene to glass-fiber-fabric
Property, waterproofing protection film, and good toughness are formd on glass-fiber-fabric surface, it is firmly bonded with glass-fiber-fabric, it is not easily stripped, improve ring
Oxygen tree fat and the interface fastness of glass-fiber-fabric, slow down the aqueous corrosion at interface, extend the service life of material, by using carbon nanometer
Pipe, continuous film is formed on glass-fiber-fabric surface, is contacted compared to the discontinuous partial dot for being directly added into CNT, is formd
Continuous passage of heat, improves the heat dispersion and intensity of material.By using micron order zinc oxide, LiFePO4, diamyl
Base zinc dithiocarbamate, improves circuit board material anti-light aging and heat aging, also with good antibiotic property and
Wearability.
Specific embodiment
A kind of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material, by following weight portion（Kilogram）Raw material system
Into：1080 glass-fiber-fabrics 32, E-51 epoxy resin 40, phenolic resin 29,4- ethyl imidazol(e)s 0.3, CNT 20, vinylidene-
Hexafluoropropylene copolymer 2.3, butadiene 25, appropriate hydrogasoline, nickel naphthenate 0.01, triisobutyl aluminium 0.4, boron trifluoride second
Ether 0.7, micron order zinc oxide 2.3, LiFePO4 1, zinc diamyldithiocarbamate 1.3.
The preparation method of the anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material, comprises the following steps：
（1）By in butadiene addition hydrogasoline, the solution of 100g/L is configured to, adds CNT, stirred, be put into
Water bath with thermostatic control, is heated to 75 DEG C, adds vinylidene fluoride-hexafluoropropylene copolymer, nickel naphthenate, triisobutyl aluminium, borontrifluoride
Borate ether reacts 10 minutes, obtains glue；
（2）1080 glass-fiber-fabrics are immersed into above-mentioned glue vibrations stirring reaction 2 hours, 1080 glass-fiber-fabrics are taken out, valve bag is put into, entered
Row irradiation, absorbed dose of radiation is 68kGy, obtains modified 1080 glass-fiber-fabrics；
（3）By E-51 epoxy resin, phenolic resin, it is well mixed, adds other residual components and be well mixed, obtains resin
Glue is coated with modified 1080 glass-fiber-fabrics, and resin glue is 1.9 with the weight ratio of glass-fiber-fabric:1, processed 4 minutes at 168 DEG C,
Obtain final product.
The electrical insulating property out-of-service time of the embodiment circuit board is 2345h, and impact strength is, 17.2KJ/cm-2, bending is by force
It is 19.7MPa to spend.
Claims (2)
1. a kind of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material, it is characterised in that：By the original of following weight portion
Material is made：1080 glass-fiber-fabric 32-34, E-51 epoxy resin 40-42, phenolic resin 29-30,4- ethyl imidazol(e) 0.3-0.4, carbon
Nanotube 20-22, vinylidene fluoride-hexafluoropropylene copolymer 2.3-2.6, butadiene 25-30, appropriate hydrogasoline, nickel naphthenate
0.01-0.02, triisobutyl aluminium 0.4-0.5, BFEE 0.7-0.8, micron order zinc oxide 2.3-2.6, LiFePO4
1-1.3, zinc diamyldithiocarbamate 1.3-1.5.
2. the preparation method of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material according to claim 1, it is special
Levy is to comprise the following steps：
（1）By in butadiene addition hydrogasoline, the solution of 100-105g/L is configured to, adds CNT, stirred,
Be put into water bath with thermostatic control, be heated to 75-78 DEG C, add vinylidene fluoride-hexafluoropropylene copolymer, nickel naphthenate, triisobutyl aluminium,
BFEE reacts 10-15 minutes, obtains glue；
（2）1080 glass-fiber-fabrics are immersed into above-mentioned glue vibrations stirring reaction 2-2.3 hours, 1080 glass-fiber-fabrics are taken out, is put into self-styled
Bag, is irradiated, and absorbed dose of radiation is 68-78kGy, obtains modified 1080 glass-fiber-fabrics；
（3）By E-51 epoxy resin, phenolic resin, it is well mixed, adds other residual components and be well mixed, obtains resin
Glue is coated with modified 1080 glass-fiber-fabrics, and resin glue is 1.9-2 with the weight ratio of glass-fiber-fabric:1, processed at 168-170 DEG C
4-5 minutes, obtain final product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611096874.7A CN106751533A (en) | 2016-12-02 | 2016-12-02 | A kind of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611096874.7A CN106751533A (en) | 2016-12-02 | 2016-12-02 | A kind of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material and preparation method thereof |
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| CN106751533A true CN106751533A (en) | 2017-05-31 |
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| CN201611096874.7A Pending CN106751533A (en) | 2016-12-02 | 2016-12-02 | A kind of anti-aging epoxy resin glass-fiber-fabric complex printed-circuit board material and preparation method thereof |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597416A (en) * | 2008-06-02 | 2009-12-09 | 南亚塑胶工业股份有限公司 | The composition of circuit support plate and manufacture method thereof |
| CN101914265A (en) * | 2010-07-24 | 2010-12-15 | 广州美嘉伟华电子材料有限公司 | A kind of non-halogen phosphorus-containing flame retardant high-frequency epoxy resin based composition and the application in bonding sheet and copper-clad plate thereof |
| CN102174242A (en) * | 2011-03-25 | 2011-09-07 | 苏州生益科技有限公司 | Halogen-free resin composition and prepreg and laminated board made of same |
| CN102276961A (en) * | 2011-07-22 | 2011-12-14 | 苏州生益科技有限公司 | Halogen-free phosphorus-free epoxy resin composition, and semi-curing sheet and laminated sheet manufactured thereby |
| CN103694639A (en) * | 2013-12-19 | 2014-04-02 | 广东生益科技股份有限公司 | Halogen-free anti-aging epoxy resin composition and method for preparing cover film by using same |
| CN104327323A (en) * | 2014-09-30 | 2015-02-04 | 青岛东泰诚恩新材料科技发展有限公司 | Butadiene rubber |
| CN105082669A (en) * | 2015-09-23 | 2015-11-25 | 李会录 | Production method of epoxy glass fiber cloth copper-clad plate |
| CN104151639B (en) * | 2014-08-20 | 2016-04-20 | 南京信息工程大学 | A kind of damp composite material and preparation method thereof |
-
2016
- 2016-12-02 CN CN201611096874.7A patent/CN106751533A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597416A (en) * | 2008-06-02 | 2009-12-09 | 南亚塑胶工业股份有限公司 | The composition of circuit support plate and manufacture method thereof |
| CN101914265A (en) * | 2010-07-24 | 2010-12-15 | 广州美嘉伟华电子材料有限公司 | A kind of non-halogen phosphorus-containing flame retardant high-frequency epoxy resin based composition and the application in bonding sheet and copper-clad plate thereof |
| CN102174242A (en) * | 2011-03-25 | 2011-09-07 | 苏州生益科技有限公司 | Halogen-free resin composition and prepreg and laminated board made of same |
| CN102276961A (en) * | 2011-07-22 | 2011-12-14 | 苏州生益科技有限公司 | Halogen-free phosphorus-free epoxy resin composition, and semi-curing sheet and laminated sheet manufactured thereby |
| CN103694639A (en) * | 2013-12-19 | 2014-04-02 | 广东生益科技股份有限公司 | Halogen-free anti-aging epoxy resin composition and method for preparing cover film by using same |
| CN104151639B (en) * | 2014-08-20 | 2016-04-20 | 南京信息工程大学 | A kind of damp composite material and preparation method thereof |
| CN104327323A (en) * | 2014-09-30 | 2015-02-04 | 青岛东泰诚恩新材料科技发展有限公司 | Butadiene rubber |
| CN105082669A (en) * | 2015-09-23 | 2015-11-25 | 李会录 | Production method of epoxy glass fiber cloth copper-clad plate |
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Application publication date: 20170531 |