CN106589815A - Nanometer sepiolite powder modified epoxy resin and fiberglass fabric composite printed circuit board material and preparation method thereof - Google Patents
Nanometer sepiolite powder modified epoxy resin and fiberglass fabric composite printed circuit board material and preparation method thereof Download PDFInfo
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- CN106589815A CN106589815A CN201611096873.2A CN201611096873A CN106589815A CN 106589815 A CN106589815 A CN 106589815A CN 201611096873 A CN201611096873 A CN 201611096873A CN 106589815 A CN106589815 A CN 106589815A
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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
- 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
- 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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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The invention discloses a nanometer sepiolite powder modified epoxy resin and fiberglass fabric composite printed circuit board material, which is prepared from the following raw materials in parts by weight: 32 to 34 parts of a 1080 fiberglass fabric, 40 to 42 parts of E-51 epoxy resin, 29 to 30 of phenolic resin, 0.3 to 0.4 part of 4-ethylimidazole, 20 to 22 parts of carbon nanotubes, 2.3 to 2.6 parts of a vinylidene fluoride-hexafluoro propylene copolymer, 25 to 30 parts of butadiene, a proper amount of hydrogenated gasoline, 0.01 to 0.02 part of nickel naphthenate, 0.4 to 0.5 part of triisobutylaluminium, 0.7 to 0.8 part of boron trifluoride diethyl ether, 1.2 to 1.4 parts of methyl tin mercaptide, 2 to 2.4 parts of nanometer sepiolite powder and 0.8 to 1 part of ethoxylated lanolin. According to the nanometer sepiolite powder modified epoxy resin and fiberglass fabric composite printed circuit board material, the nanometer sepiolite powder is used, so that the heat resistance and adhesive strength of the epoxy resin can be improved; the methyl tin mercaptide is adsorbed into pores of the nanometer sepiolite powder, so that the heat stability of the material is improved.
Description
Technical field
The present invention relates to printed circuit board (PCB) prepreg technical field, more particularly to a kind of Nano sepiolite powder modified epoxy tree
Fat glass-fiber-fabric complex 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-resisting heat aging performance electronics industry is had it is important
Meaning.Herein by with reference to various research meanses, have studied epoxy prepreg storage ageing process in chemical and physical features
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 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 keeping uniform in solidification process epoxide group and consuming, phenyl ring peak intensity is held essentially constant.
And then it is aging to have studied storage of the epoxy prepreg under different temperatures and humidity using NIR, find with storage temperature and aging
The increase of time, is accordingly increased to illustrate that NIR aging to the storage of epoxy prepreg can be carried out effectively with respect to curing degree
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 polarizing 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 affected 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 its interface water suction is substantially suppressed.Circuit malfunction test, the test result of scanning electron microscope/energy disperse spectroscopy (SEM/EDX) are said
Bright, amphipathic oligomeric silane coupling agent can suppress the generation that conductive anodic filament under hygrothermal environment (CAF) fails, and then improve electricity
The reliability of road plate.In addition, compared with circuit malfunction test, 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
Resistance to water be improved, but epoxy resin property is more crisp, it is bad with the caking property of glass surface, by vibrations can peel off,
The stability in use of circuit board is affected, needs to improve, in addition it is also necessary to improve the adhesion strength 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 Nano sepiolite powder modified epoxy
Glass-fiber-fabric complex printed-circuit board material and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of Nano sepiolite powder modified epoxy glass-fiber-fabric complex printed-circuit board material, by the raw material system of following weight portion
Into：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 nanometer
Pipe 20-22, vinylidene fluoride-hexafluoropropylene copolymer 2.3-2.6, butadiene 25-30, appropriate hydrogasoline, nickel naphthenate 0.01-
0.02nd, triisobutyl aluminium 0.4-0.5, boron trifluoride diethyl etherate 0.7-0.8, thiol methyl tin 1.2-1.4, Nano sepiolite powder 2-
2.4th, Wool wax alcohols,ethoxylated 0.8-1.
The preparation method of the Nano sepiolite powder modified epoxy glass-fiber-fabric complex printed-circuit board material, including with
Lower step：
（1）Butadiene is added in hydrogasoline, the solution of 100-105g/L is configured to, CNT is added, is 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,
Boron trifluoride diethyl etherate reacts 10-15 minutes, obtains glue；
（2）1080 glass-fiber-fabrics are immersed into above-mentioned glue and shakes stirring reaction 2-2.3 hour, take out 1080 glass-fiber-fabrics, be put into self-styled
Bag, carries out irradiation, and absorbed dose are 68-78kGy, obtains modified 1080 glass-fiber-fabrics；
（3）It is by thiol methyl tin, Nano sepiolite powder mix homogeneously then uniform with Wool wax alcohols,ethoxylated grinding, then with E-51
Epoxy resin, phenolic resin, mix homogeneously, add other residual componentss mix homogeneously, obtain resin glue and are coated with modified
On 1080 glass-fiber-fabrics, resin glue is 1.9-2 with the weight ratio of glass-fiber-fabric:1,4-5 minutes are processed at 168-170 DEG C, 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 defined 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, on glass-fiber-fabric surface continuous thin film is formed, and compares the discontinuous partial dot contact for being directly added into CNT, is defined
Continuous passage of heat, improves the heat dispersion and intensity of material.By using Nano sepiolite powder, it is possible to increase asphalt mixtures modified by epoxy resin
The thermostability and adhesion strength of fat, thiol methyl tin adsorbs in Nano sepiolite powder hole, improves the heat stability of material,
It is modified with Wool wax alcohols,ethoxylated again, improves dispersing uniformity of the sepiolite powder in resin.
Specific embodiment
A kind of Nano sepiolite powder modified epoxy glass-fiber-fabric complex printed-circuit board material, by following weight portion（It is public
Jin）Raw material make：1080 glass-fiber-fabrics 32, E-51 epoxy resin 40, phenolic resin 29,4- ethyl imidazol(e)s 0.3, CNT
20th, vinylidene fluoride-hexafluoropropylene copolymer 2.3, butadiene 25, appropriate hydrogasoline, nickel naphthenate 0.01, triisobutyl aluminium
0.4th, boron trifluoride diethyl etherate 0.7, thiol methyl tin 1.2, Nano sepiolite powder 2, Wool wax alcohols,ethoxylated 0.8.
The preparation method of the Nano sepiolite powder modified epoxy glass-fiber-fabric complex printed-circuit board material, including with
Lower step：
（1）Butadiene is added in hydrogasoline, the solution of 100g/L is configured to, CNT is added, is 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, is entered
Row irradiation, absorbed dose are 68kGy, obtain modified 1080 glass-fiber-fabrics；
（3）It is by thiol methyl tin, Nano sepiolite powder mix homogeneously then uniform with Wool wax alcohols,ethoxylated grinding, then with E-51
Epoxy resin, phenolic resin, mix homogeneously, add other residual componentss mix homogeneously, obtain resin glue and are coated with modified
On 1080 glass-fiber-fabrics, resin glue is 1.9 with the weight ratio of glass-fiber-fabric:1, process 4 minutes at 168 DEG C, obtain final product.
The electrical insulating property out-of-service time of the embodiment circuit board is 2497h, and impact strength is, 16.8KJ/cm-2, bending is by force
Spend for 18.8MPa.
Claims (2)
1. a kind of Nano sepiolite powder modified epoxy glass-fiber-fabric complex printed-circuit board material, it is characterised in that：By following
The raw material of weight portion 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, CNT 20-22, vinylidene fluoride-hexafluoropropylene copolymer 2.3-2.6, butadiene 25-30, hydrogasoline are fitted
Amount, nickel naphthenate 0.01-0.02, triisobutyl aluminium 0.4-0.5, boron trifluoride diethyl etherate 0.7-0.8, thiol methyl tin 1.2-1.4,
Nano sepiolite powder 2-2.4, Wool wax alcohols,ethoxylated 0.8-1.
2. the preparation of Nano sepiolite powder modified epoxy glass-fiber-fabric complex printed-circuit board material according to claim 1
Method, it is characterised in that comprise the following steps：
（1）Butadiene is added in hydrogasoline, the solution of 100-105g/L is configured to, CNT is added, is 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,
Boron trifluoride diethyl etherate reacts 10-15 minutes, obtains glue；
（2）1080 glass-fiber-fabrics are immersed into above-mentioned glue and shakes stirring reaction 2-2.3 hour, take out 1080 glass-fiber-fabrics, be put into self-styled
Bag, carries out irradiation, and absorbed dose are 68-78kGy, obtains modified 1080 glass-fiber-fabrics；
（3）It is by thiol methyl tin, Nano sepiolite powder mix homogeneously then uniform with Wool wax alcohols,ethoxylated grinding, then with E-51
Epoxy resin, phenolic resin, mix homogeneously, add other residual componentss mix homogeneously, obtain resin glue and are coated with modified
On 1080 glass-fiber-fabrics, resin glue is 1.9-2 with the weight ratio of glass-fiber-fabric:1,4-5 minutes are processed at 168-170 DEG C, obtain final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611096873.2A CN106589815A (en) | 2016-12-02 | 2016-12-02 | Nanometer sepiolite powder modified epoxy resin and fiberglass fabric composite printed circuit board material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611096873.2A CN106589815A (en) | 2016-12-02 | 2016-12-02 | Nanometer sepiolite powder modified epoxy resin and fiberglass fabric composite printed circuit board material and preparation method thereof |
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| Publication Number | Publication Date |
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| CN106589815A true CN106589815A (en) | 2017-04-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611096873.2A Pending CN106589815A (en) | 2016-12-02 | 2016-12-02 | Nanometer sepiolite powder modified epoxy resin and fiberglass fabric composite printed circuit board material and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
-
2016
- 2016-12-02 CN CN201611096873.2A patent/CN106589815A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
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Application publication date: 20170426 |