CN115505237B - Epoxy resin glue solution, epoxy-based CEM-3 copper-clad plate and preparation method thereof - Google Patents
Epoxy resin glue solution, epoxy-based CEM-3 copper-clad plate and preparation method thereof Download PDFInfo
- Publication number
- CN115505237B CN115505237B CN202210985025.6A CN202210985025A CN115505237B CN 115505237 B CN115505237 B CN 115505237B CN 202210985025 A CN202210985025 A CN 202210985025A CN 115505237 B CN115505237 B CN 115505237B
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- Prior art keywords
- epoxy resin
- parts
- copper
- epoxy
- clad plate
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 48
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 48
- 239000003292 glue Substances 0.000 title claims abstract description 44
- 239000011190 CEM-3 Substances 0.000 title claims abstract description 30
- 239000004593 Epoxy Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims abstract description 23
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 11
- 239000010936 titanium Substances 0.000 claims abstract description 11
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000945 filler Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000000314 lubricant Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 42
- 239000004744 fabric Substances 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 229910000831 Steel Inorganic materials 0.000 claims description 18
- 239000010959 steel Substances 0.000 claims description 18
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 12
- 239000011162 core material Substances 0.000 claims description 12
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000007598 dipping method Methods 0.000 claims description 10
- 239000003365 glass fiber Substances 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011889 copper foil Substances 0.000 claims description 6
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 claims description 6
- 230000001804 emulsifying effect Effects 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 239000004745 nonwoven fabric Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 150000001412 amines Chemical group 0.000 claims description 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 3
- ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 2-phenyl-1h-imidazole Chemical compound C1=CNC(C=2C=CC=CC=2)=N1 ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 0.000 claims description 3
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 claims description 3
- 150000004985 diamines Chemical class 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims description 3
- HLPKYOCVWVMBMR-UHFFFAOYSA-N azane benzylbenzene Chemical compound N.N.C=1C=CC=CC=1CC1=CC=CC=C1 HLPKYOCVWVMBMR-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920013636 polyphenyl ether polymer Polymers 0.000 description 2
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical compound CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 239000004643 cyanate ester Substances 0.000 description 1
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/14—Layered products comprising a layer of metal next to a fibrous or filamentary layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
- B32B37/1018—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure using only vacuum
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- B32B38/08—Impregnating
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- B32B5/266—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary characterised by one fibrous or filamentary layer being a non-woven fabric layer next to one or more non-woven fabric layers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
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- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
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- B32B2307/30—Properties of the layers or laminate having particular thermal properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- 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
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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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2203/20—Applications use in electrical or conductive gadgets
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Fluid Mechanics (AREA)
- Laminated Bodies (AREA)
Abstract
The invention belongs to the technical field of copper-clad plates, and particularly relates to an epoxy resin glue solution, an epoxy-based CEM-3 copper-clad plate and a preparation method thereof, wherein the epoxy resin glue solution comprises the following components in parts by weight: brominated bisphenol a epoxy resin: 70-80 parts; hydrogenated bisphenol a epoxy resin: 10-15 parts of a lubricant; organic titanium epoxy resin: 10-15 parts of a lubricant; curing agent: 1-5 parts; solvent: 80-120 parts; silane coupling agent: 3-4 parts; and (3) filling: 120-140 parts. The invention adopts brominated bisphenol A epoxy resin as a main body, and mixes hydrogenated epoxy resin and organic titanium epoxy resin, thereby effectively reducing the cost, improving the heat resistance and the mechanical strength, and the added high dielectric constant filler ensures that the plate has high dielectric property and lower dielectric loss.
Description
Technical Field
The invention belongs to the technical field of copper-clad plates, and particularly relates to an epoxy resin glue solution, an epoxy-based CEM-3 copper-clad plate and a preparation method thereof.
Background
Today, the electronic industry is vigorously developed, and small intelligent devices such as semiconductors, capacitors and the like are frequently used, and 5G is promoted, so that various electronic products are continuously brought out. In order to achieve the goals of miniaturization, light weight and the like, and meet the requirements of high-frequency signal transmission, high transmission speed and high-frequency low loss, a copper-clad plate product with high dielectric constant and low loss must be developed.
The existing high-dielectric-constant copper-clad plate is generally manufactured by adding high-dielectric filler into polytetrafluoroethylene resin, cyanate resin or polyphenyl ether resin. Although the polytetrafluoroethylene resin has excellent dielectric property, the polytetrafluoroethylene resin has high melt viscosity, and the polytetrafluoroethylene copper-clad plate needs to be pressed and formed at a high temperature of 380-400 ℃ and has complex process; toluene is used in the manufacturing process of the polyphenyl ether resin-based copper-clad plate, so that the environment is polluted, and the problem of high melt viscosity is solved; the cyanate ester-based copper-clad plate has too high cost; the polyimide resin-based copper-clad plate has high cost and complex process.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an epoxy resin glue solution, an epoxy CEM-3 copper-clad plate and a preparation method thereof.
The specific technical scheme of the invention is as follows:
the first aim of the invention is to provide an epoxy resin glue solution which comprises the following components in parts by weight:
brominated bisphenol a epoxy resin: 70-80 parts; hydrogenated bisphenol a epoxy resin: 10-15 parts of a lubricant; organic titanium epoxy resin: 10-15 parts of a lubricant; curing agent: 1-5 parts; solvent: 80-120 parts; silane coupling agent: 3-4 parts; and (3) filling: 120-140 parts.
Further, the curing agent is an amine curing agent and an imidazole curing agent; the amine curing agent is one of dicyandiamide, diamine diphenyl methane or diamine diphenyl sulfone; the imidazole curing agent is one of 2-phenylimidazole, 2-methylimidazole or 2-ethyl-4-methylimidazole.
Further, the silane coupling agent is one of KH550, KH560 or DL 602.
Further, the filler is two of titanium dioxide, strontium titanate, aluminum oxide and talcum powder; the solvent comprises dimethylformamide, butanone and propylene glycol monomethyl ether.
Further, the preparation method of the epoxy resin glue solution comprises the following steps:
S1: mixing brominated bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, organic titanium epoxy resin and solvent, stirring and dissolving until the mixture is transparent to obtain a solution;
S2: adding a silane coupling agent and a curing agent into the solution in the step S1, stirring and dissolving the mixture to fully disperse the mixture, and stirring the mixture uniformly to obtain a mixed solution;
s3: and (2) adding two fillers into the mixed solution in the step (S2), uniformly stirring, and fully emulsifying to obtain the epoxy resin glue solution.
Further, the gel time of the epoxy resin glue solution prepared in the step S3 is 140-170S.
The second aim of the invention is to provide an epoxy CEM-3 copper-clad plate which is prepared by adopting the epoxy resin glue solution.
The third object of the invention is to provide a preparation method of an epoxy CEM-3 copper-clad plate, which comprises the following steps:
impregnating glass fiber cloth with the epoxy resin glue solution, and preparing a fabric prepreg by an oven;
Dipping the glass non-woven fabric into the epoxy resin glue solution, and preparing a core material prepreg by an oven;
and (3) stacking copper foil 1, fabric 1, core material 1-4 sheets and fabric 1 in sequence, placing the two steel plates between them, and placing them into a vacuum press to press so as to obtain the invented epoxy CEM-3 copper-clad plate.
Further, the glass fiber cloth is 7628 glass fiber cloth.
Further, the oven temperature for preparing the fabric prepreg and the core prepreg is 170 ℃, and the baking time is 3-5min.
Further, the glue content of the fabric prepreg is 41-44wt%; the glue content of the core prepreg is 80-84wt%.
Further, the pressing process parameters of the vacuum press are as follows: the temperature is 150-170 ℃, the pressure is 1.5-5 MPa, the time is 80-120 min, and the epoxy CEM-3 copper-clad plate is taken out after the temperature is reduced below 120 ℃.
The beneficial effects of the invention are as follows:
The invention adopts brominated bisphenol A epoxy resin with good technological performance and good dielectric property as a main body, and increases hydrogenated bisphenol A epoxy resin and organic titanium epoxy resin. Besides the performance of the general epoxy resin, the hydrogenated bisphenol A epoxy resin has the advantages that the benzene ring is converted into a saturated six-membered ring, no double bond is contained, the fracture defect of unsaturated double bonds is overcome, and the hydrogenated bisphenol A epoxy resin condensate has good weather resistance, corona resistance, tracking resistance and high dielectric strength; the organic titanium modified bisphenol A epoxy resin has greatly improved water absorption, moisture resistance, dielectric property and the like, and has large bond energy, good heat resistance and greatly reduced dielectric loss tangent. The high dielectric filler is adopted, so that the cured product has high dielectric constant, low dielectric loss and good mechanical strength. The epoxy resin glue solution adopted by the invention strengthens the overall comprehensive performance of the plate, and prepares the CEM-3 copper-clad plate with high dielectric constant and low dielectric loss.
Detailed Description
The principles and features of the present invention are described below in connection with examples, which are set forth only to illustrate the present invention and not to limit the scope of the invention.
Example 1
A preparation method of a high heat-resistant low-loss epoxy CEM-3 copper-clad plate comprises the following steps:
1. Preparation of epoxy resin adhesive:
S1: according to parts by weight, 70 parts of brominated bisphenol A epoxy resin, 15 parts of hydrogenated bisphenol A epoxy resin, 15 parts of organic titanium epoxy resin, 50 parts of dimethylformamide, 25 parts of butanone and 25 parts of propylene glycol monomethyl ether are mixed and then stirred for dissolving until the mixture is transparent, so as to obtain a dissolving solution;
S2: adding 3 parts of KH550 silane coupling agent, 1.5 parts of dicyandiamide and 0.3 part of 2-methylimidazole into the solution in the step S1, stirring to fully disperse the solution, and uniformly stirring to obtain a mixed solution;
S3: and (3) adding 60 parts of titanium dioxide and talcum powder into the mixed solution in the step (S2), uniformly stirring, and fully emulsifying to obtain the epoxy resin glue solution.
2. Preparation of epoxy CEM-3 copper-clad plate:
Dipping 7628 glass fiber cloth in the epoxy resin glue solution, and baking for 3min in a baking oven at 170 ℃ to obtain a prepreg with the glue content of 42.3wt%;
dipping 75g/m 2 of glass non-woven fabric into the epoxy resin glue solution, and baking for 4min in a baking oven at 170 ℃ to obtain a prepreg with the glue content of 81.8wt%;
and stacking copper foil 1, fabric 1, core material 1 and fabric 1 in sequence, placing the two steel plates between the two steel plates, placing the steel plates in a vacuum press, wherein the temperature of the vacuum press is 160 ℃, the pressure is 1.5MPa, the pressing time is 100min, and taking out the steel plates below 120 ℃ to obtain the high heat-resistant low-loss epoxy CEM-3 copper-clad plate.
Example 2
A preparation method of a high heat-resistant low-loss epoxy CEM-3 copper-clad plate comprises the following steps:
1. Preparation of epoxy resin adhesive:
S1: according to parts by weight, 75 parts of brominated bisphenol A epoxy resin, 12.5 parts of hydrogenated bisphenol A epoxy resin, 12.5 parts of organic titanium epoxy resin, 50 parts of dimethylformamide, 25 parts of butanone and 25 parts of propylene glycol monomethyl ether are mixed and then stirred for dissolving until the mixture is transparent, so as to obtain a dissolving solution;
S2: adding 3.5 parts of KH560 silane coupling agent, 3 parts of diamine diphenyl sulfone and 0.2 part of 2-phenylimidazole into the solution in the step S1, stirring to fully disperse the materials, and stirring uniformly to obtain a mixed solution;
S3: and (2) adding 65 parts of strontium titanate and aluminum oxide into the mixed solution in the step (S2), uniformly stirring, and fully emulsifying to obtain the epoxy resin glue solution.
2. Preparation of epoxy CEM-3 copper-clad plate:
Dipping 7628 glass fiber cloth in the epoxy resin glue solution, and baking for 3.5min in a baking oven at 170 ℃ to obtain a prepreg with the glue content of 43.1wt%;
Dipping 75g/m 2 of glass non-woven fabric into the epoxy resin glue solution, and baking for 3min in a baking oven at 170 ℃ to obtain a prepreg with the glue content of 82.4wt%;
And stacking copper foil 1, fabric 1, core material 2 and fabric 1 in sequence, placing the two steel plates between the two steel plates, placing the steel plates in a vacuum press, wherein the temperature of the vacuum press is 170 ℃, the pressure is 3MPa, the pressing time is 80min, and taking out the steel plates below 120 ℃ to obtain the high heat-resistant low-loss epoxy CEM-3 copper-clad plate.
Example 3
A preparation method of a high heat-resistant low-loss epoxy CEM-3 copper-clad plate comprises the following steps:
1. Preparation of epoxy resin adhesive:
S1: mixing 80 parts of brominated bisphenol A epoxy resin, 10 parts of hydrogenated bisphenol A epoxy resin, 10 parts of organic titanium epoxy resin, 50 parts of dimethylformamide, 25 parts of butanone and 25 parts of propylene glycol monomethyl ether, and stirring to dissolve until the mixture is transparent to obtain a dissolving solution;
S2: adding 4 parts of DL602 silane coupling agent, 2.5 parts of diaminodiphenyl methane and 0.5 part of 2-ethyl-4-methylimidazole into the solution in the step S1, stirring to fully disperse the components, and uniformly stirring to obtain a mixed solution;
S3: and (2) adding 70 parts of titanium dioxide and aluminum oxide into the mixed solution in the step (S2), uniformly stirring, and fully emulsifying to obtain the epoxy resin glue solution.
2. Preparation of epoxy CEM-3 copper-clad plate:
Dipping 7628 glass fiber cloth in the epoxy resin glue solution, and baking for 4min in a baking oven at 170 ℃ to obtain a prepreg with the glue content of 42.7wt%;
Dipping 75g/m 2 of glass non-woven fabric into the epoxy resin glue solution, and baking for 5min in a baking oven at 170 ℃ to obtain a prepreg with the glue content of 83.2wt%;
And stacking copper foil 1, fabric 1, core 3 and fabric 1 in sequence, placing the two steel plates between the two steel plates, placing the steel plates in a vacuum press, wherein the temperature of the vacuum press is 150 ℃, the pressure is 5MPa, the pressing time is 120min, and taking out the steel plates below 120 ℃ to obtain the high heat-resistant low-loss epoxy CEM-3 copper-clad plate.
Comparative example
A preparation method of an epoxy CEM-3 copper-clad plate comprises the following steps:
1. Preparation of epoxy resin adhesive:
s1: 100 parts of brominated bisphenol A epoxy resin, 150 parts of dimethylformamide, 25 parts of butanone and 25 parts of propylene glycol monomethyl ether are mixed and stirred for dissolving until the mixture is transparent, so as to obtain a dissolving solution;
s2: adding 3 parts of KH550 silane coupling agent, 1.5 parts of dicyandiamide and 0.3 part of dimethyl imidazole into the solution in the step S1, stirring to fully disperse the components, and uniformly stirring to obtain a mixed solution;
s3: and (3) adding 60 parts of aluminum hydroxide and silicon micropowder into the mixed solution in the step (S2), uniformly stirring, and fully emulsifying to obtain the epoxy resin glue solution.
2. Preparation of epoxy CEM-3 copper-clad plate:
dipping 7628 glass fiber cloth in the epoxy resin glue solution, and baking for 4min in a baking oven at 170 ℃ to obtain a prepreg with the glue content of 41.9wt%;
Dipping 75g/m 2 of glass non-woven fabric into the epoxy resin glue solution, and baking for 5min in a baking oven at 170 ℃ to obtain a prepreg with the glue content of 82.6wt%;
and stacking copper foil 1, fabric 1, core material 1 and fabric 1 in sequence, placing the two steel plates between the two steel plates, placing the steel plates in a vacuum press, pressing at 165 ℃ under 4MPa for 90min, and taking out the steel plates below 120 ℃ to obtain the epoxy CEM-3 copper-clad plate.
The test method comprises the following steps:
(1) Dielectric constant: GB/T4722-2017-8.5;
(2) Dielectric loss (10G): GB/T4722-2017-8.5;
(3)T288:GB/T 4722-2017-6.11;
(4) Peel strength (N/mm): GB/T4722-2017-7.2.1;
(5) Flame retardancy: GB/T4722-2017-6.4.1;
the test experimental data of each example and comparative example are shown in table 1.
Table 1 test experimental data for each of examples and comparative examples
Test item | Example 1 | Example 2 | Example 3 | Comparative example |
Dielectric constant | 8.7 | 9.4 | 10.1 | 7.3 |
Dielectric loss (10G) | 0.0077 | 0.0075 | 0.0069 | 0.0106 |
T288/min | >10 | >10 | >10 | 6 |
Peel strength N/mm | 1.53 | 1.48 | 1.42 | 1.47 |
Flame retardancy | FV-0 | FV-0 | FV-0 | FV-0 |
As can be seen from comparison of the test experimental data in table 1, the copper clad laminate of example 3 has the highest dielectric constant of 10.1, the lowest dielectric loss of 0.0069, examples 2 and 1 times, and the worst is the comparative example. And the heat resistance of the examples is obviously better than that of the comparative examples, and other comprehensive properties are good.
It will be understood that the application has been described in terms of several embodiments, and that various changes and equivalents may be made to these features and embodiments by those skilled in the art without departing from the spirit and scope of the application. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the application without departing from the essential scope thereof. Therefore, it is intended that the application not be limited to the particular embodiment disclosed, but that the application will include all embodiments falling within the scope of the appended claims.
Claims (7)
1. The epoxy resin glue solution is characterized by comprising the following components in parts by weight:
Brominated bisphenol a epoxy resin: 70-80 parts; hydrogenated bisphenol a epoxy resin: 10-15 parts of a lubricant; organic titanium epoxy resin: 10-15 parts of a lubricant; curing agent: 1-5 parts; solvent: 80-120 parts; silane coupling agent: 3-4 parts; and (3) filling: 120-140 parts;
The curing agent is an amine curing agent and an imidazole curing agent; the amine curing agent is one of dicyandiamide, diamine diphenyl methane or diamine diphenyl sulfone; the imidazole curing agent is one of 2-phenylimidazole, 2-methylimidazole or 2-ethyl-4-methylimidazole; the silane coupling agent is one of KH550, KH560 or DL 602; the filler is two of titanium dioxide, strontium titanate, aluminum oxide and talcum powder; the solvent comprises dimethylformamide, butanone and propylene glycol monomethyl ether;
the preparation method of the epoxy resin glue solution comprises the following steps:
S1: mixing brominated bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, organic titanium epoxy resin and solvent, stirring and dissolving until the mixture is transparent to obtain a solution;
S2: adding a silane coupling agent and a curing agent into the solution in the step S1, stirring and dissolving the mixture to fully disperse the mixture, and stirring the mixture uniformly to obtain a mixed solution;
s3: and (2) adding two fillers into the mixed solution in the step (S2), uniformly stirring, fully emulsifying, and obtaining the epoxy resin glue solution with the gelling time of 140-170S.
2. An epoxy CEM-3 copper-clad plate, which is characterized in that the copper-clad plate is prepared by adopting the epoxy resin glue solution as in claim 1.
3. A method for preparing the epoxy CEM-3 copper-clad plate according to claim 2, which is characterized by comprising the following steps:
impregnating glass fiber cloth with the epoxy resin glue solution, and preparing a fabric prepreg by an oven;
Dipping the glass non-woven fabric into the epoxy resin glue solution, and preparing a core material prepreg by an oven;
And (3) stacking copper foil 1, fabric 1, core material 1-4 and fabric 1 in sequence, placing the two steel plates between them, and placing them into a vacuum press to press so as to obtain the epoxy CEM-3 copper-clad plate.
4. The method for producing an epoxy-based CEM-3 copper-clad plate according to claim 3, wherein the glass fiber cloth is 7628 glass fiber cloth.
5. The method for preparing the epoxy CEM-3 copper-clad plate according to claim 3, wherein the oven temperature for preparing the fabric prepreg and the core prepreg is 170 ℃ and the baking time is 3-5min.
6. The method for preparing the epoxy CEM-3 copper-clad plate according to claim 3, wherein the glue content of the fabric prepreg is 41-44wt%; the glue content of the core prepreg is 80-84wt%.
7. The method for preparing the epoxy CEM-3 copper-clad plate according to claim 3, wherein the pressing process parameters of the vacuum press are as follows: the temperature is 150-170 ℃, the pressure is 1.5-5 MPa, the time is 80-120 min, and the epoxy CEM-3 copper-clad plate is taken out after the temperature is reduced below 120 ℃.
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JPH06182932A (en) * | 1992-12-21 | 1994-07-05 | Toshiba Chem Corp | Copper-plated laminated plate |
CN103289322A (en) * | 2013-03-01 | 2013-09-11 | 广东丹邦科技有限公司 | Dielectric compound, embedded capacitor film and its preparation method |
CN109517538A (en) * | 2018-11-22 | 2019-03-26 | 广东莱尔新材料科技股份有限公司 | A kind of adhesive and preparation method thereof, Flexible copper-clad plate and preparation method thereof |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH06182932A (en) * | 1992-12-21 | 1994-07-05 | Toshiba Chem Corp | Copper-plated laminated plate |
CN103289322A (en) * | 2013-03-01 | 2013-09-11 | 广东丹邦科技有限公司 | Dielectric compound, embedded capacitor film and its preparation method |
CN109517538A (en) * | 2018-11-22 | 2019-03-26 | 广东莱尔新材料科技股份有限公司 | A kind of adhesive and preparation method thereof, Flexible copper-clad plate and preparation method thereof |
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