CN115044186A - Black resin glue solution, preparation method of prepreg, copper-clad plate and application - Google Patents
Black resin glue solution, preparation method of prepreg, copper-clad plate and application Download PDFInfo
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- CN115044186A CN115044186A CN202210838689.XA CN202210838689A CN115044186A CN 115044186 A CN115044186 A CN 115044186A CN 202210838689 A CN202210838689 A CN 202210838689A CN 115044186 A CN115044186 A CN 115044186A
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- Prior art keywords
- copper
- clad plate
- resin glue
- glue solution
- prepreg
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229920005989 resin Polymers 0.000 title claims abstract description 35
- 239000011347 resin Substances 0.000 title claims abstract description 35
- 239000003292 glue Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229920001690 polydopamine Polymers 0.000 claims abstract description 38
- 239000002131 composite material Substances 0.000 claims abstract description 30
- 239000004593 Epoxy Substances 0.000 claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 32
- 238000005303 weighing Methods 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000004744 fabric Substances 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- 239000007853 buffer solution Substances 0.000 claims description 10
- 239000011889 copper foil Substances 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 9
- 229920000647 polyepoxide Polymers 0.000 claims description 9
- FWLHAQYOFMQTHQ-UHFFFAOYSA-N 2-N-[8-[[8-(4-aminoanilino)-10-phenylphenazin-10-ium-2-yl]amino]-10-phenylphenazin-10-ium-2-yl]-8-N,10-diphenylphenazin-10-ium-2,8-diamine hydroxy-oxido-dioxochromium Chemical compound O[Cr]([O-])(=O)=O.O[Cr]([O-])(=O)=O.O[Cr]([O-])(=O)=O.Nc1ccc(Nc2ccc3nc4ccc(Nc5ccc6nc7ccc(Nc8ccc9nc%10ccc(Nc%11ccccc%11)cc%10[n+](-c%10ccccc%10)c9c8)cc7[n+](-c7ccccc7)c6c5)cc4[n+](-c4ccccc4)c3c2)cc1 FWLHAQYOFMQTHQ-UHFFFAOYSA-N 0.000 claims description 8
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 8
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- MCHZKGNHFPNZDP-UHFFFAOYSA-N 2-aminoethane-1,1,1-triol;hydrochloride Chemical compound Cl.NCC(O)(O)O MCHZKGNHFPNZDP-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229920000767 polyaniline Polymers 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000002390 rotary evaporation Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 2
- 239000007983 Tris buffer Substances 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 2
- AHZMUXQJTGRNHT-UHFFFAOYSA-N [4-[2-(4-cyanatophenyl)propan-2-yl]phenyl] cyanate Chemical compound C=1C=C(OC#N)C=CC=1C(C)(C)C1=CC=C(OC#N)C=C1 AHZMUXQJTGRNHT-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 229920013636 polyphenyl ether polymer Polymers 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08L71/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
- C08L71/12—Polyphenylene oxides
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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
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- 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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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/08—Impregnating
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- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/164—Drying
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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
- B32B5/00—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
- B32B5/02—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 structural features of a fibrous or filamentary layer
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- B32B5/00—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
- B32B5/22—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
- B32B5/24—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
- B32B5/26—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
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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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- B32B2250/00—Layers arrangement
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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
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
- B32B2260/021—Fibrous or filamentary layer
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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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- B32B2307/00—Properties of the layers or laminate
- 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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- B32B2457/00—Electrical equipment
- B32B2457/08—PCBs, i.e. printed circuit boards
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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
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2371/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
- C08J2371/12—Polyphenylene oxides
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
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- 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
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0041—Optical brightening agents, organic pigments
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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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- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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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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- 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
Abstract
A preparation method of a black resin glue solution, a prepreg, a copper-clad plate and an application are disclosed. The copper-clad plate prepared by utilizing the polydopamine modified nigrosine epoxy composite material has small color difference, excellent voltage resistance, insulating property and heat resistance, and can be applied to a MiniLED substrate.
Description
Technical Field
The invention relates to the technical field of copper-clad plates, in particular to a preparation method of a black resin glue solution and a prepreg, a copper-clad plate and application.
Background
The Mini LED (defined as an LED device with the chip size between 50 and 200 mu m, a unit which consists of a Mini LED pixel array and a driving circuit and has the pixel center spacing of 0.3 to 1.5 mm) display is a novel display technology based on inorganic semiconductor light emitting diodes, and because the Mini LED has excellent display brightness, fast photoelectric response speed and long service life, the LED backlight is gradually developed to the Mini LED backlight at present. The main characteristics of the Mini LED are that the unit area density of the LED is higher, and the unit size of a light source is smaller, so that the distance between the points of the Mini LED lamp beads is required to be smaller than 1 mm or even smaller. In order to meet the above requirements, the Mini LED PCB substrate needs to have good light-shielding properties and color uniformity, and further needs to have excellent heat resistance, excellent surface resistance, insulation resistance, voltage resistance, and other properties.
At present, most of black copper clad plates are prepared by adding black dyes such as carbon black or aniline black and the like into common epoxy resin to prepare a common epoxy resin black laminated plate. Although the substrate has a good light shading effect, the black dye such as carbon black or aniline black in the resin composition has the defects of high conductivity, easy adsorption and agglomeration and the like, so that the prepared black laminate is easy to form micro short circuit and even short circuit between circuits in the PCB processing process, and has the problem of large color difference; in addition, the heat resistance of the common epoxy resin composition is difficult to satisfy the requirement of the Mini LED substrate on high heat resistance.
Disclosure of Invention
Aiming at the problems of large color difference, voltage resistance, insulation resistance and insufficient heat resistance of the existing black copper-clad plate, the black resin glue solution, the preparation method of the prepreg, the copper-clad plate and the application are provided. The copper-clad plate prepared by utilizing the polydopamine modified nigrosine epoxy composite material has small color difference, excellent voltage resistance, insulating property and heat resistance, and can be applied to a Mini LED substrate.
The technical scheme for solving the technical problems is as follows:
the invention aims to prepare a black resin glue solution, which comprises a polydopamine modified nigrosine epoxy composite material as a raw material.
Preferably, the preparation method of the black resin glue solution comprises the following steps:
s1: weighing dopamine hydrochloride, adding the dopamine hydrochloride into a trihydroxymethylaminomethane buffer solution, and preparing a trihydroxymethylaminomethane-hydrochloric acid buffer solution;
s2: weighing aniline black, adding the aniline black into a trihydroxymethylaminomethane-hydrochloric acid buffer solution prepared in S1, stirring and reacting for 20-40 h at room temperature, centrifuging at 10000rpm by using a centrifuge, removing supernatant, washing precipitates for 5-10 min by using deionized water, and drying the washed precipitates in vacuum to obtain black powdery solid poly-dopamine-modified aniline black;
s3: weighing the polydopamine modified nigrosine in the S2, adding the polydopamine modified nigrosine into an ethanol-containing conical flask, and performing ultrasonic dispersion for 2-4 h;
s4: weighing epoxy resin, adding the epoxy resin into an S3 ultrasonically dispersed conical flask, carrying out ultrasonic treatment for 0.5-2 h, and carrying out rotary evaporation at 60-75 ℃ by using a rotary evaporator to remove ethanol to obtain a mixture A;
s5: weighing polyetheramine, adding the polyetheramine into the mixture A of S4, mechanically stirring for 3-12 min, and vacuumizing by using a vacuum drying oven at 50-60 ℃ to obtain a mixture B;
s6: pouring the mixture B in the S5 into a polytetrafluoroethylene mold, curing for 2-4 h at 80-120 ℃, and taking out the cured composite material, namely the polydopamine modified nigrosine epoxy composite material;
s7: mixing the polydopamine modified nigrosine epoxy composite material in the S6 with the following substances according to the mass percentage to obtain black resin glue solution,
wherein the polydopamine modified nigrosine epoxy composite material is 5-15 parts.
The second purpose of the invention is to prepare a prepreg, and the preparation method comprises the following steps: and (3) taking at least 1 piece of glass cloth, and soaking the glass cloth into the prepared black resin glue solution, wherein the baking temperature is 145-180 ℃, and the baking time is 4-8 min, so as to obtain the prepreg.
The invention also aims to prepare a copper-clad plate, and the preparation method comprises the following steps: and (3) taking at least 1 prepreg prepared above, attaching copper foil, and placing the prepreg in a vacuum hot press preheated to 140-180 ℃ to obtain the copper-clad plate.
Preferably, the vacuum hot press is pressed according to the following formula:
vacuum degree: 0-0.01 Mpa, pressure: 1.0 MP-2.0 MP, heating rate: 3-6 ℃/min, hot plate temperature: 190 ℃ and 230 ℃, and the pressing time is 120 ℃ and 180 min.
Preferably, the copper foil is single-sided covered or double-sided covered.
Preferably, the copper foil has a thickness of 10 μm to 30 μm.
The fourth purpose of the invention is to apply the copper-clad plate to a substrate of a Mini LED.
Compared with the prior art, the invention has the following technical effects:
1. the polydopamine modified nigrosine epoxy composite material is prepared and added into the black resin glue solution, the black resin glue solution is used for preparing the prepreg, and the prepared copper-clad plate has excellent heat resistance and good insulating property, so that the heat resistance of a resin system is improved, and the insulating property of the resin system is improved.
2. The black resin glue solution is added with the polydopamine modified nigrosine epoxy composite material, so that the finally prepared copper-clad plate has smaller color difference deviation compared with the traditional nigrosine composite material.
3. Polyphenyl ether and bisphenol A cyanate ester resin are also selected in the black resin glue solution, so that the dielectric loss and the dielectric constant of a resin system are reduced, and the copper-clad plate has better mechanical strength, high heat resistance, high Tg and high light shading property and simultaneously improves the color stability and reduces the chromatic aberration and the light transmittance when being matched with the polydopamine modified nigrosine epoxy composite material, and can be applied to a substrate of a Mini LED.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example one
1. The black resin glue solution is prepared from a raw material of a polydopamine modified nigrosine epoxy composite material.
The preparation method comprises the following steps:
s1: weighing 0.3g of dopamine hydrochloride, adding the dopamine hydrochloride into 300mL of tris buffer solution, and preparing tris-hydrochloric acid buffer solution with the pH value of 8.5;
s2: weighing 30mg of nigrosine, adding the nigrosine into a trihydroxymethyl aminomethane-hydrochloric acid buffer solution prepared in S1, stirring and reacting for 20h at room temperature, centrifuging at 10000rpm by using a centrifuge, discarding supernatant, washing precipitates for 5min by using deionized water, and drying the washed precipitates in vacuum to obtain black powdery solid polydopamine modified nigrosine;
s3: weighing 1g of polydopamine modified nigrosine in S2, adding the polydopamine modified nigrosine into a conical flask containing 200mL of ethanol, and performing ultrasonic dispersion for 2 hours to fully disperse the polydopamine modified nigrosine;
s4: weighing 20g of epoxy resin E44, adding into an S3 ultrasonically dispersed conical flask, carrying out ultrasonic treatment for 0.5h, and carrying out rotary evaporation at 60 ℃ by using a rotary evaporator to remove ethanol to obtain a mixture A;
s5: weighing 5g of polyetheramine D-230, adding into the mixture A of S4, mechanically stirring for 3min, and vacuumizing by using a vacuum drying oven at 50 ℃ to remove air bubbles to obtain a mixture B;
s6: pouring the mixture B in the S5 into a polytetrafluoroethylene mold, curing at 80 ℃ for 2h, and taking out the cured composite material, namely the polydopamine modified nigrosine epoxy composite material containing 0.5 mass percent of polydopamine modified nigrosine;
s7: mixing the polydopamine modified nigrosine epoxy composite material in the S6 with the following substances according to the mass percentage to obtain black resin glue solution,
wherein the polydopamine modified nigrosine epoxy composite material is 5 parts.
2. The preparation method of the prepreg comprises the following steps: and (3) taking 4 pieces of glass cloth, and soaking the glass cloth into the prepared black resin glue solution, wherein the baking temperature is 145 ℃, and the baking time is 4min, so that a prepreg is obtained.
3. The preparation method of the copper-clad plate comprises the following steps: taking 4 prepregs, attaching copper foils with the thickness of 18 μm on the front and the back of each prepreg, placing the prepregs in a vacuum hot press preheated to 140 ℃, and keeping the prepregs at the temperature of 200 ℃ for 120min within 10 min; and (4) increasing the pressure to 1.0MPa within 1min, and maintaining the pressure for 120min to obtain the copper-clad plate.
Example two
1. The black resin glue solution is prepared from a raw material of a polydopamine modified nigrosine epoxy composite material.
The preparation method comprises the following steps:
s1: weighing 0.6g of dopamine hydrochloride, adding the dopamine hydrochloride into 600mL of tris buffer solution, and preparing tris-hydrochloric acid buffer solution with the pH value of 8.5;
s2: weighing 60mg of nigrosine, adding the nigrosine into a trihydroxymethyl aminomethane-hydrochloric acid buffer solution prepared in S1, stirring and reacting for 40h at room temperature, centrifuging at 10000rpm by using a centrifuge, removing supernatant, washing precipitates for 10min by using deionized water, and drying the washed precipitates in vacuum to obtain black powdery solid polydopamine modified nigrosine;
s3: weighing 2g of polydopamine modified nigrosine in S2, adding the polydopamine modified nigrosine into a conical flask containing 100mL of ethanol, and performing ultrasonic dispersion for 2 hours to fully disperse the polydopamine modified nigrosine;
s4: weighing 80g of epoxy resin E44, adding into an S3 ultrasonically dispersed conical flask, carrying out ultrasonic treatment for 0.5h, and carrying out rotary evaporation at 60 ℃ by using a rotary evaporator to remove ethanol to obtain a mixture A;
s5: weighing 20g of polyetheramine D-230, adding into the mixture A of S4, mechanically stirring for 12min, and vacuumizing by using a vacuum drying oven at 60 ℃ to remove air bubbles to obtain a mixture B;
s6: pouring the mixture B in the S5 into a polytetrafluoroethylene mold, curing for 4 hours at 120 ℃, and taking out the cured composite material, namely the polydopamine modified nigrosine epoxy composite material containing 2 mass percent of polydopamine modified nigrosine;
s7: mixing the polydopamine modified nigrosine epoxy composite material in the S6 with the following substances according to the mass percentage to obtain black resin glue solution,
wherein the polydopamine modified nigrosine epoxy composite material is 15 parts.
2. The preparation method of the prepreg comprises the following steps: and (3) taking 6 pieces of glass cloth, and soaking the glass cloth into the prepared black resin glue solution, wherein the baking temperature is 160 ℃, and the baking time is 5min, so as to obtain a prepreg.
3. The preparation method of the copper-clad plate comprises the following steps: taking 6 prepregs, attaching copper foils with the thickness of 18 μm on the front and back prepregs respectively, placing in a vacuum hot press preheated to 180 ℃, and keeping the temperature at 230 ℃ for 180min within 10 min; and (4) increasing the pressure to 1.5MPa within 1min, and maintaining the pressure for 130min to obtain the copper-clad plate.
Comparative example 1
1. The black resin glue solution without the polydopamine modified nigrosine epoxy composite material is prepared by the following raw materials,
the black resin glue solution can be obtained by mixing the substances according to the mass percentage.
2. The preparation method of the prepreg comprises the following steps: and (3) taking 4 pieces of glass cloth, and soaking the glass cloth into the prepared black resin glue solution, wherein the baking temperature is 145 ℃, and the baking time is 4min, so that a prepreg is obtained.
3. The preparation method of the copper-clad plate comprises the following steps: taking 4 prepregs, attaching copper foils with the thickness of 18 μm on the front and the back of each prepreg, placing the prepregs in a vacuum hot press preheated to 140 ℃, and keeping the prepregs at the temperature of 200 ℃ for 120min within 10 min; and (4) increasing the pressure to 1.0MPa within 1min, and maintaining the pressure for 120min to obtain the copper-clad plate.
Comparative example No. two
1. The black resin glue solution without the polydopamine modified nigrosine epoxy composite material is prepared by the following raw materials,
the black resin glue solution can be obtained by mixing the substances according to the mass percentage.
2. The preparation method of the prepreg comprises the following steps: and (3) taking 6 pieces of glass cloth, and soaking the glass cloth into the prepared black resin glue solution, wherein the baking temperature is 160 ℃, and the baking time is 5min, so as to obtain a prepreg.
3. The preparation method of the copper-clad plate comprises the following steps: taking 6 prepregs, attaching copper foils with the thickness of 18 μm on the front and back prepregs respectively, placing in a vacuum hot press preheated to 180 ℃, and keeping the temperature at 230 ℃ for 180min within 10 min; and (4) increasing the pressure to 1.5MPa within 1min, and maintaining the pressure for 130min to obtain the copper-clad plate.
The test results of the copper-clad plate prepared by the method are shown in the following table (namely the performance of the black copper-clad plate prepared from the polydopamine modified nigrosine epoxy composite material is compared with that of the copper-clad plate prepared from common nigrosine):
the results in the above table show that the copper-clad plate prepared from the black resin glue solution containing the dopamine modified nigrosine epoxy composite material has improved mechanical properties, reduced dielectric loss and dielectric constant, and reduced light transmittance compared with the comparative example according to the experimental results of the embodiment on the premise of not affecting other properties, and can be applied to a Mini LED substrate.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (8)
1. The black resin glue solution is characterized in that the raw material of the black resin glue solution comprises a polydopamine modified nigrosine epoxy composite material.
2. The black resin glue solution according to claim 1, wherein the preparation method comprises:
s1: weighing dopamine hydrochloride, adding the dopamine hydrochloride into a trihydroxymethylaminomethane buffer solution, and preparing a trihydroxymethylaminomethane-hydrochloric acid buffer solution;
s2: weighing aniline black, adding the aniline black into a trihydroxymethylaminomethane-hydrochloric acid buffer solution prepared in S1, stirring and reacting for 20-40 h at room temperature, centrifuging at 10000rpm by using a centrifuge, removing supernatant, washing precipitates for 5-10 min by using deionized water, and drying the washed precipitates in vacuum to obtain black powdery solid poly-dopamine-modified aniline black;
s3: weighing the polydopamine modified nigrosine in the S2, adding the polydopamine modified nigrosine into an ethanol-containing conical flask, and performing ultrasonic dispersion for 2-4 h;
s4: weighing epoxy resin, adding the epoxy resin into an S3 ultrasonically dispersed conical flask, carrying out ultrasonic treatment for 0.5-2 h, and carrying out rotary evaporation at 60-75 ℃ by using a rotary evaporator to remove ethanol to obtain a mixture A;
s5: weighing polyetheramine, adding the polyetheramine into the mixture A of S4, mechanically stirring for 3-12 min, and vacuumizing by using a vacuum drying oven at 50-60 ℃ to obtain a mixture B;
s6: pouring the mixture B in the S5 into a polytetrafluoroethylene mold, curing for 2-4 h at 80-120 ℃, and taking out the cured composite material, namely the polydopamine modified nigrosine epoxy composite material;
s7: mixing the polydopamine modified nigrosine epoxy composite material in the S6 with the following substances according to the mass percentage to obtain black resin glue solution,
wherein the polydopamine modified nigrosine epoxy composite material is 5-15 parts.
3. A preparation method of a prepreg is characterized in that at least 1 piece of glass cloth is taken, the glass cloth is soaked in the prepared black resin glue solution, the baking temperature is 145-180 ℃, and the baking time is 4-8 min, so that the prepreg is obtained.
4. The copper-clad plate is characterized in that the preparation method comprises the following steps: and (3) taking at least 1 prepreg prepared above, attaching copper foil, and placing the prepreg in a vacuum hot press preheated to 140-180 ℃ to obtain the copper-clad plate.
5. The copper-clad plate according to claim 4, wherein the vacuum thermocompressor is pressed according to the following formula:
vacuum degree: 0-0.01 Mpa, pressure: 1.0 MP-2.0 MP, heating rate: 3-6 ℃/min, hot plate temperature: 190 ℃ and 230 ℃, and the pressing time is 120 ℃ and 180 min.
6. The copper-clad plate according to claim 4, wherein the copper foil is single-sided covered or double-sided covered.
7. The copper-clad plate according to claim 6, wherein the thickness of the copper foil is 10 μm to 30 μm.
8. Use of the copper-clad plate according to any one of claims 4 to 7, wherein the copper-clad plate is used for a substrate of a Mini LED.
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