CN114932727A - Heat-resistant hydrocarbon resin-based copper-clad plate and preparation method thereof - Google Patents
Heat-resistant hydrocarbon resin-based copper-clad plate and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- 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
- B32B37/10—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- 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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- 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
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/241—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres
- C08J5/244—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres using glass fibres
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0366—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement reinforced, e.g. by fibres, fabrics
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/022—Processes for manufacturing precursors of printed circuits, i.e. copper-clad substrates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- 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
- B32B2260/04—Impregnation, embedding, or binder material
- B32B2260/046—Synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
- B32B2262/101—Glass fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
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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
- C08J2379/00—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 C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- 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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
-
- 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
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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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
- 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
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/548—Silicon-containing compounds containing sulfur
Abstract
The invention discloses a heat-resistant hydrocarbon resin-based copper-clad plate and a preparation method thereof. In the composite filler, silicon carbide modified by a silane coupling agent KH590 is added into an impregnating compound for compounding; the chemical connection of the dispersed black and sodium alginate combined modified silicon carbide powder is realized, the fluidity of the slurry can be effectively improved, and the modified silicon carbide is more uniformly distributed in the impregnating compound; cyano groups are introduced into resin molecules, so that the high-temperature resistance of the impregnating compound is better enhanced; the nanometer neodymium oxide is used as a modifier of thermal oxidation stability, and can enhance the heat resistance and stability of the copper-clad plate; the heat-resistant hydrocarbon resin-based copper-clad plate disclosed by the invention has better heat resistance, can effectively ensure the stability of the performance of the heat-resistant hydrocarbon resin-based copper-clad plate when the heat-resistant hydrocarbon resin-based copper-clad plate is used at a high temperature, and can effectively ensure the normal work of the heat-resistant hydrocarbon resin-based copper-clad plate.
Description
Technical Field
The invention relates to the technical field of copper-clad plates, in particular to a heat-resistant hydrocarbon resin-based copper-clad plate and a preparation method thereof.
Background
The copper-clad plate is a plate-shaped material which is prepared by soaking electronic glass fiber cloth or other reinforcing materials with resin, covering copper foil on one surface or two surfaces and performing hot pressing, and is called a copper-clad laminate, and is called the copper-clad laminate for short; the copper-clad plate manufacturing industry is a rising industry, has wide development prospect along with the development of electronic information and communication industry, and the manufacturing technology is a high and new technology with multiple disciplines of interdigitation, interpenetration and mutual promotion. The quality, performance, processability during manufacture, manufacturing cost, level of manufacture, and long-term reliability and stability of printed circuit boards are largely dependent on the copper clad laminate. The hydrocarbon resin generally refers to petroleum resin (thermoplastic resin), which is a thermoplastic resin produced by pretreating, polymerizing, distilling and the like C5 and C9 fractions by-produced by petroleum cracking, and is not a high polymer but an oligomer with a molecular weight of 300-3000.
The existing carbon-hydrogen resin-based copper-clad plate has poor heat resistance and seriously reduces the self performance when being used at a high temperature.
Disclosure of Invention
In order to overcome the defects in the prior art, the embodiment of the invention provides a heat-resistant hydrocarbon resin-based copper-clad plate and a preparation method thereof.
A heat-resistant hydrocarbon resin-based copper-clad plate comprises electronic glass fiber cloth, a dipping material and a copper foil; the impregnating material comprises the following components in percentage by weight: 24.9-25.9% of bismaleimide resin, 14.8-15.8% of cyanate ester resin, 14.6-15.6% of polytetrafluoroethylene, 1.8-2.4% of curing agent, 10.7-11.7% of composite filler and the balance of solvent.
Further, the composite filler comprises the following components in percentage by weight: 48.6-49.6% of silicon carbide, 10.6-11.2% of nano neodymium oxide, 2.6-3.2% of silane coupling agent KH590, 1.6-2.6% of disperse black and the balance of sodium alginate.
Further, the impregnation material comprises the following components in percentage by weight: 24.9 percent of bismaleimide resin, 14.8 percent of cyanate ester resin, 14.6 percent of polytetrafluoroethylene, 1.8 percent of curing agent, 10.7 percent of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 48.6 percent of silicon carbide, 10.6 percent of nano neodymium oxide, 2.6 percent of silane coupling agent KH590, 1.6 percent of disperse black and the balance of sodium alginate.
Further, the impregnating compound comprises the following components in percentage by weight: 25.9 percent of bismaleimide resin, 15.8 percent of cyanate ester resin, 15.6 percent of polytetrafluoroethylene, 2.4 percent of curing agent, 11.7 percent of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 49.6 percent of silicon carbide, 11.2 percent of nano neodymium oxide, 3.2 percent of silane coupling agent KH590, 2.6 percent of disperse black and the balance of sodium alginate.
Further, the impregnating compound comprises the following components in percentage by weight: 25.4% of bismaleimide resin, 15.3% of cyanate ester resin, 15.1% of polytetrafluoroethylene, 2.1% of curing agent, 11.2% of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 49.1 percent of silicon carbide, 10.9 percent of nano neodymium oxide, 2.9 percent of silane coupling agent KH590, 2.1 percent of disperse black and the balance of sodium alginate.
Further, the curing agent is prepared by compounding two of 2-ethyl-4-methylimidazole, 1-methylimidazole, imidazole and benzimidazole; the organic solvent is prepared by compounding two of styrene, perchloroethylene, trichloroethylene, ethylene glycol ether and triethanolamine.
A preparation method of a heat-resistant hydrocarbon resin-based copper-clad plate comprises the following specific processing steps:
the method comprises the following steps: weighing the bismaleimide resin, the cyanate ester resin, the polytetrafluoroethylene, the curing agent, the solvent and the silicon carbide, the nanometer neodymium oxide, the silane coupling agent KH590, the disperse black and the sodium alginate in the composite filler in parts by weight;
step two: mixing the silicon carbide, the nano neodymium oxide, the silane coupling agent KH590, the disperse black and the sodium alginate in the step one, and carrying out water bath ultrasonic treatment for 50-60 minutes to obtain a composite filler;
step three: carrying out mixed water bath ultrasonic treatment on one fourth of the composite filler in the second step and one half of bismaleimide resin in the first step for 30-40 minutes to obtain a mixture A;
step four: carrying out mixed water bath ultrasonic treatment on one fourth of the composite filler in the second step and one half of the cyanate ester resin in the first step for 20-30 minutes to obtain a mixture B;
step five: mixing the polytetrafluoroethylene, the curing agent, the solvent, the mixture A in the step three, the mixture B in the step three, the residual bismaleimide resin, the cyanate ester resin and the composite filler in the step two, and stirring at a high speed for 50-60 minutes to obtain an impregnating compound;
step six: dipping the dipping material prepared in the fifth step of the electronic glass fiber cloth for 20-28 min, curing at 140-160 ℃ for 5-7 h, and cooling to room temperature after curing to obtain a heat-resistant hydrocarbon resin-based prepreg;
step seven: and symmetrically superposing the heat-resistant hydrocarbon resin-based prepreg and the copper foil, putting the heat-resistant hydrocarbon resin-based prepreg and the copper foil into a hot press, and carrying out hot-pressing treatment to obtain the heat-resistant hydrocarbon resin-based copper-clad plate.
Further, in the second step, the water bath temperature is 40-50 ℃, the ultrasonic frequency is 32-38 KHz, and the ultrasonic power is 800-900W; in the third step, the temperature of the water bath is 50-60 ℃, the ultrasonic frequency is 1.6-1.8 MHz, and the ultrasonic power is 300-400W; in the fourth step, the water bath temperature is 60-70 ℃, the ultrasonic frequency is 1.2-1.4 MHz, and the ultrasonic power is 400-500W; in the fifth step, the stirring speed is 800-900 r/min; in the seventh step, the hot pressing temperature of the hot press is set to be 220-260 ℃ and the pressure is set to be 80-100 kg/cm 2 The pressing time is 16-20 h.
Further, in the second step, the water bath temperature is 40 ℃, the ultrasonic frequency is 32KHz, and the ultrasonic power is 800W; in the third step, the temperature of the water bath is 50 ℃, the ultrasonic frequency is 1.6MHz, and the ultrasonic power is 300W; in the fourth step, the temperature of the water bath is 60 ℃, the ultrasonic frequency is 1.2MHz, and the ultrasonic power is 400W; in the fifth step, the stirring speed is 800 r/min; in the seventh step, the hot pressing temperature of the hot press is set to 220 ℃ and the pressure is set to 80kg/cm 2 And the pressing time is 16 h.
Further, in the second step, the water bath temperature is 45 ℃, the ultrasonic frequency is 35KHz, and the ultrasonic power is 850W; in the third step, the temperature of the water bath is 55 ℃, the ultrasonic frequency is 1.7MHz, and the ultrasonic power is 350W; in the fourth step, the temperature of the water bath is 65 ℃, the ultrasonic frequency is 1.3MHz, and the ultrasonic power is 450W; in the fifth step, the stirring speed is 850 r/min; in the seventh step, the hot pressing temperature of the hot press is set to 240 ℃, and the pressure is set to 90kg/cm 2 The pressing time is 18 h.
The invention has the technical effects and advantages that:
1. according to the heat-resistant hydrocarbon resin-based copper-clad plate processed by adopting the raw material formula, silicon carbide in the composite filler is subjected to surface modification treatment under the action of a silane coupling agent KH590, and the silicon carbide modified by the silane coupling agent KH590 is added into an impregnating compound to neutralize bismaleimide resin, cyanate ester resin and polytetrafluoroethylene for compounding; the static mechanical property and the wear resistance of the composite material can be effectively improved, and the composite material still keeps good electrical insulation property; the silicon carbide in the composite filler is subjected to modification treatment in the dispersion black and the sodium alginate, the dispersion black and the sodium alginate are combined to modify the silicon carbide powder to realize chemical connection, the fluidity of the slurry can be effectively improved, and the slurry does not have extrusion and self-polymerization phenomena, so that the modified silicon carbide is more uniformly distributed in the impregnating compound; cyanate resin is used in the impregnating compound, the thermal stability of the cyano-containing resin molecules is higher, and the introduction of cyano into the resin molecules is more beneficial to enhancing the high-temperature resistance of the impregnating compound, so that the high-temperature resistance of the copper-clad plate is improved; the nanometer neodymium oxide is used as a modifier of thermal oxidation stability, and the neodymium oxide modified bismaleimide resin, cyanate resin and polytetrafluoroethylene are prepared by a mechanical blending method, so that the thermal oxidation stability of the impregnating compound can be further enhanced, and the heat resistance and stability of the copper-clad plate can be further enhanced; the heat-resistant hydrocarbon resin-based copper-clad plate disclosed by the invention has better heat resistance, can effectively ensure the stability of the performance of the heat-resistant hydrocarbon resin-based copper-clad plate when the heat-resistant hydrocarbon resin-based copper-clad plate is used at a high temperature, and can effectively ensure the normal work of the heat-resistant hydrocarbon resin-based copper-clad plate;
2. according to the invention, the raw materials in the composite filler are subjected to blending and water bath ultrasonic treatment, so that the materials in the composite filler can be effectively ensured to react quickly, and the modification treatment effect on silicon carbide is ensured; part of the composite filler and part of the bismaleimide resin are subjected to pre-mixing water bath ultrasonic treatment, so that the modification treatment effect of the composite filler on the bismaleimide resin can be effectively enhanced, and the heat resistance of the copper-clad plate is further ensured; part of the composite filler and part of the cyanate ester resin are subjected to pre-mixing water bath ultrasonic treatment, so that the modification treatment effect of the composite filler on the cyanate ester resin can be effectively enhanced, and the heat resistance of the copper-clad plate is further ensured; mixing all the raw materials of the impregnating material to prepare the impregnating material; dipping the electronic glass fiber cloth in a dipping material, solidifying and cooling to obtain a heat-resistant hydrocarbon resin-based prepreg; and carrying out hot-pressing compounding on the heat-resistant hydrocarbon resin-based prepreg and the copper foil to prepare the heat-resistant hydrocarbon resin-based copper-clad plate.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a heat-resistant hydrocarbon resin-based copper-clad plate, which comprises electronic glass fiber cloth, a dipping material and a copper foil; the impregnating material comprises the following components in percentage by weight: 24.9 percent of bismaleimide resin, 14.8 percent of cyanate ester resin, 14.6 percent of polytetrafluoroethylene, 1.8 percent of curing agent, 10.7 percent of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 48.6 percent of silicon carbide, 10.6 percent of nano neodymium oxide, 2.6 percent of silane coupling agent KH590, 1.6 percent of disperse black and the balance of sodium alginate;
the curing agent is prepared by compounding two of 2-ethyl-4-methylimidazole and benzimidazole in equal proportion; the organic solvent is prepared by compounding styrene and perchloroethylene in equal proportion;
the invention also provides a preparation method of the heat-resistant hydrocarbon resin-based copper-clad plate, which comprises the following specific processing steps:
the method comprises the following steps: weighing the bismaleimide resin, the cyanate ester resin, the polytetrafluoroethylene, the curing agent, the solvent and the silicon carbide, the nano neodymium oxide, the silane coupling agent KH590, the disperse black and the sodium alginate in parts by weight in the impregnating compound;
step two: mixing the silicon carbide, the nano neodymium oxide, the silane coupling agent KH590, the disperse black and the sodium alginate in the step one, and carrying out water bath ultrasonic treatment for 50-60 minutes to obtain a composite filler;
step three: carrying out mixed water bath ultrasonic treatment on one fourth of the composite filler in the second step and one half of bismaleimide resin in the first step for 30-40 minutes to obtain a mixture A;
step four: carrying out mixed water bath ultrasonic treatment on one fourth of the composite filler in the second step and one half of the cyanate ester resin in the first step for 20-30 minutes to obtain a mixture B;
step five: mixing the polytetrafluoroethylene, the curing agent, the solvent, the mixture A in the step three, the mixture B in the step three, the residual bismaleimide resin, the cyanate ester resin and the composite filler in the step two, and stirring at a high speed for 50-60 minutes to obtain an impregnating compound;
step six: dipping the dipping material prepared in the fifth step of the electronic glass fiber cloth for 20-28 min, curing at 140-160 ℃ for 5-7 h, and cooling to room temperature after curing to obtain a heat-resistant hydrocarbon resin-based prepreg;
step seven: and symmetrically superposing the heat-resistant hydrocarbon resin-based prepreg and the copper foil, putting the heat-resistant hydrocarbon resin-based prepreg and the copper foil into a hot press, and carrying out hot-pressing treatment to obtain the heat-resistant hydrocarbon resin-based copper-clad plate.
In the second step, the water bath temperature is 40 ℃, the ultrasonic frequency is 32KHz, and the ultrasonic power is 800W; in the third step, the temperature of the water bath is 50 ℃, the ultrasonic frequency is 1.6MHz, and the ultrasonic power is 300W; in the fourth step, the temperature of the water bath is 60 ℃, the ultrasonic frequency is 1.2MHz, and the ultrasonic power is 400W; in the fifth step, the stirring speed is 800 r/min; in the seventh step, the hot pressing temperature of the hot press is set to 220 ℃ and the pressure is set to 80kg/cm 2 And the pressing time is 16 h.
Example 2:
different from the embodiment 1, the impregnating material comprises the following components in percentage by weight: 25.9 percent of bismaleimide resin, 15.8 percent of cyanate ester resin, 15.6 percent of polytetrafluoroethylene, 2.4 percent of curing agent, 11.7 percent of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 49.6 percent of silicon carbide, 11.2 percent of nano neodymium oxide, 3.2 percent of silane coupling agent KH590, 2.6 percent of disperse black and the balance of sodium alginate.
Example 3:
different from the embodiments 1-2, the impregnating material comprises the following components in percentage by weight: 25.4% of bismaleimide resin, 15.3% of cyanate ester resin, 15.1% of polytetrafluoroethylene, 2.1% of curing agent, 11.2% of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 49.1 percent of silicon carbide, 10.9 percent of nano neodymium oxide, 2.9 percent of silane coupling agent KH590, 2.1 percent of disperse black and the balance of sodium alginate.
Example 4:
different from the embodiment 3, in the second step, the water bath temperature is 50 ℃, the ultrasonic frequency is 38KHz, and the ultrasonic power is 900W; in the third step, the temperature of the water bath is 60 ℃, the ultrasonic frequency is 1.8MHz, and the ultrasonic power is 400W; in the fourth step, the temperature of the water bath is 70 ℃, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 500W; in the fifth step, the stirring speed is 900 r/min; in the seventh step, the hot pressing temperature of the hot press is set to 260 ℃ and the pressure is set to 100kg/cm 2 And the pressing time is 20 h.
Example 5:
different from the embodiment 3, in the second step, the water bath temperature is 45 ℃, the ultrasonic frequency is 35KHz, and the ultrasonic power is 850W; in the third step, the temperature of the water bath is 55 ℃, the ultrasonic frequency is 1.7MHz, and the ultrasonic power is 350W; in the fourth step, the temperature of the water bath is 65 ℃, the ultrasonic frequency is 1.3MHz, and the ultrasonic power is 450W; in the fifth step, the stirring speed is 850 r/min; in the seventh step, the hot pressing temperature of the hot press is set to 240 ℃, and the pressure is set to 90kg/cm 2 And the pressing time is 18 h.
Comparative example 1:
the difference from example 3 is: the impregnating material comprises the following components in percentage by weight: 25.4% of epoxy resin, 15.3% of cyanate ester resin, 15.1% of polytetrafluoroethylene, 2.1% of curing agent, 11.2% of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 49.1 percent of silicon carbide, 10.9 percent of nano neodymium oxide, 2.9 percent of silane coupling agent KH590, 2.1 percent of disperse black and the balance of sodium alginate.
Comparative example 2:
the difference from example 3 is: the impregnating material comprises the following components in percentage by weight: 25.4% of bismaleimide resin, 15.1% of polytetrafluoroethylene, 2.1% of curing agent, 11.2% of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 49.1 percent of silicon carbide, 10.9 percent of nano neodymium oxide, 2.9 percent of silane coupling agent KH590, 2.1 percent of disperse black and the balance of sodium alginate.
Comparative example 3:
the difference from example 3 is: the impregnating material comprises the following components in percentage by weight: 25.4% of bismaleimide resin, 15.3% of cyanate ester resin, 15.1% of polytetrafluoroethylene, 2.1% of curing agent, 11.2% of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 10.9 percent of nano neodymium oxide, 2.9 percent of silane coupling agent KH590, 2.1 percent of disperse black and the balance of sodium alginate.
Comparative example 4:
the difference from example 3 is: the impregnating material comprises the following components in percentage by weight: 25.4% of bismaleimide resin, 15.3% of cyanate ester resin, 15.1% of polytetrafluoroethylene, 2.1% of curing agent, 11.2% of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 49.1 percent of silicon carbide, 2.9 percent of silane coupling agent KH590, 2.1 percent of disperse black and the balance of sodium alginate.
Comparative example 5:
the difference from example 5 is: no water bath sonication was performed in step two.
Comparative example 6:
the difference from example 5 is: and (4) directly mixing the composite filler with other materials without the operation in the third step and the fourth step.
The heat-resistant hydrocarbon resin-based copper-clad plate in the comparative example and the embodiment of the invention is detected, and the peel strength, the dielectric constant and the dielectric loss of the copper-clad plate are tested according to GB4722-2017 after the copper-clad plate is stored for 5 hours at 200 ℃; the test results are shown in table one:
table one:
| peel strength (N/m) | Dielectric constant (10 GHZ) | Dielectric loss (10 GHZ) | |
| Comparative example 1 | 0.95 | 2.86 | 0.0033 |
| Comparative example 2 | 0.96 | 2.82 | 0.0032 |
| Comparative example 3 | 0.99 | 2.70 | 0.0027 |
| Comparative example 4 | 1.02 | 2.58 | 0.0023 |
| Comparative example 5 | 1.05 | 2.45 | 0.0020 |
| Comparative example 6 | 0.98 | 2.66 | 0.0026 |
| Example 1 | 1.12 | 2.18 | 0.0012 |
| Example 2 | 1.14 | 2.14 | 0.0011 |
| Example 3 | 1.21 | 2.05 | 0.0009 |
| Example 4 | 1.24 | 2.01 | 0.0008 |
| Example 5 | 1.31 | 1.95 | 0.0006 |
From the above table, it can be seen that: the heat-resistant hydrocarbon resin-based copper-clad plate disclosed by the invention has better heat resistance, can effectively ensure the stability of the performance of the heat-resistant hydrocarbon resin-based copper-clad plate when the heat-resistant hydrocarbon resin-based copper-clad plate is used at a high temperature, and can effectively ensure the normal work of the heat-resistant hydrocarbon resin-based copper-clad plate.
The bismaleimide resin in the heat-resistant hydrocarbon resin-based copper-clad plate has the characteristics of high temperature resistance and excellent mechanical property, and the bismaleimide resin, the cyanate ester resin and the polytetrafluoroethylene are compounded and blended, so that the basic heat resistance of the heat-resistant hydrocarbon resin-based copper-clad plate can be ensured; the silicon carbide in the composite filler is subjected to surface modification treatment under the action of a silane coupling agent KH590, and the silicon carbide modified by the silane coupling agent KH590 is added into an impregnating compound to neutralize the bismaleimide resin to be compounded with the cyanate ester resin and the polytetrafluoroethylene; the static mechanical property and the wear resistance of the composite material can be effectively improved, and the composite material still keeps good electrical insulation property; the silicon carbide in the composite filler is subjected to modification treatment in the dispersion black and the sodium alginate, the dispersion black and the sodium alginate are combined to modify the silicon carbide powder to realize chemical connection, the fluidity of the slurry can be effectively improved, and the slurry does not have extrusion and self-polymerization phenomena, so that the modified silicon carbide is more uniformly distributed in the impregnating compound; cyanate resin is used in the impregnating compound, the thermal stability of the cyano-containing resin molecules is higher, and the introduction of cyano into the resin molecules is more beneficial to enhancing the high-temperature resistance of the impregnating compound, so that the high-temperature resistance of the copper-clad plate is improved; the nanometer neodymium oxide is used as a modifier of thermal oxidation stability, and the neodymium oxide modified bismaleimide resin, cyanate resin and polytetrafluoroethylene are prepared by a mechanical blending method, so that the thermal oxidation stability of the impregnating compound can be further enhanced, and the heat resistance and stability of the copper-clad plate can be further enhanced; in the second step, the raw materials in the composite filler are subjected to blending and water bath ultrasonic treatment, so that the materials in the composite filler can be effectively ensured to react quickly, and the modification treatment effect on the silicon carbide is ensured; in the third step, part of the composite filler and part of the bismaleimide resin are subjected to pre-mixing water bath ultrasonic treatment, so that the modification treatment effect of the composite filler on the bismaleimide resin can be effectively enhanced, and the heat resistance of the copper-clad plate is further ensured; in the fourth step, part of the composite filler and part of the cyanate ester resin are subjected to pre-mixing water bath ultrasonic treatment, so that the modification treatment effect of the composite filler on the cyanate ester resin can be effectively enhanced, and the heat resistance of the copper-clad plate is further ensured; in the fifth step, all the raw materials of the impregnating material are mixed to prepare the impregnating material; in the sixth step, the electronic glass fiber cloth is subjected to dipping treatment, solidification and cooling in a dipping material to obtain a heat-resistant hydrocarbon resin-based prepreg; and seventhly, performing hot-pressing compounding on the heat-resistant hydrocarbon resin-based prepreg and the copper foil to prepare the heat-resistant hydrocarbon resin-based copper-clad plate.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A heat-resistant hydrocarbon resin base copper-clad plate is characterized in that: comprises electronic glass fiber cloth, a dipping material and copper foil; the impregnating material comprises the following components in percentage by weight: 24.9-25.9% of bismaleimide resin, 14.8-15.8% of cyanate ester resin, 14.6-15.6% of polytetrafluoroethylene, 1.8-2.4% of curing agent, 10.7-11.7% of composite filler and the balance of solvent.
2. The heat-resistant hydrocarbon resin-based copper-clad plate according to claim 1, characterized in that: the composite filler comprises the following components in percentage by weight: 48.6-49.6% of silicon carbide, 10.6-11.2% of nano neodymium oxide, 2.6-3.2% of silane coupling agent KH590, 1.6-2.6% of disperse black and the balance of sodium alginate.
3. The heat-resistant hydrocarbon resin-based copper-clad plate according to claim 2, characterized in that: the impregnating material comprises the following components in percentage by weight: 24.9 percent of bismaleimide resin, 14.8 percent of cyanate ester resin, 14.6 percent of polytetrafluoroethylene, 1.8 percent of curing agent, 10.7 percent of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 48.6 percent of silicon carbide, 10.6 percent of nano neodymium oxide, 2.6 percent of silane coupling agent KH590, 1.6 percent of disperse black and the balance of sodium alginate.
4. The heat-resistant hydrocarbon resin-based copper-clad plate according to claim 2, characterized in that: the impregnating material comprises the following components in percentage by weight: 25.9 percent of bismaleimide resin, 15.8 percent of cyanate ester resin, 15.6 percent of polytetrafluoroethylene, 2.4 percent of curing agent, 11.7 percent of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 49.6 percent of silicon carbide, 11.2 percent of nano neodymium oxide, 3.2 percent of silane coupling agent KH590, 2.6 percent of disperse black and the balance of sodium alginate.
5. The heat-resistant hydrocarbon resin-based copper-clad plate according to claim 2, characterized in that: the impregnating material comprises the following components in percentage by weight: 25.4% of bismaleimide resin, 15.3% of cyanate ester resin, 15.1% of polytetrafluoroethylene, 2.1% of curing agent, 11.2% of composite filler and the balance of solvent; the composite filler comprises the following components in percentage by weight: 49.1 percent of silicon carbide, 10.9 percent of nano neodymium oxide, 2.9 percent of silane coupling agent KH590, 2.1 percent of disperse black and the balance of sodium alginate.
6. The heat-resistant hydrocarbon resin-based copper-clad plate according to claim 2, characterized in that: the curing agent is prepared by compounding two of 2-ethyl-4-methylimidazole, 1-methylimidazole, imidazole and benzimidazole; the organic solvent is prepared by compounding two of styrene, perchloroethylene, trichloroethylene, ethylene glycol ether and triethanolamine.
7. A preparation method of a heat-resistant hydrocarbon resin-based copper-clad plate is characterized by comprising the following steps: the specific processing steps are as follows: the method comprises the following steps: weighing the bismaleimide resin, the cyanate ester resin, the polytetrafluoroethylene, the curing agent, the solvent and the silicon carbide, the nanometer neodymium oxide, the silane coupling agent KH590, the disperse black and the sodium alginate in the composite filler in parts by weight; step two: mixing the silicon carbide, the nano neodymium oxide, the silane coupling agent KH590, the disperse black and the sodium alginate in the step one, and carrying out water bath ultrasonic treatment for 50-60 minutes to obtain a composite filler; step three: carrying out mixed water bath ultrasonic treatment on one fourth of the composite filler in the second step and one half of bismaleimide resin in the first step for 30-40 minutes to obtain a mixture A; step four: carrying out mixed water bath ultrasonic treatment on one fourth of the composite filler in the second step and one half of the cyanate ester resin in the first step for 20-30 minutes to obtain a mixture B; step five: mixing the polytetrafluoroethylene, the curing agent, the solvent, the mixture A in the step three, the mixture B in the step three, the residual bismaleimide resin, the cyanate ester resin and the composite filler in the step two, and stirring at a high speed for 50-60 minutes to obtain an impregnating compound; step six: dipping the dipping material prepared in the fifth step of the electronic glass fiber cloth for 20-28 min, curing at 140-160 ℃ for 5-7 h, and cooling to room temperature after curing to obtain a heat-resistant hydrocarbon resin-based prepreg; step seven: and symmetrically superposing the heat-resistant hydrocarbon resin-based prepreg and the copper foil, putting the heat-resistant hydrocarbon resin-based prepreg and the copper foil into a hot press, and carrying out hot-pressing treatment to obtain the heat-resistant hydrocarbon resin-based copper-clad plate.
8. The method for preparing the heat-resistant hydrocarbon resin-based copper-clad plate according to claim 7, which is characterized in that: in the second step, the water bath temperature is 40-50 ℃, the ultrasonic frequency is 32-38 KHz, and the ultrasonic power is 800-900W; in the third step, the temperature of the water bath is 50-60 ℃, the ultrasonic frequency is 1.6-1.8 MHz, and the ultrasonic power is 300-400W; in the fourth step, the temperature of the water bath is 60-70 ℃, the ultrasonic frequency is 1.2-1.4 MHz, and the ultrasonic power is 400-500W; in the fifth step, the stirring speed is 800-900 r/min; in the seventh step, the hot pressing temperature of the hot press is set to be 220-260 ℃ and the pressure is set to be 80-100 kg/cm 2 The pressing time is 16-20 h.
9. The preparation method of the heat-resistant hydrocarbon resin-based copper-clad plate according to claim 8, characterized in that: in the second step, the water bath temperature is 40 ℃, the ultrasonic frequency is 32KHz, and the ultrasonic power is 800W; in step three, waterThe bath temperature is 50 ℃, the ultrasonic frequency is 1.6MHz, and the ultrasonic power is 300W; in the fourth step, the temperature of the water bath is 60 ℃, the ultrasonic frequency is 1.2MHz, and the ultrasonic power is 400W; in the fifth step, the stirring speed is 800 r/min; in the seventh step, the hot press temperature is set to 220 ℃ and the pressure is set to 80kg/cm 2 And the pressing time is 16 h.
10. The method for preparing the heat-resistant hydrocarbon resin-based copper-clad plate according to claim 8, which is characterized in that: in the second step, the water bath temperature is 45 ℃, the ultrasonic frequency is 35KHz, and the ultrasonic power is 850W; in the third step, the temperature of the water bath is 55 ℃, the ultrasonic frequency is 1.7MHz, and the ultrasonic power is 350W; in the fourth step, the temperature of the water bath is 65 ℃, the ultrasonic frequency is 1.3MHz, and the ultrasonic power is 450W; in the fifth step, the stirring speed is 850 r/min; in the seventh step, the hot pressing temperature of the hot press is set to 240 ℃, and the pressure is set to 90kg/cm 2 And the pressing time is 18 h.
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