CN111378242A - Resin composition, prepreg containing resin composition, dielectric substrate and printed circuit board - Google Patents
Resin composition, prepreg containing resin composition, dielectric substrate and printed circuit board Download PDFInfo
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- CN111378242A CN111378242A CN201811643511.XA CN201811643511A CN111378242A CN 111378242 A CN111378242 A CN 111378242A CN 201811643511 A CN201811643511 A CN 201811643511A CN 111378242 A CN111378242 A CN 111378242A
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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
- C08L47/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds; Compositions of derivatives of such polymers
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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
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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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
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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
- 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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- 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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- 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
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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
- B32B2260/04—Impregnation, embedding, or binder material
- B32B2260/046—Synthetic resin
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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
- 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
- B32B2307/204—Di-electric
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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
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/302—Conductive
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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
- 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
- C08J2347/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds; Derivatives of such polymers
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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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- 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
- C08J2409/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
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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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/16—Ethene-propene or ethene-propene-diene copolymers
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- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
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Abstract
The invention provides a resin composition, a prepreg containing the resin composition, a dielectric substrate and a printed circuit board, wherein the resin composition comprises the following components: (A) a thermosetting resin having an unsaturated double bond, (B) a resin film-forming property improving material, (C) hexagonal boron nitride, (D) any one of aluminum nitride, silicon nitride or silicon carbide or a combination of at least two of them, (E) other inorganic filler than the components (C) and (D), (F) a flame retardant and (G) an initiator; wherein the mass sum of the component (C), the component (D) and the component (E) accounts for 60-80% of the total mass of the resin composition, and the mass ratio of the component (C) to the component (D) is (1-4) to 2. The dielectric substrate obtained by the resin composition provided by the invention has low dielectric constant, low dielectric loss, high thermal conductivity and stable thickness and dielectric constant, and can fully meet the requirements of high-frequency high-thermal-conductivity dielectric substrates.
Description
Technical Field
The invention belongs to the technical field of electronic materials, and relates to a resin composition, a prepreg containing the resin composition, a dielectric substrate and a printed circuit board.
Background
With the continuous development of Printed Circuit Boards (PCBs) towards high density and multilayering, the space for carrying and installing components on the PCBs is greatly reduced, the power requirements of the electronic products of the whole machine on the power components are higher and higher, and more heat accumulation is inevitably generated due to small space and high power. On the other hand, with the rapid development of modern communication technology, the working frequency of electronic equipment is higher and higher, and the heat productivity is larger and larger. In summary, the integration of a large number of powerful functions into smaller components drives the printed boards to high density and the development of high frequency or high speed digitization of signal transmission, which both cause the operating temperature of the printed boards to rise sharply. If the accumulated heat cannot be discharged in time, the working temperature of the equipment is increased, and the electrical performance of components is reduced and even damaged, so that the service life and the reliability of the equipment are seriously damaged. A large number of tests and statistical data show that the reliability of the electronic components (after the optimal working temperature is increased by 2 ℃) is reduced by 10%, and the service life of the electronic components (after the optimal working temperature is increased by 50 ℃) is only 1/6 with the temperature being increased by 25 ℃, so that the working temperature of the printed board becomes the most important factor influencing the reliability and the service life.
The demand for improving the circuit integration level and the power density of the PCB is increasing day by day, and the importance of the thermal management of the high frequency printed circuit board is more prominent. It is well known that the thermal conductivity of a material is critical to reduce the temperature rise. The heat of the high-frequency circuit board is essentially closely related to the loss on the circuit board; for example, a copper foil with a rough surface has a larger loss than a copper foil with a smooth surface. Another material parameter that affects loss is the dissipation factor of the printed wiring board dielectric layer material, with lower dissipation factors and lower dielectric losses, the printed wiring board will also generate less heat. In addition, a printed circuit board material with a lower dielectric constant will also generate less loss and less heat than a material with a higher dielectric constant. Generally, the choice of circuit board materials with good properties, such as high thermal conductivity, low dissipation factor, smooth copper foil surface, and low dielectric constant, not only helps to design high performance printed circuit boards, but also improves thermal management.
CN106867173 discloses a composite material, a high frequency circuit substrate made of the same and a method for making the same, the composite material comprising: (1) 20-70 parts of a thermosetting mixture; the thermosetting mixture comprises: (A) a thermosetting resin based on polybutadiene having a molecular weight of 11000 or less and containing 60% or more of vinyl groups or a copolymer resin of polybutadiene and styrene, which is composed of hydrocarbon elements; and (B) an ethylene-propylene rubber which is solid at room temperature and has a weight average molecular weight of more than 10 ten thousand and less than 15 ten thousand and a number average molecular weight of more than 6 ten thousand and less than 10 ten thousand; (2) 10-60 parts of glass fiber cloth; (3) 0-70 parts of powder filler; (4) 1-3 parts of a curing initiator. Although the resulting circuit board has good high-frequency dielectric properties, the thermal conductivity thereof has not been studied and may not satisfy the requirement of high thermal conductivity. US6291374 discloses a resin composition comprising a thermosetting polybutadiene or polyisoprene resin, an ethylene propylene rubber and optionally a thermoplastic unsaturated butadiene or isoprene containing polymer, a particulate filler, a flame retardant additive, a curing agent and a woven or non-woven fabric, the resulting circuit substrate having better heat aging properties and a lower dielectric constant, but does not provide how to improve the thermal conductivity of the substrate.
Therefore, it is required to develop a new resin composition, which can be used to prepare a dielectric substrate having excellent dielectric properties and high thermal conductivity, and having good thickness uniformity and dielectric constant uniformity, so as to meet the current requirements for high frequency high thermal conductivity dielectric substrates.
Disclosure of Invention
The invention aims to provide a resin composition, a prepreg containing the resin composition, a dielectric substrate and a printed circuit board.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a resin composition comprising the following components: (A) a thermosetting resin having an unsaturated double bond, (B) a resin film-forming property improving material, (C) hexagonal boron nitride, (D) any one of aluminum nitride, silicon nitride or silicon carbide or a combination of at least two of them, (E) other inorganic filler than the components (C) and (D), (F) a flame retardant and (G) an initiator.
Wherein the sum of the mass of component (C), component (D) and component (E) is 60 to 80%, for example 62%, 64%, 65%, 66%, 68%, 70%, 72%, 74%, 75%, 76%, 78% and the like, based on the total mass of the resin composition, and the mass ratio of component (C) to component (D) is (1 to 4) to 2, for example 1.5:2, 2:2, 2.5:2, 3:2, 3.5:2 and the like.
In order to obtain a medium substrate for high-frequency high heat conduction, the component (C) hexagonal boron nitride is added into the resin composition, the thermal conductivity of the hexagonal boron nitride is very high, the thermal conductivity of the substrate can be obviously improved, but the structure of the hexagonal boron nitride filler is fluffy, and the oil absorption value is very high; at the same time, hexagonal boron nitride is expensive. The aluminum nitride, silicon nitride, and silicon carbide in the component (D) have relatively high thermal conductivity and relatively low dielectric constant, but have relatively high hardness, and the aluminum nitride, silicon nitride, and silicon carbide are relatively expensive.
In the invention, the component (C) and the component (D) are added simultaneously, and the two are synergistic, so that on one hand, the phenomenon that the adhesive solution is very viscous and can not be applied due to excessive addition of the component (C) can be avoided, and even if the adhesive solution can be applied, the appearance of the bonding sheet is very much stripe; and simultaneously, the problem that the drilling processability of the substrate is very difficult due to excessive addition of the component (D), especially excessive addition of aluminum nitride, silicon nitride and silicon carbide is avoided; on the other hand, the component (C) and the component (D) are added simultaneously, so that the required dosage of the component (C) and the component (D) which are added independently can be obviously reduced, and the component (C) and the component (D) act together, so that the finally obtained dielectric substrate has very high thermal conductivity and very good drilling processability.
Because the component (C) and the component (D) are expensive, in order to reduce the cost and simultaneously improve the filling amount of the filler, the invention selects and adds part of other inorganic fillers except the component (C) and the component (D), and when the component (C), the component (D) and the component (E) are used together, the dielectric substrate can be ensured to have higher thermal conductivity, lower dielectric constant and dielectric loss, better drilling processability and more optimized comprehensive cost of raw materials. If the sum of the total addition of the three components is too much, the resin content in the resin composition is too little, so that the sizing manufacturability is poor, the thickness consistency of the substrate is poor, the total amount of the filler is too high, and the drilling and processing performances are poor; if the total amount of the three is too small, the filling rate of the filler is insufficient, resulting in a low thermal conductivity of the substrate.
Preferably, the resin composition comprises the following components in parts by weight, based on 100 parts by weight of the total resin composition:
(A) 10-20 parts by weight of thermosetting resin with unsaturated double bonds;
(B) 2-5 parts of resin film-forming property improving material;
(C) 20-40 parts of hexagonal boron nitride;
(D) 20-40 parts by weight of any one or the combination of at least two of aluminum nitride, silicon nitride or silicon carbide;
(E) 10 to 30 parts by weight of an inorganic filler other than the components (C) and (D);
(F) 5-15 parts of a flame retardant;
(G) 0.5 to 1.5 portions of initiator.
When a dielectric substrate is prepared, a person skilled in the art generally selects resin with high double bond content and low molecular weight as main resin, wherein the high double bond content is used for ensuring that the resin has high enough crosslinking density, and the low molecular weight is used for ensuring that the resin can well infiltrate the filler and the glass fiber cloth; however, when a large amount of heat conductive filler is added into the adhesive sheet, the adhesive sheet has a non-smooth appearance and poor film forming property, and even has a chap phenomenon, and particularly, the adhesive sheet has a peeling phenomenon in a serious condition.
The addition of the resin film-forming property improving material of the component (B) can improve the phenomena of unsmooth appearance, poor film-forming property and poor thickness consistency of the bonding sheet, particularly the phenomena of chapping and peeling of the bonding sheet when the content of the hexagonal boron nitride filler of the component (C) is high, and the addition of the component (B) can obviously improve the bonding sheet. However, if the amount of component (B) is too large, the viscosity of the glue solution is too high during glue mixing, the glueing manufacturability is poor, and the fluidity of the resin is poor during pressing, eventually resulting in poor thickness uniformity of the substrate. If the addition amount of the component (B) is too small, the effect of improving the film forming property of the bonding sheet cannot be achieved, the appearance of the bonding sheet is not smooth, the sizing manufacturability is poor, and the thickness consistency of the substrate is poor.
In the present invention, the unsaturated double bond-containing thermosetting resin is used in an amount of 10 to 20 parts by weight, for example, 11 parts by weight, 12 parts by weight, 14 parts by weight, 15 parts by weight, 16 parts by weight, 18 parts by weight, 19 parts by weight, or the like.
Preferably, the thermosetting resin having an unsaturated double bond includes any one of or a combination of at least two of a polyphenylene ether resin, a polybutadiene copolymer resin, or an elastomeric block copolymer having an unsaturated double bond.
Preferably, the polyphenylene ether resin having an unsaturated double bond is selected from any one of or a combination of at least two of a polyphenylene ether resin in which both terminal modifying groups are acryloyl groups, a polyphenylene ether resin in which both terminal modifying groups are styryl groups, or a polyphenylene ether resin in which both terminal modifying groups are vinyl groups.
Preferably, the polybutadiene resin is selected from any one of or a combination of at least two of 1, 2-polybutadiene resin, maleic anhydride modified polybutadiene resin, acrylate modified polybutadiene resin, epoxy modified polybutadiene resin, amine modified polybutadiene resin, carboxyl-terminated modified polybutadiene resin, or hydroxyl-terminated modified polybutadiene resin.
Preferably, the polybutadiene copolymer resin is selected from any one of or a combination of at least two of a polybutadiene-styrene copolymer resin, a polybutadiene-styrene-divinylbenzene graft copolymer resin, a maleic anhydride-modified styrene-butadiene copolymer resin, or an acrylate-modified styrene-butadiene copolymer resin.
Preferably, the elastomeric block copolymer having unsaturated double bonds is selected from any one of or a combination of at least two of a styrene-butadiene diblock copolymer, a styrene-butadiene-styrene triblock copolymer, a styrene- (ethylene-butylene) -styrene triblock copolymer, a styrene-isoprene diblock copolymer, a styrene-isoprene-styrene triblock copolymer, a styrene- (ethylene-propylene) -styrene triblock copolymer, or a styrene- (ethylene-butylene) diblock copolymer.
In the present invention, the resin film-forming property improving material is 2 to 5 parts by weight, for example, 2.5 parts by weight, 3 parts by weight, 3.5 parts by weight, 4 parts by weight, 4.5 parts by weight, and the like.
Preferably, the resin film forming property improving material is selected from any one or a combination of at least two of ethylene propylene rubber, polybutadiene rubber, styrene butadiene rubber, nitrile rubber or carboxyl-terminated nitrile rubber.
Preferably, the resin film forming property improving material has a number average molecular weight of 50000-150000, such as 60000, 70000, 80000, 90000, 100000, 110000, 120000, 130000, 140000, and the like.
When the number average molecular weight of the resin film forming property improving material is less than 5 ten thousand, the effect of improving the film forming of the resin can not be achieved, and when the number average molecular weight of the resin film forming property improving material is more than 15 ten thousand, the resin is difficult to dissolve in a solvent, the difficulty in a glue mixing process is easily caused, and the gluing process is poor due to the poor solubility of the resin composition.
In the present invention, the hexagonal boron nitride is 20 to 40 parts by weight, for example, 22 parts by weight, 25 parts by weight, 28 parts by weight, 30 parts by weight, 32 parts by weight, 35 parts by weight, 38 parts by weight, and the like.
When the addition amount of the hexagonal boron nitride is too much, the glue solution is very viscous and can not be used for gluing, even if the glue solution can be used for gluing, the appearance of the bonding sheet also has very many stripes, the gluing manufacturability is poor, and the thickness consistency of the finally obtained substrate is poor; if the amount of hexagonal boron nitride added is too small, the heat conduction channel is not formed, and the thermal conductivity of the substrate is low.
In the present invention, any one or a combination of at least two of the aluminum nitride, silicon nitride, or silicon carbide is 20 to 40 parts by weight, for example, 22 parts by weight, 25 parts by weight, 28 parts by weight, 30 parts by weight, 32 parts by weight, 35 parts by weight, 38 parts by weight, or the like.
If any one or a combination of at least two of aluminum nitride, silicon nitride or silicon carbide is added in an excessive amount, the hardness of the substrate is very high, so that the substrate drilling process can be very difficult; however, when the amount of the additive is too small, the heat conduction path is not formed, and the thermal conductivity of the substrate is low.
In the present invention, the other inorganic filler other than the components (C) and (D) is 10 to 30 parts by weight, for example, 12 parts by weight, 15 parts by weight, 18 parts by weight, 20 parts by weight, 22 parts by weight, 25 parts by weight, 28 parts by weight, or the like.
Preferably, the inorganic filler other than components (C) and (D) is selected from any one of silica, titanium dioxide, alumina, magnesium oxide, zinc oxide, barium titanate, strontium titanate, magnesium titanate, calcium titanate, potassium titanate, barium strontium titanate, lead titanate, glass powder, magnesium hydroxide, mica powder, talc, hydrotalcite, mullite, boehmite, kaolin, montmorillonite, calcium silicate or calcium carbonate, or a combination of at least two thereof.
Preferably, the silica comprises fused amorphous silica and/or crystalline silica, further preferably fused amorphous silica.
Preferably, the titanium dioxide comprises rutile titanium dioxide and/or anatase titanium dioxide, further preferably rutile titanium dioxide.
In the present invention, the flame retardant is 5 to 15 parts by weight, for example, 6 parts by weight, 7 parts by weight, 8 parts by weight, 10 parts by weight, 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, and the like.
Preferably, the flame retardant comprises a bromine-containing flame retardant and/or a phosphorus-containing flame retardant.
Preferably, the bromine-containing flame retardant is any one or a combination of at least two of decabromodiphenyl ether, decabromodiphenylethane or ethylenebistetrabromophthalimide.
Preferably, the phosphorus-containing flame retardant is any one of tris (2, 6-dimethylphenyl) phosphine, 10- (2, 5-dihydroxyphenyl) -9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 2, 6-bis (2, 6-dimethylphenyl) phosphinobenzene, or 10-phenyl-9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, or a combination of at least two thereof.
In the present invention, the initiator is 0.5 to 1.5 parts by weight, for example, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 1.0 parts by weight, 1.2 parts by weight, 1.3 parts by weight, 1.4 parts by weight, etc.
Preferably, the initiator comprises an organic peroxide free radical initiator and/or a carbon-based free radical initiator.
Preferably, the organic peroxide free radical initiator is any one or a combination of at least two selected from dicumyl peroxide, 1, 3-bis (tert-butylperoxyisopropyl) benzene, 2, 5-di-tert-butylperoxy-2, 5-dimethylhexane, 2, 5-di-tert-butylperoxy-2, 5-dimethylhexyne-3, di-tert-butyl peroxide or tert-butylcumyl peroxide.
Preferably, the carbon-based radical initiator is selected from any one of 2, 3-dimethyl-2, 3-diphenylbutane, 2, 3-dimethyl-2, 3-di (4-methylphenyl) butane, 2, 3-dimethyl-2, 3-di (4-isopropylphenyl) butane or 3, 4-dimethyl-3, 4-diphenylhexane or a combination of at least two thereof.
The term "comprising" as used herein means that it may include, in addition to the components, other components which impart different characteristics to the resin composition. In addition, the term "comprising" as used herein may be replaced by "being" or "consisting of … …" as closed.
The resin composition of the present invention can also be used in combination with various high polymers as long as it does not impair the inherent properties of the resin composition. Specifically, for example, a liquid crystal polymer, a thermoplastic resin, various flame retardant compounds or additives, and the like can be used. They may be used alone or in combination of plural kinds as required.
Preferably, the resin composition further comprises other auxiliaries.
Preferably, the other auxiliary agent includes any one or a combination of at least two of an antioxidant, a heat stabilizer, an antistatic agent, an ultraviolet absorber, a pigment, a colorant, or a lubricant.
The method for producing the resin composition of the present invention can be carried out by a known method: stirring, mixing, and the like.
In a second aspect, the present invention provides a prepreg comprising a reinforcing material (e.g. glass cloth), and the resin composition of the first aspect attached to the reinforcing material by impregnation drying.
The method for producing the prepreg of the present invention is not particularly limited as long as it is a method for producing a prepreg by combining the resin composition of the present invention with a glass fiber cloth. An exemplary prepreg preparation method is: the resin composition is prepared into glue solution with a certain concentration, and the prepreg is obtained by impregnating glass fiber cloth, drying at a certain temperature, removing the solvent and semi-curing.
In the above method for producing a prepreg, an organic solvent may be used as needed, and the organic solvent is not particularly limited as long as it is compatible with each component of the resin composition, and specific examples thereof include: alcohols such as methanol, ethanol and butanol, ethers such as ethyl cellosolve, butyl cellosolve, ethylene glycol methyl ether, diethylene glycol ethyl ether and diethylene glycol butyl ether, ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone and cyclohexanone, aromatic hydrocarbons such as toluene, xylene and mesitylene, esters such as ethoxyethyl acetate and ethyl acetate, and nitrogen-containing solvents such as N, N-dimethylformamide, N-dimethylacetamide and N-methyl-2-pyrrolidone; the above solvents may be used singly or in combination of two or more.
In a third aspect, the present invention provides a dielectric substrate comprising one or at least two stacked prepregs according to the second aspect and a metal foil applied to one or both sides of the prepregs.
The dielectric substrate can be used for a high-frequency high-heat-conductivity dielectric substrate and is formed by a sheet material or a plate material, wherein metal foils are arranged on two sides of the sheet material or the plate material as electrodes, and a dielectric layer is arranged in the middle of the sheet material or the plate material.
In the present invention, the dielectric substrate is made of a metal foil as an electrode material, and the metal foil includes copper, brass, aluminum, nickel, zinc, or an alloy or composite metal foil of these metals, and the thickness of the metal foil is 9 to 150. mu.m, for example, 12. mu.m, 20. mu.m, 30. mu.m, 40. mu.m, 50. mu.m, 70. mu.m, 90. mu.m, 110. mu.m, 120. mu.m, 130. mu.m, and 140. mu.m.
Illustratively, the method for manufacturing a dielectric substrate according to the present invention comprises: (1) dissolving or dispersing the resin composition in a solvent to prepare a glue solution, soaking glass fiber cloth, drying, and removing the solvent to prepare a prepreg; (2) and (3) stacking at least one prepreg together, placing the prepreg between two metal foils, and then placing the metal foils into a laminating machine to prepare the dielectric substrate through hot-pressing and curing.
In a fourth aspect, the present invention provides a printed circuit board comprising one or at least two superimposed prepregs according to the second aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the invention, the component (C) and the component (D) are added simultaneously, and the two are synergistic, so that on one hand, the phenomenon that the adhesive solution is very viscous and can not be applied due to excessive addition of the component (C) can be avoided, and even if the adhesive solution can be applied, the appearance of the bonding sheet is very much stripe; and simultaneously, the problem that the drilling processability of the substrate is very difficult due to excessive addition of the component (D), especially excessive addition of aluminum nitride, silicon nitride and silicon carbide is avoided; on the other hand, the component (C) and the component (D) are added simultaneously, so that the required dosage of the component (C) and the component (D) which are added independently can be obviously reduced, and the component (C) and the component (D) act together, so that the finally obtained dielectric substrate has very high thermal conductivity and very good drilling processability.
(2) The addition of the resin film-forming property improving material of the component (B) can improve the phenomena of unsmooth appearance, poor film-forming property and poor thickness consistency of the bonding sheet, particularly the phenomena of chapping and peeling of the bonding sheet when the content of the hexagonal boron nitride filler of the component (C) is high, and the addition of the component (B) can obviously improve the bonding sheet.
(3) The copper-clad plate prepared by the resin composition provided by the invention has low dielectric constant and low dielectric loss, high thermal conductivity and good gluing manufacturability, and the finally obtained copper-clad plate has good thickness consistency, drilling and processing performance; wherein the dielectric constant is less than 3.80(10GHz), the dielectric loss is less than 0.0030(10GHz), and the thermal conductivity is more than 1.45W/mK.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The following examples and comparative examples relate to materials and brand information as shown in table 1:
TABLE 1
Examples 1 to 11
Resin compositions (raw material amount units are parts by weight) were prepared according to the components shown in table 2, and copper-clad laminate samples were prepared according to the following preparation methods:
(1) the components with the formula ratio are mixed and diluted to proper viscosity by a solvent, and the resin glue solution is obtained after uniform stirring and mixing.
(2) And (3) impregnating the glue solution with glass fiber cloth, controlling the thickness to be proper, and removing the solvent to form a prepreg.
(3) Laminating the prepregs in several sheets, laminating a copper foil on each prepreg, and curing in a press at the curing temperature of 150-300 deg.C under the curing pressure of 25-70kg/cm to obtain the final product2。
Comparative examples 1 to 10
Resin compositions (the raw material amounts are in parts by weight) were prepared according to the components shown in table 3, and copper-clad laminate samples were prepared according to the method for producing a laminate described in the examples.
TABLE 2
TABLE 3
And (3) performance testing:
the copper-clad plates provided in examples 1 to 11 and comparative examples 1 to 10 were subjected to a performance test by the following method:
(1) dielectric constant (Dk) and dielectric loss factor (Df): testing the dielectric constant Dk and the dielectric loss Df of the board by adopting an SPDR method under the frequency of 10 GHz;
(2) thermal conductivity: testing by adopting a thermal conductivity tester according to an ASTMD5470 method;
(3) sizing manufacturability: according to the appearance of the bonding sheet in the gluing process, whether the bonding sheet has obvious sagging phenomenon and stripes or not is observed by naked eyes, whether the bonding sheet is smooth or not is touched by hands, and whether the bonding sheet has uneven feeling or not is judged; if the bonding sheet has no sagging, no stripe, smooth appearance and no uneven feeling, the gluing manufacturability is good;
(4) thickness uniformity: taking five samples at four corners of the plate and the middle position of the plate to test the thickness of the plate, wherein if the thickness of the plate meets the three-level tolerance of the copper-clad plate, the thickness consistency is good; if the thickness of the plate cannot meet the three-level tolerance of the copper-clad plate, the thickness consistency is poor;
(5) drilling and processing: judging according to the abrasion condition of the drill cutter in the drilling process and the cutter breaking condition of the milling cutter in the sample preparation process, wherein if the abrasion condition of the drill cutter in the drilling process is serious and the cutter breaking condition of the milling cutter in the sample preparation process is frequent, the drilling and the processing performances are poor; if the abrasion condition of the drill cutter is normal in the drilling process and the cutter breakage condition of the milling cutter cannot occur frequently in the sample preparation process, the drilling and the processing performances are good.
The results of the tests on the laminates provided in examples 1 to 11 and comparative examples 1 to 10 are shown in Table 4:
TABLE 4
According to the embodiment and the performance test, the copper-clad plate prepared from the resin composition provided by the invention has low dielectric constant and low dielectric loss, high thermal conductivity and good gluing manufacturability, and the finally obtained copper-clad plate has good thickness consistency, drilling and processing performance; wherein the dielectric constant is less than 3.80(10GHz), the dielectric loss is less than 0.0030(10GHz), and the thermal conductivity is more than 1.45W/mK.
As can be seen from the comparison between the embodiment 1 and the embodiments 7-8, the molecular weight of the preferable resin film-forming property improving material of the invention is in the range of 50000-150000, and at the moment, the copper-clad plate prepared by the resin composition of the invention has better film-forming effect and better sizing manufacturability and thickness consistency.
As can be seen from the comparison among examples 5, 9-12 and comparative examples 1-2, in the present invention, the component B hexagonal boron nitride and the component C any one or a combination of at least two of aluminum nitride, silicon nitride or silicon carbide have a synergistic effect, and the two components act together to synergistically enhance, so that the final copper clad laminate has low dielectric constant, low dielectric loss, high thermal conductivity, good drilling processability, excellent thickness consistency, etc.
As can be seen from the comparison between example 2 and comparative example 3, if the amount of the resin film-forming property-improving material of component (B) is too large, the viscosity of the glue solution is high during glue mixing, resulting in poor gluing manufacturability, and the fluidity of the resin is poor during pressing, resulting in poor thickness uniformity of the substrate, and thus poor gluing manufacturability and thickness uniformity of the sheet.
As is clear from the comparison between example 3 and comparative example 4, if the amount of the resin film-forming property-improving material of component (B) is too small, the effect of improving the film-forming property of the adhesive sheet is not obtained, the appearance of the adhesive sheet is not smooth, the sizing workability is poor, and the thickness uniformity of the substrate is also poor, so that the sizing workability and the thickness uniformity of the sheet are poor.
As can be seen from the comparison between example 3 and comparative example 5, if the amount of the hexagonal boron nitride filler as component (C) is too much, the glue solution is very viscous, the appearance of the bonding sheet during gluing has very many stripes, the gluing manufacturability is poor, and the thickness consistency is poor.
As is clear from the comparison of example 2 and comparative example 6, if the amount of the hexagonal boron nitride filler as component (C) added is too small, a heat conduction path cannot be formed, and thus the thermal conductivity of the substrate is low.
As is clear from comparison between example 4 and comparative example 7, if the component (D), which is either one of aluminum nitride, silicon nitride or silicon carbide, or a combination of at least two of them, is added in an excessive amount, the hardness of the substrate becomes very high, and drilling work becomes very difficult, so that drilling and working of the substrate become poor.
As can be seen from a comparison of example 1 and comparative example 8, if the component (D), any one of aluminum nitride, silicon nitride or silicon carbide, or a combination of at least two of them, is added in an excessively small amount, a heat conduction path is not formed, and the thermal conductivity of the substrate is low.
As is clear from the comparison of example 6 with comparative example 9, if the total amount of the components (C), (D) and (E) added is too large, the resin content is too small, the sizing workability is poor, the thickness uniformity of the substrate is poor, and the drilling and processing properties are also poor due to too high total amount of the filler.
From the comparison of example 5 and comparative example 10, it is understood that if the total amount of the component (C), the component (D) and the component (E) added is too small, the filling ratio of the filler is insufficient and the thermal conductivity of the substrate is low.
The applicant states that the present invention is illustrated by the above examples of the resin composition of the present invention, the prepreg, the dielectric substrate and the printed circuit board comprising the same, but the present invention is not limited to the above detailed method, that is, it does not mean that the present invention must be implemented by relying on the above detailed method. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A resin composition, characterized in that the resin composition comprises the following components: (A) a thermosetting resin having an unsaturated double bond, (B) a resin film-forming property improving material, (C) hexagonal boron nitride, (D) any one of aluminum nitride, silicon nitride or silicon carbide or a combination of at least two of them, (E) other inorganic filler than the components (C) and (D), (F) a flame retardant and (G) an initiator;
wherein the mass sum of the component (C), the component (D) and the component (E) accounts for 60-80% of the total mass of the resin composition, and the mass ratio of the component (C) to the component (D) is (1-4) to 2.
2. The resin composition according to claim 1, wherein the resin composition comprises the following components, based on 100 parts by weight of the total resin composition:
(A) 10-20 parts by weight of thermosetting resin with unsaturated double bonds;
(B) 2-5 parts of resin film-forming property improving material;
(C) 20-40 parts of hexagonal boron nitride;
(D) 20-40 parts by weight of any one or the combination of at least two of aluminum nitride, silicon nitride or silicon carbide;
(E) 10 to 30 parts by weight of an inorganic filler other than the components (C) and (D);
(F) 5-15 parts of a flame retardant;
(G) 0.5 to 1.5 portions of initiator.
3. The resin composition according to claim 1 or 2, wherein the thermosetting resin having an unsaturated double bond comprises any one or a combination of at least two of a polyphenylene ether resin, a polybutadiene copolymer resin, or an elastomeric block copolymer having an unsaturated double bond;
preferably, the polyphenylene ether resin with unsaturated double bonds is selected from any one of or a combination of at least two of a polyphenylene ether resin in which both terminal modifying groups are acryloyl groups, a polyphenylene ether resin in which both terminal modifying groups are styryl groups, or a polyphenylene ether resin in which both terminal modifying groups are vinyl groups;
preferably, the polybutadiene resin is selected from any one of or a combination of at least two of 1, 2-polybutadiene resin, maleic anhydride modified polybutadiene resin, acrylate modified polybutadiene resin, epoxy modified polybutadiene resin, amine modified polybutadiene resin, carboxyl-terminated modified polybutadiene resin or hydroxyl-terminated modified polybutadiene resin;
preferably, the polybutadiene copolymer resin is selected from any one of or a combination of at least two of a polybutadiene-styrene copolymer resin, a polybutadiene-styrene-divinylbenzene graft copolymer resin, a maleic anhydride-modified styrene-butadiene copolymer resin, or an acrylate-modified styrene-butadiene copolymer resin;
preferably, the elastomeric block copolymer having unsaturated double bonds is selected from any one of or a combination of at least two of a styrene-butadiene diblock copolymer, a styrene-butadiene-styrene triblock copolymer, a styrene- (ethylene-butylene) -styrene triblock copolymer, a styrene-isoprene diblock copolymer, a styrene-isoprene-styrene triblock copolymer, a styrene- (ethylene-propylene) -styrene triblock copolymer, or a styrene- (ethylene-butylene) diblock copolymer.
4. The resin composition according to any one of claims 1 to 3, wherein the resin film formation property improving material is selected from any one of ethylene propylene rubber, polybutadiene rubber, styrene butadiene rubber, nitrile rubber or carboxyl terminated nitrile rubber or a combination of at least two thereof;
preferably, the resin film-forming property improving material has a number average molecular weight of 50000-150000.
5. The resin composition according to any one of claims 1 to 4, wherein the inorganic filler other than components (C) and (D) is selected from any one of silica, titanium dioxide, alumina, magnesium oxide, zinc oxide, barium titanate, strontium titanate, magnesium titanate, calcium titanate, potassium titanate, barium strontium titanate, lead titanate, glass powder, magnesium hydroxide, mica powder, talc, hydrotalcite, mullite, boehmite, kaolin, montmorillonite, calcium silicate, or calcium carbonate, or a combination of at least two thereof;
preferably, the silica comprises fused amorphous silica and/or crystalline silica, further preferably fused amorphous silica;
preferably, the titanium dioxide comprises rutile titanium dioxide and/or anatase titanium dioxide, further preferably rutile titanium dioxide.
6. The resin composition according to any one of claims 1 to 5, wherein the flame retardant comprises a bromine-containing flame retardant and/or a phosphorus-containing flame retardant;
preferably, the bromine-containing flame retardant is any one or a combination of at least two of decabromodiphenyl ether, decabromodiphenylethane or ethylene bistetrabromophthalimide;
preferably, the phosphorus-containing flame retardant is any one of tris (2, 6-dimethylphenyl) phosphine, 10- (2, 5-dihydroxyphenyl) -9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 2, 6-bis (2, 6-dimethylphenyl) phosphinobenzene, or 10-phenyl-9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, or a combination of at least two thereof.
7. The resin composition according to any one of claims 1 to 6, wherein the initiator comprises an organic peroxide radical initiator and/or a carbon-based radical initiator;
preferably, the organic peroxide free radical initiator is any one or the combination of at least two of dicumyl peroxide, 1, 3-bis (tert-butylperoxyisopropyl) benzene, 2, 5-di-tert-butylperoxy-2, 5-dimethylhexane, 2, 5-di-tert-butylperoxy-2, 5-dimethylhexyne-3, di-tert-butyl peroxide or tert-butylcumyl peroxide;
preferably, the carbon-based radical initiator is selected from any one of 2, 3-dimethyl-2, 3-diphenylbutane, 2, 3-dimethyl-2, 3-di (4-methylphenyl) butane, 2, 3-dimethyl-2, 3-di (4-isopropylphenyl) butane or 3, 4-dimethyl-3, 4-diphenylhexane or a combination of at least two thereof;
preferably, the resin composition further comprises other auxiliaries;
preferably, the other auxiliary agent includes any one or a combination of at least two of an antioxidant, a heat stabilizer, an antistatic agent, an ultraviolet absorber, a pigment, a colorant, or a lubricant.
8. A prepreg comprising a reinforcing material and the resin composition according to any one of claims 1 to 7 attached to the reinforcing material by impregnation drying.
9. A dielectric substrate comprising one or at least two stacked prepregs according to claim 8 and a metal foil applied to one or both sides of the prepregs.
10. A printed circuit board comprising one or at least two superimposed prepregs according to claim 8.
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| CN113817414A (en) * | 2021-09-18 | 2021-12-21 | 华东理工大学 | High-temperature-resistant cyanate ester insulating heat-conducting adhesive and preparation method thereof |
| TWI766320B (en) * | 2020-07-23 | 2022-06-01 | 南亞塑膠工業股份有限公司 | Prepreg and metallic clad laminate |
| CN115701442A (en) * | 2021-08-02 | 2023-02-10 | 南亚塑胶工业股份有限公司 | High-thermal-conductivity rubber resin material and high-thermal-conductivity metal substrate |
| CN115701443A (en) * | 2021-08-02 | 2023-02-10 | 南亚塑胶工业股份有限公司 | High dielectric rubber resin material and high dielectric metal substrate |
| CN116001385A (en) * | 2022-12-15 | 2023-04-25 | 广东生益科技股份有限公司 | Circuit material and printed circuit board |
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