CN110903603B - Resin composition and application thereof - Google Patents
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- CN110903603B CN110903603B CN201911232109.7A CN201911232109A CN110903603B CN 110903603 B CN110903603 B CN 110903603B CN 201911232109 A CN201911232109 A CN 201911232109A CN 110903603 B CN110903603 B CN 110903603B
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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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
- B32B15/092—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 comprising epoxy resins
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- 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
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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
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino-carboxylic acids or of polyamines and polycarboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- B32B2262/06—Vegetal fibres
- B32B2262/062—Cellulose fibres, e.g. cotton
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- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
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- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/206—Insulating
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
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- B32B2307/70—Other properties
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
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- B32B2307/70—Other properties
- B32B2307/732—Dimensional properties
- B32B2307/734—Dimensional stability
- B32B2307/736—Shrinkable
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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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The application discloses a resin composition and application thereof, wherein the resin composition and reinforcing fibers are not designed independently but are formed integrally in the process of preparing a metal foil laminated board by adopting the resin composition, the process of impregnating the fibers by using the resin composition is not existed, and the problem of reduced interlayer adhesive force caused by packing accumulation layers is also avoided. In addition, the prepreg prepared by the resin composition can be arbitrarily overlapped with the traditional prepreg, and the performance deficiency of the traditional metal foil-clad laminated board can be improved. The reinforcing fiber in the resin composition can be any one or the combination of at least two fibers, so that the diversity of the fibers in the plate is increased, and design conditions are created for improving the performance of the product by playing the advantages of various fibers through the combination of different fibers.
Description
Technical Field
The application relates to the technical field of metal foil-clad laminated plates, in particular to a resin composition, and also relates to a prepreg, a laminated plate, a metal foil-clad laminated plate and a circuit board which are manufactured by adopting the resin composition.
Background
The traditional copper-clad laminate is prepared by impregnating reinforcing materials with resin compositions to prepare prepregs, laminating a plurality of prepregs, and coating copper foils on two sides or one side of the prepregs by hot pressing.
Disclosure of Invention
The application aims to provide a novel resin composition for a metal foil-clad laminate, which does not need to impregnate a reinforcing material with the resin composition in the process of manufacturing the metal foil-clad laminate, and also does not have the problem that the resin composition cannot fully enter the reinforcing material due to the increase of the filler amount or the increase of the particle size.
The application also aims to provide a prepreg prepared from the resin composition, which has the advantages of large single weight range, strong binding power, high filler filling rate and the like.
It is still another object of the present application to provide a metal foil-clad laminate having high heat resistance, high interlayer reliability, low water absorption, low shrinkage, high insulation, excellent alkali resistance, excellent arc resistance, excellent breakdown voltage resistance and processability, which is produced using the above resin composition.
In a first aspect, the present application provides a resin composition characterized by comprising the following raw materials in parts by weight: 100 parts of epoxy resin, 1-60 parts of curing agent, 0.1-5 parts of accelerator, 200-3200 parts of reinforcing fiber and 20-950 parts of filler.
Optionally, the reinforcing fibers have a fiber diameter of 3-50 microns.
Optionally, the reinforcing fibers have a fiber length of 2000 micrometers to 50000 micrometers.
Optionally, the reinforcing fiber is selected from one or a mixture of at least two of glass fiber, carbon fiber, boron fiber, alumina fiber, basalt fiber, wood pulp fiber, cotton pulp fiber, aramid fiber and ramie fiber.
Alternatively, the resin composition has a gelation time of 80 to 300 seconds at 171 ℃.
Optionally, the epoxy resin has an epoxy equivalent weight of 100-700g/eq.
Optionally, the epoxy resin is selected from one or a mixture of at least two of o-cresol formaldehyde epoxy resin, phenol novolac epoxy resin, DCPD phenol novolac epoxy resin, BPA novolac epoxy resin, XYLOK novolac epoxy resin, trifunctional novolac epoxy resin, bisphenol a epoxy resin, silicone modified epoxy resin, phosphate modified epoxy resin, polyurethane modified epoxy resin, polybutadiene epoxy resin, brominated epoxy resin, DOPO modified epoxy resin, cyclotriphosphazene modified epoxy resin, diphenyl phosphine oxide epoxy resin, triglycidyl isocyanurate epoxy resin, para-aminophenol epoxy resin, diaminodiphenyl methane epoxy resin, aliphatic epoxy resin, alicyclic epoxy resin, bisphenol F epoxy resin, o-cresol epoxy resin.
Optionally, the curing agent is one or a combination of at least any two of dicyandiamide, modified dicyandiamide, linear phenolic aldehyde, o-resole, biphenyl phenolic aldehyde, benzoxazine, phosphorus-containing phenolic aldehyde, DDM and DDS.
Optionally, the filler is selected from one or a combination of at least any two of aluminum hydroxide, aluminum oxide, magnesium hydroxide, magnesium oxide, silicon dioxide, calcium carbonate, aluminum nitride, boron nitride, calcium nitride, silicon carbide, titanium dioxide, zinc oxide, zirconium oxide, mica, boehmite, talc, or kaolin; the particle size of the filler is distributed between 1 and 50 microns.
Preferably, the accelerator is selected from one or a combination of at least any two of 2-methylimidazole, 1-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-undecylimidazole and 2-phenyl-4-methylimidazole.
In a second aspect, the application also provides a prepreg, a laminated board, a metal foil-clad laminated board and a circuit board prepared by adopting the resin composition. The metal foil-clad laminate manufactured by using the resin composition comprises a laminate and metal foils coated on one side or two sides of the laminate. The laminated board is formed by laminating a plurality of final prepregs singly or by mixing and hot-pressing a plurality of prepregs manufactured by a traditional impregnation method for a metal foil-clad laminated board, so that the laminated board contains at least one final prepreg.
The resin composition of the application comprises the following beneficial effects:
1. in the resin composition, the epoxy resin and the reinforcing fiber are not designed independently, but are formed integrally, the process of impregnating the fiber by using the resin composition is not existed, and the problem of reduced interlayer adhesion caused by the accumulation of the filler is avoided, so the type and the amount of the filler can be designed according to the performance requirement;
2. the metal-clad laminate produced using the resin composition of the present application has high heat resistance, high interlayer reliability, low water absorption, low shrinkage, high insulation, excellent alkali resistance, arc resistance, breakdown voltage resistance, and processability;
3. the prepreg in the application can be optionally overlapped with the traditional prepreg, so that the prepreg in the application can be used for improving the performance deficiency of the traditional metal foil-clad laminated board;
4. the reinforcing fiber can be any one or the combination of at least two fibers, so that the diversity of the fibers in the plate is increased, and design conditions are created for improving the product performance by playing the advantages of various fibers through the combination of different fibers.
Detailed Description
The present application will be further described in detail with reference to the following examples, for the purpose of making the objects, technical solutions and advantages of the present application more apparent, and it should be understood that the specific examples are only for explaining the present application and are not limiting the present application.
In order to achieve the above object, the present application provides a resin composition comprising the following raw materials in parts by weight: 100 parts of epoxy resin, 1-60 parts of curing agent, 0.1-5 parts of accelerator, 200-3200 parts of reinforcing fiber and 20-950 parts of filler.
In the application, the fiber diameter of the reinforcing fiber is 3-50 microns, and the fiber length of the reinforcing fiber is 2000-50000 microns. The reinforcing fiber is selected from one or a mixture of at least two of glass fiber, carbon fiber, boron fiber, alumina fiber, basalt fiber, wood pulp fiber, cotton pulp fiber, aramid fiber and ramie fiber.
In the present application, the gelation time of the resin composition at 171℃is 80 to 300 seconds.
In the application, the epoxy equivalent of the epoxy resin is 100-700g/eq. The epoxy resin is selected from one or a mixture of at least two of phenol novolac epoxy resin, DCPD phenol novolac epoxy resin, BPA novolac epoxy resin, XYLOK novolac epoxy resin, trifunctional novolac epoxy resin, bisphenol A epoxy resin, organosilicon modified epoxy resin, phosphate modified epoxy resin, polyurethane modified epoxy resin, polybutadiene epoxy resin, brominated epoxy resin, DOPO modified epoxy resin, cyclotriphosphazene modified epoxy resin, diphenyl phosphine oxide epoxy resin, triglycidyl isocyanurate epoxy resin, para-aminophenol epoxy resin, diaminodiphenyl methane epoxy resin, aliphatic epoxy resin, alicyclic epoxy resin, bisphenol F epoxy resin and o-cresol epoxy resin.
In the application, the curing agent is one or a combination of at least any two of dicyandiamide, modified dicyandiamide, linear phenolic aldehyde, o-resole, biphenyl phenolic aldehyde, benzoxazine, phosphorus-containing phenolic aldehyde, DDM (4' diaminodiphenyl methane) and DDS (4, 4-diaminodiphenyl sulfone).
In the application, the filler is selected from one or a combination of at least any two of aluminum hydroxide, aluminum oxide, magnesium hydroxide, magnesium oxide, silicon dioxide, calcium carbonate, aluminum nitride, boron nitride, calcium nitride, silicon carbide, titanium dioxide, zinc oxide, zirconium oxide, mica, boehmite, talcum powder and kaolin; the particle size distribution of the filler is 1-50 microns;
in the application, the accelerator is selected from one or a combination of at least any two of 2-methylimidazole, 1-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-undecylimidazole and 2-phenyl-4-methylimidazole.
The application also provides a prepreg, a laminated board, a metal foil-clad laminated board and a circuit board which are prepared by adopting the resin composition.
The metal foil-clad laminate prepared using the resin composition of the present application was tested for 288 ℃ thermal stress, T260 thermal delamination time, 240 ℃ bake plate time, peel strength, flexural strength, dimensional stability, breakdown voltage, alkali resistance, volume resistivity, arc resistance, punching resistance, water absorption, dip soldering resistance after PCT 1 hour, and water absorption, and the following examples are further described and illustrated in detail.
Please refer to examples 1-9 and comparative examples 1-3, wherein examples 1-9 are metal foil clad laminates prepared by the method of the present application and comparative examples 1-3 are metal foil clad laminates prepared by conventional methods. The fabrics in comparative examples 1-9 and examples 1-3 are glass cloth-based fabrics manufactured by the traditional method, and the specific fabrics are S1141 glass cloth-based prepregs for the benefit technology. The embodiments of the present application will be described in detail below, but the present application is not limited to the scope of the embodiments.
The performance test methods are as follows:
a: thermal stress at 288 ℃): measured according to the IPC-TM-650.2.4.13.1 method.
B: t260 thermal stratification time: the determination was carried out according to the IPC-TM-650.2.4.24.1 method.
C: drying time at 240 ℃): the method is that the metal foil-clad laminated board with metal foil on both sides of the board is baked at 240 ℃, and when the bubbles are layered, the corresponding time is recorded.
D: peel strength: measured according to IPC-TM-650.2.4.8. Method.
E: flexural strength: the determination was carried out according to the IPC-TM-650.2.4.4 method.
F: dimensional stability: measured according to the IPC-TM-6502.4.3.9 method.
G: punching property: measured according to the method of GB/T4722-2017.5.
H: water absorption rate: the determination was carried out according to the IPC-TM-650.2.6.2.1 method.
I: resistance to dip soldering and water absorption after PCT 1 hour. The determination was carried out according to the IPC-TM-650.2.6.16 method.
J: alkali resistance: measured according to the method of GB/T4722-2017.2.
K: volume resistivity: measured according to the method of GB/T4722-2017.3.
L: arc resistance: measured according to the method of GB/T4722-2017.6.
M: breakdown voltage: measured according to the method of GB/T4722-2017.1.
TABLE 1 Material and description of the amounts of examples 1-9
Table 2 Material and usage description of comparative examples 1-3
Table 3 parameters for the production of the metal foil-clad laminates of examples 1 to 9
Table 4 production parameters of the metal foil-clad laminates of comparative examples 1 to 3
Table 5 test results for the metal foil clad laminate examples 1-9
Table 6 test results of comparative examples of the metal foil-clad laminates of comparative examples 1 to 3
The test results of comparative examples and comparative examples show that the metal clad laminate manufactured using the resin composition of the present application has high heat resistance, high interlayer reliability, low water absorption, low shrinkage, high insulation, excellent alkali resistance, arc resistance, breakdown voltage resistance, and processability, as compared to the conventional metal clad laminate.
Unlike the conventional method for preparing a metal foil-clad laminate, the resin composition and the reinforcing fibers are not separately designed but integrally formed in the process of preparing the metal foil-clad laminate by using the resin composition, so that the process of impregnating the fibers with the resin composition is not performed, and the problem of lowered interlayer adhesion caused by filler accumulation is not generated. In addition, the prepreg prepared by the resin composition can be arbitrarily overlapped with the traditional prepreg, and the performance deficiency of the traditional metal foil-clad laminated board can be improved. The reinforcing fiber in the resin composition can be any one or the combination of at least two fibers, so that the diversity of the fibers in the plate is increased, and design conditions are created for improving the performance of the product by playing the advantages of various fibers through the combination of different fibers.
The embodiments of the present application described above do not limit the scope of the present application.
Claims (10)
1. The integrally formed prepreg is characterized by being prepared from the following raw materials in parts by weight: 100 parts of epoxy resin, 1-60 parts of curing agent, 0.1-5 parts of accelerator, 200-3200 parts of reinforcing fiber and 20-950 parts of filler, wherein the fiber diameter of the reinforcing fiber is 3-50 microns, and the fiber length of the reinforcing fiber is 2000-50000 microns.
2. The prepreg of claim 1, wherein the reinforcing fibers are selected from one or a mixture of at least two of glass fibers, carbon fibers, boron fibers, alumina fibers, basalt fibers, wood pulp fibers, cotton pulp fibers, aramid fibers, ramie fibers.
3. The prepreg according to claim 1, wherein the resin composition has a gelation time of 80-300 seconds at 171 ℃.
4. The prepreg according to claim 1, wherein the epoxy resin has an epoxy equivalent weight of 100-700g/eq.
5. The prepreg of claim 1, wherein the epoxy resin is selected from one or a mixture of at least two of phenol novolac epoxy, DCPD phenol novolac epoxy, BPA novolac epoxy, XYLOK novolac epoxy, trifunctional novolac epoxy, bisphenol a epoxy, silicone modified epoxy, phosphate modified epoxy, polyurethane modified epoxy, polybutadiene epoxy, brominated epoxy, DOPO modified epoxy, cyclotriphosphazene modified epoxy, diphenyl phosphine oxide epoxy, triglycidylamine isocyanurate epoxy, para-aminophenol epoxy, diaminodiphenyl methane epoxy, aliphatic epoxy, cycloaliphatic epoxy, bisphenol F epoxy, o-cresol epoxy.
6. The prepreg of claim 1, wherein the curing agent is one or a combination of at least any two of dicyandiamide, modified dicyandiamide, novolac, resole, biphenol, benzoxazine, phosphorus-containing phenol, DDM, DDS.
7. The prepreg according to claim 1, wherein the filler is selected from one or a combination of at least any two of aluminum hydroxide, aluminum oxide, magnesium hydroxide, magnesium oxide, silicon dioxide, calcium carbonate, aluminum nitride, boron nitride, calcium nitride, silicon carbide, titanium dioxide, zinc oxide, zirconium oxide, mica, boehmite, talc, or kaolin; the particle size of the filler is distributed between 1 and 50 microns.
8. The prepreg according to claim 1, wherein the accelerator is selected from one or a combination of at least any two of 2-methylimidazole, 1-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-undecylimidazole, 2-phenyl-4-methylimidazole.
9. A laminate, characterized in that it contains at least one prepreg according to any one of claims 1 to 8.
10. A metal foil-clad laminate characterized by comprising a laminate and a metal foil laminated on one or both sides of the laminate; the laminate comprising at least one prepreg according to any one of claims 1 to 8.
Priority Applications (1)
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CN201911232109.7A CN110903603B (en) | 2019-12-05 | 2019-12-05 | Resin composition and application thereof |
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CN104744891A (en) * | 2013-12-27 | 2015-07-01 | 台燿科技股份有限公司 | Prepreg and application thereof |
CN108203544A (en) * | 2016-12-16 | 2018-06-26 | 惠州市源名浩科技有限公司 | A kind of printed circuit board and preparation method thereof |
CN109251481A (en) * | 2018-08-27 | 2019-01-22 | 张玉锦 | A kind of circuit board substrate and preparation method thereof that thermal diffusivity is good |
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