CN108148352A - Compositions of thermosetting resin, prepreg, laminate and printed circuit board - Google Patents
Compositions of thermosetting resin, prepreg, laminate and printed circuit board Download PDFInfo
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- CN108148352A CN108148352A CN201711439647.4A CN201711439647A CN108148352A CN 108148352 A CN108148352 A CN 108148352A CN 201711439647 A CN201711439647 A CN 201711439647A CN 108148352 A CN108148352 A CN 108148352A
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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
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- 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
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
-
- 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
-
- 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
- C08K3/346—Clay
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions 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 C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
-
- 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
- H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
-
- 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
- B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
- B32B2264/10—Inorganic particles
-
- 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
- B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
- B32B2264/10—Inorganic particles
- B32B2264/102—Oxide or hydroxide
-
- 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
- B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
- B32B2264/12—Mixture of at least two particles made of different materials
-
- 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
-
- 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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Dispersion Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
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Abstract
The disclosure provides compositions of thermosetting resin, prepreg, laminate and printed circuit board.The compositions of thermosetting resin includes：Thermosetting resin, inorganic filler and porous molybdenum compound.By using porous molybdenum compound as kollag, both dispersion and the settlement issues of molybdenum compound can effectively have been solved, it can be evenly distributed in prepreg, porous molybdenum compound has more excellent thermal conductivity, heat can be preferably conducted during drilling, situations such as being sticked in drill after can melting to avoid resin, while hole cracking can also be reduced, and the hole wall quality after drilling can be obviously improved.
Description
Technical field
The present invention relates to a kind of compositions of thermosetting resin and prepregs.In particular it relates to a kind of thermosetting property tree
Oil/fat composition, prepreg, laminate and printed circuit board.
Background technology
With rapid development of the electronic product in terms of miniaturization, multifunction, high performance and high reliability, printing electricity
Road plate starts to grow rapidly towards high-precision, high density, high-performance, microporous, slimming and multiple stratification direction, application range
It is more and more extensive, it is fast from departments such as industrial giant brain, communication instrument, electric measurement, national defence and Aeronautics and Astronautics
Speed enters civil electric appliance and its Related product.And basis material largely determines the performance of printed circuit board, because
There is an urgent need to develop the basis materials of a new generation for this.Basis material as future new era must have high heat resistance, low
Coefficient of thermal expansion and excellent chemical stability and mechanical performance.
In order to reduce the coefficient of thermal expansion of laminate, it will usually select the resin of low thermal coefficient of expansion or improve inorganic filler
Content.But low thermal coefficient of expansion resin structure is more special, cost is higher；And by the way of inorganic filler content is improved
The coefficient of thermal expansion of compound can not only be effectively reduced, and cost can also substantially reduce.But high fillingization resin can significantly drop
The drill processability and interlayer adhesion of low layer pressing plate.Therefore someone is using adding in the block fillers such as talcum as lubricant,
Improvement processability, but effect unobvious, and the addition of these block fillers is further degrading interlayer adhesion.Separately
Outside, in order to improve drill processability, metal molybdenum compound has been added, has been added in as mentioned in CN102656234A in thermosetting property
The metals such as zinc molybdate molybdenum compound improves processability in resin combination, and is recommended in the patent and be carried on talcum etc. and form
Molybdenum compound particle, this has that the interlayer adhesion of laminate is substantially reduced, and such molybdenum compound is in resin
In dispersibility it is poor, density is also larger, easily settles, and can not obtain satisfied result.
Invention content
One of the objects of the present invention is to provide a kind of compositions of thermosetting resin, prepreg, laminate and printed circuits
Plate, wherein porous molybdenum compound is used both effectively to solve dispersion and the settlement issues of molybdenum compound as kollag, make it
It is evenly distributed in prepreg, porous molybdenum compound has more excellent thermal conductivity, and when drilling preferably conducts heat, avoids setting
Fat is sticked to after melting in drill, while also reduces situations such as hole is cracked, and is obviously improved the hole wall quality after drilling.
In one aspect, the disclosure provides a kind of compositions of thermosetting resin, and the compositions of thermosetting resin includes：Heat
Thermosetting resin, inorganic filler and porous molybdenum compound.
Optionally, 0.01-10 weight of the porous molybdenum compound content for the compositions of thermosetting resin gross mass
Measure %.
Optionally, the porous molybdenum compound is selected from：Molybdenum disulfide, molybdenum dioxide, molybdenum trioxide, molybdate or molybdenum alloy
In any one or at least two mixture.
Optionally, the average grain diameter of the porous molybdenum compound is 0.1 to 50 μm.
Optionally, the porosity of the porous molybdenum compound is 5-80%.
Optionally, the aperture of the porous molybdenum compound is 50nm to 10 μm；It is preferred that 50nm to 1 μm.
Optionally, the thermosetting resin accounts for 20 to 70 weight % of compositions of thermosetting resin gross mass.
Optionally, the content of the inorganic filler is 10 to 80 weight % of the compositions of thermosetting resin gross mass.
Optionally, the inorganic filler is selected from：Silica, boehmite, aluminium oxide, talcum, mica, kaolin, hydrogen-oxygen
Change aluminium, magnesium hydroxide, zinc borate, zinc stannate, zinc oxide, titanium oxide, boron nitride, calcium carbonate, barium sulfate, barium titanate, aluminium borate,
In potassium titanate, E glass dust, S glass dust, D glass dust, NE glass dust, hollow powder or boehmite any one or at least
Two kinds of mixture.
Optionally, the average grain diameter of the inorganic filler is 0.1 to 100 μm.
Optionally, the compositions of thermosetting resin further includes curing agent, wherein the curing agent accounts for thermosetting resin group
Close 1 to 30 weight % of object gross mass.
Optionally, the compositions of thermosetting resin further includes accelerating agent, wherein the accelerating agent is in thermosetting resin group
The content in object is closed more than 0 and less than or equal in the range of 10 weight %.
On the other hand, the disclosure provides a kind of prepreg, and the prepreg includes reinforcing material and passes through impregnation drying
Compositions of thermosetting resin as described above attached thereto afterwards.
In another aspect, the disclosure provides a kind of laminate, wherein the laminate contains at least one as described above
Prepreg.
It yet still another aspect, the disclosure provides a kind of printed circuit board, wherein the printed circuit board contains at least one such as
The upper prepreg.
According to the disclosure, by using porous molybdenum compound as kollag, molybdenum compound both can be effectively solved
Dispersion and settlement issues, can be evenly distributed in prepreg, porous molybdenum compound have more excellent thermal conductivity, bore
Heat can be preferably conducted during hole, is sticked in drill after can melting to avoid resin, while the feelings such as hole cracking can also be reduced
Condition, and the hole wall quality after drilling can be obviously improved.
Specific embodiment
Below in conjunction with the specific embodiment of the disclosure, the technical solution in the embodiment of the present disclosure is carried out clear, complete
Site preparation describes, it is clear that described embodiment and/or embodiment are only a part of embodiment of the disclosure and/or implementation
The embodiment and/or embodiment of example rather than whole.Based on the embodiment and/or embodiment in the disclosure, this field is general
The every other embodiment and/or every other implementation that logical technical staff is obtained without making creative work
Example belongs to the range of disclosure protection.
In the disclosure, all numerical characteristics all refer within the error range of measurement, for example, the numerical value limited ±
Within 10% or within ± 5% or within ± 1%.
"comprising" of the present invention, " comprising " or " containing ", it is intended that it can also have other groups in addition to the component
Part, these other components assign the prepreg different characteristics.In addition to this, "comprising" of the present invention, " comprising " or
" containing " can also include " substantially by ... form ", and could alternatively be " for " or " by ... form ".
In the disclosure, if do not particularly pointed out, what amount, ratio etc. were by weight.
As described above, the disclosure can provide a kind of compositions of thermosetting resin, the compositions of thermosetting resin includes：
Thermosetting resin, inorganic filler and porous molybdenum compound.
The disclosure in compositions of thermosetting resin by including porous molybdenum compound, the lamination for the preparation that can not only be improved
The thermal conductivity of plate and the drill processability for being obviously improved laminate, and hole wall quality can be obviously improved.It is further, since more
The density of hole molybdenum compound is small, and to be porous, good with the compatibility of resin system, does not need to using complicated dispersing apparatus
The resin combination that can be uniformly dispersed and stablized.
According to another embodiment of the disclosure, the porous molybdenum compound content can be the thermosetting resin group
Close the about 0.01 weight % to about 10 weight %, preferably from about 0.5 weight % to about 5 weight % of object gross mass.By by the content
It is arranged in the range, can further improve drill processability, and do not interfere with the original of compositions of thermosetting resin
Overall performance.
According to another embodiment of the disclosure, the porous molybdenum compound can be selected from：Molybdenum disulfide, titanium dioxide
In molybdenum, molybdenum trioxide, molybdate or molybdenum alloy any one or at least two mixture.
The example of molybdenum alloy can include：Mo-Au alloys, Mo-Ag alloys, Mo-Cu alloys, Mo-Al alloys, Mo-Ti are closed
Gold, molybdenum silicon boron triple-phase alloys etc..
The example of molybdate can include：Ammonium molybdate, sodium molybdate, zinc molybdate, calcium molybdate, magnesium molybdate etc..
It is prepared by the method that porous zinc molybdate is referred to described in the embodiment of CN 101660078A.By adjusting technique
Condition can prepare the porous zinc molybdate with different porosities, aperture and grain size.
According to another embodiment of the disclosure, the average grain diameter of the porous molybdenum compound can be about 0.1 μm extremely
About 50 μm, preferably from about 0.5 μm to about 20 μm.
By the way that the average grain diameter of porous molybdenum compound is arranged in the range, expected effect can be realized, simultaneously
Being mixed into probability and inhibiting to cause the undesirable generation of oversize grain for oversize grain can be reduced.
According to another embodiment of the disclosure, the porosity of the porous molybdenum compound can be about 5% to about
80%, preferably from about 20% to about 70%.When porosity is less than 5%, is nearly solid solid, the special effect of porous compounds
It should cannot reach；After porosity is more than 80%, heat conductivility is deteriorated, and resin is easily bonded in drill surface, it is caused to add
Work is deteriorated.The aperture of the porous molybdenum compound can be more than 50nm to 10 μm, preferably 50-1 μm, when aperture is less than 50nm
When, due to capillarity, resin compound is difficult in access aperture, and the special effects of porous compounds cannot reach；Work as aperture
More than 10 μm, heat conductivility also rapid drawdown therewith, it is impossible to reach the special effects of porous compounds, overall effect is also deteriorated..It is logical
It crosses and puts the porosity of porous molybdenum compound and aperture in the range, further can effectively solve the dispersion of molybdenum compound
And settlement issues, it can be evenly distributed in prepreg.
According to another embodiment of the disclosure, the thermosetting resin can account for compositions of thermosetting resin gross mass
About 20 weight % to about 70 weight %, preferably from about 25 weight % to about 65 weight %, further preferably about 30 weight % are to about
60 weight %.The mass percent that the thermosetting resin accounts for compositions of thermosetting resin gross mass can be, for example, about 23 weights
Measure %, about 26 weight %, about 31 weight %, about 35 weight %, about 39 weight %, about 43 weight %, about 47 weight %, about 51 weights
Measure %, about 55 weight % about, about 59 weight %, about 63 weight % or about 67 weight % and any range between them, example
Such as from about 23 weight %, about 26 weight %, about 31 weight %, about 35 weight % or about 39 weight % are to about 43 weight %, about 47 weights
Measure %, about 51 weight %, about 55 weight % about, about 59 weight %, about 63 weight % or about 67 weight %.
According to another embodiment of the disclosure, the content of the inorganic filler can be that the thermosetting resin combines
About 10 weight % of object gross mass to about 80 weight %, preferably from about 20 weight % are to about 60 weight %, for example, about 23 weight %, about
28 weight %, about 32 weight %, about 37 weight %, about 42 weight %, about 47 weight %, about 52 weight %, about 57 weight %, about
62 weight %, about 67 weight %, about 72 weight %, about 76 weight % or about 78 weight % and any range between them,
Such as from about 23 weight %, about 28 weight %, about 32 weight %, about 37 weight % or about 42 weight % are to about 47 weight %, about 52 weights
Measure %, about 57 weight %, about 62 weight %, about 67 weight %, about 72 weight %, about 76 weight % or about 78 weight %.
By the way that the content of inorganic filling material is arranged in the range, thermosetting resin can be kept to combine well
The formability and low thermal expansion of object, and in the case where realizing high fillingization inorganic filler and using porous molybdenum compound,
It can inhibit the deterioration of drill processability and interlayer adhesion, obtained laminate has low coefficient of thermal expansion, excellent brill
Hole machined and heat resistance and high interlayer adhesion.
According to another embodiment of the disclosure, the inorganic filler can be selected from：Silica, boehmite, oxidation
Aluminium, talcum, mica, kaolin, aluminium hydroxide, magnesium hydroxide, zinc borate, zinc stannate, zinc oxide, titanium oxide, boron nitride, carbonic acid
Calcium, barium sulfate, barium titanate, aluminium borate, potassium titanate, E glass dust, S glass dust, D glass dust, NE glass dust, hollow powder or vigorous
In nurse stone any one or at least two mixture.
The example of hollow powder can include：Hollow silicon dioxide, hollow boron nitride, hollow glass powder, hollow alumina
Deng.
According to another embodiment of the disclosure, the average grain diameter of the inorganic filler can be about 0.1 μm to about 100
μm, preferably from about 0.5 μm to about 20 μm.It, can be well by the way that the average grain diameter of inorganic filler is arranged in the range
Mobility during high filling in compositions of thermosetting resin is kept, and at the same time can reduce oversize grain is mixed into probability and suppression
System causes the undesirable generation of oversize grain.Here, average grain diameter refers to the total volume of particle being obtained based on grain as 100%
During the accumulation number of degrees distribution curve of diameter, the grain size for the point that volume is 50% is just equivalent to, it can be to use laser diffraction and scattering
The particle size distribution of method.
According to another embodiment of the disclosure, the compositions of thermosetting resin can further include curing agent.It is described
Curing agent can account for about 1 weight % to the about 30 weight % preferably from about 4 weight % to about 25 of compositions of thermosetting resin gross mass
Weight %, further preferably about 10 weight % are to about 20 weight %, for example, about 2 weight %, about 5 weight %, about 8 weight %, about
11 weight %, about 14 weight %, about 17 weight %, about 19 weight %, about 22 weight %, about 26 weight % or about 28 weight % with
And any range between them, such as from about 2 weight %, about 5 weight %, about 8 weight %, about 11 weight % or about 14 weight % are extremely
About 17 weight %, about 19 weight %, about 22 weight %, about 26 weight % or about 28 weight %.
According to another embodiment of the disclosure, the compositions of thermosetting resin can further include accelerating agent.It is described
Content of the accelerating agent in compositions of thermosetting resin can be excellent in the range of more than 0 and less than or equal to about 10 weight %
It is selected in the range of about 1 weight % to about 10 weight %, further preferably in the range of about 2 weight % to about 8 weight %, example
Such as from about 0.5 weight %, about 1.5 weight %, about 2.5 weight %, about 3.5 weight %, about 4.5 weight %, about 5.5 weight %, about
6.5 weight %, about 7.5 weight %, about 8.5 weight % or about 9.5 weight % and any range between them, such as from about 0.5
Weight %, about 1.5 weight %, about 2.5 weight %, about 3.5 weight % or about 4.5 weight % are to about 5.5 weight %, about 6.5 weights
Measure %, about 7.5 weight %, about 8.5 weight % or about 9.5 weight %.
According to another embodiment of the disclosure, the compositions of thermosetting resin further includes solvent.
The disclosure can also provide a kind of prepreg, and the prepreg includes reinforcing material and by adhering to after impregnation drying
The compositions of thermosetting resin as described in any one above on it.
The example of reinforcing material can include glass-fiber-fabric.In the following description, glass-fiber-fabric reinforcing material and glass-fiber-fabric can
To be used interchangeably.
Compositions of thermosetting resin can include thermosetting resin, curing agent, accelerating agent and solvent.Heat of the present invention
Thermosetting resin for it is cross-linking formed reticular structure polymer in arbitrary a kind or at least two kinds of of combination, preferred epoxy,
Phenolic resin, cyanate ester resin, polyamide, polyimide resin, polyether resin, polyester resin, hydrocarbon resin or organosilicon
Arbitrary a kind or at least two kinds of of combination in resin；Further preferred epoxy resin or phenolic resin.
The concrete example of the combination of the thermosetting resin can be the combination of epoxy resin and polyamide, polyimides
The combination of resin and hydrocarbon resin, the combination of cyanate ester resin, polyamide and polyether resin, cyanate ester resin, polyamide resin
Combination of fat, polyimide resin and epoxy resin etc..
Combination for epoxy resin and its with other resins, the curing agent can be phenolic resin, anhydride compound, work
In property ester type compound, dicyandiamide, diaminodiphenylmethane, diaminodiphenylsulfone, diaminodiphenyl ether and maleimide
One or more kinds of mixtures；The curing accelerator is 2-methylimidazole, 2-ethyl-4-methylimidazole and 2-
The mixture of one or more of methyl 4-phenyl imidazoles；
Combination for phenolic resin and its with other resins, the curing agent can be organic acid anhydride, organic amine, Louis
This acid, organic amide, glyoxaline compound, organic phosphine compound and its mixture mixed in any proportion.
Reactable polyphenylene oxide resin, polyamide for olefin resin, containing two or more unsaturated double-bonds
Resin and its with other resin combinations, the curing agent is selected from organic peroxide crosslinking agent, preferably peroxidating diisopropyl
Benzene, benzoyl peroxide, di-tert-butyl peroxide, two carbon of diacetyl peroxide, peroxide tert pivalate ester and peroxidating
It is one or more in sour hexichol oxide ester.The accelerating agent is allylic organic compound, preferably triallyl cyanogen urea
In acid esters, Triallyl isocyanurate, trimethylol-propane trimethacrylate and trimethylolpropane trimethacrylate
It is one or more.
For organic siliconresin, the accelerating agent is selected from organic platinum-like compounds.
The compositions of thermosetting resin can further include silane coupling agent or/and wetting dispersing agent.As these silane
Coupling agent, if be that typically in inorganic orderliness I be surface-treated used in silane coupling agent, there is no special
It limits.It as concrete example, can enumerate, gamma-aminopropyl-triethoxy-silane, N- β-(aminoethyl)-γ-aminopropyl trimethoxy
The epoxy silanes systems such as the aminopropyl silanes such as silane system, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl third
The vinyl silanes such as base trimethoxy silane system, N- β-(N- vinyl benzene idols sulfonylaminoethyl)-γ-aminopropyl trimethoxy silicon
The anion silicons such as heptane hydrochloride salt methane series, phenyl silane system etc. can select a kind therein or at least two kinds of appropriately combined uses.
As long as in addition, the Ricinate that Ricinate uses in compositions of thermosetting resin, just there is no particular limitation.It can
Enumerating the Disperbyk-110 such as BYKChemie Japan, 111,180,161, BYK-W996, W9010, W903
Ricinate.
The compositions of thermosetting resin can also contain various additives, as concrete example, can enumerate fire retardant, resist
Oxygen agent, heat stabilizer, antistatic agent, ultra-violet absorber, pigment, colorant or lubricant etc..These various additives can be with
It is used alone, two kinds or two or more can also be used in mixed way.
It, can be by well known method as described in cooperation, stirring, mixing as the preparation method of invention resin composition
Thermosetting resin, inorganic filler, porous molybdenum compound, curing agent and accelerating agent and various additives, to prepare.
It as the solvent in the present invention, is not particularly limited, as concrete example, the alcohol such as methanol, ethyl alcohol, butanol can be enumerated
Class, the ethers such as ethyl cellosolve, butyl cellosolve, ethylene glycol-methyl ether, carbitol, butyl carbitol, acetone, butanone, methyl second
The ketones such as base ketone, hexone, cyclohexanone, toluene, dimethylbenzene, mesitylene etc. are aromatic hydrocarbon, ethyoxyl second
The esters such as yl acetate, ethyl acetate, n,N-Dimethylformamide, n,N-dimethylacetamide, n-methyl-2-pyrrolidone etc.
Nitrogen-containing solvent.Above-mentioned solvent can be used alone, can also two kinds or it is two or more be used in mixed way, preferably toluene,
The aromatic hydrocarbon solvents such as dimethylbenzene, mesitylene and acetone, butanone, methyl ethyl ketone, hexone, cyclohexanone
Ketones flux is waited to be used in mixed way.Usage amount those skilled in the art of the solvent can select according to the experience of oneself, make
Obtained resin adhesive liquid reaches the viscosity suitable for using.
Specifically, disperseed by mechanical agitation, emulsification or ball milling, compositions of thermosetting resin is configured to glue, then
Glass-fiber-fabric is infiltrated using the glue, drying obtains prepreg.By the hot pressing in the vacuum press of the prepreg and metal foil such as copper foil
Laminate can be prepared.
Specifically, it may comprise steps of by the method that reinforcing material prepares laminate：
(1) glue：Solvent is added in proportion container, epoxy resin, curing agent solution and rush are separately added under stirring
Into the solution of agent.After stirring, inorganic filler is added in, continues to stir, obtains glue,
(2) it impregnates：Reinforcing material is immersed in glue.
(3) it is impregnated with：By the reinforcing material of dipped glue by vertical or horizontal type containing dipping machine, by control squeeze wheel speed,
Prepreg is made in the conditions such as linear speed, wind-warm syndrome and furnace temperature.
Specifically using vertical demonstration example containing dipping machine as：Squeeze wheel speed：- 1.3 to -2.5 ± 0.1M/min.Main line speed：4 to 18m/
min.Wind-warm syndrome：120 to 170 DEG C.Furnace temperature：130 to 220 DEG C.
(4) it suppresses：After the prepreg reduced and metal foil such as copper foil are combined, it is put into vacuum hotpressing machine, by one
Simultaneously metal-coated laminated board such as copper clad laminate is finally made in fixed temperature, time and pressure, and specific demonstration example is：
Temperature formula：
130℃/30min+155℃/30min+190℃/90min+220℃/60min。
Pressure formula：
25kgf·cm-2/30min+50kgf·cm-2/30min+90kgf·cm-2/120min+30kgf·cm-2/
90min。
Vacuum formula：
30mmHg/130min+800mmHg/130min。
By above procedure, prepreg is laminated between metal foil such as copper foil, laminate is can be prepared by after hot pressing
(that is, copper clad laminate).
The disclosure can also provide a kind of laminate and a kind of printed circuit board.
Laminate can contain an at least prepreg as described in any one above.
Printed circuit board can contain an at least prepreg as described in any one above.
According to the disclosure, by using porous molybdenum compound as kollag, molybdenum compound both can be effectively solved
Dispersion and settlement issues, can be evenly distributed in prepreg, porous molybdenum compound have more excellent thermal conductivity, bore
Heat can be preferably conducted during hole, is sticked in drill after can melting to avoid resin, while the feelings such as hole cracking can also be reduced
Condition, and the hole wall quality after drilling can be obviously improved.
In addition, by including porous molybdenum compound, the lamination for the preparation that can not only be improved in compositions of thermosetting resin
The thermal conductivity of plate and the drill processability for being obviously improved laminate, and hole wall quality can be obviously improved.It is further, since more
The density of hole molybdenum compound is small, and to be porous, good with the compatibility of resin system, does not need to using complicated dispersing apparatus
The resin combination that can be uniformly dispersed and stablized.
Embodiment
The technical solution further illustrated the present invention below by specific embodiment.
Porosity in embodiment is measured using volume weight method, and aperture is measured using mercury injection apparatus.
Embodiment 1-22
By brominated bisphenol a type epoxy resin (DOW Chemical, epoxide equivalent 435, bromine content 19%, ProductName DER530)
(epoxy resin), dicyandiamide (curing agent), 2-methylimidazole (accelerating agent), porous zinc molybdate (porous molybdenum compound) and melting two
Silica (Singapore's silicon than section, 525,2 μm of average grain diameter) is added in butanone (solvent), mechanical agitation and be configured to 65 weights
The glue of % is measured, glass fabric (7628, Zhuhai Zhu Bo Electron Material Co., Ltd) (reinforcing material) is then impregnated with, by adding
Prepreg (prepreg) is formed after heated drying, copper foil is placed on two sides, and copper clad laminate is made in pressurized, heated.
The copper clad laminate of embodiment and comparative example is prepared according to following preparation process：
(1) glue：Solvent is added in proportion container, epoxy resin, curing agent and accelerating agent are separately added under stirring；It stirs
After mixing 2 hours, porous molybdenum compound and inorganic filler are added in, continues stirring 6 hours, obtains glue.
(2) it impregnates：Reinforcing material is immersed in glue.
(3) it is impregnated with：The reinforcing material of dipped glue is squeezed into wheel speed, linear speed, wind-warm syndrome containing dipping machine by vertical by control
And the conditions such as furnace temperature, prepreg is made.The vertical condition containing dipping machine is：Squeeze wheel speed：-1.8±0.1M/min；Main line speed：
10m/min；Wind-warm syndrome：150℃；Furnace temperature：180℃.
(3) it suppresses：After the prepreg reduced and copper foil are combined, it is put into vacuum hotpressing machine, by certain temperature,
Simultaneously copper clad laminate is finally made in time and pressure, and actual conditions are：
Temperature formula：
130℃/30min+155℃/30min+190℃/90min+220℃/60min；
Pressure formula：
25kgf·cm-2/30min+50kgf·cm-2/30min+90kgf·cm-2/120min+30kgf·cm-2/
90min；
Vacuum formula：
30mmHg/130min+800mmHg/130min。
By above procedure, 8 thickness is used to be laminated on for the prepreg of 0.2mm between the copper foil of 35 μ m-thicks, after hot pressing
It can be prepared by the laminate of 1.6mm thickness.Obtain copper clad laminate.Using obtained copper clad laminate, with method described below,
To drill processability, hole wall lineae ablicantes, estimation of stability, 1 the results are shown in Table.
Embodiment 23
By brominated bisphenol a type epoxy resin (DOW Chemical, epoxide equivalent 435, bromine content 19%, ProductName DER530)
(epoxy resin), dicyandiamide (curing agent), 2-methylimidazole (accelerating agent), porous silica molybdenum are (according to 105977479 A of CN
Prepare) (porous molybdenum compound) and boehmite (one Shi Tong materials Science and Technology Co., Ltd. of Anhui, BG601,0.5 μ of average grain diameter
M) be added in butanone (solvent), mechanical agitation and the glue for being configured to 65 weight %, be then impregnated with glass fabric (7628,
Zhuhai Zhu Bo Electron Material Co., Ltd) (reinforcing material), prepreg (prepreg) is formed after heat drying, two sides is put
Copper foil is put, copper clad laminate is made in pressurized, heated.
With method similarly to Example 1, the copper clad laminate using resin combination is obtained.It measures, evaluation result is shown
In table 2.
Embodiment 24
By 100g brominated bisphenol a type epoxy resin (DOW Chemical, epoxide equivalent 435, bromine content 19%, ProductName
DER530), 24g linear phenol-aldehyde resins (Japanese group is flourish, hydroxyl equivalent 105, ProductName TD2090), 0.05g 2-methylimidazoles,
(one stone of Anhui leads to material for porous silica molybdenum (according to 105977479 A of CN preparations) (porous molybdenum compound) and 50g boehmites
Science and Technology Co., Ltd., BG601,0.5 μm of average grain diameter) be added in butanone (solvent), mechanical agitation and be configured to 65 weights
The glue of % is measured, glass fabric (7628, Zhuhai Zhu Bo Electron Material Co., Ltd) (reinforcing material) is then impregnated with, by adding
Prepreg (prepreg) is formed after heated drying, copper foil is placed on two sides, and copper clad laminate is made in pressurized, heated.
Embodiment 25
By 20g phenol novolak type cyanate PT30,40g ortho-methyl phenol phenol aldehyde type epoxy resin N695,20g bromination benzene second
Alkene and suitable octoate catalyst zinc, 0.05g 2- phenylimidazoles, porous silica molybdenum (being prepared according to 105977479 A of CN)
(porous molybdenum compound) and 50g boehmites (one Shi Tong materials Science and Technology Co., Ltd. of Anhui, BG601,0.5 μm of average grain diameter)
Be added in butanone (solvent), mechanical agitation and the glue for being configured to 65 weight %, be then impregnated with glass fabric (7628, pearl
Hai Zhu glass Electron Material Co., Ltd) (reinforcing material), prepreg (prepreg) is formed after heat drying, two sides is placed
Copper clad laminate is made in copper foil, pressurized, heated.
Embodiment 26
By 30g dicyclopentadiene epoxy HP-7200H, 60g benzoxazine colophony D125,5g linear phenolic resins EPONOL
6635M65,5g dicyandiamide, porous silica molybdenum (prepare) (porous molybdenum compound) and the vigorous nurses of 50g according to 105977479 A of CN
Stone (one Shi Tong materials Science and Technology Co., Ltd. of Anhui, BG601,0.5 μm of average grain diameter) is added in butanone (solvent), machinery
The glue of 65 weight % is stirred and be configured to, is then impregnated with glass fabric (7628, Zhuhai Zhu Bo Electron Material Co., Ltd)
(reinforcing material) forms prepreg (prepreg) after heat drying, and copper foil is placed on two sides, and copper clad layers are made in pressurized, heated
Pressing plate.
Embodiment 24-26 with method similarly to Example 1, obtains the copper clad laminate using resin combination.It surveys
Determine, evaluation result is shown in table 3.
Comparative example 1
In addition to zinc molybdate (Kemgard, 911B) is substituted outside porous molybdenum compound, with method similarly to Example 1, obtain
To the copper clad laminate for using resin combination.It measures, evaluation result is shown in table 4.
Comparative example 2
Other than mismatching porous molybdenum compound, with method similarly to Example 1, covering using resin combination is obtained
Copper laminated board.It measures, evaluation result is shown in table 4.
1st, the evaluation of drill processability
By the copper-clad plate of making, two piece one is folded, use the new knives of 0.3mm drilling machine (HITACHI NDR-1V 212E) with
The rotating speed of 155krmp carries out Drilling operation, and every piece of twist drill 6 is every that knife is bored 6000 holes new knife.By the drill of different hole numbers
Drill bit knife edge part is observed using microscope verifier (herding moral PM-2824 in Taiwan), measures cutting edge tip abrasion back amount to survey
The distance for measuring vertical line and central axes intersection point and abrasion top edge is drill size, and the wear rate of drill is calculated by the following formula
To evaluate drilling effect.Wear rate %=drilling back edges and central axes distance/drilling leading edge and central axes distance × 100%
2nd, hole wall lineae ablicantes is tested
By the plank de-smear that hole number is 5000, then copper facing makes slice, using micro- sem observation and measures hole wall
The length of lineae ablicantes, length is longer to illustrate that hole wall quality is poorer.
3rd, the estimation of stability of resin combination
100ml resin combinations are placed in the band plug graduated cylinder of 100ml, are stood in 25 DEG C of environment, measure sediment
It is detained to the time of the bottom of sedimentation pipe, evaluates stability.
Overall merit：
Wear rate is less than or equal to 80%, hole wall lineae ablicantes less than or equal to 80 μm and stability is greater than or equal to 7 days
Sample is assessed as outstanding；
By wear rate be less than or equal to 95% and more than 80%, hole wall lineae ablicantes be less than or equal to 105 μm and more than 85 μm and
Stability is greater than or equal to 3 days and the sample less than 7 days is assessed as qualification；And
By wear rate be more than the sample of 95%, 105 μm of hole wall lineae ablicantes and stability less than 3 days be assessed as it is unqualified.
Table 3
Table 4
It can be seen that for embodiment 1-22 and comparative example 1-2 from table 1-4, add porous molybdenum compound and compare non-poreization
The stability for closing object is remarkably reinforced, and its drilling property, also significantly than being not added with the good of porous molybdenum compound, hole wall quality is also bright
It is aobvious to improve.It is the thermosetting resin group in the amount for adding porous molybdenum compound for embodiment 1-4 and embodiment 16-17
In the case of the 0.01-10 weight % for closing object gross mass, it can further improve drilling property and hole wall quality, while improve combination
The stability of object.From the point of view of embodiment 5-9 and comparative example 20-21, porous molybdenum compound grain size is smaller, the compatibility with resin
Better, stability is better, play processability it is also better, and its be greater than or equal to 0.01 μm when, due to its dispersibility
Become more preferable, it is not easy to reunite；Similarly, when grain size is less than or equal to 50 μm, sedimentation stability significantly becomes more preferable, and
And drilling performance is also obtained reinforcement.In addition, for embodiment 11-12 and comparative example 20-21, porosity is in 5-80%, especially
It is that porosity its sedimentation stability in 20-60% is best, and its drill processability is also best.
Obviously, those skilled in the art can carry out the embodiment of the present disclosure various modification and variations without departing from this public affairs
The spirit and scope opened.In this way, if these modifications and variations of the disclosure belong to disclosure claim and its equivalent technologies
Within the scope of, then the disclosure is also intended to include these modifications and variations.
Claims (13)
1. a kind of compositions of thermosetting resin, the compositions of thermosetting resin includes：Thermosetting resin, inorganic filler and more
Hole molybdenum compound.
2. compositions of thermosetting resin as described in claim 1, wherein the porous molybdenum compound content is the thermosetting property
The 0.01-10 weight % of resin combination gross mass.
3. compositions of thermosetting resin as claimed in claim 1 or 2, wherein the porous molybdenum compound is selected from：Molybdenum disulfide,
In molybdenum dioxide, molybdenum trioxide, molybdate or molybdenum alloy any one or at least two mixture.
4. compositions of thermosetting resin as described in claim 1, wherein the average grain diameter of the porous molybdenum compound for 0.1 to
50μm。
5. compositions of thermosetting resin as described in claim 1, wherein the porosity of the porous molybdenum compound is 5-80%.
6. compositions of thermosetting resin as described in claim 1, wherein the aperture of the porous molybdenum compound is 50nm to 10 μ
m；Preferably, the aperture of the porous molybdenum compound is 50nm to 1 μm.
7. compositions of thermosetting resin as described in claim 1, wherein the thermosetting resin accounts for compositions of thermosetting resin
20 to 70 weight % of gross mass.
8. compositions of thermosetting resin as described in claim 1, wherein the content of the inorganic filler is the thermosetting property tree
10 to 80 weight % of oil/fat composition gross mass.
9. compositions of thermosetting resin as described in claim 1, wherein the inorganic filler is selected from：Silica, boehmite,
Aluminium oxide, talcum, mica, kaolin, aluminium hydroxide, magnesium hydroxide, zinc borate, zinc stannate, zinc oxide, titanium oxide, boron nitride,
Calcium carbonate, barium sulfate, barium titanate, aluminium borate, potassium titanate, E glass dust, S glass dust, D glass dust, NE glass dust, hollow powder
Or in boehmite any one or at least two mixture.
10. compositions of thermosetting resin as described in claim 1, wherein the average grain diameter of the inorganic filler is 0.1 to 100
μm。
11. a kind of prepreg, the prepreg includes reinforcing material and by attached thereto as right will after impregnation drying
Seek the compositions of thermosetting resin described in 1.
12. a kind of laminate, the laminate contains an at least prepreg as claimed in claim 11.
13. a kind of printed circuit board, the printed circuit board contains an at least prepreg as claimed in claim 11.
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| WO2019126928A1 (en) * | 2017-12-25 | 2019-07-04 | 广东生益科技股份有限公司 | Thermosetting resin composition, prepreg, laminate, and printed circuit board |
| CN114700480A (en) * | 2022-04-25 | 2022-07-05 | 长沙升华微电子材料有限公司 | Production method for obtaining high-thermal-conductivity tungsten-copper alloy |
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