CN109486111A - A kind of compositions of thermosetting resin and application thereof - Google Patents
A kind of compositions of thermosetting resin and application thereof Download PDFInfo
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- CN109486111A CN109486111A CN201811317989.3A CN201811317989A CN109486111A CN 109486111 A CN109486111 A CN 109486111A CN 201811317989 A CN201811317989 A CN 201811317989A CN 109486111 A CN109486111 A CN 109486111A
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- thermosetting resin
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- alkene
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- 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
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/067—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of fibres or filaments
-
- 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
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- 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
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C08L61/04, C08L61/18 and C08L61/20
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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
-
- 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
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
- B32B2260/021—Fibrous or filamentary layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/04—Impregnation, embedding, or binder material
- B32B2260/046—Synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- 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
- B32B2307/206—Insulating
-
- 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
- B32B2307/70—Other properties
- B32B2307/732—Dimensional properties
- B32B2307/734—Dimensional stability
-
- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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)
- Microelectronics & Electronic Packaging (AREA)
- Reinforced Plastic Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a kind of compositions of thermosetting resin and application thereof, and compositions of thermosetting resin contains thermosetting resin and inorganic filler, and carries out cladding processing to the inorganic filler using molybdenum disulfide alkene；Based on compositions of thermosetting resin gross mass, the content of inorganic filler is 10wt%~80wt%.Compositions of thermosetting resin provided by the invention, treatment inorganic filling material is coated by using molybdenum disulfide alkene, the compatibility that inorganic filler and resin system can be effectively improved is good, does not need to can be obtained using complicated dispersing apparatus and is uniformly dispersed and stable resin combination.Prepreg provided by the invention is made and being impregnated into reinforcing material and drying with above-mentioned compositions of thermosetting resin, is effectively solved the dispersion and settlement issues of molybdenum compound, can be evenly distributed in prepreg.Laminate provided by the invention contains an at least above-mentioned prepreg；Printed circuit board provided by the invention contains an at least above-mentioned prepreg.
Description
Technical field
The present invention relates to a kind of compositions of thermosetting resin and application thereof.
Background technique
Printed circuit board starts swift and violent towards high-precision, high density, high-performance, microporous, slimming and multiple stratification direction
Development, will be used wider and wider general, and basis material largely determines the performance of printed circuit board.It is at present
Reduce the thermal expansion coefficient of laminate, it will usually select the resin of low thermal coefficient of expansion or improve the content of inorganic filler.But
It is that low thermal coefficient of expansion resin structure is more special, higher cost；And can not only be had by the way of improving inorganic filler content
Effect reduces the thermal expansion coefficient of compound, and cost can also substantially reduce.But high fillingization resin can be substantially reduced laminate
Drill processability and interlayer adhesion.Therefore someone improves processing using the block fillers such as talcum are added as lubricant
Property, but effect is unobvious, and the addition of these block fillers is further degrading interlayer adhesion.In addition, in order to mention
High drill processability has been added metal molybdenum compound, and the metal molybdenums such as zinc molybdate are added in compositions of thermosetting resin
Closing object improves processability, and molybdenum compound particle is carried on talcum etc., and there are the interlayer adhesions of laminate to be substantially reduced for this
The problem of, and dispersibility of such molybdenum compound in resin is poor, and density is also larger, easily settles, and is unable to get full
The result of meaning.
Summary of the invention
In view of this, the thermosetting property tree of a kind of the present invention provides thermal expansivities low, drill processability and excellent heat resistance
Oil/fat composition and application thereof.
The technological means that the present invention uses is as follows:
A kind of compositions of thermosetting resin, the compositions of thermosetting resin contain thermosetting resin and inorganic filler, and
And cladding processing is carried out to the inorganic filler using molybdenum disulfide alkene；Based on the compositions of thermosetting resin gross mass,
The content of the inorganic filler is 10wt%~80wt%.
Compositions of thermosetting resin provided by the invention coats treatment inorganic filling material by using molybdenum disulfide alkene, can have
Effect improves the compatibility of inorganic filler and resin system, does not need to can be obtained using complicated dispersing apparatus and is uniformly dispersed and surely
Fixed resin combination, hot curing resin composition of the invention are especially suitable for that thermal expansivity is low and drilling processing
In electronic component of property and excellent heat resistance etc..
A kind of prepreg is made and being impregnated into reinforcing material and drying with above-mentioned compositions of thermosetting resin.
Prepreg provided by the invention, the compositions of thermosetting resin used are handled by using molybdenum disulfide alkene cladding
Inorganic filler both can effectively solve the dispersion and settlement issues of molybdenum compound, can be evenly distributed in prepreg, warp
The inorganic filler of molybdenum disulfide alkene cladding has more excellent thermal conductivity, and when drilling can preferably conduct heat, can be to avoid
Resin is sticked in drill after melting, while can also reduce situations such as hole is cracked, and can be obviously improved the hole wall after drilling
Quality.
A kind of laminate, the laminate contain an at least above-mentioned prepreg.
According to the present invention, using laminate made of above-mentioned prepreg, in processing, its drill processability is very excellent,
Also there is good electrical insulating property and low heat expansion.
A kind of printed circuit board, the printed circuit board contain an at least above-mentioned prepreg.
According to the present invention, using printed circuit board made of above-mentioned prepreg, in processing, its drill processability is very
It is excellent, it may have good electrical insulating property and low heat expansion.
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 description, it is clear that described embodiment and/or embodiment are only a part of embodiment of the disclosure and/or implementation
Example, rather than whole embodiments and/or embodiment.Based on the embodiment and/or embodiment in the disclosure, this field is general
Logical technical staff every other embodiment obtained and/or every other implementation 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, such as the numerical value defined by
Within 10% or within 5% or within 1%.
"comprising" of the present invention, " comprising " or " containing ", it is intended that it especially, can also have other groups except described group
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.
The present invention provides a kind of compositions of thermosetting resin, and the compositions of thermosetting resin contains thermosetting resin and nothing
Machine filler, and cladding processing is carried out to the inorganic filler using molybdenum disulfide alkene；Based on the compositions of thermosetting resin
Gross mass meter, the content of the inorganic filler are 10wt%~80wt%.
Compositions of thermosetting resin provided by the invention coats treatment inorganic filling material by using molybdenum disulfide alkene, can have
The compatibility that effect improves inorganic filler and resin system is good, do not need to can be obtained using complicated dispersing apparatus be uniformly dispersed and
Stable resin combination, hot curing resin composition of the invention be especially suitable for thermal expansivity it is low and drilling plus
In electronic component of work and excellent heat resistance etc..
Cladding processing is carried out to inorganic filler using molybdenum disulfide alkene in the present invention, wherein molybdenum disulfide alkene is that have and stone
The molybdenum disulfide of the similar structure of black alkene structure, while also with the advantageous property of graphene, such as with good heat transfer
With light conductive performance, and also there is great specific surface area, for the cladding to inorganic particulate, can play improves inorganic grain
The effect in sublist face, and then improve its dispersion performance.Since the thermal conductivity of molybdenum disulfide alkene is high, coefficient of friction is small, can not only have
Effect improves the thermal conductivity of the laminate of preparation, and is obviously improved the drill processability of laminate, and can be obviously improved hole wall
Quality.Further, since the present invention is by that can be effectively improved inorganic filler and resin for molybdenum disulfide alkene coated inorganic filler surface
The compatibility of system is good, does not need to can be obtained using complicated dispersing apparatus and is uniformly dispersed and stable resin combination.
The content of inorganic filler as used in the present invention can be the compositions of thermosetting resin gross mass
10wt%~80wt%, it may be about 10wt% to about 80wt%, preferably from about 20wt% to about 60wt% in the present invention,
For example, about 23wt%, about 28wt%, about 32wt%, about 37wt%, about 42wt%, about 47wt%, about 52wt%, about 57wt%,
About 62wt%, about 67wt%, about 72wt%, about 76wt% or about 78wt% and any range between them, such as from about
23wt%, about 28wt%, about 32wt%, about 37wt% or about 42wt% are to about 47wt%, about 52wt%, about 57wt%, about
62wt%, about 67wt%, about 72wt%, about 76wt% or about 78wt%.Remaining is thermosetting resin and other necessary additions
Component.
By being arranged the content of inorganic filling material in the range, thermosetting resin can be kept to combine well
The formability and low thermal expansion of object, and realizing high fillingization inorganic filler and handled using molybdenum disulfide alkene cladding inorganic
In the case where filler, the deterioration of drill processability and interlayer adhesion can be inhibited, obtained laminate has low thermal expansion
Coefficient, excellent drill processability and heat resistance and high interlayer adhesion.
Preferred embodiment according to the present invention, the quality of the molybdenum disulfide alkene for carrying out cladding processing to inorganic filler are nothing
0.01~5wt% of machine packing quality, in the present invention preferably 0.5wt%~2wt%, it may be about in the present invention
0.5wt% to about 2wt%.By being arranged the content in the range, it can further improve drill processability and thermally conductive
Performance, and will not influence original overall performance of compositions of thermosetting resin.
In addition, the thickness of molybdenum disulfide alkene is not more than 20 nanometers, preferably no greater than 10 nanometers, is further preferably not more than
5 nanometers.Since molybdenum disulfide alkene of the invention is New Two Dimensional nano material, monolithic molybdenum disulfide lamellar spacing is only
0.65nm, the molybdenum disulfide alkene actually prepared are usually the superposition of single layer or several monolithic layers, and the thickness of molybdenum disulfide alkene is more than
20 nanometers, the effect of monolithic layer molybdenum disulfide cannot be played, in order to obtain identical drilling performance and heating conduction effect needs
The usage amount for increasing molybdenum disulfide alkene, to influence the insulation performance of material.Molybdenum disulfide alkene used in preferred is averaged
Width is 0.05~10 micron, preferably 0.1~5 micron, further preferably 0.5~2 micron.Because if molybdenum disulfide alkene
Mean breadth cannot form effective cladding less than 0.05 micron to inorganic filler；And if the mean breadth of molybdenum disulfide alkene
Greater than 10 microns, conductive path is easily formed, to influence the insulation performance of composite material, therefore moderate mean breadth is selected to have
Conducive to the raising of overall performance.
Molybdenum disulfide alkene used in the present invention can pass through conventional mechanical stripping method, liquid phase stripping method and chemical synthesis
The preparation of method method can prepare the molybdenum disulfide alkene with different-thickness and width by adjusting process conditions.Molybdenum disulfide
Alkene coated inorganic filler can be handled by modes such as dry and wet, and wherein dry process can stir machine, fluidized bed by height
Etc. processing equipments molybdenum disulfide alkene is coated on inorganic filler surface at a certain temperature；Wet-treating can then pass through ball milling
Molybdenum disulfide alkene is coated on inorganic filler surface under certain revolving speed by the equipment such as machine, sand mill.
Wherein the inorganic filler used in the present invention is selected from silica, boehmite, aluminium oxide, talcum, mica, height
Ridge soil, aluminium hydroxide, magnesium hydroxide, zinc borate, zinc stannate, zinc oxide, titanium oxide, boron nitride, calcium carbonate, barium sulfate, metatitanic acid
At least one in barium, aluminium borate, potassium titanate, E glass powder, S glass powder, D glass powder, NE glass powder, hollow powder or boehmite
Kind.
The average grain diameter of inorganic filler can be about 0.1 μm to about 100 μm, preferably from about 0.5 μm to about 20 μm.Passing through will
The average grain diameter setting of inorganic filler within the above range, can be kept when height is filled in compositions of thermosetting resin well
Mobility, and at the same time the mixed probability of oversize grain can be reduced and inhibition causes the undesirable generation of oversize grain.Here, flat
Equal partial size refers to the total volume of particles is taken as 100% and when finding out the cumulative degree distribution curve based on partial size, just quite
It, can be to use the size distribution of laser diffraction scattering method to measure in the partial size for the point that volume is 50%.
Wherein hollow powder may include: hollow silicon dioxide in a particular application, hollow boron nitride, hollow glass
Powder, hollow alumina etc..
Thermosetting resin as used in the present invention can account for the 20wt% of compositions of thermosetting resin gross mass~
70wt%, in the present invention its can also about 20wt% to about 70wt%, preferably from about 25wt% to about 65wt%, further preferably
About 30wt% to about 60wt%.The mass percent that the thermosetting resin accounts for compositions of thermosetting resin gross mass can be such as
It is about 23wt%, about 26wt%, about 31wt%, about 35wt%, about 39wt%, about 43wt%, about 47wt%, about 51wt%, about
55wt% about, about 59wt%, about 63wt% or about 67wt% and any range between them, for example, about 23wt%, about
26wt%, about 31wt%, about 35wt% or about 39wt% to about 43wt%, about 47wt%, about 51wt%, about 55wt% about, about
59wt%, about 63wt% or about 67wt%.
Thermosetting resin used in the present invention is for any a kind in the cross-linking polymer for forming reticular structure or at least
2 kinds of combination is preferably selected from epoxy resin, phenolic resin, cyanate ester resin, polyamide, polyimide resin, polyethers
At least one of resin, polyester resin, hydrocarbon resin or organic siliconresin；Further preferred epoxy resin or phenolic resin.
The combination of above-mentioned thermosetting resin is also possible to the combination of epoxy resin and polyamide, polyimide resin and
The combination of hydrocarbon resin, the combination of cyanate ester resin, polyamide and polyether resin, cyanate ester resin, polyamide, polyamides
Imide resin and the combination of epoxy resin etc..
Other compositions of thermosetting resin can also include curing agent, promotor and solvent.
When wherein for selection epoxy resin and its with the combination of other resins, the curing agent can be phenolic resin, acid
Acid anhydride compound, active ester compound, dicyandiamide, diaminodiphenylmethane, diaminodiphenylsulfone, diaminodiphenyl ether and
The mixture of one or more of maleimide；The curing accelerator is 2-methylimidazole, 2- ethyl -4- methyl
The mixture of one or more of imidazoles and 2- methyl 4-phenyl imidazoles；
For selection phenolic resin and its when with the combination of other resins, the curing agent can be organic acid anhydride, organic
Amine, lewis 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
One of sour hexichol oxide ester is a variety of.The promotor 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 promotor is selected from organic platinum-like compounds.
It as the solvent in the present invention, is not particularly limited, can be the alcohols such as methanol, ethyl alcohol, butanol, the molten fibre of ethyl
The ethers such as agent, butyl cellosolve, ethylene glycol-methyl ether, carbitol, butyl carbitol, acetone, butanone, methyl ethyl ketone, methyl
The ketones such as isobutyl ketone, cyclohexanone, toluene, dimethylbenzene, mesitylene etc. are aromatic hydrocarbon, ethoxyethyl acetate, vinegar
The esters such as acetoacetic ester, the nitrogen-containing solvents such as n,N-Dimethylformamide, n,N-dimethylacetamide, n-methyl-2-pyrrolidone.
Above-mentioned solvent can be used alone, and two or more can also be used in mixed way, preferably toluene, dimethylbenzene, equal three
The ketones flux such as the aromatic hydrocarbon solvents such as toluene and acetone, butanone, methyl ethyl ketone, hexone, cyclohexanone
It is used in mixed way.Usage amount those skilled in the art of the solvent can select according to the experience of oneself, the resin made
Glue reaches the viscosity for being suitable for using.
Compositions of thermosetting resin of the invention can further include silane coupling agent or/and wetting dispersing agent.As these
Silane coupling agent is not particularly limited as long as being that typically in silane coupling agent used in surface treatment.Make
It for concrete example, can enumerate, gamma-aminopropyl-triethoxy-silane, N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane etc.
The epoxy silanes systems such as aminopropyl silane system, γ-glycidyl ether oxygen propyl trimethoxy silicane, gamma-methyl allyl acyloxypropyl front three
The vinyl silanes such as oxysilane system, N- β-(N- vinyl benzene idol sulfonylaminoethyl)-γ-aminopropyltrimethoxysilane hydrochloric acid
The anion silicons such as salt methane series, phenyl silane system etc. can choose a kind therein or at least two kinds of appropriately combined uses.In addition,
As long as Ricinate Ricinate used in compositions of thermosetting resin, just there is no particular limitation.It can enumerate
It is moistened such as the Disperbyk-110 of BYKChemie Japan, 111,180,161, BYK-W996, W9010, W903 out
Dispersing agent.
In addition, compositions of thermosetting resin of the invention can also contain various additives, as concrete example, Ke Yiju
Fire retardant, antioxidant, heat stabilizer, antistatic agent, ultraviolet absorbing agent, pigment, colorant or lubricant etc. out.These are various
Additive can be used alone, and two or more can also be used in mixed way.
As another real-time proposals of the invention, the present invention also provides a kind of prepregs, pass through with above-mentioned thermosetting
Property resin combination is impregnated into reinforcing material and drying and is made.
Prepreg provided by the invention, the compositions of thermosetting resin used are handled by using molybdenum disulfide alkene cladding
Inorganic filler both can effectively solve the dispersion and settlement issues of molybdenum compound, can be evenly distributed in prepreg, warp
The inorganic filler of molybdenum disulfide alkene cladding has more excellent thermal conductivity, and when drilling can preferably conduct heat, can be to avoid
Resin is sticked in drill after melting, while can also reduce situations such as hole is cracked, and can be obviously improved the hole wall after drilling
Quality.
Specifically the reinforcing material in the present invention may include glass fabric, also referred to as glass-fiber-fabric.In following description
In, glass-fiber-fabric reinforcing material and glass fabric use in which can be interchanged.
When wherein specifically with above-mentioned compositions of thermosetting resin preparing prepreg, pass through mechanical stirring, emulsification or ball
Mill dispersion, is configured to glue for compositions of thermosetting resin, then infiltrates glass-fiber-fabric using the glue, and drying obtains prepreg.
As another real-time proposals of the invention, the present invention also provides a kind of laminate, laminate contains at least one
Above-mentioned prepreg.
According to the present invention, using laminate made of above-mentioned prepreg, in processing, its drill processability is very excellent,
Also there is good electrical insulating property and low heat expansion.
A kind of laminate provided by the present invention is by above-mentioned prepreg and metal foil such as copper foil hot pressing in the vacuum press
Prepare the laminate.
Specifically, it is at least included the following steps by the method for using above-mentioned prepreg to prepare laminate:
(1) glue: will solvent be added proportion container in, be separately added under stirring thermosetting resin, curing agent solution and
The solution of promotor；After stirring, inorganic filler is added, continues to stir, obtains glue, inorganic filler therein first passes through this hair in advance
Bright molybdenum disulfide alkene cladding processing.Glue therein is compositions of thermosetting resin provided by the present invention.
(2) it impregnates: reinforcing material is immersed in glue.
(3) be impregnated with: by the reinforcing material of dipped glue by vertical or horizontal type contain dipping machine, by control extruding wheel speed,
Prepreg is made after dry in the conditions such as linear speed, wind-warm syndrome and furnace temperature.
Specifically with vertical demonstration example containing dipping machine are as follows: 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, being put into vacuum hotpressing machine, by one
Simultaneously metal-coated laminated board such as copper clad laminate, specific demonstration example is finally made in fixed temperature, time and pressure are as follows:
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, can be prepared by laminate after hot pressing, i.e.,
It is copper clad laminate if covering copper.
As another real-time proposals of the invention, the present invention also provides a kind of printed circuit board, printed circuit board contains
An at least above-mentioned prepreg.
According to the present invention, using printed circuit board made of above-mentioned prepreg, in processing, its drill processability is very
It is excellent, it may have good electrical insulating property and low heat expansion.
Illustrate above-mentioned technical proposal of the invention below by way of specific embodiment.
Embodiment 1~15:
It is raw materials used almost the same in embodiment 1~15, the difference is that the proportion of each embodiment, is implementing
In example 1~15, using use brominated bisphenol a type epoxy resin as thermosetting resin, use dicyandiamide as of the invention
For curing agent, use 2-methylimidazole as promotor of the invention, for inorganic filler uses fused silica,
In other applications, by above-mentioned thermosetting resin, inorganic filler, curing agent, promotor using the present invention cited by its
He replaces material, and acquired technical effect and the embodiment of the present invention 1~15 are essentially identical, is only used for illustrating herein, and has
Body proportion is referring to table 1:
By brominated bisphenol a type epoxy resin (DOW Chemical, epoxide equivalent 435, bromine content 19%, ProductName DER530)
The fused silica that (epoxy resin), dicyandiamide (curing agent), 2-methylimidazole (promotor), molybdenum disulfide alkene cladding are handled
(Singapore's silicon than section, 525,2 μm of average grain diameter) is added in butanone (solvent), mechanical stirring and the glue for being configured to 65wt%
Liquid, then impregnated glass fiber cloth (7628, Zhuhai Zhu Bo Electron Material Co., Ltd) (reinforcing material), after heating and drying
Prepreg is formed, copper foil is placed on two sides, and copper clad laminate is made in pressurized, heated.
Above-mentioned prepreg is respectively prepared printed circuit board, printed circuit board therein contain at least one it is above-mentioned pre-
Leaching material.
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 promotor are separately added under stirring；It stirs
After mixing 2 hours, the inorganic filler through the cladding processing of molybdenum disulfide alkene is added, continues stirring 6 hours, obtains glue.Glue therein
Liquid is compositions of thermosetting resin provided by the present invention.
(2) it impregnates: reinforcing material is immersed in glue.
(3) it is impregnated with: the reinforcing material of dipped glue being contained into dipping machine by vertical, wheel speed, linear speed, wind-warm syndrome are squeezed by control
And the conditions such as furnace temperature, prepreg is made.The vertical condition containing dipping machine are as follows: squeeze wheel speed: -1.8 ± 0.1M/min；Main line speed:
10m/min；Wind-warm syndrome: 150 DEG C；Furnace temperature: 180 DEG C.
(3) it suppresses: after the prepreg cut and copper foil are combined, being put into vacuum hotpressing machine, by certain temperature,
Simultaneously copper clad laminates, actual conditions are finally made in time and pressure are as follows:
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, it is laminated on using 8 prepregs with a thickness 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 laminates, with side described below
Method the results are shown in Table 1 to drill processability, hole wall lineae ablicantes, thermal conductivity, volume resistance and filler dispersion uniformity evaluation.
Embodiment 16
By 100g brominated bisphenol a type epoxy resin (DOW Chemical, epoxide equivalent 435, bromine content 19%, ProductName
DER530) (epoxy resin), 3g dicyandiamide (curing agent), 0.05g 2-methylimidazole (promotor), 100g are through molybdenum disulfide alkene
The boehmite (one Shi Tong material Science and Technology Co., Ltd. of Anhui, BG601,0.5 μm of average grain diameter) of cladding processing is added to fourth
In ketone (solvent), mechanical stirring and the glue for being configured to 65wt%, then impregnated glass fiber cloth (7628, Zhuhai pearl glass electronics
Materials Co., Ltd) (reinforcing material), prepreg is formed after heating and drying, and copper foil is placed on two sides, and pressurized, heated, which is made, to be covered
The laminate of copper.
Printed circuit board is made in above-mentioned prepreg, printed circuit board therein contains an at least above-mentioned preimpregnation
Material.
Embodiment 17
By 100g brominated bisphenol a type epoxy resin (DOW Chemical, epoxide equivalent 435, bromine content 19%, ProductName
DER530), 24g linear phenol-aldehyde resin (Japanese group is flourish, hydroxyl equivalent 105, ProductName TD2090), 0.05g 2-methylimidazole,
E- glass micro mist (Jiangsu Lian Rui new material limited liability company, DS1032, average grain of the 100g through the cladding processing of molybdenum disulfide alkene
3 μm of diameter) it is added in butanone (solvent), then mechanical stirring and the glue for being configured to 65wt% are impregnated with glass fabric
(7628, Zhuhai Zhu Bo Electron Material Co., Ltd) (reinforcing material), forms prepreg after heating and drying, and copper is placed on two sides
Copper clad laminate is made in foil, pressurized, heated.
Printed circuit board is made in above-mentioned prepreg, printed circuit board therein contains an at least above-mentioned preimpregnation
Material.
Embodiment 18
By 20g phenol novolak type cyanate PT30,40g ortho-methyl phenol phenol aldehyde type epoxy resin N695,20g bromination benzene second
The calcium carbonate of alkene and suitable octoate catalyst zinc, 0.05g 2- phenylimidazole, 100g through the cladding processing of molybdenum disulfide alkene
(specialty minerals, THIXO-500,0.15 μm of average grain diameter) is added in butanone (solvent), mechanical stirring and match
The glue of 65wt% is made, then impregnated glass fiber cloth (7628, Zhuhai Zhu Bo Electron Material Co., Ltd) (reinforcing material),
Prepreg is formed after heating and drying, and copper foil is placed on two sides, and copper clad laminate is made in pressurized, heated.
Printed circuit board is made in above-mentioned prepreg, printed circuit board therein contains an at least above-mentioned preimpregnation
Material.
Embodiment 19
By 30g dicyclopentadiene epoxy HP-7200H, 60g benzoxazine resin D125,5g linear phenolic resin EPONOL
(Jin Yingtai Chemical Co., Ltd., ATH are put down the aluminium hydroxide of 6635M65,5g dicyandiamide, 100g through the cladding processing of molybdenum disulfide alkene
Equal 10 μm of partial size) it is added in butanone (solvent), mechanical stirring and the glue for being configured to 65wt%, then impregnated glass fiber cloth
(7628, Zhuhai Zhu Bo Electron Material Co., Ltd) (reinforcing material), forms prepreg after heating and drying, and copper is placed on two sides
Copper clad laminate is made in foil, pressurized, heated.
Printed circuit board is made in above-mentioned prepreg, printed circuit board therein contains an at least above-mentioned preimpregnation
Material.
Embodiment 16-19 obtains combining using thermosetting resin provided by the invention with method similarly to Example 1
The copper clad laminate of object.It measures, evaluation result is shown in table 2.
Comparative example 1
It is substantially consistent with embodiment in the present embodiment, the difference is that inorganic filler is handled without molybdenum disulfide alkene
Outside, and with method similarly to Example 1, the copper clad laminate using resin combination is obtained.Measurement, evaluation result is shown in table
3。
Measurement:
1, the evaluation of drill processability
By the copper-clad plate of production, two piece one is folded, use the new knife of 0.3mm drilling machine (HITACHI NDR-1V212E) with
The revolving speed of 155krmp carries out drilling processing, 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), measurement cutting edge tip abrasion back amount is to survey
It is drill size that vertical line, which is measured, at a distance from central axes intersection point and abrasion top edge, is calculated by the following formula the wear rate of drill
To evaluate drilling effect.
Wear rate %=drilling back edge and central axes distance/drilling leading edge and central axes distance × 100%.
2, hole wall lineae ablicantes is tested
The plate de-smear for being 5000 by hole number, then copper facing, production slice using micro- sem observation and measure hole wall
The length of lineae ablicantes, length is longer to illustrate that hole wall quality is poorer.
3, laminate thermal conductivity is tested
According to ASTMD5470 standard testing laminate thermal conductivity, thermal conductivity is higher, and thermal conductivity is better.
4, the volume resistivity test of laminate
According to the volume resistance of IPC-TM-650 standard testing laminate, volume resistivity is higher, illustrates the insulation of plate
Property is better.
5, dispersion uniformity evaluation of the filler in resin
Copper-clad laminate is cut into the size of 5mm square, carries out casting polishing, is placed on conductive adhesive, metal spraying, is made
Observation test piece.It is observed with scanning electron microscope, observes dispersion of the filler in resin, and evaluate it.
Table 1
Table 2
Table 3
| Comparative example | 1 |
| DER530/g | 100 |
| Dicyandiamide/g | 3 |
| 2-methylimidazole/g | 0.05 |
| Fused silica/g | 100 |
| Drill abrasion/% | 100 |
| Hole wall lineae ablicantes/μm | 130 |
| Thermal conductivity/Wm-1k-1 | 0.30 |
| Volume resistivity/M Ω cm | 107 |
| Dispersing uniformity | × |
By in dispersion uniformity evaluation, indicating excellent in table 1~3, △ indicates good, × indicate poor.
From table 1~3 as can be seen that for embodiment 1-15 and embodiment 16~19 and comparative example 1, add through curing
The drill processability and thermal conductivity of the inorganic filler of molybdenum alkene cladding processing are generally obviously than using without the processing of molybdenum disulfide alkene
Inorganic filler is good, and hole wall quality is also obviously improved.For embodiment 1-4 and embodiment 5, it is in the amount of addition molybdenum disulfide alkene
In the case where the 0.01-5wt% of the inorganic filler quality, it can further improve drilling property and hole wall quality, improve simultaneously
Inorganic filler dispersing uniformity, when dosage is more than 5wt%, insulating properties and filler dispersing uniformity are decreased obviously.From reality
From the point of view of applying a 6-8, the average thickness of molybdenum disulfide alkene is bigger within the scope of one, and drilling property is better, and thermal conductivity is better, hair
The processability waved is also better, and its be greater than or equal to 2nm when, boring capacity is better, and thermal conductivity is better；Similarly, when flat
When equal thickness is less than or equal to 20nm, inorganic filler dispersing uniformity and insulating properties are better, and the performance that drills also is obtained
Reinforce, for embodiment 9, when average thickness is greater than 20nm, inorganic filler dispersing uniformity and insulating properties are relatively poor.
In addition, the mean breadth of molybdenum disulfide alkene is wider, and drill processability is better for embodiment 10-19, especially average width
Degree its insulating properties and thermal conductivity at 0.05-10 μm is best, and its drill processability is also best.
The technical solution of above-described embodiment 1~19 in a preferred embodiment of the present invention will be cited by the present invention
Raw material in other raw material alternative embodiments 1~19, or be used in any combination, it can also obtain such as embodiment 1~19
In indices shown in technical effect, or reach comparable technical effect, no longer repeat herein.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent substitution, improvement and etc. done should be included in the scope of protection of the invention.
Claims (10)
1. a kind of compositions of thermosetting resin, which is characterized in that the compositions of thermosetting resin contains thermosetting resin and nothing
Machine filler, and cladding processing is carried out to the inorganic filler using molybdenum disulfide alkene；Based on the compositions of thermosetting resin
Gross mass meter, the content of the inorganic filler are 10wt%~80wt%.
2. compositions of thermosetting resin according to claim 1, which is characterized in that the quality of the molybdenum disulfide alkene is nothing
0.01~5wt% of machine packing quality.
3. compositions of thermosetting resin according to claim 1, which is characterized in that the molybdenum disulfide alkene thickness is not more than
20 nanometers, mean breadth is 0.05~10 micron.
4. compositions of thermosetting resin according to claim 3, which is characterized in that the molybdenum disulfide alkene thickness is not more than
10 nanometers, mean breadth is 0.5~5 micron.
5. compositions of thermosetting resin according to claim 1, which is characterized in that the inorganic filler is selected from titanium dioxide
Silicon, boehmite, aluminium oxide, talcum, mica, kaolin, aluminium hydroxide, magnesium hydroxide, zinc borate, zinc stannate, zinc oxide, oxidation
Titanium, boron nitride, calcium carbonate, barium sulfate, barium titanate, aluminium borate, potassium titanate, E glass powder, S glass powder, D glass powder, NE glass
At least one of powder, hollow powder or boehmite.
6. compositions of thermosetting resin according to claim 1, which is characterized in that the thermosetting resin is selected from epoxy
Resin, phenolic resin, cyanate ester resin, polyamide, polyimide resin, polyether resin, polyester resin, hydrocarbon resin have
At least one of machine silicone resin.
7. a kind of prepreg, which is characterized in that it with the thermosetting resin of any one of claims 1 to 6 by being combined
Object is impregnated into reinforcing material and drying and is made.
8. prepreg according to claim 8, which is characterized in that the reinforcing material is glass fabric.
9. a kind of laminate, which is characterized in that the laminate contains an at least preimpregnation as described in claim 7 or 8
Material.
10. a kind of printed circuit board, which is characterized in that the printed circuit board contains at least one such as claim 7 or 8 institutes
The prepreg stated.
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