CN109266262A - A method of preparing low-dielectric loss composite caking agent - Google Patents
A method of preparing low-dielectric loss composite caking agent Download PDFInfo
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- CN109266262A CN109266262A CN201810840158.8A CN201810840158A CN109266262A CN 109266262 A CN109266262 A CN 109266262A CN 201810840158 A CN201810840158 A CN 201810840158A CN 109266262 A CN109266262 A CN 109266262A
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- polybutadiene
- silica
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- styrene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J147/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds; Adhesives based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C08L2312/00—Crosslinking
Abstract
The present invention relates to a kind of low-dielectric loss composite caking agents and preparation method thereof, the composite caking agent is with the 1 of different contents of ethylene, 2- polybutadiene is matrix, and the composition such as silica, tackifier, curing agent for adding two kinds of different-grain diameters, the content of two kinds of different-grain diameter silica are the 50~100% of 1,2- polybutadiene weight, the content of tackifier is 1, the 9~53.8% of 2- polybutadiene weight, the content of curing agent are the 2.7~7.6% of 1,2- polybutadiene weight.Low-dielectric loss composite caking agent of the invention has low-dielectric loss, low-expansion coefficient, high-adhesive-strength and good processing fluidity, it can apply to spray mo(u)lding processing, product is able to satisfy requirement of the high-frequency circuit field to multiple functions such as high molecular material low-expansion coefficient, low-dielectric loss, high-adhesive-strength and high flowings, application prospect is good, its simple production process, convenient operation and control, quality are stablized, high production efficiency has wide industrialization and market prospects.
Description
Technical field
The present invention relates to a kind of methods for preparing low-dielectric loss composite caking agent, belong to functional composite material technology neck
Domain.
Background technique
With the rapid development of high frequency communications information technology, the high-frequency microwave communication technology is to integrated, multifunction, high frequency
Low-loss microwave system development is trend of the times.The integrated circuit of high integration, more low-power consumption and higher performance is to high frequency
Medium substrate material proposes more harsh requirement.In order to reduce integrated circuit bring capacitance-resistance (RC) time delay
With string acoustic jamming, while meeting the characteristic impedance requirement of different transmission conditions, to reach high-fidelity constant low-loss high frequency information biography
Defeated, the exploitation of low-dielectric loss dielectric material and its dielectric properties regulate and control the concern by more and more researchers.But it should
Material needs to ask dielectric loss lower, while having both and have good cementability to copper foil and substrate.To reduce polymer material
Dielectric loss, on the one hand by Molecular Design make Polymeric dielectric loss reduce, but this method usually require it is special
Equipment, complex process, process regulation are stringent, therefore realize Polymeric dielectric loss reduction by Molecular Design, glue
The method industrialization for connecing intensity raising is more difficult.On the other hand, polymer material and low-dielectric loss filler are generally selected
It is compound, so that composite material has the good easy processing of polymer, cementability, dielectric constant and dielectric loss easy-regulating simultaneously
Advantage.It improves composite material cementability and usually requires matrix with polar group, reduction dielectric loss, which usually requires matrix, to be had
Nonpolarity, as far as possible reduction dielectric loss, while composite material being kept to have excellent cementability, good mobility, processability
The regulation of energy, solidification temperature and substrate matching, has become the one of the development that restrict low-dielectric loss composite bonding material
Hang-up.
Summary of the invention
For above-mentioned dielectric composite bonding material disadvantage of the existing technology, the purpose of the present invention is intended to provide a kind of system
The method of standby low-dielectric loss adhesives, low-dielectric loss composite material can both have when higher filler is filled
Low-dielectric loss, strong cementability, and keep good mobility, toughness and processing performance.
Technical principle of the invention is that the cementability intensity of composite material and tough is adjusted by resin ethylene base content
Property, the processability and film forming of low-dielectric loss composite material are adjusted by styrene-butadiene-styrene triblock copolymer
Property and viscous chirality, the dielectric constant and thermal expansion coefficient of composite material are adjusted by the compounding of different-grain diameter silica,
Based on the adjusting and balance of above-mentioned three aspect, the functional composite material of low-dielectric loss, high-adhesive-strength can be developed.
The present invention is based on above-mentioned technical principle, realize that technical solution used by its goal of the invention is:
The method that the present invention prepares low-loss functional composite material, using the resin of high-vinyl-content as matrix, feature exists for it
Be in this method the following steps are included:
The first step is stocked up by following components and weight:
(1) 1,2-polybutadiene A:50 (contents of ethylene >=90)
(2) 1,2-polybutadiene B:5 ~ 15 (80 >=contents of ethylene >=40)
(3) styrene-butadiene-styrene triblock copolymer: 5 ~ 35
(4) 1~5 micron of silica A:25~70(partial size)
(5) silica B:10~50 (100~600 nanometers of partial size)
(6) cumyl hydroperoxide: 1.5~5
(7) vinyl silicane coupling agent: 0.6~1.5
Silica A, silica B is dried in second step, is cooled to room temperature and then even with vinyl silanes
Connection agent is handled and is dried；
Third step, above-mentioned 1,2-polybutadiene A, 1,2-polybutadiene B, s-B-S three block is total
For polymers solvent in good solvent, stirring and dissolving obtains 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-
The homogeneous solution of styrene triblock copolymer；
4th step, the silica A that cumyl hydroperoxide and second step medium vinyl silane coupling agent are handled and dried, two
Silica B is added to 1,2-polybutadiene A in third step, 1,2-polybutadiene B, s-B-S three
In the homogeneous solution of block copolymer, stirring is mixed to get low-dielectric loss composite caking agent is arrived.
In the above-mentioned first step, 1,2-polybutadiene A, 1,2-polybutadiene B, s-B-S three
Block copolymer, silica A, silica B, cumyl hydroperoxide, vinyl silicane coupling agent weight part ratio can be excellent
First it is selected as 50:10:15:70:10:2:0.8.
Two kinds of polybutadiene, i.e., 1,2-polybutadiene A(contents of ethylene >=90% are added in the above-mentioned first step) and 1,
2-polybutadiene B(80% >=contents of ethylene >=40%) main purpose be that composite wood is adjusted by the content of vinyl
The sizing material degree of material, makes adhesive strength and toughness have certain balance.
The purpose of addition styrene-butadiene-styrene triblock copolymer is mainly adjusted compound in the above-mentioned first step
The viscous chirality of material is to have certain shape after composite caking agent solvent volatilizees, and be able to maintain certain mobility, main
Principle is using the characteristic of the physical crosslinking point of styrene-butadiene-styrene triblock copolymer, is that high temperature can flow
It is dynamic, cross-linked state is presented under low temperature, while there is crosslinkable double bond to crosslink with polybutadiene again and react, so benzene second
Alkene-butadiene-styrene triblock copolymer has multifunctionality in the present invention.
It is worth noting that above-mentioned low-dielectric loss composite caking agent can be carried out the spray mo(u)lding on substrate, to molten
After agent volatilization the binding function of low-dielectric loss composite caking agent can be given full play to copper foil hot pressing.Since this is compound
Bonding agent has good fluidity, can fill up the groove of the different row circuit of copper foil, keep entire circuit substrate more closely knit, copper foil and base
Bubble is not present between plate, will affect the signal transmission performance of entire high-frequency circuit if there is bubble.
The invention has the following advantages over the prior art:
The content that the present invention passes through vinyl first adjusts the density of crosslinking points, realizes the balance of toughness and rigidity, passes through fourth two
The addition of alkene can give full play to the binding function of low-dielectric loss composite caking agent, secondly by s-B-S
The addition of triblock copolymer adjusts the viscous chirality of composite material, is to have certain shape after composite caking agent solvent volatilizees,
And it is able to maintain certain mobility, cardinal principle is handed over using the physics of styrene-butadiene-styrene triblock copolymer
The characteristic for joining point, is that high temperature can flow, cross-linked state is presented under low temperature, while having crosslinkable double bond and polybutadiene again
Alkene crosslinks reaction.For current dielectric composite caking agent, adhesive strength is low, and dielectric loss is big, and thermal expansion coefficient is high, this hair
The bright method using the design of polymer interface structure and the design of composite material aggregated structure, the low-dielectric loss being prepared are multiple
The adhesive strength for closing bonding agent and copper foil reaches 0.89 N/m(Newton/meter), dielectric loss is down to 0.0015, linear thermal expansion system
Number reaches 2.90 × 10-5 ℃-1, while requirement of the spray mo(u)lding to Polymer Processing rheological property can be met.
Low-dielectric loss composite caking agent provided by the invention both had while realizing reduction composite material dielectric loss
There are preferable adhesive property and low thermal coefficient of expansion, and has after keeping the high fluidity of good polymer composites, solidification
There is good toughness, improve the surcharge of polymeric articles, has widened the application range of polymeric articles, it is multiple in polymer
Condensation material theoretical research and application and development etc. are of great significance.Meanwhile simple production process, convenient operation and control, matter
Amount stabilization, high production efficiency, production cost is low, has a wide range of application, and has wide industrialization and market prospects.
Specific implementation method:
The present invention is further described specifically by the following examples.In following embodiment, the dosage of each component
It is quality dosage.It is necessary to it is pointed out here that, following example only to further explanation of the invention, should not be understood as to this
The limitation of invention protection scope, person skilled in art can carry out some non-to the present invention according to aforementioned present invention content
The modifications and adaptations of matter.
Embodiment 1
The present embodiment prepares low-dielectric loss composite caking agent, and with 1,2- polybutadiene for main base, silica is to fill out
Material, comprising the following steps:
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:5
(3) styrene-butadiene-styrene triblock copolymer: 20
(4) silica A:60
(5) silica B:30
(6) cumyl hydroperoxide: 1.5
(7) vinyl silicane coupling agent: 1.5
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 60 grams, silica B
30 grams of (particle size range is in normal distribution, and particle size range is 100~600 nanometers), is dried at 120 DEG C respectively, cold
But it is put into high mixer together to room temperature (herein referring to 25 DEG C) and then by the silica A of drying process and silica B,
It is mixed 5 minutes with 600 rpms of speed, then puts into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Mixing 5 minutes, whole process temperature of charge are controlled at 80 DEG C, are cooled to room temperature spare；
Third step takes 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene
45%) 5 grams, 20 grams of solvents of styrene-butadiene-styrene triblock copolymer in 336 grams of dimethylbenzene, be stirred at room temperature molten
Solution obtain 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer it is uniform
Solution for standby；
4th step, the silica C that 1.5 grams of cumyl hydroperoxides and second step medium vinyl silane coupling agent are handled, two
Silica D is added to 1,2-polybutadiene A in third step, 1,2-polybutadiene B, s-B-S three
In the solution of block copolymer, stirring is mixed to get low-dielectric loss composite caking agent is arrived；
5th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.78 Newton/meter
(N/m), dielectric loss 0.0018, linear expansion coefficient are 3.21 × 10-5 ℃-1, obtained composite caking agent has good
Mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complicated shapes) stay
Under groove.
Comparative example 1-1
Each component content in comparative example is consistent with the content in embodiment 1, difference with only use dioxy in comparative example
SiClx A.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:5
(3) styrene-butadiene-styrene triblock copolymer: 20
(4) silica A:90
(5) cumyl hydroperoxide: 1.5
(6) vinyl silicane coupling agent: 1.5
It is comprised the concrete steps that:
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 90 grams, at 120 DEG C
It is dried, is cooled to room temperature and (herein refers to 25 DEG C) and then puts into the silica A of drying process in high mixer,
It is mixed 5 minutes with 600 rpms of speed, then puts into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Mixing 5 minutes, whole process temperature of charge are controlled at 80 DEG C, are cooled to room temperature spare；
Third step takes 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene
45%) 5 grams, 20 grams of solvents of styrene-butadiene-styrene triblock copolymer in 336 grams of dimethylbenzene, be stirred at room temperature molten
Solution obtain 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer it is uniform
Solution for standby；
4th step, the silica A that 1.5 grams of cumyl hydroperoxides and second step medium vinyl silane coupling agent are handled, adds
Enter into third step 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer
Solution in, stirring, mix to get arrive low-dielectric loss composite caking agent；
5th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.73 N/m(ox
/ rice), dielectric loss 0.0022, thermal linear expansion coefficient reaches 3.44 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Comparative example 1-2
Each component content in comparative example is consistent with the content in embodiment 1, difference with only use dioxy in comparative example
SiClx B.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:5
(3) styrene-butadiene-styrene triblock copolymer: 20
(4) silica B:90
(5) cumyl hydroperoxide: 1.5
(6) vinyl silicane coupling agent: 1.5
It is comprised the concrete steps that:
Second step takes silica B(particle size range in normal distribution, and particle size range is 100~600 nanometers) 90 grams, 120
It DEG C is dried, is cooled to room temperature and (herein refers to 25 DEG C) and then the silica B of drying process is put into high mixer
In, it is mixed 5 minutes with 600 rpms of speed, then put into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Degree mixing 5 minutes, whole process temperature of charge is controlled at 80 DEG C, is cooled to room temperature spare；
Third step takes 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene
45%) 5 grams, 20 grams of solvents of styrene-butadiene-styrene triblock copolymer in 336 grams of dimethylbenzene, be stirred at room temperature molten
Solution obtain 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer it is uniform
Solution for standby；
4th step, the silica B that 1.5 grams of cumyl hydroperoxides and second step medium vinyl silane coupling agent are handled, adds
Enter into third step 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer
Solution in, stirring, mix to get arrive low-dielectric loss composite caking agent；
5th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.68 N/m(ox
/ rice), dielectric loss 0.0024, thermal linear expansion coefficient reaches 3.31 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Comparative example 1-3
Each component content in comparative example is consistent with the content in embodiment 1, the difference is that, all add together in comparative example
Enter, rather than the implementation steps in the present invention.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:5
(3) styrene-butadiene-styrene triblock copolymer: 20
(4) silica A:60
(5) silica B:30
(6) cumyl hydroperoxide: 1.5
(7) vinyl silicane coupling agent: 1.5
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 60 grams, silica B
30 grams of (particle size range is in normal distribution, and particle size range is 100~600 nanometers), is dried at 120 DEG C respectively, cold
But it is put into high mixer together to room temperature (herein referring to 25 DEG C) and then by the silica A of drying process and silica B,
It is mixed 5 minutes with 600 rpms of speed, then puts into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Mixing 5 minutes, whole process temperature of charge are controlled at 80 DEG C, are cooled to room temperature spare；
Third step, by 1.5 grams of cumyl hydroperoxides, silica C, the dioxy of the processing of second step medium vinyl silane coupling agent
SiClx D, 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene 45%) 5 grams,
20 grams of solvents of styrene-butadiene-styrene triblock copolymer are stirred at room temperature dissolution, mix in 336 grams of dimethylbenzene
Obtain low-dielectric loss composite caking agent；
4th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.64 N/m(ox
/ rice), dielectric loss 0.0023, thermal linear expansion coefficient reaches 3.67 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Embodiment 2
The present embodiment prepares low-dielectric loss composite caking agent, and with 1,2-polybutadiene for main base, silica is to fill out
Material, comprising the following steps:
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:10
(3) styrene-butadiene-styrene triblock copolymer: 15
(4) silica A:70
(5) silica B:10
(6) cumyl hydroperoxide: 2
(7) vinyl silicane coupling agent: 0.8
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 70 grams, silica B
10 grams of (particle size range is in normal distribution, and particle size range is 100~600 nanometers), is dried at 120 DEG C respectively, cold
But it is put into high mixer together to room temperature (herein referring to 25 DEG C) and then by the silica A of drying process and silica B,
It is mixed 5 minutes with 600 rpms of speed, then puts into 0.8 gram of vinyl silicane coupling agent, 800 rpms of speed
Mixing 5 minutes, whole process temperature of charge are controlled at 80 DEG C, are cooled to room temperature spare；
Third step takes 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene
45%) 10 grams, 15 grams of solvents of styrene-butadiene-styrene triblock copolymer in 336 grams of dimethylbenzene, be stirred at room temperature molten
Solution obtain 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer it is uniform
Solution for standby；
4th step, silica C, the dioxy that 2 grams of cumyl hydroperoxides and second step medium vinyl silane coupling agent are handled
It is embedding to be added to 1,2-polybutadiene A in third step, 1,2-polybutadiene B, s-B-S three by SiClx D
In the solution of section copolymer, stirring is mixed to get low-dielectric loss composite caking agent is arrived；
5th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.89 N/m(ox
/ rice), dielectric loss 0.0015, thermal linear expansion coefficient reaches 2.90 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Comparative example 2-1
Each component content in comparative example is consistent with the content in embodiment 2, difference with only use dioxy in comparative example
SiClx A.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:10
(3) styrene-butadiene-styrene triblock copolymer: 15
(4) silica A:80
(5) cumyl hydroperoxide: 2
(6) vinyl silicane coupling agent: 0.8
It is comprised the concrete steps that:
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 80 grams, respectively 120
It DEG C is dried, is cooled to room temperature and (herein refers to 25 DEG C) and then the silica A of drying process is put into high mixer
In, it is mixed 5 minutes with 600 rpms of speed, then put into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Degree mixing 5 minutes, whole process temperature of charge is controlled at 80 DEG C, is cooled to room temperature spare；
Third step takes 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene
45%) 5 grams, 20 grams of solvents of styrene-butadiene-styrene triblock copolymer in 336 grams of dimethylbenzene, be stirred at room temperature molten
Solution obtain 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer it is uniform
Solution for standby；
4th step, the silica A that 1.5 grams of cumyl hydroperoxides and second step medium vinyl silane coupling agent are handled, adds
Enter into third step 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer
Solution in, stirring, mix to get arrive low-dielectric loss composite caking agent；
5th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.83 N/m(ox
/ rice), dielectric loss 0.0027, thermal linear expansion coefficient reaches 2.93 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Comparative example 2-2
Each component content in comparative example is consistent with the content in embodiment 2, difference with only use dioxy in comparative example
SiClx B.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:10
(3) styrene-butadiene-styrene triblock copolymer: 15
(4) silica B:80
(5) cumyl hydroperoxide: 2
(6) vinyl silicane coupling agent: 0.8
It is comprised the concrete steps that:
Second step takes silica B(particle size range in normal distribution, and particle size range is 1~5 micron) 80 grams, respectively 120
It DEG C is dried, is cooled to room temperature and (herein refers to 25 DEG C) and then the silica B of drying process is put into high mixer
In, it is mixed 5 minutes with 600 rpms of speed, then put into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Degree mixing 5 minutes, whole process temperature of charge is controlled at 80 DEG C, is cooled to room temperature spare；
Third step takes 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene
45%) 5 grams, 20 grams of solvents of styrene-butadiene-styrene triblock copolymer in 336 grams of dimethylbenzene, be stirred at room temperature molten
Solution obtain 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer it is uniform
Solution for standby；
4th step, the silica B that 1.5 grams of cumyl hydroperoxides and second step medium vinyl silane coupling agent are handled, adds
Enter into third step 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer
Solution in, stirring, mix to get arrive low-dielectric loss composite caking agent；
5th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.74 N/m(ox
/ rice), dielectric loss 0.0023, thermal linear expansion coefficient reaches 3.12 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Comparative example 2-3
Each component content in comparative example is consistent with the content in embodiment 2, the difference is that, all add together in comparative example
Enter, rather than the implementation steps in the present invention.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:10
(3) styrene-butadiene-styrene triblock copolymer: 15
(4) silica A:70
(5) silica B:10
(6) cumyl hydroperoxide: 2
(7) vinyl silicane coupling agent: 0.8
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 70 grams, silica B
10 grams of (particle size range is in normal distribution, and particle size range is 100~600 nanometers), is dried at 120 DEG C respectively, cold
But it is put into high mixer together to room temperature (herein referring to 25 DEG C) and then by the silica A of drying process and silica B,
It is mixed 5 minutes with 600 rpms of speed, then puts into 0.8 gram of vinyl silicane coupling agent, 800 rpms of speed
Mixing 5 minutes, whole process temperature of charge are controlled at 80 DEG C, are cooled to room temperature spare；
Third step, by 2 grams of cumyl hydroperoxides, the silica A of second step medium vinyl silane coupling agent processing, titanium dioxide
Silicon B, 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene 45%) 10 grams, benzene
15 grams of solvents of ethylene-butadiene-styrene triblock copolymer are stirred at room temperature dissolution, mix i.e. in 336 grams of dimethylbenzene
Obtain low-dielectric loss composite caking agent；
4th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.0.74 N/m
(Newton/meter), dielectric loss 0.0023, thermal linear expansion coefficient reaches 3.12 × 10-5 ℃-1, obtained composite caking agent tool
Have good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Comparative example 2-3
Each component content in comparative example is consistent with the content in embodiment 2, the difference is that, all add together in comparative example
Enter, rather than the implementation steps in the present invention.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:10
(3) styrene-butadiene-styrene triblock copolymer: 15
(4) silica A:70
(5) silica B:10
(6) cumyl hydroperoxide: 2
(7) vinyl silicane coupling agent: 0.8
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 70 grams, silica B
10 grams of (particle size range is in normal distribution, and particle size range is 100~600 nanometers), is dried at 120 DEG C respectively, cold
But it is put into high mixer together to room temperature (herein referring to 25 DEG C) and then by the silica A of drying process and silica B,
It is mixed 5 minutes with 600 rpms of speed, then puts into 0.8 gram of vinyl silicane coupling agent, 800 rpms of speed
Mixing 5 minutes, whole process temperature of charge are controlled at 80 DEG C, are cooled to room temperature spare；
Third step, by 2 grams of cumyl hydroperoxides, the silica A of second step medium vinyl silane coupling agent processing, titanium dioxide
Silicon B, 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene 45%) 10 grams, benzene
15 grams of solvents of ethylene-butadiene-styrene triblock copolymer are stirred at room temperature dissolution, mix i.e. in 336 grams of dimethylbenzene
Obtain low-dielectric loss composite caking agent；
4th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.70 N/m(ox
/ rice), dielectric loss 0.0021, thermal linear expansion coefficient reaches 3.01 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Embodiment 3
The present embodiment prepares low-dielectric loss composite caking agent, and with 1,2-polybutadiene for main base, silica is to fill out
Material, comprising the following steps:
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:15
(3) styrene-butadiene-styrene triblock copolymer: 25
(4) silica A:60
(5) silica B:30
(6) cumyl hydroperoxide: 1.5
(7) vinyl silicane coupling agent: 1.5
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 60 grams, silica B
30 grams of (particle size range is in normal distribution, and particle size range is 100~600 nanometers), is dried at 120 DEG C respectively, cold
But it is put into high mixer together to room temperature (herein referring to 25 DEG C) and then by the silica A of drying process and silica B,
It is mixed 5 minutes with 600 rpms of speed, then puts into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Mixing 5 minutes, whole process temperature of charge are controlled at 80 DEG C, are cooled to room temperature spare；
Third step takes 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene
45%) 15 grams, 25 grams of solvents of styrene-butadiene-styrene triblock copolymer in 336 grams of dimethylbenzene, be stirred at room temperature molten
Solution obtain 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer it is uniform
Solution for standby；
4th step, the silica A that 1.5 grams of cumyl hydroperoxides and second step medium vinyl silane coupling agent are handled, two
Silica A is added to 1,2-polybutadiene A in third step, 1,2-polybutadiene B, s-B-S three
In the solution of block copolymer, stirring is mixed to get low-dielectric loss composite caking agent is arrived；
5th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.82 N/m(ox
/ rice), dielectric loss 0.0017, thermal linear expansion coefficient reaches 3.10 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Comparative example 3-1
Each component content in comparative example is consistent with the content in embodiment 3, difference with only use dioxy in comparative example
SiClx A.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:15
(3) styrene-butadiene-styrene triblock copolymer: 25
(4) silica A:90
(5) cumyl hydroperoxide: 1.5
(6) vinyl silicane coupling agent: 1.5
It is comprised the concrete steps that:
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 90 grams, respectively 120
It DEG C is dried, is cooled to room temperature and (herein refers to 25 DEG C) and then the silica A of drying process is put into high mixer
In, it is mixed 5 minutes with 600 rpms of speed, then put into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Degree mixing 5 minutes, whole process temperature of charge is controlled at 80 DEG C, is cooled to room temperature spare；
Third step takes 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene
45%) 15 grams, 25 grams of solvents of styrene-butadiene-styrene triblock copolymer in 336 grams of dimethylbenzene, be stirred at room temperature molten
Solution obtain 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer it is uniform
Solution for standby；
4th step, the silica A that 1.5 grams of cumyl hydroperoxides and second step medium vinyl silane coupling agent are handled, adds
Enter into third step 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer
Solution in, stirring, mix to get arrive low-dielectric loss composite caking agent；
5th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.80 N/m(ox
/ rice), dielectric loss 0.0019, thermal linear expansion coefficient reaches 3.13 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Comparative example 3-2
Each component content in comparative example is consistent with the content in embodiment 3, difference with only use dioxy in comparative example
SiClx B.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:15
(3) styrene-butadiene-styrene triblock copolymer: 25
(4) silica B:90
(5) cumyl hydroperoxide: 1.5
(6) vinyl silicane coupling agent: 1.5
It is comprised the concrete steps that:
Second step takes silica B(particle size range in normal distribution, and particle size range is 1~5 micron) 90 grams, respectively 120
It DEG C is dried, is cooled to room temperature and (herein refers to 25 DEG C) and then the silica B of drying process is put into high mixer
In, it is mixed 5 minutes with 600 rpms of speed, then put into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Degree mixing 5 minutes, whole process temperature of charge is controlled at 80 DEG C, is cooled to room temperature spare；
Third step takes 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene
45%) 15 grams, 25 grams of solvents of styrene-butadiene-styrene triblock copolymer in 336 grams of dimethylbenzene, be stirred at room temperature molten
Solution obtain 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer it is uniform
Solution for standby；
4th step, the silica B that 1.5 grams of cumyl hydroperoxides and second step medium vinyl silane coupling agent are handled, adds
Enter into third step 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer
Solution in, stirring, mix to get arrive low-dielectric loss composite caking agent；
5th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.77 N/m(ox
/ rice), dielectric loss 0.0024, thermal linear expansion coefficient reaches 3.24 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Comparative example 3-3
Each component content in comparative example is consistent with the content in embodiment 3, the difference is that, all add together in comparative example
Enter, rather than the implementation steps in the present invention.
The first step, by following components and weight stock (unit is gram):
(1) 1,2-polybutadiene A:50
(2) 1,2-polybutadiene B:15
(3) styrene-butadiene-styrene triblock copolymer: 25
(4) silica A:60
(5) silica B:30
(6) cumyl hydroperoxide: 1.5
(7) vinyl silicane coupling agent: 1.5
Second step takes silica A(particle size range in normal distribution, and particle size range is 1~5 micron) 60 grams, silica B
30 grams of (particle size range is in normal distribution, and particle size range is 100~600 nanometers), is dried at 120 DEG C respectively, cold
But it is put into high mixer together to room temperature (herein referring to 25 DEG C) and then by the silica A of drying process and silica B,
It is mixed 5 minutes with 600 rpms of speed, then puts into 1.5 grams of vinyl silicane coupling agent, 800 rpms of speed
Mixing 5 minutes, whole process temperature of charge are controlled at 80 DEG C, are cooled to room temperature spare；
Third step, by 1.5 grams of cumyl hydroperoxides, silica a, the dioxy of the processing of second step medium vinyl silane coupling agent
SiClx B, 1,2-polybutadiene A(contents of ethylene 91%) 50 grams, 1,2-polybutadiene B(contents of ethylene 45%) 15 grams,
25 grams of solvents of styrene-butadiene-styrene triblock copolymer are stirred at room temperature dissolution, mix in 336 grams of dimethylbenzene
Obtain low-dielectric loss composite caking agent；
4th step sprays to above-mentioned low-dielectric loss composite caking agent on epoxy resin base plate, in 80 DEG C of dryings, passes through control
System spraying dosage can control bondline thickness, and bondline thickness control is then micro- with 50 at 20 microns after drying in the present embodiment
The copper foil hot pressing together of rice, 200 DEG C of hot pressing temperature, 1 megapascal of pressure can test peel strength.Low-dielectric loss is compound viscous
It connects agent to spray on polytetrafluoroethylene film, covers other one piece of polytetrafluoroethylene film hot pressing together, 200 DEG C of hot pressing temperature, pressure
1 megapascal, obtained sample can carry out thermal expansion coefficient and dielectric properties test.
Low-dielectric loss composite caking agent manufactured in the present embodiment, the dielectric peel strength with copper foil are 0.71 N/m(ox
/ rice), dielectric loss 0.0022, thermal linear expansion coefficient reaches 3.02 × 10-5 ℃-1, obtained composite caking agent has
Good mobility, can fill well copper foil corrosion after (because of circuit design needs, copper foil can be etched into various complex shapes
Shape) groove that leaves.
Claims (4)
1. a kind of method for preparing low-dielectric loss composite caking agent, it is characterised in that the preparation method the following steps are included:
The first step is stocked up by following components and weight:
(1) 1,2-polybutadiene A:50 (contents of ethylene >=90%)
(2) 1,2-polybutadiene B:5 ~ 15 (80% >=contents of ethylene >=40%)
(3) styrene-butadiene-styrene triblock copolymer: 5 ~ 35
(4) 1~5 micron of silica A:25~70(partial size)
(5) silica B:10~50 (100~600 nanometers of partial size)
(6) cumyl hydroperoxide: 1.5~5
(7) vinyl silicane coupling agent: 0.6~1.5
Silica A, silica B is dried in second step, is cooled to room temperature and then even with vinyl silanes
Connection agent is handled and is dried；
Third step, above-mentioned 1,2-polybutadiene A, 1,2-polybutadiene B, s-B-S three block is total
Polymers is dissolved in good solvent, and stirring and dissolving obtains 1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-
The homogeneous solution of styrene triblock copolymer；
4th step, the silica A that cumyl hydroperoxide and second step medium vinyl silane coupling agent are handled and dried, two
Silica B is added to 1,2-polybutadiene A in third step, 1,2-polybutadiene B, s-B-S three
In the homogeneous solution of block copolymer, stirring is mixed to get low-dielectric loss composite caking agent is arrived.
2. the method according to claim 1 for preparing low-dielectric loss composite caking agent, it is characterised in that in the first step,
1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer, silica A, two
Silica B, cumyl hydroperoxide, vinyl silicane coupling agent weight part ratio be 50:5:20:60:30:1.5:1.5.
3. the method according to claim 1 for preparing low-dielectric loss composite caking agent, it is characterised in that in the first step,
1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer, silica A, two
Silica B, cumyl hydroperoxide, vinyl silicane coupling agent weight part ratio be 50:10:15:70:10:2:0.8.
4. the method according to claim 1 for preparing low-dielectric loss composite caking agent, it is characterised in that in the first step,
1,2-polybutadiene A, 1,2-polybutadiene B, styrene-butadiene-styrene triblock copolymer, silica A, two
Silica B, cumyl hydroperoxide, vinyl silicane coupling agent weight part ratio be 50:15:25:60:30:1.5:1.5.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105130274A (en) * | 2015-07-15 | 2015-12-09 | 中国电子科技集团公司第四十六研究所 | High-thermal-stability microwave composite dielectric substrate and preparation method thereof |
| CN107090065A (en) * | 2017-06-22 | 2017-08-25 | 陕西生益科技有限公司 | High frequency resin composition and its application in prepreg and metal-clad laminate |
| CN107964203A (en) * | 2017-12-26 | 2018-04-27 | 浙江华正新材料股份有限公司 | A kind of low dielectric prepreg composition, copper-clad plate and preparation method thereof |
| JP2018095749A (en) * | 2016-12-14 | 2018-06-21 | 味の素株式会社 | Resin composition |
-
2018
- 2018-07-27 CN CN201810840158.8A patent/CN109266262B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105130274A (en) * | 2015-07-15 | 2015-12-09 | 中国电子科技集团公司第四十六研究所 | High-thermal-stability microwave composite dielectric substrate and preparation method thereof |
| JP2018095749A (en) * | 2016-12-14 | 2018-06-21 | 味の素株式会社 | Resin composition |
| CN107090065A (en) * | 2017-06-22 | 2017-08-25 | 陕西生益科技有限公司 | High frequency resin composition and its application in prepreg and metal-clad laminate |
| CN107964203A (en) * | 2017-12-26 | 2018-04-27 | 浙江华正新材料股份有限公司 | A kind of low dielectric prepreg composition, copper-clad plate and preparation method thereof |
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