CN108299780A - A kind of preparation method and applications of the dielectric materials of addition epoxy resin - Google Patents
A kind of preparation method and applications of the dielectric materials of addition epoxy resin Download PDFInfo
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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
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
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- C08L33/12—Homopolymers or copolymers of methyl methacrylate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a kind of preparation method and applications of the dielectric materials of addition epoxy resin, this method is used magnesium silicate, it is calcined after bismuth oxide ball milling, calcined product is pulverized into carry out secondary ball milling again, the calcined product ball milling particle and polymethyl methacrylate that will be obtained, epoxy resin heating stirring is reacted, it is ultrasonically treated after thermal response mixture is mixed with the concentrated sulfuric acid again, it filters, washing filter cake is simultaneously dried to obtain sulfonated products, finally by sulfonated products and boron trifluoride ether, n-Hexacosanyl lsovalerate mixes, polyethylene glycol heating stirring is added, crosslinking agent is added to continue to stir, the curing process after vacuum outgas, hot pressing, obtain finished product dielectric materials.The dielectric materials for the addition epoxy resin being prepared, dielectric constant is low, bending strength is high, has a good application prospect on electronic component.
Description
Technical field
The present invention relates to this technical fields of electronic material, are related specifically to a kind of dielectric materials of addition epoxy resin
Preparation method and applications.
Background technology
Advanced low-k materials or low-K material are the hot issues of current semiconductor industry research.It is integrated by reducing
The dielectric constant of the dielectric material used in circuit can reduce the leakage current of integrated circuit, reduce the capacitance between conducting wire
Effect reduces integrated circuit fever etc..Along with electronics, the fast development of microelectronics industry, microelectronic element function is not
While disconnected enhancing, volume is but reduced constantly, therefore its internal component density gradually increases, this will lead to signal transmission
Delay, crosstalk noise enhancing etc., the delay of wherein signal seems even more serious, in order to accelerate the transmission speed of signal, reduces letter
Number interference and induction coupling, there is an urgent need to use advanced low-k materials.
There are epoxy resin excellent adhesive property, electrical insulation capability, mechanical performance, raw material sources to enrich, of low cost,
Advantage easily processed into type becomes the composite material for being now widely used for printed wiring board.High-performance epoxy resin is to IC
The encapsulation of chip play the role of it is extremely important, make IC chip working environment stability inferior improve, service life increase.But
It is the rapid development of microelectronic industry in recent years so that the dielectric properties of general epoxy resin cannot be satisfied current low dielectric at all
The requirement of material.
Invention content
In order to solve the above technical problems, the present invention provide it is a kind of addition epoxy resin dielectric materials preparation method and
It is applied, and this method is used and will be calcined after magnesium silicate, bismuth oxide ball milling, then calcined product is pulverized carry out secondary ball milling, will
The calcined product ball milling particle arrived is reacted with polymethyl methacrylate, epoxy resin heating stirring, then by thermal response mixture
Be ultrasonically treated, filter after being mixed with the concentrated sulfuric acid, washing filter cake and being dried to obtain sulfonated products, finally by sulfonated products with it is borontrifluoride
Borate ether, n-Hexacosanyl lsovalerate mixing are added polyethylene glycol heating stirring, add crosslinking agent and continue to stir, through true
Curing process, hot pressing after sky degassing, obtain finished product dielectric materials.The dielectric materials for the addition epoxy resin being prepared,
Its dielectric constant is low, bending strength is high, has a good application prospect on electronic component.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of the dielectric materials of addition epoxy resin, includes the following steps：
(1) steel ball in 4-6 parts of 7-9 parts of magnesium silicate, bismuth oxide input ball mills, will be added and carries out ball-milling treatment for the first time, with
2-4 parts of obtained ball-milled mixtures and agglutinant are placed in tube furnace afterwards and calcined, calcination temperature is 1500 DEG C, and calcination time is
It 2-3 hours, after calcined product is cooled to room temperature, is pulverized and carries out secondary ball milling processing, obtain calcined product ball milling particle；
(2) the calcined product ball for obtaining 25-35 parts of polymethyl methacrylate, 20-30 parts of epoxy resin and step (1)
Abrasive particle is added in heating stirrer, according to 200 revs/min of rotating speed heating stirring 80-100 minutes at 80-90 DEG C, is obtained
To thermal response mixture；
(3) in mass ratio 1:The 10 thermal response mixtures for obtaining step (2) and the concentrated sulfuric acid that mass concentration is 85% are mixed
Conjunction is ultrasonically treated, and then filters ultrasonic mixing liquid, collects filter cake, filter cake is washed with deionized 4-6 times, with
It is 10 hours dry at 75-85 DEG C afterwards, obtain sulfonated products；
(4) 12-16 parts of boron trifluoride ether, 6-10 parts of n-Hexacosanyl lsovalerate are produced with sulfonation obtained by step (3)
Object mixes, and the polyethylene glycol of 10 times of parts by weight of mixture is added, and is warming up to 80-90 DEG C, and insulated and stirred 15-25 minutes is added and hands over
Join 2-4 part of agent, continuation insulated and stirred 10-20 minutes, then by gained thermal agitation reactant at 120 DEG C vacuum outgas 90 minutes,
Then 150 DEG C of curing process are warming up to 2-3 hours, obtain cured product；
(5) cured product for obtaining step (4) obtains finished-product material in 130-150 DEG C of hot pressing.
Further, the ratio of grinding media to material of the ball-milling treatment for the first time in the step (1) is 15:1, the rotating speed of ball mill is 350
Rev/min, Ball-milling Time is 3-5 hours, and the ratio of grinding media to material of secondary ball milling processing is 20:1, the rotating speed of ball mill is 300 revs/min
Clock, Ball-milling Time are 60-90 minutes.
Further, the agglutinant in the step (1) is preferably with glass sand and potassium feldspar according to 2:1 mass ratio is matched
Mixture made of system.
Further, the power being ultrasonically treated in the step (3) is 350-450W, and the time is 20-30 minutes.
Further, pressure used in hot pressing is 1-2MPa in the step (5), and hot pressing time is 10-20 minutes.
Further, the invention also discloses the dielectric materials of epoxy resin are added made from the preparation method in electricity
Application on sub- component.
Compared with prior art, the present invention advantage is：
(1) preparation method of the dielectric materials of addition epoxy resin of the invention is used magnesium silicate, bismuth oxide ball milling
After calcine, then calcined product is pulverized into carry out secondary ball milling, the calcined product ball milling particle and poly-methyl methacrylate that will be obtained
Ester, the reaction of epoxy resin heating stirring, then be ultrasonically treated, filter after thermal response mixture is mixed with the concentrated sulfuric acid, washing filter cake
And sulfonated products are dried to obtain, sulfonated products are mixed with boron trifluoride ether, n-Hexacosanyl lsovalerate finally, are added poly-
Ethylene glycol heating stirring, adds crosslinking agent and continues to stir, curing process, hot pressing after vacuum outgas obtain the low dielectric of finished product
Material.The dielectric materials for the addition epoxy resin being prepared, dielectric constant is low, bending strength is high, in electronic component
On have a good application prospect.
(2) present invention employs polymethyl methacrylate, epoxy resin, boron trifluoride ether, isovaleric acid positive 26
Alcohol ester these types raw material participation prepares dielectric materials, and the dielectric materials to adding epoxy resin have carried out effective performance and carried
It rises, although these materials are not first Application in dielectric materials, according to a certain ratio after amount combination, is aided with corresponding place
Reason mode brings increasing substantially in performance to the dielectric materials for the addition epoxy resin being finally prepared,
This is never to report in previous research, for realizing that it is conclusive that the technique effect of the present invention plays the role of.
Specific implementation mode
The technical solution of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1) steel ball in 4 parts of 7 parts of magnesium silicate, bismuth oxide input ball mills, will be added and carries out ball-milling treatment for the first time, ratio of grinding media to material
It is 15:1, the rotating speed of ball mill is 350 revs/min, and Ball-milling Time is 3 hours, then by obtained ball-milled mixtures and sintering
2 parts of agent, which is placed in tube furnace, calcines, and agglutinant is with glass sand and potassium feldspar according to 2:The mixing that 1 mass ratio is formulated
Object, calcination temperature are 1500 DEG C, and calcination time is 2 hours, after calcined product is cooled to room temperature, is pulverized carry out secondary ball
Mill processing, ratio of grinding media to material 20:1, the rotating speed of ball mill is 300 revs/min, and Ball-milling Time is 60 minutes, obtains calcined product ball
Abrasive particle；
(2) the calcined product ball milling particle for obtaining 25 parts of polymethyl methacrylate, 20 parts of epoxy resin and step (1)
It is added in heating stirrer, according to 200 revs/min of rotating speed heating stirring 80 minutes at 80 DEG C, obtains thermal response mixing
Material；
(3) in mass ratio 1:The 10 thermal response mixtures for obtaining step (2) and the concentrated sulfuric acid that mass concentration is 85% are mixed
Conjunction is ultrasonically treated, and the power of supersound process is 350W, and the time is 20 minutes, then filters ultrasonic mixing liquid, is received
Collect filter cake, filter cake is washed with deionized 4 times, it is then 10 hours dry at 75 DEG C, obtain sulfonated products；
(4) 12 parts of boron trifluoride ether, 6 parts of n-Hexacosanyl lsovalerate are mixed with sulfonated products obtained by step (3),
The polyethylene glycol of 10 times of parts by weight of mixture is added, is warming up to 80 DEG C, 2 parts of crosslinking agent is added, after continuation of insurance in insulated and stirred 15 minutes
Temperature stirring 10 minutes, then by gained thermal agitation reactant at 120 DEG C vacuum outgas 90 minutes, be then warming up to 150 DEG C of solidifications
Processing 2 hours, obtains cured product；
(5) for the cured product for obtaining step (4) in 130 DEG C of hot pressing, pressure used in hot pressing is 1MPa, hot pressing time 10
Minute, obtain finished-product material.
The performance test results of the dielectric materials of addition epoxy resin obtained are as shown in table 1.
Embodiment 2
(1) steel ball in 5 parts of 8 parts of magnesium silicate, bismuth oxide input ball mills, will be added and carries out ball-milling treatment for the first time, ratio of grinding media to material
It is 15:1, the rotating speed of ball mill is 350 revs/min, and Ball-milling Time is 4 hours, then by obtained ball-milled mixtures and sintering
3 parts of agent, which is placed in tube furnace, calcines, and agglutinant is with glass sand and potassium feldspar according to 2:The mixing that 1 mass ratio is formulated
Object, calcination temperature are 1500 DEG C, and calcination time is 2.5 hours, and after calcined product is cooled to room temperature, it is secondary to be pulverized progress
Ball-milling treatment, ratio of grinding media to material 20:1, the rotating speed of ball mill is 300 revs/min, and Ball-milling Time is 75 minutes, obtains calcined product
Ball milling particle；
(2) the calcined product ball milling particle for obtaining 30 parts of polymethyl methacrylate, 25 parts of epoxy resin and step (1)
It is added in heating stirrer, according to 200 revs/min of rotating speed heating stirring 90 minutes at 85 DEG C, obtains thermal response mixing
Material；
(3) in mass ratio 1:The 10 thermal response mixtures for obtaining step (2) and the concentrated sulfuric acid that mass concentration is 85% are mixed
Conjunction is ultrasonically treated, and the power of supersound process is 400W, and the time is 25 minutes, then filters ultrasonic mixing liquid, is received
Collect filter cake, filter cake is washed with deionized 5 times, it is then 10 hours dry at 80 DEG C, obtain sulfonated products；
(4) 14 parts of boron trifluoride ether, 8 parts of n-Hexacosanyl lsovalerate are mixed with sulfonated products obtained by step (3),
The polyethylene glycol of 10 times of parts by weight of mixture is added, is warming up to 85 DEG C, 3 parts of crosslinking agent is added, after continuation of insurance in insulated and stirred 20 minutes
Temperature stirring 15 minutes, then by gained thermal agitation reactant at 120 DEG C vacuum outgas 90 minutes, be then warming up to 150 DEG C of solidifications
Processing 2.5 hours, obtains cured product；
(5) for the cured product for obtaining step (4) in 140 DEG C of hot pressing, pressure used in hot pressing is 1.5MPa, and hot pressing time is
15 minutes, obtain finished-product material.
The performance test results of the dielectric materials of addition epoxy resin obtained are as shown in table 1.
Embodiment 3
(1) steel ball in 6 parts of 9 parts of magnesium silicate, bismuth oxide input ball mills, will be added and carries out ball-milling treatment for the first time, ratio of grinding media to material
It is 15:1, the rotating speed of ball mill is 350 revs/min, and Ball-milling Time is 5 hours, then by obtained ball-milled mixtures and sintering
4 parts of agent, which is placed in tube furnace, calcines, and agglutinant is with glass sand and potassium feldspar according to 2:The mixing that 1 mass ratio is formulated
Object, calcination temperature are 1500 DEG C, and calcination time is 3 hours, after calcined product is cooled to room temperature, is pulverized carry out secondary ball
Mill processing, ratio of grinding media to material 20:1, the rotating speed of ball mill is 300 revs/min, and Ball-milling Time is 90 minutes, obtains calcined product ball
Abrasive particle；
(2) the calcined product ball milling particle for obtaining 35 parts of polymethyl methacrylate, 30 parts of epoxy resin and step (1)
It is added in heating stirrer, according to 200 revs/min of rotating speed heating stirring 100 minutes at 90 DEG C, obtains thermal response mixing
Material；
(3) in mass ratio 1:The 10 thermal response mixtures for obtaining step (2) and the concentrated sulfuric acid that mass concentration is 85% are mixed
Conjunction is ultrasonically treated, and the power of supersound process is 450W, and the time is 30 minutes, then filters ultrasonic mixing liquid, is received
Collect filter cake, filter cake is washed with deionized 6 times, it is then 10 hours dry at 85 DEG C, obtain sulfonated products；
(4) 16 parts of boron trifluoride ether, 10 parts of n-Hexacosanyl lsovalerate is mixed with sulfonated products obtained by step (3)
It closing, the polyethylene glycol of 10 times of parts by weight of mixture is added, be warming up to 90 DEG C, 4 parts of crosslinking agent is added in insulated and stirred 25 minutes, after
Continuous insulated and stirred 20 minutes, then by gained thermal agitation reactant at 120 DEG C vacuum outgas 90 minutes, be then warming up to 150 DEG C
Curing process 3 hours, obtains cured product；
(5) for the cured product for obtaining step (4) in 150 DEG C of hot pressing, pressure used in hot pressing is 2MPa, hot pressing time 20
Minute, obtain finished-product material.
The performance test results of the dielectric materials of addition epoxy resin obtained are as shown in table 1.
Comparative example 1
(1) steel ball in 5 parts of 8 parts of magnesium silicate, bismuth oxide input ball mills, will be added and carries out ball-milling treatment for the first time, ratio of grinding media to material
It is 15:1, the rotating speed of ball mill is 350 revs/min, and Ball-milling Time is 4 hours, then by obtained ball-milled mixtures and sintering
3 parts of agent, which is placed in tube furnace, calcines, and agglutinant is with glass sand and potassium feldspar according to 2:The mixing that 1 mass ratio is formulated
Object, calcination temperature are 1500 DEG C, and calcination time is 2.5 hours, and after calcined product is cooled to room temperature, it is secondary to be pulverized progress
Ball-milling treatment, ratio of grinding media to material 20:1, the rotating speed of ball mill is 300 revs/min, and Ball-milling Time is 75 minutes, obtains calcined product
Ball milling particle；
(2) the calcined product ball milling particle that 25 parts of epoxy resin and step (1) obtain is added in heating stirrer,
According to 200 revs/min of rotating speed heating stirring 90 minutes at 85 DEG C, thermal response mixture is obtained；
(3) in mass ratio 1:The 10 thermal response mixtures for obtaining step (2) and the concentrated sulfuric acid that mass concentration is 85% are mixed
Conjunction is ultrasonically treated, and the power of supersound process is 400W, and the time is 25 minutes, then filters ultrasonic mixing liquid, is received
Collect filter cake, filter cake is washed with deionized 5 times, it is then 10 hours dry at 80 DEG C, obtain sulfonated products；
(4) 14 parts of boron trifluoride ether, 8 parts of n-Hexacosanyl lsovalerate are mixed with sulfonated products obtained by step (3),
The polyethylene glycol of 10 times of parts by weight of mixture is added, is warming up to 85 DEG C, 3 parts of crosslinking agent is added, after continuation of insurance in insulated and stirred 20 minutes
Temperature stirring 15 minutes, then by gained thermal agitation reactant at 120 DEG C vacuum outgas 90 minutes, be then warming up to 150 DEG C of solidifications
Processing 2.5 hours, obtains cured product；
(5) for the cured product for obtaining step (4) in 140 DEG C of hot pressing, pressure used in hot pressing is 1.5MPa, and hot pressing time is
15 minutes, obtain finished-product material.
The performance test results of dielectric materials obtained are as shown in table 1.
Comparative example 2
(1) steel ball in 5 parts of 8 parts of magnesium silicate, bismuth oxide input ball mills, will be added and carries out ball-milling treatment for the first time, ratio of grinding media to material
It is 15:1, the rotating speed of ball mill is 350 revs/min, and Ball-milling Time is 4 hours, then by obtained ball-milled mixtures and sintering
3 parts of agent, which is placed in tube furnace, calcines, and agglutinant is with glass sand and potassium feldspar according to 2:The mixing that 1 mass ratio is formulated
Object, calcination temperature are 1500 DEG C, and calcination time is 2.5 hours, and after calcined product is cooled to room temperature, it is secondary to be pulverized progress
Ball-milling treatment, ratio of grinding media to material 20:1, the rotating speed of ball mill is 300 revs/min, and Ball-milling Time is 75 minutes, obtains calcined product
Ball milling particle；
(2) the calcined product ball milling particle that 30 parts of polymethyl methacrylate and step (1) obtain heating is added to stir
It mixes in device, according to 200 revs/min of rotating speed heating stirring 90 minutes at 85 DEG C, obtains thermal response mixture；
(3) in mass ratio 1:The 10 thermal response mixtures for obtaining step (2) and the concentrated sulfuric acid that mass concentration is 85% are mixed
Conjunction is ultrasonically treated, and the power of supersound process is 400W, and the time is 25 minutes, then filters ultrasonic mixing liquid, is received
Collect filter cake, filter cake is washed with deionized 5 times, it is then 10 hours dry at 80 DEG C, obtain sulfonated products；
(4) 14 parts of boron trifluoride ether, 8 parts of n-Hexacosanyl lsovalerate are mixed with sulfonated products obtained by step (3),
The polyethylene glycol of 10 times of parts by weight of mixture is added, is warming up to 85 DEG C, 3 parts of crosslinking agent is added, after continuation of insurance in insulated and stirred 20 minutes
Temperature stirring 15 minutes, then by gained thermal agitation reactant at 120 DEG C vacuum outgas 90 minutes, be then warming up to 150 DEG C of solidifications
Processing 2.5 hours, obtains cured product；
(5) for the cured product for obtaining step (4) in 140 DEG C of hot pressing, pressure used in hot pressing is 1.5MPa, and hot pressing time is
15 minutes, obtain finished-product material.
The performance test results of dielectric materials obtained are as shown in table 1.
Comparative example 3
(1) steel ball in 5 parts of 8 parts of magnesium silicate, bismuth oxide input ball mills, will be added and carries out ball-milling treatment for the first time, ratio of grinding media to material
It is 15:1, the rotating speed of ball mill is 350 revs/min, and Ball-milling Time is 4 hours, then by obtained ball-milled mixtures and sintering
3 parts of agent, which is placed in tube furnace, calcines, and agglutinant is with glass sand and potassium feldspar according to 2:The mixing that 1 mass ratio is formulated
Object, calcination temperature are 1500 DEG C, and calcination time is 2.5 hours, and after calcined product is cooled to room temperature, it is secondary to be pulverized progress
Ball-milling treatment, ratio of grinding media to material 20:1, the rotating speed of ball mill is 300 revs/min, and Ball-milling Time is 75 minutes, obtains calcined product
Ball milling particle；
(2) the calcined product ball milling particle for obtaining 30 parts of polymethyl methacrylate, 25 parts of epoxy resin and step (1)
It is added in heating stirrer, according to 200 revs/min of rotating speed heating stirring 90 minutes at 85 DEG C, obtains thermal response mixing
Material；
(3) in mass ratio 1:The 10 thermal response mixtures for obtaining step (2) and the concentrated sulfuric acid that mass concentration is 85% are mixed
Conjunction is ultrasonically treated, and the power of supersound process is 400W, and the time is 25 minutes, then filters ultrasonic mixing liquid, is received
Collect filter cake, filter cake is washed with deionized 5 times, it is then 10 hours dry at 80 DEG C, obtain sulfonated products；
(4) 8 parts of n-Hexacosanyl lsovalerate mix with sulfonated products obtained by step (3), addition 10 times of weights of mixture
The polyethylene glycol for measuring part is warming up to 85 DEG C, and 3 parts of crosslinking agent is added in insulated and stirred 20 minutes, continues insulated and stirred 15 minutes, then
By gained thermal agitation reactant at 120 DEG C vacuum outgas 90 minutes, be then warming up to 150 DEG C of curing process 2.5 hours, must consolidate
Change product；
(5) for the cured product for obtaining step (4) in 140 DEG C of hot pressing, pressure used in hot pressing is 1.5MPa, and hot pressing time is
15 minutes, obtain finished-product material.
The performance test results of dielectric materials obtained are as shown in table 1.
Comparative example 4
(1) steel ball in 5 parts of 8 parts of magnesium silicate, bismuth oxide input ball mills, will be added and carries out ball-milling treatment for the first time, ratio of grinding media to material
It is 15:1, the rotating speed of ball mill is 350 revs/min, and Ball-milling Time is 4 hours, then by obtained ball-milled mixtures and sintering
3 parts of agent, which is placed in tube furnace, calcines, and agglutinant is with glass sand and potassium feldspar according to 2:The mixing that 1 mass ratio is formulated
Object, calcination temperature are 1500 DEG C, and calcination time is 2.5 hours, and after calcined product is cooled to room temperature, it is secondary to be pulverized progress
Ball-milling treatment, ratio of grinding media to material 20:1, the rotating speed of ball mill is 300 revs/min, and Ball-milling Time is 75 minutes, obtains calcined product
Ball milling particle；
(2) the calcined product ball milling particle for obtaining 30 parts of polymethyl methacrylate, 25 parts of epoxy resin and step (1)
It is added in heating stirrer, according to 200 revs/min of rotating speed heating stirring 90 minutes at 85 DEG C, obtains thermal response mixing
Material；
(3) in mass ratio 1:The 10 thermal response mixtures for obtaining step (2) and the concentrated sulfuric acid that mass concentration is 85% are mixed
Conjunction is ultrasonically treated, and the power of supersound process is 400W, and the time is 25 minutes, then filters ultrasonic mixing liquid, is received
Collect filter cake, filter cake is washed with deionized 5 times, it is then 10 hours dry at 80 DEG C, obtain sulfonated products；
(4) 14 parts of boron trifluoride ether mix with sulfonated products obtained by step (3), addition 10 times of parts by weight of mixture
Polyethylene glycol, is warming up to 85 DEG C, insulated and stirred 20 minutes, and 3 parts of crosslinking agent is added, and continues insulated and stirred 15 minutes, then by gained
Thermal agitation reactant vacuum outgas 90 minutes at 120 DEG C, are then warming up to 150 DEG C of curing process 2.5 hours, must cure production
Object；
(5) for the cured product for obtaining step (4) in 140 DEG C of hot pressing, pressure used in hot pressing is 1.5MPa, and hot pressing time is
15 minutes, obtain finished-product material.
The performance test results of dielectric materials obtained are as shown in table 1.
By the dielectric materials obtained of embodiment 1-3 and comparative example 1-4 carry out respectively dielectric constant, bending strength this two
Item performance test.
Table 1
| Dielectric constant | Bending strength (MPa) | |
| Embodiment 1 | 2.5 | 192 |
| Embodiment 2 | 2.7 | 198 |
| Embodiment 3 | 2.4 | 195 |
| Comparative example 1 | 3.1 | 182 |
| Comparative example 2 | 3.0 | 179 |
| Comparative example 3 | 3.4 | 183 |
| Comparative example 4 | 2.9 | 176 |
The preparation method of the dielectric materials of the addition epoxy resin of the present invention is used and will be forged after magnesium silicate, bismuth oxide ball milling
It burns, then calcined product is pulverized into carry out secondary ball milling, by obtained calcined product ball milling particle and polymethyl methacrylate, ring
Oxygen resin heating stirring is reacted, then is ultrasonically treated after thermal response mixture is mixed with the concentrated sulfuric acid, filters, is washed filter cake and drying
Sulfonated products are obtained, finally mix sulfonated products with boron trifluoride ether, n-Hexacosanyl lsovalerate, polyethylene glycol is added
Heating stirring, adds crosslinking agent and continues to stir, curing process, hot pressing after vacuum outgas obtain finished product dielectric materials.System
The dielectric materials of epoxy resin are added made of standby, dielectric constant is low, bending strength is high, has on electronic component good
Good application prospect.Also, present invention employs polymethyl methacrylate, epoxy resin, boron trifluoride ether, isovaleric acid just
Hexacosyl alcohol ester these types raw material participation prepares dielectric materials, and the dielectric materials to adding epoxy resin have carried out effectively
Performance boost according to a certain ratio after amount combination, is aided with phase although these materials are not first Application in dielectric materials
The processing mode answered is brought in performance significantly to the dielectric materials for the addition epoxy resin being finally prepared
It improves, this is never to report in previous research, for realizing that the technique effect of the present invention plays conclusive work
With.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of the dielectric materials of addition epoxy resin, which is characterized in that include the following steps：
(1) steel ball in 4-6 parts of 7-9 parts of magnesium silicate, bismuth oxide input ball mills, will be added and carries out ball-milling treatment for the first time, then will
2-4 parts of obtained ball-milled mixtures and agglutinant, which is placed in tube furnace, to be calcined, and calcination temperature is 1500 DEG C, calcination time 2-3
Hour, after calcined product is cooled to room temperature, is pulverized and carry out secondary ball milling processing, obtain calcined product ball milling particle；
(2) the calcined product ball milling for obtaining 25-35 parts of polymethyl methacrylate, 20-30 parts of epoxy resin and step (1)
Grain is added in heating stirrer, according to 200 revs/min of rotating speed heating stirring 80-100 minutes at 80-90 DEG C, obtains heat
React mixture；
(3) in mass ratio 1:10 are mixed into the concentrated sulfuric acid that the thermal response mixture that step (2) obtains is 85% with mass concentration
Row is ultrasonically treated, and then filters ultrasonic mixing liquid, collects filter cake, filter cake is washed with deionized 4-6 times, is then existed
It is 10 hours dry at 75-85 DEG C, obtain sulfonated products；
(4) 12-16 parts of boron trifluoride ether, 6-10 parts of n-Hexacosanyl lsovalerate is mixed with sulfonated products obtained by step (3)
It closes, the polyethylene glycol of 10 times of parts by weight of mixture is added, be warming up to 80-90 DEG C, crosslinking agent is added in insulated and stirred 15-25 minutes
2-4 parts, continue insulated and stirred 10-20 minutes, then by gained thermal agitation reactant at 120 DEG C vacuum outgas 90 minutes, then
It is warming up to 150 DEG C of curing process 2-3 hours, obtains cured product；
(5) cured product for obtaining step (4) obtains finished-product material in 130-150 DEG C of hot pressing.
2. the preparation method of the dielectric materials of addition epoxy resin according to claim 1, which is characterized in that the step
Suddenly the ratio of grinding media to material of the ball-milling treatment for the first time in (1) is 15:1, the rotating speed of ball mill is 350 revs/min, and Ball-milling Time is that 3-5 is small
When, the ratio of grinding media to material of secondary ball milling processing is 20:1, the rotating speed of ball mill is 300 revs/min, and Ball-milling Time is 60-90 minutes.
3. the preparation method of the dielectric materials of addition epoxy resin according to claim 1, which is characterized in that the step
Suddenly the agglutinant in (1) is preferably with glass sand and potassium feldspar according to 2:The mixture that 1 mass ratio is formulated.
4. the preparation method of the dielectric materials of addition epoxy resin according to claim 1, which is characterized in that the step
Suddenly the power being ultrasonically treated in (3) is 350-450W, and the time is 20-30 minutes.
5. the preparation method of the dielectric materials of addition epoxy resin according to claim 1, which is characterized in that the step
Suddenly pressure used in hot pressing is 1-2MPa in (5), and hot pressing time is 10-20 minutes.
6. according to the dielectric materials of epoxy resin are added made from any one of the claim 1-5 preparation methods in electronics member
Application on device.
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| CN103756253A (en) * | 2013-12-17 | 2014-04-30 | 北京化工大学 | Low dielectric constant hollow carbon sphere/epoxy resin composite material and preparation method thereof |
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