CN106832948A - A kind of boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material preparation method - Google Patents
A kind of boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material preparation method Download PDFInfo
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- CN106832948A CN106832948A CN201710105501.XA CN201710105501A CN106832948A CN 106832948 A CN106832948 A CN 106832948A CN 201710105501 A CN201710105501 A CN 201710105501A CN 106832948 A CN106832948 A CN 106832948A
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- boron nitride
- polymerization thing
- encapsulating material
- based polymerization
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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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
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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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
Abstract
The invention discloses a kind of boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material preparation method, the fluorine silicon epoxy-based polymerization thing that the present invention is prepared by the process of free radical and hydrolytic condensation, it has been provided simultaneously with the property of organosilicon, Organic fluoride, and it is modified to cycloaliphatic epoxy resin with it, impart the excellent weatherability of encapsulating material and surface property, so that encapsulating material internal stress changing value scope after hardening is smaller, mechanical performance and impact resistance are excellent；The preparation method is also adulterated boron nitride nanosheet in the electronic package material so that encapsulating material has good dispersiveness, compatibility and heat resistance.
Description
Technical field
The present invention relates to electronic device manufacture field, and in particular to a kind of boron nitride doped fluor-containing silicon epoxy-based polymerization thing envelope
Package material preparation method.
Background technology
Encapsulation be using specific encapsulating material will arrange each element solidification of the electronic product that connects wherein with environment
The safeguard measure of isolation.The intrusion for preventing moisture, dust and pernicious gas to electronic component is played, slows down vibrations, prevent external force
Damage the effect with stable element parameter.
When the packaging body of encapsulating material and electronic product composition ties up to temperature shock, the unit of encapsulating material and electronic product
Thermal stress, encapsulation system can be produced to crack and ftracture between part, cause the damage of embedded components.In domestic encapsulating material, should
Most commonly used epoxy resin is used, is also the most encapsulating material of cost minimum amount.It has as traditional encapsulating material
Excellent mechanical property and adhesive property, it is cheap, but simultaneously because epoxy resin impact strength is low, weatherability is poor, folding
The low defect of light rate limits its application in encapsulation field.And organosilicon material is used as a kind of more new encapsulating material,
It is high with light transmittance compared with epoxy resin, good weatherability, the features such as anti-aging.
Traditional electronic package material has been difficult to meet the requirement of hyundai electronicses encapsulation.It is multiple with SiC particle-reinforced Al matrix
Condensation material and silicon particle intensifying aluminum based compound material are that the aluminum matrix composite of representative has the advantages that high heat conduction, low bulk, are
Current widely used electron-like encapsulating material, but because aluminium base bulk melting point is relatively low, its heat resistance it is poor and can not be very
The encapsulation of third generation semiconductor devices is met well.Fine copper has the thermal conductivity higher than fine aluminium, and silicon-carbide particle increases in theory
Strong Cu-base composites have thermal conductivity higher, lower thermal coefficient of expansion, more preferable heat resistance and more excellent welding
The advantages of performance, there is very big application potential in Electronic Packaging field.
The content of the invention
The present invention provides a kind of boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material preparation method, and the present invention passes through
Fluorine silicon epoxy-based polymerization thing prepared by the process of free radical and hydrolytic condensation, has been provided simultaneously with the property of organosilicon, Organic fluoride,
And it is modified to cycloaliphatic epoxy resin with it, impart the excellent weatherability of encapsulating material and surface property so that encapsulating material
Internal stress changing value scope after hardening is smaller, and mechanical performance and impact resistance are excellent；The preparation method is also described
Adulterate boron nitride nanosheet in electronic package material so that encapsulating material has good dispersiveness, compatibility and heat resistance.
To achieve these goals, the invention provides a kind of boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material
Preparation method, the method comprises the following steps：
（1）Prepare fluorine silicon epoxy-based polymerization thing
By 30-45 weight portions epoxide containing aliphatic ring acrylic monomers, 10-20 parts by weight of ethylene base silane monomers and 50-100 weight
Amount part acetone mixing, magnetic agitation is uniform, and 50-80 DEG C of temperature is heated under nitrogen protection, is added after temperature is constant and triggered
Agent 2-5 weight portions, continue to heat 3-5h, and the product that will be obtained is rotated, and after removing solvent and accessory substance, obtain product containing ring
Epoxide polysiloxanes；
The above-mentioned 5-15 of based polysiloxane containing epoxy weight portions, 10-35 weight portions are contained into fluorine based silicone, water, catalyst and 50-
100 pbw acetones mix, and stir, and are heated to 60-90 DEG C, and 5-8h is reacted under a nitrogen, product is rotated and is removed
Solvent and accessory substance, obtain fluorine silicon epoxy-based polymerization thing.
（2）Prepare boron nitride nanosheet
Boron nitride powder is added to and mixes equal Uniform in DMF solution, be then centrifuged in centrifuge, remove the unstripped nitrogen in bottom
Change boron powder, collect the mixed solution on upper strata, then remove solvent, be dried in vacuum drying oven, obtain boron nitride nanometer
Piece；
（3）According to following weight portion dispensing:
Hydrogeneous silicones 3-5 parts of vinyl
Above-mentioned boron nitride nanosheet 3-6 parts
Methylnadic anhydride 1-1.5 parts
18-20 parts of above-mentioned fluorine silicon epoxy-based polymerization thing
Titante coupling agent 0.5-1 parts
1-3 parts of containing hydrogen silicone oil crosslinking agent；
（4）Mixed in proportion by said components, heating stirring is carried out mixture to well mixed in vacuum degasing machine
Deaeration, inclined heated plate is 5-7h；
Mixture after the deaeration is added in the hopper of double screw extruder, screw speed is set as 600-800r/
Min, by melting extrusion, water-cooled pelletizing obtains pellet；Then, low temperature high-pressure drying is carried out, injection machine injection moulding is used, is prepared
Obtain boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material.
Specific embodiment
Embodiment one
30 weight portion epoxide containing aliphatic ring acrylic monomers, 10 parts by weight of ethylene base silane monomers and 50 pbw acetones are mixed
Close, magnetic agitation is uniform, and temperature 50 C is heated under nitrogen protection, the weight portion of initiator 2 is added after temperature is constant, continue
Heating 3h, the product that will be obtained is rotated, and after removing solvent and accessory substance, obtains product based polysiloxane containing epoxy.
The weight portion of above-mentioned based polysiloxane containing epoxy 5,10 weight portions are contained into fluorine based silicone, water, catalyst and 50 weight
Part acetone mixing, is stirred, and is heated to 60 DEG C, and 5-8h is reacted under a nitrogen, and product revolving is removed into solvent and by-product
Thing, obtains fluorine silicon epoxy-based polymerization thing.
Boron nitride powder is added to and mixes equal Uniform in DMF solution, be then centrifuged in centrifuge, removed bottom and do not shell
From boron nitride powder, collect upper strata mixed solution, then remove solvent, be dried in vacuum drying oven, nitrogenized
Boron nanometer sheet.
By following weight portion dispensing：
3 parts of the hydrogeneous silicones of vinyl
3 parts of above-mentioned boron nitride nanosheet
1 part of methylnadic anhydride
Above-mentioned 18 parts of fluorine silicon epoxy-based polymerization thing
0.5 part of titante coupling agent
1 part of containing hydrogen silicone oil crosslinking agent；
Mixed in proportion by said components, heating stirring is taken off mixture to well mixed in vacuum degasing machine
Bubble, inclined heated plate is 5h.
Mixture after the deaeration is added in the hopper of double screw extruder, screw speed is set as 600r/
Min, by melting extrusion, water-cooled pelletizing obtains pellet；Then, low temperature high-pressure drying is carried out, injection machine injection moulding is used, is prepared
Obtain boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material.
Embodiment two
By 45 weight portion epoxide containing aliphatic ring acrylic monomers, 20 parts by weight of ethylene base silane monomers and 100 pbw acetones
Mixing, magnetic agitation is uniform, and 80 DEG C of temperature is heated under nitrogen protection, and the weight portion of initiator 5 is added after temperature is constant, after
Continuous heating 5h, the product that will be obtained is rotated, and after removing solvent and accessory substance, obtains product based polysiloxane containing epoxy.
The weight portion of above-mentioned based polysiloxane containing epoxy 15,35 weight portions are contained into fluorine based silicone, water, catalyst and 100 weights
The acetone mixing of amount part, is stirred, and is heated to 90 DEG C, and 8h is reacted under a nitrogen, and product revolving is removed into solvent and by-product
Thing, obtains fluorine silicon epoxy-based polymerization thing.
Boron nitride powder is added to and mixes equal Uniform in DMF solution, be then centrifuged in centrifuge, removed bottom and do not shell
From boron nitride powder, collect upper strata mixed solution, then remove solvent, be dried in vacuum drying oven, nitrogenized
Boron nanometer sheet.
By following weight portion dispensing：
5 parts of the hydrogeneous silicones of vinyl
6 parts of above-mentioned boron nitride nanosheet
1.5 parts of methylnadic anhydride
Above-mentioned 20 parts of fluorine silicon epoxy-based polymerization thing
1 part of titante coupling agent
3 parts of containing hydrogen silicone oil crosslinking agent；
Mixed in proportion by said components, heating stirring is taken off mixture to well mixed in vacuum degasing machine
Bubble, inclined heated plate is 7h.
Mixture after the deaeration is added in the hopper of double screw extruder, screw speed is set as 800r/
Min, by melting extrusion, water-cooled pelletizing obtains pellet；Then, low temperature high-pressure drying is carried out, injection machine injection moulding is used, is prepared
Obtain boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material.
Claims (1)
1. a kind of boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material preparation method, the method comprises the following steps：
（1）Prepare fluorine silicon epoxy-based polymerization thing
By 30-45 weight portions epoxide containing aliphatic ring acrylic monomers, 10-20 parts by weight of ethylene base silane monomers and 50-100 weight
Amount part acetone mixing, magnetic agitation is uniform, and 50-80 DEG C of temperature is heated under nitrogen protection, is added after temperature is constant and triggered
Agent 2-5 weight portions, continue to heat 3-5h, and the product that will be obtained is rotated, and after removing solvent and accessory substance, obtain product containing ring
Epoxide polysiloxanes；
The above-mentioned 5-15 of based polysiloxane containing epoxy weight portions, 10-35 weight portions are contained into fluorine based silicone, water, catalyst and 50-
100 pbw acetones mix, and stir, and are heated to 60-90 DEG C, and 5-8h is reacted under a nitrogen, product is rotated and is removed
Solvent and accessory substance, obtain fluorine silicon epoxy-based polymerization thing,
（2）Prepare boron nitride nanosheet
Boron nitride powder is added to and mixes equal Uniform in DMF solution, be then centrifuged in centrifuge, remove the unstripped nitrogen in bottom
Change boron powder, collect the mixed solution on upper strata, then remove solvent, be dried in vacuum drying oven, obtain boron nitride nanometer
Piece；
（3）According to following weight portion dispensing:
Hydrogeneous silicones 3-5 parts of vinyl
Above-mentioned boron nitride nanosheet 3-6 parts
Methylnadic anhydride 1-1.5 parts
18-20 parts of above-mentioned fluorine silicon epoxy-based polymerization thing
Titante coupling agent 0.5-1 parts
1-3 parts of containing hydrogen silicone oil crosslinking agent；
（4）Mixed in proportion by said components, heating stirring is carried out mixture to well mixed in vacuum degasing machine
Deaeration, inclined heated plate is 5-7h；
Mixture after the deaeration is added in the hopper of double screw extruder, screw speed is set as 600-800r/
Min, by melting extrusion, water-cooled pelletizing obtains pellet；Then, low temperature high-pressure drying is carried out, injection machine injection moulding is used, is prepared
Obtain boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710105501.XA CN106832948A (en) | 2017-02-26 | 2017-02-26 | A kind of boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material preparation method |
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| CN201710105501.XA CN106832948A (en) | 2017-02-26 | 2017-02-26 | A kind of boron nitride doped fluor-containing silicon epoxy-based polymerization thing encapsulating material preparation method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865271A (en) * | 2014-03-20 | 2014-06-18 | 贺建芸 | Nano hybrid material modified organosilicone heat-conductive electronic pouring sealant and preparation method of sealant |
| CN104479606A (en) * | 2014-12-24 | 2015-04-01 | 中科院广州化学有限公司 | High-temperature-resistant high-thermal-conductivity boron-dopedorganosilicon epoxy pouring sealant as well as preparation method and application thereof |
| CN105062082A (en) * | 2015-08-16 | 2015-11-18 | 朱志 | Nano-diamond doped high-strength silicone resin-polymethyl methacrylate composite material for LED packaging and preparation method of composite material |
-
2017
- 2017-02-26 CN CN201710105501.XA patent/CN106832948A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865271A (en) * | 2014-03-20 | 2014-06-18 | 贺建芸 | Nano hybrid material modified organosilicone heat-conductive electronic pouring sealant and preparation method of sealant |
| CN104479606A (en) * | 2014-12-24 | 2015-04-01 | 中科院广州化学有限公司 | High-temperature-resistant high-thermal-conductivity boron-dopedorganosilicon epoxy pouring sealant as well as preparation method and application thereof |
| CN105062082A (en) * | 2015-08-16 | 2015-11-18 | 朱志 | Nano-diamond doped high-strength silicone resin-polymethyl methacrylate composite material for LED packaging and preparation method of composite material |
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Application publication date: 20170613 |
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