CN106832785A - A kind of preparation method of modified carborundum boron nitride electronic package material - Google Patents
A kind of preparation method of modified carborundum boron nitride electronic package material Download PDFInfo
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- CN106832785A CN106832785A CN201710105503.9A CN201710105503A CN106832785A CN 106832785 A CN106832785 A CN 106832785A CN 201710105503 A CN201710105503 A CN 201710105503A CN 106832785 A CN106832785 A CN 106832785A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The invention discloses a kind of preparation method of modified carborundum boron nitride electronic package material, the modified carborundum complicated shape that the present invention is added in encapsulating material, and with thermal conductivity it is high, the coefficient of expansion is low, specific stiffness is big, density is small the features such as, 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 modified carborundum boron nitride electronic 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.Although addition filler can be
The cure shrinkage of encapsulating material is reduced to a certain extent, is prevented from ftractureing, is reduced heat release when solidifying, but filler is in aliphatic ring
It is dispersed poor in oxygen tree fat, can increase the initial viscosity of encapsulating material, manufacturability is reduced, and prevent the effect of cracking
It is bad, obtained encapsulating material or easily cracking.It is reported that temperature often raises 10 DEG C, because of GaAs the or Si semiconductor chip longevity
The shortening of life and the failure that produces are just for original 3 times.Its reason is because in microelectronic integrated circuit and power rectifier
In device, the thermal stress that heat fatigue and thermal coefficient of expansion are mismatched and caused caused by heat dispersion is not good between material is made
Into.
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 preparation method of modified carborundum boron nitride electronic package material, and the present invention is in encapsulating material
The modified carborundum complicated shape of middle addition, and with thermal conductivity it is high, the coefficient of expansion is low, specific stiffness is big, density is small the features such as, make
Encapsulating material internal stress changing value scope after hardening it is smaller, mechanical performance and impact resistance are excellent；The preparation side
Method is also adulterated boron nitride nanosheet in the electronic package material so that encapsulating material has good dispersiveness, compatibility
And heat resistance.
To achieve these goals, the invention provides a kind of preparation side of modified carborundum boron nitride electronic package material
Method, the method comprises the following steps：
（1）Prepare modified carborundum
200-300 weight portion peanut shells are weighed, is washed with deionized 3-5 times, be placed in 115-120 DEG C of drying box and dry to perseverance
After weight, add in 500-530 DEG C of vacuum tube furnace, be carbonized 2-3h under nitrogen atmosphere, is cooled to room temperature, take out, by itself and 3-5
Weight portion titante coupling agent, 1-2 weight portions potassium fluoride is well mixed, and inserts in vacuum tube furnace, and vacuum is evacuated in stove
After for 5-10Pa, argon gas is passed through with 150-200mL/min, and 1150-1300 DEG C is warming up to 15 DEG C/min, then with 5 DEG C/min
1500-1550 DEG C is warming up to, after keeping temperature reaction 4-6h, room temperature is naturally cooled to, air is passed through, burnt at 750-800 DEG C
3-5h is burnt, room temperature is cooled to, silicon carbide whisker is obtained；
The above-mentioned silicon carbide whisker of 60-80 weight portions is weighed, in addition 150-200 pbw acetones, and 300W ultrasonic echographies is used
Oil removing 20-30min, filtering, it is 8-10h in 25% hydrofluoric acid solution that filter residue is immersed in into mass fraction, and deionized water is used in filtering
Washing filter residue, in neutrality, is transferred in 115-120 DEG C of vacuum drying chamber and dries to constant weight to cleaning solution pH, obtains modified carborundum；
（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:
Above-mentioned modified carborundum 10-15 parts
Hydrogeneous silicones 3-5 parts of vinyl
Above-mentioned boron nitride nanosheet 3-6 parts
Methylnadic anhydride 1-1.5 parts
Aliphatic epoxy resin 18-20 parts
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 modified carborundum boron nitride electronic package material.
Specific embodiment
Embodiment one
200 weight portion peanut shells are weighed, is washed with deionized 3 times, be placed in 115 DEG C of drying boxes and dry to constant weight, added
In 500 DEG C of vacuum tube furnaces, be carbonized 2h under nitrogen atmosphere, is cooled to room temperature, takes out, by itself and 3 weight portion titanate ester idols
Connection agent, 1 weight portion potassium fluoride is well mixed, inserts in vacuum tube furnace, vacuum is evacuated in stove for after 5Pa, with 150mL/min
Argon gas is passed through, and 1150 DEG C are warming up to 15 DEG C/min, then 1500 DEG C, after keeping temperature reaction 4h are warming up to 5 DEG C/min, from
Room temperature so is cooled to, air is passed through, calcination 3h, is cooled to room temperature at 750 DEG C, obtains silicon carbide whisker.
The above-mentioned silicon carbide whisker of 60 weight portions is weighed, in adding 150 pbw acetones, and with 300W ultrasonic echography oil removings
20min, filtering, it is 8h in 25% hydrofluoric acid solution that filter residue is immersed in into mass fraction, and filtering is washed with deionized filter residue extremely
In neutrality, drying obtains modified carborundum to cleaning solution pH to constant weight in being transferred to 115 DEG C of vacuum drying chambers.
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：
10 parts of above-mentioned modified carborundum
3 parts of the hydrogeneous silicones of vinyl
3 parts of above-mentioned boron nitride nanosheet
1 part of methylnadic anhydride
18 parts of aliphatic epoxy resin
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 modified carborundum boron nitride electronic package material.
Embodiment two
300 weight portion peanut shells are weighed, is washed with deionized 5 times, be placed in 120 DEG C of drying boxes and dry to constant weight, added
In 530 DEG C of vacuum tube furnaces, be carbonized 3h under nitrogen atmosphere, is cooled to room temperature, takes out, by itself and 5 weight portion titanate ester idols
Connection agent, 2 weight portion potassium fluorides are well mixed, insert in vacuum tube furnace, vacuum are evacuated in stove for after 10Pa, with 200mL/
Min is passed through argon gas, and is warming up to 1300 DEG C with 15 DEG C/min, then is warming up to 1550 DEG C, keeping temperature reaction 6h with 5 DEG C/min
Afterwards, room temperature is naturally cooled to, air is passed through, calcination 5h, is cooled to room temperature at 800 DEG C, obtains silicon carbide whisker.
The above-mentioned silicon carbide whisker of 80 weight portions is weighed, in adding 200 pbw acetones, and with 300W ultrasonic echography oil removings
30min, filtering, it is 10h in 25% hydrofluoric acid solution that filter residue is immersed in into mass fraction, and filtering is washed with deionized filter residue extremely
In neutrality, drying obtains modified carborundum to cleaning solution pH to constant weight in being transferred to 120 DEG C of vacuum drying chambers.
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：
15 parts of above-mentioned modified carborundum
5 parts of the hydrogeneous silicones of vinyl
6 parts of above-mentioned boron nitride nanosheet
1.5 parts of methylnadic anhydride
20 parts of aliphatic epoxy resin
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 modified carborundum boron nitride electronic package material.
Claims (1)
1. a kind of preparation method of modified carborundum boron nitride electronic package material, the method comprises the following steps：
（1）Prepare modified carborundum
200-300 weight portion peanut shells are weighed, is washed with deionized 3-5 times, be placed in 115-120 DEG C of drying box and dry to perseverance
After weight, add in 500-530 DEG C of vacuum tube furnace, be carbonized 2-3h under nitrogen atmosphere, is cooled to room temperature, take out, by itself and 3-5
Weight portion titante coupling agent, 1-2 weight portions potassium fluoride is well mixed, and inserts in vacuum tube furnace, and vacuum is evacuated in stove
After for 5-10Pa, argon gas is passed through with 150-200mL/min, and 1150-1300 DEG C is warming up to 15 DEG C/min, then with 5 DEG C/min
1500-1550 DEG C is warming up to, after keeping temperature reaction 4-6h, room temperature is naturally cooled to, air is passed through, burnt at 750-800 DEG C
3-5h is burnt, room temperature is cooled to, silicon carbide whisker is obtained；
The above-mentioned silicon carbide whisker of 60-80 weight portions is weighed, in addition 150-200 pbw acetones, and 300W ultrasonic echographies is used
Oil removing 20-30min, filtering, it is 8-10h in 25% hydrofluoric acid solution that filter residue is immersed in into mass fraction, and deionized water is used in filtering
Washing filter residue, in neutrality, is transferred in 115-120 DEG C of vacuum drying chamber and dries to constant weight to cleaning solution pH, obtains modified carborundum；
（2）Prepare boron nitride nanosheet
Boron nitride powder is added to and mixes equal Uniform in DMF solution, be then centrifuged in centrifuge, remove bottom unstripped
Boron nitride powder, collects the mixed solution on upper strata, then removes solvent, is dried in vacuum drying oven, obtains boron nitride and receives
Rice piece；
（3）According to following weight portion dispensing:
Above-mentioned modified carborundum 10-15 parts
Hydrogeneous silicones 3-5 parts of vinyl
Above-mentioned boron nitride nanosheet 3-6 parts
Methylnadic anhydride 1-1.5 parts
Aliphatic epoxy resin 18-20 parts
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 modified carborundum boron nitride electronic package material.
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| CN201710105503.9A CN106832785A (en) | 2017-02-26 | 2017-02-26 | A kind of preparation method of modified carborundum boron nitride electronic package material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107201006A (en) * | 2017-07-22 | 2017-09-26 | 苏州南尔材料科技有限公司 | A kind of preparation method of Waterproof LED encapsulating material |
| CN107201003A (en) * | 2017-07-14 | 2017-09-26 | 苏州南尔材料科技有限公司 | A kind of preparation method of graphene boron nitride electronic package material |
| CN107316845A (en) * | 2017-07-12 | 2017-11-03 | 苏州南尔材料科技有限公司 | A kind of boron nitride organic silicon electronic encapsulating material preparation method |
| CN108084557A (en) * | 2017-11-26 | 2018-05-29 | 苏州南尔材料科技有限公司 | A kind of boron doped electronic package material preparation method of nitridation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107316845A (en) * | 2017-07-12 | 2017-11-03 | 苏州南尔材料科技有限公司 | A kind of boron nitride organic silicon electronic encapsulating material preparation method |
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Application publication date: 20170613 |