CN109535658A - A kind of hexagonal boron nitride/epoxy resin composite material preparation method of high heat conductance - Google Patents
A kind of hexagonal boron nitride/epoxy resin composite material preparation method of high heat conductance Download PDFInfo
- Publication number
- CN109535658A CN109535658A CN201811469670.2A CN201811469670A CN109535658A CN 109535658 A CN109535658 A CN 109535658A CN 201811469670 A CN201811469670 A CN 201811469670A CN 109535658 A CN109535658 A CN 109535658A
- Authority
- CN
- China
- Prior art keywords
- boron nitride
- hexagonal boron
- epoxy resin
- composite material
- resin composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a kind of hexagonal boron nitride/epoxy resin composite material preparation methods of high heat conductance, the preparation method comprises the following steps: preparing hexagonal boron nitride/epoxy resin composite material of high thermal conductivity by solvent dispersion, vacuum filtration, compressing tablet process and curing process using hexagonal boron nitride, epoxy resin as raw material.The high-content of business level bulk hexagonal boron nitride in the epoxy may be implemented to fill and realize the higher thermal conductivity of composite material.The business level hexagonal boron nitride that 70% can be filled in the epoxy by this method, makes heat conductivity be up to 2.6 W/mk, improves 13 times than pure epoxy resin.The method can significantly reduce production cost simultaneously, simple for process, be suitable for large-scale production.
Description
Technical field
The present invention relates to inorganic-organic composite material field more particularly to a kind of hexagonal boron nitride/epoxy resin composite woods
Material.
Background technique
With the high speed development of electronics technology, insulator electronic device field just turns to miniaturization and multifunction, while right
It is increasingly promoted in the requirement of Electronic Encapsulating Technology.It is well known that high molecular material is because of its good mechanical strength, light insulation, and
It is widely used in electronic circuit and its encapsulating material, but the thermal conductivity of high molecular material is usually very low (< 0.5 W/mk), this
Greatly limit the application of high molecular material in practice.Also, as the working frequency of electronic component and relevant device is big
Big to improve, equipment can generate amount of heat in operation, if cannot exclude in time heat, can not only reduce the work of device
Efficiency can also shorten the service life of electronic device.Therefore, how to improve polymer thermal conductivity and become one and widely pay close attention to
Academic hot spot.Currently, research hotspot focuses on and adds inorganic high thermal conductivity particle into macromolecule matrix and prepare inorganic-organic hybrid
Material structure, this composite material can not only guarantee the mechanical strength of material, can also greatly promote the capacity of heat transmission of material.And
In all inorganic fillers, hexagonal boron nitride (h-BN) has superior heating conduction, and thermal conductivity is up in level
300W/mk, and have outstanding insulating properties, fabulous high temperature resistance and electric breakdown strength are closest with polymer performance.
Diabatic process is substantially the process that phonon is propagated through in crystal, therefore influences the factor master of heat conductivity
There are the filling content of boron nitride, the wetability between particle microscopic appearance and filler and polymer interface.Because epoxy resin is viscous
Spend it is larger, so boron nitride powder mass fraction in resin is more than 40% to be just difficult to be prepared with traditional casting method.Another party
Face, h-BN microscopic appearance have bulk, sheet, spherical, fibrous etc., be largely in previous document by platelet boron nitride into
The a large amount of fillings of row.Business level (bulk) boron nitride for directly buying acquisition on the market is carried out high-content filling by rare report,
The thermal conductivity of business level (bulk) boron nitride is generally 30W/mk, so the high-content for solving business level h-BN is filled and realized multiple
The higher thermal conductivity of condensation material is a problem.
Summary of the invention
In view of the drawbacks of the prior art, the present invention provides a kind of hexagonal boron nitride/epoxy resin composite wood of high heat conductance
The preparation method of material passes through solvent dispersion, vacuum filtration, compressing tablet process and solidification using hexagonal boron nitride, epoxy resin as raw material
Hexagonal boron nitride/epoxy resin composite material of processing preparation high thermal conductivity；Specific preparation method the following steps are included:
(1) hexagonal boron nitride, epoxy resin E-51, curing agent methyl tetrahydro phthalic anhydride and altax P-30 are mixed in beaker
In, progress high-speed stirred ultrasound is uniformly mixed solution after ethanol solution is added；
(2) mixed solution obtained by step (1) is placed in oven and dried after vacuum filtration, to remove residual alcohol, is done
Hexagonal boron nitride/epoxy resin composite material filter cake is obtained after dry；
(3) the resulting hexagonal boron nitride of step (2)/epoxy resin composite material filter cake is placed in the tabletting for having coated release agent
In machine mold, and filter cake tow sides are subjected to compressing tablet process respectively, take out filter cake after compressing tablet process and are placed on baking oven progress
Curing process obtains hexagonal boron nitride/epoxy resin composite material；The compressing tablet process is to realize six by way of pressurization
Close connection between square boron nitride forms more passage of heat, and hexagonal boron nitride obtains uniformly in the epoxy
And high-content is filled.
Further, hexagonal boron nitride described in step (1) carries out surface-functionalized, detailed process are as follows: by six side's nitrogen of 5g
Change boron and the 200ml concentrated sulfuric acid is put into ball milling 48h in ball grinder.Solution is taken out after ball milling, be put into 1500ml beaker and is added
The dilution of 1000ml deionized water, and ultrasound 2h in ultrasonator is placed the beaker, so that hexagonal boron nitride is uniformly dispersed, Zhi Houyong
Vacuum filtration device filters the solution, and be washed with deionized filter cake to solution pH value be it is neutral after be put into 80 DEG C of baking ovens
Dry 12h, obtains hydroxylated hexagonal boron nitride；Further functionalization, by silane coupling agent KH-540, water, ethyl alcohol with 1:
The volume ratio configuration of 4:36 is dissolved and ultrasound 3h, and hydroxylated hexagonal boron nitride is dissolved in the silane coupler solution prepared later
Middle magnetic agitation 12h, filtration washing obtains the hexagonal boron nitride of silanization later.
Further, filter cake oven drying temperature is 80 DEG C in the step (2), drying time 2h.
Further, compressing tablet process is that hexagonal boron nitride/epoxy resin composite material filter cake is positive and negative in the step (3)
Two sides applies the pressure of 5-20Mpa, application time 15min respectively；The solidification temperature of curing process is in the step (3)
80-180 DEG C, curing time 6h.
Further, the hexagonal boron nitride/epoxy resin composite material, wherein the mass fraction of hexagonal boron nitride be
10-70%。
Further, the hexagonal boron nitride is directly to buy the business level bulk hexagonal boron nitride obtained in the market.
Further, in the tow sides tableting processes, filter cake is placed in and has applied the tablet press machine for wiping release agent mill
In tool, and it will just apply 15min pressure, which is rapidly brought up to 10Mpa in 1min, then keeps constant, after 14min slowly
Pressure relief, then slowly boosts to 10Mpa then at reverse side within 15min, then presses down quickly sizing.
Compared with prior art, the beneficial effects of the present invention are:
1, the content of the bulk hexagonal boron nitride of business level can in hexagonal boron nitride/epoxy resin composite material prepared by the present invention
Reach 70%, realizes the uniform and high-content filling of business level hexagonal boron nitride in the epoxy.
2, existed using hexagonal boron nitride in hexagonal boron nitride/epoxy resin composite material of tow sides compressing tablet process preparation
It can slowly be adjusted in compression process and sprawl direction, realize the both horizontally and vertically close connection between hexagonal boron nitride, shape
At more passage of heat, to significantly improve the thermal coefficient of composite material, the wherein quality of the hexagonal boron nitride of silanization
When score is 70%, the thermal conductivity of composite material is 2.6W/mk, improves 13 times than pure epoxy resin.
3, production cost can be significantly reduced using business level hexagonal boron nitride.
4, method provided by the invention is simple and easy, is suitable for large-scale production.
Detailed description of the invention
Fig. 1 is hexagonal boron nitride/epoxy resin composite material photo in kind that embodiment 10 is prepared.
A, b, c, d are respectively that hexagonal boron nitride/epoxy resin for preparing of comparative example and embodiment 14,16,18 is compound in Fig. 2
The section SEM image of material.
Fig. 3 is epoxy resin prepared by embodiment 1 to 9 and hexagonal boron nitride/epoxy resin composite material thermal conductivity folding
Line chart.
Fig. 4 is epoxy resin and hexagonal boron nitride/epoxy resin composite material thermal conductivity prepared by embodiment 10 to 18
Line chart.
Specific embodiment
Below in conjunction with attached drawing and specific preferred embodiment, the invention will be further described, but does not therefore limit this
The protection scope of invention.
Specific embodiment 1: a kind of hexagonal boron nitride/epoxy resin composite material preparation method packet of high thermal conductivity
It includes:
(1) 4g bulk h-BN and suitable epoxy resin and curing agent methyl tetrahydro phthalic anhydride, altax P-30 are weighed and is mixed
In beaker, 200ml ethanol solution is added, speed stirring ultrasound 6h is uniformly mixed solution.
(2) by mixed solution obtained by step (1), after vacuum filtration, dry 2h is put into 80 DEG C of baking ovens, it is surplus to remove
Remaining alcohol obtains hexagonal boron nitride/epoxy resin composite material filter cake after dry；
(3) the resulting hexagonal boron nitride of step (2)/epoxy resin composite material filter cake is placed in the tabletting for having coated release agent
In machine mold, and filter cake tow sides are subjected to compressing tablet process respectively, pressure 5-20Mpa, application time 15min take out
After compressing tablet process filter cake and be placed on baking oven carry out curing process, solidification temperature be 80-180 DEG C, curing time be 6h obtain six
Square boron nitride/epoxy resin composite material.
Specific embodiment 2: formation efficiency is more in order to reduce the contact resistance between hexagonal boron nitride and epoxy resin
High passage of heat, the progress of hexagonal boron nitride described in specific embodiment one is surface-functionalized, method particularly includes: by 5g six
Square boron nitride and the 200ml concentrated sulfuric acid are put into ball milling 48h in ball grinder.Solution is taken out after ball milling, is put into 1500ml beaker simultaneously
The dilution of 1000ml deionized water is added, and places the beaker ultrasound 2h in ultrasonator, hexagonal boron nitride is made to be uniformly dispersed, it
The solution is filtered with Vacuum filtration device afterwards, and be washed with deionized filter cake to solution pH value be it is neutral after be put into 80 DEG C of bakings
Dry 12h, obtains hydroxylated hexagonal boron nitride, by silane coupling agent KH-540, water, ethyl alcohol with the volume ratio of 1:4:36 in case
Configuration dissolution and ultrasound 3h, are dissolved in magnetic agitation in the silane coupler solution prepared for hydroxylated hexagonal boron nitride later
12h, filtration washing obtains the hexagonal boron nitride of silanization later.Using the hexagonal boron nitride of silanization as raw material, using specific
The method of embodiment one prepares hexagonal boron nitride/epoxy resin composite material of high thermal conductivity.
Specific embodiment three
In order to make to connect between hexagonal boron nitride more sufficiently, tabletting mode in front and back sides described in specific embodiment two is carried out
Pressure adjustment, method particularly includes: 5g hexagonal boron nitride and the 200ml concentrated sulfuric acid are put into ball milling 48h in ball grinder.It will be molten after ball milling
Liquid takes out, and is put into 1500ml beaker and the dilution of 1000ml deionized water is added, and places the beaker ultrasonic in ultrasonator
2h makes hexagonal boron nitride be uniformly dispersed, and is later filtered the solution with Vacuum filtration device, and filter cake is washed with deionized extremely
Solution pH value obtains hydroxylated hexagonal boron nitride, by silane coupling agent KH- to be put into 80 DEG C of baking ovens dry 12h after neutrality
540, hydroxylated hexagonal boron nitride is dissolved in is matched later by water, ethyl alcohol with the volume ratio configuration dissolution of 1:4:36 and ultrasound 3h
Magnetic agitation 12h in good silane coupler solution, filtration washing obtains the hexagonal boron nitride of silanization later.By silanization
Hexagonal boron nitride prepares hexagonal boron nitride/epoxy resin of high thermal conductivity using the method for specific embodiment one as raw material
Filter cake is placed in and has applied in the tablet press machine grinding tool for wiping release agent in positive and negative tableting processes by composite material, and will just apply
15min pressure, the pressure are rapidly brought up to 10Mpa in 1min, then keep constant, slow pressure relief after 14min, then again
10Mpa is slowly boosted within 15min in reverse side, then presses down quickly sizing, is removed filter cake later and is covered with filter paper and is wrapped
It wraps up in, is placed in 150 DEG C of baking ovens and solidifies 6h, obtain hexagonal boron nitride/epoxy resin composite material of high thermal conductivity, i.e. EP/h-
MBNS。
Embodiment 1:
(1) epoxy resin and curing agent methyl tetrahydro phthalic anhydride 2g, 0.2g altax P-30 for weighing 4g bulk h-BN and 36g are simultaneously
It is mixed in beaker, 200ml ethanol solution is added, magnetic agitation 6h is uniformly mixed solution, later by the mixed solution
Vacuum filtration removes alcohol, and hexagonal boron nitride/epoxy resin composite material filter cake is obtained in funnel.
(2) gently filter cake is removed and is placed on planar silicon plate, remove filter paper, then the new filter paper of the filter cake is covered
It wraps up and is placed in 80 DEG C oven drying 2h to remove remaining a little alcohol.
(3) after filtration cakes torrefaction, filter cake is placed in and has been applied in the tablet press machine grinding tool for wiping release agent, and by tow sides
Apply 15min, 10Mpa pressure respectively.Filter cake is removed later and is covered with filter paper and is wrapped up, and is placed in 150 DEG C of baking ovens and is solidified 6h, obtains
To hexagonal boron nitride/epoxy resin composite material of high thermal conductivity, i.e. EP/h-BNS.
Embodiment 2-9:
Preparation method is same as Example 1, only changes content of epoxy resin, so that six sides in epoxy resin composite material nitrogenize
The mass percent of boron is 15%, 20%, 25%, 30%, 40%, 50%, 60%, 70%, the heat conductivity value of embodiment 1 to 9 such as Fig. 3 institute
Show.
Embodiment 10:
(1) 5g h-BN and the 200ml concentrated sulfuric acid is put into ball milling 48h in ball grinder.Solution is taken out after ball milling, is put into 1500ml
In beaker and the dilution of 1000ml deionized water is added, and places the beaker ultrasound 2h in ultrasonator, h-BN is made to be uniformly dispersed,
The solution is filtered with Vacuum filtration device later, and filter cake is washed with deionized for several times to being put into 80 DEG C of baking ovens after neutral
Dry 12h, obtains hydroxylated hexagonal boron nitride.Silane coupling agent KH-540, water, ethyl alcohol are configured with the volume ratio of 1:4:36
Simultaneously ultrasound 3h is dissolved, dried hydroxylated hexagonal boron nitride is dissolved in magnetic force in the silane coupler solution prepared later
12h is stirred, filtration washing obtains the hexagonal boron nitride of silanization later.
(2) epoxy resin and curing agent methyl tetrahydro phthalic anhydride 2g, 0.2g altax P- of 4g bulk h-BN and 36g are weighed
It 30 and is mixed in beaker, 200ml ethanol solution is added, magnetic agitation 6h is uniformly mixed solution, later by the mixing
Solution vacuum filtration removes alcohol, and hexagonal boron nitride/epoxy resin composite material filter cake is obtained in funnel.
(3) gently filter cake is removed and is placed on planar silicon plate, remove filter paper, then the new filter paper of the filter cake is covered
It wraps up and is placed in 80 DEG C oven drying 2h to remove remaining a little alcohol.
(4) after filtration cakes torrefaction, filter cake is placed in and has been applied in the tablet press machine grinding tool for wiping release agent, and by tow sides
Apply 15min, 10Mpa pressure respectively.Filter cake is removed later and is covered with filter paper and is wrapped up, and is placed in 150 DEG C of baking ovens and is solidified 6h, obtains
To hexagonal boron nitride/epoxy resin composite material of high thermal conductivity, i.e. EP/h-MBNS.
Embodiment 11-18:
Preparation method is same as Example 1, only changes content of epoxy resin, so that six sides in epoxy resin composite material nitrogenize
The mass percent of boron is 15%, 20%, 25%, 30%, 40%, 50%, 60%, 70%, the heat conductivity value of embodiment 10 to 18 such as Fig. 4
It is shown.
Embodiment 19:
(1) epoxy resin and curing agent methyl tetrahydro phthalic anhydride 2g, 0.2g altax P-30 for weighing 4g bulk h-BN and 36g are simultaneously
It is mixed in beaker, 200ml ethanol solution is added, magnetic agitation 6h is uniformly mixed solution, later by the mixed solution
Vacuum filtration removes alcohol, and hexagonal boron nitride/epoxy resin composite material filter cake is obtained in funnel.
(2) gently filter cake is removed and is placed on planar silicon plate, remove filter paper, then the new filter paper of the filter cake is covered
It wraps up and is placed in 80 DEG C oven drying 2h to remove remaining a little alcohol.
(3) after filtration cakes torrefaction, filter cake is placed in and has been applied in the tablet press machine grinding tool for wiping release agent, and by tow sides
Apply 15min, 10Mpa pressure respectively.Filter cake is removed later and is covered with filter paper and is wrapped up, and is placed in 100 DEG C of baking ovens and is solidified 6h, obtains
To hexagonal boron nitride/epoxy resin composite material of high thermal conductivity.
Embodiment 20:
(1) 5g h-BN and the 200ml concentrated sulfuric acid is put into ball milling 48h in ball grinder.Solution is taken out after ball milling, is put into 1500ml
In beaker and the dilution of 1000ml deionized water is added, and places the beaker ultrasound 2h in ultrasonator, h-BN is made to be uniformly dispersed,
The solution is filtered with Vacuum filtration device later, and filter cake is washed with deionized for several times to being put into 80 DEG C of baking ovens after neutral
Dry 12h, obtains hydroxylated hexagonal boron nitride.Silane coupling agent KH-540, water, ethyl alcohol are configured with the volume ratio of 1:4:36
Simultaneously ultrasound 3h is dissolved, dried hydroxylated hexagonal boron nitride is dissolved in magnetic force in the silane coupler solution prepared later
12h is stirred, filtration washing obtains the hexagonal boron nitride of silanization later.
(2) epoxy resin and curing agent methyl tetrahydro phthalic anhydride 2g, 0.2g altax P- of 4g bulk h-BN and 36g are weighed
It 30 and is mixed in beaker, 200ml ethanol solution is added, magnetic agitation 6h is uniformly mixed solution, later by the mixing
Solution vacuum filtration removes alcohol, and hexagonal boron nitride/epoxy resin composite material filter cake is obtained in funnel.
(3) gently filter cake is removed and is placed on planar silicon plate, remove filter paper, then the new filter paper of the filter cake is covered
It wraps up and is placed in 80 DEG C oven drying 2h to remove remaining a little alcohol.
(4) after filtration cakes torrefaction, filter cake is placed in and has been applied in the tablet press machine grinding tool for wiping release agent, and by tow sides
Apply 15min, 10Mpa pressure respectively.Filter cake is removed later and is covered with filter paper and is wrapped up, and is placed in 150 DEG C of baking ovens and is solidified 6h, obtains
To hexagonal boron nitride/epoxy resin composite material of high thermal conductivity.Filter cake is removed later and is covered with filter paper and is wrapped up, and is placed on 180
Solidify 6h in DEG C baking oven, obtains hexagonal boron nitride/epoxy resin composite material of high thermal conductivity.
Embodiment 21
(1) 5g h-BN and the 200ml concentrated sulfuric acid is put into ball milling 48h in ball grinder.Solution is taken out after ball milling, is put into 1500ml
In beaker and the dilution of 1000ml deionized water is added, and places the beaker ultrasound 2h in ultrasonator, h-BN is made to be uniformly dispersed,
The solution is filtered with Vacuum filtration device later, and filter cake is washed with deionized for several times to being put into 80 DEG C of baking ovens after neutral
Dry 12h, obtains hydroxylated hexagonal boron nitride.Silane coupling agent KH-540, water, ethyl alcohol are configured with the volume ratio of 1:4:36
Simultaneously ultrasound 3h is dissolved, dried hydroxylated hexagonal boron nitride is dissolved in magnetic force in the silane coupler solution prepared later
12h is stirred, filtration washing obtains the hexagonal boron nitride of silanization later.
(2) epoxy resin and curing agent methyl tetrahydro phthalic anhydride 2g, 0.2g altax P- of 4g bulk h-BN and 36g are weighed
It 30 and is mixed in beaker, 200ml ethanol solution is added, magnetic agitation 6h is uniformly mixed solution, later by the mixing
Solution vacuum filtration removes alcohol, and hexagonal boron nitride/epoxy resin composite material filter cake is obtained in funnel.
(3) gently filter cake is removed and is placed on planar silicon plate, remove filter paper, then the new filter paper of the filter cake is covered
It wraps up and is placed in 80 DEG C oven drying 2h to remove remaining a little alcohol.
(4) after filtration cakes torrefaction, filter cake is placed in and has been applied in the tablet press machine grinding tool for wiping release agent, and will just applied
15min pressure, the pressure are rapidly brought up to 10Mpa in 1min, then keep constant, slow pressure relief after 14min, then again
10Mpa is slowly boosted within 15min in reverse side, then presses down quickly sizing, is removed filter cake later and is covered with filter paper and is wrapped
It wraps up in, is placed in 150 DEG C of baking ovens and solidifies 6h, obtain hexagonal boron nitride/epoxy resin composite material of high thermal conductivity, i.e. EP/h-
MBNS。
Comparative example:
This comparative example is related to a kind of preparation process of epoxide resin material, comprising:
(1) 40g epoxy resin and curing agent methyl tetrahydro phthalic anhydride 2g, 0.2g altax P-3 are weighed and is mixed in beaker, is added
Enter 200ml ethanol solution, magnetic agitation 6h is uniformly mixed solution, the mixed solution is filtered by vacuum removes alcohol later
It removes, and obtains epoxy resin filter cake in funnel.
(2) gently filter cake is removed and is placed on planar silicon plate, remove filter paper, then the new filter paper of the filter cake is covered
It wraps up and is placed in 80 DEG C oven drying 2h to remove remaining a little alcohol.
(3) after filtration cakes torrefaction, filter cake is placed in and has been applied in the tablet press machine grinding tool for wiping release agent, and by tow sides
Apply 15min, 15Mpa pressure respectively.Filter cake is removed later and is covered with filter paper and is wrapped up, and is placed in 150 DEG C of baking ovens and is solidified 6h, obtains
To sheet type epoxy.
Claims (8)
1. a kind of hexagonal boron nitride/epoxy resin composite material preparation method of high heat conductance, it is characterised in that: with six side's nitrogen
Change boron, epoxy resin as raw material, six sides of high thermal conductivity are prepared by solvent dispersion, vacuum filtration, compressing tablet process and curing process
Boron nitride/epoxy resin composite material；Specific preparation method the following steps are included:
(1) hexagonal boron nitride, epoxy resin E-51, curing agent methyl tetrahydro phthalic anhydride and altax P-30 are mixed in beaker
In, progress high-speed stirred ultrasound is uniformly mixed solution after ethanol solution is added；
(2) mixed solution obtained by step (1) is placed in oven and dried after vacuum filtration, to remove residual alcohol, is done
Hexagonal boron nitride/epoxy resin composite material filter cake is obtained after dry；
(3) the resulting hexagonal boron nitride of step (2)/epoxy resin composite material filter cake is placed in the tabletting for having coated release agent
In machine mold, and filter cake tow sides are subjected to compressing tablet process respectively, take out filter cake after compressing tablet process and are placed on baking oven progress
Curing process obtains hexagonal boron nitride/epoxy resin composite material；
The compressing tablet process is to realize the close connection between hexagonal boron nitride by way of pressurization, is formed more thermally conductive
Channel, and hexagonal boron nitride obtains in the epoxy uniformly and high-content is filled.
2. hexagonal boron nitride/epoxy resin composite material preparation method of high heat conductance according to claim 1, special
Sign is: the hexagonal boron nitride carries out surface-functionalized, detailed process are as follows: puts 5g hexagonal boron nitride and the 200ml concentrated sulfuric acid
Enter ball milling 48h in ball grinder, take out solution after ball milling, is put into 1500ml beaker and is added the dilution of 1000ml deionized water,
And ultrasound 2h in ultrasonator is placed the beaker, and so that hexagonal boron nitride is uniformly dispersed, it is with Vacuum filtration device that this is molten later
Liquid filtering, and filter cake is washed with deionized to solution pH value to be put into 80 DEG C of baking ovens dry 12h after neutrality, obtain hydroxylating
Hexagonal boron nitride.
3. hexagonal boron nitride/epoxy resin composite material preparation method of high heat conductance according to claim 2, special
Sign is: the hexagonal boron nitride carries out further surface-functionalized, detailed process are as follows: by silane coupling agent KH-540, water, second
Alcohol with the volume ratio of 1:4:36 configuration dissolution and ultrasound 3h, hydroxylated hexagonal boron nitride is dissolved in later prepare it is silane coupled
Magnetic agitation 12h in agent solution, filtration washing obtains the hexagonal boron nitride of silanization later.
4. hexagonal boron nitride/epoxy resin composite material system of high heat conductance according to any one of claim 1-3
Preparation Method, it is characterised in that: filter cake oven drying temperature is 80 DEG C in the step (2), drying time 2h.
5. hexagonal boron nitride/epoxy resin composite material system of high heat conductance according to any one of claim 1-3
Preparation Method, it is characterised in that: in the step (3) compressing tablet process be by hexagonal boron nitride/epoxy resin composite material filter cake just
Anti- two sides applies the pressure of 5-20Mpa, application time 15min respectively.
6. hexagonal boron nitride/epoxy resin composite material preparation of the high heat conductance according to any one of claim 5
Method, it is characterised in that: the solidification temperature of curing process is 80-180 DEG C in the step (3), curing time 6h.
7. hexagonal boron nitride/epoxy resin composite material system of high heat conductance according to any one of claim 1-3
Preparation Method, it is characterised in that: the hexagonal boron nitride/epoxy resin composite material, the wherein mass percent of hexagonal boron nitride
For 10-70%.
8. hexagonal boron nitride/epoxy resin composite material system of high heat conductance according to any one of claim 1-3
Preparation Method, it is characterised in that: the hexagonal boron nitride is directly to buy the business level bulk hexagonal boron nitride obtained in the market.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811469670.2A CN109535658A (en) | 2018-12-04 | 2018-12-04 | A kind of hexagonal boron nitride/epoxy resin composite material preparation method of high heat conductance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811469670.2A CN109535658A (en) | 2018-12-04 | 2018-12-04 | A kind of hexagonal boron nitride/epoxy resin composite material preparation method of high heat conductance |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109535658A true CN109535658A (en) | 2019-03-29 |
Family
ID=65853488
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811469670.2A Pending CN109535658A (en) | 2018-12-04 | 2018-12-04 | A kind of hexagonal boron nitride/epoxy resin composite material preparation method of high heat conductance |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109535658A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111423699A (en) * | 2020-05-12 | 2020-07-17 | 河北工业大学 | Preparation method of high-filling-amount hexagonal boron nitride/polymer blocky composite material |
| CN113004736A (en) * | 2021-03-09 | 2021-06-22 | 中山大学 | Preparation method of modified boron nitride nanosheet and application of modified boron nitride nanosheet in improving corrosion resistance of aqueous organic protective coating |
| CN113956617A (en) * | 2021-10-27 | 2022-01-21 | 江苏拜富科技股份有限公司 | Preparation method of high-insulation low-temperature electronic packaging material |
| CN114318312A (en) * | 2022-01-07 | 2022-04-12 | 河北工业大学 | Polyaniline modified boron nitride composite material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1114843A1 (en) * | 1999-12-16 | 2001-07-11 | Edison Polymer Innovation Corporation | Surface treated boron nitride for forming a low viscosity high thermal conductivity polymer based boron nitride composition and method |
| CN103539085A (en) * | 2013-11-05 | 2014-01-29 | 河北工业大学 | Synthesis method for hexagonal boron nitride nanosheet |
-
2018
- 2018-12-04 CN CN201811469670.2A patent/CN109535658A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1114843A1 (en) * | 1999-12-16 | 2001-07-11 | Edison Polymer Innovation Corporation | Surface treated boron nitride for forming a low viscosity high thermal conductivity polymer based boron nitride composition and method |
| CN103539085A (en) * | 2013-11-05 | 2014-01-29 | 河北工业大学 | Synthesis method for hexagonal boron nitride nanosheet |
Non-Patent Citations (3)
| Title |
|---|
| HOU J, ET AL: "Preparation and characterization of surface modified boron nitride epoxy composites with enhanced thermal conductivity", 《RSC ADVANCES》 * |
| 刘建华: "《材料成型工艺基础》", 29 February 2016, 西安电子科技大学出版社 * |
| 谢圣英: "《塑料材料》", 31 January 2010, 中国轻工业出版社 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111423699A (en) * | 2020-05-12 | 2020-07-17 | 河北工业大学 | Preparation method of high-filling-amount hexagonal boron nitride/polymer blocky composite material |
| CN111423699B (en) * | 2020-05-12 | 2022-11-11 | 河北工业大学 | Preparation method of high-filling-amount hexagonal boron nitride/polymer blocky composite material |
| CN113004736A (en) * | 2021-03-09 | 2021-06-22 | 中山大学 | Preparation method of modified boron nitride nanosheet and application of modified boron nitride nanosheet in improving corrosion resistance of aqueous organic protective coating |
| CN113956617A (en) * | 2021-10-27 | 2022-01-21 | 江苏拜富科技股份有限公司 | Preparation method of high-insulation low-temperature electronic packaging material |
| WO2022156832A3 (en) * | 2021-10-27 | 2022-09-22 | 江苏拜富科技股份有限公司 | Preparation method for high-insulativity low-temperature electronic packaging material |
| CN114318312A (en) * | 2022-01-07 | 2022-04-12 | 河北工业大学 | Polyaniline modified boron nitride composite material and preparation method and application thereof |
| CN114318312B (en) * | 2022-01-07 | 2024-04-23 | 河北工业大学 | Polyaniline modified boron nitride composite material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109535658A (en) | A kind of hexagonal boron nitride/epoxy resin composite material preparation method of high heat conductance | |
| CN104788909B (en) | A kind of heat conductive insulating composite and preparation method thereof | |
| CN109181316A (en) | Heat-conductive composite material and preparation method thereof | |
| CN102653622A (en) | Preparation method of high-dielectric-constant ceramics/polymer-based composite dielectric materials | |
| CN103936401B (en) | A kind of preparation method of low dielectric constant microwave dielectric ceramic material | |
| CN103732557B (en) | Glass ceramic body, substrate for mounting light-emitting element and light-emitting device | |
| CN105541389A (en) | Barium titanate foam ceramic/thermosetting resin composite material and preparation method thereof | |
| CN102133634A (en) | Preparation methods of carbon nanotube metal powder mixture and metal composite material | |
| CN108570202A (en) | The preparation method of polytetrafluoroethylene (PTFE) composite substrate material | |
| CN112479630A (en) | Ceramic composite heat dissipation device and preparation method thereof | |
| CN113329608B (en) | Preparation method of nano barium titanate/ferroferric oxide hybrid material with high wave-absorbing performance | |
| CN106521230A (en) | Graphite flake/copper composite material used for vertical directional heat dissipation, and preparation method thereof | |
| CN107674349A (en) | A kind of fluoropolymer composite of low-k and preparation method thereof | |
| CN112225186B (en) | Preparation method of spherical boron nitride | |
| CN113337126A (en) | Heat-conducting insulating silicon rubber and preparation method and application thereof | |
| CN104961471A (en) | Cast film slurry of ultrathin lamination flaky inductor and manufacturing method for cast film of ultrathin lamination flaky inductor | |
| CN109096620B (en) | Ethylene propylene diene monomer rubber-based direct-current cable accessory material and preparation method thereof | |
| CN102351467B (en) | Preparation method of wave-absorbing composite material used for isolator loading | |
| CN110343276A (en) | A kind of graphene with negative dielectric properties/polyvinyl alcohol flexible composite film and preparation method thereof | |
| CN109679142A (en) | A kind of preparation method of the compound heat filling of macromolecule | |
| CN115746498A (en) | Preparation method of high-thermal-conductivity graphene phenolic moulding plastic | |
| CN106221086B (en) | A kind of new PTFE based composites and preparation method thereof | |
| CN115073932A (en) | High-dielectric liquid crystal polymer composite material and preparation method thereof | |
| CN112143145B (en) | Low dielectric loss type polytetrafluoroethylene microwave board and preparation method thereof | |
| CN112794314A (en) | Preparation method of high-density graphene heat-conducting film regulated and controlled by groups and obtained product |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190329 |