CN113549296A - Epoxy resin high-thermal-conductivity composite material and preparation method thereof - Google Patents
Epoxy resin high-thermal-conductivity composite material and preparation method thereof Download PDFInfo
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- CN113549296A CN113549296A CN202010217057.2A CN202010217057A CN113549296A CN 113549296 A CN113549296 A CN 113549296A CN 202010217057 A CN202010217057 A CN 202010217057A CN 113549296 A CN113549296 A CN 113549296A
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- boron nitride
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 24
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052582 BN Inorganic materials 0.000 claims abstract description 36
- 239000002071 nanotube Substances 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- -1 aminopropyltrimethoxysilane modified boron nitride Chemical class 0.000 claims abstract description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 239000006185 dispersion Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000001723 curing Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000001029 thermal curing Methods 0.000 claims description 7
- 150000004982 aromatic amines Chemical class 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 5
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims description 5
- 238000009775 high-speed stirring Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 238000011049 filling Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 239000000945 filler Substances 0.000 abstract description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011231 conductive filler Substances 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- 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
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
-
- 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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
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Abstract
The invention provides a boron nitride nanotube-epoxy resin high-thermal-conductivity composite material and a preparation method thereof. The composite material is composed of a boron nitride nanotube, epoxy resin and a curing agent, wherein the boron nitride nanotube is an aminopropyltrimethoxysilane modified boron nitride nanotube and accounts for 0.5-10% of the mass fraction. The composite material disclosed by the invention is simple in preparation method and good in process operability, and achieves the purpose of high thermal conductivity by filling a small amount of heat-conducting filler. The prepared composite material has outstanding high heat-conducting property, mechanical property and insulating property.
Description
Technical Field
The invention relates to the field of heat-conducting composite materials, in particular to a boron nitride nanotube-epoxy resin high-heat-conducting composite material and a preparation method thereof.
Background
Epoxy resins are widely used for electrical equipment insulation and microelectronic equipment packaging due to their excellent adhesion, dielectric properties and processability. However, the thermal conductivity of pure epoxy resins is very low, only about 0.2W/(m.K). Therefore, in order to improve the heat dissipation capability of the epoxy resin, the epoxy resin must be modified to improve its thermal conductivity.
At present, the thermal conductivity of epoxy resin is improved by adopting a particle filling method at home and abroad, namely, inorganic filler with higher thermal conductivity, such as oxide (Al) is added into the epoxy resin2O3、SiO2And ZnO), carbides (SiC), and nitrides (AlN and BN), and the like. However, in order to obtain higher thermal conductivity, 50% or more by mass of the thermally conductive filler is usually added to form a complete thermally conductive network in the epoxy resin. The mechanical property of the composite material is inevitably caused by the excessively high filling amount of the heat-conducting fillerThe performance is degraded. Therefore, how to realize a small amount of the heat conductive filler filled while achieving a high heat conductivity has been a technical problem that is difficult to overcome by those skilled in the art.
Disclosure of Invention
The invention aims to provide a boron nitride nanotube-epoxy resin high-thermal-conductivity composite material and a preparation method thereof, which overcome the defects and shortcomings in the background technology.
The technical scheme adopted by the invention is as follows:
in order to solve the above problems, the present invention provides a boron nitride nanotube-epoxy resin high thermal conductivity composite material, comprising: the boron nitride nano-tube is an aminopropyl trimethoxy silane modified boron nitride nano-tube, and accounts for 0.5-10% of the mass fraction;
preferably, the pipe diameter of the boron nitride nanotube is 5 nm-50 nm, and the pipe length is 20 microns-200 microns;
preferably, the epoxy resin is one or a mixture of two of liquid bisphenol A epoxy resin and liquid bisphenol F epoxy resin;
preferably, the curing agent is a liquid aromatic amine curing agent or a polyether amine curing agent;
the invention also provides a preparation method of the boron nitride nanotube-epoxy resin high-thermal-conductivity composite material, which comprises the following steps:
(1) adding boron nitride nanotubes into 5mol/L NaOH solution, stirring and refluxing at 100-140 ℃ for 12-30 h, centrifuging, washing and drying;
(2) and (2) preparing the boron nitride nanotube treated in the step (1) into 1 g/L-2 g/L boron nitride nanotube water dispersion, adding aminopropyl trimethoxy silane, stirring and refluxing at 70-90 ℃ for 8-14 h, centrifuging, washing and drying. The mass fraction of APS is 1-2% by weight of the boron nitride nanotube aqueous dispersion;
(3) dispersing the aminopropyl trimethoxy silane modified boron nitride nanotube prepared in the step (2) in acetone through high-speed stirring, then adding epoxy resin and a curing agent, and performing ultrasonic treatment for 50-70 min to obtain a boron nitride nanotube dispersion liquid;
(4) and (4) heating the dispersion liquid prepared in the step (3) and performing vacuum pumping treatment to remove acetone and bubbles, and finally performing a thermal curing reaction. The thermal curing reaction proceeds as follows: keeping the temperature at 70-100 ℃ for 15-30 h, and then keeping the temperature at 120-150 ℃ for 8-15 h.
Compared with the prior art, the invention has the following advantages:
the composite material provided by the invention is simple in preparation method and good in process operability, and achieves the purpose of high thermal conductivity by filling a small amount of heat-conducting filler. The prepared composite material has outstanding high heat-conducting property, compared with a resin matrix, the heat conductivity of the composite material can be improved by 3-10 times, the mechanical property of the composite material is improved by 20-90%, and the excellent insulating property is kept.
Drawings
FIG. 1 is a SEM image of a cross-section of the composite material obtained in step (4) of example 1.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1:
(1) adding 2g of boron nitride nanotube into 5mol/L NaOH solution, stirring and refluxing for 24h at 120 ℃, centrifuging, washing and drying;
(2) preparing the boron nitride nanotube treated in the step (1) into 2g/L of boron nitride nanotube aqueous dispersion, then adding aminopropyltrimethoxysilane with the mass ratio of 2%, stirring and refluxing for 12h at 80 ℃, centrifuging, washing and drying;
(3) dispersing the aminopropyl trimethoxy silane modified boron nitride nanotube prepared in the step (2) in acetone through high-speed stirring, then adding 14.4g of bisphenol A epoxy resin and 3.6g of aromatic amine curing agent, and performing ultrasonic treatment for 70min to obtain a boron nitride nanotube dispersion liquid;
(4) and (4) heating the dispersion liquid prepared in the step (3) and performing vacuum pumping treatment to remove acetone and bubbles, and finally performing a thermal curing reaction. The thermosetting condition is that the constant temperature of 80 ℃ is kept for 24 hours, and then the constant temperature of 130 ℃ is kept for 12 hours to obtain the composite material;
the composite material has the boron nitride nanotube in 10 wt%, and has heat conductivity of 1.75W/(m.K) at 25 deg.c, tensile strength of 70MPa, and resistivity of 3 x 1015Ω·m。
Example 2:
(1) adding 1g of boron nitride nanotube into 5mol/L NaOH solution, stirring and refluxing for 12h at 120 ℃, centrifuging, washing and drying;
(2) preparing 1g/L boron nitride nanotube aqueous dispersion from the boron nitride nanotubes treated in the step (1), adding 1% by mass of aminopropyl trimethoxysilane, stirring and refluxing for 12h at 80 ℃, centrifuging, washing and drying;
(3) dispersing the aminopropyl trimethoxy silane modified boron nitride nanotube prepared in the step (2) in acetone through high-speed stirring, then adding 15.2g of bisphenol F epoxy resin and 3.8g of aromatic amine curing agent, and performing ultrasonic treatment for 60min to obtain a boron nitride nanotube dispersion liquid;
(4) and (4) heating the dispersion liquid prepared in the step (3) and performing vacuum pumping treatment to remove acetone and bubbles, and finally performing a thermal curing reaction. The thermosetting condition is that the constant temperature of 80 ℃ is kept for 24 hours, and then the constant temperature of 130 ℃ is kept for 12 hours to obtain the composite material;
the composite material has boron nitride nanotube in 5 wt%, 25 deg.c heat conductivity of 0.62W/(m.K), tensile strength of 85 MPa and resistivity of 5 x 1015Ω·m。
Comparative example 1:
14.4g of bisphenol F epoxy resin and 3.6g of aromatic amine curing agent are stirred and mixed uniformly, heating and vacuum pumping treatment are carried out, air bubbles are removed, and finally, thermosetting reaction is carried out. The thermosetting condition is that the constant temperature of 80 ℃ is kept for 24 hours, and then the constant temperature of 130 ℃ is kept for 12 hours to obtain the composite material;
the composite material has boron nitride nanotube in 0 wt%, heat conductivity at 25 deg.c of 0.2W/(m.K), tensile strength of 45 MPa and resistivity of 6 x 1015Ω·m。
Comparative example 2:
(1) dispersing 2g of boron nitride nanotubes in acetone by high-speed stirring, then adding 14.4g of bisphenol F epoxy resin and 3.6g of aromatic amine curing agent, and carrying out ultrasonic treatment for 70min to obtain a boron nitride nanotube dispersion liquid;
(2) and (2) heating the dispersion liquid prepared in the step (1), performing vacuum pumping treatment to remove acetone and bubbles, and finally performing a thermal curing reaction. The thermosetting condition is that the constant temperature of 80 ℃ is kept for 24 hours, and then the constant temperature of 130 ℃ is kept for 12 hours to obtain the composite material;
the composite material has a boron nitride nanotube mass fraction of 10%, and unlike example 1, the boron nitride nanotubes in comparative example 2 were not modified with aminopropyltrimethoxysilane, and the composite material prepared in comparative example 2 was tested to have a thermal conductivity of 0.3W/(m.K) at 25 deg.C, a tensile strength of 20 MPa, and an electrical resistivity of 4X 1015Ω·m。
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (5)
1. A boron nitride nanotube-epoxy resin high thermal conductivity composite material is characterized by comprising: the boron nitride nano-tube is an aminopropyl trimethoxy silane modified boron nitride nano-tube and accounts for 0.5 to 10 mass percent.
2. The boron nitride nanotube-epoxy resin high thermal conductivity composite material according to claim 1, wherein: the pipe diameter of the boron nitride nanotube is 5 nm-50 nm, and the pipe length is 20 microns-200 microns.
3. The boron nitride nanotube-epoxy resin high thermal conductivity composite material according to claim 1, wherein: the epoxy resin is one or a mixture of two of liquid bisphenol A epoxy resin and liquid bisphenol F epoxy resin.
4. The boron nitride nanotube-epoxy resin high thermal conductivity composite material according to claim 1, wherein: the curing agent is liquid aromatic amine curing agent or polyether amine curing agent.
5. A preparation method of a boron nitride nanotube-epoxy resin high-thermal-conductivity composite material is characterized by comprising the following steps:
(1) adding boron nitride nanotubes into 5mol/L NaOH solution, stirring and refluxing at 100-140 ℃ for 12-30 h, centrifuging, washing and drying;
(2) preparing the boron nitride nanotube treated in the step (1) into 1-2 g/L boron nitride nanotube aqueous dispersion, adding aminopropyltrimethoxysilane, stirring and refluxing at 70-90 ℃ for 8-14 h, centrifuging, washing and drying, wherein the APS mass fraction is 1-2% based on the boron nitride nanotube aqueous dispersion;
(3) dispersing the aminopropyl trimethoxy silane modified boron nitride nanotube prepared in the step (2) in acetone through high-speed stirring, then adding epoxy resin and a curing agent, and performing ultrasonic treatment for 50-70 min to obtain a boron nitride nanotube dispersion liquid;
(4) heating and vacuum pumping treatment is carried out on the dispersion liquid prepared in the step (3), acetone and bubbles are removed, and finally, thermocuring reaction is carried out; the thermal curing reaction proceeds as follows: keeping the temperature at 70-100 ℃ for 15-30 h, and then keeping the temperature at 120-150 ℃ for 8-15 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010217057.2A CN113549296A (en) | 2020-04-26 | 2020-04-26 | Epoxy resin high-thermal-conductivity composite material and preparation method thereof |
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| CN202010217057.2A CN113549296A (en) | 2020-04-26 | 2020-04-26 | Epoxy resin high-thermal-conductivity composite material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117603555A (en) * | 2024-01-24 | 2024-02-27 | 四川大学 | High-heat-conductivity high-toughness epoxy resin composite material and preparation method and application thereof |
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2020
- 2020-04-26 CN CN202010217057.2A patent/CN113549296A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117603555A (en) * | 2024-01-24 | 2024-02-27 | 四川大学 | High-heat-conductivity high-toughness epoxy resin composite material and preparation method and application thereof |
| CN117603555B (en) * | 2024-01-24 | 2024-03-22 | 四川大学 | High-heat-conductivity high-toughness epoxy resin composite material and preparation method and application thereof |
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