CN107501610A - A kind of composite heat interfacial material based on boron nitride and preparation method thereof - Google Patents
A kind of composite heat interfacial material based on boron nitride and preparation method thereof Download PDFInfo
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- CN107501610A CN107501610A CN201710760089.5A CN201710760089A CN107501610A CN 107501610 A CN107501610 A CN 107501610A CN 201710760089 A CN201710760089 A CN 201710760089A CN 107501610 A CN107501610 A CN 107501610A
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- 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
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- 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
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- C09K5/14—Solid materials, e.g. powdery or granular
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a kind of composite heat interfacial material based on boron nitride and preparation method thereof, it is related to thermal interfacial material technical field, mainly for solving the problems, such as the thermal conductivity and thermal contact resistance that how to improve epoxy resin-base composite material, this method carries out surface modification treatment using suitable coupling agent to hexagonal boron nitride, improve the compatibility and dispersiveness of boron nitride and matrix material, can fine dispersion in matrix material, reduce gather and produce height and matrix between interface resistance.Then doping hexagonal boron nitride is into the composite of Nanometer Copper and epoxy resin, using nanometer copper particle, in solidification, the molten condition that occurs is connected between boron nitride layer to strengthen, form three-dimensional heat flow conducting network, the interface resistance of composite inner is further reduced, so as to the overall heat conductivility for improving composite.
Description
Technical field
The present invention relates to thermal interfacial material technical field, and in particular to a kind of composite heat interfacial material based on boron nitride and
Its preparation method.
Background technology
With the rapid development of electronic system and the device fabrication including mechanical structure, integrated circuit (IC) core
Piece is all the time all approximate to be developed with Moore's Law, is even more multifunction, the integrated, work with electronic system in recent years
The rapidly development of working frequency, packing density, its side effect being derived are drastically ascending to heaven for electronic device caloric value.According to
Semi-conductor industry federation(The Semiconductor Industry Association)The ITRS 2010 of publication reports pre-
100 W/cm2 will be broken through in the near future by surveying the power density of electronic device, and the thermal resistance of whole cooling system is also required
Control is below 50 mm2 K/W.
In order to obtain good thermo-contact between two surfaces, thermal interfacial material is widely used for filling and produced by processing mode
Raw surface topography space and groove, the contact area between surface is improved with this, strengthens the heat transfer efficiency between contact interface.
Currently used heat-conducting cream, heat-conducting glue and phase-change material(PCM)Deng thermal interfacial material, not only its own effective thermal conductivity is low,
The problems such as aging, seepage, failure also easily occur under cyclic loading, so as to seriously restrict reliability and the longevity of electronic device
Life.Due to the excellent heat conductivity performance of low-dimensional materials and brazing metal, the study hotspot of current thermal interfacial material of future generation mainly collects
In in application of the nanometer technology in thermal interfacial material and low-temperature sintering type thermal interfacial material.There is research to point out, single more wall carbon are received
The thermal conductivity of mitron is used as the filler of epoxy resin-base generally using CNT up to 1000 W/m K even more highs, researcher
The composite with higher heat-conductivity is made, can improve the thermal conductivity of epoxy composite material by the mixing of different proportion
More than 60%.But because the micro interface thermal resistance between this type nano granular and matrix material is larger, the composite conductivity of heat of formation
Thermal interfacial material advantage that can be more traditional is not special protrusion.
The content of the invention
In view of the shortcomings of the prior art, the technical problem to be solved in the present invention is how to improve epoxy resin-matrix compound thermal circle
The thermal conductivity of plane materiel material is with reducing thermal contact resistance.
For above-mentioned technical problem, technical scheme provided by the invention is:A kind of composite heat interfacial based on boron nitride
Material preparation method, comprise the following steps:
Step 1, the composite heat interfacial material of Nanometer Copper and epoxy resin is prepared, it is specifically as follows step by step:
(1)Epoxy resin and curing agent are mixed to obtain mixed liquor;
(2)It will clean and dried nano copper particle is added in the mixed liquor, and add diluent agitation grinding;
(3)Add acetone and carry out ultrasonic disperse;
(4)Simultaneously vacuum defoamation obtains the composite heat interfacial material of Nanometer Copper and epoxy resin in 3 ~ 5 hours to heating stirring;
Step 2, the composite heat interfacial material based on boron nitride is prepared, it is specifically as follows step by step:
(1)Surface modification treatment is carried out to boron nitride using silane coupler and is dried in vacuo;
(2)Dried boron nitride is added in the composite heat interfacial material of the Nanometer Copper and epoxy resin, and add dilution
Agent agitation grinding obtains compound mixed liquor;
(3)Acetone and ultrasonic disperse are added in the compound mixed liquor;
(4)The compound mixed liquor after disperseing that will eliminate the noise is heated and is slowly stirred under vacuo, and vacuum defoamation 5-8 hours obtain
Composite heat interfacial material based on boron nitride.
In the step 1:
Step by step(1)The mixing time be 40mins, and temperature conditionss are 40 DEG C;
Step by step(2)The agitation grinding time be 1h;
Step by step(3)Temperature conditionss be 55 DEG C and ultrasonic disperse 15mins;
Step by step(4)Vacuum suction speed be 2 liters/second, control temperature be 70 DEG C.
In the step 2:
Step by step(1)Vacuum drying temperature be 60 DEG C, dry 24h;
Step by step(2)The agitation grinding time be 1h;
Step by step(3)Temperature adjustment be 55 DEG C and ultrasonic disperse 30mins;
Step by step(4)Vacuum suction speed be 2 liters/second, control temperature be 70-90 DEG C.
Present invention also offers a kind of composite heat interfacial material based on boron nitride, by the above-mentioned compound thermal based on boron nitride
Interface material producing method is made, and its component composition is in parts by weight:
10 ~ 50 parts of boron nitride,
30 ~ 225 parts of nano copper particle,
70 ~ 80 parts of epoxy resin,
5 ~ 15 parts of curing agent,
5 ~ 15 parts of diluent,
5 ~ 15 parts of coupling agent.
The epoxy resin is epoxy resin by using liquid crystal, is further 4,4 '-bigeminy phenol ester;
The curing agent is at least one of aromatic polyamine, acid anhydrides, imidazoles, polyamide curing agent, is preferably gathered
Amide resin;
The diluent is 660A type rings the third butane of oxygen;
The coupling agent is Z-6020 silane couplers or titanate coupling agent, preferably Z-6020 silane couplers;
The boron nitride is hexagonal boron nitride particles, and granular size is 0.1 ~ 50 μm, and shape can be sheet or spherical or both mixed
Close;
The average grain diameter of the nano copper particle is 100nm.
Compared with prior art, beneficial effect of the present invention:
1. by being modified processing to hexagonal boron nitride, the compatibility of boron nitride and matrix material is improved, can well be divided
It is dispersed in matrix material, reduction is gathered and produces high thermal resistance.
2. by adulterating hexagonal boron nitride into the composite of Nanometer Copper and epoxy resin, using nanometer copper particle solid
The molten condition occurred during change is connected between boron nitride layer to strengthen, and forms the Heat transmission approach of 3 D stereo network, is reduced multiple
Interface resistance inside condensation material.
Brief description of the drawings
Fig. 1 is the composite heat interfacial material preparation method flow chart of Nanometer Copper and epoxy resin;
Fig. 2 is the preparation method flow chart of the composite heat interfacial material based on boron nitride.
Embodiment
Below by the invention will be further described in conjunction with the accompanying drawings and embodiments, but it is not limitation of the present invention.
Fig. 1 to Fig. 2 shows a kind of composite heat interfacial material preparation method based on boron nitride, comprises the following steps:
Step 1, the composite heat interfacial material of Nanometer Copper and epoxy resin is prepared, it is specifically as follows step by step:
(1)Epoxy resin and curing agent are mixed to obtain mixed liquor;
(2)It will clean and dried nano copper particle is added in the mixed liquor, and add diluent agitation grinding;
(3)Add acetone and carry out ultrasonic disperse;
(4)Simultaneously vacuum defoamation obtains the composite heat interfacial material of Nanometer Copper and epoxy resin in 3 ~ 5 hours to heating stirring;
Step 2, the composite heat interfacial material based on boron nitride is prepared, it is specifically as follows step by step:
(1)Surface modification treatment is carried out to boron nitride using silane coupler and is dried in vacuo;
(2)Dried boron nitride is added in the composite heat interfacial material of the Nanometer Copper and epoxy resin, and add dilution
Agent agitation grinding obtains compound mixed liquor;
(3)Acetone and ultrasonic disperse are added in the compound mixed liquor;
(4)The compound mixed liquor after disperseing that will eliminate the noise is heated and is slowly stirred under vacuo, and vacuum defoamation 5-8 hours obtain
Composite heat interfacial material based on boron nitride.
In the step 1:
Step by step(1)The mixing time be 40mins, and temperature conditionss are 40 DEG C;
Step by step(2)The agitation grinding time be 1h;
Step by step(3)Temperature conditionss be 55 DEG C and ultrasonic disperse 15mins;
Step by step(4)Vacuum suction speed be 2 liters/second, control temperature be 70 DEG C;
In the step 2:
Step by step(1)Vacuum drying temperature be 60 DEG C, dry 24h;
Step by step(2)The agitation grinding time be 1h;
Step by step(3)Temperature adjustment be 55 DEG C and ultrasonic disperse 30mins;
Step by step(4)Vacuum suction speed be 2 liters/second, control temperature be 70-90 DEG C.
Embodiment 1:
In order that boron nitride can be better dispersed in epoxy resin, hexagonal boron nitride is entered using silane coupler Z-6020
Row surface is modified.Weigh necessarily dry boron nitride and be added to volume ratio as 1:3 concentrated sulfuric acid and the mixed solution of concentrated nitric acid, room
Ultrasonic cleaner is placed in after being well mixed under temperature and carries out ultrasonic disperse 8h, is then diluted, washs, drying, grinding, obtaining
Powder add solvent in dry toluene liquid, then to add appropriate silane coupler Z-6020, be placed in after well mixed
Ultrasonic disperse 1h at room temperature, then pass through cooling, absolute ethyl alcohol washing, deionized water washing, dry 24h.
100g epoxy resin and 1g polyamides curing agent 650 are mixed into 40min at 40 DEG C;To the copper after freezing
Nano particle unpacking is simultaneously dried in vacuo;The dried copper nano particles of 67.5g are added into above-mentioned epoxy curing agent
In mixing liquid, and add 0.5g epoxy propane butyl ether diluent agitation grindings 1h;250g is added in previous step mixed liquor
Acetone and in 55 DEG C of ultrasonic disperse 15min;Mixed liquor after ultrasonic disperse is put into de-airing mixer, regulation vacuum suction
Speed is 2 liters/second and to be heated to 70 DEG C, is slowly stirred and vacuum defoamation can be prepared into Nanometer Copper and epoxy resin for 5 hours
Composite.
Surface modification treatment is carried out to boron nitride and is dried in vacuo;The dried boron nitride of 0.5g is added on 100g
State in the Nanometer Copper/epoxy resin composite prepared, and add 0.5g epoxy propane butyl ether diluent agitation grindings 1h;
250g acetone is added in mixed liquor and in 55 DEG C of ultrasonic disperse 30min;Mixed liquor after ultrasonic disperse is put into de-airing mixer
In, regulation vacuum suction speed is 2 liters/second and is heated to 85 DEG C, is slowly stirred and vacuum defoamation can be prepared into and receive for 8 hours
The composite heat interfacial material based on boron nitride that rice copper mass share is 40%.
Embodiment 2:
In order that boron nitride can be better dispersed in epoxy resin, hexagonal boron nitride is entered using silane coupler Z-6020
Row surface is modified.Weigh necessarily dry boron nitride and be added to volume ratio as 1:3 concentrated sulfuric acid and the mixed solution of concentrated nitric acid, room
Ultrasonic cleaner is placed in after being well mixed under temperature and carries out ultrasonic disperse 8h, is then diluted, washs, drying, grinding, obtaining
Powder add solvent in dry toluene liquid, then to add appropriate silane coupler Z-6020, be placed in after well mixed
Ultrasonic disperse 1h at room temperature, then pass through cooling, absolute ethyl alcohol washing, deionized water washing, dry 24h.
100g epoxy resin and 2g polyamides curing agent 650 are mixed into 40min at 40 DEG C;To the copper after freezing
Nano particle unpacking is simultaneously dried in vacuo;The dried copper nano particles of 67.5g are added into above-mentioned epoxy curing agent
In mixing liquid, and add 2g epoxy propane butyl ether diluent agitation grindings 1h;350g third is added in previous step mixed liquor
Ketone and in 55 DEG C of ultrasonic disperse 15min;Mixed liquor after ultrasonic disperse is put into de-airing mixer, regulation vacuum suction speed
Rate is 2 liters/second and is heated to 70 DEG C, is slowly stirred and vacuum defoamation can be prepared into Nanometer Copper/epoxy resin composite wood for 5 hours
Material.
Surface modification treatment is carried out to boron nitride and is dried in vacuo;The dried boron nitride of 19g is added on 100g
State in the Nanometer Copper/epoxy resin composite prepared, and add 2g epoxy propane butyl ether diluent agitation grindings 1h;Mixed
Close and 250g acetone is added in liquid and in 55 DEG C of ultrasonic disperse 30min;Mixed liquor after ultrasonic disperse is put into de-airing mixer,
Regulation vacuum suction speed is 2 liters/second and is heated to 90 DEG C, is slowly stirred and vacuum defoamation can be prepared into boron nitride in 8 hours
Quality share is 10% composite heat interfacial material based on boron nitride.
The interface resistance of composite inner can be further reduced using technical scheme, is improved so as to overall
The heat conductivility of composite.
Embodiments of the present invention are made that with detailed description above in association with drawings and examples, but the present invention is not limited to
Described embodiment.To those skilled in the art, without departing from the principles and spirit of the present invention, it is right
These embodiments carry out various change, modification, replacement and modification and still fallen within protection scope of the present invention.
Claims (10)
- A kind of 1. composite heat interfacial material preparation method based on boron nitride, it is characterised in that:Comprise the following steps:Step 1, the composite heat interfacial material of Nanometer Copper and epoxy resin is prepared, it is specifically as follows step by step:(1)Epoxy resin and curing agent are mixed to obtain mixed liquor;(2)It will clean and dried nano copper particle is added in the mixed liquor, and add diluent agitation grinding;(3)Add acetone and carry out ultrasonic disperse;(4)Simultaneously vacuum defoamation obtains the composite heat interfacial material of Nanometer Copper and epoxy resin in 3 ~ 5 hours to heating stirring;Step 2, the composite heat interfacial material based on boron nitride is prepared, it is specifically as follows step by step:(1)Surface modification treatment is carried out to boron nitride using silane coupler and is dried in vacuo;(2)Dried boron nitride is added in the composite heat interfacial material of the Nanometer Copper and epoxy resin, and add dilution Agent agitation grinding obtains compound mixed liquor;(3)Acetone and ultrasonic disperse are added in the compound mixed liquor;(4)The compound mixed liquor after disperseing that will eliminate the noise is heated and is slowly stirred under vacuo, and vacuum defoamation 5-8 hours obtain Composite heat interfacial material based on boron nitride.
- 2. the composite heat interfacial material preparation method according to claim 1 based on boron nitride, it is characterised in that:The step In rapid one:Step by step(1)The mixing time be 40mins, and temperature conditionss are 40 DEG C;Step by step(2)The agitation grinding time be 1h;Step by step(3)Temperature conditionss be 55 DEG C and ultrasonic disperse 15mins;Step by step(4)Vacuum suction speed be 2 liters/second, control temperature be 70 DEG C.
- 3. the composite heat interfacial material preparation method according to claim 1 based on boron nitride, it is characterised in that:The step In rapid two:Step by step(1)Vacuum drying temperature be 60 DEG C, dry 24h;Step by step(2)The agitation grinding time be 1h;Step by step(3)Temperature adjustment be 55 DEG C and ultrasonic disperse 30mins;Step by step(4)Vacuum suction speed be 2 liters/second, control temperature be 70-90 DEG C.
- 4. it is based on boron nitride made of a kind of composite heat interfacial material preparation method based on boron nitride as described in claim 1 Composite heat interfacial material, it is characterised in that:Its component forms:10 ~ 50 parts of boron nitride,30 ~ 225 parts of nano copper particle,70 ~ 80 parts of epoxy resin,5 ~ 15 parts of curing agent,5 ~ 15 parts of diluent,5 ~ 15 parts of coupling agent.
- 5. the composite heat interfacial material according to claim 4 based on boron nitride, it is characterised in that:The epoxy resin is Epoxy resin by using liquid crystal, it is further 4,4 '-bigeminy phenol ester.
- 6. the composite heat interfacial material according to claim 4 based on boron nitride, it is characterised in that:The curing agent is virtue At least one of fragrant race's polyamines, acid anhydrides, imidazoles, polyamide curing agent, preferably polyamide.
- 7. the composite heat interfacial material according to claim 4 based on boron nitride, it is characterised in that:The diluent is 660A type rings the third butane of oxygen.
- 8. the composite heat interfacial material according to claim 4 based on boron nitride, it is characterised in that:The coupling agent is Z- 6020 silane couplers or titanate coupling agent, preferably Z-6020 silane couplers.
- 9. the composite heat interfacial material based on boron nitride according to any one of claim 4 to 8, it is characterised in that:It is described Boron nitride is hexagonal boron nitride particles, and granular size is 0.1 ~ 50 μm, and shape can be sheet or spherical or both mixing.
- 10. the composite heat interfacial material based on boron nitride according to any one of claim 4 to 8, it is characterised in that:It is described The average grain diameter of nano copper particle is 100nm.
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Cited By (6)
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CN108503890A (en) * | 2018-04-12 | 2018-09-07 | 中国科学院理化技术研究所 | The preparation method of organosilicon functionalization boron nitride nanosheet |
CN109021202A (en) * | 2018-08-16 | 2018-12-18 | 德清舒华泡沫座椅有限公司 | A kind of high-strength polyurethane foam |
CN109181301A (en) * | 2018-07-21 | 2019-01-11 | 上海大学 | A kind of doped quantum dot functionalization boron nitride polymer bond composite membrane and preparation method |
CN111892749A (en) * | 2020-07-03 | 2020-11-06 | 浙江荣泰科技企业有限公司 | Boron nitride high-thermal-conductivity insulating filler with imidazole-copper complex adsorbed on surface, insulating and heat-dissipating epoxy resin composition and preparation method thereof |
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 |
CN115748244A (en) * | 2022-11-07 | 2023-03-07 | 哈尔滨工业大学 | High-interface bonding sizing agent, preparation thereof, modified carbon fiber reinforced polyether-ether-ketone composite material based on sizing agent and preparation method of modified carbon fiber reinforced polyether-ether-ketone composite material |
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CN108503890A (en) * | 2018-04-12 | 2018-09-07 | 中国科学院理化技术研究所 | The preparation method of organosilicon functionalization boron nitride nanosheet |
CN109181301A (en) * | 2018-07-21 | 2019-01-11 | 上海大学 | A kind of doped quantum dot functionalization boron nitride polymer bond composite membrane and preparation method |
CN109181301B (en) * | 2018-07-21 | 2021-01-01 | 上海大学 | Quantum dot doped functionalized boron nitride polymer heat conduction composite film and preparation method thereof |
CN109021202A (en) * | 2018-08-16 | 2018-12-18 | 德清舒华泡沫座椅有限公司 | A kind of high-strength polyurethane foam |
CN111892749A (en) * | 2020-07-03 | 2020-11-06 | 浙江荣泰科技企业有限公司 | Boron nitride high-thermal-conductivity insulating filler with imidazole-copper complex adsorbed on surface, insulating and heat-dissipating epoxy resin composition and preparation method thereof |
CN111892749B (en) * | 2020-07-03 | 2022-03-22 | 浙江荣泰科技企业有限公司 | Boron nitride high-thermal-conductivity insulating filler with imidazole-copper complex adsorbed on surface, insulating and heat-dissipating epoxy resin composition and preparation method thereof |
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 |
CN115748244A (en) * | 2022-11-07 | 2023-03-07 | 哈尔滨工业大学 | High-interface bonding sizing agent, preparation thereof, modified carbon fiber reinforced polyether-ether-ketone composite material based on sizing agent and preparation method of modified carbon fiber reinforced polyether-ether-ketone composite material |
CN115748244B (en) * | 2022-11-07 | 2024-04-12 | 哈尔滨工业大学 | High-interface bonding sizing agent, preparation thereof, modified carbon fiber reinforced polyether-ether-ketone composite material based on high-interface bonding sizing agent and preparation method of modified carbon fiber reinforced polyether-ether-ketone composite material |
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