CN103409094A - Composite glue made from micro-, nano-filler and epoxy resin, and preparation method and applications thereof - Google Patents
Composite glue made from micro-, nano-filler and epoxy resin, and preparation method and applications thereof Download PDFInfo
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- CN103409094A CN103409094A CN2013103116062A CN201310311606A CN103409094A CN 103409094 A CN103409094 A CN 103409094A CN 2013103116062 A CN2013103116062 A CN 2013103116062A CN 201310311606 A CN201310311606 A CN 201310311606A CN 103409094 A CN103409094 A CN 103409094A
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Abstract
The invention belongs to the field of polymer composite materials, and more specifically relates to a composite glue made from a micro-, nano-filler and epoxy resin, and a preparation method and applications thereof. The composite glue comprises, by weight, 15 to 30 portions of liquid epoxy resin, 2 to 5 portions of a flexibilizer, 1 to 8 portions of a curing agent, 0.2 to 0.4 portion of a curing accelerator, 15 to 35 portions of an inorganic micro-filler with high thermal conductivity, 15 to 35 portions of an inorganic nano-filler with high thermal conductivity and 10 to 40 portions of an organic solvent. The micro-, nano-filler and epoxy resin are combined, a special interface interphase is formed, and the microscopic structure and compactness of the insulating composite glue with high thermal conductivity are improved and increased greatly, so that the thermal conductivity of the composite glue is much higher than that of traditional interlayer materials, and the composite glue is suitable for production of thermal conductive aluminium-based copper-clad plates used for LED heat-dissipation substrates. In addition, dimension of the composite glue is stable, electromagnetic shielding performance is excellent, and mechanical strength and smoothness are high.
Description
Technical field
The present invention relates to the polymer composite field, specifically relate to a kind of micro-, Nano filling-epoxy resin composite gum, preparation method and application thereof.
Background technology
LED is as a kind of photodiode, and very natural will be encapsulated on certain wiring board, and the performance quality of wiring board has a significant impact the efficient performance of LED performance.LED is as a kind of luminescent material, and nature can produce certain heat in luminescence process, and wherein only having the electric energy conversion of 15-25% left and right is luminous energy, and remaining electric energy nearly all is converted into heat exhaustion and falls, and meanwhile, the LED device heats up will affect work quality.
The Copper Foil of LED by the aluminum-based copper-clad plate surface be welded on aluminum-based copper-clad plate conducts heat to middle dielectric layer, then heat passes to aluminium sheet by middle dielectric layer, heat just can be dissipated in air ambient like this, impels LED cooling in certain temperature, and performance has proposed excellent performance.This LED-based aluminum-based copper-clad plate has but proposed very high requirement to the material of middle medium layer, requires the over-all propertieies such as this intermediate medium layer material has good thermal diffusivity, dimensional stabilizing, electromagnetic wave shielding is good, physical strength is high, high planarization.And traditional copper-clad plate technology is subject to new challenge, can't meet this requirement.Therefore, the LED heat-radiating substrate thermal conductivity aluminum matrix copper-clad plate of adopting which kind of intermediate medium layer material to produce to have high thermal conductivity, will become the research and development focus of novel material.
Summary of the invention
One of purpose of the present invention is to provide a kind of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum, microstructure and the compactness of this high heat conductive insulating composite gum have all obtained significantly and have improved, therefore, its heat conductivility is obviously excellent in traditional intermediate medium layer material.
To achieve these goals, the technical solution adopted in the present invention is: a kind of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum, include epoxy resin, and according to weight part, made by following component:
15～30 parts of liquid-state epoxy resins;
2～5 parts of toughner;
1～8 part, solidifying agent;
0.2～0.4 part of solidifying agent promotor;
15～35 parts of high heat conduction micron mineral fillers;
15～35 parts of high heat conducting nano mineral fillers;
10～40 parts of organic solvents;
Wherein, described liquid-state epoxy resin is E-51 epoxy resin and/or E-44 epoxy resin;
Described toughner is polyvinyl butyral acetal;
Described solidifying agent is 4,4-diaminodiphenylsulfone(DDS), 3, the mixture of one or more in 3-diaminodiphenylsulfone(DDS) and diphenylmethanediamiand;
Described solidifying agent promotor is one or more the mixture in glyoxal ethyline, 1-Methylimidazole and 2-ethyl-4-methylimidazole;
The mineral filler of described high heat conduction micron is one or more the mixture in micron order aluminum oxide, micron order aluminium nitride and micron order silicon carbide;
Described high heat conducting nano mineral filler is one or more the mixture in alumina in Nano level, nano level aluminium nitride and nanometer silicon carbide;
Described organic solvent is one or more the mixture in acetone, 2-butanone, positive acetone, toluene, ethyl acetate and N,N-DIMETHYLACETAMIDE.
Further, the median size of described high heat conduction micron mineral filler is 0.4～2.0 μ m, and the median size of described high heat conducting nano mineral filler is 30～60nm.
Micro-, Nano filling-epoxy resin high heat conductive insulating composite gum of the present invention, the heat conductive filler of micro-, nanometer is compound with rational volume ratio and suitable technique and epoxy resin, formed phase in the middle of special interface, microstructure and the compactness of the high heat conductive insulating composite gum of preparation have all obtained significantly and have improved, therefore, its heat conductivility is obviously excellent in traditional intermediate medium layer material.The over-all propertieies such as in addition, this is micro-, Nano filling-epoxy resin high heat conductive insulating composite gum also has dimensional stabilizing, electromagnetic wave shielding is good, physical strength is high, high planarization.
As another object of the present invention, the invention provides that this is micro-, the preparation method of Nano filling-epoxy resin high heat conductive insulating composite gum, comprise the steps:
1., the mineral filler of high heat conduction micron, high heat conducting nano mineral filler and organic solvent are mixed, disperse 30～60min in the ultrasonic dispersion machine of packing into, filter through 300 mesh filter screens;
2., add liquid-state epoxy resin, toughner, solidifying agent and solidifying agent promotor, be uniformly mixed 2～4h, make micro-, Nano filling-epoxy resin high heat conductive insulating composite gum.
The preparation method of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum of the present invention, its technique is comparatively simple, and raw material is cheap and easy to get, is applicable to suitability for industrialized production, and production efficiency is high.
As another purpose of the present invention, the invention provides a kind of LED heat-radiating substrate thermal conductivity aluminum matrix copper-clad plate, it consists of Copper Foil and aluminium foil, bonding by micro-, Nano filling-epoxy resin high heat conductive insulating composite gum between Copper Foil and aluminium foil.
Preferably, this LED heat-radiating substrate is 30～250 μ m with the film thickness of micro-in the thermal conductivity aluminum matrix copper-clad plate, Nano filling-epoxy resin high heat conductive insulating composite gum.
LED heat-radiating substrate thermal conductivity aluminum matrix copper-clad plate of the present invention, by scientific and reasonable design middle dielectric layer, namely select micro-, Nano filling-epoxy resin high heat conductive insulating composite gum as middle dielectric layer, thereby realize heat is transmitted to aluminium sheet from Copper Foil fast, by aluminium sheet, it is scattered and disappeared to environment again, thereby impel LED cooling in certain temperature.Therefore, the LED heat-radiating substrate is high with the heat transfer efficiency of thermal conductivity aluminum matrix copper-clad plate, can significantly improve the work-ing life of LED light fixture.
As four of purpose of the present invention, the invention provides the production technique of this LED heat-radiating substrate with the thermal conductivity aluminum matrix copper-clad plate, micro-, Nano filling-epoxy resin high heat conductive insulating composite gum directly is coated in to copper foil surface, then at the surface with glue clad aluminum foil of Copper Foil, process and get final product by hot-forming, hot setting.
Further, it is successively through 100 ℃, 120 ℃ and 150 ℃ of three temperature control sections that described hot-forming, hot setting is processed, and the hot pressing pressure of three temperature control sections is 5～10MPa, and the treatment time is 60～120min.
The LED heat-radiating substrate of the present invention production technique of thermal conductivity aluminum matrix copper-clad plate, operation is comparatively succinct, and production cost is low, and working (machining) efficiency is high.
Embodiment
The present invention is further illustrated below in conjunction with embodiment, but the present invention is not limited only to these embodiment, do not breaking away under the prerequisite of aim of the present invention, within any improvement of doing all drops on protection scope of the present invention.
Embodiment 1
The preparation of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum:
1., by 15 parts of median sizes aluminum oxide that is 0.4 μ m, 25 parts of median sizes, being 40nm, silicon carbide and 39.75 parts of acetone mix, and disperse 30min in the ultrasonic dispersion machine of packing into, through 300 mesh filter screens, filter a small amount of impurity of filtering;
2., to adding 15 parts of E-44 epoxy resin, 4 parts of polyvinyl butyral acetals, 1 part 3 in filtrate, 3-diaminodiphenylsulfone(DDS) and 0.25 part of 2-ethyl-4-methylimidazole, be uniformly mixed 4h, makes micro-, Nano filling-epoxy resin high heat conductive insulating composite gum.
Embodiment 2
The preparation of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum:
1., by 35 parts of median sizes silicon carbide that is 2.0 μ m, 15 parts of median sizes, being 30nm, silicon carbide and 14.7 parts of 2-butanone mix, and disperse 40min in the ultrasonic dispersion machine of packing into, through 300 mesh filter screens, filter a small amount of impurity of filtering;
2., add 22 parts of E-44 epoxy resin, 5 parts of polyvinyl butyral acetals, 8 parts of diphenylmethanediamiands and 0.3 part of 1-Methylimidazole in filtrate, be uniformly mixed 2.5h, make micro-, Nano filling-epoxy resin high heat conductive insulating composite gum.
Embodiment 3
The preparation of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum:
1., by 20 parts of median sizes aluminium nitride that is 1 μ m, 20 parts of median sizes, being 50nm, aluminium nitride and 23.8 parts of ethyl acetate are mixed, and disperse 45min in the ultrasonic dispersion machine of packing into, through 300 mesh filter screens, filter a small amount of impurity of filtering;
2., to adding 27 parts of E-51 epoxy resin, 2 parts of polyvinyl butyral acetals, 7 part 4 in filtrate, 4-diaminodiphenylsulfone(DDS) and 0.2 part of methylimidazole, be uniformly mixed 3h, makes micro-, Nano filling-epoxy resin high heat conductive insulating composite gum.
Embodiment 4
The preparation of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum:
1., by 10 parts of median sizes aluminium nitride that is 1 μ m, 30 parts of median sizes, being 50nm, aluminium nitride and 23.8 parts of ethyl acetate are mixed, and disperse 45min in the ultrasonic dispersion machine of packing into, through 300 mesh filter screens, filter a small amount of impurity of filtering;
2., to adding 27 parts of E-51 epoxy resin, 2 parts of polyvinyl butyral acetals, 7 part 4 in filtrate, 4-diaminodiphenylsulfone(DDS) and 0.2 part of methylimidazole, be uniformly mixed 3h, makes micro-, Nano filling-epoxy resin high heat conductive insulating composite gum.
Embodiment 5
The preparation of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum:
1., by 25 parts of median sizes aluminium nitride that is 1.5 μ m, 15 parts of median sizes, being 60nm, aluminum oxide and 22.6 parts of N,N-DIMETHYLACETAMIDEs mix, and disperse 60min in the ultrasonic dispersion machine of packing into, through 300 mesh filter screens, filter a small amount of impurity of filtering;
2., in filtrate, add 15 parts of E-44 epoxy resin, 15 parts of E-51 epoxy resin, 3 parts of polyvinyl butyral acetals, 4 parts of diphenylmethanediamiands and 0.4 part of 1-Methylimidazole, be uniformly mixed 2h, make micro-, Nano filling-epoxy resin high heat conductive insulating composite gum.
Embodiment 6
Micro-, the Nano filling-epoxy resin high heat conductive insulating composite gum of embodiment 1～5 preparation are applied to respectively to the production of LED heat-radiating substrate with the thermal conductivity aluminum matrix copper-clad plate.
The LED heat-radiating substrate by the production technique of thermal conductivity aluminum matrix copper-clad plate is: micro-, Nano filling-epoxy resin high heat conductive insulating composite gum directly is coated in to copper foil surface, then, at the surface with glue clad aluminum foil of Copper Foil, processes and get final product by hot-forming, hot setting.It is successively through 100 ℃, 120 ℃ and 150 ℃ of three temperature control sections that hot-forming, hot setting is processed, and the hot pressing pressure of three temperature control sections is respectively 5MPa, 7MPa, 10MPa, and the treatment time is respectively 60min, 80min, 120min.
The LED heat-radiating substrate is with the film thickness of composite gum in the thermal conductivity aluminum matrix copper-clad plate, the performance test of thermal conductivity aluminum matrix copper-clad plate, in Table 1.
The performance test table of table 1 composite gum film thickness, thermal conductivity aluminum matrix copper-clad plate
From data table 1, can find out that composite gum film thickness of the present invention is controlled, it is high that the aluminum-based copper-clad plate thermal conductivity is high, voltage is worn in resistance, can be used as the aluminum-based copper-clad plate that the LED heat-radiating substrate is used.
Claims (7)
1. micro-, Nano filling-epoxy resin high heat conductive insulating composite gum, include epoxy resin, it is characterized in that this high heat conductive insulating composite gum made by following component according to weight part:
Wherein, described liquid-state epoxy resin is E-51 epoxy resin and/or E-44 epoxy resin;
Described toughner is polyvinyl butyral acetal;
Described solidifying agent is 4,4-diaminodiphenylsulfone(DDS), 3, the mixture of one or more in 3-diaminodiphenylsulfone(DDS) and diphenylmethanediamiand;
Described solidifying agent promotor is one or more the mixture in glyoxal ethyline, 1-Methylimidazole and 2-ethyl-4-methylimidazole;
The mineral filler of described high heat conduction micron is one or more the mixture in micron order aluminum oxide, micron order aluminium nitride and micron order silicon carbide;
Described high heat conducting nano mineral filler is one or more the mixture in alumina in Nano level, nano level aluminium nitride and nanometer silicon carbide;
Described organic solvent is one or more the mixture in acetone, 2-butanone, positive acetone, toluene, ethyl acetate and N,N-DIMETHYLACETAMIDE.
2. micro-, Nano filling-epoxy resin high heat conductive insulating composite gum according to claim 1, it is characterized in that: the median size of described high heat conduction micron mineral filler is 0.4～2.0 μ m, and the median size of described high heat conducting nano mineral filler is 30～60nm.
3. the preparation method of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum as claimed in claim 1 or 2, is characterized in that comprising the steps:
1., the mineral filler of high heat conduction micron, high heat conducting nano mineral filler and organic solvent are mixed, disperse 30～60min in the ultrasonic dispersion machine of packing into, filter through 300 mesh filter screens;
2., add liquid-state epoxy resin, toughner, solidifying agent and solidifying agent promotor, be uniformly mixed 2～4h, make micro-, Nano filling-epoxy resin high heat conductive insulating composite gum.
4. one kind contains the LED heat-radiating substrate thermal conductivity aluminum matrix copper-clad plate of micro-, Nano filling-epoxy resin high heat conductive insulating composite gum as claimed in claim 1 or 2, by Copper Foil and aluminium foil, formed, it is characterized in that: be bonding by micro-, Nano filling-epoxy resin high heat conductive insulating composite gum between described Copper Foil and aluminium foil.
5. LED heat-radiating substrate thermal conductivity aluminum matrix copper-clad plate according to claim 4 is characterized in that: this LED heat-radiating substrate is 30～250 μ m with the film thickness of micro-in the thermal conductivity aluminum matrix copper-clad plate, Nano filling-epoxy resin high heat conductive insulating composite gum.
6. one kind as the production technique of LED heat-radiating substrate as described in claim 4 or 5 with the thermal conductivity aluminum matrix copper-clad plate, it is characterized in that: micro-, Nano filling-epoxy resin high heat conductive insulating composite gum directly is coated in to copper foil surface, then at the surface with glue clad aluminum foil of Copper Foil, process and get final product by hot-forming, hot setting.
7. production technique according to claim 6, it is characterized in that: it is successively through 100 ℃, 120 ℃ and 150 ℃ of three temperature control sections that described hot-forming, hot setting is processed, and the hot pressing pressure of three temperature control sections is 5～10MPa, and the treatment time is 60～120min.
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| CN2013103116062A CN103409094A (en) | 2013-07-23 | 2013-07-23 | Composite glue made from micro-, nano-filler and epoxy resin, and preparation method and applications thereof |
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| CN2013103116062A CN103409094A (en) | 2013-07-23 | 2013-07-23 | Composite glue made from micro-, nano-filler and epoxy resin, and preparation method and applications thereof |
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| CN103773298A (en) * | 2014-01-24 | 2014-05-07 | 临安金奥科技有限公司 | High thermal-conductive and insulating adhesive for high-power LED lamp and preparation method thereof |
| CN104262901A (en) * | 2014-08-28 | 2015-01-07 | 广东狮能电气股份有限公司 | Epoxy resin material with nano aluminum nitride filler and manufacturing method thereof |
| CN104486938A (en) * | 2015-01-04 | 2015-04-01 | 东莞市威力固电路板设备有限公司 | Method for preparing water cooling plate |
| CN104497785A (en) * | 2014-11-25 | 2015-04-08 | 浙江大学自贡创新中心 | Preparation method for nanometer modified resin composite paint used for LED base plate |
| CN104610701A (en) * | 2015-01-14 | 2015-05-13 | 景旺电子科技(龙川)有限公司 | Insulating layer material, stainless steel based copper clad plate, surface treatment method and preparation method |
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| WO2016090859A1 (en) * | 2014-12-11 | 2016-06-16 | 广东生益科技股份有限公司 | Thermosetting resin composition for degradable heat-conducting aluminum-based copper-clad plate, heat-conducting aluminum-based copper-clad plate, and preparation method and recovery method thereof |
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| CN108410134A (en) * | 2018-03-29 | 2018-08-17 | 苏州银禧新能源复合材料有限公司 | A kind of fibrous composite composition epoxy resin and its application |
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| CN113372688A (en) * | 2021-07-28 | 2021-09-10 | 海南必凯水性新材料有限公司 | Modified epoxy resin and preparation method thereof |
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| CN103773298A (en) * | 2014-01-24 | 2014-05-07 | 临安金奥科技有限公司 | High thermal-conductive and insulating adhesive for high-power LED lamp and preparation method thereof |
| CN104262901A (en) * | 2014-08-28 | 2015-01-07 | 广东狮能电气股份有限公司 | Epoxy resin material with nano aluminum nitride filler and manufacturing method thereof |
| CN104497785A (en) * | 2014-11-25 | 2015-04-08 | 浙江大学自贡创新中心 | Preparation method for nanometer modified resin composite paint used for LED base plate |
| WO2016090859A1 (en) * | 2014-12-11 | 2016-06-16 | 广东生益科技股份有限公司 | Thermosetting resin composition for degradable heat-conducting aluminum-based copper-clad plate, heat-conducting aluminum-based copper-clad plate, and preparation method and recovery method thereof |
| CN104486938A (en) * | 2015-01-04 | 2015-04-01 | 东莞市威力固电路板设备有限公司 | Method for preparing water cooling plate |
| CN104610701A (en) * | 2015-01-14 | 2015-05-13 | 景旺电子科技(龙川)有限公司 | Insulating layer material, stainless steel based copper clad plate, surface treatment method and preparation method |
| CN104610701B (en) * | 2015-01-14 | 2017-08-25 | 景旺电子科技(龙川)有限公司 | Insulating layer material, stainless base steel copper-clad plate, surface treatment method and preparation method |
| CN104761831B (en) * | 2015-04-10 | 2017-10-27 | 安徽华能电缆集团有限公司 | The nuclear power cable Insulation Material and preparation method of EP rubbers based on micro-nano filler |
| CN104761832A (en) * | 2015-04-10 | 2015-07-08 | 安徽华能电缆集团有限公司 | Mesoporous silica nano-composite nuclear cable insulation material and preparation method |
| CN104761832B (en) * | 2015-04-10 | 2017-10-13 | 安徽华能电缆集团有限公司 | A kind of mesoporous silicon dioxide nano is combined nuclear power cable Insulation Material and preparation method |
| CN104761831A (en) * | 2015-04-10 | 2015-07-08 | 安徽华能电缆集团有限公司 | Micro-nano filler based ethylene propylene rubber nuclear cable insulation material and preparation method |
| CN107418146A (en) * | 2017-07-25 | 2017-12-01 | 南方电网科学研究院有限责任公司 | Insulator material, insulator and preparation method |
| CN107418146B (en) * | 2017-07-25 | 2020-02-18 | 南方电网科学研究院有限责任公司 | Insulator material, insulator and preparation method |
| CN108410134A (en) * | 2018-03-29 | 2018-08-17 | 苏州银禧新能源复合材料有限公司 | A kind of fibrous composite composition epoxy resin and its application |
| CN111534016A (en) * | 2020-06-01 | 2020-08-14 | 中国科学院合肥物质科学研究院 | Electronic packaging material with heat conduction and electromagnetic shielding performance and preparation method thereof |
| CN111534016B (en) * | 2020-06-01 | 2023-03-21 | 中国科学院合肥物质科学研究院 | Electronic packaging material with heat conduction and electromagnetic shielding performance and preparation method thereof |
| CN111777840A (en) * | 2020-07-14 | 2020-10-16 | 浙江大学 | Epoxy resin micro-nano blending composite material for packaging power electronic high-power device and preparation method thereof |
| CN113372688A (en) * | 2021-07-28 | 2021-09-10 | 海南必凯水性新材料有限公司 | Modified epoxy resin and preparation method thereof |
| CN115403928A (en) * | 2022-08-01 | 2022-11-29 | 中国科学院合肥物质科学研究院 | Electronic packaging material with heat-conducting electromagnetic shielding performance and preparation method thereof |
| CN115403928B (en) * | 2022-08-01 | 2023-05-30 | 中国科学院合肥物质科学研究院 | Electronic packaging material with heat conduction electromagnetic shielding performance and preparation method thereof |
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Application publication date: 20131127 |