CN105061994A - Preparation method for epoxy resin composite casting material with high thermal conductivity for LED (light-emitting diode) - Google Patents

Preparation method for epoxy resin composite casting material with high thermal conductivity for LED (light-emitting diode) Download PDF

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CN105061994A
CN105061994A CN201510443642.3A CN201510443642A CN105061994A CN 105061994 A CN105061994 A CN 105061994A CN 201510443642 A CN201510443642 A CN 201510443642A CN 105061994 A CN105061994 A CN 105061994A
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epoxy resin
minutes
casting material
thermal conductivity
composite casting
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CN105061994B (en
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徐旭
虞锦洪
陆绍荣
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Guilin University of Technology
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Guilin University of Technology
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Abstract

The invention discloses a preparation method for epoxy resin composite casting material with high thermal conductivity for a LED (light-emitting diode). The preparation method comprises: weighing raw materials comprising liquid epoxy resin, a curing agent and a modified mixed filler in a mass ratio of 100 to (13-15) to (300-400); adding the weighed liquid epoxy resin into a thin-layer defoaming kettle, starring to stir the liquid epoxy resin, pre-heating the liquid epoxy resin for 20 minutes while rising the temperature to 60 DEG C; then, adding weighed modified fixed filler, defoaming under reduced pressure after uniformly stirring the modified fixed filler, defoaming under a condition with 100-200 Pa until no gas bubbles are released, standing and cooling to the room temperature and keeping the room temperature for 30 minutes, and then, starting to stir; adding the weighed curing agent, uniformly stirring at the room temperature, and defoaming for 10 minutes under reduced pressure, then, discharging, thereby preparing the epoxy resin composite casting material with high thermal conductivity for the LED. The preparation method is easy to operate and low in manufacturing cost; by virtue of low-temperature curing, the energy consumption is greatly reduced; and after being formed, the prepared composite casting material with high thermal conductivity has a higher thermal conductivity coefficient, shock strength, a coefficient of linear expansion and ageing resistance.

Description

A kind of preparation method of LED high-thermal-conductivity epoxy resin composite casting material
Technical field
The invention belongs to technical field of composite preparation, particularly a kind of preparation method of LED high-thermal-conductivity epoxy resin composite casting material.
Background technology
Under the tide that Contemporary Environmental protection and Sustainable development require, electronic machine and equipment are day by day ultralight, thin, and towards the development of short, little aspect, but under high operate frequency, electronic devices and components are rapidly to high temperature direction and move.Now, the heat run-up that electronic devices and components produce, increase, electronic devices and components be made still normally to work with high reliability, and the ability of timely distribute heat becomes the key and limiting factor thereof that affect its work-ing life.For ensureing components and parts safe operations, being badly in need of adopting highly heat-conductive material to distribute the amount of heat produced in unicircuit, making electronic devices and components at a suitable temperature can steady operation.
Description of materials at present for Electronic Packaging is a lot, can be divided into metal matrix, plastic base and ceramic base packaged material from material composition.Plastic base packaged material is because of advantages such as cost is low, technique is simple, quality is light, good insulation preformances, and in electronic package material, consumption is maximum, with fastest developing speed.The material that plastic package uses mainly thermosetting resin, comprise phenolic, unsaturated polyester class, epoxies etc., its epoxy resin is because having excellent resistance toheat, adhesiveproperties, electrical insulation capability, chemically-resistant, corrosion resistance nature and mechanical property, moulding process is simple, series of advantages such as curing molding shrinking percentage is low and become most widely used general, one of packaged material that prospect is the most wide.
Plastics replace traditional aluminium and are used as the inexorable trend that LED illumination radiator shell has become current environment protection and Sustainable development requirement.Heat-conducting polymer material is ground zero at home, domestic thermally conductive material is no matter all difficult from performance, kind to contend with inlet guide hot material, and factor hinders the generally application of thermally conductive material on LED illumination scatterer because production technology level is lower, production cost is high etc.In order to develop efficient, low cost heat conduction engineering materials as early as possible, meet the megatrend of LED illumination development need, the highly thermally conductive polymeric that preparation has excellent combination property is extremely urgent.But macromolecular material be all generally heat poor conductor, its thermal conductivity 25 DEG C time all lower than 0.50W/ (mK), as epoxy resin only has 0.20W/ (mK).In order to meet the growth requirement of the industries such as electrical equipment encapsulation, LED, overcome the shortcoming and defect of prior art and performance, the highly thermally conductive polymeric that preparation has excellent combination property is object of the present invention.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of preparation method of LED high-thermal-conductivity epoxy resin composite casting material is provided.
For solving the problems of the technologies described above, the present invention improves the thermal conductivity of mould material as the method for filler by adopt high heat conduction inorganic powder to substitute silicon powder that prior art uses.In order to eliminate high heat conduction inorganic powder due to the comparatively large phenomenon that sedimentation easily occurs of density ratio, the present invention takes technical measures: one is select silane coupler modified filler, strengthens the reactive force between inorganic powder and matrix resin molecule; Two is add the mechanical property that carbon fiber improves matrix material; Three be optimize the formula of mould material and mixed glue deaeration technique, controls material viscosity larger as far as possible in exercisable scope, reduce material internal air gap amount further.
Concrete steps are:
(1) raw material is taken according to following mass ratio, liquid epoxies: solidifying agent: modification mixed fillers=100:13 ~ 15:300 ~ 400.
(2) liquid epoxies step (1) taken drops in thin layer deaeration still, start stirring, preheating 20 minutes when being warming up to 60 DEG C, then the modification mixed fillers that step (1) takes is dropped into, vacuum deaerator after stirring, under 100 ~ 200Pa condition, deaeration is to bubble-free is released, leave standstill and be cooled to after room temperature keeps 30 minutes, start stirring, add the solidifying agent that step (1) takes, stirring at room temperature is rear vacuum deaerator discharging after 10 minutes evenly, i.e. obtained LED high-thermal-conductivity epoxy resin composite casting material.
Described liquid epoxies is one or more in bisphenol A type epoxy resin, bisphenol f type epoxy resin, aliphatic epoxy resin and cycloaliphatic epoxy resin.
Described solidifying agent is tetraethylene pentamine.
Described modification mixed fillers is prepared according to the following steps:
1 mass parts aluminum oxide powder and 7 mass parts carbon fiber mixed fillers are dropped in reaction vessel after dry 10 hours at 100 DEG C, add the silane coupling agent of 5wt% mixed fillers and the dehydrated alcohol of silane coupling agent consumption 10 times again, 60 DEG C are warming up to after mixing and stirring, ultrasonication 20 minutes, by washing with alcohol 1 time, then ultrasonication 10 minutes, use washing with alcohol again 1 time, 30 minutes are left standstill, finally under 80 DEG C of vacuum dry 14 hours, i.e. obtained modification mixed fillers after suction filtration; Wherein aluminum oxide powder is 200 orders, and the diameter of carbon fiber is 7um, and length is 4mm, density 1.76g/cm 3.
The present invention has the following advantages:
(1) preparation method's processing ease of the present invention, low cost of manufacture, equipment is simple, and low-temperature curing, greatly reduce power consumption.
(2) after the high heat conduction composite casting material that the inventive method is obtained is shaping, there is good thermal conductivity, resistance to impact shock, linear expansivity and resistance to deterioration.
Embodiment
embodiment:
(1) raw material is taken according to following quality, liquid epoxies 100kg, solidifying agent 14kg, modification mixed fillers 300kg.
(2) liquid epoxies step (1) taken drops in thin layer deaeration still, start stirring, preheating 20 minutes when being warming up to 60 DEG C, then the modification mixed fillers that step (1) takes is dropped into, vacuum deaerator after stirring, under 150Pa condition, deaeration is to still releasing, leave standstill and be cooled to after room temperature keeps 30 minutes, start stirring, add the solidifying agent that step (1) takes, stirring at room temperature is rear vacuum deaerator discharging after 10 minutes evenly, i.e. obtained LED high-thermal-conductivity epoxy resin composite casting material.
Described liquid epoxies is bisphenol A type epoxy resin (EPON828).
Described solidifying agent is tetraethylene pentamine.
Described modification mixed fillers is prepared according to the following steps:
60kg aluminum oxide powder and 420kg carbon fiber mixed fillers are dropped in reaction vessel after dry 10 hours at 100 DEG C, add 24kg silane coupling agent and 240kg dehydrated alcohol again, 60 DEG C are warming up to after mixing and stirring, ultrasonication 20 minutes, by washing with alcohol 1 time, then ultrasonication 10 minutes, use washing with alcohol again 1 time, 30 minutes are left standstill, finally under 80 DEG C of vacuum dry 14 hours, i.e. obtained modification mixed fillers after suction filtration; Wherein aluminum oxide powder is 200 orders, and the diameter of carbon fiber is 7um, and length is 4mm, density 1.76g/cm 3.
By composite casting material obtained for the present embodiment 35 DEG C of Procuring 24 hours, 70 DEG C of after fixing 2 hours, the thermal conductivity of gained cured article is 1.35w/(mk); Workpiece top density 2.433g/cm 3, workpiece bottom density is 2.458g/cm 3; Shock strength is 17kJ/m 2; Flexural strength 140MPa; Breaking down field strength is 29kv/cm 3; Linear expansivity is 43x10 -6k -1, all comparatively excellent, be enough to meet LED and build part use.

Claims (1)

1. a LED preparation method for high-thermal-conductivity epoxy resin composite casting material, is characterized in that concrete steps are:
(1) raw material is taken according to following mass ratio, liquid epoxies: solidifying agent: modification mixed fillers=100:13 ~ 15:300 ~ 400;
(2) liquid epoxies step (1) taken drops in thin layer deaeration still, start stirring, preheating 20 minutes when being warming up to 60 DEG C, then the modification mixed fillers that step (1) takes is dropped into, vacuum deaerator after stirring, under 100 ~ 200Pa condition, deaeration is to bubble-free is released, leave standstill and be cooled to after room temperature keeps 30 minutes, start stirring, add the solidifying agent that step (1) takes, stirring at room temperature is rear vacuum deaerator discharging after 10 minutes evenly, i.e. obtained LED high-thermal-conductivity epoxy resin composite casting material;
Described liquid epoxies is one or more in bisphenol A type epoxy resin, bisphenol f type epoxy resin, aliphatic epoxy resin and cycloaliphatic epoxy resin;
Described solidifying agent is tetraethylene pentamine;
Described modification mixed fillers is prepared according to the following steps:
1 mass parts aluminum oxide powder and 7 mass parts carbon fiber mixed fillers are dropped in reaction vessel after dry 10 hours at 100 DEG C, add the silane coupling agent of 5wt% mixed fillers and the dehydrated alcohol of silane coupling agent consumption 10 times again, 60 DEG C are warming up to after mixing and stirring, ultrasonication 20 minutes, by washing with alcohol 1 time, then ultrasonication 10 minutes, use washing with alcohol again 1 time, 30 minutes are left standstill, finally under 80 DEG C of vacuum dry 14 hours, i.e. obtained modification mixed fillers after suction filtration; Wherein aluminum oxide powder is 200 orders, and the diameter of carbon fiber is 7um, and length is 4mm, density 1.76g/cm 3.
CN201510443642.3A 2015-07-27 2015-07-27 A kind of LED preparation methods of high-thermal-conductivity epoxy resin composite casting material Active CN105061994B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107474482A (en) * 2017-07-05 2017-12-15 安徽中威光电材料有限公司 A kind of high heat conduction type ring epoxy resin composite material of LED encapsulation fibre reinforced and preparation method thereof
CN113426338A (en) * 2021-06-29 2021-09-24 深圳市金菱通达电子有限公司 Manufacturing method of insulating ultrahigh heat conduction composite material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103059513A (en) * 2013-02-17 2013-04-24 桂林理工大学 Castable for manufacturing high-voltage motor nano composite main insulation
CN103450638A (en) * 2013-09-06 2013-12-18 天津学子电力设备科技有限公司 Preparation method of highly thermal conductive epoxy resin for epoxy resin cast dry-type transformer
CN104017537A (en) * 2014-06-26 2014-09-03 轻工业部南京电光源材料科学研究所 Heat-conducting adhesive for LED (light-emitting diode) lamp packaging and preparation method thereof

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN103059513A (en) * 2013-02-17 2013-04-24 桂林理工大学 Castable for manufacturing high-voltage motor nano composite main insulation
CN103450638A (en) * 2013-09-06 2013-12-18 天津学子电力设备科技有限公司 Preparation method of highly thermal conductive epoxy resin for epoxy resin cast dry-type transformer
CN104017537A (en) * 2014-06-26 2014-09-03 轻工业部南京电光源材料科学研究所 Heat-conducting adhesive for LED (light-emitting diode) lamp packaging and preparation method thereof

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Title
曾柏顺等: ""干式变压器用高导热抗开裂环氧浇注料"", 《绝缘材料》 *
李攀敏等: ""环氧树脂/氧化铝复合材料的制备及导热模型"", 《电子元件与材料》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107474482A (en) * 2017-07-05 2017-12-15 安徽中威光电材料有限公司 A kind of high heat conduction type ring epoxy resin composite material of LED encapsulation fibre reinforced and preparation method thereof
CN113426338A (en) * 2021-06-29 2021-09-24 深圳市金菱通达电子有限公司 Manufacturing method of insulating ultrahigh heat conduction composite material

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