CN105111681A

CN105111681A - Oxidation-resistant high-heat-conductivity maleic-anhydride-grafted polyphenyl ether modified epoxy resin composite material for LED packaging and preparation method thereof

Info

Publication number: CN105111681A
Application number: CN201510522238.5A
Authority: CN
Inventors: 王兴松; 许飞云; 罗翔; 戴挺; 章功国
Original assignee: Anhui Jisite Intelligent Equipment Co Ltd
Current assignee: Anhui Jisite Intelligent Equipment Co Ltd
Priority date: 2015-08-21
Filing date: 2015-08-21
Publication date: 2015-12-02

Abstract

The invention discloses an oxidation-resistant high-heat-conductivity maleic-anhydride-grafted polyphenyl ether modified epoxy resin composite material for LED packaging. According to the composite material, epoxy resin is modified through grafted polyphenyl ether; the polyphenyl ether obtained after maleic anhydride, nano titania and other raw materials are grafted maintains the excellent properties of low dielectric, low loss and high heat resistance, compatibility between the polyphenyl ether and the epoxy resin is improved, and the defects of traditional epoxy resin serving as a packaging material are effectively overcome; added nano copper and aquadag powder are good in adhesiveness, improve the heat conducting capacity, heat dissipating capacity and heat oxidation resisting capacity of the composite material, delay heat ageing of the material and also can shield certain electromagnetic radiation and delay ageing of the material. Serving as an LED packaging material, the prepared modified composite epoxy resin is excellent in overall performance, long in service life, more economical and more durable.

Description

A kind of LED polyphenyl ether modified epoxy resin composite material of maleic anhydride graft of anti-oxidant high heat conduction and preparation method thereof

Technical field

The present invention relates to LED encapsulation material technical field, particularly relate to polyphenyl ether modified epoxy resin composite material of maleic anhydride graft of the anti-oxidant high heat conduction of a kind of LED and preparation method thereof.

Background technology

LED refers to the encapsulation of luminescence chip, the encapsulation of LED is different from the encapsulation of other unicircuit, not only want protect IC, also there is light transmission, therefore special requirement is had to the performance of the packaged material of LED, the requirement of packaged material is mainly reflected in the light wanting extraction chip as much as possible to send, also want to reduce thermal resistance, reach the effect improving heat-sinking capability and light extraction efficiency, along with the develop rapidly of LED industry, day by day strong to the demand of novel high-quality packaged material, packaged material conventional at present mainly contains epoxy resin and silicone resin, epoxy resin cost is lower, its resistance to ultraviolet, ageing-resistant ability is poor, and silicone resin possesses excellent heat-proof aging, ultraviolet aging resistance, light transmission rate advantages of higher, but its production cost is higher.

Summary of the invention

The object of the invention is exactly the defect in order to make up prior art, provides polyphenyl ether modified epoxy resin composite material of maleic anhydride graft of the anti-oxidant high heat conduction of a kind of LED and preparation method thereof.

The present invention is achieved by the following technical solutions:

The LED polyphenyl ether modified epoxy resin composite material of maleic anhydride graft of anti-oxidant high heat conduction, this matrix material is prepared by the raw material of following weight part: bisphenol A type epoxy resin 70-80, polyphenylene oxide powder 20-24, hydroxy silicon oil 0.1-0.2, nano titanium oxide 4-5, benzoyl peroxide 0.1-0.2, maleic anhydride 0.4-0.5, Nanometer Copper 0.1-0.2, oildag powder 0.2-0.3, silane coupling agent 0.1-0.2, chloroform are appropriate, oxidation inhibitor 0.01-0.02, solidifying agent DDS20-25.

Described a kind of LED preparation method of the polyphenyl ether modified epoxy resin composite material of maleic anhydride graft of anti-oxidant high heat conduction, described preparation method is:

(1) first polyphenylene oxide powder is carried out pre-irradiation process, radiation parameter is: using rumbatron as irradiation source, under normal temperature, normal pressure, air atmosphere, utilize β ray to carry out radiation treatment, pre-irradiation dosage range is 20-30kGy, obtains pre-irradiation polyphenylene oxide material;

(2) the polyphenylene oxide material after pre-irradiation is dropped into stirrer high speed together with maleic anhydride, silane coupling agent, nano titanium oxide, benzoyl peroxide, oxidation inhibitor to be uniformly mixed, drop into extruding pelletization in twin screw extruder together subsequently, obtain grafted polyphenylene ether material;

(3) grafted polyphenylene ether step (2) prepared, bisphenol A type epoxy resin and other leftover materials except solidifying agent DDS drop in chloroform together, be warming up to 120-130 DEG C, mix and blend 1.5-2h, be cooled to 100-110 DEG C subsequently, drop into solidifying agent DDS, to continue sizing material insulation to be uniformly mixed after 20-30min and through vacuum defoamation process, the sizing material after deaeration is poured in mould, under 150-180 DEG C of condition, make it solidify completely and get final product.

Advantage of the present invention is: through maleic anhydride, the polyphenylene oxide material obtained after the raw material grafting such as nano titanium oxide not only maintains its excellent low dielectric, low-loss, high heat-resisting performance, and the consistency of itself and epoxy resin improves, effectively improve the defect of conventional epoxies as encapsulating compound, the Nanometer Copper added, oildag powder tack is good, improve the heat conduction of matrix material, heat radiation, thermal oxidation resistance ability, delay the thermal ageing of material, certain electromagnetic radiation can also be shielded, delay material aging, modification composite epoxy resin prepared by the present invention is as LED encapsulation material high comprehensive performance, long service life, more economy and durability.

Embodiment

The matrix material of this embodiment is prepared by the raw material of following weight part: bisphenol A type epoxy resin 70, polyphenylene oxide powder 20, hydroxy silicon oil 0.1, nano titanium oxide 4, benzoyl peroxide 0.1, maleic anhydride 0.4, Nanometer Copper 0.1, oildag powder 0.2, silane coupling agent 0.1, chloroform are appropriate, oxidation inhibitor 0.01, solidifying agent DDS20.

(1) first polyphenylene oxide powder is carried out pre-irradiation process, radiation parameter is: using rumbatron as irradiation source, under normal temperature, normal pressure, air atmosphere, utilize β ray to carry out radiation treatment, pre-irradiation dosage range is 20kGy, obtains pre-irradiation polyphenylene oxide material;

(3) grafted polyphenylene ether step (2) prepared, bisphenol A type epoxy resin and other leftover materials except solidifying agent DDS drop in chloroform together, be warming up to 120 DEG C, mix and blend 1.5h, be cooled to 100 DEG C subsequently, drop into solidifying agent DDS, to continue sizing material insulation to be uniformly mixed after 20min and through vacuum defoamation process, the sizing material after deaeration is poured in mould, under 150 DEG C of conditions, make it solidify completely and get final product.

Relevant criterion followed by matrix material obtained by the present embodiment, and measured performance index are as follows:

Specific refractory power: 1.52; Transmittance: 84.5%; Tensile strength: 48.2MPa.

Ultraviolet resistance burn-in test: test condition: specimen surface temperature 60 ± 5 DEG C, selects the ultraviolet lamp of UVB313 model, and irradiation intensity is 1.5kwh/m ², irradiation time is respectively 0h, 720h, 1500h, 2000h, the yellowness index of sequentially determining material and the change of visible light transmissivity, and test result is:

Irradiation time	720h	1500h	2000h
				Yellowness index	1.2	2.4	3.4
Visible light transmissivity velocity of variation	-4.1％	-7.6％	-12.2％

Claims

1. a LED polyphenyl ether modified epoxy resin composite material of maleic anhydride graft of anti-oxidant high heat conduction, it is characterized in that, this matrix material is prepared by the raw material of following weight part: bisphenol A type epoxy resin 70-80, polyphenylene oxide powder 20-24, hydroxy silicon oil 0.1-0.2, nano titanium oxide 4-5, benzoyl peroxide 0.1-0.2, maleic anhydride 0.4-0.5, Nanometer Copper 0.1-0.2, oildag powder 0.2-0.3, silane coupling agent 0.1-0.2, chloroform are appropriate, oxidation inhibitor 0.01-0.02, solidifying agent DDS20-25.

2. a kind of LED as claimed in claim 1 preparation method of the polyphenyl ether modified epoxy resin composite material of maleic anhydride graft of anti-oxidant high heat conduction, it is characterized in that, described preparation method is:

(1) first polyphenylene oxide powder is carried out pre-irradiation process, radiation parameter is: using rumbatron as irradiation source, and under normal temperature, normal pressure, air atmosphere, utilize β ray to carry out radiation treatment, pre-irradiation dosage range is 20-30kGy, obtains pre-irradiation polyphenylene oxide material;