CN105273363A

CN105273363A - Nano diamond-containing maleic anhydride grafted polyphenyl ether modified epoxy resin composite material for LED package and preparation method

Info

Publication number: CN105273363A
Application number: CN201510522171.5A
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: 2016-01-27

Abstract

The present invention discloses a nano diamond-containing maleic anhydride grafted polyphenyl ether modified epoxy resin composite material for LED package, the composite material uses grafted polyphenyl ether for modification of epoxy resin, the polyphenyl ether material obtained by grafting maleic anhydride, nano-titanium dioxide and other raw materials not only maintains excellent low dielectric, low loss, and high thermal resistant performances, and the compatibility of the polyphenyl ether and the epoxy resin is improved, the defect of the epoxy resin as a package material can be effectively improved, added fluorocarbon emulsion gives the composite material excellent water resistant, corrosion resistant and antifouling and other performances, the blended nano-diamond greatly improves the mechanical properties of the composite resin, and greatly enhances temperature stability, and the modified epoxy resin composite material prepared by the method is strong in cohesion, strong in adhesion, good in packages effect, higher in light transmittance and stability, and especially suitable for high-power LED package.

Description

A kind of LED polyphenyl ether modified epoxy resin composite material of maleic anhydride graft containing Nano diamond and preparation method thereof

Technical field

The present invention relates to LED encapsulation material technical field, particularly relate to a kind of high-power LED encapsulation polyphenyl ether modified epoxy resin composite material of maleic anhydride graft containing Nano diamond 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 a kind of high-power LED encapsulation polyphenyl ether modified epoxy resin composite material of maleic anhydride graft containing Nano diamond and preparation method thereof.

The present invention is achieved by the following technical solutions:

High-power LED encapsulation is with containing the polyphenyl ether modified epoxy resin composite material of maleic anhydride graft of Nano diamond, and this matrix material is prepared by the raw material of following weight part: bisphenol A type epoxy resin 70-80, Nano diamond 0.01-0.02, solid content are that the fluorine carbon emulsion 5-6 of 40-50%, polyphenylene oxide powder 18-22, hydroxy silicon oil 0.1-0.2, nano titanium oxide 4-5, benzoyl peroxide 0.1-0.2, maleic anhydride 0.4-0.5, silane coupling agent 0.1-0.2, chloroform are appropriate, oxidation inhibitor 0.01-0.02, solidifying agent DDS20-25.

Described a kind of high-power LED encapsulation preparation method of the polyphenyl ether modified epoxy resin composite material of maleic anhydride graft containing Nano diamond, 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 diamond, 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, fluorine carbon emulsion 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 epoxy resin as packaged material, the fluorine carbon emulsion that adds gives matrix material excellent water-fast, corrosion resistant, the performance such as antifouling, the Nano diamond of blending improves the mechanical property of compound resin greatly, the stability of temperature is improved greatly, modification composite epoxy resin packaged material force of cohesion prepared by the present invention is strong, adhere well, packaging effect is good, to the transmitance of light and stability higher, especially be suitable as high-power LED encapsulation to use.

Embodiment

The matrix material of this embodiment is prepared by the raw material of following weight part: bisphenol A type epoxy resin 70, Nano diamond 0.01, solid content are fluorine carbon emulsion 5, polyphenylene oxide powder 18, hydroxy silicon oil 0.1, nano titanium oxide 4, benzoyl peroxide 0.1, maleic anhydride 0.4, silane coupling agent 0.1, chloroform appropriate, oxidation inhibitor 0.01, the solidifying agent DDS20 of 40%.

(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, fluorine carbon emulsion 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: 1.528; Transmittance: 84.2%; Tensile strength: 49.2MPa.

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	1.3	2.8	3.6
Visible light transmissivity velocity of variation	-5.0％	-8.7％	-14.2％

Claims

1. the maleic anhydride graft polyphenyl ether modified epoxy resin composite material of a high-power LED encapsulation containing Nano diamond, 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, Nano diamond 0.01-0.02, solid content are that the fluorine carbon emulsion 5-6 of 40-50%, polyphenylene oxide powder 18-22, hydroxy silicon oil 0.1-0.2, nano titanium oxide 4-5, benzoyl peroxide 0.1-0.2, maleic anhydride 0.4-0.5, silane coupling agent 0.1-0.2, chloroform are appropriate, oxidation inhibitor 0.01-0.02, solidifying agent DDS20-25.

2. a kind of high-power LED encapsulation as claimed in claim 1 preparation method of the polyphenyl ether modified epoxy resin composite material of maleic anhydride graft containing Nano diamond, 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;