CN106047276A - High-hardness high-adhesion modified high-heat conduction LED organosilicon package glue and preparation method thereof - Google Patents

Abstract

The invention discloses a high-hardness and high-adhesion modified high-thermal-conductivity LED organosilicon encapsulation adhesive. In the preparation process of the encapsulation adhesive, nano-ceramic powder and nano-zinc oxide are surface-treated with a silane coupling agent and then put into an imidazole-based ionic liquid. Medium reaction to obtain highly dispersed nano-powder with ionic liquid on the surface, which effectively improves the agglomeration phenomenon of nano-fillers. Together with the added hydrogenated rosin, it is chemically bonded to the surface of organic silica gel to form a continuous network of nano-materials. The thermal conductivity and bonding strength of the material are effectively improved, and a packaging glue with high hardness, high thermal conductivity and high adhesion is obtained. The LED lamps encapsulated with the silica gel of the present invention can maintain good luminous performance for a long time and have a longer service life.

Description

A modified high thermal conductivity LED organic silicon encapsulant with high hardness and high adhesion and its preparation preparation method

technical field

The invention relates to the technical field of organosilicon encapsulation glue, in particular to a modified high heat conduction LED organosilicon encapsulation glue with high hardness and high adhesion and a preparation method thereof.

Background technique

LED is called the fourth-generation light source, which has the characteristics of energy saving, environmental protection, safety, low power consumption, low heat, high brightness, concentrated beam, easy maintenance, etc., and can be widely used in various indications, displays, decorations, backlights, and general lighting and other fields. At present, improving the luminous efficiency of LED is still a key technical issue. In the process of LED production, the packaging material has a significant impact on the luminous efficiency and service life of the product. The packaging material is required to have high transparency, high refraction, high bonding strength, and light resistance. , heat aging and other properties. At present, the commonly used packaging glue mainly includes epoxy resin and silica gel. Compared with epoxy resin, silica gel has higher light transmittance, UV resistance and heat resistance stability, and has become an ideal packaging material at present. However, the refractive index of silicone material , mechanical properties and bonding performance are not good, and its application is limited. Therefore, the synthesis of silicone encapsulants with high refractive index and high adhesion is a hot spot in industry research.

The current research on silicone encapsulants shows that increasing the refractive index of silica gel can effectively reduce the photon loss caused by the physical barrier of the refractive index and improve the external quantum efficiency. However, the performance of silica gel is greatly affected by the ambient temperature. As the temperature increases, the The increase of thermal stress leads to the decrease of the refractive index of silica gel, which affects the light efficiency and light intensity distribution of LED. Therefore, improving the thermal conductivity of silica gel plays a vital role in ensuring the refractive index of the material. At present, the main way to improve the thermal conductivity of silicone encapsulants is to directly add thermal conductive fillers. In order to obtain a more ideal thermal conductivity effect, a large amount of filling is required, which will affect the viscosity, light transmittance and comprehensive mechanical properties of the resin, and thermal conductive fillers The decentralization of is also a thorny problem.

Contents of the invention

The object of the present invention is to provide a modified high thermal conductivity LED organic silicon encapsulant with high hardness and high adhesion and a preparation method thereof in order to remedy the defects of the prior art.

The present invention is achieved through the following technical solutions:

A modified high thermal conductivity LED silicone encapsulant with high hardness and high adhesion, which is prepared from the following raw materials in parts by weight: vinyl MQ silicone resin 50-80, vinyl silicone oil 80-120, hydrogen-containing silicone oil 5 -10, Polydimethylsiloxane 3-5, Custer platinum catalyst 0.5-1, 2-vinyl isoamyl alcohol 0.01-0.02, ionic liquid 20-30, hydrogenated rosin 4-8, nano ceramic powder 0.8 -1.5, nano zinc oxide 4-8, silane coupling agent kh-560 0.1-0.2.

The vinyl content of the vinyl MQ resin is 6-10%, and the viscosity is 8000-12000mP.s.

The vinyl content in the vinyl silicone oil is 1-3%, and the viscosity is 2000-6000mP.s.

The hydrogen content of the hydrogen-containing silicone oil is 0.8-1%.

The ionic liquid is an imidazole ionic liquid.

The preparation method of the modified high thermal conductivity LED organosilicon encapsulant with high hardness and high adhesion is as follows:

(1) First prepare a mixed solution with silane coupling agent kh-560 and absolute ethanol at a weight ratio of 1:150, then put nano-ceramic powder and nano-zinc oxide into the mixed solution, stir and mix at high speed for 1-2 hours, then add Ionic liquid, stir and mix evenly, reflux at 100-120°C for 3-5h, then cool to room temperature for later use;

(2) Dissolving hydrogenated rosin in an appropriate amount of dichloromethane, then mixing and stirring it with the material obtained in step (1), and reacting at 180-200°C for 2-3 hours before use;

(3) Mix and stir other remaining materials with the materials in step (2) evenly, wash with absolute ethanol 2-3 times, and vacuum defoam to obtain the silicone encapsulating glue.

In the present invention, nano-ceramic powder and nano-zinc oxide are treated with a silane coupling agent and put into imidazole-based ionic liquids for reaction to obtain highly dispersed nano-powders with surface-wrapped ionic liquids, which effectively improves the agglomeration of nano-fillers. The added hydrogenated rosin is chemically bonded to the surface of the organic silica gel to form a continuous network of nanomaterials, which effectively improves the thermal conductivity and bonding strength of the material, and obtains a packaging adhesive with high hardness, high thermal conductivity and high adhesion. , the LED lamp encapsulated by the silica gel of the present invention can maintain good luminous performance for a long time, and has a longer service life.

detailed description

The silicone encapsulant of this embodiment is made from the following raw materials in parts by weight: vinyl MQ silicone resin 50, vinyl silicone oil 80, hydrogen-containing silicone oil 5, polydimethylsiloxane 3, Castel platinum catalyst 0.5, 2-vinyl isoamyl alcohol 0.01, ionic liquid 20, hydrogenated rosin 4, nano ceramic powder 0.8, nano zinc oxide 4, silane coupling agent kh-560 0.1.

Among them, the vinyl content of vinyl MQ resin is 6%, the viscosity is 8000mP.s, the vinyl content in vinyl silicone oil is 1%, the viscosity is 2000mP.s, the hydrogen content of hydrogen-containing silicone oil is 0.8%, and the ionic liquid is 1 -Butyl-3-methylimidazolium trifluoroacetate.

The preparation method of this packaging glue is:

(1) First prepare a mixed solution with silane coupling agent kh-560 and absolute ethanol at a weight ratio of 1:150, then put nano-ceramic powder and nano-zinc oxide into the mixed solution, stir and mix at high speed for 1 hour, and then add ionic liquid , stir and mix evenly, reflux at 100°C for 3 hours, then cool to room temperature for later use;

(2) Dissolve hydrogenated rosin in an appropriate amount of dichloromethane, then mix and stir it with the material obtained in step (1), and react at 180°C for 2 hours before use;

(3) Mix and stir other remaining materials with the materials in step (2) evenly, wash twice with absolute ethanol, and vacuum defoam to obtain the silicone encapsulating glue.

The performance test results of the prepared encapsulation glue after encapsulation and curing are as follows:

Test items value Shore D hardness 45 degree Tensile Strength 12.5MPa Refractive index (25°C) 1.5520 Light transmittance (500nm) ≥85% Adhesion (MPa) 1.8MPa Thermal Conductivity 0.198W/mk

Claims (6)

1. the modification of a high rigidity high adhesion force high thermally conductive LED organic silicon packaging glue, it is characterised in that this packaging plastic is by following The raw material of weight portion prepares: Vinyl MQ silicon resin 50-80, vinyl silicone oil 80-120, containing hydrogen silicone oil 5-10, poly dimethyl silicon Oxygen alkane 3-5, Karst platinum catalyst 0.5-1,2-vinyl isoamyl alcohol 0.01-0.02, ionic liquid 20-30, hydrogenated rosin 4-8, nano-ceramic powder 0.8-1.5, nano zine oxide 4-8, silane coupler kh-560 0.1-0.2.

The modification high thermally conductive LED organic silicon packaging glue of a kind of high rigidity high adhesion force the most as claimed in claim 1, its feature exists In, the contents of ethylene of described vinyl MQ resin is 6-10%, and viscosity is 8000-12000mP.s.

The modification high thermally conductive LED organic silicon packaging glue of a kind of high rigidity high adhesion force the most as claimed in claim 1, its feature exists In, described vinyl silicone oil medium vinyl content is 1-3%, and viscosity is 2000-6000mP.s.

The modification high thermally conductive LED organic silicon packaging glue of a kind of high rigidity high adhesion force the most as claimed in claim 1, its feature exists In, the hydrogen content of described containing hydrogen silicone oil is 0.8-1%.

The modification high thermally conductive LED organic silicon packaging glue of a kind of high rigidity high adhesion force the most as claimed in claim 1, its feature exists In, described ionic liquid is glyoxaline ion liquid.

The preparation side of the modification high thermally conductive LED organic silicon packaging glue of a kind of high rigidity high adhesion force the most as claimed in claim 1 Method, it is characterised in that described preparation method is:

(1) first silane coupler kh-560 is prepared mixed solution, subsequently by nanometer with dehydrated alcohol according to the weight ratio of 1:150 Ceramics, nano zine oxide put in mixed solution, high-speed stirred mixing 1-2h, are subsequently added ionic liquid, and stirring mixing is all Reflux after even at a temperature of 100-120 DEG C 3-5h, is then cooled to room temperature standby；

(2) hydrogenated rosin is dissolved in appropriate dichloromethane, subsequently by itself and the material mix and blend of step (1) gained, and React standby after 2-3h under the conditions of 180-200 DEG C；

(3) take off washing 2-3 final vacuum with dehydrated alcohol after the material mixing and stirring of other leftover materials and step (2) Bubble, obtains described organic silicon packaging glue.