A composite material for LED encapsulation and a method of manufacturing the same

Abstract

The application provides a composite material for LED packaging and a preparation method thereof, and belongs to the technical field of packaging materials. The composite material for LED packaging comprises A components and B components in a weight ratio of 100:18-100:22. The A components comprise 58-85 parts of an alicyclic epoxy resin, 12-25 parts of a toughening agent and 1.5-4 parts of a coupling agent in terms of weight fraction. The B components comprise 108 parts of a modified acid anhydride and 1 part of a cation in terms of weight fraction. When the composite material is used as a packaging material, the cracking of lamp beads during reflow soldering after 85% humidity absorption can be effectively reduced, and the dead lamp phenomenon of the patch lamp beads after cold and hot impact at-40 DEG C and 120 DEG C can be effectively reduced. The composite material has the characteristics of low stress and high performance, and is suitable for the packaging of various fantasy patch LEDs and other semiconductors.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of packaging materials, in particular to a composite material for LED packaging and a preparation method thereof. BACKGROUND

[0002] RGB fantasy LED semiconductor is a light emitting diode device based on RGB technology, which realizes white light and full-color light emission through the mixing of red, green and blue (RGB) three primary color chips. With the advantages of high color rendering index, high reliability and large color rendering range, it is widely used in lighting and display fields.

[0003] LED packaging refers to the packaging of light emitting chips, which not only requires protection of the lamp core, but also requires light transmission, better light emitting efficiency and heat dissipation environment of the LED, thereby improving the service life of the LED. Therefore, the packaging material for packaging various optical semiconductor elements such as LEDs must have the characteristics of transparency, moisture resistance, heat resistance and light resistance.

[0004] At present, most LED packaging materials use epoxy resin. Specifically, bisphenol A type epoxy resin, alicyclic epoxy resin and thermosetting epoxy resin containing anhydride curing agent are usually used. However, in the case of simply melting and using multifunctional epoxy resin and alicyclic epoxy resin, the strength is reduced, and when a semiconductor element is packaged using such an epoxy resin composition, the packaging material is prone to moisture aging, and problems such as chip explosion (cracking and screen cracking), lamp bead cracking and lamp bead dead lamp (as shown in Figure 6 ).

[0005] In view of the above problems, the present application aims to apply a composite material for LED packaging and a preparation method thereof, which can effectively reduce the cracking of the lamp bead when over-reflow soldering after double 85 moisture absorption, and the dead lamp of the patch lamp bead after cold and hot impact at-40℃ and 120℃. The composite material has low stress, high performance and other characteristics, and is suitable for packaging of various fantasy patch LEDs and other semiconductors. SUMMARY

[0006] In order to overcome the problems in the related art, the present application provides a composite material for LED packaging and a preparation method thereof, which can effectively reduce the cracking of the lamp bead when over-reflow soldering after double 85 moisture absorption, and the dead lamp of the patch lamp bead after cold and hot impact at-40℃ and 120℃. The composite material has low stress, high performance and other characteristics, and is suitable for packaging of various fantasy patch LEDs and other semiconductors.

[0007] One of the purposes of the present application is to provide a composite material for LED packaging, comprising: 100:18~100:22 of A component and B component by weight ratio;

[0008] The A component comprises: 58-85 parts of alicyclic epoxy resin, 12-25 parts of toughening agent and 1.5-4 parts of coupling agent by weight;

[0009] The B component comprises: 108 parts of modified anhydride and 1 part of cation by weight.

[0010] In the preferred technical solution of the present application, the alicyclic epoxy resin comprises:

[0011] 50-70 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 5-10 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether and 3-5 parts of bis((3,4-epoxycyclohexyl) methyl) adipate.

[0012] In the preferred technical solution of the present application, the toughening agent comprises: 10-20 parts of polycaprolactone polyol and 2-5 parts of oxetane.

[0013] In the preferred technical solution of the present application, the coupling agent comprises: 1-3 parts of epoxy silane and 0.5-1 part of mercapto silane.

[0014] In the preferred technical solution of the present application, the modified anhydride comprises: 100 parts of anhydride and 8 parts of alkylene oxide.

[0015] In the preferred technical solution of the present application, the alicyclic epoxy resin comprises:

[0016] 60-65 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 10 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether and 5 parts of bis((3,4-epoxycyclohexyl) methyl) adipate.

[0017] In the preferred technical solution of the present application, the weight ratio of the epoxy silane to the mercapto silane is 2:1.

[0018] In the preferred technical solution of the present application, the anhydride comprises 70 parts of methylhexahydrophthalic anhydride and 30 parts of hexahydrophthalic anhydride;

[0019] The alkylene oxide comprises 8 parts of any one of 1,2-epoxydodecane, 1,2-epoxytetradecane and 1,2-epoxyhexadecane.

[0020] In the preferred technical solution of the present application, the weight ratio of the A component and the B component is 100:20.

[0021] The second object of the present application is to provide a preparation method of a composite material for preparing the composite material for LED packaging.

[0022] Preparation of the A component: 58-85 parts by weight of alicyclic epoxy resin, 12-25 parts by weight of a toughening agent, and 1.5-4 parts by weight of a coupling agent are weighed and mixed, stirred, vacuum degassed, and filtered;

[0023] Preparation of the B component: 100 parts by weight of an anhydride, 8 parts by weight of an epoxy alkane, and 1 part by weight of a cation are weighed, heated to a first temperature, stirred and dissolved, heated to a second temperature, maintained for 4 hours, stirred, and filtered; the second temperature is greater than the first temperature;

[0024] Preparation of the composite material: the A component and the B component are fully mixed in a weight ratio of 100:18-100:22.

[0025] Compared with the prior art, the present application has the following advantages:

[0026] (1) The composite material provided by the present application uses alicyclic epoxy resin, polycaprolactone polyol and oxetane as a toughening agent, and a coupling agent is compounded; an epoxy alkane is used as a modifier to modify an anhydride, and a cation is mixed as a curing agent, so that the composite material has the characteristics of low stress and high performance, and is suitable for packaging of various color-changing patch LEDs and other semiconductors.

[0027] (2) The present application uses three different types of alicyclic epoxy resins, and strictly controls the ratio range of the three different types of alicyclic epoxy resins, which can effectively reduce the cracking of the lamp beads after reflow soldering after double 85 humidity absorption and the dead lamp condition of the patch lamp beads after cold and hot impact at-40℃ and 120℃, and has excellent performance and low cost.

[0028] (3) The present application strictly controls the weight ratio of the A component and the B component, which can effectively reduce the cracking of the lamp beads after reflow soldering after double 85 humidity absorption and the dead lamp condition of the patch lamp beads after cold and hot impact at-40℃ and 120℃.

[0029] (4) The present application modifies the anhydride with an epoxy alkane (crosslinking reaction between epoxy groups and anhydride), which can effectively reduce the volatility of the anhydride, thereby increasing the toughness and improving the moisture resistance. Compared with the unmodified anhydride in the prior art, which can easily cause cracking of the lamp beads and dead lamp condition of the lamp beads, the present application uses modified anhydride, which can greatly reduce the cracking of the lamp beads after reflow soldering after double 85 humidity absorption and the dead lamp condition of the patch lamp beads after cold and hot impact at-40℃ and 120℃.

[0030] (5) The application can accelerate the cross-linking reaction of alkylene oxide and acid anhydride by using cations as catalysts in the process of modifying acid anhydride by alkylene oxide, and also can be used as curing agent and accelerator of A component and B component in the preparation of composite materials, thereby effectively reducing the cost and improving the efficiency. BRIEF DESCRIPTION OF DRAWINGS

[0031] Figure 1 is a flowchart of the preparation method of the composite material for LED packaging provided by the application;

[0032] Figure 2 is a schematic diagram of the double 85 moisture absorption of the cured composite material for 24h and then reflow soldering;

[0033] Figure 3 is a schematic diagram of the double 85 moisture absorption of the cured composite material for 48h and then reflow soldering;

[0034] Figure 4 is a schematic diagram of the double 85 moisture absorption of the cured composite material for 96h and then reflow soldering;

[0035] Figure 5 is a schematic diagram of the double 85 moisture absorption of the cured composite material for 120h and then reflow soldering;

[0036] Figure 6 is a schematic diagram of the double 85 moisture absorption of the existing packaging material (such as the product IK0010 of Japan Inada Company) for 120h and then reflow soldering. DETAILED DESCRIPTION

[0037] The above content of the application will be further described in detail through the specific embodiments in the form of examples. However, it should not be understood that the above-mentioned subject matter of the application is limited to the following examples. Any technology realized based on the above-mentioned content of the application belongs to the scope of the application.

[0038] At present, most of the LED packaging adopts epoxy resin as the material, but in the case of simply melting and using multifunctional epoxy resin and alicyclic epoxy resin, the strength is easily reduced. When the semiconductor element is packaged by using such an epoxy resin composition, the packaging material is easy to absorb moisture and age, and problems such as chip explosion (cracking and screen cracking), lamp bead cracking and lamp bead dead lamp are easily caused.

[0039] To solve the above problems, the embodiment of the present application provides a composite material for LED packaging and a preparation method thereof, which can effectively reduce the cracking of the lamp beads during reflow soldering after double 85 moisture absorption and the dead lamp condition of the patch lamp beads after cold and hot impact at-40℃ and 120℃. The composite material has low stress, high performance and other characteristics, and is suitable for packaging of various fantasy patch LEDs and other semiconductors.

[0040] The technical solutions of the embodiments of the present application are described in detail below with reference to the drawings.

[0041] Embodiment

[0042] The composite material for LED packaging provided by the embodiment of the present application comprises, by weight ratio, 100:18-100:22 of A component and B component; the A component comprises, by weight fraction, 58-85 parts of alicyclic epoxy resin, 12-25 parts of toughening agent and 1.5-4 parts of coupling agent; the B component comprises, by weight fraction, 108 parts of modified anhydride and 1 part of cation. Preferably, the weight ratio of the A component to the B component is 100:20.

[0043] The alicyclic epoxy resin comprises at least one of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester (model number: 2121P), poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether (model number: 3150) and bis((3,4-epoxycyclohexyl)methyl) adipate (model number: AT26); the structural formula of the 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester is , the structural formula of the poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether is , and the structural formula of the bis((3,4-epoxycyclohexyl)methyl) adipate is .

[0044] Preferably, the alicyclic epoxy resin comprises 50-70 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 5-10 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether and 3-5 parts of bis((3,4-epoxycyclohexyl)methyl) adipate. More preferably, the alicyclic epoxy resin comprises 60-65 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 10 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether and 5 parts of bis((3,4-epoxycyclohexyl)methyl) adipate. Further, the alicyclic epoxy resin comprises 65 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 10 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether and 5 parts of bis((3,4-epoxycyclohexyl)methyl) adipate.

[0045] The toughening agent comprises a polycaprolactone polyol and an oxetane, the polycaprolactone polyol comprises a polycaprolactone triol (model number: 3057), a molecular weight of 550, and a structural formula of The oxetane comprises 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane (model number: 221), a structural formula of .

[0046] Specifically, the toughening agent comprises 10-20 parts of the polycaprolactone polyol and 2-5 parts of the oxetane, more specifically, the toughening agent comprises 10-20 parts of the polycaprolactone triol and 2-5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane. Preferably, the toughening agent comprises 15-20 parts of the polycaprolactone triol and 5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane.

[0047] The coupling agent comprises an epoxy silane and a mercapto silane, the epoxy silane comprises 3-glycidyloxypropyltrimethoxysilane (model number: KH-560), a structural formula of The mercapto silane comprises mercaptopropyltrimethoxysilane (model number: 189), a structural formula of .

[0048] Specifically, the coupling agent includes 1-3 parts of an epoxy silane and 0.5-1 part of a mercapto silane; preferably, the weight ratio of the epoxy silane to the mercapto silane is 2:1. More specifically, the coupling agent includes 1-3 parts of 3-glycidoxypropyltrimethoxysilane and 0.5-1 part of mercaptopropyltrimethoxysilane; preferably, the coupling agent includes 2 parts of 3-glycidoxypropyltrimethoxysilane and 1 part of mercaptopropyltrimethoxysilane.

[0049] The modified anhydride includes 100 parts of an anhydride and 8 parts of an alkylene oxide; the anhydride includes at least one of methylhexahydrophthalic anhydride and hexahydrophthalic anhydride, and the alkylene oxide includes any one of 1,2-epoxydodecane, 1,2-epoxytetradecane and 1,2-epoxyhexadecane; preferably, the alkylene oxide is 1,2-epoxyhexadecane. By modifying the anhydride with the alkylene oxide (cross-linking reaction between the epoxy group and the anhydride), the volatility of the anhydride can be effectively reduced, thereby increasing the toughness and improving the moisture resistance.

[0050] Specifically, the anhydride includes 70 parts of methylhexahydrophthalic anhydride and 30 parts of hexahydrophthalic anhydride; more specifically, the modified anhydride includes 70 parts of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride and 8 parts of 1,2-epoxyhexadecane.

[0051] The cation includes a hexafluoroantimonic acid blocked amine salt. By providing the cation, the cross-linking reaction between the alkylene oxide and the anhydride can be accelerated as a catalyst during the modification of the anhydride with the alkylene oxide, and meanwhile, the cation can also serve as a curing agent and an accelerator for the A component and the B component in the preparation of the composite material, thereby effectively reducing the cost and improving the efficiency.

[0052] Correspondingly, as shown in Figure 1 The embodiment of the present application further provides a preparation method of a composite material, which is used for preparing the composite material for LED packaging and specifically includes the following steps:

[0053] Preparation of the A component: 58-85 parts of alicyclic epoxy resin, 12-25 parts of a toughening agent and 1.5-4 parts of a coupling agent are weighed by weight fraction, mixed, stirred, vacuum degassed and filtered;

[0054] Preparation of the B component: 100 parts of an anhydride, 8 parts of an alkylene oxide and 1 part of a cation are weighed by weight fraction, heated to a first temperature, stirred and dissolved, heated to a second temperature, maintained for 4 h, stirred and filtered; the second temperature is greater than the first temperature;

[0055] Preparation of the composite material: the A component and the B component are fully mixed in a weight ratio of 100:18~100:22.

[0056] Further, in the preparation of the A component, 50-70 parts by weight of 3,4-epoxycyclohexyl methyl-3',4'-epoxycyclohexyl methyl ester, 5-10 parts of poly[(2-oxiranyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 3-5 parts of bis((3,4-epoxycyclohexyl) methyl) adipate, 10-20 parts of polycaprolactone triol, 2-5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane, 1-3 parts of 3-glycidyl ether oxypropyl trimethoxysilane and 0.5-1 part of mercaptopropyl trimethoxysilane are weighed, mixed, wall-stirred, vacuum degassed and filtered to obtain the A component; wherein the stirring speed is 500-800 rpm and the stirring time is 20 min.

[0057] In the preparation of the B component, 70 parts by weight of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride, 8 parts of 1,2-epoxyhexadecane and 1 part of hexafluoroantimonic acid blocked amine salt are weighed, heated to a first temperature, stirred and dissolved, then stirred for 1 h, heated to a second temperature and maintained for 4 h, and then stirred and filtered to obtain the B component, wherein the stirring speed is 60-100 rpm; the first temperature is 70-80°C and the second temperature is 120°C.

[0058] In the preparation of the composite material, the A component and the B component are weighed in a weight ratio of 100:20, and the A component and the B component are thoroughly mixed to obtain the composite material.

[0059] It should be noted that the specific raw materials of the above components are commercially available, and the specific conditions are as follows:

[0060]

[0061] In the embodiments of the present application, the composite material provided by the present application adopts an alicyclic epoxy resin, uses polycaprolactone polyol and oxetane as a toughening agent, and is compounded with a coupling agent; uses an epoxy alkane as a modifier to modify an anhydride, and mixes a cation to serve as a curing agent, so that the composite material has the characteristics of low stress and high performance, can effectively reduce the cracking of lamp beads during reflow soldering after moisture absorption of double 85, and can effectively reduce the dead lamp of the patch lamp bead after cold and hot impact at-40°C and 120°C, and is suitable for packaging of various fantasy patch LEDs and other semiconductors.

[0062] Example 1

[0063] The preparation method of the composite material for LED packaging provided in the embodiment 1 of the present application specifically includes the following steps:

[0064] Preparation of A component: 70 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 7 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 3 parts of bis((3,4-epoxycyclohexyl)methyl) adipate, 15 parts of polycaprolactone triol, 5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane, 2 parts of 3-glycidyloxypropyltrimethoxysilane and 1 part of mercaptopropyltrimethoxysilane are weighed out in parts by weight, and after mixing the above raw materials, wall-hung stirring is performed for 20 min at a stirring speed of 500-800 rpm, vacuum degassing is performed, and then filtration is performed, to obtain the A component.

[0065] Preparation of B component: 70 parts of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride, 8 parts of 1,2-epoxyhexadecane and 1 part of hexafluoroantimonic acid blocked amine salt are weighed out in parts by weight, heated to 70-80°C, stirred for 1 h, and after complete dissolution, heating is continued to 120°C for 4 h, stirring is performed at a stirring speed of 60-100 rpm, and then filtration is performed, to obtain the B component.

[0066] Preparation of composite material: the A component and the B component are weighed out in a weight ratio of 100:20, and the A component and the B component are mixed to obtain a composite material (i.e., a composite material for LED packaging).

[0067] Example 2

[0068] The preparation method of the composite material for LED packaging provided in Example 2 of the present application specifically includes the following steps:

[0069] Preparation of A component: 65 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 10 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 5 parts of bis((3,4-epoxycyclohexyl)methyl) adipate, 15 parts of polycaprolactone triol, 5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane, 2 parts of 3-glycidyloxypropyltrimethoxysilane and 1 part of mercaptopropyltrimethoxysilane are weighed out in parts by weight, and after mixing the above raw materials, wall-hung stirring is performed for 20 min at a stirring speed of 500-800 rpm, vacuum degassing is performed, and then filtration is performed, to obtain the A component.

[0070] Preparation of B component: 70 parts of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride, 8 parts of 1,2-epoxyhexadecane and 1 part of hexafluoroantimonic acid blocked amine salt are weighed out in parts by weight, heated to 70-80°C, stirred for 1 h, and after complete dissolution, heating is continued to 120°C for 4 h, stirring is performed at a stirring speed of 60-100 rpm, and then filtration is performed, to obtain the B component.

[0071] Preparation of the composite material: the A component and the B component are weighed according to the weight ratio of 100:20, and the A component and the B component are mixed to obtain the composite material (i.e. the composite material for LED packaging).

[0072] Example 3

[0073] The preparation method of the composite material for LED packaging provided in Example 3 of the present application specifically comprises the following steps:

[0074] Preparation of the A component: 60 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 10 parts of poly[(2-oxiranyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 5 parts of bis((3,4-epoxycyclohexyl) methyl) adipate, 20 parts of polycaprolactone triol, 5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane, 2 parts of 3-glycidyl ether oxypropyl trimethoxysilane and 1 part of mercaptopropyl trimethoxysilane are weighed by weight fraction, and after the above raw materials are mixed, wall stirring is carried out at a speed of 500-800 rpm for 20 min, vacuum degassing is carried out, and then filtration is carried out to obtain the A component.

[0075] Preparation of the B component: 70 parts of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride, 8 parts of 1,2-epoxyhexadecane and 1 part of hexafluoroantimonic acid blocked amine salt are weighed by weight fraction, heated to 70-80℃, stirred for 1 h, fully dissolved, then heated to 120℃, maintained for 4 h, stirred at a speed of 60-100 rpm, and then filtered to obtain the B component.

[0076] Preparation of the composite material: the A component and the B component are weighed according to the weight ratio of 100:20, and the A component and the B component are mixed to obtain the composite material (i.e. the composite material for LED packaging).

[0077] Example 4

[0078] The preparation method of the composite material for LED packaging provided in Example 4 of the present application specifically comprises the following steps:

[0079] Preparation of A component: 70 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 5 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 5 parts of bis((3,4-epoxycyclohexyl)methyl) adipate, 20 parts of polycaprolactone triol, 5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane, 2 parts of 3-glycidyloxypropyltrimethoxysilane and 1 part of mercaptopropyltrimethoxysilane are weighed out in parts by weight, and after mixing the above raw materials, wall-hung stirring is performed for 20 min at a stirring speed of 500-800 rpm, vacuum degassing is performed, and then filtration is performed, to obtain the A component.

[0080] Preparation of B component: 70 parts of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride, 8 parts of 1,2-epoxyhexadecane and 1 part of hexafluoroantimonic acid blocked amine salt are weighed out in parts by weight, heated to 70-80°C, stirred for 1 h, and after complete dissolution, heating is continued to 120°C for 4 h, stirring is performed at a stirring speed of 60-100 rpm, and then filtration is performed, to obtain the B component.

[0081] Preparation of composite material: the above A component and the above B component are weighed out in a weight ratio of 100:20, and the A component and the B component are thoroughly mixed, to obtain a composite material (i.e., a composite material for LED packaging).

[0082] Comparative Example 1

[0083] The preparation method of a composite material for LED packaging provided in Comparative Example 1 of the present application specifically includes the following steps:

[0084] Preparation of A component: 80 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 20 parts of polycaprolactone triol, 5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane, 2 parts of 3-glycidyloxypropyltrimethoxysilane and 1 part of mercaptopropyltrimethoxysilane are weighed out in parts by weight, and after mixing the above raw materials, wall-hung stirring is performed for 20 min at a stirring speed of 500-800 rpm, vacuum degassing is performed, and then filtration is performed, to obtain the A component.

[0085] Preparation of B component: 70 parts of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride, 8 parts of 1,2-epoxyhexadecane and 1 part of hexafluoroantimonic acid blocked amine salt are weighed out in parts by weight, heated to 70-80°C, stirred for 1 h, and after complete dissolution, heating is continued to 120°C for 4 h, stirring is performed at a stirring speed of 60-100 rpm, and then filtration is performed, to obtain the B component.

[0086] Preparation of the composite material: the A component and the B component are weighed according to the weight ratio of 100:20, and the A component and the B component are fully mixed to obtain the composite material (i.e. the composite material for LED packaging).

[0087] Comparative Example 2

[0088] The preparation method of the composite material for LED packaging provided by Comparative Example 2 of the present application specifically comprises the following steps:

[0089] Preparation of the A component: 65 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 10 parts of poly[(2-oxiranyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 5 parts of bis((3,4-epoxycyclohexyl) methyl) adipate, 15 parts of polycaprolactone triol, 5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane, 2 parts of 3-glycidyl ether oxypropyl trimethoxysilane and 1 part of mercaptopropyl trimethoxysilane are weighed by weight fraction. After mixing the above raw materials, wall stirring is carried out at a speed of 500-800 rpm for 20 min, and then filtration is carried out after vacuum degassing. The A component is obtained.

[0090] Preparation of the B component: 70 parts of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride, 8 parts of 1,2-epoxyhexadecane and 1 part of hexafluoroantimonic acid blocked amine salt are weighed by weight fraction. Heating is carried out to 70-80℃, stirring is carried out for 1 h, and then filtration is carried out after sufficient dissolution, continuous heating to 120℃ for 4 h and stirring at a speed of 60-100 rpm.

[0091] Preparation of the composite material: the A component and the B component are weighed according to the weight ratio of 100:15, and the A component and the B component are fully mixed to obtain the composite material (i.e. the composite material for LED packaging).

[0092] Comparative Example 3

[0093] The preparation method of the composite material for LED packaging provided by Comparative Example 3 of the present application specifically comprises the following steps:

[0094] Preparation of A component: 65 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 10 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 5 parts of bis((3,4-epoxycyclohexyl)methyl) adipate, 15 parts of polycaprolactone triol, 5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane, 2 parts of 3-glycidyloxypropyltrimethoxysilane and 1 part of mercaptopropyltrimethoxysilane are weighed out in parts by weight, and after mixing the above raw materials, wall-hung stirring is performed for 20 min at a stirring speed of 500-800 rpm, vacuum degassing is performed, and then filtration is performed, to obtain the A component.

[0095] Preparation of B component: 70 parts of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride, 8 parts of 1,2-epoxyhexadecane and 1 part of hexafluoroantimonic acid blocked amine salt are weighed out in parts by weight, heated to 70-80°C, stirred for 1 h, and after complete dissolution, heating is continued to 120°C for 4 h, stirring is performed at a stirring speed of 60-100 rpm, and then filtration is performed, to obtain the B component.

[0096] Preparation of composite material: the above A component and the above B component are weighed out in a weight ratio of 100:25, and the A component and the B component are thoroughly mixed, to obtain a composite material (i.e., a composite material for LED packaging).

[0097] Comparative Example 4

[0098] The preparation method of a composite material for LED packaging provided in Comparative Example 4 of the present application specifically includes the following steps:

[0099] Preparation of A component: 65 parts of 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, 10 parts of poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 5 parts of bis((3,4-epoxycyclohexyl)methyl) adipate, 15 parts of polycaprolactone triol, 5 parts of 3,3'-[oxybis(methylene)]bis[3-ethyl]oxetane, 2 parts of 3-glycidyloxypropyltrimethoxysilane and 1 part of mercaptopropyltrimethoxysilane are weighed out in parts by weight, and after mixing the above raw materials, wall-hung stirring is performed for 20 min at a stirring speed of 500-800 rpm, vacuum degassing is performed, and then filtration is performed, to obtain the A component.

[0100] Preparation of B component: 70 parts of methylhexahydrophthalic anhydride, 30 parts of hexahydrophthalic anhydride and 1 part of hexafluoroantimonic acid blocked amine salt are weighed out in parts by weight, heated to 70-80°C, stirred for 1 h, and after complete dissolution, heating is continued to 120°C for 4 h, stirring is performed at a stirring speed of 60-100 rpm, and then filtration is performed, to obtain the B component.

[0101] Preparation of the composite material: the above-mentioned component A and the above-mentioned component B were weighed in a weight ratio of 100:20, and the component A and the component B were mixed thoroughly to obtain the composite material (i.e. the composite material for LED packaging).

[0102] Experimental data

[0103] The composite materials of the above-mentioned examples 1-4 and comparative examples 1-4 were subjected to a curing process, specifically: after vacuum degassing of the composite materials, dispensing, baking at 90℃ for 2h, and baking at 150℃ for 4h.

[0104] After curing, the LED semiconductor support with model number 5050 and 50 lamp beads were subjected to cold and hot impact experiments (-40℃, 120℃, 30 minutes each, 300 cycles) and double 85 moisture absorption experiments, and after the moisture absorption was completed, reflow soldering (260℃) was carried out, please refer to Figures 2-5 , and the performance index data are as follows:

[0105]

[0106] As shown in the above table, according to examples 1, 2, 4 and comparative example 1, although the alicyclic epoxy resins are all 80 parts, the different ratios among 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester, poly[(2-oxiranylmethyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether and bis((3,4-epoxycyclohexyl) methyl) adipate have different effects on the heat distortion temperature, hardness, lamp bead cracking after double 85 moisture absorption and lamp bead dead lamp after cold and hot impact, and the effect is not a linear change, and the ratio needs to be matched in a suitable range to achieve the effects of moisture resistance, anti-cracking and reducing lamp bead dead lamp, etc. Although the 3,4-epoxycyclohexyl carboxylic acid-3',4'-epoxycyclohexyl methyl ester (alicyclic epoxy resin 2121P) in comparative example 1 is 80 parts, but due to the absence of alicyclic epoxy resin 3150 and alicyclic epoxy resin AT-26, the lamp bead cracking after double 85 moisture absorption and the lamp bead dead lamp after cold and hot impact are much more than examples 1-4 (especially examples 2-3), which shows that the three different types of alicyclic epoxy resins can have a synergistic effect, and cannot be simply replaced by each other.

[0107] As can be seen from Example 2 and Comparative Examples 2-3, different weight ratios of component A and component B have a significant impact on issues such as LED cracking after moisture absorption by the dual 85 and LED failure after thermal shock. For example, when the weight ratio of component A to component B is 100:20 or 100:25, the number of LED cracking after moisture absorption by the dual 85 and LED failure after thermal shock are both higher than in Example 2, and the results are significantly different. This indicates that the weight ratio of component A to component B needs to be strictly controlled within a certain range to achieve the desired effect of this application.

[0108] As can be seen from Example 2 and Comparative Example 4, when acid anhydride is directly used in the packaging material (i.e., composite material), as mentioned in the background art of this application, the packaging material has low strength and is prone to problems such as chip bursting (cracking and screen explosion), LED cracking, and LED failure after moisture absorption and aging. This application modifies the acid anhydride with epoxy alkane. The modified acid anhydride can effectively solve the above problems. The effect is shown in Examples 1-4. The LED cracking after moisture absorption and the LED failure after thermal shock are far less than the effect when acid anhydride is directly used in Comparative Example 4.

[0109] like Figures 2-5 As shown, using the composite material provided in this application as the encapsulation material, the double 85 moisture absorption test verified that after reflow soldering at 24h, 48h, 96h, and 120h (highest standard) of double 85 moisture absorption, there was no cracking or leakage. Figure 6 The prior art encapsulation materials shown exhibit severe spore bursting after 120 hours of moisture absorption by dual 85 and reflow soldering. This indicates that the composite material of this application can effectively reduce the cracking of LED beads during reflow soldering after moisture absorption by dual 85. Furthermore, the composite material has characteristics such as low stress and high performance, making it suitable for the encapsulation of various semiconductors such as RGB surface mount LEDs.

[0110] Unless otherwise specifically stated, the relative arrangement, numerical expressions, and values ​​of the components and steps described in these embodiments do not limit the scope of this application. In the above embodiments, the descriptions of each embodiment have their own emphasis; parts not described in detail in a certain embodiment can be referred to in the relevant descriptions of other embodiments. Those skilled in the art should also understand that the steps in the methods of the embodiments of this application can be adjusted, combined, and deleted according to actual needs.

[0111] In addition, it should be noted that the use of "first", "second", and the like words to define parts is merely for the convenience of distinguishing the corresponding parts, and the above words have no special meaning unless otherwise stated, and therefore cannot be understood as limiting the scope of protection of the present application. The above is only the preferred embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application can have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included in the scope of protection of the present application.

Claims

1. A composite material for LED encapsulation, characterized in that, The components include, by weight ratio, components A and B in the range of 100:18 to 100:

22. Component A, by weight, comprises: 58-85 parts of alicyclic epoxy resin, 12-25 parts of toughening agent, and 1.5-4 parts of coupling agent; the alicyclic epoxy resin comprises: 50-70 parts of 3,4-epoxycyclohexylcarboxylate-3',4'-epoxycyclohexylmethyl ester; 5-10 parts of poly[(2-epoxyethylene)-1,2-cyclohexanediol]2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether; and 3-5 parts of bis((3,4-epoxycyclohexyl)methyl)adipate; the toughening agent comprises: 10-20 parts of polycaprolactone polyol and 2-5 parts of oxetane; Component B comprises, by weight, 108 parts of modified acid anhydride and 1 part of cation; the modified acid anhydride comprises 100 parts of acid anhydride and 8 parts of epoxy alkane; the cation comprises hexafluoroantimony acid blocked amine salt.

2. The composite material for LED encapsulation according to claim 1, characterized in that, The coupling agent includes: 1-3 parts of epoxy silane and 0.5-1 part of mercapto silane.

3. The composite material for LED encapsulation according to claim 1, characterized in that, The alicyclic epoxy resin includes: 60-65 parts of 3,4-epoxycyclohexylcarboxylic acid-3',4'-epoxycyclohexylmethyl ester; 10 parts of poly[(2-epoxyethylene)-1,2-cyclohexanediol]2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether and 5 parts of bis((3,4-epoxycyclohexyl)methyl) adipate.

4. The composite material for LED encapsulation according to claim 2, characterized in that, The weight ratio of the epoxy silane to the mercapto silane is 2:

1.

5. The composite material for LED encapsulation according to claim 1, characterized in that, The acid anhydride comprises 70 parts of methylhexahydrophthalic anhydride and 30 parts of hexahydrophthalic anhydride; The epoxide alkane includes 8 parts of any one of 1,2-epoxide dodecane, 1,2-epoxide tetradecane, and 1,2-epoxide hexadecane.

6. The composite material for LED encapsulation according to claim 1, characterized in that, The weight ratio of component A to component B is 100:

20.

7. A method for preparing a composite material, characterized in that: The preparation of the composite material for LED encapsulation as described in claim 1 specifically includes the following steps: Preparation of component A: Weigh 58-85 parts by weight of alicyclic epoxy resin, 12-25 parts by weight of toughening agent and 1.5-4 parts by weight of coupling agent, mix, stir, degas under vacuum and filter. Preparation of component B: Weigh 100 parts by weight of acid anhydride, 8 parts by weight of epoxide and 1 part by weight of cation, heat to the first temperature, stir to dissolve, heat to the second temperature, maintain for 4 hours, stir and filter; the second temperature is higher than the first temperature; Preparation of composite materials: Mix component A and component B thoroughly at a weight ratio of 100:18 to 100:22.

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