CN117106286A - LED composite packaging material and preparation method thereof - Google Patents

LED composite packaging material and preparation method thereof Download PDF

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Publication number
CN117106286A
CN117106286A CN202311354446.XA CN202311354446A CN117106286A CN 117106286 A CN117106286 A CN 117106286A CN 202311354446 A CN202311354446 A CN 202311354446A CN 117106286 A CN117106286 A CN 117106286A
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China
Prior art keywords
parts
silicon carbide
led composite
silane coupling
coupling agent
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CN202311354446.XA
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CN117106286B (en
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徐志军
陈浩
陈传国
江汉
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Focus Lightings Technology Suqian Co ltd
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Focus Lightings Technology Suqian Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/52Encapsulations
    • H01L33/56Materials, e.g. epoxy or silicone resin
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention relates to an LED composite packaging material and a preparation method thereof, wherein the LED composite packaging material comprises the following components in parts by weight: 20-25 parts of bisphenol A type epoxy resin, 15-20 parts of hydantoin epoxy resin, 2-4 parts of modified silicon carbide, 5-8 parts of inorganic filler, 5-10 parts of curing agent, 3-5 parts of antioxidant and 10-15 parts of diluent; wherein the modified silicon carbide is obtained by reacting gallic acid modified silane coupling agent with silicon carbide. According to the invention, gallic acid modified silane coupling agent is adopted to react with silicon carbide, so that the reactivity and compatibility of components are improved, and meanwhile, the gallic acid modified silane coupling agent is compounded with components such as epoxy resin, hydantoin epoxy resin and the like to obtain the LED composite packaging material with good stability and excellent mechanical property, so that the defects in the prior art are overcome, and the LED composite packaging material has a good application prospect.

Description

LED composite packaging material and preparation method thereof
Technical Field
The invention belongs to the technical field of LED materials, and particularly relates to an LED composite packaging material and a preparation method thereof.
Background
LEDs (light emitting diodes) are the most popular light source material in the current market due to their high brightness, low heat, long life, recyclability, etc., and are called as the most promising green illumination sources in the twenty-first century. However, after the LEDs are thinned, miniaturized, and arrayed, how to achieve high reliability and stability of the package faces a great challenge.
In order to improve the effect of LED packaging, various performances such as stability, hardness, heat conduction and electric conduction of products are usually improved by adding materials such as epoxy resin, silica gel and filler. However, most technical schemes are difficult to ensure the balance among various performances, and the existing LED packaging materials have the defects of low stability and poor mechanical performance, so that the market demands are difficult to meet.
In view of the foregoing, it is necessary to develop a new technical solution to solve the problems existing in the prior art.
Disclosure of Invention
In order to solve the problems, the invention provides an LED composite packaging material and a preparation method thereof. According to the invention, gallic acid modified silane coupling agent is adopted to react with silicon carbide, so that the reactivity and compatibility of components are improved, and meanwhile, the gallic acid modified silane coupling agent is compounded with components such as epoxy resin, hydantoin epoxy resin and the like to obtain the LED composite packaging material with good stability and excellent mechanical property, and the defects in the prior art are overcome.
The invention aims to provide an LED composite packaging material, which comprises the following components in parts by weight:
20-25 parts of bisphenol A type epoxy resin
Hydantoin epoxy resin 15-20 parts
2-4 parts of modified silicon carbide
5-8 parts of inorganic filler
5-10 parts of curing agent
3-5 parts of antioxidant
10-15 parts of a diluent;
wherein the modified silicon carbide is obtained by reacting gallic acid modified silane coupling agent with silicon carbide.
Further, the preparation method of the modified silicon carbide comprises the following steps:
s1, mixing gallic acid, a silane coupling agent and a catalyst, heating, stirring, reacting, and filtering to obtain a modified silane coupling agent;
s2, adding silicon carbide into the solution of the modified silane coupling agent, heating for reaction under the protection of inert gas, and purifying to obtain the modified silicon carbide.
Further, in the step S1, the molar ratio of the gallic acid to the silane coupling agent is 1 (8-12).
Further, in the step S1, the temperature of the heating and stirring reaction is 70-80 ℃ and the time is 3-6 h.
Further, in step S2, the temperature of the heating reaction is 80-90 ℃ and the time is 2-5 h.
Further, the silane coupling agent is an epoxy silane coupling agent.
Further, the curing agent is one or more selected from diethylaminopropylamine, dipropylenetriamine, trimethylhexamethylenediamine and trimethylhexamethylenediamine.
Further, the antioxidant is selected from one or more of tri (2, 4-di-tert-butylphenyl) phosphite, p-phenylenediamine, dihydroquinoline, 2, 6-di-tert-butyl-4-methylphenol and didodecyl alcohol ester.
The invention also provides a preparation method of the LED composite packaging material, which comprises the following steps:
adding bisphenol A epoxy resin, hydantoin epoxy resin, modified silicon carbide and inorganic filler into a reaction kettle, heating and stirring, then adding a curing agent, an antioxidant and a diluent, uniformly stirring, defoaming, solidifying and cooling to obtain the LED composite packaging material.
The invention has the following beneficial effects:
according to the invention, gallic acid is reacted with an epoxy silane coupling agent to react epoxy ring opening with carboxyl to form ester, so that a modified silane coupling agent grafted with gallic acid is obtained, and then the modified silane coupling agent is further reacted with silicon carbide to obtain modified silicon carbide, so that a large amount of phenolic hydroxyl groups are introduced into the surface of the silicon carbide, on one hand, the reactivity of the modified silicon carbide is enhanced, and the modified silicon carbide is more easily fully crosslinked with active groups in components such as bisphenol A epoxy resin, hydantoin epoxy resin and the like, so that a more stable and three-dimensional structure is obtained; on the other hand, a large amount of organic oxygen-containing functional groups in each component are easier to form intermolecular forces (such as hydrogen bonds), so that the dispersibility of the components is effectively improved, the stability of the material is further enhanced, and the product has good stability and mechanical properties and has wide application prospect.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following examples are set forth. The starting materials, reactions and workup procedures used in the examples are those commonly practiced in the market and known to those skilled in the art unless otherwise indicated.
The words "preferred," "more preferred," and the like in the present disclosure refer to embodiments of the present disclosure that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
It should be understood that all numbers expressing, for example, amounts of ingredients used in the specification and claims, except in any operating example or otherwise indicated, are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention.
Bisphenol A epoxy resin in the embodiment of the invention is purchased from Yueyang petrochemical epoxy resin factories and industrial grade.
Hydantoin epoxy resin in the embodiment of the invention is purchased from Kang Disi chemical industry (Hubei) limited company and has the purity of 99 percent.
The inorganic filler in the embodiment of the invention is magnesium sulfate and aluminum oxide with the mass ratio of 1:1.
The curing agent in the embodiment of the invention is diethylaminopropylamine.
The antioxidant in the embodiment of the invention is 2, 6-di-tert-butyl-4-methylphenol.
The diluent in the embodiment of the invention is diglycidyl ether.
The preparation method of the modified silicon carbide comprises the following steps:
s1, adding gallic acid, KH560 (gallic acid: KH 560=1:8, n/n) and triphenylphosphine (0.5% of the total mass of reactants) into a reaction kettle, stirring at 70 ℃ for reaction for 4 h, cooling, and filtering to remove impurities to obtain a modified silane coupling agent;
s2, adding silicon carbide and the modified silane coupling agent into enough toluene (silicon carbide: modified silane coupling agent: toluene=50:1.5:350, m/m/m), reacting at 80 ℃ under nitrogen atmosphere for 4 h, cooling, filtering, washing and drying to obtain the modified silicon carbide.
The parts in the embodiment of the invention are all parts by weight.
Example 1
An LED composite packaging material comprises the following components in parts by weight:
bisphenol A type epoxy resin 20 parts
Hydantoin epoxy resin 15 parts
2 parts of modified silicon carbide
Inorganic filler 5 parts
5 parts of curing agent
Antioxidant 3 parts
10 parts of diluent.
The preparation method of the LED composite packaging material comprises the following steps:
adding bisphenol A epoxy resin, hydantoin epoxy resin, modified silicon carbide and inorganic filler into a reaction kettle according to the parts by weight, heating and stirring at 80 ℃, then adding a curing agent, an antioxidant and a diluent, stirring uniformly, then adding into a vacuum deaerating machine for deaeration, then adding into a mould for curing at 150 ℃ for 3 h, and cooling to obtain the LED composite packaging material.
Example 2
An LED composite packaging material comprises the following components in parts by weight:
bisphenol A type epoxy resin 25 parts
Hydantoin epoxy resin 20 parts
4 parts of modified silicon carbide
8 parts of inorganic filler
10 parts of curing agent
Antioxidant 5 parts
15 parts of diluent.
The preparation method of the LED composite packaging material comprises the following steps:
adding bisphenol A epoxy resin, hydantoin epoxy resin, modified silicon carbide and inorganic filler into a reaction kettle according to the parts by weight, heating and stirring at 80 ℃, then adding a curing agent, an antioxidant and a diluent, stirring uniformly, then adding into a vacuum deaerating machine for deaeration, then adding into a mould for curing at 150 ℃ for 3 h, and cooling to obtain the LED composite packaging material.
Example 3
An LED composite packaging material comprises the following components in parts by weight:
bisphenol A type epoxy resin 23 parts
Hydantoin epoxy resin 17 parts
3 parts of modified silicon carbide
Inorganic filler 7 parts
7 parts of curing agent
Antioxidant 4 parts
13 parts of diluent.
The preparation method of the LED composite packaging material comprises the following steps:
adding bisphenol A epoxy resin, hydantoin epoxy resin, modified silicon carbide and inorganic filler into a reaction kettle according to the parts by weight, heating and stirring at 80 ℃, then adding a curing agent, an antioxidant and a diluent, stirring uniformly, then adding into a vacuum deaerating machine for deaeration, then adding into a mould for curing at 150 ℃ for 3 h, and cooling to obtain the LED composite packaging material.
Comparative example 1
The difference between this comparative example and example 1 is that in the preparation method of modified silicon carbide, step S1 is omitted, and in step S2, the modified silane coupling agent is replaced with KH560 of equal mass, and other components and preparation methods are the same as in example 1.
Comparative example 2
An LED composite package material is different from example 1 in that modified silicon carbide is replaced with unmodified silicon carbide of equal mass, and other components and preparation methods are the same as example 1.
Test case
The LED composite packages prepared in example 1 and comparative examples 1-2 were subjected to performance testing.
The testing method comprises the following steps:
and performing performance tests such as hardness, refractive index and the like according to the standards such as GBT2411-2008 and GB/T6488.
Stability test: the initial luminous flux of the sample tested using the integrating sphere, and the luminous flux after 1000 h was lit, with 5% phosphor added.
The results obtained are shown in Table 1.
TABLE 1 Performance test results
Sample of Shore hardness of Refractive index Initial luminous flux (mlm) 1200 h luminous flux (mlm)
Example 1 70A 1.55 7560 7210
Comparative example 1 64A 1.54 7540 7090
Comparative example 2 61A 1.54 7540 7010
According to table 1, it can be seen that the LED composite packaging material prepared in the embodiment of the present invention has higher hardness and refractive index, and the luminous flux remains at a higher level after being lightened 1200-h, and the performance is excellent, while the performances of the comparative examples 1-2 of the replacement component are all reduced, and the stability is also weaker, which proves that the modified silicon carbide of the present invention has better compatibility with other components, and can form a more stable structure, and the performance of the LED composite packaging material is improved, so the present invention has good application prospects.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.

Claims (9)

1. The LED composite packaging material is characterized by comprising the following components in parts by weight:
20-25 parts of bisphenol A type epoxy resin
Hydantoin epoxy resin 15-20 parts
2-4 parts of modified silicon carbide
5-8 parts of inorganic filler
5-10 parts of curing agent
3-5 parts of antioxidant
10-15 parts of a diluent;
wherein the modified silicon carbide is obtained by reacting gallic acid modified silane coupling agent with silicon carbide.
2. The LED composite package material of claim 1, wherein the method of preparing the modified silicon carbide comprises the steps of:
s1, mixing gallic acid, a silane coupling agent and a catalyst, heating, stirring, reacting, and filtering to obtain a modified silane coupling agent;
s2, adding silicon carbide into the solution of the modified silane coupling agent, heating for reaction under the protection of inert gas, and purifying to obtain the modified silicon carbide.
3. The LED composite packaging material according to claim 2, wherein in step S1, the molar ratio of gallic acid to silane coupling agent is 1 (8-12).
4. The LED composite package according to claim 2, wherein in step S1, the temperature of the heating and stirring reaction is 70-80 ℃ for 3-6 h.
5. The LED composite package according to claim 2, wherein in step S2, the heating reaction is performed at a temperature of 80-90 ℃ for a time of 2-5 h.
6. The LED composite package material of claim 2, wherein the silane coupling agent is an epoxy silane coupling agent.
7. The LED composite encapsulant of claim 1, wherein the curing agent is selected from one or more of diethylaminopropylamine, dipropylenetriamine, trimethylhexamethylenediamine, and trimethylhexamethylenediamine.
8. The LED composite encapsulant of claim 1, wherein the antioxidant is selected from one or more of tris (2, 4-di-t-butylphenyl) phosphite, p-phenylenediamine, dihydroquinoline, 2, 6-di-t-butyl-4-methylphenol, didodecyl alcohol ester.
9. The method for preparing the LED composite packaging material according to any one of claims 1 to 8, comprising the steps of:
adding bisphenol A epoxy resin, hydantoin epoxy resin, modified silicon carbide and inorganic filler into a reaction kettle, heating and stirring, then adding a curing agent, an antioxidant and a diluent, uniformly stirring, defoaming, solidifying and cooling to obtain the LED composite packaging material.
CN202311354446.XA 2023-10-19 2023-10-19 LED composite packaging material and preparation method thereof Active CN117106286B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6562482B1 (en) * 1999-03-15 2003-05-13 Sumitomo Bakelite Company, Ltd. Liquid potting composition
CN101457133A (en) * 2009-01-09 2009-06-17 宜兴市江南药用化工厂 Lead accumulator epoxy resin sealant and preparation method thereof
JP2011225653A (en) * 2010-04-16 2011-11-10 Chubu Electric Power Co Inc Insulating polymer material composition and production method of the same
CN106317778A (en) * 2016-08-17 2017-01-11 安徽福恩光电科技有限公司 LED package material and preparation method thereof
CN113201271A (en) * 2021-04-23 2021-08-03 天津工业大学 Preparation method and application of high-voltage insulation silicon carbide-epoxy resin composite coating

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6562482B1 (en) * 1999-03-15 2003-05-13 Sumitomo Bakelite Company, Ltd. Liquid potting composition
CN101457133A (en) * 2009-01-09 2009-06-17 宜兴市江南药用化工厂 Lead accumulator epoxy resin sealant and preparation method thereof
JP2011225653A (en) * 2010-04-16 2011-11-10 Chubu Electric Power Co Inc Insulating polymer material composition and production method of the same
CN106317778A (en) * 2016-08-17 2017-01-11 安徽福恩光电科技有限公司 LED package material and preparation method thereof
CN113201271A (en) * 2021-04-23 2021-08-03 天津工业大学 Preparation method and application of high-voltage insulation silicon carbide-epoxy resin composite coating

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘科: "硅烷偶联剂KH560的改性及在铝合金表面的应用研究", 万方学位论文, pages 10 *
刘科: "硅烷偶联剂KH560的改性及在铝合金表面的应用研究", 中国优秀硕士学位论文全文数据库 *

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