CN106189249A - A kind of LED encapsulation material - Google Patents

A kind of LED encapsulation material Download PDF

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Publication number
CN106189249A
CN106189249A CN201610568770.5A CN201610568770A CN106189249A CN 106189249 A CN106189249 A CN 106189249A CN 201610568770 A CN201610568770 A CN 201610568770A CN 106189249 A CN106189249 A CN 106189249A
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CN
China
Prior art keywords
led encapsulation
encapsulation material
organic siliconresin
exchange resin
anion exchange
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CN201610568770.5A
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Chinese (zh)
Inventor
黄飞必
谢文省
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Individual
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Individual
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Priority to CN201610568770.5A priority Critical patent/CN106189249A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • C08L83/06Polysiloxanes containing silicon bound to oxygen-containing groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F212/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F212/02Monomers containing only one unsaturated aliphatic radical
    • C08F212/04Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06Hydrocarbons
    • C08F212/08Styrene
    • 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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

Abstract

Open a kind of LED encapsulation material of the present invention and preparation method thereof, methacrylate, organic siliconresin, benzene polyethers, styrene, butadiene, allene are put in reactor, heated and stirred, then phosphate ester flame retardants, melamine cyanurate, aluminium acetylacetonate and 1 are added, 2 dihydroxyanthraquinones, are heated to 140 160 DEG C, continue reaction 20 30min, then pour the mixture in mould and cool and solidify, the LED encapsulation material obtained.LED encapsulation material of the present invention is for the packaging technology of LED, and its intensity is big, and light transmission is good, the coefficient of expansion is low, heat conductivity is big, good heat dissipation effect, can be widely applied in the encapsulation technology of LED.

Description

A kind of LED encapsulation material
Technical field
The present invention relates to LED field, particularly to a kind of LED encapsulation material.
Background technology
Light emitting diode (English: Light-Emitting Diode is called for short LED) is that one can convert electrical energy into light The semiconductor electronic component of energy.This electronic component occurred as far back as 1962, can only send the HONGGUANG of low luminosity in early days, send out afterwards Putting on display other monochromatic versions, the light that can send even to this day is throughout visible ray, infrared ray and ultraviolet, and luminosity also improves To suitable luminosity.And purposes is also by the beginning as display lamp, display panel etc.;Along with the continuous progress of technology, light emitting diode Display, television set daylighting decoration and illumination it are widely used in.
The material requirements being presently used for LED encapsulation has intensity greatly, light transmission is good, the coefficient of expansion is low, heat conductivity is big, Good heat dissipation effect etc., otherwise can result in the problem reduced the service life of LED device.
Summary of the invention
In sum, the present invention is necessary to provide a kind of LED encapsulation material, and its intensity is big, and light transmission is good, the coefficient of expansion Low, heat conductivity is big, good heat dissipation effect, can be widely used in the encapsulation technology of LED.
Additionally, there is a need to provide a kind of preparation method preparing above-mentioned encapsulating material.
A kind of LED encapsulation material, including following material based on its weight portion:
Methacrylate 5-6 part;
Organic siliconresin 20-30 part;
Benzene polyethers 1-2 part;
Styrene 8-12 part;
Butadiene 5-8 part;
Allene 5-8 part;
Phosphate ester flame retardants 0.3-0.5 part;
Melamine cyanurate 0.3-0.5 part;
Aluminium acetylacetonate 0.5-0.8 part;
1,2-dihydroxyanthraquinone 0.5-0.8 part.
Wherein, above-mentioned LED encapsulation material includes that following material is based on its weight portion:
Methacrylate 5-6 part;
Organic siliconresin 23-25 part;
Benzene polyethers 1-2 part;
Styrene 10-12 part;
Butadiene 6-8 part;
Allene 6-8 part;
Phosphate ester flame retardants 0.3-0.5 part;
Melamine cyanurate 0.3-0.5 part;
Aluminium acetylacetonate 0.5-0.8 part;
1,2-dihydroxyanthraquinone 0.6-0.7 part.
Wherein, described organic siliconresin is prepared by the following method and obtains:
By 2-(3,4-7-oxa-bicyclo[4.1.0) ethyl trimethoxy silane and the diphenyl silanediol ratio with mol ratio as 1:0.5-0.8 Put under example in reactor, add the anion exchange resin of reactant gross mass 5%, react under conditions of temperature 60-70 DEG C 10-12 hour, after completion of the reaction, removing anion exchange resin, decompression removes low-boiling-point substance, obtains organic siliconresin.
Described anion exchange resin is basic anion exchange resin, can be selected from U.S. Amberlite, IRA- 400。
Described mode of heating can use oil bath pan heating and thermal insulation.
Wherein, described phosphate ester flame retardants is selected from bisphenol-A double (diphenyl phosphoester), resorcinol (diphenylphosphoric acid Ester) and triphenyl phosphorus at least one.
A kind of method preparing LED encapsulation material as above,
Step 1): by 2-(3,4-7-oxa-bicyclo[4.1.0) ethyl trimethoxy silane and diphenyl silanediol with mol ratio for 1: (0.5-0.8) put under ratio in reactor, add the basic anion exchange resin of reactant gross mass 5%, in temperature Reacting under conditions of 60-70 DEG C 10-12 hour, after completion of the reaction, remove anion exchange resin, decompression removes low-boiling-point substance, To organic siliconresin;
2) weight portion as shown in form prepares material, by methacrylate, organic siliconresin, benzene polyethers, styrene, fourth two Alkene, allene are put in reactor, are heated to 100-110 DEG C, stir 30-40min, then add phosphoric acid ester fire-retardant Agent, melamine cyanurate, aluminium acetylacetonate and 1,2-dihydroxyanthraquinone, it is heated to 140-160 DEG C, continues reaction 20- 30min, then pours the mixture in mould and cools and solidifies, and the LED encapsulation material obtained compares prior art, the present invention's LED encapsulation material, good insulating, the coefficient of expansion are low, heat conductivity is big, good heat dissipation effect and the LED encapsulation material of light weight
LED encapsulation material of the present invention is for the packaging technology of LED, and its intensity is big, and light transmission is good, the coefficient of expansion is low, lead Hot coefficient is big, good heat dissipation effect, can be widely applied in the encapsulation technology of LED.
Detailed description of the invention
Below in conjunction with some detailed description of the invention, the present invention is described further.Specific embodiment is the most specifically The bright present invention, non-limiting protection scope of the present invention.
Explanation to the material used by the present invention: material derives from commercially available.
Wherein, halogen-free flame retardants, from Clariant Corporation, trade mark OP1230.
Anion exchange resin is U.S. Amberlite, IRA-400.
Method of testing
Shore hardness:
Use the organosilicon after shore durometer (LA-X type) the test solidification of Hypon Instrument Ltd. of Wenzhou City The hardness of encapsulating material (thickness is about 15mm).
Transmittance: GB2410-80 transparent plastic light transmittance.
Thermostability:
Observe the defect of test piece, such as shrink mark, cutout and roughness under an optical microscope.When there are these defects, will Video disc is classified as substandard products.The result obtained with following ranking method evaluation.
In every 100 products, the quantity of substandard products is when 0-5, grade be A, 5-10 grade be B, when 11 or above, grade is C.
Expansion character: GB1036-70 linear expansion coefficient of plastics test method
Embodiment 1
The preparation method of LED encapsulation material
1) preparation method of organosilicon material:
By under 2-(3,4-7-oxa-bicyclo[4.1.0) ethyl trimethoxy silane and the diphenyl silanediol ratio with mol ratio as 1:0.5 Put in reactor, add the anion exchange resin of reactant gross mass 5%, under conditions of temperature 60-70 DEG C, react 10 little Time, after completion of the reaction, removing anion exchange resin, decompression removes low-boiling-point substance, obtains organic siliconresin;
2) weight portion as shown in form prepares material, by methacrylate, organic siliconresin, benzene polyethers, styrene, fourth two Alkene, allene are put in reactor, are heated to 100-110 DEG C, stir 30min, then add phosphate ester flame retardants, Melamine cyanurate, aluminium acetylacetonate and 1,2-dihydroxyanthraquinone, it is heated to 140-160 DEG C, continues reaction 20-30min, Then pour the mixture in mould and cool and solidify, the LED encapsulation material obtained.
Embodiment 2
1) preparation method of organosilicon material:
By under 2-(3,4-7-oxa-bicyclo[4.1.0) ethyl trimethoxy silane and the diphenyl silanediol ratio with mol ratio as 1:0.6 Put in reactor, add the anion exchange resin of reactant gross mass 5%, under conditions of temperature 60-70 DEG C, react 12 little Time, after completion of the reaction, removing anion exchange resin, decompression removes low-boiling-point substance, obtains organic siliconresin;
2) weight portion as shown in form prepares material, by methacrylate, organic siliconresin, benzene polyethers, styrene, fourth two Alkene, allene are put in reactor, are heated to 100-110 DEG C, stir 40min, then add phosphate ester flame retardants, Melamine cyanurate, aluminium acetylacetonate and 1,2-dihydroxyanthraquinone, it is heated to 140-160 DEG C, continues reaction 20-30min, Then pour the mixture in mould and cool and solidify, the LED encapsulation material obtained.
Embodiment 3
1) preparation method of organosilicon material:
By under 2-(3,4-7-oxa-bicyclo[4.1.0) ethyl trimethoxy silane and the diphenyl silanediol ratio with mol ratio as 1:0.7 Put in reactor, add the anion exchange resin of reactant gross mass 5%, under conditions of temperature 60-70 DEG C, react 11 little Time, after completion of the reaction, removing anion exchange resin, decompression removes low-boiling-point substance, obtains organic siliconresin;
2) weight portion as shown in form prepares material, by methacrylate, organic siliconresin, benzene polyethers, styrene, fourth two Alkene, allene are put in reactor, are heated to 100-110 DEG C, stir 30min, then add phosphate ester flame retardants, Melamine cyanurate, aluminium acetylacetonate and 1,2-dihydroxyanthraquinone, it is heated to 140-160 DEG C, continues reaction 20-30min, Then pour the mixture in mould and cool and solidify, the LED encapsulation material obtained.
Embodiment 4
1) preparation method of organosilicon material:
By under 2-(3,4-7-oxa-bicyclo[4.1.0) ethyl trimethoxy silane and the diphenyl silanediol ratio with mol ratio as 1:0.8 Put in reactor, add the anion exchange resin of reactant gross mass 5%, under conditions of temperature 60-70 DEG C, react 12 little Time, after completion of the reaction, removing anion exchange resin, decompression removes low-boiling-point substance, obtains organic siliconresin;
2) weight portion as shown in form prepares material, by methacrylate, organic siliconresin, benzene polyethers, styrene, fourth two Alkene, allene are put in reactor, are heated to 100-110 DEG C, stir 40min, then add phosphate ester flame retardants, Melamine cyanurate, aluminium acetylacetonate and 1,2-dihydroxyanthraquinone, it is heated to 140-160 DEG C, continues reaction 20-30min, Then pour the mixture in mould and cool and solidify, the LED encapsulation material obtained.
Embodiment 5
1) preparation method of organosilicon material:
By under 2-(3,4-7-oxa-bicyclo[4.1.0) ethyl trimethoxy silane and the diphenyl silanediol ratio with mol ratio as 1:0.5 Put in reactor, add the anion exchange resin of reactant gross mass 5%, under conditions of temperature 60-70 DEG C, react 10 little Time, after completion of the reaction, removing anion exchange resin, decompression removes low-boiling-point substance, obtains organic siliconresin;
2) weight portion as shown in form prepares material, by methacrylate, organic siliconresin, benzene polyethers, styrene, fourth two Alkene, allene are put in reactor, are heated to 100-110 DEG C, stir 30min, then add phosphate ester flame retardants, Melamine cyanurate, aluminium acetylacetonate and 1,2-dihydroxyanthraquinone, it is heated to 140-160 DEG C, continues reaction 20-30min, Then pour the mixture in mould and cool and solidify, the LED encapsulation material obtained.
Embodiment 6
Compared with Example 2, by methyl silicon resin, (being purchased from Laiyang Sheng Bang organosilicon Science and Technology Ltd., article number is SI- MQ102) replacing organic siliconresin prepared by the present invention, remaining is consistent with embodiment 2 with step with material formula, prepares LED Encapsulating material.
Table 1:
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Comparative example 1
Methacrylate 5 6 5 6 5
Organic siliconresin 20 30 25 23 20
Benzene polyethers 1 2 2 1 1
Styrene 8 12 10 8 8
Butadiene 5 8 8 6 5
Allene 5 8 8 6 5
Phosphate ester flame retardants 0.3 0.5 0.5 0.3 0.3
Melamine cyanurate 0.3 0.5 0.5 0.3 0.3
Aluminium acetylacetonate 0.5 0.8 0.6 0.8 0.5
1,2-dihydroxyanthraquinone 0.5 0.8 0.6 0.7 0
Table 2
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Comparative example 1 Comparative example 2
Shore hardness/A 68 67 67 66 62 59
Transmittance/% 98 98 98 98 92 95
Thermostability A A A A B B
Linear expansion coefficient/(× 10-5/ DEG C) 3 3.5 3.8 3.5 6 7
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every present invention of utilization says Equivalent structure or equivalence flow process that bright book content is made convert, or are directly or indirectly used in other relevant technical fields, all In like manner it is included in the scope of patent protection of the present invention.

Claims (5)

1. a LED encapsulation material, it is characterised in that include that following material is based on its weight portion:
Methacrylate 5-6 part;
Organic siliconresin 20-30 part;
Benzene polyethers 1-2 part;
Styrene 8-12 part;
Butadiene 5-8 part;
Allene 5-8 part;
Phosphate ester flame retardants 0.3-0.5 part;
Melamine cyanurate 0.3-0.5 part;
Aluminium acetylacetonate 0.5-0.8 part;
1,2-dihydroxyanthraquinone 0.5-0.8 part.
2. LED encapsulation material as claimed in claim 2, it is characterised in that include that following material is based on its weight portion::
Methacrylate 5-6 part;
Organic siliconresin 23-25 part;
Benzene polyethers 1-2 part;
Styrene 10-12 part;
Butadiene 6-8 part;
Allene 6-8 part;
Phosphate ester flame retardants 0.3-0.5 part;
Melamine cyanurate 0.3-0.5 part;
Aluminium acetylacetonate 0.5-0.8 part;
1,2-dihydroxyanthraquinone 0.6-0.7 part.
3. LED encapsulation material as claimed in claim 2, it is characterised in that described organic siliconresin is prepared by the following method Arrive:
By 2-(3,4-7-oxa-bicyclo[4.1.0) ethyl trimethoxy silane and the diphenyl silanediol ratio with mol ratio as 1:0.5-0.8 Put under example in reactor, add the anion exchange resin of reactant gross mass 5%, react under conditions of temperature 60-70 DEG C 10-12 hour, after completion of the reaction, removing anion exchange resin, decompression removes low-boiling-point substance, obtains organic siliconresin.
4. LED encapsulation material as claimed in claim 2, it is characterised in that:
Described phosphate ester flame retardants is selected from bisphenol-A double (diphenyl phosphoester), resorcinol (diphenyl phosphoester) and triphen At least one in base phosphorus.
5. the method for the LED encapsulation material prepared as described in any one of claim 1-4, it is characterised in that:
Step 1): by 2-(3,4-7-oxa-bicyclo[4.1.0) ethyl trimethoxy silane and diphenyl silanediol with mol ratio for 1: (0.5-0.8) put under ratio in reactor, add the basic anion exchange resin of reactant gross mass 5%, in temperature Reacting under conditions of 60-70 DEG C 10-12 hour, after completion of the reaction, remove anion exchange resin, decompression removes low-boiling-point substance, To organic siliconresin;
2) weight portion as shown in form prepares material, by methacrylate, organic siliconresin, benzene polyethers, styrene, fourth two Alkene, allene are put in reactor, are heated to 100-110 DEG C, stir 30-40min, then add phosphoric acid ester fire-retardant Agent, melamine cyanurate, aluminium acetylacetonate and 1,2-dihydroxyanthraquinone, it is heated to 140-160 DEG C, continues reaction 20- 30min, then pours the mixture in mould and cools and solidifies, the LED encapsulation material obtained.
CN201610568770.5A 2016-07-19 2016-07-19 A kind of LED encapsulation material Pending CN106189249A (en)

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Application Number Priority Date Filing Date Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108285633A (en) * 2017-12-25 2018-07-17 柳州璞智科技有限公司 A kind of encapsulating material and preparation method thereof
WO2021168954A1 (en) * 2020-02-28 2021-09-02 Tcl华星光电技术有限公司 Encapsulation fluorescent glue layer and manufacturing method therefor, and quantum dot backlight source
CN115894934A (en) * 2022-11-21 2023-04-04 江南大学 Phosphorus-containing polysiloxane, preparation method thereof and application of modified epoxy resin

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101302343A (en) * 2008-07-10 2008-11-12 天津市凯华绝缘材料有限公司 Flame-retardant organosilicon powder encapsulating material for electronic component
CN102115600A (en) * 2010-11-26 2011-07-06 苏州生益科技有限公司 Thermosetting resin composition, prepreg and laminated board
CN102719096A (en) * 2012-06-20 2012-10-10 广东汕头超声电子股份有限公司覆铜板厂 Resin composition and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101302343A (en) * 2008-07-10 2008-11-12 天津市凯华绝缘材料有限公司 Flame-retardant organosilicon powder encapsulating material for electronic component
CN102115600A (en) * 2010-11-26 2011-07-06 苏州生益科技有限公司 Thermosetting resin composition, prepreg and laminated board
CN102719096A (en) * 2012-06-20 2012-10-10 广东汕头超声电子股份有限公司覆铜板厂 Resin composition and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108285633A (en) * 2017-12-25 2018-07-17 柳州璞智科技有限公司 A kind of encapsulating material and preparation method thereof
WO2021168954A1 (en) * 2020-02-28 2021-09-02 Tcl华星光电技术有限公司 Encapsulation fluorescent glue layer and manufacturing method therefor, and quantum dot backlight source
US11870014B2 (en) 2020-02-28 2024-01-09 Tcl China Star Optoelectronics Technology Co., Ltd. Encapsulated fluorescent adhesive layer having a quantum dot material
CN115894934A (en) * 2022-11-21 2023-04-04 江南大学 Phosphorus-containing polysiloxane, preparation method thereof and application of modified epoxy resin

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