CN105602259A - Curable organic polysiloxane composition and application thereof - Google Patents

Curable organic polysiloxane composition and application thereof Download PDF

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Publication number
CN105602259A
CN105602259A CN201610148000.5A CN201610148000A CN105602259A CN 105602259 A CN105602259 A CN 105602259A CN 201610148000 A CN201610148000 A CN 201610148000A CN 105602259 A CN105602259 A CN 105602259A
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CN
China
Prior art keywords
magnesium
composition
organic polysiloxane
organopolysiloxane composition
polysiloxane composition
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201610148000.5A
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Chinese (zh)
Inventor
宋宁冈
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Dongguan Tisky Electronic Co Ltd
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Dongguan Tisky Electronic Co Ltd
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Application filed by Dongguan Tisky Electronic Co Ltd filed Critical Dongguan Tisky Electronic Co Ltd
Priority to CN201610148000.5A priority Critical patent/CN105602259A/en
Publication of CN105602259A publication Critical patent/CN105602259A/en
Priority to JP2017004246A priority patent/JP2017165943A/en
Pending legal-status Critical Current

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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
    • 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
    • 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
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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

Abstract

The invention discloses a curable organic polysiloxane composition. The composition is one or more of magnesium oxide, magnesium hydroxide, magnesium carbonate, hydrotalcite, hydrotalcite-like compounds and britesorb. The organic polysiloxane composition added in a semiconductor of a light-emitting component can be used for effectively inhibiting penetration of hydrogen sulfide or sulfide under the condition that the original light-emitting efficiency is not influenced, so that the silver layer is prevented from being oxidized to achieve the effect of effectively protecting the silver layer, and the effect of resisting vulcanization is improved.

Description

A kind of curable organopolysiloxane composition and application thereof
Technical field
The present invention relates to a kind of curable organopolysiloxane composition and the semiconductor device at light-emitting component thereofApplication in part.
Background technology
Contain the organopolysiloxane compound that phenyl-alkyl-thiazolinyl and silicon bond are closed, comprise straight bond structure and Zhi JianStructure. The reaction of Tonghua hydrosilanes, taking organic platinum as catalyst, alkynes ene compound is working time adjusting agent,Suitably appropriate fluorescent material, as light efficiency adjusting agent, forms a kind of curable organopolysiloxane composition,The protection sealant that is applied in widely LED bis-utmost point illuminators is industrial, forms a kind of printing opacity, and refractive index exists1.40~1.57 resinite. The photoelectric coupling effect of light-emittingdiode, sheds by stamen sheet electricity with the form of light,By the effect of electrodeless fluorescent powder, form photoelectric subassembly miscellaneous, be used on demonstration and lighting industry.This photoelectric subassembly, is reflected away light by the silver-plated laminate of bottom, reaches certain photoelectricity usefulness.
But the organopolysiloxane structure of the above-mentioned type, no matter refractive index or hardness level have certainGas penetration rate. In large natural environment, or in electronics, electrical equipment, combination of devices thing, have certain alwaysThe hydrogen sulfide of content or sulfide, this kind of sulfide penetrated organopolysiloxane in be everlasting normal temperature or high temperatureCoating, is accumulated on the silver layer of bottom, has formed dark-coloured silver sulfide, makes the assembly of light-emittingdiode graduallyGradually light cannot be reflected away and cause light decay. This kind of phenomenon perplexing diode encapsulation dealer always, and it alsoSeeking better solution always.
Summary of the invention
The object of this invention is to provide a kind of curable organopolysiloxane composition, said composition can beDo not affect under the condition of original light extraction efficiency, can very effective obstruct hydrogen sulfide or the penetrating of sulfide,Avoid silver layer oxidized, play a kind of effectiveness of effective protection silver layer, improved anti-cure efficiency.
For achieving the above object, technical scheme of the present invention is:
A curable organopolysiloxane composition, is characterized in that: described composition also comprises magnesiumInorganic matter, the inorganic content of described magnesium is 0.1~50%wt%, particle size is 0.01~50 micron;
A curable organopolysiloxane composition, the inorganic matter of described magnesium be magnesia, magnesium hydroxide,One or more in magnesium carbonate, hydrotalcite, houghite and magnesium silicate salt;
The inorganic content of described magnesium is 0.1~20%wt%, is preferably 3~10wt%, and particle size is 0.01~20Micron, is preferably 0.1~20 micron;
Having the present invention also aims to provide a kind of answers described curable organopolysiloxane compositionBe used in the method in the semiconductor devices of luminescence component.
In addition, only otherwise damage object of the present invention, the present invention can contain suitable heat stabilizer, pigment,Then auxiliary agent, anti-heavy agent etc. are as optional component.
The technique effect that the present invention obtains is:
(1) compare with the organopolysiloxane composition that does not contain magnesium salts, add respectively 3%, 5%, 10%Magnesium hydroxide, be encapsulated on the assembly of light-emittingdiode, then put into the appearance of closing dress environment sulfur-bearing powder and waterIn device, deposit with the temperature of 85 DEG C. After 7 hours, not hydrogeneous magnesian organopolysiloxane composition groupPart, light emission rate, by 28 lumens, becomes 20 lumens, has decayed nearly 29%; And containing 3%, 5%, 10% hydrogen-oxygenThe organopolysiloxane composition assembly of changing magnesium, light emission rate, by 28 lumens, becomes respectively 27.3 lumens, 27.8Lumen, 28 lumens, decay only has 2.5%, 0.7% and undamped.
(2) the present invention by creatively adding the inorganic matter of magnesium, simultaneously in organopolysiloxane compositionIn conjunction with content and the particle size thereof of preferred magnesium inorganic matter, do not affecting under the condition of original light extraction efficiency,Can very effective obstruct hydrogen sulfide or the penetrating of sulfide, avoid silver layer oxidized, play one veryEffectively the effectiveness of protection silver layer, has improved anti-cure efficiency, adds after the inorganic salts of magnesium, and brightness decay existsBelow 2%. Simultaneously this type of preferred magnesium inorganic matter is in solidification process and have concurrently and prevent expecting of fluorescent material sedimentationLess than technique effect.
Detailed description of the invention
Enforcement project and condition:
1. hot and humid Reflow Soldering: place 24 hours in 85 DEG C and 85%RH case, take out after drying and enter265 DEG C of Reflow Soldering tunnels, 5 minutes two bouts.
2. high temperature ageing: 200 DEG C of heated-air circulation ovens are placed 72 hours.
3. cold cycling :-40 DEG C~100 DEG C single-channel type boards, 20 times circulations/day, totally 10 days.
4. sulfuration: in 20 liters of closed containers (30 centimeters of diameters, 30 centimeters of height), contain into 10 bottomG Cosan and mineral water 300CC face down lamp pearl justifying to be measured to be attached in container head. InsertIn 80 DEG C of circulation constant temperature baking ovens 8 hours. Then take out the corrosion on silver-colored pin on support is clashed clean, then withInspection machine testing brightness (Lv) and colour temperature before special lamp pearl.
5. nude film penetrance: spectrophotometer is at the penetrance % of 420nm (optical path 10mm).
6. hardness: measure in ASTMD2240D mode.
Embodiment 1:
By the polymethyl-benzene base silicon resin copolymer that contains silicon bond vinyl, and contain the poly-of silicon bond hydrogen baseMethyl phenyl silicone resin polymer, evenly mixes. Wherein silicon bond contents of ethylene 4.5wt%, silicon bond hydrogenBase content 0.13wt%, silicon bond phenyl content 49wt%. Coordinate upper 1,3-divinyl-1,1,3,3-tetra-The platinum complex of methyl disiloxane is as catalyst. (platinum accounts for general construction weight 3ppm) coordinates 1-acetylene againBasic ring hexanol is as working time adjusting agent. (accounting for general construction weight 150ppm) full and uniform mixing of above compositionAfter, viscosity is 3500cps at 25 DEG C. This thing is evenly divided into three parts, is respectively (A) (B) (C).
(A) be used as blank test;
(B) sneak into magnesium hydroxide (Sigma-AldrichcompanyU.S.A reagent level, the purity of wt3%95%);
(C) sneak into the above-mentioned magnesium hydroxide of wt5%;
In (A), (B), (C), add respectively again YAG fluorescent material Y959, wt10%. Mixing also vacuum removesAfter bubble, with the positive displacement point gum machine MPP-1 of Japan musashi company, click and enter the three stamen chips that are of a size of 5050In the body support frame of (0.2W × 3) luminous the two poles of the earth (every 8 × 15 lamp beads). Then be introduced into 80 DEG C of hot air circulationIn baking oven, toast one hour, then enter in 150 DEG C of heated-air circulation ovens two hours, take out and put coldly, do follow-upReliability test.
Reliability result
(every 8 × 15, the average result of totally 120)
Table 1
Separately with (A) (B) (C) do not add fluorescent material, directly make the transparent nude film of 20mm × 50mm × 1mm (thickness)
Table 2
Embodiment 2
By the polymethyl-benzene base silicon resin copolymer that contains silicon bond vinyl, and the poly-methyl that contains silicon bond hydrogen basePhenyl polysiloxane polymer, all in mixing. Wherein silicon bond contents of ethylene 4.7wt%, silicon bond hydrogen base containAmount 0.14wt%, silicon bond phenyl content 49wt%. Coordinate upper 1,3-divinyl-1,1,3,3-tetramethylThe platinum complex of disiloxane is as catalyst. (platinum accounts for general construction weight 3ppm) coordinates 1-acetylene basic ring againHexanol is as working time adjusting agent. After (accounting for general construction weight 150ppm) full and uniform mixing of above composition,Viscosity is 3500cps at 25 DEG C. This thing is evenly divided into three parts, is respectively (A) (B) (C).
(A) be used as blank test
(B) sneak into magnesia (Sigma-AldrichcompanyU.S.A reagent level, the specific area of wt5%130 ㎡/g, particle diameter < 25 μ m (XRD)).
(C) (Sigma-AldrichcompanyU.S.A.10 μ m) to sneak into the talcum powder of wt5%.
In (A), (B), (C), add respectively again YAG fluorescent material Y959, wt10%.
Mix and froth in vacuum after, with the positive displacement point gum machine MPP-1 of Japan musashi company, click and enter and be of a size ofIn the three luminous the two poles of the earth of stamen chip (0.2W × 3) body support frames of 5050 (every 8 × 15 lamp beads). Then advancedEnter in 80 DEG C of heated-air circulation ovens and toast one hour, then enter in 150 DEG C of heated-air circulation ovens two hours, getGo out to put cold, do the test of follow-up reliability.
Reliability result
(every 8 × 15, the average result of totally 120)
Table 3
Separately with (A) (B) (C) do not add fluorescent material, directly make the transparent nude film of 20mm × 50mm × 1mm (thickness)
Table 4
From above table, can find out, in organopolysiloxane, add after the inorganic salts of magnesium, putting down before sulfurationAll brightness is uninfluenced, can effectively intercept penetrating of hydrogen sulfide or sulfide simultaneously, avoids silver layer oxidized,Play a kind of effectiveness of very effective protection silver layer, improved anti-cure efficiency, and add the inorganic salts of magnesiumAfter, brightness decay is below 2%.

Claims (4)

1. a curable organopolysiloxane composition, is characterized in that: described composition also comprises magnesiumInorganic matter, the inorganic content of described magnesium is 0.1~50%wt%, particle size is 0.01~50 micron.
2. a kind of curable organopolysiloxane composition as claimed in claim 1, is characterized in that: instituteThe inorganic matter of stating magnesium is magnesia, magnesium hydroxide, magnesium carbonate, hydrotalcite, houghite and magnesium silicate saltIn one or more.
3. a kind of curable organopolysiloxane composition as claimed in claim 1 or 2, is characterized in that:The inorganic content of described magnesium is 0.1~20%wt%, and particle size is 0.01~20 micron.
4. in claim 1-3, the curable organopolysiloxane composition described in any one claim is being sent outApplication in the semiconductor devices of optical assembly.
CN201610148000.5A 2016-03-15 2016-03-15 Curable organic polysiloxane composition and application thereof Pending CN105602259A (en)

Priority Applications (2)

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CN201610148000.5A CN105602259A (en) 2016-03-15 2016-03-15 Curable organic polysiloxane composition and application thereof
JP2017004246A JP2017165943A (en) 2016-03-15 2017-01-13 Curable organic polysiloxane composition and application thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113686763A (en) * 2021-07-20 2021-11-23 华南理工大学 Evaluation method for vulcanization resistance

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CN103827216A (en) * 2011-07-22 2014-05-28 Lg化学株式会社 Curable composition
CN104164197A (en) * 2013-05-17 2014-11-26 达兴材料股份有限公司 Packaging adhesive for light-emitting device and light-emitting device

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JP2006206816A (en) * 2005-01-31 2006-08-10 Ge Toshiba Silicones Co Ltd Room temperature-curable polyorganosiloxane composition
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CN102329501A (en) * 2010-03-30 2012-01-25 信越化学工业株式会社 Resin composition, reflector for light-emitting semiconductor device, and light-emitting semiconductor unit
CN103827216A (en) * 2011-07-22 2014-05-28 Lg化学株式会社 Curable composition
CN104164197A (en) * 2013-05-17 2014-11-26 达兴材料股份有限公司 Packaging adhesive for light-emitting device and light-emitting device

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Publication number Priority date Publication date Assignee Title
CN113686763A (en) * 2021-07-20 2021-11-23 华南理工大学 Evaluation method for vulcanization resistance

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Application publication date: 20160525