CN101016446A - Organosilicon electronic encapsulation material - Google Patents
Organosilicon electronic encapsulation material Download PDFInfo
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- CN101016446A CN101016446A CN 200710027003 CN200710027003A CN101016446A CN 101016446 A CN101016446 A CN 101016446A CN 200710027003 CN200710027003 CN 200710027003 CN 200710027003 A CN200710027003 A CN 200710027003A CN 101016446 A CN101016446 A CN 101016446A
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- ethenyl blocking
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Abstract
The invention discloses a organic silicon embedding material in embedding technical domain of electronic product, which is characterized by the following: It is composed by 100 wt ethenyl dead-end polymethyl phenyl group phenyl group oxosilane, 10-30 wt ethenyl metyl group silicon resin, 5-20 wt poly metyl group hydrogen phenyl group, 0.1-2 wt accelerant and 0.05-2 wt blocking agent, which is based on ethenyl dead-end polymethyl phenyl group phenyl group oxosilane. The light transmittance ratio of this material can reach 99% and refractive index can reach 1.49-1.53, which is fit for packaging of LED electronic product.
Description
Technical field:
The present invention relates to the encapsulation technology field of electronic product, refer in particular to a kind of organosilicon electronic encapsulation material.
Background technology:
Electronics embedding development so far, oneself has obtained very big progress, at present more general electronic encapsulation material mainly is made up of Resins, epoxy or urethane resin, solidifying agent, promotor, toughner, filler, thixotropic agent etc., but adopt Resins, epoxy to face many difficulties, as thermotolerance problem, wet fastness problem, internal stress problem etc. as the raw material Development of Packaging Technology.Such as, poor heat resistance is an extremely adverse factors concerning the LED encapsulation, damages element easily, and reduction of service life, same, moisture resistance properties is low, and aqueous vapor enters element internal, causes easily short circuit to burn out element.In addition, because of epoxide resin material only just can have certain mechanical property and other use propertieies after curing, it mainly is because the epoxide group in the Resins, epoxy and the ring opening polyaddition reaction between the solidifying agent or ring-opening polymerization and solidified, and contain sulphur in the solidifying agent that has, easily environment is polluted, be unfavorable for environmental protection.So variety of problems has restricted the development of electronics embedding, does not conform to the flourish electron trade utmost point, therefore, needs a kind of high performance packaged material to substitute present Resins, epoxy.This novel organic silicon electronic packaged material can solve several hang-ups in the electronic encapsulation material, as problems such as thermotolerance, wet fastness, shrinkabilitys, can produce more effective packaging effect, increase the service life, particularly for the packaged material of high-capacity LED, a kind of solution is provided, has impelled the sound development of electronic applications products such as LED.
The composition that is made into ethenyl blocking PSI, poly-methyl hydrogen phenyl siloxane, platinum catalyst and inhibitor early has report [CN1009938B], but similar compositions is used for yet there are no report in the electronics embedding; And also there is following shortcoming in top patent of invention for the electronics embedding: one, used inhibitor is organic-silicon-modified, the boiling point height, to storage, the operating time is highly beneficial, but resulting need could curing at (more than 400 ℃) under the very high temperature is not fit to the electronics embedding; Two, in the composition without any supporting material, the cured product poor mechanical properties that obtains also is not suitable for the electronics embedding.
At above present situation, the invention provides a kind of silicon composition, be used for the electronics embedding; In addition, the present invention also provides a kind of preparation method of ethenyl blocking PSI.
Summary of the invention:
The objective of the invention is to overcome the weak point of existing electronic encapsulation material, a kind of organosilicon electronic encapsulation material is provided.
This material of organosilicon electronic encapsulation material of the present invention system by: ethenyl blocking PSI, vinyl methyl silicon resin, poly-methyl hydrogen phenyl siloxane, catalyzer and inhibitor mixed form, and its mass ratio (is reference with the ethenyl blocking PSI) is:
100 parts of ethenyl blocking PSIs
10～30 parts of vinyl methyl silicon resins
5～20 parts of poly-methyl hydrogen phenyl siloxanes
0.1～2 part of catalyzer
0.05～2 part in inhibitor.
Particularly, the structure of the ethenyl blocking PSI that is adopted among the present invention is:
Wherein integer a, b, c, span be respectively: a=10～200, b=5～100, c=3～20, R is-CH
3Or-CH=CH
2The rare basic phenyl polysiloxane of described methyl second can be made by following method: get methylsiloxane ring body 100 mass parts, phenyl siloxane ring body 50～100 mass parts, vinylsiloxane end-capping reagent 2～10 mass parts, silicon alkoxide catalyzer 0.05～0.2 mass parts of KOH made at 160～180 ℃ of following stirring reactions in 6～10 hours; And wherein the structural formula of methylsiloxane ring body is:
Integer α=3～5 in the formula
The phenyl siloxane ring body is:
Integer β=3～5 in the formula
The structural formula of vinylsiloxane end-capping reagent is:
Integer θ=0～10 in the formula.
The structure of the poly-methyl hydrogen phenyl siloxane that is adopted among the present invention is:
Wherein the span of integer m, n, p is respectively m=0～50, n=5～30, p=3～30.
The structural formula of described vinyl methyl silicon resin is:
[(CH
3)
3SiO
0.5]
x[(CH
3)
2(CH
2=CH) SiO
0.5]
y(SiO
2)
z, (x+y)/z=0.5～1 wherein.
Described catalyzer is a platinum catalyst, i.e. the title complex of platinum, and in the catalyzer content of platinum between 1200～6000ppm.
Described inhibitor is an alkynol, and in the alkynol carbon atom number less than 15.
Organosilicon electronic encapsulation material of the present invention, manufacture craft and flow process are simple, and adopt Embedding Material of the present invention, performances such as product thermotolerance, wet fastness, shrinkability all improve greatly, can produce more effective packaging effect, increase the service life, and the material transmittance can reach 99%, specific refractory power can reach 1.49～1.53, is suitable for very much the encapsulation of electronic products such as LED.
Embodiment:
The present invention is further described for following embodiment.
Example 1
Get clean 500ml there-necked flask, to wherein adding octamethylcyclotetrasiloxane 100g, octaphenyl cyclotetrasiloxane 50g, structural formula are (CH
2=CH) (CH
3)
2SiOSi (CH
3)
2(CH=CH
2) end-capping reagent 2g, siloxanes potassium alcoholate catalyzer 0.1g after 8 hours, adds (Me at 160～180 ℃ of following stirring reactions
3SiO)
2The OHP=O neutralization is until till the neutrality, remove low-boiling-point substance under the vacuum then; Be cooled to room temperature, filtration can obtain water white ethenyl blocking PSI, and viscosity is 1100mpaS (25 ℃).
Get above-mentioned ethenyl blocking PSI 100g, get the poly-methyl hydrogen phenyl siloxane 10g of viscosity 100mpaS (25 ℃) again, viscosity is 800mpaS (25 ℃) vinyl methyl silicon resin 20g, ethylene methacrylic radical siloxane coordinate platinum catalyst 0.2g, methylparafynol 0.15g stirs, row's bubble, inject in the mould of a 2mm * 13mm * 13mm, toasted 1 hour down, make it to be shaped to the silica gel sheet at 150 ℃.
Example 2
Get clean 500ml there-necked flask, to wherein adding octamethylcyclotetrasiloxane 100g, octaphenyl cyclotetrasiloxane 100g, structural formula are (CH
2=CH) (CH
3)
2SiOSi (CH
3)
2OSi (CH
3)
2(CH=CH
2) end-capping reagent 2g, siloxanes potassium alcoholate catalyzer 0.1g after 8 hours, adds (Me at 160～180 ℃ of following stirring reactions
3SiO) (OH)
2The P=O neutralization is until till the neutrality, remove low-boiling-point substance under the vacuum; Be cooled to room temperature, filtration can obtain the ethenyl blocking PSI that water white viscosity is 1300mpaS (25 ℃).
Get above-mentioned ethenyl blocking PSI 100g, get the poly-methyl hydrogen phenyl siloxane 15g of viscosity 100mpaS (25 ℃) again, viscosity is the vinyl methyl silicon resin 30g of 600mpaS (25 ℃), tetrahydrofuran (THF) coordinate platinum catalyst 0.3g, methylparafynol 0.15g stirs, row's bubble, inject in the mould of 2mmx13mmx13mm, toasted 1 hour down, make it to be shaped to the silica gel sheet at 150 ℃.
Product (existing example: extracting epoxy resin 100g with the making of materials such as product of the present invention and available technology adopting Resins, epoxy, amine curing agent 15g, row's bubble, inject in the mould of 2mm * 13mm * 13mm, toasted 1 hour down at 150 ℃, take out the matrix of moulding, carry out the performance analysis contrast, utilize spectrophotometric to measure transmittance, utilize refractometer to measure specific refractory power; And do anti-ultraviolet, humidity resistance and Elongation test, test result such as following table:
By above table as can be known, the packaged material product that adopts the present invention to make, not only transmittance can reach existing high level, and performances such as the specific refractory power of product, elongation, cure shrinkage, UV resistant, humidity resistance are all significantly improved, help improving the packaging effect of product and the success ratio of encapsulation, increase product work-ing life.
Claims (7)
1. organosilicon electronic encapsulation material, it is characterized in that: this material system by: ethenyl blocking PSI, vinyl methyl silicon resin, poly-methyl hydrogen phenyl siloxane, catalyzer and inhibitor mixed form, and its mass ratio (is reference with the ethenyl blocking PSI) is:
100 parts of ethenyl blocking PSIs
10～30 parts of vinyl methyl silicon resins
5～20 parts of poly-methyl hydrogen phenyl siloxanes
0.1～2 part of catalyzer
0.05～2 part in inhibitor.
2. a kind of organosilicon electronic encapsulation material according to claim 1 is characterized in that: the structure of described ethenyl blocking PSI is:
Wherein integer a, b, c, span be respectively: a=10～200, b=5～100, c=3～20, R is-CH
3Or-CH=CH
2
3. a kind of organosilicon electronic encapsulation material according to claim 1 is characterized in that:
The structure of described poly-methyl hydrogen phenyl siloxane is
Wherein the span of integer m, n, p is respectively m=0～50, n=5～30, p=3～30.
4. a kind of organosilicon electronic encapsulation material according to claim 1 is characterized in that: the structural formula of described vinyl methyl silicon resin is:
[(CH
3)
3SiO
0.5]
x[(CH
3)
2(CH
2=CH) SiO
0.5]
y(SiO
2)
z, (x+y)/z=0.5～1 wherein.
5. a kind of organosilicon electronic encapsulation material according to claim 1 is characterized in that:
Described catalyzer is a platinum catalyst, i.e. the title complex of platinum, and in the catalyzer content of platinum between 1200～6000ppm.
6. a kind of organosilicon electronic encapsulation material according to claim 1 is characterized in that: described inhibitor is an alkynol, and in the alkynol carbon atom number less than 15.
7. a kind of organosilicon electronic encapsulation material according to claim 1 and 2 is characterized in that: the making method of described ethenyl blocking PSI is as follows:
Get methylsiloxane ring body 100 mass parts, phenyl siloxane ring body 50～100 mass parts, vinylsiloxane end-capping reagent 2～10 mass parts, siloxanes potassium alcoholate catalyzer 0.05～0.2 mass parts, after 160-180 ℃ of following stirring reaction 6-10 hour, with silica-based phosphoric acid ester neutralization, until till the neutrality, deviate to hang down then and boil, promptly get the ethenyl blocking PSI; And wherein the structural formula of methylsiloxane ring body is:
α=3-5 in the formula
The phenyl siloxane ring body is:
β=3-5 in the formula
The structural formula of vinylsiloxane end-capping reagent is:
θ=0-10 in the formula.
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|---|---|---|---|
| CN 200710027003 CN101016446A (en) | 2007-02-15 | 2007-02-15 | Organosilicon electronic encapsulation material |
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|---|---|---|---|
| CN 200710027003 CN101016446A (en) | 2007-02-15 | 2007-02-15 | Organosilicon electronic encapsulation material |
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|---|---|
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Family
ID=38725669
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101872832A (en) * | 2010-06-13 | 2010-10-27 | 汕头市骏码凯撒有限公司 | Packaging material applied to light-emitting diode (LED) and preparation method and using method thereof |
| CN101875725A (en) * | 2010-07-14 | 2010-11-03 | 广州市高士实业有限公司 | Vinyl silicon resin for reinforcing organic silicon pouring sealant and preparation method thereof |
| CN101475689B (en) * | 2008-12-03 | 2011-01-12 | 杭州师范大学 | Preparation of methyl phenyl vinyl silicon resin |
| CN101608068B (en) * | 2009-07-10 | 2011-09-07 | 茂名市信翼化工有限公司 | Organ silicon material for encapsulating power-type LED and synthetic method thereof |
| CN101381516B (en) * | 2008-10-23 | 2011-11-23 | 上海大学 | Room temperature vulcanized organosilicon pouring sealant for LED |
| CN101693765B (en) * | 2009-10-19 | 2012-03-21 | 株洲时代电气绝缘有限责任公司 | Organic silicon perfusion resin and preparation method thereof |
| CN102382617A (en) * | 2011-08-25 | 2012-03-21 | 江苏创景科技有限公司 | Single-component high-strength transparent organic silicon potting adhesive and preparation method thereof |
| CN101508882B (en) * | 2009-03-30 | 2012-09-19 | 汕头市骏码凯撒有限公司 | Encapsulating material applied to LED and method of preparing the same |
| CN102863799A (en) * | 2012-10-17 | 2013-01-09 | 东莞市贝特利新材料有限公司 | High-refractive-index organosilicon material for light-emitting diode (LED) packaging and preparation method of high-refractive-index organosilicon material |
| CN102993753A (en) * | 2012-11-23 | 2013-03-27 | 中科院广州化学有限公司 | Composite hybrid organic silicon LED (Light Emitting Diode) packaging material, preparation method and applications thereof |
| CN103122149A (en) * | 2013-03-18 | 2013-05-29 | 株洲时代新材料科技股份有限公司 | Silicon rubber with high refractive index and high transparency for optical encapsulation and preparation method thereof |
| CN103773235A (en) * | 2014-01-22 | 2014-05-07 | 冠研（上海）企业管理咨询有限公司 | Preparation method of primer for addition type organosilicone potting adhesive |
| CN103788872A (en) * | 2014-01-22 | 2014-05-14 | 上海铂优新材料有限公司 | Primer for addition type organic silicon pouring sealant |
| CN104151839A (en) * | 2014-08-08 | 2014-11-19 | 广东省工业技术研究院(广州有色金属研究院) | Phenyl silicone resin for optical fiber matching block |
| CN105348809A (en) * | 2015-12-17 | 2016-02-24 | 刘爱华 | Novel organic siloxane polymer material for electronic packaging |
| CN105384935A (en) * | 2015-12-16 | 2016-03-09 | 烟台德邦先进硅材料有限公司 | Vinyl-terminated polydimethyldiphenylsiloxane synthesis method |
| CN105585957A (en) * | 2014-10-22 | 2016-05-18 | 株洲时代新材料科技股份有限公司 | Silicone impregnating varnish, and preparing method and applications thereof |
| CN106977723A (en) * | 2017-04-28 | 2017-07-25 | 深圳天鼎新材料有限公司 | End-vinyl phenyl silicone oil, preparation method and the usage |
| WO2019051742A1 (en) * | 2017-09-14 | 2019-03-21 | 韦荣群 | Method for preparing highly transparent silicone rubber having uv-absorption capability |
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2007
- 2007-02-15 CN CN 200710027003 patent/CN101016446A/en active Pending
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|---|---|---|---|---|
| CN101381516B (en) * | 2008-10-23 | 2011-11-23 | 上海大学 | Room temperature vulcanized organosilicon pouring sealant for LED |
| CN101475689B (en) * | 2008-12-03 | 2011-01-12 | 杭州师范大学 | Preparation of methyl phenyl vinyl silicon resin |
| CN101508882B (en) * | 2009-03-30 | 2012-09-19 | 汕头市骏码凯撒有限公司 | Encapsulating material applied to LED and method of preparing the same |
| CN101608068B (en) * | 2009-07-10 | 2011-09-07 | 茂名市信翼化工有限公司 | Organ silicon material for encapsulating power-type LED and synthetic method thereof |
| CN101693765B (en) * | 2009-10-19 | 2012-03-21 | 株洲时代电气绝缘有限责任公司 | Organic silicon perfusion resin and preparation method thereof |
| CN101872832B (en) * | 2010-06-13 | 2013-03-06 | 汕头市骏码凯撒有限公司 | Packaging material applied to light-emitting diode (LED) and preparation method and using method thereof |
| CN101872832A (en) * | 2010-06-13 | 2010-10-27 | 汕头市骏码凯撒有限公司 | Packaging material applied to light-emitting diode (LED) and preparation method and using method thereof |
| CN101875725A (en) * | 2010-07-14 | 2010-11-03 | 广州市高士实业有限公司 | Vinyl silicon resin for reinforcing organic silicon pouring sealant and preparation method thereof |
| CN101875725B (en) * | 2010-07-14 | 2013-01-02 | 广州市高士实业有限公司 | Vinyl silicon resin for reinforcing organic silicon pouring sealant and preparation method thereof |
| CN102382617A (en) * | 2011-08-25 | 2012-03-21 | 江苏创景科技有限公司 | Single-component high-strength transparent organic silicon potting adhesive and preparation method thereof |
| CN102863799A (en) * | 2012-10-17 | 2013-01-09 | 东莞市贝特利新材料有限公司 | High-refractive-index organosilicon material for light-emitting diode (LED) packaging and preparation method of high-refractive-index organosilicon material |
| CN102863799B (en) * | 2012-10-17 | 2014-02-26 | 东莞市贝特利新材料有限公司 | High-refractive-index organosilicon material for light-emitting diode (LED) packaging and preparation method of high-refractive-index organosilicon material |
| CN102993753A (en) * | 2012-11-23 | 2013-03-27 | 中科院广州化学有限公司 | Composite hybrid organic silicon LED (Light Emitting Diode) packaging material, preparation method and applications thereof |
| CN102993753B (en) * | 2012-11-23 | 2015-08-05 | 中科院广州化学有限公司 | A kind of composite hybridization organosilicon LED encapsulation material and its preparation method and application |
| CN103122149B (en) * | 2013-03-18 | 2016-06-15 | 株洲时代新材料科技股份有限公司 | Optical package high refractive index High-transparency silicon rubber and its preparation method |
| CN103122149A (en) * | 2013-03-18 | 2013-05-29 | 株洲时代新材料科技股份有限公司 | Silicon rubber with high refractive index and high transparency for optical encapsulation and preparation method thereof |
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| CN103788872A (en) * | 2014-01-22 | 2014-05-14 | 上海铂优新材料有限公司 | Primer for addition type organic silicon pouring sealant |
| CN103788872B (en) * | 2014-01-22 | 2016-06-29 | 上海铂优新材料有限公司 | A kind of additional organosilicon casting glue silane coupling agent |
| CN103773235B (en) * | 2014-01-22 | 2017-01-11 | 冠研（上海）专利技术有限公司 | Preparation method of primer for addition type organosilicone potting adhesive |
| CN104151839A (en) * | 2014-08-08 | 2014-11-19 | 广东省工业技术研究院(广州有色金属研究院) | Phenyl silicone resin for optical fiber matching block |
| CN105585957B (en) * | 2014-10-22 | 2017-12-15 | 株洲时代新材料科技股份有限公司 | Silicone impregnating varnish and its preparation method and application |
| CN105585957A (en) * | 2014-10-22 | 2016-05-18 | 株洲时代新材料科技股份有限公司 | Silicone impregnating varnish, and preparing method and applications thereof |
| CN105384935A (en) * | 2015-12-16 | 2016-03-09 | 烟台德邦先进硅材料有限公司 | Vinyl-terminated polydimethyldiphenylsiloxane synthesis method |
| CN105348809A (en) * | 2015-12-17 | 2016-02-24 | 刘爱华 | Novel organic siloxane polymer material for electronic packaging |
| CN105348809B (en) * | 2015-12-17 | 2018-07-03 | 刘爱华 | A kind of organic siloxane polymer material used for electronic packaging |
| CN106977723A (en) * | 2017-04-28 | 2017-07-25 | 深圳天鼎新材料有限公司 | End-vinyl phenyl silicone oil, preparation method and the usage |
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