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CN102863801A - High-hardness high-adhesion silicone resin composition - Google Patents

High-hardness high-adhesion silicone resin composition Download PDF

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Publication number
CN102863801A
CN102863801A CN2012104123800A CN201210412380A CN102863801A CN 102863801 A CN102863801 A CN 102863801A CN 2012104123800 A CN2012104123800 A CN 2012104123800A CN 201210412380 A CN201210412380 A CN 201210412380A CN 102863801 A CN102863801 A CN 102863801A
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Prior art keywords
organopolysiloxane resins
organic radical
polysilicone
resin
organic
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CN2012104123800A
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卢育彦
黄伟翔
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SWANCOR (SHANGHAI) FINE CHEMICAL CO Ltd
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SWANCOR (SHANGHAI) FINE CHEMICAL CO Ltd
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Abstract

The invention provides a high-hardness high-adhesion silicone resin composition, which comprises (A) organic polysiloxane resin, (B) hydrogen-terminated polysiloxane resin, (C) a platinum group metal catalyst, and (D) fumed silica. When the silicone resin composition is used, the thixotropy effect of the fumed silica can be exerted without an extra thixotropic agent, and other auxiliary agents cannot be gradually failed with time. Moreover, the silicone resin composition can be rapidly shaped for effectively protecting the interior gold wire and chip and avoiding damages to the interior gold wire and chip.

Description

A kind of have high rigidity, a high tack polysilicone composition
Technical field
The present invention relates to the encapsulation adhesives technical field, relate in particular to and a kind ofly can formalize fast and effectively protect the not damageable organic polysilicone composition of inner gold thread and chip.
Background technology
Use lens in present photodiode (light-emitting diode) encapsulation process, be use thermoplastic resin (such as allyl resin, polycarbonate resin etc.) injection molding it.In the manufacture craft in recent years, adopt is welded in technique on the substrate with high temperature lead-free solder processing procedure more than 260 ℃ with assembly more, it is very high that but it dissolves temperature, if when using the scolding tin processing procedure under like this temperature, the lens of thermoplastically material will Yin Gaowen and produce distortion and the situation of flavescence occurs.
Owing to existing the plastic product resin of above-mentioned heat that the problem of thermal distortion and hot xanthochromia is arranged, therefore there is the people to attempt using polysilicone.Therefore in recent years, (Japanese Patent: JP 2007-123891), and the thixotropy of the packaging plastic constituent that uses derives from the thixotropic agent of other interpolation the package method that discloses direct use polysilicone and form lensing.But as a whole, the thixotropy effect of polysilicone is not good, cause be shaped and process of setting in can produce flowability, thereby can't obtain the problem of the molded lens package of expecting.
Summary of the invention
The present invention is directed to Shortcomings part in the prior art, a kind of polysilicone composition with high thixotropic, high rigidity and high adhesion is provided, needn't add the effect that thixotropic agent can produce aerosil performance thixotroping additionally outward again when this organic polysilicone composition uses, and in time deferred and situation that lost efficacy gradually of other auxiliary agents can not occur.
To achieve these goals, the invention provides a kind of organic polysilicone composition, comprise (A) organopolysiloxane resins, (B) organic radical hydrogen polysiloxanes resin, (C) platinum metal catalysts, (D) aerosil in the polysilicone composition
Described (A) organopolysiloxane resins is the organopolysiloxane resins that has two above aliphatics unsaturated link(age)s and two above epoxide functional groups in every a part and have resin construction; Wherein, described unsaturated link(age) is preferably C=C, such as the cycloalkenyl group of the alkenyl of vinyl, allyl group, propenyl, pseudoallyl, butenyl, pentenyl, hexenyl etc., cyclohexenyl etc.; Wherein, most preferably be vinyl and allyl group.Described unsaturated link(age) and epoxy-functional can be side chain, main chain or the ends that is positioned at molecule.
The viscosity of organopolysiloxane resins generally can be: be 500 ~ 100000 mPas under 25 ℃, be preferably 1000 ~ 10000 mPas.
Described (B) organic radical hydrogen polysiloxanes resin is the organic radical hydrogen polysiloxanes resin that has the hydrogen atom that is connected with Siliciumatom more than two in every a part.Described organic radical can be aliphatic hydrocarbon or aromatic hydrocarbon substituting group, such as alkyl, phenyl, alkyl-substituted phenyl, with the alkyl of aromatic base side group, phenylalkyl etc., concrete example such as methyl, ethyl, phenyl, benzyl etc.
In the preferred embodiment provided by the invention, the mol ratio of the hydrogen atom that is connected with Siliciumatom in the unsaturated link(age) in wherein said (A) organopolysiloxane resins and (B) organic radical hydrogen polysiloxanes resin is 1 :0.8 ~ 4.0.
In the preferred embodiment provided by the invention, in wherein said organic polysilicone composition, by (A) organopolysiloxane resins with (B) in the resin Composition that organic radical hydrogen polysiloxanes resin forms, (A) weight percent of organopolysiloxane resins is that the weight percent of 5.0 ~ 95.0 wt%, (B) organic radical hydrogen polysiloxanes resin is 5.0 ~ 95.0 wt%.
In the preferred embodiment provided by the invention, the particle diameter of wherein said (D) aerosil is 5 nm ~ 50 nm, and specific surface area is 10 ~ 500 m 2/ g.
In the preferred embodiment provided by the invention, the weight of wherein said (D) aerosil is (A) organopolysiloxane resins and (B) 0.1 ~ 50.0 wt% of the gross weight of organic radical hydrogen polysiloxanes resin.
In the foregoing of the present invention, described platinum metal catalysts can be platinum group, palladium system, rhodium series catalysts, is preferably the platinum group materials such as platinum, platinum black, chlorination platinic acid, such as H 2PtCl 6MH 2O, K 2PtCl 6, KHPtCl 6MH 2O, K 2PtCl 4, K 2PtCl 4MH 2O, PtO 2MH 2O(m is positive integer) etc.
In the preferred embodiment provided by the invention, the weight of wherein said (C) platinum metal catalysts is (A) organopolysiloxane resins and (B) 0.1 ~ 10.0 wt% of the gross weight of organic radical hydrogen polysiloxanes resin.
The present invention also provides a kind of organic poly-silicone rubber hardening thing, should be obtained by above-mentioned organic polysilicone composition sclerosis by poly-silicone rubber hardening thing, described organic poly-silicone rubber hardening thing is under the 1 mm state at thickness, and the light penetration rate that 25 ℃ of lower wavelength are 450 nm is more than 85%.
Provided by the inventionly add the effect that thixotropic agent can produce aerosil performance thixotroping needn't be additionally when having high rigidity, high tack polysilicone composition and using outward again; and can not occur along with other auxiliary agents are deferred and situation about losing efficacy gradually can formalize and effectively protect inner gold thread and chip to be difficult for infringement fast in time.
Description of drawings
Fig. 1 is brightness contrast test result figure.
Fig. 2 is as a result figure of colour temperature contrast test.
Fig. 3 is as a result figure of colour rendering index contrast test.
Fig. 4 is the penetration coefficient detected result figure of resin combination of the present invention.
Fig. 5 is the penetration coefficient detected result figure of comparative example's product.
Embodiment
When using, polysilicone composition provided by the invention needn't additionally add again the effect that thixotropic agent can produce aerosil performance thixotroping outward; and can not occur along with other auxiliary agents are deferred and situation about losing efficacy gradually can formalize and effectively protect inner gold thread and chip to be difficult for infringement fast in time.
By the following examples polysilicone composition provided by the invention is described in further detail, in order to better understand the invention, but the content of embodiment does not limit the protection domain of the invention.
Comprise the compositions such as (A) organopolysiloxane resins, (B) organic radical hydrogen polysiloxanes resin, (C) platinum metal catalysts, (D) aerosil in organic polysilicone composition provided by the invention, the specific refractory power of described organopolysiloxane composition is 1.44 ~ 1.46.
The weight percent of (A) organopolysiloxane resins is between 5.0 ~ 95.0 wt% in organic polysilicone composition, in the time of the containing quantity not sufficient 5.0 wt% or surpass 95 wt% of (A) organopolysiloxane resins, the incomplete situation of hardening can appear in organopolysiloxane composition.(A) organopolysiloxane resins is the organopolysiloxane resins that every a part has two above aliphatics unsaturated link(age)s and two above epoxide functional groups and has resin construction.Unsaturated link(age) can be alkenyls such as vinyl, allyl group, propenyl, pseudoallyl, butenyl, pentenyl, hexenyl or such as cycloalkenyl groups such as cyclohexenyls.Wherein, vinyl and allyl group are best unsaturated link(age).
(A) to be generally under 25 ℃ be 500 ~ 100000 mPas to the viscosity of organopolysiloxane resins, especially take (A) organopolysiloxane resins of 1000 ~ 10000 mPas as best.
The weight percent of (B) organic radical hydrogen polysiloxanes resin is 5.0 ~ 95.0 wt% in the organopolysiloxane composition, in the time of the containing quantity not sufficient 5.0 wt% or surpass 95 wt% of (B) organic radical hydrogen polysiloxanes resin, the incomplete situation of hardening can appear in organopolysiloxane composition.(B) consumption of organic radical hydrogen polysiloxanes resin is closely related with the consumption of (A) organopolysiloxane resins, and the mol ratio of the hydrogen atom that (A) is connected with Siliciumatom in the unsaturated link(age) in the organopolysiloxane resins and (B) organic radical hydrogen polysiloxanes resin is 1 :0.8 ~ 4.0, the mol ratio that is more preferably is 1 :1.1 ~ 2.9, highly preferred mol ratio is 1 :1.1 ~ 2.0.
The weight of (C) platinum metal catalysts in the organopolysiloxane composition and (A) organopolysiloxane resins and (B) gross weight of organic radical hydrogen polysiloxanes resin sum than between 0.1 to 10.0 wt%.(C) platinum metal catalysts can be selected the metal of platinum group, palladium system, rhodium system, the material of platiniferous such as platinum, platinum black, Platinic chloride, for example H 2PtCl 6MH 2O, K 2PtCl 6, KHPtCl 6MH 2O, K 2PtCl 4, K 2PtCl 4MH 2O, PtO 2MH 2O(wherein m is positive integer) etc.Above-mentioned (C) platinum metal catalysts can select the multiple mixing of a kind of independent use or selection to use.
Aerosil (fumed silica) joins in the organopolysiloxane composition as weighting agent, the weight of (D) aerosil in the organopolysiloxane composition and (A) organopolysiloxane resins and (B) gross weight of organic radical hydrogen polysiloxanes resin sum than between 0.1 ~ 50.0 wt%.The particle diameter of preferred gas (D) aerosil is 5 nm ~ 50 nm, and specific surface area is 10 ~ 500 m 2/ g.
Embodiment 1
Get the organopolysiloxane resins that the 50g viscosity is 11000 mPas (in the organic group with respect to all and silicon bonding in the organopolysiloxane resins, contain the vinyl of 18mol% and silicon bonding and the phenyl of 48mol% and silicon bonding), the 50g viscosity is that the organic radical hydrogen polysiloxanes resin of 5300 mPas is (in the organic radical hydrogen polysiloxanes resin with respect to the organic group of all and silicon bonding, contain hydrogen atom that 18mol% is connected with the silicon key and the phenyl of 35mol% and silicon bonding), 2g 1,3-divinyl-1,1, the platinum complexes catalyzer of 3,3-tetramethyl disiloxane (metal platinum that weight unit comprises is 4.0 ppm in the catalyzer) and 10g particle diameter are 20 nm, specific surface area is 200 m 2The aerosil of/g forms polysiloxane composition provided by the invention after uniformly mixing 10 minutes.Add 10g fluorescent material toward polysiloxane composition and continue to stir the stable mixture of formation.
With the mixture that stir to form and on the market common packaging plastic (selecting the commercial COB of SHIN-ETSU HANTOTAI moulding silica gel LPS-3421T) harden and carry out contrast test on the performance, and with test condition and outcome record in following table.Fig. 4 and Fig. 5 be respectively among the embodiment 1 among product and the comparative example penetration coefficient of product detect test result figure.
Table 1 experimental result
Figure 2012104123800100002DEST_PATH_IMAGE002
Mixture among the embodiment 1 and comparative example's product is respectively applied to the encapsulation of photodiode, and test respectively photodiode brightness (lumen, Lm), the technical indicator such as colour temperature and development index.Fig. 1 to Fig. 3 is respectively photodiode, and (lumen, Lm), the colour temperature and development index test draws data, the graph of a relation of drafting is among the figure ◆ be the data that the mixture test obtains among the embodiment 1, the data that ■ obtains for comparative example's product test among the figure in brightness.
Data on Fig. 1 and Fig. 2 can draw, and the data that the photodiode that polysilicone composition provided by the invention is used for encapsulating obtains in test aspect brightness and the colour temperature are better than the common brand product in existing market.Test obtains the equally matched of the common brand product of data and existing market aspect colour rendering index.
Embodiment 2
Get the organopolysiloxane resins that the 50g viscosity is 50000 mPas (in the organic group with respect to all and silicon bonding in the organopolysiloxane resins, contain the vinyl of 18mol% and silicon bonding and the methyl of 28mol% and silicon bonding), the 50g viscosity is that the organic radical hydrogen polysiloxanes resin of 5000 mPas is (in the organic radical hydrogen polysiloxanes resin with respect to the organic group of all and silicon bonding, contain hydrogen atom that 18mol% is connected with the silicon key and the methyl of 15mol% and silicon bonding), 2g 1,3-divinyl-1,1, the platinum complexes catalyzer of 3,3-tetramethyl disiloxane (metal platinum that weight unit comprises is 4.0 ppm in the catalyzer) and 10g particle diameter are 20 nm, specific surface area is 200 m 2The aerosil of/g forms polysiloxane composition provided by the invention after uniformly mixing 10 minutes.Add 10g fluorescent material toward polysiloxane composition and continue to stir the stable mixture of formation.
The encapsulation glue composition for preparing in the above embodiment of the present invention, specific refractory power is between 1.44 ~ 1.46; And under thickness 1 mm, 25 ℃, the penetration coefficient of the light of 450 nm wavelength is more than 85%.
Above specific embodiments of the invention are described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, not breaking away from impartial conversion and the modification of doing under the spirit and scope of the present invention, all should contain within the scope of the invention.

Claims (7)

1. one kind has high rigidity, high tack polysilicone composition, it is characterized in that, comprise (A) organopolysiloxane resins, (B) organic radical hydrogen polysiloxanes resin, (C) platinum metal catalysts, (D) aerosil in the polysilicone composition
The organopolysiloxane resins that has two above aliphatics unsaturated link(age)s and two above epoxide functional groups in the every a part of described (A) organopolysiloxane resins and have resin construction; The organic radical hydrogen polysiloxanes resin that has the hydrogen atom that is connected with Siliciumatom more than two in the every a part of described (B) organic radical hydrogen polysiloxanes resin.
2. polysilicone composition according to claim 1 is characterized in that, the mol ratio of the hydrogen atom that is connected with Siliciumatom in the unsaturated link(age) in described (A) organopolysiloxane resins and (B) organic radical hydrogen polysiloxanes resin is 1:0.8 ~ 4.0.
3. polysilicone composition according to claim 1 is characterized in that, the particle diameter of described (D) aerosil is 5 nm ~ 50 nm, and specific surface area is 10 ~ 500 m 2/ g.
4. polysilicone composition according to claim 1, it is characterized in that, by (A) organopolysiloxane resins with (B) in the resin Composition that organic radical hydrogen polysiloxanes resin forms, (A) weight percent of organopolysiloxane resins is that the weight percent of 5.0 ~ 95.0 wt%, (B) organic radical hydrogen polysiloxanes resin is 5.0 ~ 95.0 wt% in described organic polysilicone composition.
5. according to claim 1 or 4 described polysilicone compositions, it is characterized in that, the weight of described (C) platinum metal catalysts and (A) organopolysiloxane resins and (B) gross weight of organic radical hydrogen polysiloxanes resin than at 0.1 to 10.0 wt%.
6. according to claim 1 or 4 described polysilicone compositions, it is characterized in that, the weight of described (D) aerosil and (A) organopolysiloxane resins and (B) gross weight of organic radical hydrogen polysiloxanes resin than at 0.1 ~ 50.0 wt%.
7. an organic poly-silicone rubber hardening thing is characterized in that, described poly-silicone rubber hardening thing is obtained by organic polysilicone composition sclerosis described in above-mentioned any claim;
Described organic poly-silicone rubber hardening thing is under the 1 mm state at thickness, and the light penetration rate that 25 ℃ of lower wavelength are 450 nm is more than 85%.
CN2012104123800A 2012-10-25 2012-10-25 High-hardness high-adhesion silicone resin composition Pending CN102863801A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103131190A (en) * 2013-02-05 2013-06-05 广州市爱易迪新材料科技有限公司 Double-component self-molding lens silica gel for light-emitting diode (LED) package and package process of double-component self-molding lens silica gel
CN104130585A (en) * 2014-08-12 2014-11-05 铜陵国鑫光源技术开发有限公司 High-refractive-index organic silicon material for LED encapsulation
CN104177616A (en) * 2014-08-12 2014-12-03 铜陵国鑫光源技术开发有限公司 Moisture-proof organic silicon material for LED encapsulation

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101636450A (en) * 2007-03-19 2010-01-27 三友瑞克株式会社 Silicone resin composition for light-emitting element encapsulation and method for producing optical semiconductor electronic parts by casting method using the same
CN102268186A (en) * 2010-06-02 2011-12-07 日东电工株式会社 Composition for thermosetting silicone resin

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101636450A (en) * 2007-03-19 2010-01-27 三友瑞克株式会社 Silicone resin composition for light-emitting element encapsulation and method for producing optical semiconductor electronic parts by casting method using the same
CN102268186A (en) * 2010-06-02 2011-12-07 日东电工株式会社 Composition for thermosetting silicone resin

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103131190A (en) * 2013-02-05 2013-06-05 广州市爱易迪新材料科技有限公司 Double-component self-molding lens silica gel for light-emitting diode (LED) package and package process of double-component self-molding lens silica gel
CN104130585A (en) * 2014-08-12 2014-11-05 铜陵国鑫光源技术开发有限公司 High-refractive-index organic silicon material for LED encapsulation
CN104177616A (en) * 2014-08-12 2014-12-03 铜陵国鑫光源技术开发有限公司 Moisture-proof organic silicon material for LED encapsulation

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Application publication date: 20130109