CN104449550B - Silicon composition and application thereof - Google Patents

Silicon composition and application thereof Download PDF

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CN104449550B
CN104449550B CN201310750313.4A CN201310750313A CN104449550B CN 104449550 B CN104449550 B CN 104449550B CN 201310750313 A CN201310750313 A CN 201310750313A CN 104449550 B CN104449550 B CN 104449550B
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silicon
compositions
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silicon composition
vinyl
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CN104449550A (en
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张汝志
张景博
宁新国
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Florian Photoelectric Materials (suzhou) Co Ltd
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Florian Photoelectric Materials (suzhou) Co Ltd
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Abstract

The invention discloses a kind of silicon composition and application thereof.Described silicon composition comprises the basic components such as at least one vinyl silicone polymer and at least one hydrogen-based siloxane polymer that can be solidified and at least one vinyl POSS, the nano silicon of organic group modification and silicon hydrogenation addition curing catalyst by hydrosilylation addition reaction, the most also can comprise the components such as hydrosilylation addition reaction inhibitor, adhesive accelerant.The silicon composition of the present invention has good physics, chemical synthesis performance, including good fluidity, curing rate is fast, curing degree is high, solidification hardness is high, light transmittance is high, and also there is the features such as sulfuration resistant performance is strong, aging speed slow, stable performance, being adapted as bonding, the encapsulating material application of optical, electrical sub-device, the encapsulating material especially as semiconductor light-emitting elements such as LED is applied.

Description

Silicon composition and application thereof
Technical field
The present invention be more particularly directed to a kind of silicon composition, it is adapted as the application such as cementing compositions, encapsulating material.
Background technology
Luminous efficiency, brightness, power and the service life of LED are had and important shadow by LED encapsulation material Ring.Wherein, the encapsulating material of the resistance to ultraviolet/heat ageing of high index of refraction, high transmission rate and excellence can be effectively improved LED light output rating and service life.
Current conventional power type LED encapsulation material is mainly organosilicon material, and it has low-shrinkage and in solidification During do not discharge the advantages such as by-product, but, it still suffers from relatively in refractive index, the solidification performance such as hardness The most not enough.To this end, industry proposes kinds of schemes to promoting the respective performances of organosilicon encapsulating material, so Then, although truly having lifting through modified material performance in some aspects, but it can cause again it simultaneously The decline of some performances in terms of it.
Such as, Publication No. US7527871A, US2004116640A1, EP1424363B1, CN101066446A, The modification technology that CN102181159A, CN103022320A, CN101565535A etc. are involved, its The organosilicon material comprehensive lifting at aspects such as refractive index, weatherability, light transmittance, mechanical properties cannot be realized.
Summary of the invention
An object of the present invention is to provide a kind of silicon composition, and it has excellent optics, mechanics etc. and combines Close performance, to overcome deficiency of the prior art.
The basic components of a kind of silicon composition of the present invention comprises:
Can be by least one ethylene of silicon hydrogenation addition (hydrosilylation reaction) reaction solidification Silicone polymer and at least one hydrogen-based siloxane polymer,
And, nano silicon and silicon that at least one vinyl POSS, organic group are modified hydrogenate addition curing Catalyst.
Further, in the basic components of described compositions, described vinyl silicone polymer and hydrogen-based silica The content of alkane polymer is 60~99wt%, preferably 75~99wt%, especially preferably 85~95wt%. Further, in the basic components of described compositions, described hydrogen-based siloxane polymer institute silicon-hydrogen bond containing with The mol ratio of vinyl contained by described vinyl silicone polymer is 1:0.7~1:1.4.
Further, in the basic components of described compositions, the content of described vinyl POSS is 0.1~20wt%, It is preferably 1~10wt%, especially preferably 1~6wt%.
Further, in the basic components of described compositions, the content of described nano silicon be 0.1~ 20wt%, preferably 1~10wt%.
Further, described compositions also comprises hydrosilylation inhibitor,
Wherein, the content of described silicon hydrogenation addition curing catalyst is 0.1~1000ppm, preferably 1~100ppm, Especially preferably 1~20ppm.
And based on the consumption of described hydrosilylation inhibitor component 0.001~1wt%, preferably 0.005~ 0.5wt%, especially preferably 0.01~0.1wt%.
Further, described compositions also comprises more than one adhesive accelerants, and the containing of described adhesive accelerant Amount is 0.001~10wt%, preferably 0.01~5.0wt%, and especially preferably 0.01~1.0wt% are the most excellent Elect 0.01~0.05wt% as.
Further, described compositions the solidfied material formed for the index of refraction of visible ray between 1.35~1.60, Preferably more than 1.5.
Another object of the present invention is to provide aforementioned organic silicon compositions bonding article or at least packaged articles local Application in surface.
It is still another object of the present invention to provide a kind of article adhering method, including:
First article and the second article are provided,
Aforementioned organic silicon compositions is applied between the first article and the second article,
And, under the conditions of selected temperature, make the complete heat cure of described silicon composition, thus by the first article with Second article are adhesively fixed.
A further object of the present invention is to provide a kind of method for packing, including:
At least at the selected regional area of article surface and/or inside as packaging area,
And, apply described silicon composition at described packaging area,
And, under the conditions of selected temperature, make the complete heat cure of described silicon composition, it is achieved the encapsulation to article. Such as, as more one of preferred embodiment, can be in the time of 1min~24h at room temperature~260 DEG C Inside make the complete heat cure of described silicon composition, it is achieved to the encapsulation of article or be adhesively fixed.
A further object of the present invention is to provide a kind of electronic device or photoelectric device, comprises described silicon composition The solidfied material formed.
Wherein, described photoelectric device includes that semiconductor light-emitting elements, described semiconductor light-emitting elements include LED, but It is not limited to this.
In the present invention, aforesaid " encapsulation " (packaging) should be understood including at least following connotation, e.g., By described silicon composition by bonding for two or more article (adhesive), or, by described organic Silicon composition some regions curing formation protective layer (coating) of article surface, or, by one or many The local of individual article is immersed in the solidfied material formed by described silicon composition, or, by one or more Article entirety embedding seal (encapsulation) in the solidfied material formed by described silicon composition, when So, it is possible to realize simultaneously aforesaid bonding, coat, the function such as sealing.
Compared with prior art, as it was previously stated, the silicon composition that the present invention provides has excellent thing, changes performance, Include but not limited to good mobility, there are good optical, electrical performance and mechanical property etc. after hardening, And its application process is the simplest.
Detailed description of the invention
One aspect of the present invention provides a kind of silicon composition, and its basic components includes: can pass through silicon hydrogen Change at least one vinyl silicone polymer (vinyl that additive reaction (hydrosilylation reaction) solidifies Siloxane polymer) and at least one hydrogen-based siloxane polymer (Si-H siloxane polymer), and, At least one vinyl POSS(vinyl POSS) and the nano silicon (vinyl-or of organic group modification Phenyl-modified nano-sized silica).
Further, described compositions also can bag silyl hydride addition curing catalyst, by its catalytic action, can Realize the heat cure of said composition.
And further, also can insert hydrosilylation inhibitor, then be catalyzed by adjusting silicon hydrogenation addition curing Agent and the kind of hydrosilylation inhibitor, consumption etc., can regulate and control the state of cure of said composition with solid Change speed etc..
Aforesaid hydrosilylation addition reaction means and is added on unsaturated organic compound by the hydride of silicon, thus generates The reaction of various organo-silicon compound, it can be to use three kinds of modes: (1) is the most straight with alkene or alkynes It is bonded into.(2) ultraviolet, gamma-rays or organic peroxide free radical is utilized to cause.(3) with transition metal and Its coordination compound catalytic reaction.Planting mode particularly with (3rd), its reaction condition is gentle, and selectivity is good, Productivity is high.
In the present invention, described silicon composition can be linear polymer, branched polymers or network polymerization Thing.
Obvious, the compositions of the present invention should comprise at least one liquid component, with remaining material in said composition Material is combined as the liquid with good fluidity, so that can be transported by the conventional equipment such as syringe or pump, Dispensing.
For the vinyl silicone polymer of the present invention, it can select any one siloxanes containing vinyl group Polymer, and the approach that can be noted by industry, including commercially available or self-control etc., various ways obtains.
Such as, the general molecular formula of described vinyl silicone polymer monomer can be:
(R5)m(R6)nSi(OR7)4-m-n
Wherein, R5For vinyl, pi-allyl or vinyl benzyl;R6For methyl, ethyl or phenyl;R7For methyl Or ethyl, m is 0,1 or 2;N is 0,1 or 2, and m+n < 4, and such as, it can be selected from CH2=CHSi(OCH3)3、CH2=CHSi(OC2H5)3、CH2=CHSi(OCH(CH3)2)3、 CH2=CHSi(OC4H9)3、(CH2=CH)(C2H5)Si(OC2H5)2、(CH2=CH)(C6H5)Si(OC2H5)2、 CH2=CHCH2Si(OCH3)3、CH2=CHCH2Si(OC2H5)3、(CH2=CHCH2)2(CH3)SiOC2H5、 (CH2=CHCH2)(CH3)2SiOC2H5、(CH2=CHCH2)2Si(OC2H5)2、(CH2=CHCH2)3SiOC2H5 Or CH2=CHC6H4Si(OCH3)3Etc..
Or, described vinyl silicone polymer molecular structural formula can be:
Me2R1SiO(Me2SiO)a(MeViSiO)b(MePhSiO)cSiR1Me2,
In formula, Me represents methyl, and Vi represents vinyl, and Ph represents phenyl, the positive integer of a=3~3000, and b is 1~300 Positive integer, the positive integer of c=0 or 1~3000, and meet 0≤c/ (a+b+c)≤0.99, R1For Me or Vi. For the hydrogen-based siloxane polymer of the present invention, it can select any one siloxanes containing Si--H to gather Compound, and the approach that can be noted by industry, including commercially available or self-control etc., various ways obtains.
Such as, the general structure of described hydrogen-based siloxanyl monomers can be:
(R4’)m’(R5’)n’Si(H)p’(OR6’)(4-m’-n’-p’)
Wherein, R4’、R5' it is methyl, ethyl or phenyl;R6' it is methyl or ethyl;M ', n ', p ' are 0,1 Or 2, and m '+n '+p ' < 4.
The most such as, the molecular structure of described hydrogen-based siloxane polymer can be:
Me2R2SiO(Me2SiO)d(MeHSiO)e(MePhSiO)fSiR2Me2,
In formula, Me represents methyl, and Ph represents phenyl, the positive integer of d=3~900, the positive integer of e=3~600, f=0 Or the positive integer of 1~900, and meet 0≤f/ (d+e+f)≤0.99, R2For Me or H.
Further, in the basic components of the compositions of the present invention, vinyl silicone polymer and hydrogen-based silica Alkane polymer content can be between 60~99wt%, preferably 75~99wt%, more preferably 85~95wt%, so that transparent and there is good mobility after said composition solidification.
Further, in the present compositions, the si-h bond in hydrogen-based siloxane polymer and vinyl silicon The mol ratio of the vinyl in oxygen alkane polymer is between 1:0.7~1:1.4.
Vinyl POSS(polyhedral oligomeric silsesquioxane for the present invention), it can be selected containing vinyl Any one POSS of group, and the approach that can be noted by industry, (such as, referred to including commercially available or self-control CN100503757A, CN101906116B etc.) etc. various ways obtain.
Such as, described POSS can be by vinyl trichlorosilane, vinyltrimethoxy silane, vinyl three second TMOS, vinyl triisopropyl TMOS, vinyl three normal-butyl silane, vinyl tri-tert One or more reactions in silane, vinyltriphenoxysilane are prefabricated and obtain;Or in them Plant or several and methyl trichlorosilane, MTMS, MTES, methyl 3 third TMOS, methyl three normal-butyl silane, methyl tri-tert silane, phenyl trichlorosilane, phenyl front three In TMOS, phenyl triethoxysilane, phenyl three isopropoxy silane, phenyl three tert-butoxy silane One or more reactions prefabricated and obtain, but be not limited to this.
Further, in the basic components of the present composition, the content of described vinyl POSS can 0.1~ Between 20wt%, preferably 1~10wt%, more preferably 1~6wt%, its can uniform dissolution in combination In thing and solidification after transparent.
In the present invention, the nano silicon that described organic group is modified refers to that surface should be modified with at least one The nano-silicon dioxide particle of organic group, it can be scattered in silicon composition of the present invention institute by good Among the liquid component comprised, wherein, described organic group preferably is selected from vinyl or phenyl, wherein the former energy Enough refering to curing reaction, and the latter can increase the phase of nano-silicon dioxide particle and the organosilicon containing aromatic group Capacitive.
The nano-silicon dioxide particle that this surface is modified by organic group also can be obtained by approach such as commercially available or self-controls, Such as, following Access to publication at least it is referred to:
1, Zhang Xinmeng, " surface modification of silica ", Shenyang University of Technology's master thesis, 2006 12 Month.
2, remaining east liter etc., " nano-silica surface modification of graft progress ", coatings industry, 2010 years The 7th phase of volume 40 July.
Again and, the mean diameter of the nano-silicon dioxide particle in the present invention is not more than 500nm, particularly preferably 1nm-100 nanometer, and visible ray should be able to be made much more as far as possible to transmit from described compositions.
Further, in the composition, the content of described nano silicon can be 0.1~20wt%, excellent It is selected in 1~10wt%, so that can be the most transparent after compositions solidification.
In the present compositions, aforementioned silicon hydrogenation addition curing catalyst is preferably noble metal catalyst, such as Platinum and rhodium compound.Especially with patent US-A-3159601, US-A-3159602 and US-A-3220972 And platinum described in European patent EP-A-0057459, EP-A-0188978 and EP-A-0190530 and having The complex of machine product, or patent US-A-3419593, US-A-3715334, US-A-3377432 and Platinum described in US-A-3814730 and the complex of vinylated organosilicon oxygen alkane.This catalyst is generally preferable For the coordination compound of platinum catalyst, i.e. platinum, particularly platinum complex, including chloroplatinic acid, H2PtCl6、Pt(PPh3)4、 Cp2PtCl2, methyl vinyl silicone polymer coordination platinum complex, diethyl phthalate coordination The platinum complex etc. of platinum complex, dichloro double (triphenylphosphine), preferably platinum complex is chloroplatinic acid, H2PtCl6、 The platinum complex of methyl vinyl silicone polymer coordination, more preferably methyl vinyl silicone polymer The platinum complex of coordination.
In the present compositions, silicon hydrogenation addition curing catalyst content can between 0.1~1000ppm, Preferably at 1-100ppm, more preferably at 1-50ppm, more preferably 1~20ppm.
In the present compositions, aforementioned hydrosilylation inhibitor refers to cause hydrosilylation not Good material, this kind of material include alkynol compound, alkene-alkine compounds, siloxanes or benzotriazole and His hydrosilanes reaction suppressor.Wherein, alkynol compound inhibitor be selected from 2-phenyl-3-butyne-2-alcohol, 2-methyl-3-butyne-2-alcohol, 3,5-dimethyl-1-hexin-3-alcohol etc.;Alkene-alkine compounds is selected from such as 3-methyl -pirylene etc., siloxanes is selected from 1,3,5,7-tetramethyl-1,3,5,7-tetra-hexenyl cyclotetrasiloxanes, 1,3,5,7-tetramethyl-1,3,5,7-tetravinyl cyclotetrasiloxane etc..Wherein preferred alkynol compound, the most excellent Select 2-phenyl-3-butyne-2-alcohol.
In the present invention, for basic components (if setting it as 100 weight portions), this hydrosilylation presses down The content of preparation can be preferably at 0.005~0.5 weight portion, the most excellent between 0.001~1 weight portion Elect 0.01~0.1 weight portion as.
Additionally, in the present compositions, a kind of applicable adhesion promotor or multiple adhesion promotor can also be comprised Mixture, it is selected from defoamer (defoamer), rheology modifier (rheology modifier), ink Water (ink) and/or pigment (pigments), infrared absorbent (IR absorber) etc..
Such as, in the composition, described adhesive accelerant can be selected from tetraethyl orthosilicate, vinyl trimethoxy Base silane, n-butyl boronate, boric acid isopropyl ester, isooctyl acid titanium, zirconium iso-octoate, tetrabutyl titanate, metatitanic acid One or several mixture in isopropyl ester, KH-171, KH-560 and KH-570 or they in The hydrolysate of one or more, preferred vinyl trimethoxy silane, boric acid isopropyl ester, isooctyl acid titanium, One or several mixture in tetrabutyl titanate, KH-560 and KH-570, or one or more Hydrolysate;Particularly preferably in vinyltrimethoxy silane, tetrabutyl titanate, KH-560 one or more Mixture, or their hydrolysate.
Such as, the adhesive accelerant that can be obtained by commercially available approach can be Dow Corning Corporation produce JCR6101, JCR6101UP, EG6301, OE6336, JCR6175, JCR6109, Hipec4939, Hipec1-9224, OE6250, SR7010, SE9207, SE1740, SE9187L etc., but it is not limited to this.
In the present compositions, the content of described adhesive accelerant can be 0.001~10wt%, is preferably 0.01~5.0wt%, especially preferably 0.01~1.0wt%, more preferably 0.01~0.05wt%
Although as it was previously stated, having some bonding agents at present is by by polytype siloxane polymer, micron Or nano silicon and corresponding activator etc. assemble, it is achieved the modification to siloxane polymer, but thus Although the binding agent obtained is promoted at some aspect of performance, can cause again under other side performance simultaneously Fall or disappearance so that its combination property cannot meet the demand of actual application.And for light and/or electrical part, For the semiconductor light-emitting elements such as the most such as LED, for convenience of its bonding, packaging technology, it usually needs Use and there is the adhesive composite of good fluidity so that its can to pass through syringe, pump, printer etc. general Some select location leading to equipment and accurately inject or be coated on device, and in order to make between device or device Good isolation can be kept with the external world, including physics and chemical isolation, and/or make device can keep good light Output or take in efficiency, and/or make device produce the most voluntarily or the passive heat accepted etc. can be quick Dissipate, and other is not limited to this target, also requires that the solidfied material formed by adhesive composite should have concurrently Good bonding force, hardness, pliability, light transmittance (the most under visible light), dielectric constant, heat conduction The performance such as efficiency, aging resistance.
Inventor is after numerous studies, and helps and assemble test with substantial amounts of, has been found out the skill of the present invention Art scheme, that is, by gathering because of at least one vinylsiloxane of hydrosilylation addition reaction solidification Compound, at least one hydrogen-based siloxane polymer, at least one vinyl POSS and organic group are modified Nano silicon assemble, and be aided with curing catalysts and hydrosilylation inhibitor, it is thus achieved that a kind of There is the compositions of good fluidity.Further, inventor is found surprisingly that and determines the most very much, this Bright compositions have concurrently good bonding force, hardness, pliability, light transmittance (the most under visible light), The performances such as dielectric constant, heat transfer efficiency, aging resistance.
Such as, the silicon composition of the present invention index of refraction of the solidfied material formed is between 1.35~1.60, excellent It is selected in more than 1.5.Therefore, the compositions of the present invention is particularly suited for electronic installation, Optical devices, photoelectricity Device carries out bonding or encapsulation, especially as light emitting semiconductor device, such as the encapsulating material of LED.
Below in conjunction with some more specifically embodiments and corresponding comparative example, technical scheme is made specifically Explanation.But still it is emphasized that these embodiments are not to be construed as protection scope of the present invention structure Become any restriction.Postscript, except as otherwise noted, otherwise all numbers in description of the invention, percent, Ratios etc. are by weight.
Is the composition of the silicon composition involved by reference examples 1-16 and embodiment 1-2 as shown in table 1-table 2, And prepared by the method that these silicon compositions all can use industry to note, such as, uniformly mixed by each component After conjunction, corresponding compositions can be obtained.
Further, in the embodiment as involved by table 1-table 2 and comparative example, involved vinylsiloxane Polymer, Si-H siloxanes, vinyl POSS, micron silica or hydrophilic nanoscale titanium dioxide Silicon or vinyl or the content of phenyl modified nano silicon, refer to that it is being polymerized by vinylsiloxane Thing, Si-H siloxanes, vinyl POSS and micron silica or hydrophilic nano grade silicon dioxide or Content in the basis composition of the silicon composition of vinyl or phenyl modified nano silicon composition, Rather than as the content in the silicon composition of finished product.And adhesive accelerant, catalyst, inhibitor Content then refers to its content in finished product silicon composition.
It should be noted that, in reference examples 1-16 and embodiment 1-2, for each reference examples and each embodiment In each component of relating to, it is in fact to have chosen many kinds of substance to be assembled with other component, then Carry out correlated performance test.Such as, for vinyl silicone polymer therein, it is to have selected above Multiple the vinyl silicone polymer be applicable to the present invention addressed is tested.For other Component, including Si-H siloxanes, vinyl POSS, vinyl or phenyl modified nano silicon etc., Also it is such.
And for micron silica therein, be to be respectively adopted hydrophilic micron silica, hydrophilic Property micron silica be tested, its all can by commercially available (SHENNA that such as, receives produce SQ-1, SQ-2, SQ-5, SQ-10) or self-control approach (such as, refer to " micron-size spherical titanium dioxide The preparation of silicon powder and Technology research thereof ", Bu Xiangmei, Institutes Of Technology Of Nanjing, master thesis, 2008 June in year;J.AM.CHEM.SOC.2010, vol.132, p4834 4842) obtain.
For hydrophilic nano grade silicon dioxide therein, it is to be respectively adopted to modify and the most modified nanoscale two Silicon oxide is tested, its also can through commercially available approach (R972 that such as, Degussa (EVONIK) is produced, R974, R104, R106, R20, R812, R812S, R816, R7200, R8200, R711, R719, H13L, H15, H17, H18, H20, H30, H2000 that Wa Ke (WACKER) produces, Cabot (CABOT) F01, SD10, F08, F09 that TS-530, TS-610, the TS-720 produced, the SHENNA that receives produce, The DM-10 produced in moral mountain (TOKUYAMA)) and self-control approach obtain and (such as, refer to that " single dispersing is received The preparation of rice silicon dioxide microsphere and carboxylated modification " (" functional material ", 2009,11 phases, volume 40), CN101428807A, WO2009/088250A, Polyethylene Glycol/nano silicon dioxide hybridization material preparation with Characterize " document such as (" Chinese science and technology paper online fine work paper ", volume 2 the 22nd phase in November, 2009).) Refering to table 3, it is clear that it will be seen that the silicon composition of the present invention has good combination property, including stream Dynamic property is good, curing rate is fast, curing degree is high, solidification hardness is high, light transmittance is high.
Such as, in the more specifically case of in embodiment 1, its operation may include that
In a planet strrier special plastic cup, add 76.3 parts of vinyl silicone polymer polymer, 14.5 parts of Si-H siloxane polymers, 4.6 parts of vinyl POSS, the nano-silica of 4.6 parts of modified by vinyl SiClx, 0.008 part of 2-phenyl-3-butyne-2-alcohol, the platinum (0)-1 of 5.2ppm, 3-divinyl-1,1,3,3-tetramethyl two Siloxanes etc., and make vinyl and the Si-H siloxane polymerization of wherein vinyl silicone polymer polymer The mol ratio of the si-h bond of thing is 1.1:1.0, and after mix homogeneously, the viscosity of obtained liquid is 1000cPs.
Obtained liquid is injected in 0.8mm thickness mould, 150 degrees Celsius of lower heat cures 4 hours, obtains one Individual solid transparent, that 0.8mm is thick.The index of refraction of gained silicon composition is 1.41.
The liquid stirred is injected in 2mm thickness mould, 150 degrees Celsius of lower heat cures 4 hours, To a solid thick for 2mm, its hardness is Shao A37.5.
Being injected into by obtained liquid in 2mm thickness mould, heat cure 24 hours, obtain one at 200 degrees celsius The solid that individual 2mm is thick, its hardness is Shao A61.0.
Obtained liquid is injected in 6mm thickness mould, 150 degrees Celsius of lower heat cures 4 hours, obtains one The solid that 6mm is thick, its hardness is Shao A33.5.
Being injected into by obtained liquid in 6mm thickness mould, heat cure 24 hours, obtain one at 200 degrees celsius The solid that individual 6mm is thick, its hardness is Shao A42.4.
Additionally, it is surprising that the shelf-life of the silicon composition of the present invention than existing silicone adhesive Agent is also significantly improved, and this characteristic is allowed to the encapsulation field being also very suitable at electronic device and applies.Example As, the compositions involved by reference examples 16 i.e. can form gel within the time less than one day, and embodiment 2 Steady-state viscosity still can be kept after the experience time of more than two weeks.
Below it is only the concrete exemplary applications of the present invention, protection scope of the present invention is not constituted any limitation.All adopt The technical scheme replaced with equivalents or equivalence and formed, within the scope of all falling within rights protection of the present invention. Table 1: reference examples 1-14 and the composition of embodiment 1 compositions
Table 2: reference examples 15-16 and the composition of embodiment 2 compositions
Table 3: the performance of the compositions of reference examples 1-16 and embodiment 1-2

Claims (21)

1. a silicon composition, it is characterised in that the basic components of described compositions comprises:
At least one vinyl silicone polymer that can be solidified by hydrosilylation addition reaction and at least one hydrogen-based siloxane polymer,
And, nano silicon and silicon that at least one vinyl POSS, organic group are modified hydrogenate addition curing catalyst, and wherein said organic group includes that vinyl or phenyl, the mean diameter of described nano silicon are 1nm~100nm;
In the basic components of described compositions, described vinyl silicone polymer is 60~99wt% with the content of hydrogen-based siloxane polymer, and the content of described vinyl POSS is 0.1~20wt%, and the content of described nano silicon is 0.1~20wt%;
Further, the mol ratio of vinyl contained by described hydrogen-based siloxane polymer institute silicon-hydrogen bond containing and described vinyl silicone polymer is 1:0.7~1:1.4.
Silicon composition the most according to claim 1, it is characterised in that in the basic components of described compositions, described vinyl silicone polymer is 75~99wt% with the content of hydrogen-based siloxane polymer.
Silicon composition the most according to claim 2, it is characterised in that in the basic components of described compositions, described vinyl silicone polymer is 85~95wt% with the content of hydrogen-based siloxane polymer.
Silicon composition the most according to claim 1, it is characterised in that in the basic components of described compositions, the content of described vinyl POSS is 1~10wt%.
Silicon composition the most according to claim 4, it is characterised in that in the basic components of described compositions, the content of described vinyl POSS is 1~6wt%.
Silicon composition the most according to claim 1, it is characterised in that in the basic components of described compositions, the content of described nano silicon is 1~10wt%.
Silicon composition the most according to claim 1, it is characterized in that, described compositions also bag silyl hydride addition curing catalyst and hydrosilylation inhibitor, the content of wherein said silicon hydrogenation addition curing catalyst is 0.1~1000ppm, and based on the consumption of described hydrosilylation inhibitor the 0.001~1wt% of component.
Silicon composition the most according to claim 7, it is characterised in that the content of the hydrogenation addition curing catalyst of silicon described in described compositions is 1~100ppm.
Silicon composition the most according to claim 8, it is characterised in that the content of the hydrogenation addition curing catalyst of silicon described in described compositions is 1~20ppm.
Silicon composition the most according to claim 7, it is characterised in that based on the consumption of described hydrosilylation inhibitor the 0.005~0.5wt% of component.
11. silicon compositions according to claim 10, it is characterised in that based on the consumption of described hydrosilylation inhibitor the 0.01~0.1wt% of component.
12. silicon compositions according to claim 1, it is characterised in that described compositions also comprises more than one adhesive accelerants, and the content of described adhesive accelerant is 0.001~10wt%.
13. silicon compositions according to claim 12, it is characterised in that the content of adhesive accelerant described in described compositions is 0.01~5.0wt%.
14. silicon compositions according to claim 13, it is characterised in that the content of adhesive accelerant described in described compositions is 0.01~1.0wt%.
15. silicon compositions according to claim 14, it is characterised in that the content of adhesive accelerant described in described compositions is 0.01~0.05wt%.
16. silicon compositions according to claim 1, it is characterised in that the solidfied material formed by described compositions for the index of refraction of visible ray between 1.35~1.60.
17. silicon compositions according to claim 16, it is characterised in that the solidfied material formed by described compositions is 1.5~1.60 for the index of refraction of visible ray.
Silicon composition according to any one of 18. claim 1-17 is in bonding article or at least application in packaged articles local surfaces.
19. 1 kinds of article adhering methods, it is characterised in that including:
First article and the second article are provided,
The silicon composition according to any one of claim 1-17 is applied between the first article and the second article,
And, under the conditions of selected temperature, make described silicon composition heat cure, thus the first article and the second article are adhesively fixed.
20. 1 kinds of method for packing, it is characterised in that including:
At least at the selected regional area of article surface and/or inside as packaging area,
And, apply the silicon composition according to any one of claim 1-17 at described packaging area,
And, in described silicon composition heat cure under the conditions of selected temperature, complete the encapsulation to article.
21. 1 kinds of electronic devices or photoelectric device, it is characterised in that it comprises the solidfied material that silicon composition according to any one of claim 1-17 is formed, and wherein said photoelectric device includes that semiconductor light-emitting elements, described semiconductor light-emitting elements include LED.
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JP2017504715A (en) 2013-12-05 2017-02-09 ハネウェル・インターナショナル・インコーポレーテッド Stannous methanesulfonate solution with controlled pH
CA2951437C (en) 2014-07-07 2022-03-15 Honeywell International Inc. Thermal interface material with ion scavenger
ES2886846T3 (en) 2014-12-05 2021-12-21 Honeywell Int Inc High performance thermal interface materials with low thermal impedance
CN104927403B (en) * 2015-06-18 2017-06-06 合肥工业大学 A kind of preparation method of high perofmrnace lubricating oils additive
US10312177B2 (en) 2015-11-17 2019-06-04 Honeywell International Inc. Thermal interface materials including a coloring agent
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US10501671B2 (en) 2016-07-26 2019-12-10 Honeywell International Inc. Gel-type thermal interface material
US11041103B2 (en) 2017-09-08 2021-06-22 Honeywell International Inc. Silicone-free thermal gel
CN109651615A (en) * 2017-10-12 2019-04-19 弗洛里光电材料(苏州)有限公司 Nano hybridization molecular compound and application containing multiple si-h bonds and phenyl
US10428256B2 (en) 2017-10-23 2019-10-01 Honeywell International Inc. Releasable thermal gel
US11072706B2 (en) 2018-02-15 2021-07-27 Honeywell International Inc. Gel-type thermal interface material
CN108865029A (en) * 2018-05-29 2018-11-23 滁州君越高分子新材料有限公司 A kind of super-low-hardness glue
JP7391401B2 (en) * 2019-02-22 2023-12-05 浙江三時紀新材科技有限公司 Method for preparing polysiloxane powder filler, polysiloxane powder filler obtained thereby and its application
WO2020168542A1 (en) * 2019-02-22 2020-08-27 湖州五爻硅基材料研究院有限公司 Method for preparing spherical or angular powder filler, spherical or angular powder filler obtained thereby and application thereof
US11373921B2 (en) 2019-04-23 2022-06-28 Honeywell International Inc. Gel-type thermal interface material with low pre-curing viscosity and elastic properties post-curing
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JP4991881B2 (en) * 2007-03-07 2012-08-01 サン−ゴバン パフォーマンス プラスティックス コーポレイション Articles containing silicone compositions and methods for their production
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