CN108203545A - Solid-state silicon resin composition and its preparation method and application and optoelectronic part case - Google Patents
Solid-state silicon resin composition and its preparation method and application and optoelectronic part case Download PDFInfo
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- CN108203545A CN108203545A CN201611175374.2A CN201611175374A CN108203545A CN 108203545 A CN108203545 A CN 108203545A CN 201611175374 A CN201611175374 A CN 201611175374A CN 108203545 A CN108203545 A CN 108203545A
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- resin composition
- silicon resin
- state silicon
- silicones
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 60
- 239000010703 silicon Substances 0.000 title claims abstract description 60
- 239000011342 resin composition Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 230000005693 optoelectronics Effects 0.000 title claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 52
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 51
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 48
- 239000003054 catalyst Substances 0.000 claims abstract description 25
- 238000006459 hydrosilylation reaction Methods 0.000 claims abstract description 22
- 239000003112 inhibitor Substances 0.000 claims abstract description 21
- 239000011256 inorganic filler Substances 0.000 claims abstract description 18
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 18
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 14
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 230000009477 glass transition Effects 0.000 claims abstract description 12
- 238000007711 solidification Methods 0.000 claims abstract description 7
- 230000008023 solidification Effects 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 229910020388 SiO1/2 Inorganic materials 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 7
- 239000004408 titanium dioxide Substances 0.000 claims description 7
- 229910020487 SiO3/2 Inorganic materials 0.000 claims description 6
- 238000006482 condensation reaction Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 239000012670 alkaline solution Substances 0.000 claims description 5
- 235000013339 cereals Nutrition 0.000 claims description 5
- 229910052736 halogen Inorganic materials 0.000 claims description 4
- 150000002367 halogens Chemical class 0.000 claims description 4
- 125000002524 organometallic group Chemical group 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 230000005764 inhibitory process Effects 0.000 claims description 3
- 239000003929 acidic solution Substances 0.000 claims description 2
- 238000007259 addition reaction Methods 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 2
- 235000013312 flour Nutrition 0.000 claims description 2
- 239000000413 hydrolysate Substances 0.000 claims description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 2
- 125000006527 (C1-C5) alkyl group Chemical group 0.000 claims 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 238000004383 yellowing Methods 0.000 abstract description 5
- 238000005538 encapsulation Methods 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 239000007788 liquid Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 235000010215 titanium dioxide Nutrition 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 6
- 239000004954 Polyphthalamide Substances 0.000 description 4
- 229920006375 polyphtalamide Polymers 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 206010015856 Extrasystoles Diseases 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000007430 reference method Methods 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 108010011438 H 77 Proteins 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- QYSYEILYXGRUOM-UHFFFAOYSA-N [Cl].[Pt] Chemical compound [Cl].[Pt] QYSYEILYXGRUOM-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- RCNRJBWHLARWRP-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane;platinum Chemical compound [Pt].C=C[Si](C)(C)O[Si](C)(C)C=C RCNRJBWHLARWRP-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- -1 tetramethyl divinyl Alkane Chemical class 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor 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
- H01L33/48—Semiconductor 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
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
Landscapes
- 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 present invention relates to LED encapsulation fields, disclose a kind of solid-state silicon resin composition and its preparation method and application and optoelectronic part case.The solid-state silicon resin composition contains thermoset solid silicones, inhibitor, white inorganic filler and hydrosilylation catalyst, containing vinyl and silicon hydrogen-based and its glass transition temperature Tg it is simultaneously 80 DEG C or more in the thermoset solid silicones, the inhibitor is can inhibit the thermoset solid silicones less than cured substance occurs under solidification temperature；Relative to the thermoset solid silicones of 100 parts by weight, the content of the inhibitor is 0.1 10 parts by weight, and the content of the white inorganic filler is 40 500 parts by weight, and the content of the hydrosilylation catalyst is 0.1 10 parts by weight.Silicon resin composition provided by the invention is with excellent adhesive property, high temperature resistance, light transmission, anti-yellowing property and higher hardness.
Description
Technical field
The present invention relates to LED encapsulation fields, and in particular, to a kind of solid-state silicon resin composition and preparation method thereof and should
With and optoelectronic part case.
Background technology
Light emitting diode (LED) is a kind of solid state semiconductor devices, can directly convert electrical energy into luminous energy.LED
Headlamp has the characteristics that size is small, efficient, low energy consumption, color clear, ageing time are long, is easily installed, and LED illumination lamp will
Replace the conventional light sources such as incandescent lamp, fluorescent lamp and become forth generation lighting source.With LED illumination lamp power it is continuous promoted and
The continuous diminution of volume, the calorific value of single device are obviously improved, so as to also propose higher want to LED support encapsulating material
It asks.LED support encapsulating material mainly includes polyphthalamide (PPA) resin, thermoplasticity amide resinoid, thermoset epoxy
Resin and organic siliconresin.Wherein, PPA resins degrade there are serious and visual aberration easily occurs, come off and machine
The reduction of tool intensity, and PPA resins easily tend to turn yellow under long-time hot conditions, the compatibility with LED encapsulation silicones
It is poor, easy peeling off phenomenon.In addition, traditional thermoplasticity amide resinoid has that temperature tolerance is poor, is bonded force difference,
And there is anti-yellowing variation in thermosetting epoxy resin.This three classes material cannot gradually meet LED support encapsulating material
Requirement to high power, high heat, high bonding.Then there is no these problems for organic siliconresin, it has high-mechanical property and height
Heat resistance, but existing thermoset silicone material is usually liquid, can not be normally used for LED support Packaging Industry.Cause
This, at present there is an urgent need for developing a kind of new LED support encapsulating material, to meet the above demand of LED illumination lamp.
Invention content
The present invention be in order to solve existing LED support encapsulating material there are the defects of bonding force and poor high temperature resistance,
And provide a kind of new solid-state silicon resin composition and its preparation method and application and optoelectronic part case.
Specifically, the present invention provides a kind of solid-state silicon resin composition, wherein, the solid-state silicon resin composition contains
Thermoset solid silicones, inhibitor, white inorganic filler and hydrosilylation catalyst, it is same in the thermoset solid silicones
Shi Hanyou vinyl and silicon hydrogen-based and its glass transition temperature Tg are 80 DEG C or more, and the inhibitor is can inhibit the heat
Solidity solid silicon resin is less than occurring cured substance under solidification temperature；Relative to the thermoset solid of 100 parts by weight
Silicones, the content of the inhibitor are 0.1-10 parts by weight, and the content of the white inorganic filler is 40-500 parts by weight, institute
The content for stating hydrosilylation catalyst is 0.1-10 parts by weight.
The present invention also provides the preparation method of the solid-state silicon resin composition, this method includes consolidating the thermosetting property
Body silicones, inhibitor, white inorganic filler and hydrosilylation catalyst are uniformly mixed.
The present invention also provides application of the solid-state silicon resin composition as LED support encapsulating material.
In addition, the present invention also provides a kind of optoelectronic part case, wherein, the optoelectronic part case is by the present invention
The cured formation of solid-state silicon resin composition of offer.
The present inventor has found after further investigation, when will be simultaneously containing vinyl and silicon hydrogen-based and with spy
The thermoset solid silicones of glass transition temperature is determined with inhibitor, white inorganic filler and hydrosilylation catalyst according to spy
Fixed ratio is used cooperatively, and the silicon resin composition of gained is not only solid-state, can successfully be applied to LED support encapsulation row
Industry, it is even more important that the silicon resin composition is also with excellent adhesive property, high temperature resistance, light transmission, resistance to Huang
Become performance and higher hardness, adhesive strength is more than 5MPa, and heat resisting temperature can reach 200 DEG C or more, hardness be 80D,
Light transmittance under 400nm wavelength may be up to more than 92%, and baking 10h is non-discolouring at 200 DEG C, and hardness is more than 80D, very suitable
It shares and makees LED support encapsulating material, great prospects for commercial application.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
The specific embodiment of the present invention is described in detail below.It is it should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood to comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It between the endpoint value of a range and individual point value and can be individually combined with each other between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
Solid-state silicon resin composition provided by the invention contains thermoset solid silicones, inhibitor, white inorganic filler
And hydrosilylation catalyst, simultaneously containing vinyl and silicon hydrogen-based and its glass transition temperature in the thermoset solid silicones
It is 80 DEG C or more to spend Tg, and the inhibitor is can inhibit the thermoset solid silicones solid less than occurring under solidification temperature
The substance of change；Relative to the thermoset solid silicones of 100 parts by weight, the content of the inhibitor is 0.1-10 weight
Part, the content of the white inorganic filler is 40-500 parts by weight, and the content of the hydrosilylation catalyst is 0.1-10 weight
Part.
According to the present invention, the glass transition temperature Tg of the thermoset solid silicones should be 80 DEG C or more, preferably
It is 90-250 DEG C, most preferably 100-200 DEG C.The content of the thermoset solid silicones medium vinyl and the content of silicon hydrogen-based
Molar ratio be preferably (1-2): 1, more preferably (1-1.5): 1, most preferably (1-1.3): 1.
In accordance with the present invention it is preferred that relative to the thermoset solid silicones of 100 parts by weight, the inhibitor
Content is 0.1-8 parts by weight, and the content of the white inorganic filler is 45-450 parts by weight, and the hydrosilylation catalyst contains
It measures as 0.1-8 parts by weight；It is highly preferred that relative to the thermoset solid silicones of 100 parts by weight, the inhibitor contains
It measures as 0.2-5 parts by weight, the content of the white inorganic filler is 45-400 parts by weight, the content of the hydrosilylation catalyst
For 0.2-0.5 parts by weight.
A preferred embodiment of the invention, shown in the composition such as formula (1) of the thermoset solid silicones：
(R1SiO3/2)a(R2SiO)b(R3SiO1/2)c(R4SiO1/2)d (1)
Wherein, R1And R2It is each independently C6-C10Aryl or C1-C5Alkyl, R3For vinyl, R4For silicon hydrogen
Base, a, b, c and d are each independently more than 2 integer；Preferably, R1And R2It is each independently phenyl or C1-C3Alkane
Base, R3For vinyl, R4For silicon hydrogen-based, a, b, c and d are each independently the integer of 4-100.
The thermoset solid silicones can be commercially available, can also be according to well known to a person skilled in the art each
Kind method is prepared.A kind of specific embodiment according to the present invention, the thermoset solid silicones is in accordance with the following methods
It is prepared：
(1) by R1Si(R)3(R2)2Si(R’)2Mixture be hydrolyzed in an acidic solution or in alkaline solution instead
Should, hydrolysate is subjected to condensation reaction later；
(2) product of the condensation reaction is used into the mixing containing organosilicon shown in organosilicon shown in formula (2) and formula (3)
Object carries out end capping reaction；
Wherein, R1And R2It is each independently C6-C10Aryl or C1-C5Alkyl, R3And R4It is each independently
C1-C5Alkyl, R and R ' are each independently halogen or C1-C5Alkoxy, R3And R4It is each independently C1-C5Alkane
Base；Preferably, R1And R2It is each independently phenyl or C1-C3Alkyl, R and R ' are each independently halogen or C1-C3's
Alkoxy, R3And R4It is each independently C1-C3Alkyl.
According to the present invention, in the preparation process of the thermoset solid silicones, the acid solution can be hydrochloric acid
At least one of aqueous solution, aqueous sulfuric acid, phosphate aqueous solution, aqueous solution of nitric acid, the alkaline solution can be ammonium hydroxide, carbon
Acid sodium aqueous solution, wet chemical, ammonium carbonate solution, sodium bicarbonate aqueous solution, potassium bicarbonate aqueous solution and ammonium hydrogen carbonate
At least one of aqueous solution.It is full to it that the concentration of the acid solution and alkaline solution can be each independently 10 weight %
And concentration.In addition, the dosage of the acid solution and alkaline solution can be the conventional selection of this field, as long as enabling to
R1Si(R)3(R2)2Si(R’)2Mixture be fully hydrolyzed, this those skilled in the art can be known, do not made herein
It repeats.
According to the present invention, in the preparation process of the thermoset solid silicones, do not have to the dosage of four kinds of organosilicons
It is special to limit, it is preferable that relative to the R of 1mol1Si(R)3, (R2)2Si(R’)2Dosage for 0.1-8mol, more preferably
0.1-0.5mol；The dosage of organosilicon shown in formula (3) is 0.01-1mol, more preferably 0.05-0.5mol；It is organic shown in formula (4)
The dosage of silicon is 0.01-1mol, more preferably 0.05-0.5mol.
There is no particular limitation for condition of the present invention to the condensation reaction, it is preferable that including reaction temperature be 40-60
DEG C, more preferably 45-50 DEG C；Reaction time is 1-5h, more preferably 4-5h.
There is no particular limitation for condition of the present invention to the end capping reaction, it is preferable that including reaction temperature be 100-120
DEG C, more preferably 105-110 DEG C；Reaction time is 2-10h, more preferably 5-8h.
The present invention is not particularly limited the type of the inhibitor, can be that existing various can inhibit the heat
Solidity solid silicon resin is less than occurring cured substance under solidification temperature.For example, the inhibitor can be alkynol, tetramethyl
Tetravinyl cyclotetrasiloxane (D4viAt least one of) and tetramethyl divinyl disiloxane.The angle ready availability from raw material
Degree considers that the inhibitor is particularly preferably alkynol and/or t etram-ethyltetravinylcyclotetrasiloxane.
The present invention is not particularly limited the type of the white filler, can be that existing various can improve whiteness
With the substance of reflectivity.For example, the white inorganic filler can be at least one in titanium dioxide, silica flour and gas-phase silica
Kind.From the point of view of raw material is ready availability, the white filler is particularly preferably titanium dioxide and/or gas-phase silica.In addition,
The average grain diameter of the white inorganic filler is preferably 0.1-3 μm, more preferably 0.5-0.8 μm.
The present invention is not particularly limited the type of the hydrosilylation catalyst, can be existing various can make
Obtain the substance that vinyl and silicon hydrogen-based in the thermoset solid silicones react.For example, the Si―H addition reaction catalysis
Agent can be Organometallic complex catalyst.The specific example of the Organometallic complex catalyst includes but not limited to 1,3- bis-
Vinyl -1,1,3,3- tetramethyl disiloxane platinum complexs, t etram-ethyltetravinylcyclotetrasiloxane platinum complex and chlorine platinum
At least one of acid.From the point of view of raw material is ready availability, the hydrosilylation catalyst is particularly preferably 1,3- divinyls
Base -1,1,3,3- tetramethyl disiloxane platinum complexs.
The preparation method of the solid-state silicon resin composition provided by the invention include by the thermoset solid silicones,
Inhibitor, white inorganic filler and hydrosilylation catalyst are uniformly mixed.Wherein, the mixing can be in existing various mixing
It is carried out in equipment, for example, can be carried out in existing various twin-roll machines, kneader-mixer.
The present invention also provides application of the solid-state silicon resin composition as LED support encapsulating material.
In addition, the present invention also provides a kind of optoelectronic part case, wherein, the optoelectronic part case is by described solid
The cured formation of state silicon resin composition.
The concrete shape and structure of the optoelectronic part case can be designed according to actual needs, and can be led to
The shape and structure for crossing mold are controlled.A kind of specific embodiment according to the present invention, the optoelectronic part case lead to
It crosses and injects the solid-state silicon resin composition in mold, then cured to obtain.
The present invention is not particularly limited the cured condition, as long as enabling to the thermoset solid silicones
In vinyl and silicon hydrogen-based hydrosilylation occurs under the action of hydrosilylation catalyst.For example, the curing
Condition generally include solidification temperature can be 80-150 DEG C, preferably 100-120 DEG C；Hardening time can be 10-120s, excellent
It is selected as 50-60s.
The present invention will be described in detail by way of examples below.
In following embodiment and comparative example：
Glass transition temperature is surveyed using MDSC2910 types differential scanning calorimetry (DSC) instrument of TA companies of the U.S.
It is fixed, wherein, modulation period 60s, modulated amplitude is ± 1.5 DEG C, and heating rate is 10 DEG C/min, nitrogen protection, N2Flow velocity
For 50mL/min.
Preparation example 1
The preparation example is used for the preparation method for illustrating thermoset solid silicones provided by the invention.
(1) organosilicon shown in raw material 3.5mol formulas (4) and the organosilicon shown in 1.4mol formulas (5) are uniformly mixed, connect
The HCl solution that a concentration of 37 weight % of 50g are added dropwise at 0 DEG C, is added dropwise in 1 hour；Then reaction temperature is increased to
And 4h is reacted at such a temperature, vacuumize later by 40 DEG C, the waste liquid generated except dereaction.
(2) organosilicon shown in 0.2mol formulas (6), organosilicon and 4mol solvents two shown in 0.2mol formulas (7) are added in
Reaction temperature is increased to 100 DEG C later and reacts 8h at such a temperature by toluene, then washes product, and liquid separation removes low-boiling-point substance,
Obtain thermoset solid silicones (ph-SiO3/2)35(ph2-SiO)14(Vi-SiO1/2)4(H-SiO1/2)4(wherein, ph represents benzene
Base, Vi represent vinyl, similarly hereinafter), glass transition temperature Tg is 105 DEG C.
Preparation example 2
The preparation example is used for the preparation method for illustrating thermoset solid silicones provided by the invention.
(1) organosilicon shown in raw material 3.5mol formulas (4) and the organosilicon shown in 1.4mol formulas (5) are uniformly mixed, connect
The HCl solution that a concentration of 37 weight % of 50g are added dropwise at 10 DEG C, is added dropwise in 1 hour；Then reaction temperature is increased to
And 2h is reacted at such a temperature, vacuumize later by 60 DEG C, the waste liquid generated except dereaction.
(2) organosilicon shown in 0.5mol formulas (6), organosilicon and 4mol solvents two shown in 0.45mol formulas (7) are added in
Reaction temperature is increased to 120 DEG C later and reacts 8h at such a temperature by toluene, then washes product, and liquid separation removes low-boiling-point substance,
Obtain thermoset solid silicones (ph-SiO3/2)70(ph2-SiO)35(Vi-SiO1/2)10(H-SiO1/2)9, glass transition temperature
It is 101 DEG C to spend Tg.
Preparation example 3
The preparation example is used for the preparation method for illustrating thermoset solid silicones provided by the invention.
(1) organosilicon shown in raw material 5mol formulas (4) and the organosilicon shown in 1mol formulas (5) are uniformly mixed, then 5
The HCl solution of a concentration of 37 weight % of 50g is added dropwise at DEG C, is added dropwise in 1 hour；Then reaction temperature is increased to 50 DEG C simultaneously
3h is reacted at such a temperature, is vacuumized later, the waste liquid generated except dereaction.
(2) organosilicon shown in 0.5mol formulas (6), organosilicon and 4mol solvents two shown in 0.45mol formulas (7) are added in
Reaction temperature is increased to 110 DEG C later and reacts 8h at such a temperature by toluene, then washes product, and liquid separation removes low-boiling-point substance,
Obtain thermoset solid silicones (ph-SiO3/2)50(ph2-SiO)10(Vi-SiO1/2)10(H-SiO1/2)8, glass transition temperature
It is 200 DEG C to spend Tg.
Compare preparation example 1
The comparison preparation example is used for the preparation method for illustrating the thermoset solid silicones of reference.
(1) organosilicon shown in raw material 1mol formulas (4) and the organosilicon shown in 0.5mol formulas (5) are uniformly mixed, then
The HCl solution of a concentration of 37 weight % of 50g is added dropwise at 5 DEG C, is added dropwise in 1 hour；Then reaction temperature is increased to 50
DEG C and react 3h at such a temperature, vacuumize later, except dereaction generate waste liquid.
(2) organosilicon shown in 0.5mol formulas (6), organosilicon and 1mol solvents two shown in 0.5mol formulas (7) are added in
Reaction temperature is increased to 110 DEG C later and reacts 8h at such a temperature by toluene, then washes product, and liquid separation removes low-boiling-point substance,
Obtain thermoset solid silicones (ph-SiO3/2)10(ph2-SiO)5(Vi-SiO1/2)10(H-SiO1/2)10, glass transition temperature
It is 30 DEG C to spend Tg.
Embodiment 1
The embodiment is used to illustrate solid-state silicon resin composition provided by the invention and preparation method thereof.
By the thermoset solid silicones obtained by preparation example 1 of 20 weight %, the D4 of 1 weight %Vi, 78 weight % it is flat
Titanium dioxide that equal grain size is 0.2 μm, (hydrosilylation catalyst is chloroplatinic acid and MM to the hydrosilylation catalyst of 1 weight %vi's
Complex compound, is the commercial product that the Jinan Fu Jing chemical companies trade mark is H-77, MMviRepresent two silica of tetramethyl divinyl
Alkane, similarly hereinafter) uniformly mixed at 100 DEG C, mixing 5min is then heated by bigeminy roller at 100 DEG C, it is then solid at 150 DEG C
Change 20s, obtain cured product, be denoted as G1.
Embodiment 2
The embodiment is used to illustrate solid-state silicon resin composition provided by the invention and preparation method thereof.
By the thermoset solid silicones obtained by preparation example 2 of 50 weight %, the D4 of 0.1 weight %Vi, 49.8 weight %
Average grain diameter be 0.2 μm titanium dioxide, 0.1 weight % hydrosilylation catalyst uniformly mixed at 100 DEG C, then exist
Mixing 5min is heated by bigeminy roller at 100 DEG C, then cures 90s at 150 DEG C, obtains cured product, be denoted as G2.
Embodiment 3
The embodiment is used to illustrate solid-state silicon resin composition provided by the invention and preparation method thereof.
By the thermoset solid silicones obtained by preparation example 3 of 30 weight %, the D4 of 0.5 weight %Vi, 68.5 weight %
Average grain diameter be 0.2 μm titanium dioxide, 1 weight % hydrosilylation catalyst uniformly mixed at 100 DEG C, then 100
Mixing 5min is heated by bigeminy roller at DEG C, then cures 10s at 150 DEG C, obtains cured product, be denoted as G3.
Comparative example 1
The embodiment is used to illustrate solid-state silicon resin composition of reference and preparation method thereof.
Solid-state silicon resin composition and cured product are prepared according to the method for embodiment 1, unlike, the thermosetting property is consolidated
The dosage of body silicones is 10 weight %, and the dosage of the titanium dioxide is 88 weight %, obtains reference cured product, is denoted as
DG1。
Comparative example 2
The embodiment is used to illustrate solid-state silicon resin composition of reference and preparation method thereof.
Solid-state silicon resin composition and cured product are prepared according to the method for embodiment 1, unlike, it is added without titanium white
Powder obtains reference cured product, is denoted as DG2.
Comparative example 3
The embodiment is used to illustrate solid-state silicon resin composition of reference and preparation method thereof.
Solid-state silicon resin composition and cured product are prepared according to the method for embodiment 1, unlike, it will be by preparation example 1
Obtained thermoset solid silicones is replaced using the thermoset solid silicones obtained by comparison preparation example 1 of identical weight part
In generation, obtains reference cured product, is denoted as DG3.
Test case
The test of product property that test case is cured for explanation by solid-state silicon resin composition.
(1) test of hardness：
Above-mentioned cured product at 30 DEG C is toasted into 0.5h respectively, hardness is tested using Shore durometer later, as a result sees
Table 1.
(2) test of adhesive property：
Corresponding solid-state silicon resin composition in above example and comparative example is respectively adopted, two silver strips are bonded in one
It rises, wherein, bonded areas size is (28.1mm × 10mm), later using model machine is drawn to pull open two silver strips, measures maximum drawing
Intensity is stretched, the results are shown in Table 1.
(3) test of light transmittance：
The light transmittance of above-mentioned cured product is measured using determination of light transmittance instrument, wherein, use the wavelength of light for
400nm the results are shown in Table 1.
(4) test of heat resisting temperature and anti-yellowing property：
Heat resisting temperature is exactly the non-discolouring temperature of material baking 10h, the results are shown in Table 1.
Color inhibition experiment is that 10h is toasted under the conditions of 200 DEG C, and the resin is non-discolouring on this condition, then illustrates color inhibition
Property is good, on the contrary then illustrate that yellowing resistance is poor, the results are shown in Table 1.
Table 1
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Appearance | White | White | White | White | White | White |
| Hardness | 80 | 80 | 80 | 50 | 50 | 50 |
| Adhesive strength | 5.6MPa | 5.4MPa | 6.4MPa | 4.2MPa | 4.1MPa | 4.2MPa |
| Light transmittance % | 92 | 94 | 94 | 90 | 91 | 90 |
| Heat resisting temperature DEG C | 200 | 200 | 200 | 200 | 200 | 200 |
As can be seen from the above results, silicon resin composition provided by the invention is with excellent adhesive property, resistance to height
Warm nature energy, light transmission, anti-yellowing property and higher hardness, adhesive strength are more than 5MPa, and heat resisting temperature can reach 200
DEG C or more, the light transmittance in the case where hardness is 80D, 400nm wavelength may be up to more than 92%, and baking 10h is non-discolouring at 200 DEG C,
Hardness is more than 80D, is highly suitable as LED support encapsulating material.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail, within the scope of the technical concept of the present invention, a variety of simple variants can be carried out to technical scheme of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, it can be combined by any suitable means.In order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (11)
1. a kind of solid-state silicon resin composition, which is characterized in that the solid-state silicon resin composition contains thermoset solid silicon tree
Fat, inhibitor, white inorganic filler and hydrosilylation catalyst, in the thermoset solid silicones simultaneously containing vinyl and
Silicon hydrogen-based and its glass transition temperature Tg are 80 DEG C or more, and the inhibitor is can inhibit the thermoset solid silicones
Less than cured substance occurs under solidification temperature；Relative to the thermoset solid silicones of 100 parts by weight, the inhibition
The content of agent is 0.1-10 parts by weight, and the content of the white inorganic filler is 40-500 parts by weight, the Si―H addition reaction catalysis
The content of agent is 0.1-10 parts by weight.
2. solid-state silicon resin composition according to claim 1, wherein, the thermoset solid silicones medium vinyl
The molar ratio of content and the content of silicon hydrogen-based is (1-2): 1；The glass transition temperature Tg of the thermoset solid silicones is
100-200℃。
3. solid-state silicon resin composition according to claim 1, wherein, the composition such as formula of the thermoset solid silicones
(1) shown in：
(R1SiO3/2)a(R2SiO)b(R3SiO1/2)c(R4SiO1/2)d (1)
Wherein, R1And R2It is each independently C6-C10Aryl or C1-C5Alkyl, R3For vinyl, R4For silicon hydrogen-based,
A, b, c and d are each independently more than 2 integer；Preferably, R1And R2It is each independently phenyl or C1-C3Alkyl, R3
For vinyl, R4 is silicon hydrogen-based, and a, b, c and d are each independently the integer of 4-100.
4. the solid-state silicon resin composition according to any one in claim 1-3, wherein, the thermoset solid silicon tree
Fat is prepared in accordance with the following methods：
(1) by R1Si(R)3(R2)2Si(R’)2Mixture reaction is hydrolyzed in an acidic solution or in alkaline solution, it
Hydrolysate is subjected to condensation reaction afterwards；
(2) by the product of the condensation reaction use the mixture containing organosilicon shown in organosilicon shown in formula (2) and formula (3) into
Row end capping reaction；
Wherein, R1And R2It is each independently C6-C10Aryl or C1-C5Alkyl, R3And R4It is each independently C1-C5
Alkyl, R and R ' are each independently halogen or C1-C5Alkoxy, R3And R4It is each independently C1-C5Alkyl；
Preferably, R1And R2It is each independently phenyl or C1-C3Alkyl, R and R ' are each independently halogen or C1-C3Alcoxyl
Base, R3And R4It is each independently C1-C3Alkyl；
Preferably, it is 40-60 DEG C that the condition of the condensation reaction, which includes reaction temperature, reaction time 1-5h；
Preferably, it is 100-120 DEG C that the condition of the end capping reaction, which includes reaction temperature, reaction time 2-10h.
5. the solid-state silicon resin composition according to any one in claim 1-3, wherein, the inhibitor is alkynol,
At least one of t etram-ethyltetravinylcyclotetrasiloxane and tetramethyl divinyl disiloxane.
6. the solid-state silicon resin composition according to any one in claim 1-3, wherein, the white inorganic filler is
At least one of titanium dioxide, silica flour and gas-phase silica；Preferably, the average grain diameter of the white inorganic filler is 0.1-
3μm。
7. the solid-state silicon resin composition according to any one in claim 1-3, wherein, the hydrosilylation catalyst
For Organometallic complex catalyst；Preferably, the Organometallic complex catalyst be 1,3- divinyl -1,1,3,3- tetramethyls
At least one of base disiloxane platinum complex, t etram-ethyltetravinylcyclotetrasiloxane platinum complex and chloroplatinic acid.
8. the preparation method of the solid-state silicon resin composition in claim 1-7 described in any one, this method is included by described in
Thermoset solid silicones, inhibitor, white inorganic filler and hydrosilylation catalyst are uniformly mixed.
9. application of the solid-state silicon resin composition as LED support encapsulating material in claim 1-7 described in any one.
10. a kind of optoelectronic part case, which is characterized in that the optoelectronic part case is by any one in claim 1-7
The cured formation of solid-state silicon resin composition described in.
11. optoelectronic part case according to claim 10, wherein, the cured condition is including solidification temperature
80-150 DEG C, hardening time 10-120s.
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