CN103834356A - Carbon-based white light-emitting material encapsulation adhesive - Google Patents

Carbon-based white light-emitting material encapsulation adhesive Download PDF

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Publication number
CN103834356A
CN103834356A CN201210488519.XA CN201210488519A CN103834356A CN 103834356 A CN103834356 A CN 103834356A CN 201210488519 A CN201210488519 A CN 201210488519A CN 103834356 A CN103834356 A CN 103834356A
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white light
emitting material
light emitting
packaging plastic
carbon back
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CN103834356B (en
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裴昌龙
徐立环
陈卡凌
阮环阳
陶杰
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Zhejiang Chemical Industry Research Institute Co Ltd
Sinochem Lantian Co Ltd
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Zhejiang Chemical Industry Research Institute Co Ltd
Sinochem Lantian Co Ltd
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Abstract

The invention provides a novel white light-emitting material encapsulation adhesive. The encapsulation adhesive is prepared from vinyl-terminated polysiloxane, MQ resin, hydrogen-containing silicone oil, a carbon-based white light-emitting material, a platinum catalyst, a catalyst inhibitor and a tackifier. The encapsulation adhesive has the characteristics of high bonding strength, high light transmittance, heat resistance, cold resistance, ultraviolet radiation resistance, chemical corrosion resistance, good mechanical property, good electrical property and the like. The encapsulation adhesive has a small encapsulation curing shrinkage rate. Thus, the encapsulation requirement of a photoelectric device is satisfied.

Description

A kind of carbon back white light emitting material packaging plastic
Technical field
The present invention relates to a kind of carbon back white light emitting material packaging plastic.
Background technology
Along with the raising of the Performance And Reliability of luminescent material in recent years, the application of high-performance white light emitting material has been penetrated into every subjects field, has formed a huge application network and has covered.Luminescent material has that efficiency is high, good reliability, stable performance, volume is little, the life-span is long and the advantage such as lightweight, be widely used in illumination, information processing, biology and medical science,, the field such as communication, laser chemistry and national defense safety, and greatly promoted technology and the industry development in these fields.Along with the development of luminescent device, luminescence technology and perfect, the demand of the laser apparatus of people to high-energy, high light beam quality, compact construction, good stability is more and more urgent.
In recent years the novel white-light luminescent material of exploitation have luminous efficiency high, produces that laser, energy height are concentrated, monochromaticity is good, color is pure, directive property is good, diffustivity is little etc. by photoluminescence and has very much advantage.This its principle of luminosity of class New Type of Carbon based luminescent material is the optical excitation New Type of Carbon sill of certain wavelength; send very strong white light; but this carbon back white light emitting material itself does not possess uvioresistant, the provide protection such as anti-oxidation; when luminescent material is by the optical excitation of certain wavelength simultaneously, can produce a large amount of heats, this just need to be encapsulated in carbon-based material in one protection system.And keeping conventional cure package glue in high transmission rate situation at present, the present invention is the organosilicon material for individual laser package.Just like the encapsulation of LED, the packaged material of laser apparatus requires to have the higher transparency (transmittance reaches more than 90%), heat-resisting (at 200 DEG C can life-time service), and corrosion-resistant, percent thermal shrinkage is low, UV resistant and stronger mechanical property.At present, can meet the packaged material of properties.Only have organic silica gel and epoxy resin glue, but the not resistance to ultraviolet of epoxy resin, for a long time under rayed, can produce the phenomenon of jaundice, therefore can only use organosilicon silica gel to encapsulate, ensure that white light laser is keeping higher transmittance and mechanical property under ultraviolet excitation state for a long time, and under long illumination, without Yellowing.Organic silica gel is divided into two kinds conventionally, and one is condensed type silica gel, and one is add-on type silica gel.In the time using condensed type silica gel to be cured, due to condensation cured middle generation small molecules, the terminal hydroxy group of part can not get solidifying simultaneously, and causes at high temperature from terminal portion generation molecular rupture, thereby causes the defects such as mechanical property variation.Use add-on type silica gel can avoid this situation.
Summary of the invention
The object of the present invention is to provide a kind of packaging plastic of novel carbon back white light laser.
For reaching goal of the invention the technical solution used in the present invention be:
A kind of carbon back white light emitting material packaging plastic, preparation by the following method:
(1), after the polysiloxane of ethenyl blocking is fully mixed in reactor with MQ resin, add containing hydrogen silicone oil to mix;
The structural formula of the polysiloxane of described ethenyl blocking is: V ir 3r 4siO (R 1r 2siO) nsiR 3r 4v i, wherein R 1, R 2, R 3, R 4independently selected from methyl or phenyl, V ifor dimethyl vinyl-functional, the integer that n is 200～400;
The structural formula of described MQ resin is: (R 5r 6r 7siO 0.5) m(R 8r 9r 10siO 0.5) n '(SiO 2) y, wherein R 5, R 6, R 7, R 8, R 9independently selected from methyl, ethyl, propyl group, phenyl or sec.-propyl, R 10be selected from propenyl or vinyl, the integer that m is 20～110, n ' is 20～80 integers, the integer that y is 120～300;
The structural formula of described containing hydrogen silicone oil is: R 11r 12r 13siO (R 14hSiO) m 'siR 15r 16r 17, wherein R 11, R 12, R 13, R 14, R 15, R 16, R 17independently selected from methyl, ethyl, propyl group, phenyl, sec.-propyl or aryl, the integer that m ' is 5～240;
The weight ratio of polysiloxane and MQ resin is 0.2～3.1:1, and the mass ratio of polysiloxane and containing hydrogen silicone oil is 0.1～2.7:1;
(2) in reactor, add carbon back white light emitting material;
(3) in reactor, add platinum catalyst, catalyst-initiator and tackifier, fully mix;
(4) reactor being evacuated to reactor pressure is-0.1～-0.09MPa, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 1～3 hour, solidification value is 60～95 DEG C, obtains carbon back white light emitting material packaging plastic after then keeping 1.2～2.8 hours at 140～160 DEG C of temperature.
As preferred mode, the viscosity of the polysiloxane of above-mentioned ethenyl blocking is 6000～140000mPas.
As preferred mode, mole proportioning of the M/Q of above-mentioned MQ resin is 0.6～0.9:1; In MQ resin structure formula, m is preferably 50～90 integer, and n ' is preferably 20～60 integers, and y is preferably 140～220 integer.
As preferred mode, above-mentioned Silicon Containing Hydrogen oil viscosity is 25～3500mPas; In containing hydrogen silicone oil structural formula, m ' is preferably 20～110 integer.
Above-mentioned platinum catalyst is preferably the platinum catalyst of tetrahydrofuran (THF) coordination and/or the platinum catalyst of tetramethyl divinyl siloxanes coordination, and the consumption of platinum catalyst accounts for 0.01 ‰～0.8 ‰ of packaging plastic total mass.
Above-mentioned catalyst-initiator be preferably be selected from 3-methyl isophthalic acid-butine-3-alcohol, 1-acetylene basic ring ethanol and-one, two or three in phenyl-ethyl acetylene-3-alcohol, the consumption of catalyst-initiator accounts for 0.2%～1.3% of packaging plastic total mass.
Above-mentioned tackifier are preferably γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and/or γ-methacryloxypropyl trimethoxy silane, and the consumption of tackify knot accounts for 0.2%～3% of packaging plastic total mass.
Carbon back white light emitting material used in the present invention can be according to Observation of white-lightamplified spontaneous emission from carbon nanodots under laserexcitation, Adv Mater, method preparation described in 24,2263-2267.
Carbon back white light emitting material packaging plastic prepared by the present invention compared to existing technology, has the following advantages:
(1) preparation technology is simple, production cost is low;
(2) packaging plastic of preparing not only has high bond strength and high transmission rate, possesses heat-resisting, cold-resistant, ultraviolet light resistant, chemicals-resistant corrosion and good mechanical property and electrical property simultaneously;
(3) package curing shrinking percentage is little, meets the encapsulation requirement of photoelectric device.
Embodiment
Below in conjunction with specific embodiment, the present invention will be described, but do not limit the invention in these specific embodiments.One skilled in the art would recognize that the present invention contained all alternativess, improvement project and the equivalents that within the scope of claims, may comprise.
Embodiment 1:
(1) be ViMe by structural formula 2siO (Me 2siO) 350siMe 2the ethenyl blocking polysiloxane 20.03g of Vi, its viscosity is that 65000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 14.62g be mixed in reactor, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 35.46g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.21g is added in the system that above-mentioned (1) mix;
(3) in the product obtaining in step (2), add the platinum catalyst 5.24*10 of tetramethyl divinyl siloxanes coordination -4g, 1-ethynyl-ring ethanol 0.0076g, γ-methacryloxypropyl trimethoxy silane 0.016g, then mix with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 1.37MPa, transmittance are 99%, 1000h is 92% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 2:
(1) be ViMe by structural formula 2siO (Me 2siO) 350siMe 2the ethenyl blocking polysiloxane 20.03g of Vi, its viscosity is that 65000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 14.62g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 35.46g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.21g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.46*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0049g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation be 2.1MPa, transmittance be 99%, at 80 DEG C 1000h without xanthochromia send out, luminous efficiency is 96%.
Embodiment 3:
(1) be ViMe by structural formula 2siO (Me 2siO) 350siMe 2the ethenyl blocking polysiloxane 20.03g of Vi, its viscosity is that 65000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 14.62g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 35.46g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.21g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 4.48*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.034g of g, 1-ethynyl-ring ethanol 0.0062g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 1.75MPa, transmittance are 97%, 1000h is 91% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 4:
(1) be ViMe by structural formula 2siO (Me 2siO) 350siMe 2the ethenyl blocking polysiloxane 20.03g of Vi, its viscosity is that 65000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 14.62g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 35.46g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.21g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.89*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.024g of g, 1-ethynyl-ring ethanol 0.0057g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 2.53MPa, transmittance are 98%, 1000h is 92% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 5:
(1) be ViMe by structural formula 2siO (Me 2siO) 350siMe 2the ethenyl blocking polysiloxane 18.74g of Vi, its viscosity is that 65000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 13.68g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 26.97g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.18g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.26*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0048g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 2.74MPa, transmittance are 98%, 1000h is 94% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 6:
(1) be ViMe by structural formula 2siO (Me 2siO) 350siMe 2the ethenyl blocking polysiloxane 18.74g of Vi, its viscosity is that 65000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 13.68g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 25.81g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.18g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.26*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0048g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 3.05MPa, transmittance are 98%, 1000h is 94% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 7:
(1) be ViMe by structural formula 2siO (Me 2siO) 350siMe 2the ethenyl blocking polysiloxane 18.74g of Vi, its viscosity is that 65000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 13.68g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 24.85g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.18g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.26*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0048g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 4.08MPa, transmittance are 98%, 1000h is 95% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 8:
(1) be ViMe by structural formula 2siO (Me 2siO) 350siMe 2the ethenyl blocking polysiloxane 18.74g of Vi, its viscosity is that 65000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 13.68g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 22.72g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.18g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.26*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0048g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 4.92MPa, transmittance are 98%, 1000h is 96% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 9:
(1) be ViMe by structural formula 2siO (Me 2siO) 300siMe 2the ethenyl blocking polysiloxane 18.74g of Vi, its viscosity is that 53000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 13.68g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 22.72g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.18g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.26*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0048g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 2.69MPa, transmittance are 98%, 1000h is 96% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 10:
(1) be ViMe by structural formula 2siO (Me 2siO) 240siMe 2the ethenyl blocking polysiloxane 18.74g of Vi, its viscosity is that 42000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 13.68g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 25siMe 3containing hydrogen silicone oil 22.72g mix, wherein Silicon Containing Hydrogen oil viscosity is 45mPas;
(2) novel carbon back white light emitting material 0.18g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.26*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0048g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 1.73MPa, transmittance are 99%, 1000h is 96% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 11:
(1) be ViMe by structural formula 2siO (Me 2siO) 240siMe 2the ethenyl blocking polysiloxane 16.45g of Vi, its viscosity is that 42000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 13.68g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 45siMe 3containing hydrogen silicone oil 22.72g mix, wherein Silicon Containing Hydrogen oil viscosity is 104mPas;
(2) novel carbon back white light emitting material 0.18g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.26*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0048g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 2.18MPa, transmittance are 99%, 1000h is 96% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 12:
(1) be ViMe by structural formula 2siO (Me 2siO) 240siMe 2the ethenyl blocking polysiloxane 18.74g of Vi, its viscosity is that 42000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 13.68g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 63siMe 3containing hydrogen silicone oil 22.72g g mix, wherein Silicon Containing Hydrogen oil viscosity is 168mPas;
(2) novel carbon back white light emitting material 0.18g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.26*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0048g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 3.25MPa, transmittance are 99%, 1000h is 96% without xanthochromia, luminous efficiency at 80 DEG C.
Embodiment 13:
(1) be ViMe by structural formula 2siO (Me 2siO) 240siMe 2the ethenyl blocking polysiloxane 18.74g of Vi, its viscosity is that 42000mPas and structural formula are (Me 3siO 0.5) 65(Me 2viSiO 0.5) 88(SiO 2) 206mQ resin 13.68g be mixed in beaker, wherein M/Q mol ratio 0.743, then adding structural formula is Me 3siO (MeHSiO) 80siMe 3containing hydrogen silicone oil 22.72g g mix, wherein Silicon Containing Hydrogen oil viscosity is 290mPas;
(2) novel carbon back white light emitting material 0.18g is added in the system that above-mentioned (1) mix;
(3) the platinum catalyst 3.26*10 of tetramethyl divinyl siloxanes coordination will be added in the product obtaining in step (2) -4the tackifier 0.021g of g, 1-ethynyl-ring ethanol 0.0048g, γ-methacryloxypropyl trimethoxy silane, then mixes with mulser;
(4) product step (3) being obtained vacuumizes the small bubbles in discharge system, until be down to-0.08MPa of reactor pressure, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 2h, solidification value is 80 DEG C, then at 150 DEG C, keeps obtaining after 2 hours carbon back white light emitting material packaging plastic.
The carbon back white light emitting material packaging plastic of preparation is irradiated under the light of certain wavelength, send strong white light.After tested, the cohesive strength of the carbon back white light emitting material packaging plastic of preparation is that 2.67MPa, transmittance are 99%, 1000h is 96% without xanthochromia, luminous efficiency at 80 DEG C.

Claims (9)

1. a carbon back white light emitting material packaging plastic, is characterized in that preparing by the following method:
(1), after the polysiloxane of ethenyl blocking is fully mixed in reactor with MQ resin, add containing hydrogen silicone oil to mix;
The structural formula of the polysiloxane of described ethenyl blocking is: V ir 3r 4siO (R 1r 2siO) nsiR 3r 4v i, wherein R 1, R 2, R 3, R 4independently selected from methyl or phenyl, V ifor dimethyl vinyl-functional, the integer that n is 200～400;
The structural formula of described MQ resin is: (R 5r 6r 7siO 0.5) m(R 8r 9r 10siO 0.5) n '(SiO 2) y, wherein R 5, R 6, R 7, R 8, R 9independently selected from methyl, ethyl, propyl group, phenyl or sec.-propyl, R 10be selected from propenyl or vinyl, the integer that m is 20～110, n ' is 20～80 integers, the integer that y is 120～300;
The structural formula of described containing hydrogen silicone oil is: R 11r 12r 13siO (R 14hSiO) m 'siR 15r 16r 17, wherein R 11, R 12, R 13, R 14, R 15, R 16, R 17independently selected from methyl, ethyl, propyl group, phenyl, sec.-propyl or aryl, the integer that m ' is 5～240;
The weight ratio of polysiloxane and MQ resin is 0.2～3.1:1, and the mass ratio of polysiloxane and containing hydrogen silicone oil is 0.1～2.7:1;
(2) in reactor, add carbon back white light emitting material;
(3) in reactor, add platinum catalyst, catalyst-initiator and tackifier, fully mix;
(4) reactor being evacuated to reactor pressure is-0.1～-0.09MPa, the polyfluortetraethylene pipe of reaction mixture being put into an end closure solidifies 1～3 hour, solidification value is 60～95 DEG C, obtains carbon back white light emitting material packaging plastic after then keeping 1.2～2.8 hours at 140～160 DEG C of temperature.
2. according to carbon back white light emitting material packaging plastic claimed in claim 1, the viscosity that it is characterized in that the polysiloxane of described ethenyl blocking is 6000～140000mPas.
3. according to carbon back white light emitting material packaging plastic claimed in claim 1, mole proportioning that it is characterized in that the M/Q of described MQ resin is 0.6～0.9:1.
4. according to carbon back white light emitting material packaging plastic claimed in claim 1, it is characterized in that described Silicon Containing Hydrogen oil viscosity is 25～3500mPas.
5. according to carbon back white light emitting material packaging plastic claimed in claim 1, it is characterized in that described platinum catalyst is platinum catalyst/or the platinum catalyst of tetramethyl divinyl siloxanes coordination of tetrahydrofuran (THF) coordination, the consumption of platinum catalyst accounts for 0.01 ‰～0.8 ‰ of packaging plastic total mass.
6. according to carbon back white light emitting material packaging plastic claimed in claim 1, it is characterized in that described catalyst-initiator be selected from 3-methyl isophthalic acid-butine-3-alcohol, 1-acetylene basic ring ethanol and-one, two or three in phenyl-ethyl acetylene-3-alcohol, the consumption of catalyst-initiator accounts for 0.2%～1.3% of packaging plastic total mass.
7. according to carbon back white light emitting material packaging plastic claimed in claim 1, it is characterized in that described tackifier are γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and/or γ-methacryloxypropyl trimethoxy silane, the consumption of tackify knot accounts for 0.2%～3% of packaging plastic total mass.
8. according to carbon back white light emitting material packaging plastic claimed in claim 1, it is characterized in that the integer that in described MQ resin, m is 50～90, n ' is 20～60 integers, the integer that y is 140～220.
9. according to carbon back white light emitting material packaging plastic claimed in claim 1, it is characterized in that the integer that in described containing hydrogen silicone oil, m ' is 20～110.
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CN104882529A (en) * 2015-05-14 2015-09-02 天津德高化成新材料股份有限公司 Quick packaging method for COB-type LED chip
CN104900783A (en) * 2015-05-14 2015-09-09 天津德高化成新材料股份有限公司 Preparation method for inverted LED white-light chip of chip scale package
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Denomination of invention: A carbon based white light emitting material packaging adhesive

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