CN106381121A - Transparent organic pouring sealant - Google Patents
Transparent organic pouring sealant Download PDFInfo
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- CN106381121A CN106381121A CN201610785323.5A CN201610785323A CN106381121A CN 106381121 A CN106381121 A CN 106381121A CN 201610785323 A CN201610785323 A CN 201610785323A CN 106381121 A CN106381121 A CN 106381121A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
Abstract
The invention provides a transparent organic pouring sealant formed by curing and crosslinking curable two-component organosilicone composition; the curable organosilicone composition contains an A component and a B component, the A component includes first vinyl-terminated silicone oil, hydrogen-containing silicone oil, an inhibitor and a reinforcing filler, the B component includes second vinyl-terminated silicone oil, a reinforcing filler, a catalyst and a thermal conducting filler; the viscosity of the first vinyl-terminated silicone oil is 10-2000 mPa*s, the viscosity of the second vinyl-terminated silicone oil is 3000-4000 mPa*s, and the mass ratio of the first vinyl-terminated silicone oil to the second vinyl-terminated silicone oil is (2-30) to 100. The transparent organic pouring sealant with good thermal conducting performance is prepared, can greatly improve the thermal performance of the pouring sealant, emits heat timely, prolongs the life, improves the reliability, and ensures light source output.
Description
Technical field
The present invention relates to encapsulating material, more specifically can be used for organic casting glue of electronic device.
Background technology
Since 21 century, people increasingly increase to the worry of global energy shortage, and with low energy consumption, efficient green
Light emitting diode (Light-Emitting Diode) LED that color light source occurs for synonym enjoys the concern of people.LED is one
Kind can directly convert electric energy to the light emitting semiconductor device of luminous energy, possess that structure is simple, energy-conservation, life-span length, environmental protection, luminous effect
Rate is high, the advantage such as abundant bright in luster, is expected to become forth generation lighting source.As a kind of new lighting engineering, LED is in recent years
Just to develop towards directions such as high chromaticity, high-luminous-efficiency, high uniformity of luminance, high reliability, shine in Landscape Lighting, automobile
The field such as bright, traffic lighting and special lighting has a very wide range of applications.
The performance of LED casting glue has important impact to the brightness of LED component, luminous efficiency and service life.LED fills
The effect of sealing mainly has following four aspect：1) to LED chip sealing and protection, it is to avoid moisture and temperature etc. affect, improve
Reliability is it is ensured that chip normal work；(2) improve heat-sinking capability, the heat that timely and effectively exclusion chip produces；(3) optics
Control, reduce the refractive index difference of LED chip and air, optimize the distribution of light beam, to realize specific optical profile, maximization
Ground output luminous flux, plays lens light gathering effect；(4) mechanically fix and support wire.With in succession pushing away both at home and abroad
Gone out the development policy of semiconductor lighting industry and plan, LED technology constantly progressive and perfect so that GaN base power-type is white
Light LED is fast-developing, proposes more harsh requirement to the performance of LED casting glue.And traditional epoxy resin embedding adhesive exposes
Go out many shortcomings it is impossible to meet the growth requirement of power-type LED.Therefore, develop and there is high transmission rate, high index of refraction, high heat conduction
Rate, high adhesiveness, high intensity, light aging resisting, heat-proof aging, heat shock resistance, low thermal coefficient of expansion, low stress, low ion concentration
With the organic silicon potting adhesive of agent of low hygroscopicity, it is the development trend of LED encapsulation, meets the demand for development of power-type LED.
With the continuous improvement of light-emitting diode luminance and power, organic silicon potting adhesive rely on its high transmission rate, heat resistance,
The premium properties such as weatherability, low mechanical stress and hydrophobicity it is considered to be for large power white light LED encapsulation ideal material,
Increasing LED encapsulation enterprise uses organosilicon material to replace epoxy resin.Organic silicon potting adhesive is divided into low folding by refractive index
(((1.50-1.55) type is divided into Silica hydrogel, silicon rubber and silicon tree by elastic modelling quantity to (1.40-1.45) type with high index of refraction to penetrate rate
Fat.The raw material of organic silicon potting adhesive mainly adopts three kinds of method synthesis：Sol-gel process, hydrolysis-condensation method and ring-opening polymerisation
Method.
Based on the fast development of GaN base power type white light LED, more harsh requirement is proposed to the performance of LED casting glue.
The main chain of organosilicon material is made up of the silicon oxygen bond that bond angle is big and bond energy is high, determine its have excellent pliability, heat-resisting always
Change and anti-ultraviolet ageing performance, the advantages of by its good in optical property, agent of low hygroscopicity, broad use temperature, convenient disassembly, just
In gradually substituted epoxy resin, become the LED encapsulation material of a new generation.
The one of important function of LED casting glue is light-emitting diode to be packaged protect, mechanically solid
Mechanical property that is fixed and supporting wire.This service life directly determining LED and reliability, therefore LED casting glue need tool
There is certain mechanical performance, and a universal non-binding of organosilicon material, if cementability can be improved, the silica gel after solidification and base material
Between will there is no space, can prevent the steam that occurs for a long time from permeating the fault leading to.If the heat that device produces is no
Method is discharged in time and will be directly affected its operating efficiency, produces device open circuit and serious light decay problem, shortens the life-span, reducing it can
By property it is impossible to meet the growth requirement of power-type LED.So the heat conductive transparent organic silicon potting adhesive that exploitation possesses cementability has
Important meaning.
The method that heat conductive insulating organic silicon potting adhesive is frequently used filling heat filling at present, is filled out using conventional thermal conductive filler
Fill polymer and will largely effect on the transparency of encapsulating material, and the little grade uniqueness effect big with specific surface area of the particle diameter of inorganic nano-filler
The problems such as should apply to LED encapsulation material, but need to resolve the easy reunion of inorganic nano-filler, therefore, there is still a need for exploitation is same
When possess the liquid silicone casting glue of excellent thermal conductivity and light transmittance.
Content of the invention
In order to solve the above problems, the present invention is directed to the growth requirement of current power-type LED, by vinyl silicone oil and
The architectural characteristic of containing hydrogen silicone oil and reinforced filling Miscibility etc. are studied, and are prepared for possessing high intensity and high transmission rate
Organic silicon potting adhesive, have studied VMQ silicones, nano silicon, the impact to casting glue performance such as coupling agent modified.?
On the basis of this, using addition reaction by 1- allyloxy -2,3- expoxy propane, 1,3,5,7- tetramethyl-ring tetrasiloxanes, ethene
Base trimethoxy silane and VTES have synthesized different types of tackifier, thus being prepared for possessing good power
Learn the organic silicon potting adhesive of performance, optical property and adhesive property, finally add heat filling nano aluminium oxide and nano oxidized
Zinc, is prepared for the organic silicon potting adhesive possessing high intensity, high heat conductance and high transmission rate further.
As follows in place of the characteristic of the present invention and main innovation：
(1) different vinyl-terminated silicone fluids are used cooperatively with different quality ratio, select VMQ silicones and nano silicon to make
For reinforced filling, it is prepared for the transparent organic silicon casting glue possessing excellent mechanical performances, light-emitting diode is packaged
Protection.
(2) shortcoming being directed to organic silicon potting adhesive adhesive property, adds in transparent organic silicon casting glue and has epoxy radicals
Group and the containing hydrogen silicone oil of siloxane group, are prepared for the transparent organic silicon casting glue possessing good bonding performance, improve organosilicon
The adhesive strength to aluminium and PPA for the casting glue, will not have space between the silica gel after solidification and base material, can prevent from occurring for a long time
The fault that steam infiltration leads to.
(3) on the basis of transparent organic silicon casting glue, add heat filling nano aluminium oxide through surface silanization and
Nano zine oxide, is prepared for the transparent organic silicon casting glue with Thermal conductivity, can greatly improve the hot of casting glue
Can, in time heat is shed, extend the life-span, improve reliability it is ensured that light source output.
Therefore, in an aspect, the invention provides one kind is transparent with mechanical irrigation sealing, it is by will be curable
Two-component silicone composition passes through what solidification was cross-linked to form, and described curable silicon composition comprises component A and B group
Part, described component A comprises the first vinyl-terminated silicone fluid, containing hydrogen silicone oil, inhibitor and reinforced filling, and described B component comprises second
Vinyl-terminated silicone fluid, reinforced filling, catalyst and and heat filling, wherein, the viscosity of described first vinyl-terminated silicone fluid is 10-
The viscosity of 2000mpa S and the second vinyl-terminated silicone fluid is 3000-4000mpa S, and wherein said first end-vinyl
Silicone oil is 2-30: 100 with the mass ratio of described second vinyl-terminated silicone fluid.
Preferably, described in, B component also comprises tackifier, and this tackifier is selected from 1- allyloxy -2,3- expoxy propane
With 1, the tackifier that 3,5,7- tetramethyl-ring tetrasiloxanes reactions are obtained, allyl glycidol is cruel, 1,3,5,7- tetramethyl-rings
Tetrasiloxane and KH-151 three react the tackifier being obtained, and/or 1- allyloxy -2,3- expoxy propane, 1,3,5,7- tetra-
Methyl cyclotetrasiloxane and A-171 three react the tackifier being obtained.
For the deficiency of liquid silastic cementability, generally use silane coupling agent or tackifier.Silane resin acceptor kh-550,
KH-56040 etc. can improve cementability, but for above-mentioned tackifier, situation about being heating and curing improves tackifier
Activity, tackifier contain vinyl, curing reaction can be participated in so that organic silicon potting adhesive aluminium flake and PC material etc. are all had excellent
Good cementability, thus prepares and has excellent cementability and durothermic cold curing fluid sealant.
Preferably, inhibitor is ethynylcyclohexanol.Inhibitor matches with catalyst to adjust operable time and to consolidate
The change time, especially single-component package needed excellent bin stability, certainly so as to meet certain construction operation time
Require there is good intermiscibility with silicone oil.It is divided into two classes for the inhibitor in add-on type liquid silicon rubber by inhibiting mechanism：The
One class is suppression hydrosilylation under normal temperature, after the material such as alkynol compound, phthalein amines volatilization after heating, silicon rubber
Normal reaction；Equations of The Second Kind is non-volatile under normal temperature, and the inhibitor such as maleic acid ester type compound can degradation failure.
Preferably, catalyst is platinum-type catalyst.Platinum catalyst has following three types：Platinum-vinyl siloxane coordinates
Thing, alcohol modification chloroplatinic acid catalyst and platinum-alkynes basigamy compound, apply should have in add-on type liquid silicon rubber good
Compatibility, catalysis activity and storage stability.
Preferably, with respect to the total amount of curable silicon composition, the consumption of described platinum-type catalyst is 10-
100ppm, the consumption of described inhibitor is 0.007-0.13phr.When inhibitor consumption is more than 0.007phr, casting glue has
Preferably operating characteristics.If inhibitor consumption is very little, the activity of platinum catalyst is too high, and the curing rate of casting glue is too fast, solidification
Easily defect in afterwards apparent.Inhibitor consumption is excessive, extends hardening time, affects production efficiency, improves production cost.Cause
This, suppression agent consumption is most widely suited in the range of this in 0.06-0.13phr.
When platinum catalyst consumption is less than 24ppm, casting glue has good operating characteristics.And it is big to work as platinum catalyst consumption
When 48ppm, platinum catalyst consumption is excessive, and hydrosilylation speed is too fast, the easy autohemagglutination of containing hydrogen silicone oil, introduces bubble, solidification
Afterwards apparent becomes a small amount of point-like from smooth zero defect.Therefore platinum catalyst consumption is the most suitable in the range of this in 12-24ppm
Preferably.
Preferably, described reinforced filling is selected from VMQ silicones, silica dioxide granule or its any combination, more preferably VMQ silicon
Resin
The one of important function of LED casting glue is light-emitting diode to be packaged protect, mechanically solid
Determine and support wire, this service life directly determining LED and reliability.Therefore LED casting glue needs there is certain power
Word performance, the mechanical property without the silicon rubber of reinforcement is poor, and conventional reinforced filling white carbon can affect casting glue
Viscosity and transparency.VMQ silicones is a kind of reinforced filling between organic and inorganic for structure, has contents of ethylene
Feature many, that outer layer is covered by organic group, molecular weight is little, and have good dispersiveness and compatibility with organic silicon potting adhesive,
Preferable mobility and light transmittance can be kept.Vinyl can also occur hydrosilylation with containing hydrogen silicone oil, thus and embedding
Glue produces chemical crosslinking, improves the mechanical property of casting glue.
Preferably, with respect to the total amount of described curable silicon composition, the consumption of described VMQ silicones is 1-
40phr.
Nano silicon is a kind of tasteless, free of contamination unformed white powder, because the size of nano-particle is little and
Specific surface area is big, when loading is little (generally less than 5%), has the excellent smooth electroacoustic magnetic that micro particles do not have
Etc. performance.There is the light base of different bond styles in nano-silica surface, molecular state is in three-dimensional chain structure.But nanometer
Particle specific surface area is big, surface energy is very high and surface has light base in a large number, easily forms reunion to reduce surface energy, directly affects
The performance of its performance, reduces the light transmittance of organic silicon potting adhesive, therefore carries out surface-hydrophobicized modification to it, so that nano-particle is existed
Effectively disperse in casting glue, and its surface silanization is conducive to increase the compatibility with organosilicon material.Therefore, nanometer two
The surface silanization of silica processes the precondition being to play nano-particle effect, its preparation to transparent organic silicon casting glue
Play key effect.With silicone compounds, surface-hydrophobicized process can be carried out to silica dioxide granule.Silicone compounds can
With selected from γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane (KH-
570), HMDS or its any combination.
With the increase of modified manometer silicon dioxide content, the hardness of casting glue also increases therewith, because it is a kind of benefit
Strong filler.Meanwhile, the viscosity ascensional range of casting glue less, still has good mobility and wellability, reaches embedding
Process conditions.Nano silicon, after surface silanization process, is changed into hydrophobicity from hydrophily, significantly improves and basis
The compatibility of polymer, will not increase substantially the viscosity of casting glue, wherein obvious with KH-570 modification.This is due to idol
The introducing of connection agent KH-570, so that trimethoxy silane is reacted with the light base of nanoparticle surface, increases and organosilicon material
The compatibility of material, the agglomeration of nano-particle makes moderate progress, and reduces the viscosity of casting glue.
If as described above, the heat that device produces cannot be discharged in time and will be directly affected its operating efficiency, producing device
Open circuit and serious light decay problem, shorten the life-span, reduce its reliability it is impossible to meet the growth requirement of power-type LED.Lead at present
The method that heat insulation organic silicon potting adhesive is frequently used filling heat filling, will significantly using conventional thermal conductive filler filled polymer
The transparency of impact encapsulating material, and the particle diameter of inorganic nano-filler is little and specific surface area is big etc., and unique effect is applied to LED envelope
Package material, but the problems such as the easy reunion of inorganic nano-filler need to be resolved.Metal oxide, nitride and carbide have higher
Thermal conductivity factor, good insulating properties, price is low, the advantages of easily preparation, therefore becomes and prepares heat conductive insulating composite and commonly use
Filler.The present invention adds heat filling nano aluminium oxide through surface silanization and nano zine oxide, is prepared for having good
The transparent organic silicon casting glue of heat conductivility, can greatly improve the heat conductivility of casting glue, in time heat shed, and extend the longevity
Life, improves reliability it is ensured that light source output.
Accordingly, it is preferred that heat filling is nano zine oxide or the nano aluminium oxide through siloxane treated.
Preferably, the reactive hydrogen mass fraction of described containing hydrogen silicone oil is 0.1-0.8%.
Preferably, the reactive hydrogen of described containing hydrogen silicone oil and the mol ratio of the vinyl of described vinyl-terminated silicone fluid are 1-3.
The beneficial effects of the present invention is：It is prepared for the transparent organic silicon casting glue possessing excellent mechanical performances, to luminous
Diode element is packaged protecting；It is prepared for the transparent organic silicon casting glue possessing good bonding performance, improve organosilicon and fill
The adhesive strength to aluminium and PPA for the sealing, will not have space between the silica gel after solidification and base material, can prevent the water occurring for a long time
The fault that vapour infiltration leads to；It is prepared for the transparent organic silicon casting glue with Thermal conductivity, filling can be greatly improved
Heat is shed by the hot property of sealing in time, extends the life-span, improves reliability it is ensured that light source output.
Specific embodiment
Enforcement embodiment of the present invention explained below.However, the scope of the present invention is not limited to described embodiment party
Formula, as long as not damaging purport, can carry out various changes to the present invention.
The surface silanization of heat conduction nano particle is processed
Weigh nano aluminium oxide and zinc oxide in vacuum drying chamber, be heated to 130 DEG C, and constant temperature 6h.
(1) VTES (KH-151) modified nano-alumina：Weigh 3%KH-151, drip distilled water
And oxalic acid solution, adjust pH value to 3=4；Weigh a small amount of nano aluminium oxide, be dissolved in a certain amount of ethanol, in ultrasonic disperse instrument
Middle dispersion 30min, obtains unit for uniform suspension, then in system add KH-151, continue ultrasonic disperse 5min, transfer to equipped with return
In the 500mL there-necked flask of stream condenser pipe, it is warming up to 60 DEG C and isothermal reaction 3h, cooling, mixed liquor centrifugal precipitation mechanism is divided
From, washing, drying, obtain KH-151 modified nano-alumina powder.
(2) KH-570 modified nano zinc oxide：Weigh 6%KH-570, dropping distilled water and oxalic acid solution, adjust pH value to
3.5=4 between；Weigh a small amount of nano zine oxide, be dissolved in a certain amount of ethanol, in ultrasonic disperse instrument, disperse 30min, obtain uniformly
Suspension, then add 6%KH-570 in system, continue ultrasonic disperse 5min, transfer to the 500mL equipped with the condensable pipe that flows back
In there-necked flask, it is warming up to 85 DEG C and isothermal reaction 2h, cooling, by mixed liquor centrifugation KH-570 modified nano zinc oxide
Powder.The preparation of the property sent out phenol formaldehyde foam
The preparation of organic silicon potting adhesive and the preparation of sample
Weigh a small amount of nano-particle, be dissolved in a certain amount of acetone, disperse 15min in ultrasonic disperse instrument, obtain even suspension
Liquid, then add vinyl-terminated silicone fluid in system, continue ultrasonic disperse 1min, make modified Nano particle in vinyl-terminated silicone fluid
Disperse and mix, at 65 DEG C, then vacuumize removing solvent, after cooling ,-acetylene basic ring neat with containing hydrogen silicone oil, suppression
Hexanol mixes by a certain percentage, is sufficiently stirred for 25min component A is obtained in the presence of vacuum power mixer；By end-vinyl
Silicone oil, tackifier and platinum catalyst mix by a certain percentage, be sufficiently stirred for 25min and be obtained in the presence of vacuum power mixer
B component.
Described component A is mixed by weight for 1: 1 with component B in the presence of high speed shear dispersion, is placed in true
Vacuum (vacuum -0.1MPa) deaeration 10min in empty drying box, pours into a size of in the mould of 150mm x 120mm x 2mm
Cold curing or be heating and curing, solidification obtains organic silicon potting adhesive, makes test piece, carries out properties test.
Result：
It is modified that 1.FT-IR spectrogram shows that KH-151 and KH-570 successfully carries out surface silanization to nano-particle.With changing
Property nanoparticle content increase, viscosity B coefficent less, suitable embedding, the thermal conductivity of casting glue and refractive index are gradually increasing, thoroughly
Light rate, thermal coefficient of expansion and specific insulation are all gradually lowered, and heat resistance significantly improves.
2. with respect to KH-151, when KH-570 modified nano-alumina loading is 1phr, between filler and casting glue
Interface binding power is higher, has higher thermal conductivity 0.352W/ (m-K), improves 153% than pure organic silicon potting adhesive；With filling
The compatibility of sealing is slightly poor, has relatively low light transmittance 68%；580 DEG C of higher thermal weight loss temperature (weightless 50%),
3., under same filling fraction 0.5phr, compare the size of thermal conductivity, KH-570 modified nano-alumina
(0.256W/ (m K)) ＞ KH-570 modified nano zinc oxide (0.238W/ (m K))；KH-570 modified nano-alumina is filled
Afterwards, casting glue has higher light transmittance 80%；And KH-570 modified nano zinc oxide makes casting glue have relatively low thermal expansion
Coefficient and higher refractive index, simultaneously heat resistance greatly improve, thermal weight loss temperature is 653 DEG C (weightless 50%).
4. comprehensive thermal conductivity and two performance requirements of light transmittance, when KH-151 modified nano-alumina loading is
During 0.75phr, LED organic silicon potting adhesive has optimal combination property：Thermal conductivity is 0.296W/ (m K), and light transmittance is 79%
, and the performance such as excellent electrical insulating property, heat resistance, low thermal coefficient of expansion and high index of refraction (450nm).
Claims (11)
1. transparent with mechanical irrigation sealing, it is by curable Two-component silicone composition is passed through the crosslinked shape of solidification to one kind
Become, described curable silicon composition comprises component A and B component, described component A comprise the first vinyl-terminated silicone fluid,
Containing hydrogen silicone oil, inhibitor and reinforced filling, described B component comprises the second vinyl-terminated silicone fluid, reinforced filling, catalyst and and leads
Hot filler, wherein, the viscosity of described first vinyl-terminated silicone fluid is the viscosity of 10-2000mPa S and the second vinyl-terminated silicone fluid
For 3000-4000mPa S, and the mass ratio of wherein said first vinyl-terminated silicone fluid and described second vinyl-terminated silicone fluid
Example is 2-30: 100.
2. according to claim 1 transparent with mechanical irrigation sealing, wherein said B component also comprises tackifier, this tackifier
It is selected from 1- allyloxy -2,3- expoxy propane and 1, the tackifier that 3,5,7- tetramethyl-ring tetrasiloxanes reactions are obtained, allyl
Base glycidol is cruel, 1,3,5,7- tetramethyl-ring tetrasiloxanes react, with KH-151 three, the tackifier being obtained, and/or 1- allyl
Epoxide -2,3- expoxy propane, 1,3,5,7- tetramethyl-ring tetrasiloxanes and A-171 three react the tackifier being obtained.
3. according to claim 1 transparent with mechanical irrigation sealing, wherein said inhibitor is ethynylcyclohexanol.
4. according to claim 1 transparent with mechanical irrigation sealing, wherein said reinforced filling is selected from VMQ silicones, dioxy
Silicon carbide particle or its any combination.
5. according to claim 2 transparent with mechanical irrigation sealing, wherein said silicone compounds are selected from γ-glycidol
Ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, HMDS or it is any
Combination.
6. according to claim 1-5 transparent with mechanical irrigation sealing, wherein said catalyst is platinum-type catalyst.
7. according to claim 1 transparent with mechanical irrigation sealing, wherein said heat filling is receiving through siloxane treated
Rice zinc oxide or nano aluminium oxide.
8. according to claim 1 transparent with mechanical irrigation sealing, the reactive hydrogen mass fraction of wherein said containing hydrogen silicone oil is
0.1-0.8%.
9. according to claim 1 transparent with mechanical irrigation sealing, the reactive hydrogen of wherein said containing hydrogen silicone oil and described end second
The mol ratio of the vinyl of thiazolinyl silicone oil is 1-3.
10. according to claim 6 transparent with mechanical irrigation sealing, wherein with respect to described curable silicon composition
Total amount, the consumption of described platinum-type catalyst is 10-100ppm, and the consumption of described inhibitor is 0.007-0.13phr.
11. according to claim 4 transparent with mechanical irrigation sealing, wherein with respect to described curable silicon composition
Total amount, the consumption of described VMQ silicones is 1-40phr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610785323.5A CN106381121A (en) | 2016-08-31 | 2016-08-31 | Transparent organic pouring sealant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610785323.5A CN106381121A (en) | 2016-08-31 | 2016-08-31 | Transparent organic pouring sealant |
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| CN106381121A true CN106381121A (en) | 2017-02-08 |
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| CN201610785323.5A Pending CN106381121A (en) | 2016-08-31 | 2016-08-31 | Transparent organic pouring sealant |
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| CN107189071A (en) * | 2017-06-23 | 2017-09-22 | 广东信翼科技有限公司 | A kind of preparation method of liquid silastic platinum catalyst |
| CN107345070A (en) * | 2017-07-05 | 2017-11-14 | 安徽中威光电材料有限公司 | Organic silicon composite of a kind of light aging resisting containing nano zine oxide and preparation method thereof |
| CN109054715A (en) * | 2018-07-12 | 2018-12-21 | 广东恒大新材料科技有限公司 | LED backlight modified silane sealant and preparation method thereof |
| CN110144190A (en) * | 2019-05-29 | 2019-08-20 | 罗青菊 | A kind of add-on type high heat conduction organosilicon electronic seal glue preparation method |
| CN110527486A (en) * | 2019-09-11 | 2019-12-03 | 丁爱顺 | Resistance to ultraviolet organosilicon adhesive of one kind and preparation method thereof |
| CN114395368A (en) * | 2022-01-14 | 2022-04-26 | 东风汽车集团股份有限公司 | Double-component modified thermosetting silica gel and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189071A (en) * | 2017-06-23 | 2017-09-22 | 广东信翼科技有限公司 | A kind of preparation method of liquid silastic platinum catalyst |
| CN107345070A (en) * | 2017-07-05 | 2017-11-14 | 安徽中威光电材料有限公司 | Organic silicon composite of a kind of light aging resisting containing nano zine oxide and preparation method thereof |
| CN109054715A (en) * | 2018-07-12 | 2018-12-21 | 广东恒大新材料科技有限公司 | LED backlight modified silane sealant and preparation method thereof |
| CN109054715B (en) * | 2018-07-12 | 2021-07-13 | 广东恒大新材料科技有限公司 | Modified silane sealant for LED backlight source and preparation method thereof |
| CN110144190A (en) * | 2019-05-29 | 2019-08-20 | 罗青菊 | A kind of add-on type high heat conduction organosilicon electronic seal glue preparation method |
| CN110527486A (en) * | 2019-09-11 | 2019-12-03 | 丁爱顺 | Resistance to ultraviolet organosilicon adhesive of one kind and preparation method thereof |
| CN114395368A (en) * | 2022-01-14 | 2022-04-26 | 东风汽车集团股份有限公司 | Double-component modified thermosetting silica gel and preparation method thereof |
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Application publication date: 20170208 |