CN105778850B - A kind of ultraviolet leds packaging plastic and preparation method thereof - Google Patents
A kind of ultraviolet leds packaging plastic and preparation method thereof Download PDFInfo
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- CN105778850B CN105778850B CN201610171065.1A CN201610171065A CN105778850B CN 105778850 B CN105778850 B CN 105778850B CN 201610171065 A CN201610171065 A CN 201610171065A CN 105778850 B CN105778850 B CN 105778850B
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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
- C09J183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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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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- 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
- C09J11/08—Macromolecular additives
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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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- 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
- 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
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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
Abstract
A kind of ultraviolet leds packaging plastic, it is characterised in that be made of the raw material that following weight matches: poly- fluorosilicone 50-80 parts of methyl ethylene, 25-40 parts of crosslinking agent, 0.1-0.5 parts of catalyst, 0.01-0.1 parts of inhibitor, 0-5 parts of auxiliary material.The present invention also provides a kind of preparation methods of above-mentioned ultraviolet leds packaging plastic.Ultraviolet leds packaging plastic of the invention has the excellent performances such as high uv transmittance, radiation hardness, high-low temperature resistant, weather-proof; its refractive index is 1.40-1.42; viscosity is at 1000-7000mPa.s(25 DEG C) between; hardness is from seal protection adjustable between 30-70A, suitable for 100-400 nanometers of ultraviolet leds after solidification.The preparation method raw material of ultraviolet leds packaging plastic of the present invention is easy to get, easy to operate, easily controllable, pollution-free, mild condition, is convenient for industrialization.
Description
Technical field
The present invention relates to LED sealing materials, and in particular to a kind of ultraviolet leds packaging plastic and preparation method thereof.
Background technique
Since nineteen nineties, GaN base blue green light LED be made breakthrough progress, at present the red indigo plant of high brightness
Green light LED has been commercialized, and all shows powerful potentiality, white light in fields such as Landscape Lighting, large screen backlight, optical communications
LED solid-state lighting is even more like a raging fire, positive to cause third time illumination revolution.With reaching its maturity for visible regime, people is studied
Member gradually shifts research emphasis to the ultraviolet light of short wavelength.Compared with traditional mercury lamp, ultraviolet leds light source have it is small in size,
At low cost, long-life and the advantages such as environmentally protective, just because of these advantages, ultraviolet leds technology is becoming ultraviolet source row
The very attractive selection scheme of industry.
The Wavelength distribution of ultraviolet light can further be subdivided into three classes: UV-A(315- between 100 nanometers to 400 nanometers
400 nanometers, also referred to as long wave ultraviolet light), UV-B(280-315 nanometers, also referred to as medium wave ultraviolet light), UV-C(100-280 receives
Rice, also referred to as short wave ultraviolet light or deep ultraviolet light).The sealing material of red blue green light LED mainly has methyl silicone rubber, phenyl silicon
Resin and epoxy resin three classes, in the market not with the presence of the sealing material specifically for ultraviolet leds.Since epoxy resin is anti-
Ultraviolet ability is poor, and phenyl polysiloxane has absorption in ultraviolet light wave band, so current ultraviolet leds sealing material is mainly adopted
With methyl silicone rubber, but the unbearable ultraviolet light of methyl silicone rubber irradiates for a long time, affects the service life of ultraviolet leds,
UV-B and UV-C wave band is particularly evident, so exploitation becomes the field technology and city dedicated for the sealing material of ultraviolet leds
The problem of urgent need to resolve, is developed in field.
Summary of the invention
The technical problem to be solved by the present invention is to develop a kind of ultraviolet leds encapsulation suitable for ultraviolet leds encapsulation
Glue, the excellent performances such as this ultraviolet leds packaging plastic uv transmittance with higher, radiation hardness, high-low temperature resistant, weather-proof,
Preparation method is easy to operate, easily controllable.The technical solution adopted is as follows:
A kind of ultraviolet leds packaging plastic, it is characterised in that be made of the raw material that following weight matches: methyl ethylene is poly-
50-80 parts of fluorosilicone, 25-40 parts of crosslinking agent, 0.1-0.5 parts of catalyst, 0.01-0.1 parts of inhibitor, auxiliary material 0-5
Part.
It is preferred that the above-mentioned poly- fluorosilicone of methyl ethylene be viscosity be 1000-60000mPa.s(25 DEG C), vinyl quality
The poly- fluorosilicone of linear methyl vinyl or viscosity that score is 1-6%, fluorine-based mass fraction is 5-19% are 1000-
60000mPa.s(25 DEG C), the methyl ethylene T-type fluorine that vinyl mass fraction is 1-6%, fluorine-based mass fraction is 5-19%
Silicone resin or the poly- fluorosilicone of the linear methyl vinyl, methyl ethylene T-type fluorine silicon resin and vinyl quality point
A variety of combinations in methyl vinyl MQ type fluorine silicon resin that number is 1-6%, fluorine-based mass fraction is 5-19%.On it is preferred that
State M/Q=0.8-1.5 of methyl vinyl MQ type fluorine silicon resin.
In preferred embodiment, above-mentioned crosslinking agent is that viscosity is 50-2000mPa.s(25 DEG C), hydrogen-based mass fraction be 0.1-
0.5%, the poly- fluorosilicone of linear methyl hydrogen-based or viscosity that fluorine-based mass fraction is 1-10% are 50-2000mPa.s
The methyl hydrogen-based T-type fluorine silicon resin that (25 DEG C), hydrogen-based mass fraction are 0.1-0.5%, fluorine-based mass fraction is 1-10%, or
Be the poly- fluorosilicone of the linear methyl hydrogen-based, methyl hydrogen-based T-type fluorine silicon resin and hydrogen-based mass fraction be 0.1-0.5%, fluorine
Base mass fraction is a variety of combinations in the methyl hydrogen-based MQ type fluorine silicon resin of 1-10%.It is preferred that above-mentioned methyl hydrogen-based MQ type fluorine
M/Q=0.8-1.5 of silicone resin.
Above-mentioned catalyst for promoting going on smoothly for silicon hydrogenation, preferably noble metal (including rhodium, ruthenium, iridium, platinum or
The noble metals such as palladium) with the complex compound of silicone oligomer, more preferable above-mentioned catalyst is the platinum network of methylvinyl-polysiloxane
Close the platinum complex of the more ethylene low polymer coordinations of object, methyl, platinum complex, the organosilicon microballoon of diethyl phthalate coordination
The platinum catalyst of platinum catalyst or the organic siliconresin cladding of cladding.
The main function of above-mentioned inhibitor is the speed of regulation and control silicon hydrogenation, to extend the storage of packaging plastic
The time is deposited and used, and packaging plastic is enable to obtain preferable stress release in solidification process, improves its reliability.It is preferred that above-mentioned suppression
Preparation is 1-Ethynylcyclohexanol, 2,2- 2-butyne methanol, 3,5- dimethyl -3- hydroxyl -1- hexin, 3- Methyl-1-pentene -
3- alcohol or poly- methyl ethylene cyclic compound.
Above-mentioned auxiliary material can be the combination of fluorine-containing acrylate and one or both of nano silica.Fluorine-containing
Acrylate primarily serves the effect of the caking property of enhancing LED packaging plastic.Nano silica primarily serves enhancing LED encapsulation
The intensity of glue, improves the effects of unfailing performance of LED packaging plastic at the brightness for helping stress release, increasing LED packaging plastic.
More preferable above-mentioned fluorine-containing acrylate is 2- trifluoromethyl -2- acrylic acid 2,2,2- trifluoro ethyl ester, n-butyric acie 2,
One of 2,2- trifluoro ethyl ester and acrylic acid 2,2,2- trifluoro ethyl ester or in which a variety of combinations.
More preferable above-mentioned nano silica is the preparing spherical SiO 2 of crystal type, partial size < 50nm.Nanometer titanium dioxide
Silicon is divided into crystal type and two kinds unformed, and the gas phase or sedimentation thermal oxidation silicon that tradition uses are amorphous silica,
There are certain absorption and the effect of blocking to ultraviolet light, so the nano silica of crystal type is preferentially used, so that ultraviolet luminous energy
It passes through, and the pattern of crystal type nano silica, closer to spherical shape, light extraction efficiency is higher.
The present invention also provides a kind of preparation methods of above-mentioned ultraviolet leds packaging plastic, it is characterised in that under successively including
State step:
(1) by weight, it is equipped with following raw materials: poly- fluorosilicone 50-80 parts of methyl ethylene, 25-40 parts of crosslinking agent,
0.1-0.5 parts of catalyst, 0.01-0.1 parts of inhibitor, 0-5 parts of auxiliary material；
(2) the poly- fluorosilicone of methyl ethylene, crosslinking agent, catalyst, inhibitor and auxiliary material provisioned in step (1) are added
Enter into reaction vessel, is stirred (preferably under conditions of vacuum degree is-0.05-- 0.09Mpa, temperature is 20-28 DEG C
Mixing speed is 30-80 revs/min, and mixing time is 1-4 hours), it is uniformly mixed the material in reaction vessel, obtains purple
Outer smooth LED packaging plastic.
Contain methyl vinyl MQ type fluorine silicon resin, and methyl vinyl MQ type in the poly- fluorosilicone of above-mentioned methyl ethylene
In the case that fluorine silicon resin is solid material, it in reaction vessel is added in the poly- fluorosilicone of methyl ethylene in step (2)
Before, in advance by the poly- fluorosilicone mixed dissolution of methyl ethylene (i.e. with the poly- fluorosilicone of linear methyl vinyl, the methyl being equipped with
Vinyl T-type fluorine silicon resin will dissolve methyl vinyl MQ type fluorine silicon resin).
Contain methyl hydrogen-based MQ type fluorine silicon resin in above-mentioned crosslinking agent, and methyl hydrogen-based MQ type fluorine silicon resin is solid material
In the case where, before crosslinking agent is added in reaction vessel in step (2), in advance by crosslinking agent mixed dissolution (i.e. with outfit
The poly- fluorosilicone of linear methyl hydrogen-based, methyl hydrogen-based T-type fluorine silicon resin by methyl hydrogen-based MQ type fluorine silicon resin dissolve).
In organic chemistry, carbon-fluorine bond (C-F key) is strongest singly-bound and relatively short and small key, just because of the F of C-F key
The shielding protection of atom pair C-C key skeleton acts on, and fluororesin high polymer is made to have a series of special performance, such as weatherability, resistance to
The performances such as long property, chemical resistance, anti-corrosive properties and ultraviolet resistance.The present invention by silicon-fluorine polymer object introduce LED sealing material it
In, by the reasonably combined of the polysiloxanes of different structure and fluorine content, obtain the superior ultraviolet leds that are suitable for of performance and encapsulate
Packaging plastic.
Ultraviolet leds packaging plastic of the invention has high uv transmittance, radiation hardness, high-low temperature resistant, weather-proof etc. excellent
Performance, refractive index 1.40-1.42, viscosity is at 1000-7000mPa.s(25 DEG C) between, hardness is from 30-70A after solidification
Between adjustable, the seal protection suitable for 100-400 nanometers of ultraviolet leds.The system of ultraviolet leds packaging plastic of the present invention
Preparation Method raw material is easy to get, easy to operate, easily controllable, pollution-free, mild condition, is convenient for industrialization.
Specific embodiment
Embodiment 1
In the present embodiment, the preparation method of ultraviolet leds packaging plastic successively includes the following steps:
(1) be equipped with following raw materials: (wherein 30 kilograms are that viscosity is to 70 kilograms of the poly- fluorosilicone of methyl ethylene
1000mPa.s(25 DEG C), the poly- fluorine silicon oxygen of linear methyl vinyl that vinyl mass fraction is 1%, fluorine-based mass fraction is 10%
Alkane, remaining 40 kilograms are that viscosity is 20000mPa.s(25 DEG C), vinyl mass fraction be 4%, fluorine-based mass fraction is 5%
Methyl ethylene T-type fluorine silicon resin), 30 kilograms of crosslinking agent (be viscosity be 500mPa.s(25 DEG C), hydrogen-based mass fraction are
0.2%, the poly- fluorosilicone of linear methyl hydrogen-based that fluorine-based mass fraction is 1%), 0.15 kilogram of catalyst (is the more ethylene of methyl
The platinum complex of oligomer coordination, Pt content are 0.5% (weight)), 0.015 kilogram of inhibitor (is 1- acetylene hexamethylene
Alcohol), 1 kilogram of auxiliary material (being 2,2,2- trifluoro ethyl ester of 2- trifluoromethyl -2- acrylic acid)；
(2) the poly- fluorosilicone of methyl ethylene, crosslinking agent, catalyst, inhibitor and auxiliary material provisioned in step (1) are added
Enter into reaction vessel, be stirred under conditions of vacuum degree is -0.09Mpa, temperature is 25 DEG C (mixing speed be 50 turns/
Minute, mixing time is 3 hours), it is uniformly mixed the material in reaction vessel, obtains ultraviolet leds packaging plastic.
The viscosity of packaging plastic obtained is about 5000mPa.s(25 DEG C), fluorinated volume about 5%, suitable for the ultraviolet of UV-A wave band
Light LED encapsulation.It (is encapsulated for SMD5050 ultraviolet light lamp bead) when use, above-mentioned ultraviolet leds packaging plastic vacuum is arranged and is steeped
Afterwards, it injects in 2mm × 10mm × 2mm mold, precuring 1 hour at 80 DEG C, then solidifies 4 hours at 150 DEG C, be allowed to
As silica gel piece, after tested, which is 95% in the transmitance of UV-A wave band, (in a length of 365nm of incident light wave, silica gel piece
It is measured in the case where with a thickness of 2mm)；After 365nm ultraviolet light 1000h, transmitance decaying < 2%；Packaged is ultraviolet
Light SMD5050 lamp bead is without exception through red ink, Reflow Soldering and 1000 bout of cooling thermal impact.
Embodiment 2
In the present embodiment, the preparation method of ultraviolet leds packaging plastic successively includes the following steps:
(1) be equipped with following raw materials: (wherein 20 kilograms are that viscosity is to 50 kilograms of the poly- fluorosilicone of methyl ethylene
2000mPa.s(25 DEG C), the poly- fluorine silicon of linear methyl vinyl that vinyl mass fraction is 1.5%, fluorine-based mass fraction is 12%
Oxygen alkane, remaining 30 kilograms are that viscosity is 5000mPa.s(25 DEG C), vinyl mass fraction be 2%, fluorine-based mass fraction is 15%
Methyl ethylene T-type fluorine silicon resin), 30 kilograms of crosslinking agent (be viscosity be 200mPa.s(25 DEG C), hydrogen-based mass fraction are
0.16%, the poly- fluorosilicone of linear methyl hydrogen-based that fluorine-based mass fraction is 10%), 0.2 kilogram of catalyst (is ethylene methacrylic
The platinum complex of based polysiloxane, Pt content are 0.3% (weight)), 0.01 kilogram of inhibitor (is 3,5- dimethyl -3-
Hydroxyl -1- hexin), 1 kilogram of auxiliary material (being 2,2,2- trifluoro ethyl ester of n-butyric acie)；
(2) the poly- fluorosilicone of methyl ethylene, crosslinking agent, catalyst, inhibitor and auxiliary material provisioned in step (1) are added
Enter into reaction vessel, be stirred under conditions of vacuum degree is -0.08Mpa, temperature is 25 DEG C (mixing speed be 70 turns/
Minute, mixing time is 2 hours), it is uniformly mixed the material in reaction vessel, obtains ultraviolet leds packaging plastic.
The viscosity of packaging plastic obtained is about 3000mPa.s(25 DEG C), fluorinated volume about 10%, the purple suitable for UV-B wave band
Outer smooth LED encapsulation.It (is encapsulated for SMD5050 ultraviolet light lamp bead) when use, above-mentioned ultraviolet leds packaging plastic vacuum is arranged and is steeped
Afterwards, it injects in 2mm × 10mm × 2mm mold, precuring 1 hour at 80 DEG C, then solidifies 4 hours at 150 DEG C, be allowed to
As silica gel piece.After tested, which is 95%(in a length of 310nm of incident light wave, silica gel piece in the transmitance of UV-B wave band
It is measured in the case where with a thickness of 2mm)；After 310nm ultraviolet light 1000h, transmitance decaying < 2%；Packaged is ultraviolet
Light SMD5050 lamp bead is without exception through red ink, Reflow Soldering and 1000 bout of cooling thermal impact.
Embodiment 3
In the present embodiment, the preparation method of ultraviolet leds packaging plastic successively includes the following steps:
(1) be equipped with following raw materials: (wherein 30 kilograms are that viscosity is to 80 kilograms of the poly- fluorosilicone of methyl ethylene
1000mPa.s(25 DEG C), the poly- fluorine silicon oxygen of linear methyl vinyl that vinyl mass fraction is 1%, fluorine-based mass fraction is 15%
Alkane, remaining 50 kilograms of viscosity is 20000mPa.s(25 DEG C), the first that vinyl mass fraction is 5%, fluorine-based mass fraction is 19%
Base vinyl T-type fluorine silicon resin), 25 kilograms of crosslinking agent (be viscosity be 100mPa.s(25 DEG C), hydrogen-based mass fraction are
0.3%, the poly- fluorosilicone of linear methyl hydrogen-based that fluorine-based mass fraction is 9%), 0.3 kilogram of catalyst (is organosilicon microballoon
The platinum catalyst of cladding, Pt content are 0.3% (weight)), 0.02 kilogram of inhibitor (being 1-Ethynylcyclohexanol), auxiliary material 1
Kilogram (being acrylic acid 2,2,2- trifluoro ethyl ester)；
(2) the poly- fluorosilicone of methyl ethylene, crosslinking agent, catalyst, inhibitor and auxiliary material provisioned in step (1) are added
Enter into reaction vessel, be stirred under conditions of vacuum degree is -0.09Mpa, temperature is 25 DEG C (preferably mixing speed be 40
Rev/min, mixing time is 4 hours), it is uniformly mixed the material in reaction vessel, obtains ultraviolet leds packaging plastic.
The viscosity of packaging plastic obtained is about 5000mPa.s(25 DEG C), fluorinated volume about 19%, the purple suitable for UV-C wave band
Outer smooth LED encapsulation.It (is encapsulated for SMD5050 ultraviolet light lamp bead) when use, above-mentioned ultraviolet leds packaging plastic vacuum is arranged and is steeped
Afterwards, it injects in 2mm × 10mm × 2mm mold, precuring 1 hour at 80 DEG C, then solidifies 4 hours at 150 DEG C, be allowed to
As silica gel piece.After tested, which is 95%(in a length of 254nm of incident light wave, silica gel piece in the transmitance of UV-C wave band
It is measured in the case where with a thickness of 2mm)；After 254nm ultraviolet light 1000h, transmitance decaying < 2%；Packaged is ultraviolet
Light SMD5050 lamp bead is without exception through red ink, Reflow Soldering and 1000 bout of cooling thermal impact.
Embodiment 4
In the present embodiment, the preparation method of ultraviolet leds packaging plastic successively includes the following steps:
(1) be equipped with following raw materials: (wherein 70 kilograms are that viscosity is to 80 kilograms of the poly- fluorosilicone of methyl ethylene
4000mPa.s(25 DEG C), the poly- fluorine silicon oxygen of linear methyl vinyl that vinyl mass fraction is 1%, fluorine-based mass fraction is 13%
Alkane, remaining 10 kilograms are vinyl mass fraction is 5%, fluorine-based mass fraction is 5% methyl vinyl MQ type fluorine silicon resins,
The methyl vinyl MQ type fluorine silicon resin is powdered), 25 kilograms of crosslinking agent (be viscosity be 500mPa.s(25 DEG C), hydrogen-based
The methyl hydrogen-based T-type fluorine silicon resin that mass fraction is 0.3%, fluorine-based mass fraction is 10%), 0.5 kilogram of catalyst (is organic
The platinum catalyst of silicon micro-spheres, Pt content are 0.3% (weight)), 0.03 kilogram of inhibitor (being 1-Ethynylcyclohexanol),
(wherein 1 kilogram is n-butyric acie 2,2,2- trifluoro ethyl ester to 3 kilograms of auxiliary material；Remaining the 2 kilograms preparing spherical SiO 2s for crystal type,
Partial size < 50nm)；
(2) the poly- fluorosilicone of methyl ethylene is pre-processed: linear methyl vinyl provisioned in step (1) is poly-
Fluorosilicone and the mixing of powdered methyl vinyl MQ type fluorine silicon resin, in the item that vacuum degree is -0.09Mpa, temperature is 150 DEG C
It is stirred under part, is completely dissolved powdered methyl vinyl MQ type fluorine silicon resin, is subsequently cooled to 22 DEG C；
(3) will through crosslinking agent provisioned in the poly- fluorosilicone of step (2) pretreated methyl ethylene and step (1),
Catalyst, inhibitor and auxiliary material are added in reaction vessel, are carried out under conditions of vacuum degree is -0.08Mpa, temperature is 25 DEG C
Stirring (mixing speed is 60 revs/min, and mixing time is 3 hours), is uniformly mixed the material in reaction vessel, obtains ultraviolet
Light LED packaging plastic.
The viscosity of packaging plastic obtained is about 5000mPa.s(25 DEG C), fluorinated volume about 11%, the purple suitable for UV-B wave band
Outer smooth LED encapsulation.It (is encapsulated for SMD5050 ultraviolet light lamp bead) when use, above-mentioned ultraviolet leds packaging plastic vacuum is arranged and is steeped
Afterwards, it injects in 2mm × 10mm × 2mm mold, precuring 1 hour at 80 DEG C, then solidifies 4 hours at 150 DEG C, be allowed to
As silica gel piece.After tested, which is 95%(in a length of 310nm of incident light wave, silica gel piece in the transmitance of UV-B wave band
It is measured in the case where with a thickness of 2mm)；After 310nm ultraviolet light 1000h, transmitance decaying < 2%；Packaged is ultraviolet
Light SMD5050 lamp bead is without exception through red ink, Reflow Soldering and 1000 bout of cooling thermal impact.
Embodiment 5
In the present embodiment, the preparation method of ultraviolet leds packaging plastic successively includes the following steps:
(1) be equipped with following raw materials: (wherein 40 kilograms are that viscosity is to 80 kilograms of the poly- fluorosilicone of methyl ethylene
30000mPa.s(25 DEG C), the poly- fluorine silicon oxygen of linear methyl vinyl that vinyl mass fraction is 2%, fluorine-based mass fraction is 5%
Alkane, remaining 40 kilograms are that viscosity is 2000mPa.s(25 DEG C), the line that vinyl mass fraction is 2%, fluorine-based mass fraction is 3%
Property methyl ethylene poly- fluorosilicone), (it is 0.3%, fluorine-based quality point that wherein 5 kilograms are hydrogen-based mass fractions to 30 kilograms of crosslinking agent
The methyl hydrogen-based MQ type fluorine silicon resin that number is 2%, the methyl hydrogen-based MQ type fluorine silicon resin are powdered；Remaining 25 kilograms are viscosity
Be 1000mPa.s(25 DEG C), the poly- fluorine silicon oxygen of linear methyl hydrogen-based that hydrogen-based mass fraction is 0.1%, fluorine-based mass fraction is 5%
Alkane), 0.3 kilogram of catalyst (platinum catalyst of organosilicon micro-spheres, Pt content are 0.3% (weight)), inhibitor 0.05
Kilogram (being 1-Ethynylcyclohexanol), (wherein 1 kilogram is 2,2,2- trifluoro ethyl ester of n-butyric acie to 3 kilograms of auxiliary material；Remaining 2 kilograms are
The preparing spherical SiO 2 of crystal type, partial size < 50nm)；
(2) crosslinking agent is pre-processed: by the poly- fluorosilicone of linear methyl hydrogen-based provisioned in step (1) and powdered
The mixing of methyl hydrogen-based MQ type fluorine silicon resin, is stirred under conditions of vacuum degree is -0.09Mpa, temperature is 150 DEG C, makes powder
Last shape methyl hydrogen-based MQ type fluorine silicon resin is completely dissolved, and is subsequently cooled to 22 DEG C；
(3) will through the poly- fluorosilicone of methyl ethylene provisioned in the pretreated crosslinking agent of step (2) and step (1),
Catalyst, inhibitor and auxiliary material are added in reaction vessel, are carried out under conditions of vacuum degree is -0.09Mpa, temperature is 22 DEG C
Stirring (mixing speed is 70 revs/min, and mixing time is 2 hours), is uniformly mixed the material in reaction vessel, obtains ultraviolet
Light LED packaging plastic.
The viscosity of packaging plastic obtained is about 6000mPa.s(25 DEG C), fluorinated volume about 4%, suitable for the ultraviolet of UV-A wave band
Light LED encapsulation.It (is encapsulated for SMD5050 ultraviolet light lamp bead) when use, above-mentioned ultraviolet leds packaging plastic vacuum is arranged and is steeped
Afterwards, it injects in 2mm × 10mm × 2mm mold, precuring 1 hour at 80 DEG C, then solidifies 4 hours at 150 DEG C, be allowed to
As silica gel piece.After tested, which is 95%(in a length of 365nm of incident light wave, silica gel piece in the transmitance of UV-A wave band
It is measured in the case where with a thickness of 2mm)；After 365nm ultraviolet light 1000h, transmitance decaying < 2%；Packaged is ultraviolet
Light SMD5050 lamp bead is without exception through red ink, Reflow Soldering and 1000 bout of cooling thermal impact.
Claims (10)
1. a kind of ultraviolet leds packaging plastic, it is characterised in that be made of the raw material that following weight matches: the poly- fluorine of methyl ethylene
50-80 parts of siloxanes, 25-40 parts of crosslinking agent, 0.1-0.5 parts of catalyst, 0.01-0.1 parts of inhibitor, 0-5 parts of auxiliary material；
The crosslinking agent be viscosity be 50-2000 mPas, hydrogen-based mass fraction is 0.1-0.5%, fluorine-based mass fraction is
The poly- fluorosilicone of linear methyl hydrogen-based or viscosity of 1-10% are 50-2000 mPas, hydrogen-based mass fraction is
0.1-0.5%, the methyl hydrogen-based T-type fluorine silicon resin that fluorine-based mass fraction is 1-10% or the linear methyl hydrogen-based are poly-
Fluorosilicone, methyl hydrogen-based T-type fluorine silicon resin and hydrogen-based mass fraction are 0.1-0.5%, fluorine-based mass fraction is 1-10%'s
A variety of combinations in methyl hydrogen-based MQ type fluorine silicon resin.
2. ultraviolet leds packaging plastic according to claim 1, it is characterized in that: the poly- fluorosilicone of the methyl ethylene is
The linear methyl that viscosity is 1000-60000 mPas, vinyl mass fraction is 1-6%, fluorine-based mass fraction is 5-19%
The poly- fluorosilicone of vinyl or viscosity are 1000-60000 mPas, vinyl mass fraction is 1-6%, fluorine-based matter
Measure the methyl ethylene T-type fluorine silicon resin or the poly- fluorosilicone of the linear methyl vinyl, methyl that score is 5-19%
The methyl vinyl MQ that vinyl T-type fluorine silicon resin and vinyl mass fraction are 1-6%, fluorine-based mass fraction is 5-19%
A variety of combinations in type fluorine silicon resin.
3. ultraviolet leds packaging plastic according to claim 1, it is characterized in that: the catalyst is the poly- silicon of methyl ethylene
The platinum complex of oxygen alkane, the platinum complex of diethyl phthalate coordination, organosilicon micro-spheres platinum catalyst or organic
The platinum catalyst of silicone resin cladding.
4. ultraviolet leds packaging plastic according to claim 1, it is characterized in that: the inhibitor be 1-Ethynylcyclohexanol,
2,2- 2-butyne methanol, 3,5- dimethyl -3- hydroxyl -1- hexin, 3- Methyl-1-pentene -3- alcohol or poly- methyl ethylene
Cyclic compound.
5. ultraviolet leds packaging plastic according to claim 1, it is characterized in that: the auxiliary material be fluorine-containing acrylate and
The combination of one or both of nano silica.
6. ultraviolet leds packaging plastic according to claim 5, it is characterized in that: the fluorine-containing acrylate is 2- trifluoro
The combination of one or both of methyl 2 ', 2 ', 2 '-trifluoro ethyl ester of -2- acrylic acid and acrylic acid 2,2,2- trifluoro ethyl ester.
7. ultraviolet leds packaging plastic according to claim 1, it is characterized in that: the auxiliary material is 2,2,2- trifluoro of n-butyric acie
The combination of ethyl ester or n-butyric acie 2,2,2- trifluoro ethyl ester and nano silica.
8. the preparation method of ultraviolet leds packaging plastic described in claim 1, it is characterised in that successively include the following steps:
(1) by weight, following raw materials are equipped with: poly- fluorosilicone 50-80 parts of methyl ethylene, 25-40 parts of crosslinking agent, being catalyzed
0.1-0.5 parts of agent, 0.01-0.1 parts of inhibitor, 0-5 parts of auxiliary material；
(2) the poly- fluorosilicone of methyl ethylene, crosslinking agent, catalyst, inhibitor and auxiliary material provisioned in step (1) are added to
It in reaction vessel, is stirred under conditions of vacuum degree is-0.05-- 0.09 MPa, temperature is 20-28 DEG C, holds reaction
Material in device is uniformly mixed, and obtains ultraviolet leds packaging plastic.
9. the preparation method of ultraviolet leds packaging plastic according to claim 8, it is characterised in that: the ethylene methacrylic
The poly- fluorosilicone of base be viscosity be 1000-60000 mPas, vinyl mass fraction is 1-6%, fluorine-based mass fraction is
The poly- fluorosilicone of linear methyl vinyl or viscosity of 5-19% is 1000-60000 mPas, vinyl quality is divided
Number is 1-6%, the methyl ethylene T-type fluorine silicon resin that fluorine-based mass fraction is 5-19% or the linear methyl ethylene
The poly- fluorosilicone of base, methyl ethylene T-type fluorine silicon resin and vinyl mass fraction are 1-6%, fluorine-based mass fraction is 5-
A variety of combinations in 19% methyl vinyl MQ type fluorine silicon resin；Contain ethylene methacrylic in the poly- fluorosilicone of methyl ethylene
Base MQ type fluorine silicon resin, and methyl vinyl MQ type fluorine silicon resin be solid material in the case where, by methyl second in step (2)
Before the poly- fluorosilicone of alkenyl is added in reaction vessel, in advance by the poly- fluorosilicone mixed dissolution of methyl ethylene.
10. the preparation method of ultraviolet leds packaging plastic according to claim 8, it is characterised in that: contain in crosslinking agent
Methyl hydrogen-based MQ type fluorine silicon resin, and methyl hydrogen-based MQ type fluorine silicon resin be solid material in the case where, in step (2) will hand over
Before joining in agent addition reaction vessel, in advance by crosslinking agent mixed dissolution.
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| KR102598500B1 (en) * | 2018-09-04 | 2023-11-06 | 쑤저우 레킨 세미컨덕터 컴퍼니 리미티드 | Lighting emitting device package |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880396A (en) * | 2010-06-03 | 2010-11-10 | 杭州师范大学 | Preparation method of organic silicon rubber for encapsulating LED being convenient for vacuum defoamation |
| CN103242801A (en) * | 2013-05-14 | 2013-08-14 | 汕头市骏码凯撒有限公司 | Single-component high-refractivity LED (light-emitting diode) packaging adhesive and preparation method thereof |
| CN105418928A (en) * | 2015-12-29 | 2016-03-23 | 广东恒大新材料科技有限公司 | Trifluoropropyl-group-modification methyl phenyl vinyl silicon resin and LED packaging adhesive |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101880396A (en) * | 2010-06-03 | 2010-11-10 | 杭州师范大学 | Preparation method of organic silicon rubber for encapsulating LED being convenient for vacuum defoamation |
| CN103242801A (en) * | 2013-05-14 | 2013-08-14 | 汕头市骏码凯撒有限公司 | Single-component high-refractivity LED (light-emitting diode) packaging adhesive and preparation method thereof |
| CN105418928A (en) * | 2015-12-29 | 2016-03-23 | 广东恒大新材料科技有限公司 | Trifluoropropyl-group-modification methyl phenyl vinyl silicon resin and LED packaging adhesive |
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