CN106751883A - A kind of light transmittance is good, LED encapsulation material with fluorescent functional and preparation method thereof - Google Patents

A kind of light transmittance is good, LED encapsulation material with fluorescent functional and preparation method thereof Download PDF

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Publication number
CN106751883A
CN106751883A CN201610971777.1A CN201610971777A CN106751883A CN 106751883 A CN106751883 A CN 106751883A CN 201610971777 A CN201610971777 A CN 201610971777A CN 106751883 A CN106751883 A CN 106751883A
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Prior art keywords
silicone oil
light transmittance
led encapsulation
good
fluorescent
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Pending
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CN201610971777.1A
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Inventor
林海
陈海青
张家高
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Anhui Zhong Wei Photoelectric Material Co Ltd
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Anhui Zhong Wei Photoelectric Material Co Ltd
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Priority to CN201610971777.1A priority Critical patent/CN106751883A/en
Publication of CN106751883A publication Critical patent/CN106751883A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of 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; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor 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
    • H01L33/48Semiconductor 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
    • H01L33/52Encapsulations
    • H01L33/56Materials, e.g. epoxy or silicone resin
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer 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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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Led Device Packages (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses a kind of light transmittance is good, LED encapsulation material with fluorescent functional and preparation method thereof, it is characterised in that be made up of the raw material of following weight portion:Glass micro mist 13, vinyl silicone oil 30 40, nano titanium oxide 23, vinyl MQ resin 8 12, dimethylbenzene 10 20, citric acid 48, carragheen 24, ethylenediamine 36, deionized water 5 10, silicon powder 5 10, Silane coupling agent KH550 6 11, containing hydrogen silicone oil crosslinking agent 25 35, chloroplatinic acid isopropanol 23.The present invention soaks using with carbon point fluorescent material to silicon powder, and is incorporated into encapsulation silica gel material, and silica obtained material has fluorescent functional, and crack resistence function admirable;By adding glass micro mist etc. so that encapsulating material light transmittance is more preferable, air-tightness is superior.

Description

A kind of light transmittance is good, LED encapsulation material with fluorescent functional and preparation method thereof
Technical field
The present invention relates to a kind of LED encapsulation material, and in particular to a kind of light transmittance is good, LED encapsulation with fluorescent functional Material and preparation method thereof.
Background technology
LED organosilicon material for packaging is typically the sizing material based on vinyl polysiloxane or vinyl silicone oil, low viscosity Containing hydrogen silicone oil is crosslinking agent, then coordinates reinforced resin, diluent, catalyst, inhibitor etc., under certain condition crosslinking curing and .With the development of the progress of LED encapsulation technologies, particularly large power white light LED, organic silicon encapsulating material is increasingly Show its advantage.LED encapsulation is different from general organosilicon material with silica gel material, except to possess preferable mechanical property Can be outer, and excellent heat resistance and high transparency must be kept.The preparation of organosilicon encapsulating material uses dual composition addition type mostly Formula system, is molded under conditions of the presence of Pt series catalysts by heat cure.
Liu Jinlong is in its master thesis《The preparation of LED encapsulation silica gel materials and performance study》In, using ethene Base silicone oil and containing hydrogen silicone oil crosslinking agent are prepared for LED encapsulation silica gel materials, but also there is crack resistence performance shortcoming, do not have The problems such as having fluorescent functional.
The content of the invention
Think deeply based on more than, the present invention is intended to provide a kind of crack resistence, and the LED encapsulation material with fluorescent functional.
The technical problems to be solved by the invention are realized using following technical scheme:
A kind of light transmittance is good, LED encapsulation material with fluorescent functional, it is characterised in that be by the raw material system of following weight portion Into:
Glass micro mist 1-3, vinyl silicone oil 30-40, nano titanium oxide 2-3, vinyl MQ resin 8-12, dimethylbenzene 10- 20, citric acid 4-8, carragheen 2-4, ethylenediamine 3-6, deionized water 5-10, silicon powder 5-10, Silane coupling agent KH550 6- 11, containing hydrogen silicone oil crosslinking agent 25-35, chloroplatinic acid isopropanol 2-3.
A kind of described light transmittance is good, LED encapsulation material with fluorescent functional and preparation method thereof, it is characterised in that It is made up of following steps:
A. vinyl silicone oil, carragheen are put into equipped with agitator, the container of thermocouple, 80-120 DEG C is warming up to;By ethene Base MQ resins are dissolved in xylene solution, and stirring is slowly dropped in above-mentioned vinyl silicone oil to after dissolving, and drop continues after finishing Constant temperature stirs 10-30min, and last fully desolvation obtains basic glue;
B. with citric acid as carbon source, ethylenediamine, deionized water are added, is placed 3-7 days under the conditions of 150-250 DEG C, obtained in purple Outer light is excited down, the liquid carbon point fluorescent material with blue emission, green emission and red emission;
C. silicon powder, glass dust, nano titanium oxide are added in step b gained liquid, add silane coupler KH550, after ultrasonic disperse 10-30min, soaks 3-5h, and filtering, washing, drying obtain adsorbing the mixing of carbon point fluorescent material Thing;
D. to containing hydrogen silicone oil crosslinking agent and step c gained mixtures is added in the basic glue of step a gained, it is then injected into chloroplatinic acid Isopropanol, vacuum defoamation 20-50 min after being well mixed, then respectively at 80-100 DEG C of precrosslink 0.5-2 h, 130-160 DEG C deeply-curing 1-3 h, are cooled to room temperature and obtain encapsulating material;
A kind of described light transmittance is good, LED encapsulation material with fluorescent functional and preparation method thereof, it is characterised in that step a The condition of middle desolvation is 120-140 DEG C of temperature, pressure -0.06 ~ -0.1MPa.
The beneficial effects of the invention are as follows:Using vinyl MQ resin reinforcement vinyl silicone oil, obtained encapsulating material is heat-resisting Property preferably, tensile strength is larger;The treated silicon powder adsorptivity of Silane coupling agent KH550, dispersiveness preferably, are soaked in carbon point After in fluorescent material, carbon point fluorescent material can be adsorbed, thus assign encapsulating material can fluorescence the characteristics of, meanwhile, its uniform point It is dispersed in silica gel packaging material, it is to avoid the directly contact of carbon point fluorescent material and LED chip, efficiently solves due to LED Chip generates heat and causes the problem that fluorescent material rate of decay is too high, failure is too fast, and then improves the service life of LED lamps And integrated quality;On the other hand, the introducing of silicon powder acts not only as the carrier of carbon point fluorescent material, moreover it is possible to reduce silicon materials The exothermic peak temperature of curing reaction, reduces the linear expansion coefficient and shrinkage factor of solidfied material, so that the internal stress of solidfied material is eliminated, Prevent cracking;By adding glass micro mist etc. so that encapsulating material light transmittance is more preferable, air-tightness is superior.
Specific embodiment
With reference to embodiment, specific embodiment of the invention is further described.
Embodiment
A kind of light transmittance is good, LED encapsulation material with fluorescent functional, it is characterised in that be by the original of following weight portion Material is made:
Glass micro mist 3, vinyl silicone oil 40, nano titanium oxide 3, vinyl MQ resin 12, dimethylbenzene 20, citric acid 8, card Draw glue 4, ethylenediamine 6, deionized water 10, silicon powder 10, Silane coupling agent KH550 11, containing hydrogen silicone oil crosslinking agent 35, chloroplatinic acid Isopropanol 3.
A kind of described light transmittance is good, LED encapsulation material with fluorescent functional and preparation method thereof, it is characterised in that It is made up of following steps:
A. vinyl silicone oil, carragheen are put into equipped with agitator, the container of thermocouple, 80-120 DEG C is warming up to;By ethene Base MQ resins are dissolved in xylene solution, and stirring is slowly dropped in above-mentioned vinyl silicone oil to after dissolving, and drop continues after finishing Constant temperature stirs 10-30min, and last fully desolvation obtains basic glue;
B. with citric acid as carbon source, ethylenediamine, deionized water are added, is placed 3-7 days under the conditions of 150-250 DEG C, obtained in purple Outer light is excited down, the liquid carbon point fluorescent material with blue emission, green emission and red emission;
C. silicon powder, glass dust, nano titanium oxide are added in step b gained liquid, add silane coupler KH550, after ultrasonic disperse 10-30min, soaks 3-5h, and filtering, washing, drying obtain adsorbing the mixing of carbon point fluorescent material Thing;
D. to containing hydrogen silicone oil crosslinking agent and step c gained mixtures is added in the basic glue of step a gained, it is then injected into chloroplatinic acid Isopropanol, vacuum defoamation 20-50 min after being well mixed, then respectively at 80-100 DEG C of precrosslink 0.5-2 h, 130-160 DEG C deeply-curing 1-3 h, are cooled to room temperature and obtain encapsulating material;
A kind of described light transmittance is good, LED encapsulation material with fluorescent functional and preparation method thereof, it is characterised in that step a The condition of middle desolvation is 120-140 DEG C of temperature, pressure -0.06 ~ -0.1MPa.
Technical parameter of the invention is:Hardness >=62 degree;Tensile strength >=4.94 MPa;Elongation at break >=231%;Thoroughly Light rate >=90%.

Claims (3)

1. a kind of light transmittance is good, LED encapsulation material with fluorescent functional, it is characterised in that be by the raw material of following weight portion It is made:
Glass micro mist 1-3, vinyl silicone oil 30-40, nano titanium oxide 2-3, vinyl MQ resin 8-12, dimethylbenzene 10- 20, citric acid 4-8, carragheen 2-4, ethylenediamine 3-6, deionized water 5-10, silicon powder 5-10, Silane coupling agent KH550 6- 11, containing hydrogen silicone oil crosslinking agent 25-35, chloroplatinic acid isopropanol 2-3.
2. a kind of light transmittance according to claim 1 is good, LED encapsulation material with fluorescent functional and preparation method thereof, Characterized in that, being made up of following steps:
A. vinyl silicone oil, carragheen are put into equipped with agitator, the container of thermocouple, 80-120 DEG C is warming up to;By ethene Base MQ resins are dissolved in xylene solution, and stirring is slowly dropped in above-mentioned vinyl silicone oil to after dissolving, and drop continues after finishing Constant temperature stirs 10-30min, and last fully desolvation obtains basic glue;
B. with citric acid as carbon source, ethylenediamine, deionized water are added, is placed 3-7 days under the conditions of 150-250 DEG C, obtained in purple Outer light is excited down, the liquid carbon point fluorescent material with blue emission, green emission and red emission;
C. silicon powder, glass dust, nano titanium oxide are added in step b gained liquid, add silane coupler KH550, after ultrasonic disperse 10-30min, soaks 3-5h, and filtering, washing, drying obtain adsorbing the mixing of carbon point fluorescent material Thing;
D. to containing hydrogen silicone oil crosslinking agent and step c gained mixtures is added in the basic glue of step a gained, it is then injected into chloroplatinic acid Isopropanol, vacuum defoamation 20-50 min after being well mixed, then respectively at 80-100 DEG C of precrosslink 0.5-2 h, 130-160 DEG C deeply-curing 1-3 h, are cooled to room temperature and obtain encapsulating material.
3. a kind of light transmittance according to claim 2 is good, LED encapsulation material with fluorescent functional and preparation method thereof, Characterized in that, the condition of desolvation is 120-140 DEG C of temperature, pressure -0.06 ~ -0.1MPa in step a.
CN201610971777.1A 2016-11-07 2016-11-07 A kind of light transmittance is good, LED encapsulation material with fluorescent functional and preparation method thereof Pending CN106751883A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103045156A (en) * 2011-10-17 2013-04-17 杭州中富彩新材料科技有限公司 Carbon nanotube in situ reinforced LED packaging silica gel and preparation method thereof
CN103395771A (en) * 2013-08-01 2013-11-20 吉林大学 Carbon dots with high fluorescent quantum yield, and application thereof in fluorescent color development
CN105304793A (en) * 2015-10-08 2016-02-03 五邑大学 Insulated liquid packaged LED and preparation method thereof
CN106047275A (en) * 2016-08-05 2016-10-26 合肥毅创钣金科技有限公司 Nanometer diamond-titanium hybrid modified high-thermal conductivity LED organosilicon packaging glue and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103045156A (en) * 2011-10-17 2013-04-17 杭州中富彩新材料科技有限公司 Carbon nanotube in situ reinforced LED packaging silica gel and preparation method thereof
CN103395771A (en) * 2013-08-01 2013-11-20 吉林大学 Carbon dots with high fluorescent quantum yield, and application thereof in fluorescent color development
CN105304793A (en) * 2015-10-08 2016-02-03 五邑大学 Insulated liquid packaged LED and preparation method thereof
CN106047275A (en) * 2016-08-05 2016-10-26 合肥毅创钣金科技有限公司 Nanometer diamond-titanium hybrid modified high-thermal conductivity LED organosilicon packaging glue and preparation method thereof

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Application publication date: 20170531

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