CN107033600A - A kind of doping of acrylonitrile, LED encapsulation material with fluorescent functional and preparation method thereof - Google Patents
A kind of doping of acrylonitrile, LED encapsulation material with fluorescent functional and preparation method thereof Download PDFInfo
- Publication number
- CN107033600A CN107033600A CN201610971779.0A CN201610971779A CN107033600A CN 107033600 A CN107033600 A CN 107033600A CN 201610971779 A CN201610971779 A CN 201610971779A CN 107033600 A CN107033600 A CN 107033600A
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- China
- Prior art keywords
- acrylonitrile
- silicone oil
- vinyl
- led encapsulation
- fluorescent
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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
- C08L83/00—Compositions 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
- C08L83/04—Polysiloxanes
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
LED encapsulation material the invention discloses a kind of doping of acrylonitrile, with fluorescent functional and preparation method thereof, it is characterised in that be made up of the raw material of following parts by weight：Acrylonitrile 35, vinyl silicone oil 30 40, silicon nitride 12, vinyl MQ resin 8 12, dimethylbenzene 10 20, citric acid 48, ethylenediamine 36, magnesium sulfate 13, deionized water 5 10, silicon powder 49, 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 acrylonitrile etc., the refractive index of encapsulating material is improved.
Description
Technical field
The present invention relates to a kind of LED encapsulation material, and in particular to a kind of acrylonitrile doping, the LED envelopes with fluorescent functional
Package material and preparation method thereof.
Background technology
LED organosilicon material for packaging is typically sizing material, low viscosity based on vinyl polysiloxane or vinyl silicone oil
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 must the excellent heat resistance of holding and high transparency.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, utilize 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 acrylonitrile doping, the LED encapsulation material with fluorescent functional, it is characterised in that be by the raw material of following parts by weight
It is made：
Acrylonitrile 3-5, vinyl silicone oil 30-40, silicon nitride 1-2, vinyl MQ resin 8-12, dimethylbenzene 10-20, citric acid
4-8, ethylenediamine 3-6, magnesium sulfate 1-3, deionized water 5-10, silicon powder 4-9, Silane coupling agent KH550 6-11, containing hydrogen silicone oil
Crosslinking agent 25-35, chloroplatinic acid isopropanol 2-3.
A kind of described acrylonitrile doping, the LED encapsulation material with fluorescent functional and preparation method thereof, its feature exists
In being made up of following steps：
A. vinyl silicone oil is put into equipped with agitator, the container of thermocouple, is warming up to 80-120 DEG C；By vinyl MQ tree
Fat, acrylonitrile 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. using citric acid as carbon source, ethylenediamine, deionized water are added, places 3-7 days, is obtained in purple under the conditions of 150-250 DEG C
Outer light is excited down, the liquid carbon point fluorescent material with blue emission, green emission and red emission；
C. silicon powder, silicon nitride are added in liquid obtained by step b, add Silane coupling agent KH550, ultrasonic disperse 10-
After 30min, 3-5h is soaked, filtering, washing, drying obtain adsorbing the mixture of carbon point fluorescent material；
D. mixture obtained by adding containing hydrogen silicone oil crosslinking agent and step c into basic glue obtained by step a, is then injected into chloroplatinic acid
Isopropanol, magnesium sulfate, 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 of deeply-curing 1-3 h, is cooled to room temperature and obtains encapsulating material；
A kind of described acrylonitrile doping, the LED encapsulation material with fluorescent functional and preparation method thereof, it is characterised in that step
The condition of desolvation is 120-140 DEG C of temperature, pressure -0.06 ~ -0.1MPa in rapid a.
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 direct contact of carbon point fluorescent material and LED chip, efficiently solves due to LED
Chip generates heat and causes the problem of 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 acrylonitrile etc., the refractive index of encapsulating material is improved.
Embodiment
With reference to embodiment, the embodiment to the present invention is further described.
Embodiment
A kind of acrylonitrile doping, the LED encapsulation material with fluorescent functional, it is characterised in that be by following parts by weight
Raw material is made：
Acrylonitrile 5, vinyl silicone oil 40, silicon nitride 2, vinyl MQ resin 12, dimethylbenzene 20, citric acid 8, ethylenediamine 6, sulphur
Sour magnesium 3, deionized water 10, silicon powder 9, Silane coupling agent KH550 11, containing hydrogen silicone oil crosslinking agent 35, chloroplatinic acid isopropanol 3.
A kind of described acrylonitrile doping, the LED encapsulation material with fluorescent functional and preparation method thereof, its feature exists
In being made up of following steps：
A. vinyl silicone oil is put into equipped with agitator, the container of thermocouple, is warming up to 80-120 DEG C；By vinyl MQ tree
Fat, acrylonitrile 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. using citric acid as carbon source, ethylenediamine, deionized water are added, places 3-7 days, is obtained in purple under the conditions of 150-250 DEG C
Outer light is excited down, the liquid carbon point fluorescent material with blue emission, green emission and red emission；
C. silicon powder, silicon nitride are added in liquid obtained by step b, add Silane coupling agent KH550, ultrasonic disperse 10-
After 30min, 3-5h is soaked, filtering, washing, drying obtain adsorbing the mixture of carbon point fluorescent material；
D. mixture obtained by adding containing hydrogen silicone oil crosslinking agent and step c into basic glue obtained by step a, is then injected into chloroplatinic acid
Isopropanol, magnesium sulfate, 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 of deeply-curing 1-3 h, is cooled to room temperature and obtains encapsulating material；
A kind of described acrylonitrile doping, the LED encapsulation material with fluorescent functional and preparation method thereof, it is characterised in that step
The condition of desolvation is 120-140 DEG C of temperature, pressure -0.06 ~ -0.1MPa in rapid a.
The present invention technical parameter be：Hardness >=62 degree；The MPa of tensile strength >=4.94；Elongation at break >=231%；Thoroughly
Light rate >=90%.
Claims (3)
1. a kind of acrylonitrile doping, the LED encapsulation material with fluorescent functional, it is characterised in that be by the original of following parts by weight
Material is made：
Acrylonitrile 3-5, vinyl silicone oil 30-40, silicon nitride 1-2, vinyl MQ resin 8-12, dimethylbenzene 10-20, citric acid
4-8, ethylenediamine 3-6, magnesium sulfate 1-3, deionized water 5-10, silicon powder 4-9, Silane coupling agent KH550 6-11, containing hydrogen silicone oil
Crosslinking agent 25-35, chloroplatinic acid isopropanol 2-3.
2. a kind of acrylonitrile according to claim 1 adulterates, with the LED encapsulation material of fluorescent functional and its preparation side
Method, it is characterised in that be made up of following steps：
A. vinyl silicone oil is put into equipped with agitator, the container of thermocouple, is warming up to 80-120 DEG C；By vinyl MQ tree
Fat, acrylonitrile 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. using citric acid as carbon source, ethylenediamine, deionized water are added, places 3-7 days, is obtained in purple under the conditions of 150-250 DEG C
Outer light is excited down, the liquid carbon point fluorescent material with blue emission, green emission and red emission；
C. silicon powder, silicon nitride are added in liquid obtained by step b, add Silane coupling agent KH550, ultrasonic disperse 10-
After 30min, 3-5h is soaked, filtering, washing, drying obtain adsorbing the mixture of carbon point fluorescent material；
D. mixture obtained by adding containing hydrogen silicone oil crosslinking agent and step c into basic glue obtained by step a, is then injected into chloroplatinic acid
Isopropanol, magnesium sulfate, 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 of deeply-curing 1-3 h, is cooled to room temperature and obtains encapsulating material.
3. a kind of acrylonitrile according to claim 2 adulterates, with the LED encapsulation material of fluorescent functional and its preparation side
Method, it is characterised in that the condition of desolvation is 120-140 DEG C of temperature, pressure -0.06 ~ -0.1MPa in step a.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610971779.0A CN107033600A (en) | 2016-11-07 | 2016-11-07 | A kind of doping of acrylonitrile, LED encapsulation material with fluorescent functional and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610971779.0A CN107033600A (en) | 2016-11-07 | 2016-11-07 | A kind of doping of acrylonitrile, LED encapsulation material with fluorescent functional and preparation method thereof |
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| CN107033600A true CN107033600A (en) | 2017-08-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108511584A (en) * | 2018-03-12 | 2018-09-07 | 合肥同佑电子科技有限公司 | A kind of special encapsulating material of light emitting diode and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104292755A (en) * | 2014-10-16 | 2015-01-21 | 苏州思莱特电子科技有限公司 | High-molecule LED (Light-Emitting Diode) packaging material 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 |
-
2016
- 2016-11-07 CN CN201610971779.0A patent/CN107033600A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104292755A (en) * | 2014-10-16 | 2015-01-21 | 苏州思莱特电子科技有限公司 | High-molecule LED (Light-Emitting Diode) packaging material 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108511584A (en) * | 2018-03-12 | 2018-09-07 | 合肥同佑电子科技有限公司 | A kind of special encapsulating material of light emitting diode and preparation method thereof |
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Application publication date: 20170811 |
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