CN106566258A - LED packaging material doped with glass fiber and having fluorescent function and preparation method thereof - Google Patents

LED packaging material doped with glass fiber and having fluorescent function and preparation method thereof Download PDF

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Publication number
CN106566258A
CN106566258A CN201610971802.6A CN201610971802A CN106566258A CN 106566258 A CN106566258 A CN 106566258A CN 201610971802 A CN201610971802 A CN 201610971802A CN 106566258 A CN106566258 A CN 106566258A
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China
Prior art keywords
parts
silicone oil
glass fiber
fluorescent
preparation
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Pending
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CN201610971802.6A
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Chinese (zh)
Inventor
肖亮
马睿
陆慧
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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 CN201610971802.6A priority Critical patent/CN106566258A/en
Publication of CN106566258A publication Critical patent/CN106566258A/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
    • 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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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Surface Treatment Of Glass Fibres Or Filaments (AREA)

Abstract

The invention discloses an LED packaging material doped with glass fiber and having a fluorescent function and a preparation method thereof. The LED packaging material is characterized by being prepared from the following raw materials in parts by weight: 2-4 parts of the glass fiber, 30-40 parts of vinyl silicone oil, 1-2 parts of mica powder, 8-12 parts of vinyl MQ resin, 10-20 parts of dimethyl benzene, 4-8 parts of citric acid, 3-6 parts of ethylene diamine, 1-2 parts of polyvinyl alcohol, 5-10 parts of deionized water, 5-10 parts of silica micro powder, 6-11 parts of a silane coupling agent KH550, 25-35 parts of a hydrogen-containing silicone oil crosslinking agent, and 2-3 parts of isopropanol platinichloride. According to the preparation method disclosed by the invention, a carbon dot fluorescent material is used for soaking the silica micro powder, then the silica micro powder is introduced into a silica gel material for packaging, and the obtained silica gel material has a fluorescent function and is good in anti-cracking performance; and by correspondingly adding the glass fiber, the mica powder and the like, the high-temperature resistance and insulating property of the material are significantly improved.

Description

A kind of doped-glass fiber, the LED encapsulation material with fluorescent functional and its preparation Method
Technical field
The present invention relates to a kind of LED encapsulation material, and in particular to a kind of doped-glass fiber, the LED with fluorescent functional Encapsulating 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 cross-linking 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, silicone 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 thermostability and high transparent must be kept.The preparation of organosilicon encapsulating material adopts dual composition addition type mostly Formula system, under conditions of Pt series catalysts are present heat cure molding is passed through.
Liu Jinlong is in its master thesis《The preparation and performance study of LED encapsulation silica gel materials》In, using ethylene Base silicone oil and containing hydrogen silicone oil cross-linking 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 problem to be solved is realized using following technical scheme:
A kind of doped-glass fiber, the LED encapsulation material with fluorescent functional, it is characterised in that be by the original of following weight portion Material is made:
Glass fibre 2-4, vinyl silicone oil 30-40, mica powder 1-2, vinyl MQ resin 8-12, dimethylbenzene 10-20, Fructus Citri Limoniae Sour 4-8, ethylenediamine 3-6, polyvinyl alcohol 1-2, deionized water 5-10, silicon powder 5-10, Silane coupling agent KH550 6-11, it is hydrogeneous Silicone oil cross-linking agent 25-35, chloroplatinic acid isopropanol 2-3.
Described a kind of doped-glass fiber, 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, polyvinyl alcohol are put in equipped with agitator, the container of thermocouple, 80-120 DEG C is warming up to;By second Thiazolinyl MQ resins are dissolved in xylene solution, are stirred to dissolving, in being slowly dropped to above-mentioned vinyl silicone oil, drip Bi Houji Continuous 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, mica powder, glass fibre are added in step b gained liquid, add Silane coupling agent KH550, surpassed After sound dispersion 10-30min, 3-5h is soaked, filter, wash, dry, obtain adsorbing the mixture of carbon point fluorescent material;
D. containing hydrogen silicone oil cross-linking agent and step c gained mixture are added in the basic glue of step a gained, chloroplatinic acid is then injected into Isopropanol, vacuum defoamation 20-50 min after mix homogeneously, 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;
Described a kind of doped-glass fiber, the LED encapsulation material with fluorescent functional and preparation method thereof, it is characterised in that In step a the condition of desolvation be temperature 120-140 DEG C, pressure -0.06 ~ -0.1MPa.
The invention has the beneficial effects as follows:Using vinyl MQ resin reinforcement vinyl silicone oil, obtained encapsulating material is heat-resisting Property preferably, tensile strength is larger;Silicon powder adsorptivity, the dispersibility that Silane coupling agent KH550 was processed preferably, is soaked in carbon point After in fluorescent material, carbon point fluorescent material can be adsorbed, so as to give encapsulating material can fluorescence the characteristics of, meanwhile, its uniform point In being dispersed in silica gel packaging material, it is to avoid the directly contact of carbon point fluorescent material and LED chip, efficiently solve 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 as to eliminate the internal stress of solidfied material, Prevent cracking;By coordinating addition glass fibre, mica powder etc., heat-resisting quantity, the insulating properties of material are significantly improved.
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is further described.
Embodiment
A kind of doped-glass fiber, the LED encapsulation material with fluorescent functional, it is characterised in that be by following weight portion Raw material make:
Glass fibre 4, vinyl silicone oil 40, mica powder 2, vinyl MQ resin 12, dimethylbenzene 20, citric acid 8, ethylenediamine 6, Polyvinyl alcohol 2, deionized water 10, silicon powder 10, Silane coupling agent KH550 11, containing hydrogen silicone oil cross-linking agent 35, chloroplatinic acid isopropyl Alcohol 3.
Described a kind of doped-glass fiber, 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, polyvinyl alcohol are put in equipped with agitator, the container of thermocouple, 80-120 DEG C is warming up to;By second Thiazolinyl MQ resins are dissolved in xylene solution, are stirred to dissolving, in being slowly dropped to above-mentioned vinyl silicone oil, drip Bi Houji Continuous 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, mica powder, glass fibre are added in step b gained liquid, add Silane coupling agent KH550, surpassed After sound dispersion 10-30min, 3-5h is soaked, filter, wash, dry, obtain adsorbing the mixture of carbon point fluorescent material;
D. containing hydrogen silicone oil cross-linking agent and step c gained mixture are added in the basic glue of step a gained, chloroplatinic acid is then injected into Isopropanol, vacuum defoamation 20-50 min after mix homogeneously, 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;
Described a kind of doped-glass fiber, the LED encapsulation material with fluorescent functional and preparation method thereof, it is characterised in that In step a the condition of desolvation be temperature 120-140 DEG C, pressure -0.06 ~ -0.1MPa.
The present invention technical parameter be:Hardness >=62 degree;Tensile strength >=4.94 MPa;Elongation at break >=231%;Thoroughly Light rate >=90%.

Claims (3)

1. a kind of doped-glass fiber, the LED encapsulation material with fluorescent functional, it is characterised in that be by following weight portion Raw material is made:
Glass fibre 2-4, vinyl silicone oil 30-40, mica powder 1-2, vinyl MQ resin 8-12, dimethylbenzene 10-20, Fructus Citri Limoniae Sour 4-8, ethylenediamine 3-6, polyvinyl alcohol 1-2, deionized water 5-10, silicon powder 5-10, Silane coupling agent KH550 6-11, it is hydrogeneous Silicone oil cross-linking agent 25-35, chloroplatinic acid isopropanol 2-3.
2. a kind of doped-glass fiber according to claim 1, the LED encapsulation material with fluorescent functional and its preparation side Method, it is characterised in that be made up of following steps:
A. vinyl silicone oil, polyvinyl alcohol are put in equipped with agitator, the container of thermocouple, 80-120 DEG C is warming up to;By second Thiazolinyl MQ resins are dissolved in xylene solution, are stirred to dissolving, in being slowly dropped to above-mentioned vinyl silicone oil, drip Bi Houji Continuous 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, mica powder, glass fibre are added in step b gained liquid, add Silane coupling agent KH550, surpassed After sound dispersion 10-30min, 3-5h is soaked, filter, wash, dry, obtain adsorbing the mixture of carbon point fluorescent material;
D. containing hydrogen silicone oil cross-linking agent and step c gained mixture are added in the basic glue of step a gained, chloroplatinic acid is then injected into Isopropanol, vacuum defoamation 20-50 min after mix homogeneously, 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 doped-glass fiber according to claim 2, the LED encapsulation material with fluorescent functional and its preparation side Method, it is characterised in that in step a the condition of desolvation be temperature 120-140 DEG C, pressure -0.06 ~ -0.1MPa.
CN201610971802.6A 2016-11-07 2016-11-07 LED packaging material doped with glass fiber and having fluorescent function and preparation method thereof Pending CN106566258A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112898783A (en) * 2021-01-27 2021-06-04 湖南柯盛新材料有限公司 Double-component transfer printing silica gel and preparation method thereof
CN115093827A (en) * 2022-06-23 2022-09-23 厦门捌斗新材料科技有限公司 Organic silicon pouring sealant and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104893600A (en) * 2015-05-14 2015-09-09 天津德高化成新材料股份有限公司 Viscous fluorescent glue film for fast package of light emitting diode and preparation method and application thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104893600A (en) * 2015-05-14 2015-09-09 天津德高化成新材料股份有限公司 Viscous fluorescent glue film for fast package of light emitting diode and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
闵云浩: "荧光碳点的合成制备及其性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112898783A (en) * 2021-01-27 2021-06-04 湖南柯盛新材料有限公司 Double-component transfer printing silica gel and preparation method thereof
CN115093827A (en) * 2022-06-23 2022-09-23 厦门捌斗新材料科技有限公司 Organic silicon pouring sealant and preparation method thereof
CN115093827B (en) * 2022-06-23 2024-04-02 厦门捌斗新材料科技有限公司 Organic silicon pouring sealant and preparation method thereof

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Application publication date: 20170419