CN109294497A - A kind of LED epoxy encapsulant with matte surface characteristic - Google Patents
A kind of LED epoxy encapsulant with matte surface characteristic Download PDFInfo
- Publication number
- CN109294497A CN109294497A CN201811059262.XA CN201811059262A CN109294497A CN 109294497 A CN109294497 A CN 109294497A CN 201811059262 A CN201811059262 A CN 201811059262A CN 109294497 A CN109294497 A CN 109294497A
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- Prior art keywords
- matte surface
- led
- dbu
- epoxy
- surface characteristic
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Classifications
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
-
- 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
-
- 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
Abstract
The present invention provides a kind of LED epoxy encapsulants with matte surface characteristic.It includes have the components such as epoxy resin, anhydride curing agent, isooctyl acid metal salt promoter, DBU salt promotor and inorganic filler.Technical solution of the present invention is controlled by suitable material selection and feed ratio, and the characteristic of matte surface can be reached under independent of the type of inorganic filler and additive amount, to design providing more choices property of dumb light type LED encapsulation material.LED component using technical solution of the present invention preparation has good matte surface effect, and light is soft out, has been not easy glare；Also there are high resistance to thermal deterioration, the aging characteristics of resistance to UV simultaneously.
Description
Technical field
The present invention relates to LED encapsulation material field, specially a kind of LED encapsulation asphalt mixtures modified by epoxy resin with matte surface effect
Rouge material.
Background technique
This century starts more and more indoor and outdoor displays, and lighting system etc. is made using luminescent semiconductor device (LED)
For light source.Wherein light intensity of the LED encapsulation material to LED, reliability, resistance to ag(e)ing and apparent effect etc. have significant shadow
It rings.Material currently used for LED encapsulation mainly has organosilicon and epoxy resin two major classes.Early period, a large amount of research work mainly collected
In promoted encapsulating material the transparency and ageing-resistant performance on.
In recent years, LED component especially display device put forward new requirements encapsulating material.This major embodiment device table
Requirement on facial vision is aesthetic.Such as organic siliconresin either epoxy encapsulant, it is transparent and ageing-resistant in solution
After performance, due to packaging surfacing, it be easy to cause device surface reflective, influences sense organ.On the other hand, device surface mistake
The phenomenon that generating Surface glare is also resulted in smooth.The method of solution is that luminescent semiconductor device surface is produced to the effect of dumb light
Fruit, this is conducive to the full scattering of light, promotes visual perception's property.This demand is especially pronounced in field of display.
A certain amount of inorganic filler is added in resin system, the surface with matte effect, this kind of technology can be constructed
It is widely used in dumb light type coating.The cardinal principle of this technology be the addition of high amount of inorganic filler so that paint film table
Surface roughness increases, and causes light that diffusing reflection occurs on surface, ultimately forms matte effect.But this kind of technology is in photosemiconductor
It is relatively difficult to apply in device.Main cause is: the integral thickness of coating is relatively thin, about hundreds of microns, inorganic filler is added, especially
Big particle diameter inorganic filler is easy to accumulate, so that inorganic filler floats on resin surface layer, surface roughness is caused to rise.But in light half
In conductor device, the thickness of entire encapsulated layer has reached several millimeters, and inorganic filler is easily settled in resin solidification, this is with regard to nothing
Method forms rough surface.
The patent of invention of Patent No. CN103811634A discloses a kind of LED component for preparing matte surface, principle
Similar above-mentioned low luster coating.Difference is that, by the optimization to inorganic filler type and amount, inorganic using low-density is filled out
Material, avoids sedimentation of the inorganic filler in epoxy resin cure, it is made to float on resin surface layer, forms rough surface, reaches table
Face matte effect.The patent of invention of Patent No. CN104804688A utilizes expansion also with the optimization to inorganic filler type
Loose powder solves the problems, such as LED encapsulation material surface without matte effect.Type of the above solution to inorganic filler, addition
Amount, resin viscosity, solidification process etc. is more demanding, and in actual operation, the selection of material and technological parameter receives greatly
Limitation.
Summary of the invention
In order to solve have matte surface effect LED encapsulation material high to inorganic filler and resins selective not at present
Foot, the object of the present invention is to provide a kind of LED encapsulation materials with matte surface effect, this kind of technology is independent of nothing
Machine filler, the type and additive amount of resin, it is thus only necessary to by the adjusting to epoxy/acid anhydride group ratio, Suitable accelerators
It selects, matte surface effect can be formed using the multistage contraction of resin solidification.The present inventor to solve the above-mentioned problems into
Go in-depth study, test discovery:
In anhydride-cured epoxy system, epoxy resin has at ether and at two kinds of chain growth mechanisms of ester.This and epoxy/acid anhydride group
Ratio, the selection of promotor and additive amount are closely bound up.Gel point caused by two kinds of chain growth mechanisms, cure shrinkage, including it is rear
Continuous Solidified enzyme is different.Under specific formula design, when reaction system reaches gel point, molecular resin at this time
Segment is frozen substantially, and subsequent cure reaction will lead to system and further cure shrinkage occurs.And work as cure shrinkage
When to a certain extent, that is, it will form coarse surface.Specific mechanism is not yet completely clear at present, but should be with resin system in gel
Quick cure shrinkage and related to the squeezing action of inorganic particulate after point.The method that this kind forms matte surface effect is main
Conversion ratio and cure shrinkage power when by resin gel glue point are influenced.Low gel point conversion ratio and strong cure shrinkage
The matte effect become apparent can be reached.In addition, the method for the invention and the type selection correlation of inorganic filler are little, one
A little common fillers, either spherical or angle-style or different indexs of refraction and the filler of density have different degrees of table
The performance of face dumb light.The present invention is based on those research discoveries and completes.Specific technical solution is as follows:
A kind of LED epoxy encapsulant with matte surface characteristic includes following components (a) to (e)
(a) epoxy resin
(b) anhydride curing agent
(c) isooctyl acid metal salt promoter
(d) DBU salt promotor
(e) inorganic filler
Wherein contain a kind of multiple functionality epoxide resin in ingredient (a) epoxy resin.The feature of this kind of multiple functionality epoxide resin
Be in strand comprising there are three or three or more epoxy groups, and epoxide equivalent is less than 150 grams/equivalent.
Component (b) anhydride curing agent can be hexahydrophthalic anhydride, methyl hexahydrophthalic anhydride, tetrahydrophthalic anhydride, in methyl tetrahydro phthalic anhydride
One or more of mixing.
Anhydride group content and the molar ratio of component (a) epoxy group mass contg are 0.3-0.8 in component (b), more preferably
For 0.5-0.7.
Component (c) isooctyl acid metal salt promoter can be zinc Isoocatanoate, calcium iso-octoate, isooctyl acid iron, stannous iso caprylate,
One or more of cobalt iso-octoate is compound.
Component (d) DBU salt promotor can be DBU phenolate, DBU caprylate, DBU tosilate, DBU formates
One or more of it is compound.
Ratio between DBU salt promotor and isooctyl acid metal salt promoter is mass ratio 3:1 to 0.5:1, preferably 2:1
To 1:1.
As described above, the present invention provides a kind of LED encapsulating epoxy resin material with matte surface effect, the present invention
Technical solution and the dependence that prior art compares inorganic filler are lower, it is only necessary to pass through resin types and feed ratio and rush
Into the regulation of agent type and additive amount, matte surface effect can be both formed.In addition, prepared by the method LED package material
Material also has excellent photopermeability and ageing-resistant performance.
Specific embodiment:
Following embodiment is for being illustrated in more details the present invention, but the present invention is not limited to these embodiments restrictions.
Embodiment 1
Firstly, using high-speed mixer by 100 parts of epoxy resin (three-glycidyl chlorinated isocyanurates), anhydride curing agent (methyl
Hexahydrophthalic anhydride) 116 parts, 1 part of isooctyl acid metal salt promoter (zinc Isoocatanoate), 2 parts of DBU salt promotor (DBU caprylate) uniformly
Simultaneously deaeration is mixed, resin adhesive liquid is obtained.
Then, 60 parts of above-mentioned glue are mixed with 40 parts of no tassement polaire (preparing spherical SiO 2) using vacuum mixer
It is even, obtain LED epoxy packages glue.The glue is placed and solidifies 4 hours at 150 DEG C to get the LED with matte surface effect is arrived
Encapsulating material.
Embodiment 2-5, compare 1-2
The composition of formula is prepared according to forming shown in table 1, in addition to this, preparation process and technological parameter with embodiment 1
It is identical.
Each be formulated after design solidifies detects matte surface effect by visual mode, and surface has obvious matte effect then to determine
It is zero；Surface has visible matte effect to be then determined as；Matte surface effect is unobvious, is determined as △；It is imitated without dumb light on surface
Fruit is then determined as ×.Specific each formula composition and condensate performance are as shown in table 1.
Table 1
It should be noted that embodiment and the code name of part material component in comparative example are indicated and are described as follows in table 1:
TGIC: three-glycidyl chlorinated isocyanurates, there are three epoxy group, 100 grams/equivalents of epoxide equivalent for intramolecular tool.
YD-128: bisphenol A type epoxy resin, bifunctionality epoxy group, 185 grams/equivalent of epoxide equivalent.
3150CE: Daicel sells polyfunctionality aliphatic epoxy resin, 150 grams/equivalent of epoxide equivalent.
MeHHPA: methyl hexahydrophthalic anhydride, the domestic universal product, no cis-trans isomerism requirement.
HHPA: hexahydrophthalic anhydride, the domestic universal product.
Inorganic filler: preparing spherical SiO 2 in embodiment, angular fused silica partial size are selected as 8 microns.
Claims (8)
1. a kind of LED epoxy encapsulant with matte surface characteristic, it is characterised in that the epoxy encapsulant includes
Following components (a) to (e) :(a) epoxy resin, (b) anhydride curing agent, (c) isooctyl acid metal salt promoter, (d) DBU salt promote
Agent, (e) inorganic filler.
2. a kind of LED epoxy encapsulant with matte surface characteristic according to claim 1, wherein component
(a) contain a kind of multiple functionality epoxide resin in epoxy resin.
3. a kind of multiple functionality epoxide resin according to claims 2, it is characterised in that in strand comprising there are three or
Three or more epoxy groups, and epoxide equivalent is less than 150 grams/equivalent.
4. a kind of LED epoxy encapsulant with matte surface characteristic according to claim 1, wherein component
(b) anhydride curing agent can be one or more of hexahydrophthalic anhydride, methyl hexahydrophthalic anhydride, tetrahydrophthalic anhydride, methyl tetrahydro phthalic anhydride
Mixing.
5. a kind of LED epoxy encapsulant with matte surface characteristic according to claim 1, it is characterised in that
Anhydride group content and the molar ratio of component (a) epoxy group mass contg are 0.3-0.8, more preferably 0.5- in component (b)
0.7。
6. a kind of LED epoxy encapsulant with matte surface characteristic according to claim 1, wherein component
(c) isooctyl acid metal salt promoter can be zinc Isoocatanoate, calcium iso-octoate, isooctyl acid iron, stannous iso caprylate, in cobalt iso-octoate
It is one or more of compound.
7. a kind of LED epoxy encapsulant with matte surface characteristic according to claim 1, wherein component
(d) DBU salt promotor can be one of DBU phenolate, DBU caprylate, DBU tosilate, DBU formates or several
Kind is compound.
8. two kinds of promotors according to claims 6-7, wherein DBU salt promotor and isooctyl acid metal salt promoter it
Between ratio be mass ratio 3:1 to 0.5:1, preferably 2:1 to 1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811059262.XA CN109294497A (en) | 2018-09-12 | 2018-09-12 | A kind of LED epoxy encapsulant with matte surface characteristic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811059262.XA CN109294497A (en) | 2018-09-12 | 2018-09-12 | A kind of LED epoxy encapsulant with matte surface characteristic |
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| CN109294497A true CN109294497A (en) | 2019-02-01 |
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| CN201811059262.XA Pending CN109294497A (en) | 2018-09-12 | 2018-09-12 | A kind of LED epoxy encapsulant with matte surface characteristic |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111471420A (en) * | 2020-04-09 | 2020-07-31 | 北京康美特科技股份有限公司 | Packaging adhesive and preparation method and application thereof |
Citations (3)
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|---|---|---|---|---|
| CN1313360A (en) * | 2000-02-04 | 2001-09-19 | 日东电工株式会社 | Epoxy resin composition and semiconductor device |
| CN106833469A (en) * | 2017-02-22 | 2017-06-13 | 深圳市新光台电子科技股份有限公司 | Anti- glare LED encapsulates glue formula and preparation method |
| US9926415B2 (en) * | 2010-08-05 | 2018-03-27 | E I Du Pont De Nemours And Company | Matte finish polyimide films and methods relating thereto |
-
2018
- 2018-09-12 CN CN201811059262.XA patent/CN109294497A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313360A (en) * | 2000-02-04 | 2001-09-19 | 日东电工株式会社 | Epoxy resin composition and semiconductor device |
| US9926415B2 (en) * | 2010-08-05 | 2018-03-27 | E I Du Pont De Nemours And Company | Matte finish polyimide films and methods relating thereto |
| CN106833469A (en) * | 2017-02-22 | 2017-06-13 | 深圳市新光台电子科技股份有限公司 | Anti- glare LED encapsulates glue formula and preparation method |
Non-Patent Citations (3)
| Title |
|---|
| 夏文干: "《胶接手册》", 28 February 1989, 国防工业出版社 * |
| 王庆等: "" 中温固化单组分环氧密封胶的研制"", 《中国胶粘剂》 * |
| 王德中: "《环氧树脂生产与应用》", 30 June 2001, 化学工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111471420A (en) * | 2020-04-09 | 2020-07-31 | 北京康美特科技股份有限公司 | Packaging adhesive and preparation method and application thereof |
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