KR20130106587A - Composition for encapsulating light emitting device and light emitting device - Google Patents
Composition for encapsulating light emitting device and light emitting device Download PDFInfo
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Abstract
Description
The present invention relates to a composition for a light emitting device encapsulation material and a light emitting device, and more particularly, to form a light emitting device encapsulation material with a composition comprising a curable resin, a block copolymer dispersant and nanoparticles, thereby coupling the nanoparticles to a phosphor. The present invention relates to a light emitting device encapsulating material composition and a light emitting device that significantly improve light emitting efficiency by reducing light scattered by an effect, and improve light transmittance, heat resistance, and durability.
The light emitting device has low power consumption, long life, can be installed in a narrow space, has a fast response speed, and has strong vibration resistance. Such light emitting devices are being used as backlights for display devices, and active research is being conducted to apply them to general lighting applications.
The light emitting device package is mainly composed of a substrate, a light emitting device chip, an adhesive, an encapsulant, a phosphor, and a heat dissipation accessory. Among them, the light emitting device encapsulant protects the light emitting device chip from external impact and the environment. Since the light of the light emitting device in the light emitting device package passes through the light emitting device encapsulant, the light emitting device encapsulant must have optical transparency, that is, have a high light transmittance, and also has a high refractive index to increase the light extraction efficiency Is required.
In general, in order to improve the luminous efficiency of the light emitting device, a method of improving the luminous efficiency by forming a reflective layer on the back surface of the light emitting device chip or adding phosphor or inorganic particles to the encapsulant has been studied.
However, when the phosphor or inorganic particles are added to the encapsulant, the phosphor or inorganic particles having a higher specific gravity sink to the lower part due to the difference in specific gravity with the encapsulant resin having a relatively low specific gravity. As such, due to precipitation of the phosphor or the inorganic particles, the phosphor or the inorganic particles are unevenly distributed in the encapsulation material, thereby decreasing the color uniformity and decreasing the transmittance. That is, the light emitted from the light emitting device chip is not uniform and color staining may occur, causing problems in color reproducibility, and since the phosphor is not uniformly distributed in the molding part, the color of light emitted at each viewing angle of the light emitting device. This results in a different problem.
Korean Patent Laid-Open Publication No. 2009-0127885 (Patent Document 1) added a silica having an average particle diameter of 1 to 30 nm to a silicon composition for encapsulating a light emitting device to produce a light emitting device by utilizing the encapsulant for a light emitting device. In 2005-0096993 (Patent Document 2), a liquid encapsulant for a light emitting device package and a light emitting device package including the same were prepared by adding a fine particle conductor having excellent reflectance.
In the conventional light emitting device encapsulant and the light emitting device including the same, when particles are included, the luminous efficiency and transmittance of the light emitting device are lowered because they are not uniformly dispersed in the encapsulant, and the light emitting device is continuously maintained. Due to heat and light generated as a problem, such as durability is poor.
The present invention is to solve the conventional problems, by forming a light emitting device encapsulating material with a composition comprising a curable resin, a block copolymer dispersant and nanoparticles, reducing the light scattered by the coupling effect of the nanoparticles and the phosphor. The purpose of the present invention is to increase the luminous efficiency of a light emitting device, and to provide a light emitting device encapsulant composition with improved light transmittance, heat resistance, and durability.
In addition, an object of the present invention is to provide a light emitting device including an encapsulant manufactured from the light emitting device encapsulant composition.
According to the present invention for achieving the above object, it is characterized by providing a composition for a light emitting device encapsulant comprising a curable resin, a block copolymer dispersant and nanoparticles.
The block copolymer dispersant is characterized in that any one or more selected from the following formula (1).
[Formula 1]
(In
The molecular weight of (A) of Formula 1 is 500 to 50,000, characterized in that the molecular weight of (B) is 500 to 100,000.
In addition, the nanoparticles are titanium (Ti), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), zinc (Zn), zirconium (Zr) , A compound comprising a metal component selected from molybdenum (Mo), tungsten (W), palladium (Pd), indium (In), tin (Sn), platinum (Pt), silver (Ag), gold (Au) or Polyethylene glycol or polyvinylpyrrolidone is bonded to the nanoparticle precursor selected from the mixture thereof, and the average particle diameter is 2 to 10,000 nm.
In addition, the curable resin is characterized in that it comprises a curable epoxy resin or a curable silicone resin.
The epoxy resin is bisphenol A epoxy resin, bisphenol type epoxy resin, bisphenol S type epoxy resin, phenol novolac type epoxy resin, cresol novolac type epoxy resin, biphenyl type epoxy resin, triphenylmethane type epoxy resin,
In the light emitting device encapsulant composition, the nanoparticles and the block copolymer dispersant are included in a weight ratio of 1: 0.001 to 0.001: 1, and based on 100 parts by weight of the curable resin, 0.01 to 10 parts by weight of the block copolymer dispersant and nanoparticles It comprises 0.01 to 10 parts by weight.
In addition, the light emitting device encapsulation composition is characterized in that it further comprises a curing agent, antioxidant, flame retardant, plasticizer, ultraviolet absorber.
In addition, the substrate; Light emitting structure; electrode; And an encapsulant including a curable resin, a block copolymer dispersant, and nanoparticles, wherein the block copolymer dispersant is any one or more selected from
[Formula 1]
(In
According to the light emitting device encapsulation composition and the light emitting device of the present invention, by forming a light emitting device encapsulation material with a composition comprising a curable resin, a block copolymer dispersant and nanoparticles, the light scattered by the coupling effect of the nanoparticles and the phosphor By increasing the luminous efficiency of the light emitting device to increase, there is an advantage that the light transmittance, heat resistance, durability is significantly improved.
1 is a graph of the NMR measurement of the product of
2 is a GPC measurement graph of the first step product of Preparation Example 1 of the present invention, Figure 3 is a GPC measurement graph of the three step product of Preparation Example 1 of the present invention.
Figure 4 is a SEM image of the nanoparticles of Preparation Example 2 of the present invention.
Hereinafter, the preferred embodiment and the physical property measuring method of the light emitting device encapsulant composition and the light emitting device of the present invention will be described in detail. The invention can be better understood by the following examples, which are intended for purposes of illustration of the invention and are not intended to limit the scope of protection defined by the appended claims.
The light emitting device encapsulant composition of the present invention includes a curable resin, a block copolymer dispersant and nanoparticles.
It is preferable that the curable resin is a curable polymer that forms a three-dimensional cured structure by applying light or heat, and it is particularly effective to include a curable epoxy resin or a curable silicone resin.
For example, as curable epoxy resin, bisphenol-A epoxy resin, bisphenol-type epoxy resin, bisphenol S-type epoxy resin, phenol novolak-type epoxy resin, cresol novolak-type epoxy resin, biphenyl type epoxy resin, and triphenylmethane type Epoxy resin, stilbene type epoxy resin, hydroquinone type epoxy resin, phenol aralkyl type epoxy resin, aliphatic epoxy resin, glycidyl ether type epoxy resin, bicyclic epoxy resin, naphthalene type epoxy resin or brominated epoxy resin thereof It is preferable that it is one kind or two or more kinds, in particular poly (bisphenol A-epichlorohydrin), bisphenol A diglycidyl ether, bisphenol F diglycidyl ether or novolac, but is not limited thereto. no.
It is preferable that the molecular weight of the said epoxy resin is 300-100,000, More preferably, it is effective that it is 500-20000.
In addition, the curable silicone resin is preferably one or two or more selected from a phenyl-based silicone resin, a methyl-based silicone resin, and an epoxy-modified silicone resin, and particularly, polydimethylsiloxane or polydiphenylsiloxane is effective, but is not limited thereto. It doesn't happen.
The molecular weight of the silicone resin is preferably 300 to 100,000, more preferably 500 to 20,000.
The block copolymer dispersant of the present invention is added to uniformly disperse the nanoparticles in the curable resin, characterized in that any one or more selected from the following formula (1).
[Formula 1]
(In
It is preferable that the molecular weight of (A) of Formula 1 is 500-50,000, the molecular weight of (B) is 500-100,000, More preferably, the molecular weight of (A) is 1,000-20,000, and the molecular weight of (B) is 1,000 It is effective that it is to 50,000.
When the molecular weights of (A) and (B) of
When the molecular weight of (A) or (B) in the formula (1) is less than 500 may cause a problem of poor dispersion stability, when the molecular weight of (A) is greater than 50,000 or the molecular weight of (B) is more than 100,000 the viscosity is The problem may arise because of high processability.
In addition, the nanoparticles reduce the scattered light by using the coupling effect generated between the phosphors of the light emitting device to increase the luminous efficiency of the light emitting device, improve the transmittance, improve the mechanical properties to improve heat resistance and durability It is added to make. The nanoparticles are titanium (Ti), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), zinc (Zn), zirconium (Zr), molybdenum (Mo), a compound containing a metal component selected from tungsten (W), palladium (Pd), indium (In), tin (Sn), platinum (Pt), silver (Ag), gold (Au), or a combination thereof Polyethylene glycol or polyvinylpyrrolidone is preferably bonded to the nanoparticle precursor selected from the mixture.
It is preferable that the average particle diameter of the said nanoparticle is 2-10,000 nm, It is especially effective that it is 5-11,000 nm. When the average particle diameter of the nanoparticles is in the above numerical range, dispersion stability is good and there is an advantage of maximizing luminous efficiency. When the average particle diameter of the nanoparticles is less than 2 nm, a problem of deterioration of luminous efficiency due to the small size may occur. And, if it is more than 1,000nm may cause a problem that the luminous efficiency is lowered by light scattering.
In addition, the nanoparticles and the block copolymer dispersant in the light emitting device encapsulant composition are preferably included in a weight ratio of 1: 0.001 to 0.001: 1, more preferably 1: 0.01 to 0.01: 1 by weight. effective.
When the nanoparticles and the block copolymer dispersant have the weight ratio, the nanoparticles are effectively and stably dispersed in the curable resin.
In addition, it is preferable to contain 0.01 to 10 parts by weight of the block copolymer dispersant and 0.01 to 10 parts by weight of the nanoparticles based on 100 parts by weight of the curable resin.
The optimal amount of block copolymer dispersant and nanoparticles are included in the curable resin, thereby increasing the coupling effect generated between the phosphors of the light emitting device and reducing scattered light, thereby increasing the luminous efficiency of the light emitting device and improving the transmittance. It is improved, and mechanical properties are improved to significantly improve heat resistance and durability.
In addition, the light emitting device encapsulant composition is further effective to further include a curing agent, antioxidant, flame retardant, plasticizer, ultraviolet absorber.
The curing agent may be used without limitation as long as it is a known curing agent capable of curing the curable resin, and particularly, an acid anhydride or an amine curing agent may be exemplified. The acid anhydride is preferably selected from phthalic anhydride, hexahydrophthalic anhydride, tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, and the amine curing is a first (R-NH2) amine, a second (R-NH-R) It is preferred that the amine, the third (R3-N) amine, Monoamine, Diamine, Polyamine, Aliphatic amine, Aromatic amine is not limited thereto.
It is preferable to add 0.01-20 weight part of said hardening | curing agents with respect to 100 weight part of compositions for light emitting element sealing materials, More preferably, 0.1-10 weight part is effective. When the content of the curing agent is in the above range, there is an advantage that the encapsulant formed of the composition is not broken and maintains high thermal stability and durability.
In addition, the present invention provides a semiconductor device comprising a substrate; Light emitting structure; electrode; And an encapsulant including a curable resin, a block copolymer dispersant, and nanoparticles, wherein the block copolymer dispersant is any one or more selected from
[Formula 1]
(In
Hereinafter, a method of measuring physical properties of a light emitting device encapsulation material according to Examples and Comparative Examples of the present invention will be described in detail, and the measurement results are shown in Table 1 below.
Property measurement
1) Transmittance Measurement
The transmittance was measured using a UV-Vis Spectrophotometer (ultraviolet-visible spectrophotometer) at a wavelength of 300 nm to 1000 nm with 0.1 nm resolution.
2) Heat resistance measurement
Heat resistance measurement was compared by measuring the transmittance before and after the heat treatment for 1 hour at 190 ℃.
3) refractive index measurement
The refractive index of the film was measured using an Abbe refractometer.
[Production Example 1]
Block copolymer Preparation of dispersant
Step 1) Install a mechanical stirrer in a three-necked flask, fill with water and ice, and 50 ml of polyethylene glycol monomethyl ether (PEG5000-OH, Poly (ethylene glycol) methyl ether, average Mn 5,000, Aldrich) in 100 ml of dichloromethane. 2 ml of pyridine is added and stirred for a while. 2.40 ml of 2-bromopropionyl bromide (97%, Aldrich) is slowly added dropwise and further stirred at room temperature for 16 hours. Thereafter, 300 ml of dichloromethane was further added, and washed four times with 40 ml of saturated ammonium chloride, 50 ml of sodium bicarbonate and 50 ml of water. The remaining water is removed with magnesium sulfate and the solvent is blown off in vacuo.
Step 2) Install a mechanical stirrer in the three-necked flask, add 20 ml of dichloromethane and 4.20 ml of pyridine, potassium ethyl xanthate, DITHIOCARBONIC ACID O-ETHYL ESTER, POTASSIUM SALT DIMER , Aldrich) is added and stirred for 16 hours at room temperature. Thereafter, 140 ml of dichloromethane was further added, washed four times with 40 ml of saturated ammonium chloride, 50 ml of sodium bicarbonate and 50 ml of water, the remaining water was removed with magnesium sulfate, and the solvent was extracted with Soxhlet. .
3 steps) 2.0 g N-vinylpyrrolidone (1-Vinyl-2-pyrrolidinone, Aldrich), AIBN (Azobisisobutyronitrile, 0.2 M (solvent: toluene), Aldrich) 0.1 ml, 2-step product 0.21 g and THF (TetraHydroFuran, Aldrich) 3g was immersed in a 60 ℃ oil bath in a shrink flask and stirred for 15 hours in a vacuum to obtain a PEG-PVP block copolymer dispersant. NMR (FT-NMR Spectrometer, JNM-AL400, room temperature, D 2 O) was measured for the first step product and the third step product, and a graph is shown in FIG. 1, and molecular weights are shown in FIGS. 2 and 3.
[Production Example 2]
Preparation of Nanoparticles
5 ml of anhydrous ethylene glycol (99.8%, Aldrich) was prepared by heating to 160 ° C. for 1 hour, and 3 ml of silver nitrate solution (Aldrich, 99%) diluted in 0.25M ethylene glycol and polyvinylpyrrolidone diluted in 0.375M ethylene glycol 3 ml of the solution (PVP Mw = 55,000, Aldrich) were simultaneously added to anhydrous ethylene glycol prepared by heating at a flow rate of 0.375 ml / min. The mixture was further stirred for 45 min at 160 ° C. to prepare nanoparticles, washed thoroughly with water, filtered with 1 μm Nucleopore membranes (Whatman, Clifton, NJ), centrifuged and redispersed in water. It was prepared and confirmed by taking an SEM image, which is shown in FIG.
Example 1
1 g of the block copolymer dispersant prepared in Preparation Example 1, 1 g of the silver nanoparticles prepared in Preparation Example 2, and 5 g of the phosphor (CY-012, Comtech) were added to 100 g of silicone resin (OE6630, Dow corning), and 120 to 2 It was prepared in a coating film by curing for a time, and the physical property measurement results are shown in Table 1 below.
[Example 2]
1 g of the block copolymer dispersant prepared in Preparation Example 1, 1 g of the silver nanoparticles prepared in Preparation Example 2, 5 g of a phosphor (CY-012, Comtech) in 100 g of epoxy resin (Bisphenol A diglycidylether, Aldrich) (1- (2) -aminoethyl) piperazine, Aldrih) 1g was added, and cured at 120 to 30 minutes and 60 to 2 hours to prepare a coating film. The results of the measurement of the physical properties are shown in Table 1 below.
Comparative Example 1
To 100 g of silicone resin (OE6630, Dow corning) was added 1g of silver nanoparticles prepared in Preparation Example 2, 5g of phosphor (CY-012, Comtech), and cured at 120 for 2 hours to prepare a coating film. Table 1 shows.
Comparative Example 2
To 100 g of epoxy resin (Bisphenol A diglycidylether, Aldrich), 1 g of silver nanoparticles prepared in Preparation Example 2, 5 g of phosphor (CY-012, Comtech), and 1 g of a hardener (1- (2-aminoethyl) piperazine, Aldrih) were added thereto. 30 minutes, and cured at 60 for 2 hours to prepare a coating film, the physical properties are shown in Table 1 below.
[Comparative Example 3]
5 g of a phosphor (CY-012, Comtech) was added to 100 g of a silicone resin (OE6630, Dow corning), and cured at 120 for 2 hours to prepare a coating film. The results of the measurement of the physical properties are shown in Table 1 below.
[Table 1]
Figure 1 is a graph measuring the NMR of the product after
In addition, Figure 4 is a SEM image of the nanoparticles prepared in Preparation Example 2, it can be confirmed that the uniform nanoparticles were formed.
The block copolymer dispersant and the nanoparticles prepared as described above are added to the curable resin to prepare an encapsulant for the light emitting material, thereby improving transmittance, heat resistance, and refractive index, as shown in Table 1 above.
While the present invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the invention.
Claims (11)
The block copolymer dispersant is a composition for a light emitting device encapsulation material, characterized in that any one or more selected from the following formula (1).
[Formula 1]
(In Formula 1, (A), (B) are each independently one or two selected from ethylene glycol, vinylpyrrolidone, ethylene oxide, wherein n, m are each independently a natural number of 1 to 5,000 to be.)
The molecular weight of (A) of Formula 1 is 500 to 50,000, the molecular weight of (B) is 500 to 100,000 composition for a light emitting device sealing material, characterized in that.
The nanoparticles are titanium (Ti), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), zinc (Zn), zirconium (Zr), molybdenum (Mo), a compound containing a metal component selected from tungsten (W), palladium (Pd), indium (In), tin (Sn), platinum (Pt), silver (Ag), gold (Au), or a combination thereof The composition for light-emitting device encapsulant, characterized in that polyethylene glycol or polyvinylpyrrolidone is bonded to the nanoparticle precursor selected from the mixture.
The light emitting device encapsulation composition, characterized in that the average particle diameter of the nanoparticles is 2 to 10,000nm.
The curable resin is a composition for a light emitting device encapsulation material comprising a curable epoxy resin or a curable silicone resin.
The epoxy resin is bisphenol A epoxy resin, bisphenol type epoxy resin, bisphenol S type epoxy resin, phenol novolac type epoxy resin, cresol novolac type epoxy resin, biphenyl type epoxy resin, triphenylmethane type epoxy resin, stilbene type 1 type, or 2 or more types chosen from an epoxy resin, a hydroquinone type epoxy resin, a phenol aralkyl type epoxy resin, an aliphatic epoxy resin, a glycidyl ether type epoxy resin, a bicyclic epoxy resin, or a naphthalene type epoxy resin, The said silicone resin The composition for light-emitting device encapsulant, characterized in that one or two or more selected from phenyl-based silicone resin, methyl-based silicone resin, epoxy-modified silicone resin.
The nanoparticles and the block copolymer dispersant in the composition for a light emitting device encapsulant comprising a weight ratio of 1: 0.001 to 0.001: 1.
A composition for light-emitting device encapsulant, comprising 0.01 to 10 parts by weight of a block copolymer dispersant and 0.01 to 10 parts by weight of nanoparticles, based on 100 parts by weight of the curable resin.
The light emitting device encapsulant composition further comprises a curing agent, antioxidant, flame retardant, plasticizer, ultraviolet absorber composition for a light emitting device encapsulation material.
The block copolymer dispersant is a light emitting device, characterized in that any one or more selected from the following formula (1).
[Formula 1]
(In Formula 1, (A), (B) are each independently one or two selected from ethylene glycol, vinylpyrrolidone, ethylene oxide, wherein n, m are each independently a natural number of 1 to 5,000 to be.)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016010216A1 (en) * | 2014-07-15 | 2016-01-21 | 주식회사 포스코 | Flexible encapsulation material for encapsulating organic electronic element, organic electronic element encapsulated by same, and method for encapsulating organic electronic element |
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| KR20050096993A (en) | 2004-03-30 | 2005-10-07 | 삼성전기주식회사 | Epoxy molding compound used in led package for absorbing static electricity and led package comprising the same |
| KR20070110257A (en) * | 2004-11-16 | 2007-11-16 | 나노크리스탈 라이팅 코포레이션 | Optically reliable nanoparticle based nanocomposite hri encapsulant and photonic waveguiding material |
| JP2009529091A (en) * | 2006-03-08 | 2009-08-13 | スリーエム イノベイティブ プロパティズ カンパニー | Polymer composites |
| KR20090127885A (en) | 2007-03-19 | 2009-12-14 | 산유 레크 가부시키가이샤 | Silicone resin composition for encapsulating luminescent element and process for producing optical-semiconductor electronic part with the same through potting |
| JP2010535278A (en) * | 2007-08-02 | 2010-11-18 | ダウ グローバル テクノロジーズ インコーポレイティド | Amphiphilic block copolymers and inorganic nanofillers for improving the performance of thermosetting polymers |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050096993A (en) | 2004-03-30 | 2005-10-07 | 삼성전기주식회사 | Epoxy molding compound used in led package for absorbing static electricity and led package comprising the same |
| KR20070110257A (en) * | 2004-11-16 | 2007-11-16 | 나노크리스탈 라이팅 코포레이션 | Optically reliable nanoparticle based nanocomposite hri encapsulant and photonic waveguiding material |
| JP2009529091A (en) * | 2006-03-08 | 2009-08-13 | スリーエム イノベイティブ プロパティズ カンパニー | Polymer composites |
| KR20090127885A (en) | 2007-03-19 | 2009-12-14 | 산유 레크 가부시키가이샤 | Silicone resin composition for encapsulating luminescent element and process for producing optical-semiconductor electronic part with the same through potting |
| JP2010535278A (en) * | 2007-08-02 | 2010-11-18 | ダウ グローバル テクノロジーズ インコーポレイティド | Amphiphilic block copolymers and inorganic nanofillers for improving the performance of thermosetting polymers |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016010216A1 (en) * | 2014-07-15 | 2016-01-21 | 주식회사 포스코 | Flexible encapsulation material for encapsulating organic electronic element, organic electronic element encapsulated by same, and method for encapsulating organic electronic element |
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