WO2015190685A1 - Agent d'encapsulation de del comprenant des particules d'oxyde de métal terre rare - Google Patents

Agent d'encapsulation de del comprenant des particules d'oxyde de métal terre rare Download PDF

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Publication number
WO2015190685A1
WO2015190685A1 PCT/KR2015/003795 KR2015003795W WO2015190685A1 WO 2015190685 A1 WO2015190685 A1 WO 2015190685A1 KR 2015003795 W KR2015003795 W KR 2015003795W WO 2015190685 A1 WO2015190685 A1 WO 2015190685A1
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Prior art keywords
particles
led
encapsulant
light
rare earth
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PCT/KR2015/003795
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English (en)
Korean (ko)
Inventor
고다현
김영식
류정곤
임서영
원경일
박광진
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주식회사 효성
주식회사 이츠웰
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Publication of WO2015190685A1 publication Critical patent/WO2015190685A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/10—Metal compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers 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 having potential barriers 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

Definitions

  • the present invention relates to an LED encapsulant comprising rare earth metal oxide particles.
  • LED Light Emitting Diode
  • LED a light emitting device
  • LED light emitting diode
  • Increasing application of the light emitting diode (LED) due to the global energy saving trend and the development of compound semiconductor technology Is making rapid progress.
  • the LED package is largely composed of LED chips, adhesives, encapsulants, phosphors and heat dissipation accessories, among which the LED encapsulant surrounds the LED chip, thereby protecting the LED chip from external shocks and the environment.
  • the LED encapsulant since LED light must pass through the LED encapsulant in order to come out of the LED package, the LED encapsulant must have high optical transparency, that is, high light transmittance, and have a high refractive index suitable for increasing light extraction efficiency. Required.
  • Epoxy resins with high refractive index and low cost have been widely used as LED encapsulants, but epoxy resins have low heat resistance, which causes deterioration due to heat in high-power LEDs, and yellowing due to light near blue and ultraviolet rays in white light LEDs. There is a problem of lowering the luminance.
  • a silicone resin having excellent light resistance in the low wavelength region is used (the bonding energy of the siloxane bond (Si-O-Si) of the silicone resin is 106 kcal / mol, compared to the carbon-carbon (CC) bonding energy). 20 kcal / mol or more high heat resistance and excellent light resistance), the silicone resin has a low refractive index has a problem of low light extraction efficiency and weak adhesion.
  • Patent document 1 includes a polysiloxane prepolymer having a TiO 2 domain having an average domain size of less than 5 nm and contains 20 to 60 mol% of TiO 2 (based on total solids), has a refractive index of> 1.61 to 1.7, room temperature and It discloses a curable liquid polysiloxane / TiO 2 composite for use in liquid, a light emitting diode encapsulation material at atmospheric pressure.
  • Patent document 2 contains the epoxy resin and polysilazane which hardens reaction with the said epoxy resin, The composition for sealing materials of the optoelectronic device, the sealing material formed from the said composition, and the light emitting diode containing the said sealing material. It is started.
  • Patent Document 1 KR Publication 10-2012-0129788 A (2012.11.28.)
  • Patent Document 2 KR Publication 10-2012-0117548 A (2012.10.24.)
  • the first is to increase the total amount of light produced by the chip
  • the second method is to increase the so-called light extraction efficiency by extracting the generated light out of the LED as much as possible.
  • the encapsulant surrounds the LED chip, but only about 15% of the chip generated light energy is output as light, and the rest is absorbed by the encapsulant.
  • the focus of attention on the light efficiency of the LED is to improve the light extraction efficiency so that the light generated in the light emitting layer of the LED is effectively emitted to the outside without being lost by total reflection inside the LED chip.
  • the present invention is to provide an encapsulant composition that significantly improves the light extraction efficiency.
  • the present invention has been made to solve the above-mentioned problems of the prior art
  • LED encapsulation material represented by the following formula (1) in the polymer resin, the compound containing a compound having a particle size size within the range of 10 nm to 5 ⁇ m.
  • M is Sc, Y, La, Al, Lu, Ga, Zn, V, Zr, Ca, Sr, Ba, Sn, Mn, Bi, or Ac.
  • a is 1 or 2
  • b is 0-2
  • c is 0-3
  • d is 0-3.
  • b, c, and d are not zero at the same time, and b and c are zero at the same time or not zero at the same time.
  • the compound of Formula 1 is Y (OH) CO 3 It provides an LED encapsulation material, characterized in that the particle size is within the range of 100 to 1 ⁇ m.
  • the compound of Formula 1, Y 2 O 3 provides a LED encapsulation material, characterized in that the particle size is within the range of 100 to 1 ⁇ m.
  • the compound of Formula 1 provides an LED encapsulation material, characterized in that it has a refractive index within the range of 1.6 to 2.3.
  • the polymer resin is an LED bag, characterized in that at least one selected from silicone resins, phenolic resins, acrylic resins, polystyrene, polyurethane, benzoguanamine resin, and epoxy resin. Provide ash.
  • an LED encapsulation material characterized in that it further comprises phosphor particles.
  • the bar material composition of the present invention has the effect of significantly improving the light extraction efficiency of the light generated in the LED chip.
  • Y (OH) CO 3 particles having a size of 100 nm or less.
  • Y (OH) CO 3 is a SEM photograph showing rare earth oxide particles (Y (OH) CO 3 particles having a size of 1 ⁇ m or less) of the present invention.
  • 5 is a SEM photograph showing rare earth oxide particles (Y 2 O 3 particles of 500 nm or less) of the present invention.
  • 6 is a SEM photograph showing rare earth oxide particles (Y 2 O 3 particles having a size of 1 ⁇ m or less) of the present invention.
  • the present invention relates to an encapsulating resin and a rare earth metal oxide additive of an LED package having improved light extraction efficiency, and more particularly, to light to be trapped inside between the LED package chip and the encapsulant among the lights formed inside the LED package.
  • the present invention relates to a resin for LED encapsulation containing rare earth metal oxide nanoparticles showing high luminous efficiency by extraction.
  • the present invention is represented by the following formula (1) in the polymer resin, characterized in that it comprises a compound having a particle size size within the range of 10nm to 5 ⁇ m.
  • M is Sc, Y, La, Al, Lu, Ga, Zn, V, Zr, Ca, Sr, Ba, Sn, Mn, Bi, or Ac.
  • a is 1 or 2
  • b is 0-2
  • c is 0-3
  • d is 0-3.
  • b, c, and d are not zero at the same time, and b and c are zero at the same time or not zero at the same time.
  • the particle size is within the range of 10 nm to 5 ⁇ m. Although it may vary slightly depending on the wavelength or the type of particles, the light extraction efficiency may be lowered if the particle size is less than 10 nm, or more than 5 ⁇ m. In addition, although there are some differences depending on the wavelength and the type of particles, since there is an optimum range of light extraction efficiency according to the particle size, the range of particle size may be a very important configuration in terms of light extraction efficiency. A more detailed description thereof will be understood with reference to the following Examples and Experimental Examples.
  • the compound of Formula 1 is preferably Y (OH) CO 3 , or Y 2 O 3 , and more preferably Y (OH) CO 3 in view of light extraction efficiency.
  • Y (OH) CO 3 preferably Y (OH) CO 3
  • Y 2 O 3 preferably Y (OH) CO 3 in view of light extraction efficiency.
  • the compound of Formula 1 has a refractive index within the range of 1.6 to 2.3. Less than 1.6 and greater than 2.3 may not increase the light extraction efficiency. This is because the refractive index of a typical silicon encapsulant is about 1.5 and the refractive index of a GaN chip is about 2.4.
  • the total reflection problem in the light emitting device package chip occurs at the boundary between the device, external air, and silicon, which is an external encapsulant.
  • the critical angle ( ⁇ crit ) that can escape when light or waves pass between two isotropic media with different refractive indices is:
  • the polymer resin may be a polymer resin widely used in the related art, and is not particularly limited. For example, it can use 1 or more types chosen from silicone resin, a phenol resin, an acrylic resin, polystarene, a polyurethane, a benzoguanamine resin, and an epoxy resin, and the said silicone resin is polysilane, poly The siloxane and any one of these combinations may be used, and the phenolic resin may be at least one phenolic resin selected from bisphenol-type phenol resins, resol type phenol resins, and resol type naphthol resins.
  • the resin may be one that is at least one epoxy resin selected from bisphenol F-type epoxy, bisphenol A-type epoxy, phenol novolak-type epoxy, and cresol novolak-type epoxy.
  • the encapsulant composition of the present invention may further be used for the purpose of realizing a desired color by further including phosphor particles.
  • Y (OH) CO 3 particle preparation is based on 100 mL of distilled water. 2 g yttrium nitrate hydrate and 40 g urea were dissolved in 100 mL of distilled water, followed by mixing with sufficient stirring for 30 minutes. After stirring, the pH was adjusted to 5.7 to 5.8 through a base of nitric acid and ammonium hydroxide. The mixed solution was heated at 90 ° C. and stirred for 1 hour, followed by filtration and washing with distilled water three times. The washed Y (OH) CO 3 particles were dried in an oven at 70 ° C. for 3 hours to prepare particles having a size of 100 nm or less. In FIG. 1, SEM photographs of Y (OH) CO 3 particles having a size of 100 nm or less are shown.
  • Y (OH) CO 3 particle preparation is based on 100 mL of distilled water. 2 g yttrium nitrate hydrate and 40 g urea were dissolved in 100 mL of distilled water, followed by mixing with sufficient stirring for 30 minutes. After stirring, the pH was adjusted to 5.5-5.6 through a base of nitric acid and ammonium hydroxide. The mixed solution was heated at 90 ° C. and stirred for 1 hour, followed by filtration and washing with distilled water three times. The washed Y (OH) CO 3 particles were dried in an oven at 70 ° C. for 3 hours to prepare particles of 500 nm or less. In FIG. 2, SEM images of Y (OH) CO 3 particles having a size of 500 nm or less are shown.
  • Y (OH) CO 3 particle preparation is based on 100 mL of distilled water. 2 g yttrium nitrate hydrate and 40 g urea were dissolved in 100 mL of distilled water, followed by mixing with sufficient stirring for 30 minutes. After stirring, the pH was adjusted to 5.4 to 5.5 via a base of nitric acid and ammonium hydroxide. The mixed solution was heated at 90 ° C. and stirred for 1 hour, followed by filtration and washing with distilled water three times. The washed Y (OH) CO 3 particles were dried in an oven at 70 ° C. for 3 hours to prepare particles having a size of 1 ⁇ m or less. In FIG. 3, SEM images of Y (OH) CO 3 particles having a size of 1 ⁇ m or less are shown.
  • Y (OH) CO 3 particle preparation is based on 100 mL of distilled water. 2 g yttrium nitrate hydrate and 40 g urea were dissolved in 100 mL of distilled water, followed by mixing with sufficient stirring for 30 minutes. After stirring, the pH was adjusted to 5.2-5.3 through a base of nitric acid and ammonium hydroxide. The mixed solution was heated at 90 ° C. and stirred for 1 hour, followed by filtration and washing with distilled water three times. The washed Y (OH) CO 3 particles were dried in an oven at 70 ° C. for 3 hours to prepare particles having a size of 2 ⁇ m or less.
  • Y 2 O 3 particles were obtained by firing after the production of Y (OH) CO 3 .
  • Y (OH) CO 3 is based on 100 mL of distilled water. 2 g yttrium nitrate hydrate and 40 g urea were dissolved in 100 mL of distilled water, followed by mixing with sufficient stirring for 30 minutes. After stirring, the pH was adjusted to 5.7 to 5.8 through a base of nitric acid and ammonium hydroxide. The mixed solution was heated at 90 ° C. and stirred for 1 hour, followed by filtration and washing with distilled water three times. The washed Y (OH) CO 3 particles were dried in an oven at 70 ° C. for 3 hours.
  • the dried Y (OH) CO 3 particles were calcined in an oxidizing atmosphere at 900 ° C. for 3 hours to obtain Y 2 O 3 particles having a size of 100 nm or less.
  • SEM pictures of Y 2 O 3 particles having a size of 100 nm or less are shown.
  • a silicone resin a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio
  • the homogenizer was added to the homogenizer. It was put and homogenized to prepare a sealing material composition.
  • Y 2 O 3 particles were obtained by firing after the production of Y (OH) CO 3 .
  • Y (OH) CO 3 is based on 100 mL of distilled water. 2 g yttrium nitrate hydrate and 40 g urea were dissolved in 100 mL of distilled water, followed by mixing with sufficient stirring for 30 minutes. After stirring, the pH was adjusted to 5.5-5.6 through a base of nitric acid and ammonium hydroxide. The mixed solution was heated at 90 ° C. and stirred for 1 hour, followed by filtration and washing with distilled water three times. The washed Y (OH) CO 3 particles were dried in an oven at 70 ° C. for 3 hours.
  • the dried Y (OH) CO 3 particles were calcined at 900 ° C. for 3 hours to obtain Y 2 O 3 particles having a size of 500 nm or less.
  • SEM pictures of Y 2 O 3 particles having a size of 500 nm or less are shown.
  • Y 2 O 3 particles were obtained by firing after the production of Y (OH) CO 3 .
  • Y (OH) CO 3 is based on 100 mL of distilled water. 2 g yttrium nitrate hydrate and 40 g urea were dissolved in 100 mL of distilled water, followed by mixing with sufficient stirring for 30 minutes. After stirring, the pH was adjusted to 5.4 to 5.5 via a base of nitric acid and ammonium hydroxide. The mixed solution was heated at 90 ° C. and stirred for 1 hour, followed by filtration and washing with distilled water three times. The washed Y (OH) CO 3 particles were dried in an oven at 70 ° C. for 3 hours.
  • the dried Y (OH) CO 3 particles were calcined at 900 ° C. for 3 hours to obtain Y 2 O 3 particles having a size of 1 ⁇ m or less.
  • SEM pictures of Y 2 O 3 particles having a size of 1 ⁇ m or less are shown.
  • a silicone resin a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio
  • the homogenizer was added to the homogenizer. It was put and homogenized to prepare a sealing material composition.
  • Y 2 O 3 particles were obtained by firing after the production of Y (OH) CO 3 .
  • Y (OH) CO 3 was dissolved in 2 mL of yttrium nitrate hydrate and 40 g of urea in 100 mL of distilled water, followed by mixing with sufficient stirring for 30 minutes. After stirring, the pH was adjusted to 5.2-5.3 through a base of nitric acid and ammonium hydroxide. The mixed solution was heated at 90 ° C. and stirred for 1 hour, followed by filtration and washing with distilled water three times. The washed Y (OH) CO 3 particles were dried in an oven at 70 ° C. for 3 hours. The dried Y (OH) CO 3 particles were calcined at 900 ° C. for 3 hours to obtain Y 2 O 3 particles having a size of 2 ⁇ m or less.
  • a silicone resin a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio
  • the homogenizer was added to the homogenizer. It was put and homogenized to prepare a sealing material composition.
  • Silicone resin OE 6631 A and OE 6631 B were mixed at a ratio of 1: 2 to prepare a 100 wt% encapsulant composition.
  • the sealing material composition of the said Examples 1-8 and the comparative example was mounted in the LED package provided with a blue LED (wavelength 450 nm) chip, and the brightness increase rate was measured.
  • the light emitting device package used is a light emitting source using a chip connected by die bonding on a lead frame. After the metal wire bonding is performed so that the light emitting device and the lead frame are electrically connected, the transparent sealing material is molded with an encapsulant in which the silicone resin and the inorganic nanoparticles are dispersed.
  • the brightness increase rate is expressed as a percentage of the degree to which the brightness is increased based on Comparative Example 100. Luminance measurements were performed on a DARSA Pro 5200 PL System machine from Korean Professional Scientific Instrument.
  • Example 2 Example 3
  • Example 4 Example 5
  • Example 6 Example 7
  • Example 8 % Increase in brightness 100 102.3 106.4 105.9 103.1 100.5 107.1 102.7 97.6
  • the sealing material composition of the said Examples 1-8 and the comparative example was mounted in the LED package provided with the green LED (wavelength 520 nm) chip, and the brightness increase rate was measured.
  • the light emitting device package used is a light emitting source using a chip connected by die bonding on a lead frame. After the metal wire bonding is performed so that the light emitting device and the lead frame are electrically connected, the transparent sealing material is molded with an encapsulant in which the silicone resin and the inorganic nanoparticles are dispersed.
  • the brightness increase rate is expressed as a percentage of the degree to which the brightness is increased based on Comparative Example 100. Luminance measurements were performed on a DARSA Pro 5200 PL System machine from Korean Professional Scientific Instrument.
  • Example 2 Example 3
  • Example 4 Example 5
  • Example 6 Example 7
  • Example 8 % Increase in brightness 100 103.2 113.2 107.6 102.1 102.1 105.2 106.3 99.7
  • the sealing material composition of the said Examples 1-8 and the comparative example was mounted in the LED package provided with a red LED (wavelength 620 nm) chip, and the brightness increase rate was measured.
  • the light emitting device package used is a light emitting source using a chip connected by die bonding on a lead frame. After the metal wire bonding is performed so that the light emitting device and the lead frame are electrically connected, the transparent sealing material is molded with an encapsulant in which the silicone resin and the inorganic nanoparticles are dispersed.
  • the brightness increase rate is expressed as a percentage of the degree to which the brightness is increased based on Comparative Example 100. Luminance measurements were performed on a DARSA Pro 5200 PL System machine from Korean Professional Scientific Instrument.
  • Example 2 Example 3
  • Example 4 Example 5
  • Example 6 Example 7
  • Example 8 % Increase in brightness 100 100.5 102.7 106.5 105.8 101.2 102.8 102.5 103.6
  • Y 2 O 3 particles had a large increase or decrease in brightness according to the particle size of the particles, while Y (OH) CO 3 particles had a relatively low change in brightness according to the particle size. Approximately, the best brightness was shown around 100-1000 nm range.

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  • Chemical & Material Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Led Device Packages (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)

Abstract

La présente invention se rapporte à un agent d'encapsulation de DEL comprenant des particules d'oxyde de métal terre rare et, plus précisément, à un agent d'encapsulation de DEL comprenant, dans une résine de polymère, un composé représenté par la formule chimique (1) et comportant une taille des particules de 10 nm à 5 μm. La composition d'agent d'encapsulation selon la présente invention présente l'avantage d'améliorer considérablement l'efficacité d'extraction lumineuse de lumière formée dans une puce à DEL. [Formule chimique (1)] Ma(OH)b(CO3)cOd Dans la formule, M représente Sc, Y, La, Al, Lu, Ga, Zn, V, Zr, Ca, Sr, Ba, Sn, Mn, Bi ou Ac ; a vaut 1 ou 2, b vaut 0 à 2, c vaut 0 à 3 et d vaut 0 à 3 ; b, c et d ne valent pas simultanément 0 ; et b et c soit valent simultanément 0 soit ne valent pas simultanément 0.
PCT/KR2015/003795 2014-06-12 2015-04-15 Agent d'encapsulation de del comprenant des particules d'oxyde de métal terre rare WO2015190685A1 (fr)

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KR10-2014-0071511 2014-06-12
KR1020140071511A KR101599134B1 (ko) 2014-06-12 2014-06-12 희토류 금속 산화물 입자를 포함하는 led 봉지재

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070069669A (ko) * 2005-12-28 2007-07-03 (주)석경에이.티 발광다이오드의 봉지제
JP2013232279A (ja) * 2010-07-27 2013-11-14 Hitachi Ltd 封止膜およびそれを用いた有機発光ダイオード
KR20130140815A (ko) * 2010-12-08 2013-12-24 다우 코닝 코포레이션 봉지재의 형성에 적합한 실록산 조성물
KR20140034122A (ko) * 2010-12-08 2014-03-19 다우 코닝 코포레이션 봉지재의 형성에 적합한 금속 산화물 나노입자 함유 실록산 조성물

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101390281B1 (ko) 2011-04-15 2014-04-30 공주대학교 산학협력단 광전자 소자의 봉지재용 조성물, 상기 조성물로 형성한 봉지재 및 상기 봉지재를 포함하는 발광 다이오드
US8258636B1 (en) 2011-05-17 2012-09-04 Rohm And Haas Electronic Materials Llc High refractive index curable liquid light emitting diode encapsulant formulation

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070069669A (ko) * 2005-12-28 2007-07-03 (주)석경에이.티 발광다이오드의 봉지제
JP2013232279A (ja) * 2010-07-27 2013-11-14 Hitachi Ltd 封止膜およびそれを用いた有機発光ダイオード
KR20130140815A (ko) * 2010-12-08 2013-12-24 다우 코닝 코포레이션 봉지재의 형성에 적합한 실록산 조성물
KR20140034122A (ko) * 2010-12-08 2014-03-19 다우 코닝 코포레이션 봉지재의 형성에 적합한 금속 산화물 나노입자 함유 실록산 조성물

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KR101599134B1 (ko) 2016-03-03

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