WO2015190685A1 - Led encapsulant comprising rare earth metal oxide particles - Google Patents

Led encapsulant comprising rare earth metal oxide particles Download PDF

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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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particles
led
encapsulant
light
rare earth
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PCT/KR2015/003795
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French (fr)
Korean (ko)
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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/en

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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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Abstract

The present invention relates to an LED encapsulant comprising rare earth metal oxide particles, and more specifically to an LED encapsulant comprising, in a polymer resin, a compound represented by chemical formula (1) and having a particle size of 10nm-5μm. The encapsulant composition according to the present invention has the advantage of dramatically improving the light extraction efficiency of light formed in an LED chip. [Chemical formula (1)] Ma(OH)b(CO3)cOd, wherein 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, and d is 0-3. b, c and d are not simultaneously 0, and b and c are either simultaneously 0 or simultaneously not 0.

Description

희토류 금속 산화물 입자를 포함하는 LED 봉지재LED encapsulant including rare earth metal oxide particles
본 발명은 희토류 금속 산화물 입자를 포함하는 LED 봉지재에 관한 것이다.The present invention relates to an LED encapsulant comprising rare earth metal oxide particles.
발광소자인 발광다이오드(Lighting Emitting Diode: LED)는 화합물 반도체의 특성을 이용하여 전기를 적외선 또는 빛으로 변환시켜 신호를 보내고 받는데 사용되는 반도체의 일종인 발광 다이오드(LED)는, 고효율, 고속응답, 장수명, 소형화, 경량, 저소비 전력 등의 장점을 갖기 때문에, 디스플레이 장치의 백라이트, 조명 등으로의 널리 활용되고 있고, 세계적 에너지 절감 추세 및 화합물 반도체 기술발전에 따른 응용 고급화는 발광다이오드(LED)의 산업화를 빠르게 진전시키고 있다.Light Emitting Diode (LED), a light emitting device, is a type of semiconductor used to send and receive signals by converting electricity into infrared or light using characteristics of compound semiconductors. Due to its long life, small size, light weight, low power consumption, etc., it is widely used as a backlight and lighting of display devices.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.
통상적으로, LED 패키지는 크게 LED 칩, 접착제, 봉지재, 형광체 및 방열부속품 등으로 구성되는데, 이 중에서 LED 봉지재는, LED 칩을 감싸고 있어, 외부 충격과 환경으로부터 LED칩을 보호하는 역할을 한다.Typically, 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.
그런데, LED의 빛이 LED 패키지로부터 나오기 위해서는, LED 봉지재를 통과하여야 하기 때문에, LED 봉지재는 높은 광학적인 투명성 즉, 높은 광투과도를 가져야 하며, 또한 광추출 효율을 높이기에 적당한 고굴절율을 갖는 것이 요구된다.However, 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.
LED 봉지재로서 굴절율이 높고 가격이 저렴한 에폭시 수지가 널리 사용되어 왔지만, 에폭시 수지는 내열성이 낮아서 고출력 LED에서 열에 의하여 열화되는 문제가 있고, 백색광 LED에서 청색 및 자외선 부근의 광에 의하여 황변(yellowing)되어 휘도를 저하시키는 문제가 있다.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.
이에 대한 대안으로서, 저파장 영역에서 우수한 내광성을 갖는 실리콘 수지가 사용되고 있지만(실리콘 수지의 실록산 결합(Si-O-Si)의 결합 에너지는 106 kcal/mol 로서 탄소-탄소(C-C) 결합 에너지에 비하여 20 kcal/mol 이상 높아서 내열성 및 내광성이 뛰어나다), 실리콘 수지는 굴절율이 낮아 광추출 효율이 저하되고 접착성이 약한 문제가 있다.As an alternative to this, 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.
봉지재에 관한 종래의 기술은 하기 특허문헌 1 및 2의 것을 참조하여 이해할 수 있을 것이다. 이로써, 하기 특허문헌 1 및 2의 내용 전부는, 종래기술로서, 본 명세서와 합체된다.The conventional technique regarding the sealing material will be understood with reference to the following Patent Documents 1 and 2. Thereby, all the content of following patent documents 1 and 2 is integrated with this specification as a prior art.
특허문헌 1은, 평균 도메인 크기가 5 nm 미만인 TiO2 도메인을 갖는 폴리실록산 예비중합체를 포함하고 20 내지 60 mol%의 TiO2 (총 고체 기준)를 함유하며, 굴절율이 >1.61 내지 1.7이고, 실온 및 대기압에서 액체인, 발광 다이오드 봉지재로 사용하기 위한 경화성 액체 폴리실록산/TiO2 복합물에 대해 개시한다.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.
특허문헌 2는, 에폭시 수지 및 상기 에폭시 수지와 경화 반응을 하는 폴리 실라잔을 포함하는 것을 특징으로 하는 광전자 소자의 봉지재용 조성물, 상기 조성물로 형성한 봉지재 및 상기 봉지재를 포함하는 발광 다이오드에 대해 개시한다.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.
[선행기술문헌][Preceding technical literature]
[특허문헌][Patent Documents]
(특허문헌 1) KR 공개 10-2012-0129788 A (2012.11.28.)(Patent Document 1) KR Publication 10-2012-0129788 A (2012.11.28.)
(특허문헌 2) KR 공개 10-2012-0117548 A (2012.10.24.)(Patent Document 2) KR Publication 10-2012-0117548 A (2012.10.24.)
LED의 광효율을 높이기 위한 방법으로는 크게 두 가지가 있는데,There are two ways to increase the light efficiency of LED.
첫 번째는, 칩에서 생성되는 총 광량을 높이는 방법이고,The first is to increase the total amount of light produced by the chip,
두 번째는, 만들어진 광량을 최대한 LED 밖으로 뽑아내도록 하여 소위 광추출 효율을 높히는 방법이다.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.
그런데, 상술한 바와 같이, 통상적으로 LED 패키지에서, LED 칩을 봉지재가 감싸고 있는데, 칩 발생 광 에너지 중 약 15 %만이 광으로 출력되고 나머지는 봉지재 등에서 흡수되어 버리는 문제점이 있다.However, as described above, in the LED package, 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.
이에 따라, LED의 광효율에 있어서 관심이 집중되는 부분은 LED의 발광 층에서 생성된 빛이 LED 칩 내부의 전반사에 의해 손실되지 않고 효과적으로 외부로 방출되도록 광 추출 효율을 향상시키는 것이라 할 수 있다.Accordingly, 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.
현재 광량을 최대한 LED 밖으로 뽑아내도록 광추출 효율을 높이는 여러 기술들이 연구 중에 있으나, 아직도 더 나은 개선 방안이 필요한 실정이다.Currently, various techniques for increasing light extraction efficiency to extract the maximum amount of light out of the LED are being studied, but there is still a need for further improvement.
이에 본 발명은, 광추출 효율을 획기적으로 향상시키는 봉지재 조성물을 제공하고자 한다.Accordingly, the present invention is to provide an encapsulant composition that significantly improves the light extraction efficiency.
본 발명은, 상술한 종래 기술의 문제점을 해결하기 위해 안출된 것으로서,The present invention has been made to solve the above-mentioned problems of the prior art,
고분자 수지 내에 하기 화학식 1로 표현되고, 입경크기가 10 ㎚ 내지 5 ㎛ 범위 이내인 화합물을 포함하는 LED 봉지재를 제공한다.It provides an 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 ㎛.
[화학식 1][Formula 1]
Ma(OH)b(CO3)cOd M a (OH) b (CO 3 ) c O d
여기서, M은 Sc, Y, La, Al, Lu, Ga, Zn, V, Zr, Ca, Sr, Ba, Sn, Mn, Bi 또는 Ac이다.Where M is Sc, Y, La, Al, Lu, Ga, Zn, V, Zr, Ca, Sr, Ba, Sn, Mn, Bi, or Ac.
a는 1, 또는 2, b는 0 내지 2, c는 0 내지 3, d는 0 내지 3이다.a is 1 or 2, b is 0-2, c is 0-3, d is 0-3.
다만, b, c, 및 d는 동시에 0이 아니고, b 및 c는 동시에 0이거나, 동시에 0이 아니다.However, 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.
또한 본 발명에 있어서, 상기 화학식 1 화합물은, Y(OH)CO3이고, 입경크기가 100 내지 1 ㎛ 범위 이내인 것을 특징으로 하는 LED 봉지재를 제공한다.In the present invention, 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 ㎛.
또한 본 발명에 있어서, 상기 화학식 1 화합물은, Y2O3이고, 입경크기가 100 내지 1 ㎛ 범위 이내인 것을 특징으로 하는 LED 봉지재를 제공한다.In addition, in the present invention, 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 ㎛.
또한 본 발명에 있어서, 상기 화학식 1 화합물은, 1.6 내지 2.3 범위 이내의 굴절율을 가지는 것을 특징으로 하는 LED 봉지재를 제공한다.In addition, in the present invention, 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.
또한 본 발명에 있어서, 상기 고분자 수지는, 실리콘계 수지, 페놀계 수지, 아크릴 수지, 폴리스타렌, 폴리 우레탄, 벤조구아나민 수지, 및 에폭시계 수지에서 선택되어지는 1종 이상인 것을 특징으로 하는 LED 봉지재를 제공한다.In the present invention, 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.
또한 본 발명에 있어서, 형광체 입자를 더 포함하는 것을 특징으로 하는 LED 봉지재를 제공한다.In addition, in the present invention, it provides an LED encapsulation material, characterized in that it further comprises phosphor particles.
본 발명의 봉재재 조성물은, LED 칩에 생성된 빛의 광추출 효율이 획기적으로 향상시키는 효과가 있다.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.
도 1은, 본 발명의 희토류 산화물 입자(100 nm 크기 이하의 Y(OH)CO3입자) 나타낸 SEM 사진이다.1 is a SEM photograph showing rare earth oxide particles of the present invention (Y (OH) CO 3 particles having a size of 100 nm or less).
도 2는, 본 발명의 희토류 산화물 입자(500 nm 크기 이하의 Y(OH)CO3입자) 나타낸 SEM 사진이다.2 is a SEM photograph showing rare earth oxide particles (Y (OH) CO 3 particles of 500 nm or less) of the present invention.
도 3은, 본 발명의 희토류 산화물 입자(1 ㎛ 크기 이하의 Y(OH)CO3입자) 나타낸 SEM 사진이다.3 is a SEM photograph showing rare earth oxide particles (Y (OH) CO 3 particles having a size of 1 μm or less) of the present invention.
도 4은, 본 발명의 희토류 산화물 입자(100 nm 크기 이하의 Y2O3입자) 나타낸 SEM 사진이다.4 is a SEM photograph showing the rare earth oxide particles (Y 2 O 3 particles having a size of 100 nm or less) of the present invention.
도 5는, 본 발명의 희토류 산화물 입자(500 nm 크기 이하의 Y2O3입자) 나타낸 SEM 사진이다.5 is a SEM photograph showing rare earth oxide particles (Y 2 O 3 particles of 500 nm or less) of the present invention.
도 6은, 본 발명의 희토류 산화물 입자(1 ㎛ 크기 이하의 Y2O3입자) 나타낸 SEM 사진이다.6 is a SEM photograph showing rare earth oxide particles (Y 2 O 3 particles having a size of 1 μm or less) of the present invention.
도 7 내지 도 12는 Y(OH)CO3입자 및 Y2O3입자 각각의 크기에 따른 휘도 변화를 나타낸 보정 곡선(Calibration Curve)을 나타낸 것이다.7 to 12 illustrate calibration curves showing luminance changes according to sizes of Y (OH) CO 3 particles and Y 2 O 3 particles, respectively.
이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
본 발명은 광 추출 효율이 향상된 LED 패키지의 봉지용 수지와 희토류 금속 산화물 첨가물에 관한 것으로서, 더욱 상세하게는 LED 패키지 내부에서 형성된 빛들 중 LED 패키지 칩과 봉지재 사이에 내부에 갇히게 되는 빛을 외부로 추출해 냄으로써 높은 발광효율을 나타내는 희토류 금속 산화물 나노 입자를 함유하는 LED 봉지용 수지에 관한 것이다.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.
이를 위해, 본 발명은, 고분자 수지 내에 하기 화학식 1로 표현되고, 입경크기가 10㎚ 내지 5㎛ 범위 이내인 화합물을 포함하는 것을 특징으로 한다.To this end, 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㎛.
[화학식 1][Formula 1]
Ma(OH)b(CO3)cOd M a (OH) b (CO 3 ) c O d
여기서, M은 Sc, Y, La, Al, Lu, Ga, Zn, V, Zr, Ca, Sr, Ba, Sn, Mn, Bi 또는 Ac이다.Where M is Sc, Y, La, Al, Lu, Ga, Zn, V, Zr, Ca, Sr, Ba, Sn, Mn, Bi, or Ac.
a는 1, 또는 2, b는 0 내지 2, c는 0 내지 3, d는 0 내지 3이다.a is 1 or 2, b is 0-2, c is 0-3, d is 0-3.
다만, b, c, 및 d는 동시에 0이 아니고, b 및 c는 동시에 0이거나, 동시에 0이 아니다.However, 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.
상기 화학식 1 화합물이 고분자 수지 내에 포함되는 경우, 광추출 효율 측면에서 바람직하지만, 입경크기가 10 ㎚ 내지 5 ㎛ 범위 이내일 경우가 더 바람직하다. 파장이나 입자의 종류에 따라 다소 다를 수 있지만, 입경크기 10 ㎚미만이거나, 5 ㎛초과인 경우, 광추출 효율이 저하될 수 있기 때문이다. 또한, 파장이나 입자의 종류에 따라 다소의 차이는 있지만, 입경 크기에 따른 광추출 효율의 최적의 범위가 존재하기 때문에, 입경크기의 범위는 광추출 효율 측면에서 매우 중요한 구성이 될 수 있다. 이에 대한 보다 상세한 설명은, 후술할 실시예 및 실험예를 참조하여 이해할 수 있을 것이다.When the compound of Formula 1 is included in the polymer resin, it is preferable in terms of light extraction efficiency, but it is more preferable that the particle size is within the range of 10 nm to 5 ㎛. 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 ㎛. 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.
상기 화학식 1 화합물은, Y(OH)CO3, 또는 Y2O3인 것이 바람직하고, Y(OH)CO3인 것이 광추출 효율 측면에서, 더 바람직하다. 이에 대한, 보다 상세한 내용은 후술할 실시예 및 실험예를 통해 이해할 수 있을 것이다.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. In this regard, more details will be understood through the following Examples and Experimental Examples.
상기 화학식 1 화합물은, 1.6 내지 2.3 범위 이내의 굴절율을 가지는 것이 바람직하다. 1.6 미만, 2.3 초과에서는 광 추출 효율 증가 효과가 없을 수 있다. 왜냐하면, 통상적인 실리콘 봉지재의 굴절율이 약 1.5 내외이고, GaN 칩의 굴절율이 약 2.4 내외이기 때문이다.It is preferable that 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.
발광 소자 패키지 칩 내에서의 전반사 문제는 소자와 외부 공기, 외부 봉지재인 실리콘 등과의 경계에서 전반사가 발생한다. Snell's law에 따르면 빛이나 파동이 굴절률이 다른 두 등방성 매질 사이를 통과할 때 빠져나올 수 있는 임계각(θcrit)은 다음과 같다.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. According to Snell's law, the critical angle ( θ crit ) that can escape when light or waves pass between two isotropic media with different refractive indices is:
Figure PCTKR2015003795-appb-I000001
Figure PCTKR2015003795-appb-I000001
공기 (nair=1), 실리콘 (nsilicon=1.5)에 비해 GaN의 경우 굴절률이 약 2.5정도로 큰 차이가 나기 때문에 발광 소자 패키지 내에서 생성된 빛이 외부로 빠져나갈 수 있는 임계각은 각 θGaN/air= 23°, θGaN/Silicon= 37°으로 한정적이다. 이로 인해 광 추출 효율은 15 %정도 밖에 되지 않는 실정이다.Since GaN has a large refractive index difference of about 2.5 compared to air (n air = 1) and silicon (n silicon = 1.5), the critical angle at which light generated in the light emitting device package can escape to the outside is θ GaN / air = 23 ° and θ GaN / Silicon = 37 °. For this reason, the light extraction efficiency is only about 15%.
상기 고분자 수지는, 종래의 당해 기술분야에서 널리 사용되는 고분자 수지를 사용할 수 있고, 특별히 제한되지 않는다. 예를 들어, 실리콘계 수지, 페놀계 수지, 아크릴 수지, 폴리스타렌, 폴리 우레탄, 벤조구아나민 수지 및 에폭시계 수지에서 선택되어지는 1종 이상인 것을 사용할 수 있고, 상기 실리콘계 수지는, 폴리 실란, 폴리 실록산, 및 이들 조합 중 어느 하나를 사용할 수 있고, 상기 페놀계 수지는, 비스페놀형 페놀 수지, 레졸형 페놀수지, 및 레졸형 나프톨 수지에서 선택된 적어도 하나의 페놀 수지인 것을 사용할 수 있으며, 상기 에폭시계 수지는, 비스페놀 F형 에폭시, 비스페놀 A형 에폭시, 페놀 노볼락형 에폭시, 및 크레졸 노볼락형 에폭시에서 선택된 적어도 하나의 에폭시 수지인 것을 사용할 수 있다.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.
본 발명의 봉지재 조성물은, 형광체 입자를 더 포함하여 원하는 색상을 구현하는 용도로 사용될 수도 있다.The encapsulant composition of the present invention may further be used for the purpose of realizing a desired color by further including phosphor particles.
이하, 본 발명에 대하여 실시예를 들어 보다 더 상세히 설명한다. 이하의 실시예는 발명의 상세한 설명을 위한 것일 뿐, 이에 의해 권리범위를 제한하려는 의도가 아님을 분명히 해둔다.Hereinafter, the present invention will be described in more detail with reference to Examples. The following examples are only for the detailed description of the invention, it is made clear that it is not intended to limit the scope by this.
실시예Example
실시예 1Example 1
Y(OH)CO3입자 제조는 증류수 100 mL를 기준으로 한다. 증류수 100 mL에 2 g 이트륨 질산염 수화물, 40 g 우레아를 용해한 후, 30 분간 충분히 교반하면서 혼합하였다. 교반한 후, 질산과 수산화암모늄의 염기를 통해 pH를 5.7 내지 5.8로 조절하였다. 상기 혼합 용액을 90 ℃에서 가열하며 1 시간 교반한 후 여과, 증류수 세척을 3 회 실시하였다. 세척 완료된 Y(OH)CO3 입자를 70 ℃ 오븐에서 3 시간 건조하여 100 nm 크기 이하의 입자를 제조하였다. 도 1에는, 제조된 100 nm 크기 이하의 Y(OH)CO3입자 SEM 사진을 나타내었다.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.
실리콘계 수지(OE 6631 A 와 OE 6631 B를 1:2 비율로 섞은 것)에, 상기 Y(OH)CO3입자를 첨가한 후(실리콘계 수지 97 중량%, Y(OH)CO3 3 중량%), 이를 호모게나이저에 넣어 균질화 시켜 봉지재 조성물을 제조하였다.After adding the Y (OH) CO 3 particles to a silicone resin (a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio) (97 wt% of a silicone resin and 3 wt% of Y (OH) CO 3 ) , And homogenized into a homogenizer to prepare an encapsulant composition.
실시예 2Example 2
Y(OH)CO3입자 제조는 증류수 100 mL를 기준으로 한다. 증류수 100 mL에 2 g 이트륨 질산염 수화물, 40 g 우레아를 용해한 후, 30 분간 충분히 교반하면서 혼합하였다. 교반한 후, 질산과 수산화암모늄의 염기를 통해 pH를 5.5 내지 5.6으로 조절하였다. 상기 혼합 용액을 90 ℃에서 가열하며 1시간 교반한 후 여과, 증류수 세척을 3 회 실시하였다. 세척 완료된 Y(OH)CO3 입자를 70 ℃ 오븐에서 3 시간 건조하여 500 nm 크기 이하의 입자를 제조하였다. 도 2에는, 제조된 500 nm 크기 이하의 Y(OH)CO3입자 SEM 사진을 나타내었다.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.
실리콘계 수지(OE 6631 A 와 OE 6631 B를 1:2 비율로 섞은 것)에, 상기 Y(OH)CO3입자를 첨가한 후(실리콘계 수지 97 중량%, Y(OH)CO3 3 중량%), 이를 호모게나이저에 넣어 균질화 시켜 봉지재 조성물을 제조하였다.After adding the Y (OH) CO 3 particles to a silicone resin (a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio) (97 wt% of a silicone resin and 3 wt% of Y (OH) CO 3 ) , And homogenized into a homogenizer to prepare an encapsulant composition.
실시예 3Example 3
Y(OH)CO3입자 제조는 증류수 100 mL를 기준으로 한다. 증류수 100 mL에 2 g 이트륨 질산염 수화물, 40 g 우레아를 용해한 후, 30 분간 충분히 교반하면서 혼합하였다. 교반한 후, 질산과 수산화암모늄의 염기를 통해 pH를 5.4 내지 5.5으로 조절하였다. 상기 혼합 용액을 90 ℃에서 가열하며 1 시간 교반한 후 여과, 증류수 세척을 3회 실시하였다. 세척 완료된 Y(OH)CO3 입자를 70 ℃ 오븐에서 3 시간 건조하여 1 ㎛ 크기 이하의 입자를 제조하였다. 도 3에는, 제조된 1 ㎛ 크기 이하의 Y(OH)CO3입자 SEM 사진을 나타내었다.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 μm or less. In FIG. 3, SEM images of Y (OH) CO 3 particles having a size of 1 μm or less are shown.
실리콘계 수지(OE 6631 A 와 OE 6631 B를 1:2 비율로 섞은 것)에, 상기 Y(OH)CO3입자를 첨가한 후(실리콘계 수지 97 중량%, Y(OH)CO3 3 중량%), 이를 호모게나이저에 넣어 균질화 시켜 봉지재 조성물을 제조하였다.After adding the Y (OH) CO 3 particles to a silicone resin (a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio) (97 wt% of a silicone resin and 3 wt% of Y (OH) CO 3 ) , And homogenized into a homogenizer to prepare an encapsulant composition.
실시예 4Example 4
Y(OH)CO3입자 제조는 증류수 100 mL를 기준으로 한다. 증류수 100 mL에 2 g 이트륨 질산염 수화물, 40 g 우레아를 용해한 후, 30 분간 충분히 교반하면서 혼합하였다. 교반한 후, 질산과 수산화암모늄의 염기를 통해 pH를 5.2 내지 5.3으로 조절하였다. 상기 혼합 용액을 90 ℃에서 가열하며 1 시간 교반한 후 여과, 증류수 세척을 3 회 실시하였다. 세척 완료된 Y(OH)CO3 입자를 70 ℃ 오븐에서 3 시간 건조하여 2 ㎛ 크기 이하의 입자를 제조하였다. 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 μm or less.
실리콘계 수지(OE 6631 A 와 OE 6631 B를 1:2 비율로 섞은 것)에, 상기 Y(OH)CO3입자를 첨가한 후(실리콘계 수지 97 중량%, Y(OH)CO3 3 중량%), 이를 호모게나이저에 넣어 균질화 시켜 봉지재 조성물을 제조하였다.After adding the Y (OH) CO 3 particles to a silicone resin (a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio) (97 wt% of a silicone resin and 3 wt% of Y (OH) CO 3 ) , And homogenized into a homogenizer to prepare an encapsulant composition.
실시예 5Example 5
Y2O3입자 제조는 Y(OH)CO3 제조 후 소성하여 수득하였다. 먼저 Y(OH)CO3는 증류수 100 mL를 기준으로 한다. 증류수 100 mL에 2 g 이트륨 질산염 수화물, 40 g 우레아를 용해한 후, 30 분간 충분히 교반하면서 혼합하였다. 교반한 후, 질산과 수산화암모늄의 염기를 통해 pH를 5.7 내지 5.8로 조절하였다. 상기 혼합 용액을 90 ℃에서 가열하며 1 시간 교반한 후 여과, 증류수 세척을 3 회 실시하였다. 세척 완료된 Y(OH)CO3 입자를 70 ℃ 오븐에서 3 시간 건조하였다. 건조된 Y(OH)CO3입자를 산화 분위기 900 ℃에서 3 시간 소성하여 100 nm 크기 이하의 Y2O3 입자를 수득하였다. 도 4에는, 제조된 100 nm 크기 이하의 Y2O3입자 SEM 사진을 나타내었다.Y 2 O 3 particles were obtained by firing after the production of Y (OH) CO 3 . First, 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. In FIG. 4, SEM pictures of Y 2 O 3 particles having a size of 100 nm or less are shown.
실리콘계 수지(OE 6631 A 와 OE 6631 B를 1:2 비율로 섞은 것)에 Y2O3입자를 첨가한 후(실리콘계 수지 97 중량%, Y2O3 3 중량%), 이를 호모게나이저에 넣어 균질화 시켜 봉지재 조성물을 제조하였다.After adding Y 2 O 3 particles to a silicone resin (a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio) (97% by weight of a silicone resin and 3% by weight of Y 2 O 3 ), the homogenizer was added to the homogenizer. It was put and homogenized to prepare a sealing material composition.
실시예 6Example 6
Y2O3입자 제조는 Y(OH)CO3 제조 후 소성하여 수득하였다. 먼저, Y(OH)CO3는 증류수 100 mL를 기준으로 한다. 증류수 100 mL에 2 g 이트륨 질산염 수화물, 40 g 우레아를 용해한 후, 30 분간 충분히 교반하면서 혼합하였다. 교반한 후, 질산과 수산화암모늄의 염기를 통해 pH를 5.5 내지 5.6로 조절하였다. 상기 혼합 용액을 90 ℃에서 가열하며 1 시간 교반한 후 여과, 증류수 세척을 3 회 실시하였다. 세척 완료된 Y(OH)CO3 입자를 70 ℃ 오븐에서 3 시간 건조하였다. 건조된 Y(OH)CO3입자를 산화 분위기 900 ℃에서 3 시간 소성하여 500 nm 크기 이하의 Y2O3 입자를 수득하였다. 도 5에는, 제조된 500 nm 크기 이하의 Y2O3입자 SEM 사진을 나타내었다.Y 2 O 3 particles were obtained by firing after the production of Y (OH) CO 3 . First, 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. In FIG. 5, SEM pictures of Y 2 O 3 particles having a size of 500 nm or less are shown.
실리콘계 수지(OE 6631 A 와 OE 6631 B를 1:2 비율로 섞은 것)에 Y2O3입자를 첨가한 후(실리콘계 수지 97 중량%, Y2O3 3 중량%), 이를 호모게나이저에 넣어 균질화 시켜 봉지재 조성물을 제조하였다.After adding Y 2 O 3 particles to a silicone resin (a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio) (97% by weight of a silicone resin and 3% by weight of Y 2 O 3 ), the homogenizer was added to It was put and homogenized to prepare a sealing material composition.
실시예 7Example 7
Y2O3입자 제조는 Y(OH)CO3 제조 후 소성하여 수득하였다. 먼저, Y(OH)CO3는 증류수 100 mL를 기준으로 한다. 증류수 100 mL에 2 g 이트륨 질산염 수화물, 40 g 우레아를 용해한 후, 30 분간 충분히 교반하면서 혼합하였다. 교반한 후, 질산과 수산화암모늄의 염기를 통해 pH를 5.4 내지 5.5로 조절하였다. 상기 혼합 용액을 90 ℃에서 가열하며 1 시간 교반한 후 여과, 증류수 세척을 3 회 실시하였다. 세척 완료된 Y(OH)CO3 입자를 70 ℃ 오븐에서 3 시간 건조하였다. 건조된 Y(OH)CO3입자를 산화 분위기 900℃에서 3시간 소성하여 1㎛ 크기 이하의 Y2O3 입자를 수득하였다. 도 6에는, 제조된 1 ㎛ 크기 이하의 Y2O3입자 SEM 사진을 나타내었다.Y 2 O 3 particles were obtained by firing after the production of Y (OH) CO 3 . First, 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 μm or less. In FIG. 6, SEM pictures of Y 2 O 3 particles having a size of 1 μm or less are shown.
실리콘계 수지(OE 6631 A 와 OE 6631 B를 1:2 비율로 섞은 것)에 Y2O3입자를 첨가한 후(실리콘계 수지 97 중량%, Y2O3 3 중량%), 이를 호모게나이저에 넣어 균질화 시켜 봉지재 조성물을 제조하였다.After adding Y 2 O 3 particles to a silicone resin (a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio) (97% by weight of a silicone resin and 3% by weight of Y 2 O 3 ), the homogenizer was added to the homogenizer. It was put and homogenized to prepare a sealing material composition.
실시예 8Example 8
Y2O3입자 제조는 Y(OH)CO3 제조 후 소성하여 수득하였다. 먼저, Y(OH)CO3는 증류수 100 mL에 2 g 이트륨 질산염 수화물, 40 g 우레아를 용해한 후, 30 분간 충분히 교반하면서 혼합하였다. 교반한 후, 질산과 수산화암모늄의 염기를 통해 pH를 5.2 내지 5.3로 조절하였다. 상기 혼합 용액을 90 ℃에서 가열하며 1시간 교반한 후 여과, 증류수 세척을 3 회 실시하였다. 세척 완료된 Y(OH)CO3 입자를 70 ℃ 오븐에서 3 시간 건조하였다. 건조된 Y(OH)CO3입자를 산화 분위기 900 ℃에서 3 시간 소성하여 2 ㎛ 크기 이하의 Y2O3 입자를 수득하였다Y 2 O 3 particles were obtained by firing after the production of Y (OH) CO 3 . First, 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 μm or less.
실리콘계 수지(OE 6631 A 와 OE 6631 B를 1:2 비율로 섞은 것)에 Y2O3입자를 첨가한 후(실리콘계 수지 97 중량%, Y2O3 3 중량%), 이를 호모게나이저에 넣어 균질화 시켜 봉지재 조성물을 제조하였다.After adding Y 2 O 3 particles to a silicone resin (a mixture of OE 6631 A and OE 6631 B in a 1: 2 ratio) (97% by weight of a silicone resin and 3% by weight of Y 2 O 3 ), the homogenizer was added to the homogenizer. It was put and homogenized to prepare a sealing material composition.
비교예Comparative example
실리콘계 수지 OE 6631 A 와 OE 6631 B를 1:2 비율로 섞어 100 중량% 봉지재 조성물로 제조하였다.Silicone resin OE 6631 A and OE 6631 B were mixed at a ratio of 1: 2 to prepare a 100 wt% encapsulant composition.
실험예Experimental Example
실험예 1Experimental Example 1
상기 실시예 1 내지 8, 및 비교예의 봉지재 조성물을, 청색 LED(파장 450 ㎚) 칩을 구비하는 LED 패키지 내에 실장하여, 휘도 증가율을 측정하였다. 사용된 발광 소자 패키지는 리드 프레임 위에 다이 본딩으로 연결되어 있는 칩을 발광원으로 한다. 발광 소자와 리드프레임이 전기적으로 연결이 되도록 금속 와이어 본딩을 한 후, 상기 투명 봉지 재료인 실리콘 수지와 무기 나노 입자가 분산되어 있는 봉지재로 몰딩되어 있는 구성이다. 상기 휘도 증가율은 비교예 100 기준으로 휘도가 증가된 정도를 백분율로 표시한 것이다. 휘도 측정은 한국 Professional Scientific Instrument의 DARSA Pro 5200 PL System 기계에 의해 측정 하였다. 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.
결과는 하기 표 1와 같았다.The results were shown in Table 1 below.
표 1
비교예 실시예 1 실시예 2 실시예 3 실시예 4 실시예 5 실시예 6 실시예 7 실시예 8
휘도 증가율(%) 100 102.3 106.4 105.9 103.1 100.5 107.1 102.7 97.6
Table 1
Comparative example Example 1 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
실험예 2Experimental Example 2
상기 실시예 1 내지 8, 및 비교예의 봉지재 조성물을, 녹색 LED(파장 520 ㎚) 칩을 구비하는 LED 패키지 내에 실장하여, 휘도 증가율을 측정하였다. 사용된 발광 소자 패키지는 리드 프레임 위에 다이 본딩으로 연결되어 있는 칩을 발광원으로 한다. 발광 소자와 리드프레임이 전기적으로 연결이 되도록 금속 와이어 본딩을 한 후, 상기 투명 봉지 재료인 실리콘 수지와 무기 나노 입자가 분산되어 있는 봉지재로 몰딩되어 있는 구성이다. 상기 휘도 증가율은 비교예 100 기준으로 휘도가 증가된 정도를 백분율로 표시한 것이다. 휘도 측정은 한국 Professional Scientific Instrument의 DARSA Pro 5200 PL System 기계에 의해 측정 하였다. 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.
결과는 하기 표 2와 같았다.The results were as shown in Table 2 below.
표 2
비교예 실시예 1 실시예 2 실시예 3 실시예 4 실시예 5 실시예 6 실시예 7 실시예 8
휘도 증가율(%) 100 103.2 113.2 107.6 102.1 102.1 105.2 106.3 99.7
TABLE 2
Comparative example Example 1 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
실험예 3Experimental Example 3
상기 실시예 1 내지 8, 및 비교예의 봉지재 조성물을, 적색 LED(파장 620 ㎚) 칩을 구비하는 LED 패키지 내에 실장하여, 휘도 증가율을 측정하였다. 사용된 발광 소자 패키지는 리드 프레임 위에 다이 본딩으로 연결되어 있는 칩을 발광원으로 한다. 발광 소자와 리드프레임이 전기적으로 연결이 되도록 금속 와이어 본딩을 한 후, 상기 투명 봉지 재료인 실리콘 수지와 무기 나노 입자가 분산되어 있는 봉지재로 몰딩되어 있는 구성이다. 상기 휘도 증가율은 비교예 100 기준으로 휘도가 증가된 정도를 백분율로 표시한 것이다. 휘도 측정은 한국 Professional Scientific Instrument의 DARSA Pro 5200 PL System 기계에 의해 측정 하였다. 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.
결과는 하기 표 3와 같았다.The results were as shown in Table 3 below.
표 3
비교예 실시예 1 실시예 2 실시예 3 실시예 4 실시예 5 실시예 6 실시예 7 실시예 8
휘도 증가율(%) 100 100.5 102.7 106.5 105.8 101.2 102.8 102.5 103.6
TABLE 3
Comparative example Example 1 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
상기 표 1 내지 3에서 확인할 수 있듯이, 봉지재 조성물에 희토류 금속 무기 산화물 입자가 포함된 경우, 휘도가 놀라울 정도로 증가되었음을 알 수 있었다.As can be seen in Tables 1 to 3, when the rare earth metal inorganic oxide particles are included in the encapsulant composition, the brightness was surprisingly increased.
또한, Y2O3입자는 입자의 입경 크기에 따른 휘도 증감 정도가 컸지만, Y(OH)CO3입자는 입경 크기에 따른 휘도 증감 정도가 상대적으로 작았다. 대략적으로, 100~1000㎚ 범위 전후에서 가장 좋은 휘도를 나타내었다.In addition, 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.
도 7 내지 도 12는 Y(OH)CO3입자 및 Y2O3입자 각각의 크기에 따른 휘도 변화를 나타낸 보정 곡선(Calibration Curve)을 나타낸 것이다. 이 곡선을 통해 휘도 증가의 최고치를 나타는 입자의 크기 범위를 확인할 수 있었으며, 입자의 종류, 및 발광 파장에 따라, 최적의 발광효율을 낼 수 있는 크기 범위가 다소 다름을 확인할 수 있었다.7 to 12 illustrate calibration curves showing luminance changes according to sizes of Y (OH) CO 3 particles and Y 2 O 3 particles, respectively. Through this curve, it was confirmed that the size range of the particles showing the highest luminance increase, and the size range that can achieve the optimum luminous efficiency was somewhat different depending on the type of particles and the emission wavelength.

Claims (6)

  1. 고분자 수지 내에 하기 화학식 1로 표현되고, 입경크기가 10 ㎚ 내지 5 ㎛ 범위 이내인 화합물을 포함하는 LED 봉지재.An LED encapsulation material represented by the following Chemical Formula 1 in a polymer resin, the compound comprising a compound having a particle size within the range of 10 nm to 5 ㎛.
    [화학식 1][Formula 1]
    Ma(OH)b(CO3)cOd M a (OH) b (CO 3 ) c O d
    여기서, M은 Sc, Y, La, Al, Lu, Ga, Zn, V, Zr, Ca, Sr, Ba, Sn, Mn, Bi 또는 Ac이다.Where M is Sc, Y, La, Al, Lu, Ga, Zn, V, Zr, Ca, Sr, Ba, Sn, Mn, Bi, or Ac.
    a는 1, 또는 2, b는 0 내지 2, c는 0 내지 3, d는 0 내지 3이다.a is 1 or 2, b is 0-2, c is 0-3, d is 0-3.
    다만, b, c, 및 d는 동시에 0이 아니고, b 및 c는 동시에 0이거나, 동시에 0이 아니다.However, 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.
  2. 청구항 1에 있어서, 상기 화학식 1 화합물은, Y(OH)CO3이고, 입경크기가 100 내지 1 ㎛ 범위 이내인 것을 특징으로 하는 LED 봉지재.The LED encapsulant of claim 1, wherein the compound of Formula 1 is Y (OH) CO 3 and has a particle size of 100 to 1 µm.
  3. 청구항 1에 있어서, 상기 화학식 1 화합물은, Y2O3이고, 입경크기가 100 내지 1 ㎛ 범위 이내인 것을 특징으로 하는 LED 봉지재.The LED encapsulant of claim 1, wherein the compound of Formula 1 is Y 2 O 3 and has a particle size of 100 to 1 µm.
  4. 청구항 1에 있어서, 상기 화학식 1 화합물은, 1.6 내지 2.3 범위 이내의 굴절율을 가지는 것을 특징으로 하는 LED 봉지재.The LED encapsulant of claim 1, wherein the compound of Formula 1 has a refractive index within a range of 1.6 to 2.3.
  5. 청구항 1에 있어서, 상기 고분자 수지는, 실리콘계 수지, 페놀계 수지, 아크릴 수지, 폴리스타렌, 폴리 우레탄, 벤조구아나민 수지, 및 에폭시계 수지에서 선택되어지는 1종 이상인 것을 특징으로 하는 LED 봉지재.The LED encapsulation material according to claim 1, wherein the polymer resin is at least one selected from silicone resins, phenolic resins, acrylic resins, polystarenes, polyurethanes, benzoguanamine resins, and epoxy resins. .
  6. 청구항 1에 있어서, 형광체 입자를 더 포함하는 것을 특징으로 하는 LED 봉지재.The LED encapsulation material according to claim 1, further comprising phosphor particles.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070069669A (en) * 2005-12-28 2007-07-03 (주)석경에이.티 Molding compound for light emitting diode
JP2013232279A (en) * 2010-07-27 2013-11-14 Hitachi Ltd Sealing film and organic light-emitting diode using the same
KR20130140815A (en) * 2010-12-08 2013-12-24 다우 코닝 코포레이션 Siloxane compositions suitable for forming encapsulants
KR20140034122A (en) * 2010-12-08 2014-03-19 다우 코닝 코포레이션 Siloxane compositions including metal-oxide nanoparticles suitable for forming encapsulants

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KR101390281B1 (en) 2011-04-15 2014-04-30 공주대학교 산학협력단 Composition for encapsulation material of photoelectronic device, encapsulation material made from the composition and light emitting diode comprising the encapsulation material
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 (en) * 2005-12-28 2007-07-03 (주)석경에이.티 Molding compound for light emitting diode
JP2013232279A (en) * 2010-07-27 2013-11-14 Hitachi Ltd Sealing film and organic light-emitting diode using the same
KR20130140815A (en) * 2010-12-08 2013-12-24 다우 코닝 코포레이션 Siloxane compositions suitable for forming encapsulants
KR20140034122A (en) * 2010-12-08 2014-03-19 다우 코닝 코포레이션 Siloxane compositions including metal-oxide nanoparticles suitable for forming encapsulants

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