WO2017116000A1 - Method for manufacturing transparent ceramic phosphor plate - Google Patents

Method for manufacturing transparent ceramic phosphor plate Download PDF

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Publication number
WO2017116000A1
WO2017116000A1 PCT/KR2016/012929 KR2016012929W WO2017116000A1 WO 2017116000 A1 WO2017116000 A1 WO 2017116000A1 KR 2016012929 W KR2016012929 W KR 2016012929W WO 2017116000 A1 WO2017116000 A1 WO 2017116000A1
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transparent ceramic
phosphor
plate
present
pulverized
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PCT/KR2016/012929
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French (fr)
Korean (ko)
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이상준
정몽권
김영식
이성훈
손원배
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주식회사 효성
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
    • H01L33/50—Wavelength conversion elements
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/02—Details
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources

Definitions

  • the present invention relates to a method for producing a phosphor transparent ceramic plate. More specifically, the present invention relates to a method for producing a phosphor transparent ceramic plate which is simple in manufacturing and can improve product yield.
  • the term 'LED' used in the present specification is an abbreviation of light emitting diode (Light Emitting Diode) to generate a small number of carriers (electron or electric) injected by using a semiconductor pn junction structure, and emit light by recombination thereof Means a diode.
  • Light Emitting Diode Light Emitting Diode
  • 'LD' is an abbreviation for laser diode, which means a laser diode made of a semiconductor that uses electrons and electrons to emit light when the carrier and electrons recombine over energy. do.
  • An optical semiconductor device such as an LED device or an LD irradiation device includes, for example, an optical semiconductor element such as an LED element or an LD, and a phosphor layer disposed on the optical semiconductor element.
  • Such an optical semiconductor device emits white light by emitting light from an optical semiconductor element, that is, a mixture of blue light transmitted through a phosphor layer and yellow light in which part of blue light is wavelength-converted in the phosphor layer.
  • Such an optical semiconductor device has a mainstream LED device including an LED package in which an LED is encapsulated with a transparent encapsulation material, and a fluorescent tape laminated on an upper surface thereof, and the fluorescent tape is an acrylic layer laminated on a fluorescent layer and a back surface thereof.
  • the pressure-sensitive adhesive layer is provided and the fluorescent layer is attached to the surface of the LED package through the adhesive layer, the fluorescent tape tends to deteriorate due to the high temperature accompanying the light emission of the LED, thereby causing a problem that the luminance of the LED device is lowered.
  • the phosphor layer is formed from the ceramic of the phosphor to the ceramic plate of the phosphor in the phosphor adhesive sheet.
  • raw material powder is prepared from yttrium oxide, aluminum oxide, and garnet oxide particles, and the prepared raw material powder is mixed with a water-soluble binder resin, and further distilled water is added to wet mix and fire.
  • Yttrium-Aluminum-Garnet (hereinafter referred to as 'YAG') precursor was produced through the steps, followed by oven drying, forming a ceramic green sheet, and then heating the ceramic green sheet laminate to obtain a high temperature vacuum.
  • Phosphor transparent ceramic plates have been produced by heating and firing in a furnace. In this case, however, the final plate manufacturing takes a long time, and there is a problem in product yield.
  • the present invention has been completed by the present invention was found that the production method is simple and the product yield can also be improved by fabricating using a conventional solid phase method when producing a transparent ceramic plate after pulverizing the YAG phosphor.
  • the phosphor transparent ceramic plate is characterized in that the small particles of the YAG phosphor is pulverized to 1 ⁇ m or less, and then manufactured by forming (molding) and firing.
  • the manufacturing method of the phosphor transparent ceramic plate of the present invention it is possible to minimize the complex process, excellent thickness uniformity of the plate by precision surface processing, high color contrast of 100: 1 or more and at the same time can realize a low color dispersion, heat It can reduce color coordinate shift, have excellent luminescence uniformity, solve binning problem through fluorescent screen in the pre-mounting stage of the plate, and apply high power light emitting diode (LED) and laser diode (LD) There is an effect that can ensure the stability and reliability at the time.
  • LED light emitting diode
  • LD laser diode
  • FIG. 1 is a manufacturing process chart of a transparent ceramic plate according to the present invention.
  • FIG. 2 is a manufacturing process chart of a conventional transparent ceramic plate.
  • 3 is YAG powder particle size distribution data using a particle size analyzer before grinding.
  • FIG. 5 is a spectral comparison graph according to cesium concentration between the transparent ceramic plate according to the present invention and the transparent ceramic plate manufactured by the conventional method (FIG. 2).
  • the phosphor transparent ceramic plate comprises the steps of milling small particles of YAG phosphor by milling to 1 ⁇ m or less as illustrated in FIG. 1; Drying the pulverized YAG phosphor in an oven; Pressurizing the dry pulverized YAG phosphor to form a plate; and firing and post-processing the formed plate.
  • the step of pulverizing the YAG phosphor is preferably pulverized by milling using a ball mill, and if it is not pulverized to 1 ⁇ or less, the thickness of the plate becomes uneven, and eventually, a high power light emitting diode ( LED) and laser diode (LD) will not be able to secure stability and reliability.
  • Figure 3 shows the YAG powder particle size distribution data using a particle size analyzer before grinding
  • Figure 4 shows the YAG powder particle size distribution data using a particle size analyzer after grinding.
  • the step of drying the pulverized YAG phosphor in an oven is preferably carried out for 1 to 24 hours in the temperature range of 100 to 150 °C.
  • the step of applying the pressure is preferably carried out within a pressure range of 1,000 Mpa to 3,000 Mpa by using a cooling isotropic pressurization (CIP).
  • CIP cooling isotropic pressurization
  • the firing step is preferably carried out within a range of 8 to 15 hours at a temperature range of 1400 to 1800 °C in reducing or air using an atmosphere furnace.
  • the post-treatment of the fired transparent ceramic plate may be performed by surface polishing using an automatic polishing machine as a surface polishing process.
  • FIG. 5 is a view comparing spectra according to cesium concentration between the transparent ceramic plate according to the present invention and the transparent ceramic plate manufactured by the conventional method (FIG. 2).

Abstract

The present invention is to provide a method for manufacturing a transparent ceramic phosphor plate, which is not only simple, but can also improve product yield. The solution of the present invention comprises the steps of: pulverizing a YAG phosphor to be smaller than or equal to 1 µm by milling; drying the pulverized YAG phosphor in an oven; pressurizing the dried pulverized YAG phosphor to mold the same into a plate; and firing and post-treating the molded plate.

Description

형광체 투명 세라믹 플레이트의 제조방법Manufacturing method of phosphor transparent ceramic plate
본 발명은 형광체 투명 세라믹 플레이트의 제조방법에 관한 것이다. 더욱 상세하게, 제조방법이 간단하고, 제품 수율도 개선시킬 수 있는 형광체 투명 세라믹 플레이트의 제조방법에 관한 것이다.The present invention relates to a method for producing a phosphor transparent ceramic plate. More specifically, the present invention relates to a method for producing a phosphor transparent ceramic plate which is simple in manufacturing and can improve product yield.
본 명세서에서 사용하는 용어 'LED'는 발광다이오드(Light Emitting Diode)의 약자로서 반도체의 pn 접합 구조를 이용하여 주입된 소수 개리어(전자 또는 전공)를 만들어 내고, 이들의 재결합에 의하여 발광하는 발광다이오드를 의미한다.The term 'LED' used in the present specification is an abbreviation of light emitting diode (Light Emitting Diode) to generate a small number of carriers (electron or electric) injected by using a semiconductor pn junction structure, and emit light by recombination thereof Means a diode.
본 명세서에서 사용하는 용어 'LD'는 레이저 다이오드(Laser Diode)의 약자로서 반도체에 캐리어를 대량으로 주입했을 경우 전자와 전공이 에너지를 넘어서 재결합할 때 발광하는 효과를 이용하는 반도체로 만든 레이저 다이오드를 의미한다.As used herein, the term 'LD' is an abbreviation for laser diode, which means a laser diode made of a semiconductor that uses electrons and electrons to emit light when the carrier and electrons recombine over energy. do.
LED 장치나 LD 조사 장치 등의 광반도체 장치는 예컨대 LED 소자나 LD 등의 광반도체 소자 및 광반도체 소자의 위에 배치되는 형광체층을 구비한다. 이러한 광반도체 장치는 광 반도체 소자로부터 발광되고, 요컨대 형광체층을 투과한 청색광과, 형광체층에서 청색광의 일부가 파장 변환된 황색광의 혼색에 의해 백색광을 발광한다. An optical semiconductor device such as an LED device or an LD irradiation device includes, for example, an optical semiconductor element such as an LED element or an LD, and a phosphor layer disposed on the optical semiconductor element. Such an optical semiconductor device emits white light by emitting light from an optical semiconductor element, that is, a mixture of blue light transmitted through a phosphor layer and yellow light in which part of blue light is wavelength-converted in the phosphor layer.
이러한 광반도체 장치는 LED가 투명 봉지재료로 봉지된 LED 패키지, 및 그의 상면에 적층되는 형광 테이프를 구비하는 LED 장치가 주류를 이루고 있는 바, 이러한 형광 테이프는 형광층, 및 그의 이면에 적층되는 아크릴 감압 접착층을 구비하고 형광층이 접착층을 통해 LED 패키지의 표면에 부착되어 있으나, 형광 테이프는 LED 발광에 수반하여 고온이 되기 쉬워서 열화되기 쉽고, 그 때문에 LED 장치의 휘도가 저하되는 문제가 있었다. 이러한 이유로 형광체 접착 시트에서 형광체층을 형광체의 세라믹으로부터 형광체의 세라믹 플레이트로 형성하고 있다. Such an optical semiconductor device has a mainstream LED device including an LED package in which an LED is encapsulated with a transparent encapsulation material, and a fluorescent tape laminated on an upper surface thereof, and the fluorescent tape is an acrylic layer laminated on a fluorescent layer and a back surface thereof. Although the pressure-sensitive adhesive layer is provided and the fluorescent layer is attached to the surface of the LED package through the adhesive layer, the fluorescent tape tends to deteriorate due to the high temperature accompanying the light emission of the LED, thereby causing a problem that the luminance of the LED device is lowered. For this reason, the phosphor layer is formed from the ceramic of the phosphor to the ceramic plate of the phosphor in the phosphor adhesive sheet.
그러나, 종래 투명 세라믹 플레이트는 도 2에 예시한 바와 같이 산화이트륨, 산화알루미늄, 산화가넷 입자로부터 원료 분말을 조제하고, 조제한 원료 분말과, 수용성 바인더 수지를 혼합하고 추가로 증류수를 가하여 습식 혼합하고 소성 단계를 거쳐 이트륨-알루미늄-가넷(Yttrium-Aluminum-Garnet, 이하 'YAG'라 칭함) 전구체를 제작한 후, 오븐 건조하고, 세라믹 그린 시트를 형성한 다음에 세라믹 그린 시트 적층체를 가열, 고온 진공로에서 가열 및 소성하는 방법으로 형광체 투명 세라믹 플레이트를 제작해 왔다. 하지만 이 경우 최종 플레이트 제작 기간이 오래 걸리며, 제품 수율에 대한 문제가 발생하고 있다. However, in the conventional transparent ceramic plate, as illustrated in FIG. 2, raw material powder is prepared from yttrium oxide, aluminum oxide, and garnet oxide particles, and the prepared raw material powder is mixed with a water-soluble binder resin, and further distilled water is added to wet mix and fire. Yttrium-Aluminum-Garnet (hereinafter referred to as 'YAG') precursor was produced through the steps, followed by oven drying, forming a ceramic green sheet, and then heating the ceramic green sheet laminate to obtain a high temperature vacuum. Phosphor transparent ceramic plates have been produced by heating and firing in a furnace. In this case, however, the final plate manufacturing takes a long time, and there is a problem in product yield.
이에 본 발명은 YAG 형광체를 고상 합성하여 분쇄 후, 투명 세라믹 플레이트를 제작 시 기존 고상법을 이용하여 제작하면 제조 방법이 간단하고 제품 수율 또한 개선시킬 수 있다는 것을 알게 되어 본 발명을 완성하게 되었다.Accordingly, the present invention has been completed by the present invention was found that the production method is simple and the product yield can also be improved by fabricating using a conventional solid phase method when producing a transparent ceramic plate after pulverizing the YAG phosphor.
본 발명의 한 구현예에 따르면, 형광체 투명 세라믹 플레이트는 작은 입자의 YAG 형광체를 1㎛ 이하로 분쇄한 후 플레이트 제작(성형) 및 소성하여서 제조하는 것을 특징으로 한다.According to one embodiment of the invention, the phosphor transparent ceramic plate is characterized in that the small particles of the YAG phosphor is pulverized to 1㎛ or less, and then manufactured by forming (molding) and firing.
본 발명의 형광체 투명 세라믹 플레이트의 제조방법에 의하면, 복잡한 공정을 최소화할 수 있고, 정밀 면가공으로 플레이트의 두께 균일도 우수하며, 100: 1 이상의 높은 색 대비와 동시에 낮은 색 산포를 구현할 수 있고, 열 색 좌표 이동을 감소시킬 수 있고, 우수한 발광각 균일도를 갖고, 플레이트의 실장 전 단계에서 형광 특성 스크린을 통한 바이닝(binning) 문제 해결할 수 있으며, 고출력 발광다이오드(LED) 및 레이저 다이오드(LD) 적용 시 안정성 및 신뢰성 확보할 수 있는 효과가 있다.According to the manufacturing method of the phosphor transparent ceramic plate of the present invention, it is possible to minimize the complex process, excellent thickness uniformity of the plate by precision surface processing, high color contrast of 100: 1 or more and at the same time can realize a low color dispersion, heat It can reduce color coordinate shift, have excellent luminescence uniformity, solve binning problem through fluorescent screen in the pre-mounting stage of the plate, and apply high power light emitting diode (LED) and laser diode (LD) There is an effect that can ensure the stability and reliability at the time.
도 1은 본 발명에 따른 투명 세라믹 플레이트의 제조 공정도이다.1 is a manufacturing process chart of a transparent ceramic plate according to the present invention.
도 2는 종래의 투명 세라믹 플레이트의 제조 공정도이다.2 is a manufacturing process chart of a conventional transparent ceramic plate.
도 3은 분쇄하기 전의 입도 분석기를 이용한 YAG 분말 입도 분포 데이타이다.3 is YAG powder particle size distribution data using a particle size analyzer before grinding.
도 4는 분쇄한 후에 입도 분석기를 이용한 YAG 분말 입도 분포 데이타이다.4 is YAG powder particle size distribution data using a particle size analyzer after grinding.
도 5는 본 발명에 따른 투명 세라믹 플레이트와 종래의 방법(도 2)으로 제조된 투명 세라믹 플레이트 간의 세슘 농도에 따른 스펙트럼 비교 그래프이다.5 is a spectral comparison graph according to cesium concentration between the transparent ceramic plate according to the present invention and the transparent ceramic plate manufactured by the conventional method (FIG. 2).
이와 같은 본 발명을 다음에서 상세하게 설명하기로 하며, 다음의 구현예 또는 실시예는 단지 예시하기 위한 것으로 본 발명이 반드시 이에 한정되는 것은 아니다. The present invention will be described in detail below, and the following embodiments or examples are merely to illustrate, but the present invention is not necessarily limited thereto.
본 발명의 한 구현예에 따르면, 형광체 투명 세라믹 플레이트는 도 1에 예시한 바와 같이 작은 입자의 YAG 형광체를 1㎛ 이하로 밀링에 의해 분쇄하는 단계; 분쇄한 YAG 형광체를 오븐에서 건조하는 단계; 건조한 분쇄된 YAG 형광체에 압력을 가하여 플레이트로 성형하는 단계 및 성형된 플레이트를 소성 및 후처리하는 단계로 이루어진다.According to one embodiment of the present invention, the phosphor transparent ceramic plate comprises the steps of milling small particles of YAG phosphor by milling to 1 μm or less as illustrated in FIG. 1; Drying the pulverized YAG phosphor in an oven; Pressurizing the dry pulverized YAG phosphor to form a plate; and firing and post-processing the formed plate.
본 발명에 의하면, 상기 YAG 형광체를 분쇄하는 단계는 볼밀을 이용하여 밀링에 의해 분쇄하는 것이 바람직하고, 만일 1㎛ 이하로 분쇄하지 않을 경우에는 플레이트의 두께 균일하지 않게되고, 결국, 고출력 발광다이오드(LED) 및 레이저 다이오드(LD) 적용 시 안정성 및 신뢰성 확보할 수 없게 된다. 도 3은 분쇄하기 전의 입도 분석기를 이용한 YAG 분말 입도 분포 데이타를 나타낸 것이고, 도 4는 분쇄한 후에 입도 분석기를 이용한 YAG 분말 입도 분포 데이타를 나타낸 것이다.According to the present invention, the step of pulverizing the YAG phosphor is preferably pulverized by milling using a ball mill, and if it is not pulverized to 1 탆 or less, the thickness of the plate becomes uneven, and eventually, a high power light emitting diode ( LED) and laser diode (LD) will not be able to secure stability and reliability. Figure 3 shows the YAG powder particle size distribution data using a particle size analyzer before grinding, Figure 4 shows the YAG powder particle size distribution data using a particle size analyzer after grinding.
본 발명에 의하면, 상기 분쇄한 YAG 형광체를 오븐에서 건조하는 단계는 100 내지 150℃의 온도 범위 내에서 1 내지 24시간 동안 실시하는 것이 바람직하다. According to the invention, the step of drying the pulverized YAG phosphor in an oven is preferably carried out for 1 to 24 hours in the temperature range of 100 to 150 ℃.
본 발명에 의하면, 상기 압력을 가하여 성형하는 단계는 냉방등방압 가압법(CIP)를 이용하여 1,000 Mpa 내지 3,000 Mpa 사이의 압력 범위 내에서 실시하는 것이 바람직하다. According to the present invention, the step of applying the pressure is preferably carried out within a pressure range of 1,000 Mpa to 3,000 Mpa by using a cooling isotropic pressurization (CIP).
본 발명에 의하면, 상기 소성 단계는 분위기로를 이용하여 환원 또는 공기 중에서 1400 내지 1800℃ 사이의 온도 범위에서 8 내지 15시간의 범위내에서 실시하는 것이 바람직하다. According to the invention, the firing step is preferably carried out within a range of 8 to 15 hours at a temperature range of 1400 to 1800 ℃ in reducing or air using an atmosphere furnace.
본 발명에 의하면, 상기 소성된 투명 세라믹 플레이트를 후처리하는 단계는 표면 연마하는 공정으로 자동연마기를 이용하여 표면 연마를 수행하는 것이 바람직하다. According to the present invention, the post-treatment of the fired transparent ceramic plate may be performed by surface polishing using an automatic polishing machine as a surface polishing process.
본 발명의 투명 세라믹 플레이트의 제조시 활성체로서 세슘을 0.01 내지 0.03몰농도로 사용하는 것이 바람직하며, 다음 표 1은 활성체의 농도에 따라 제조된 본 발명의 투명 세라믹 플레이트와 종래의 방법(도 2)의 방법으로 제조된 투명 세라믹 플레이트 간의 광량(lm)을 비교한 것이다. 표 1에 의하면 본 발명의 방법에 따라 제조된 투명 세라믹 플레이트의 광량이 상당히 양호하다는 것을 알 수 있다.In the preparation of the transparent ceramic plate of the present invention, cesium is preferably used in an amount of 0.01 to 0.03 mole as an active agent, and the following Table 1 shows the transparent ceramic plate of the present invention prepared according to the concentration of the active agent and the conventional method (Fig. The amount of light lm between the transparent ceramic plates manufactured by the method of 2) is compared. From Table 1 it can be seen that the light quantity of the transparent ceramic plate produced according to the method of the present invention is quite good.
항목Item Ce 농도Ce concentration
0.03 mol%0.03 mol% 0.02 mol%0.02 mol% 0.01 mol%0.01 mol%
본 발명에 따른 투명 세라믹 플레이트Transparent ceramic plate according to the present invention 광량(lm)Light quantity (lm) 51.9851.98 83.0883.08 131.01131.01
종래의 투명 세라믹 플레이트Conventional transparent ceramic plate 광량(lm)Light quantity (lm) 42.4942.49 66.1866.18 124.75124.75
도 5는 본 발명에 따른 투명 세라믹 플레이트와 종래의 방법(도 2)으로 제조된 투명 세라믹 플레이트 간의 세슘 농도에 따른 스펙트럼을 비교한 것 도면이다.5 is a view comparing spectra according to cesium concentration between the transparent ceramic plate according to the present invention and the transparent ceramic plate manufactured by the conventional method (FIG. 2).
이상에서 실시예를 참조하여 설명하였지만, 해당 기술 분야의 숙련된 당업자는 하기의 특허청구범위에 기재된 본 발명의 기술적 사상으로부터 벗어나지 않는 범위 내에서 본 발명을 다양하게 수정 및 변경시킬 수 있음을 이해할 수 있을 것이다.Although described with reference to the embodiments above, those skilled in the art can understand that the present invention can be variously modified and changed without departing from the spirit of the invention described in the claims below. There will be.

Claims (4)

  1. 작은 입자의 YAG 형광체를 1㎛ 이하로 밀링에 의해 분쇄하는 단계; 분쇄한 YAG 형광체를 오븐에서 건조하는 단계; 건조한 분쇄 YAG 형광체에 압력을 가하여 플레이트로 성형하는 단계 및 성형된 플레이트를 소성 및 후처리하는 단계로 이루어지는 것을 특징으로 하는 형광체 투명 세라믹 플레이트의 제조방법.Milling the small particles of the YAG phosphor by milling to 1 μm or less; Drying the pulverized YAG phosphor in an oven; A method of manufacturing a phosphor transparent ceramic plate, comprising the steps of: forming a plate by applying pressure to a dry pulverized YAG phosphor; and firing and post-processing the molded plate.
  2. 제1항에 있어서, 상기 분쇄한 YAG 형광체를 오븐에서 건조하는 단계는 100 내지 150℃의 온도 범위 내에서 1 내지 24시간 동안 실시하는 것을 특징으로 하는 방법.The method of claim 1, wherein the drying of the pulverized YAG phosphor in an oven is performed for 1 to 24 hours in a temperature range of 100 to 150 ° C.
  3. 제1항에 있어서, 상기 압력을 가하여 성형하는 단계는 냉방등방압 가압법(CIP)를 이용하여 1,000 Mpa 내지 3,000 Mpa 사이의 압력 범위 내에서 실시하는 것을 특징으로 하는 방법.The method as claimed in claim 1, wherein the molding by applying pressure is performed within a pressure range of 1,000 Mpa to 3,000 Mpa using a cooling isotropic pressure press method (CIP).
  4. 제1항에 있어서, 상기 소성 단계는 분위기로를 이용하여 환원 또는 공기 중에서 1400 내지 1800℃ 사이의 온도 범위에서 8 내지 15시간의 범위내에서 실시하는 것을 특징으로 하는 방법.The method according to claim 1, wherein the firing step is carried out in a reducing or air atmosphere using an atmosphere furnace in a temperature range of 1400 to 1800 ° C within a range of 8 to 15 hours.
PCT/KR2016/012929 2015-12-31 2016-11-10 Method for manufacturing transparent ceramic phosphor plate WO2017116000A1 (en)

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