KR100223518B1 - A znga204(:mn) phosphor for low-voltage and a method for manufacturing a phosphor screen by using it - Google Patents
A znga204(:mn) phosphor for low-voltage and a method for manufacturing a phosphor screen by using it Download PDFInfo
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- KR100223518B1 KR100223518B1 KR1019960033447A KR19960033447A KR100223518B1 KR 100223518 B1 KR100223518 B1 KR 100223518B1 KR 1019960033447 A KR1019960033447 A KR 1019960033447A KR 19960033447 A KR19960033447 A KR 19960033447A KR 100223518 B1 KR100223518 B1 KR 100223518B1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J29/00—Details of cathode-ray tubes or of electron-beam tubes of the types covered by group H01J31/00
- H01J29/02—Electrodes; Screens; Mounting, supporting, spacing or insulating thereof
- H01J29/10—Screens on or from which an image or pattern is formed, picked up, converted or stored
- H01J29/18—Luminescent screens
- H01J29/20—Luminescent screens characterised by the luminescent material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/20—Manufacture of screens on or from which an image or pattern is formed, picked up, converted or stored; Applying coatings to the vessel
- H01J9/22—Applying luminescent coatings
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Abstract
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Description
본 발명은 저전압발광 ZnGa2O4(:Mn) 형광체 및 이를 이용한 형광막 제조방법에 관한 것으로, 보다 상세하게는 전계방출형 디스플레이(Field Emission Display; FED)또는 진공형광판(Vacuum Fluorescent Display; VFD)에 사용되는 저전압 발광특성이 향상된 ZnGa2O4(:Mn) 형광체 및 이를 이용한 형광막 제조방법에 관한 것이다.The present invention relates to a low voltage ZnGa 2 O 4 (: Mn) phosphor and a method for manufacturing a fluorescent film using the same, and more particularly, to a field emission display (FED) or a vacuum fluorescence display (VFD). The present invention relates to a ZnGa 2 O 4 (: Mn) phosphor having improved low voltage emission characteristics and a method of manufacturing a fluorescent film using the same.
전계방출형 디스플레이 (이하 FED라 칭함)는 전자가 형광체를 때려 빛을 내는 음극선발광(냉광)(cathodoluminescence) 현상을 이용한 디스플레이로서 강한 전계에 의해 전자가 방출되는 원리를 이용한 것이다.A field emission type display (hereinafter referred to as FED) is a display using a cathodoluminescence phenomenon in which electrons strike a phosphor and emit light by a strong electric field.
FED는 각 화소에 대하여 수백개의 음극을 대응시키는 면상의 전자원을 사용하여 편향없이 직접 화상을 형성하므로 패널의 두께를 수mm로 얇게 하는 것이 가능할 뿐 아니라 LCD와는 달리 시야각을 확보한 채로 계조를 올리는 것이 가능하고, 화질이 우수하고, 생산효율이 높고, 응답속도가 빠르고, 저온동작이 가능하고, 휘도가 높고, 전력효율이 높은 등의 많은 장점이 있는 첨단 디스플레이 장치이다.The FED forms images directly without deflection by using on-plane electron sources that correspond to hundreds of cathodes for each pixel, making it possible to reduce the thickness of the panel to several millimeters and to increase the gradation with a viewing angle unlike LCD. It is an advanced display device with many advantages such as high image quality, high production efficiency, fast response speed, low temperature operation, high brightness, high power efficiency, and the like.
따라서 FED는 평면박판화가 가능한 이상적인 디스플레이로 최근에 연구개발이 활발히 진행되고 있다.Therefore, FED is an ideal display that can be flat-plated, and research and development have been actively conducted recently.
일반적으로 CRT는 방출된 전자가 약30KV 이상의 고압으로 가속되어 형광체를 자극하지만 FED 및 VFD는 패널사이의 거리가 100-200｜Lm에 불과하여 실제로 CRT에서와 같은 고압을 인가하기는 불가능하므로 FED 및 VFD에 사용되는 형광체는 저전압에서 작동되어야 한다.In general, CRT stimulates the phosphor by accelerating the emitted electrons to a high pressure of about 30KV or higher, but FED and VFD have a distance between panels of 100-200 | Lm. Phosphors used in VFDs must be operated at low voltages.
따라서, FED의 실용화를 위해서는 500V 이하의 저전압에서도 휘도특성이 우수한 형광체의 개발이 필수적 이다.Therefore, for the practical use of the FED, it is essential to develop a phosphor having excellent luminance even at a low voltage of 500V or less.
또한 FED 및 VFD의 형광체는 안정성이 우수해야 한다. 형광체는 계속적인 전자의 자극에 의해 배기가스나 입자가 발생하여 패널내의 진공도를 저하시켜 FED 및 VFD의 수명을 단축하기 때문이다. 특히, CRT용 형광체의 주류인 황화물계 형광체에서는 전자자극에 의해 유출된 황입자가 금속이나 실리콘 팁에 흡착되어 에미터의 심각한 성능저하를 초래할 수 있다.In addition, the phosphors of FED and VFD should have excellent stability. This is because the phosphor emits exhaust gas or particles due to the continuous stimulation of electrons, which lowers the degree of vacuum in the panel, thereby shortening the lifespan of the FED and VFD. In particular, in sulfide-based phosphors, which are the mainstream of phosphors for CRTs, sulfur particles leaked out by electron stimulation may be adsorbed onto metal or silicon tips and cause serious performance degradation of emitters.
CRT에서는 형광체 표면에 알루미늄막을 코팅하여 형광체의 안정성을 향상시키고 있으나, FED나 VFD의 경우에는 입사되는 전자의 에너지가 작기 때문에 이러한 전자가 투과하지 못하는 알루미늄막을 사용할 수 없다. 또한, 알루미늄 같은 전도막을 사용할 수 없음에 따라 상기 형광체가 음으로 대전되는 문제점이 야기된다.In the CRT, an aluminum film is coated on the surface of the phosphor to improve the stability of the phosphor. However, in the case of FED or VFD, the energy of incident electrons is small so that the aluminum film cannot pass through such electrons. In addition, the use of a conductive film such as aluminum causes a problem that the phosphor is negatively charged.
종래에 저전압 작동 가능성 및 안정성이 우수한 형광체로 ZnGa2O4를 모체로 하는 형광체가 알려져 있다.Background Art Conventionally, phosphors based on ZnGa 2 O 4 are known as phosphors having excellent low voltage operability and stability.
종래 ZnGa2O4를 모체로 하는 형광체는 ZnO와 Ga2O3를 혼합하여 1,200℃ 이상에서 3시간 이상 반응시켰을 때 1 - 5｜Lm의 스피넬 형태의 폴리크리스탈 분말이 얻어지며 상기 폴리크리스탈 분말을 환원시킴으로써 파란색(1= 470mm)을 발광할 수 있는 ZnGa2O4 형광체가 합성된다. 또한 상기와 같이 합성된 ZnGa2O4의 폴리크리스탈의 Zn 위치에 Mn을 극미량으로 대치한 후 환원시키면 초록색(1 = 560mm)을 발광하는 형광체를 얻을 수 있다.Conventional phosphors based on ZnGa2O4 are obtained by mixing ZnO and Ga2O3 and reacting at 1,200 ° C. or more for 3 hours or more to obtain a crystallized polycrystalline powder having a spinel form of 1-5 | Lm and reducing the polycrystalline powder to blue (1 = ZnGa 2 O 4 phosphors capable of emitting 470 mm) are synthesized. In addition, by replacing a very small amount of Mn at the Zn position of the polycrystal of ZnGa 2 O 4 synthesized as described above and reducing it, a phosphor emitting green color (1 = 560 mm) can be obtained.
상기 ZnGa2O4 형광체를 합성한 후 인듐-주석산화물(Indium-TinOxide, 이하 ITO) 글라스 위에 도포하여 형광막을 형성한다.The ZnGa 2 O 4 phosphor is synthesized, and then coated on an indium tin oxide (ITO) glass to form a fluorescent film.
위에 기술한 바와 같이 형성된 형광막(이하, 양극판)을 진공속에서 전계 방출소자나 열방출선에서 나오는 200 - 500eV의 에너지를 갖는 전자들로 여기시키면 파란색 혹은 초록색을 발광하게 되는데, 황화물계 형광체에 비해서 진공속에서 방출하는 배기 가스가 대단히 적고 화학적 변화에 대한 내성이 강한 안정된 발광을 보이는 양극판이 얻어지며 저전압 발광특성이 비교적 좋다.Exciting a fluorescent film (hereinafter referred to as a bipolar plate) formed as described above with electrons having energy of 200-500 eV from a field emission device or a heat emission line in a vacuum emits blue or green light. A bipolar plate exhibiting stable light emission with very little exhaust gas emitted in a vacuum and strong resistance to chemical changes is obtained, and low voltage light emission characteristics are relatively good.
그러나, 상기한 ZnGa2O4나 ZnGa2O4:Mn 형광체는 안정하며 저전압 발광효율이 비교적 우수하나 천연색(Full-color) FED나 VFD에 채택되기 위해서는 효율을 현재 수준인 1.5lm/W에서 4.2lm/W로 2 - 3배 향상시켜야 한다. 또한, 이같은 저효율을 보충하기 위해 FED의 양극판을 높은 전류밀도에서 여기하여야 하는데, 이렇게 할 경우 형광체의 표면에 축적되는 전하에 의한 형광체의 열화현상(Coulomb Degradation)이 야기되어 발광효율을 매우 떨어뜨릴 뿐만 아니라 작동시간이 제한되어 상용화를 가로막는 요인이 되었다.However, the ZnGa2O4 or ZnGa2O4: Mn phosphors are stable and have relatively low voltage luminous efficiency, but in order to be adopted in full-color FED or VFD, the efficiency is reduced from the current level of 1.5lm / W to 4.2lm / W. It should be improved 3 times. In addition, in order to compensate for such low efficiency, the positive electrode plate of the FED should be excited at a high current density, which causes a deterioration of the phosphor due to charges accumulated on the surface of the phosphor, resulting in a very low luminous efficiency. However, the operating time was limited and became a factor preventing commercialization.
본 발명의 목적은 상기와 같은 문제점을 해결하여 저전압 발광효율이 향상되고 발광수명이 연장된 저전압발광 ZnGa2O4(:Mn) 형광체를 제공하는 것이다.SUMMARY OF THE INVENTION An object of the present invention is to provide a low voltage light emitting ZnGa 2 O 4 (: Mn) phosphor which has improved low voltage light emission efficiency and has an extended light emission life by solving the above problems.
본 발명의 다른 목적은 저전압발광 ZnGa2O4(:Mn) 형광체를 이용하여 전기영동법에 의한 형광막 제조방법을 제공하는 것이다.Another object of the present invention is to provide a method for producing a fluorescent film by electrophoresis using low voltage light emitting ZnGa 2 O 4 (: Mn) phosphor.
상기와 같은 목적을 달성하기 위하여 본 발명은 ZnGa2O4(:Mn)을 모체로하여 산소공극을 만들 수 있는 금속산화물을 첨가하여 형성되는 저전압발광 ZnGa2O4(:Mn) 형광체를 제공한다.In order to achieve the above object, the present invention provides a low-voltage light-emitting ZnGa 2 O 4 (: Mn) phosphor formed by adding a metal oxide capable of forming oxygen pores based on ZnGa 2 O 4 (: Mn).
본 발명에서의 형광체 모체는 PL세기가 가장 큰 조건에서 합성되며, 상기 모체에 첨가되는 금속산화물은 WO3, V2O5, 또는 SiO2 로 구성된다.The phosphor matrix in the present invention is synthesized under the condition of the greatest PL intensity, and the metal oxide added to the matrix is composed of WO3, V2O5, or SiO2.
본 발명은 또한 저전압발광 ZnGa2O4(:Mn)형광체를 이소-프로필알콜(iso-prophly alcohol; 이하 IPA라 칭함)에 분산시켜 전기영동법으로 ITO 글라스상에 증착시키는 형광막 제조방법을 제공한다.The present invention also provides a method for producing a fluorescent film in which a low voltage ZnGa2O4 (: Mn) phosphor is dispersed in iso-prophly alcohol (hereinafter referred to as IPA) and deposited on ITO glass by electrophoresis.
본 발명에서 ITO 글라스에 증착되는 형광막은 3.5 - 5.5｜Lm, 바람직하게는 4.0 - 4.5｜Lm 두께로 형성된다.In the present invention, the fluorescent film deposited on the ITO glass is formed to have a thickness of 3.5-5.5 | Lm, preferably 4.0-4.5 | Lm.
도1은 WO3의 첨가량에 따른 저전압발광 ZnGa2O4(:Mn)형광체의 CL세기 측정결과도1 is a CL intensity measurement result of a low voltage ZnGa 2 O 4 (: Mn) phosphor according to the amount of WO 3 added;
도2는 V2O5의 첨가량에 따른 저전압발광 ZnGa2O4(:Mn) 형광체의 CL세기 측정결과도2 is a CL intensity measurement result of a low voltage ZnGa 2 O 4 (: Mn) phosphor according to the amount of V 2 O 5 added;
도3은 SiO2의 첨가량에 따른 저전압발광 ZnGa2O4(:Mn) 형광체의 CL세기 측정결과도3 is a CL intensity measurement result of a low voltage ZnGa 2 O 4 (: Mn) phosphor according to the amount of SiO 2 added;
도4은 본 발명의 저전압발광 ZnGa2O4(:Mn) 형광막의 두께에 따른 CL세기 측정결과도4 is a CL intensity measurement result according to the thickness of the low-voltage light-emitting ZnGa 2 O 4 (: Mn) fluorescent film of the present invention
이하, 본 발명의 실시예를 첨부도면을 참조하여 상세히 설명한다. 본 실시예에서의 PL(Photoluminescence)은 광자에 의해 형광체가 에너지를 받아 빛을 내는 현상이고, CL(Catholuminescence)은 음극선관(Cathode)에서 방출되는 전자에 의해서 형광체가 발광하는 현상이다.Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the present embodiment, PL (Photoluminescence) is a phenomenon in which a phosphor receives energy by photons and emits light, and CL (Catholuminescence) is a phenomenon in which a phosphor emits light by electrons emitted from a cathode ray tube.
[실시예 1]Example 1
저전압발광 형광체의 제조방법Manufacturing method of low voltage light emitting phosphor
본 발명의 저전압발광 ZnGa2O4(:Mn) 형광체는 다음과 같은 단계를 거쳐 제조된다.The low voltage light emitting ZnGa 2 O 4 (: Mn) phosphor of the present invention is prepared through the following steps.
i. 모체인 ZnGa2O4(:Mn)의 합성i. Synthesis of parent ZnGa2O4 (: Mn)
모체물질로 사용된 ZnGa2O4(:Mn)은 ZnO와 Ga2O4를 1:1 몰비로 혼합하고, Mn은 0.1중량%로 첨가하여 1,000-1,400℃, 6 - 15시간, 바람직하게는 1,200℃에 서 9 - 11시간 합성한 후 환원하여 얻었다.ZnGa2O4 (: Mn) used as the parent material mixes ZnO and Ga2O4 in a 1: 1 molar ratio, and Mn is added in an amount of 0.1% by weight at 1,000-1,400 ° C for 6-15 hours, preferably at 1,200 ° C. It synthesize | combined for 11 hours, and obtained by reducing.
ii. 금속산화물첨가ii. Metal Oxide Addition
상기 합성된 모체분말에 발광효율(휘도)를 향상시키는 WO3, V2O5, 또는 SiO2를 극미량, 바람직하게는 0.001-1.000중량% 첨가하여 IPA 용액에 2-5시간, 바람직하게는 3 - 4시간 동안 스터링(stirring)하여 첨가 금속산화물이 모체인 ZnGa2O4(:Mn)형광체에 완전히 혼합됨으로써 저전압발광 ZnGa2O4(:Mn) 형광체가 완성된다.A very small amount of WO3, V2O5, or SiO2, which improves the luminous efficiency (luminance), is added to the synthesized mother powder, preferably 0.001-1.000% by weight, for 2-5 hours, preferably 3-4 hours, in the IPA solution. The low-voltage light-emitting ZnGa2O4 (: Mn) phosphor is completed by stirring and completely mixing the added metal oxide with the parent ZnGa2O4 (: Mn) phosphor.
[실시예 2 ]Example 2
전기영동법에 의한 형광막(양극판) 제조방법Method for manufacturing fluorescent film (anode plate) by electrophoresis
i. 실시예1에서 완성된 형광체분말이 분산된 IPA용액 300ml에 양이온으로 이온 화되면서 모체 및 금속산화물을 둘러싸고 양전하를 인가하기 위한 염으로 Mg(NO3)2 를 5 x 10-4mol/l 의 비율로 첨가후 분산시켰다.i. Mg (NO 3) 2 was added at a rate of 5 × 10 −4 mol / l as a salt for applying positive charges to the mother and metal oxides while ionizing with cations in 300 ml of the IPA solution in which the phosphor powder was dispersed in Example 1 And then dispersed.
ii. 상기 용액에 전류를 흘러보내어 Mg No3+ 로 인하여 양전하가 인가된 모체 및 금속산화물은 음극판인 ITO 글라스상에 증착되게 하였다. 이때 전압을 400V로 걸어주면 증착이 진행됨에 따라 MgNO3+가 감소되므로 전류가 떨어진다.ii. A current was flowed into the solution to cause the mother and metal oxides to which positive charge was applied due to Mg No 3+ to be deposited on ITO glass, which is a negative electrode plate. At this time, if the voltage is applied to 400V, the current decreases because MgNO 3+ decreases as the deposition proceeds.
이때, 증착막은 3.5 - 5.5｜Lm, 바람직하기로는 4.0 - 4.5｜Lm 두께를 유지하도록 하였다.At this time, the deposited film was maintained at a thickness of 3.5-5.5 | Lm, preferably 4.0-4.5 | Lm.
iii. 상기 증착막을 400 - 500℃, 바람직하게는 460 - 480℃에서 1시간 - 3시간 동안 아닐링하여 최종적으로 양극판을 완성하였다.iii. The deposited film was annealed at 400-500 ° C, preferably 460-480 ° C for 1 hour-3 hours to finally complete the positive electrode plate.
이때, 생성된 MgO는 상기 저전압 발광형광체를 ITO 유리판에 붙여놓는 바인더로 작용하였다.At this time, the produced MgO acted as a binder for pasting the low voltage light-emitting phosphor on the ITO glass plate.
이상과 같은 제조방법에 의한 형광막(양극판)의 발광 효율을 다음과 같이 측정하였다.The luminous efficiency of the fluorescent film (anode plate) by the above manufacturing method was measured as follows.
제조된 양극판을 진공(10-7torr) 챔버내에서 전자총(electron gun)으로부터 방출되는 전자에 노출시켰다. 400V 양극 전압과, 1.5｜LA의 방출전류(emission current) 정도의 에너지를 가해 상기 양극판의 형광체를 여기시켰다. 이때 발광되는 빛의 휘도를 광도계(Minolt CS-100)에 의해서 빛의 휘도단위(cd/m2)로 측정하였다. 금속산화물로써 WO3가 첨가된 경우의 ZnGa2O4(:Mn) 형광막의 CL세기 측정결과를 도1에 나타내었다.The prepared bipolar plate was exposed to electrons emitted from an electron gun in a vacuum (10-7torr) chamber. A phosphor of the positive electrode plate was excited by applying a 400V anode voltage and energy of about 1.5 | LA emission current. At this time, the luminance of the light emitted was measured in the luminance unit (cd / m2) of light by a photometer (Minolt CS-100). The CL intensity measurement result of the ZnGa 2 O 4 (: Mn) fluorescent film when WO 3 is added as the metal oxide is shown in FIG. 1.
또한, 금속산화물로써 V2O5 및 SiO2가 첨가된 경우의 ZnGa2O4(:Mn) 형광막의 CL세기 측정 결과를 도2 및 도3에 각각 나타내었다.In addition, the CL intensity measurement results of the ZnGa 2 O 4 (: Mn) fluorescent film when V 2 O 5 and SiO 2 were added as metal oxides are shown in FIGS. 2 and 3, respectively.
도1, 도2 및 도3에 나타나 있는 바와 같이 금속산화물의 극미량, 바람직하게는 0.001-1.000중량% 첨가는 모체인 ZnGa2O4(:Mn) 형광체의 발광효율을 현저히 향상시킴을 알 수 있었다.As shown in Fig. 1, Fig. 2 and Fig. 3, the addition of an extremely small amount of metal oxide, preferably 0.001-1.000% by weight, significantly improved the luminous efficiency of the parent ZnGa 2 O 4 (: Mn) phosphor.
이와 같은 현저한 발광효율의 향상은 ZnGa2O4(:Mn) 모체에 WO3, SiO2 또는 V2O5를 첨가하면 상기 ZnGa2O4(:Mn) 모체 표면에 양으로 하전된 산소공극을 제공하여 양극판의 축적된 전하를 원활히 소모시킴으로써 음극으로부터의 입사전자들이 용이하게 상기 형광체를 여기할 수 있기 때문이다.This remarkable improvement in luminous efficiency is achieved by the addition of WO3, SiO2 or V2O5 to the ZnGa2O4 (: Mn) matrix to provide positively charged oxygen voids on the surface of the ZnGa2O4 (: Mn) matrix, thereby consuming the accumulated charge on the positive electrode plate smoothly. This is because incident electrons from the cathode can easily excite the phosphor.
도4는 증착된 형광막 두께에 따른 CL세기를 나타낸 도면이다.4 is a diagram showing CL intensity according to the thickness of the deposited fluorescent film.
증착량이 0.5mg/cm2 으로 증착되었을 때 최고의 CL 휘도를 얻을 수 있으며 이때에 막두께는 4｜Lm 임을 알 수 있다. 저전압발광 ZnGa2O4(:Mn) 형광체를 이용하여 양극판을 제조하는 경우 3.5 - 5.5｜Lm, 바람직하기로는 4.0 - 4.5｜Lm 두께의 양극판이 발광효율이 우수함을 도4로부터 알 수 있다.The highest CL luminance can be obtained when the deposition amount is deposited at 0.5 mg / cm 2, and the film thickness is 4 | Lm at this time. It can be seen from FIG. 4 that a positive electrode plate having a thickness of 3.5-5.5 | Lm, preferably 4.0-4.5 | Lm is excellent in the case of manufacturing the positive electrode plate using the low-voltage light-emitting ZnGa 2 O 4 (: Mn) phosphor.
본 발명에서 제공한 ZnGa2O4(:Mn)을 모체로 WO3, SiO2 또는 V2O5를 첨가함으로써 형성된 형광체 및 이를 이용한 형광막은 FED 또는 VFD에 양극판으로 사용될 경우 저전압으로 형광막을 발광시킬 수 있을 뿐 아니라 발광수명이 현저하게 연장되는 효과를 얻을 수 있다.Phosphor formed by adding WO3, SiO2 or V2O5 as a mother ZnGa2O4 (: Mn) provided in the present invention and a fluorescent film using the same can not only emit a fluorescent film at low voltage when used as an anode plate in the FED or VFD, but also has a long lifespan. The effect can be extended.
Claims (12)
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| KR100365583B1 (en) * | 2001-07-18 | 2002-12-26 | 이엘코리아 주식회사 | Phosphors and method for fabricating the same |
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| JPS5530176A (en) * | 1978-08-25 | 1980-03-03 | Matsushita Electric Ind Co Ltd | Fluorescent display device |
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| JPS5530176A (en) * | 1978-08-25 | 1980-03-03 | Matsushita Electric Ind Co Ltd | Fluorescent display device |
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| KR100365583B1 (en) * | 2001-07-18 | 2002-12-26 | 이엘코리아 주식회사 | Phosphors and method for fabricating the same |
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