KR20010063937A - A oxide-based red phosphor for fluorescent display and a preparation method thereof - Google Patents
A oxide-based red phosphor for fluorescent display and a preparation method thereof Download PDFInfo
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Abstract
Description
본 발명은 디스플레이 소자 기술에 관한 것으로, 특히 형광디스플레이(fluorescent display)용 적색 형광체 및 그 제조방법에 관한 것이다.TECHNICAL FIELD The present invention relates to display device technology, in particular red for fluorescent displays. The present invention relates to a phosphor and a method of manufacturing the same.
형광 디스플레이, 특히 전계방출 디스플레이(Field Emission Display, FED)는 브라운관과 동일한 원리로 동작되는 평판 디스플레이로서, 열전자 대신에 전계에 의해 전자를 방출하는 전계방출 소자 어레이 패널인 음극판(cathod plate)과, 전자를 받아 빛을 방출하는 형광판 패널인 양극판(anode plate)이 일정한 간격을 두고 고진공으로 패키징되어 구성된다.Fluorescent displays, in particular field emission displays (FEDs), are flat panel displays operated on the same principle as CRTs, including cathode plates (cathod plates), which are field emission device array panels that emit electrons by electric fields instead of hot electrons, and The anode plate, which is a fluorescent panel that emits light, is packaged in high vacuum at regular intervals.
기존의 브라운관에는 일반적으로 색순도가 좋고 발광효율이 높은 황화물계 형광체가 주로 사용되고 있다. 그러나, 전계방출 디스플레이에서는 음극판과 양극판의 거리가 짧아 브라운관에서와 같이 10 kV 이상의 고전압을 사용할 경우에는 방전이 일어나므로 5kV 이하의 저전압을 사용하며, 특히 1 kV 이하의 전압에서 작동 가능한 FED를 개발하기 위해 전세계적으로 다양한 연구가 이루어지고 있다.In the conventional CRT, sulfide-based phosphors having good color purity and high luminous efficiency are mainly used. However, in the field emission display, the distance between the negative electrode plate and the positive electrode plate is short, so when a high voltage of 10 kV or more is used as in a CRT, discharge occurs, so a low voltage of 5 kV or less is used, and in particular, to develop a FED that can operate at a voltage of 1 kV or less. For this purpose, various studies are being conducted worldwide.
한편, 전자의 에너지가 1 kV 이하로 낮을 경우, 전자는 형광체 표면으로부터 50nm 이하의 깊이에만 주사가 가능하므로 저전압 동작 FED용 형광체의 효율 특히, 휘도(luminescence)가 고전압을 사용하는 브라운관의 경우에 비해 크게 떨어지며, 형광체의 표면 상태가 형광체 발광효율에 크게 영향을 미친다는 문제점이 있었다.On the other hand, when the energy of electrons is lower than 1 kV, electrons can be scanned only at a depth of 50 nm or less from the surface of the phosphor, so that the efficiency of the phosphor for low voltage operation FED, in particular, is higher than that of a CRT tube using high voltage. There is a problem that greatly falls, the surface state of the phosphor greatly affects the phosphor luminous efficiency.
특히, 브라운관에서 널리 사용되는 기존의 황화물계 적색 형광체인 Y2O2S:Eu3+는 FED용 형광체로 사용할 경우에 저전압에서의 발광효율이 낮고 색순도가 나쁠뿐만 아니라, 장시간 동안의 전자빔의 주사에 의해 황화물계 형광체로부터 소량의 황이 탈착되어 FED 패널과 같이 음극판과 양극판의 간격이 1mm 정도인 작은용적 내부의 진공도를 떨어뜨리거나 전계방출 어레이(Field Emitter Array, FEA)를 손상시켜 디스플레이의 성능을 저하시킨다는 문제점이 있었다.In particular, Y 2 O 2 S: Eu 3+ , a conventional sulfide-based red phosphor widely used in CRTs, has low luminous efficiency at low voltage and poor color purity when used as a phosphor for FED, and also scans an electron beam for a long time. The small amount of sulfur is desorbed from the sulfide-based phosphors, and as in the case of the FED panel, the degree of vacuum in the small volume of 1 mm between the cathode and anode plates is reduced or the field emitter array (FEA) is damaged. There was a problem of lowering.
최근에는, 이와 같은 문제점을 해결하기 위하여 황의 탈착 위험이 없는 산화물계 형광체인 Y2O3:Eu3+등을 사용하거나, 표면처리된 Y2O2S:Eu3+등을 사용하여 저전압 구동 FED용 적색 형광체를 제조하는 기술이 제안되었다[미국특허 제5,525,259호].Recently, in order to solve such a problem, low voltage driving is performed using Y 2 O 3 : Eu 3+ or the like, which is an oxide-based phosphor that does not have a risk of desorption of sulfur, or using Y 2 O 2 S: Eu 3+ , which is surface-treated. A technique for producing a red phosphor for FED has been proposed (US Pat. No. 5,525,259).
이 기술에 따르면, 수분에 대해 내성이 강한 형광체를 제조하기 위해 산화 이트륨, 산화 유로퓸과 융제(flux)를 혼합하여 소성한 후, 소성된 형광체를 평균입도가 쿨터 카운터(Coulter Counter) 값으로 5보다 크게 분쇄하여 입도를 선별한 다음, 얻어진 Y2O3:Eu3+입자의 표면에 화학증기증착법을 사용하여 감마 알루미나를 코팅함으로써 Y2O3:Eu3+램프 형광체를 제조하였다.According to this technique, after firing by mixing yttrium oxide, europium oxide, and flux to produce a phosphor that is resistant to moisture, the calcined phosphor has an average particle size greater than 5 as the Coulter Counter value. After pulverizing to select a particle size, a Y 2 O 3 : Eu 3+ lamp phosphor was prepared by coating gamma alumina on the surface of the obtained Y 2 O 3 : Eu 3+ particles by chemical vapor deposition.
또한, K. G. Cho 연구팀은 펄스 레이저 증착법을 이용하여 (100) 실리콘 웨이퍼와 다이아몬드 증착된 실리콘 웨이퍼 상에 유로퓸(Eu)이 활성화된 산화이트륨(Eu:Y2O3) 형광체 박막을 증착하여 적색 박막 형광체를 제조하는 기술을 제안한 바 있다[K. G. Cho et al, "Improved luminescence properties of pulsed laser deposited Eu:Y2O3thin film", Appl. Phys. Lett., 71(23), 3335-3337, 1997].In addition, KG Cho's team deposited a thin film of europium (Eu) activated yttrium oxide (Eu: Y 2 O 3 ) phosphor on a (100) silicon wafer and a diamond deposited silicon wafer using pulse laser deposition. It has been proposed a technique for preparing a [KG Cho et al, "Improved luminescence properties of pulsed laser deposited Eu: Y 2 O 3 thin film", Appl. Phys. Lett., 71 (23), 3335-3337, 1997].
그러나, 상기의 종래기술 중에서 Y2O2S:Eu3+등을 표면처리하여 형광체를 제조하는 방법은 그 제조공정이 복잡할 뿐 아니라 경제성이 떨어진다. 한편, 산화물계인 Eu:Y2O3형광체의 경우에는 저전압에서 휘도가 낮고 색순도가 떨어지며 장시간 전자주사에 의해 열화 현상(aging effect)이 일어나므로 저전압 구동 형광디스플레이용 적색 형광체로 사용하기에는 한계가 있었다.However, the method of manufacturing phosphors by surface treatment of Y 2 O 2 S: Eu 3+ and the like in the above-described prior art is not only complicated in the manufacturing process but also inferior in economic efficiency. On the other hand, the Eu: Y 2 O 3 phosphor, which is an oxide-based phosphor, has low luminance at low voltage, low color purity, and a aging effect caused by electron injection for a long time.
본 발명의 주된 목적은, 장시간의 전자 주사에 대해서도 황의 탈착이 일어나지 않고 열화 현상이 적어 저전압에서도 높은 발광효율과 높은 색순도를 갖는 형광 디스플레이용 적색 형광체를 제공함에 있다.The main object of the present invention is red for fluorescent display, which has no desorption of sulfur even with prolonged electron scanning, less deterioration, and high luminous efficiency and high color purity even at low voltage. In providing a phosphor.
본 발명의 다른 목적은, 상기한 형광 디스플레이용 적색 형광체를 간단하면서도 경제적으로 제조할 수 있는 제조방법을 제공함에 있다.Another object of the present invention is to provide a manufacturing method which can produce the above-mentioned red phosphor for fluorescent display simply and economically.
도 1은 SrTiO3에 (1 mol% Li+)과 (1 mol% Pr3+, 8 mol% Ga3+)가 첨가된 SrTiO3계 형광체의 X-선 회절(XRD) 스펙트럼.Figure 1 is a SrTiO 3 (1 mol% Li +) and (1 mol% Pr 3+, 8 mol% Ga 3+) The X- ray diffraction (XRD) spectrum of the 3-base phosphor doped SrTiO.
도 2는 소성 온도에 따른 Li+첨가된 SrTi1-xGaxO3:Pr3+형광체의 광루미느센스(PL) 여기 및 방출 스펙트럼.FIG. 2 shows photoluminescence (PL) excitation and emission spectra of Li + added SrTi 1-x Ga x O 3 : Pr 3+ phosphors with firing temperature.
도 3은 첨부된 도면 도 3은 본 발명의 일 실시예에 따라 제조된 Li+첨가된 SrTi1-xGaxO3:Pr3+형광체와 상용 CRT 형광체(Y2O2S:3+)의 음극선루미느센스(CL) 비교 스펙트럼.3 is an accompanying drawing. FIG. 3 is a Li + added SrTi 1-x Ga x O 3 : Pr 3+ phosphor prepared according to an embodiment of the present invention and a commercial CRT phosphor (Y 2 O 2 S: 3+ ). Cathode luminescence (CL) comparison spectrum.
상기의 목적을 달성하기 위한 본 발명의 특징적인 형광 디스플레이용 형광체는, SrTiO3모체에 적어도 하나 이상의 1가 알카리금속 원소와 둘 이상의 3가 금속 원소를 포함하는 것을 특징으로 하며, 하기의 화학식 1 또는 화학식 2로 표현된다.Characteristic fluorescent display phosphor of the present invention for achieving the above object, characterized in that at least one monovalent alkali metal element and at least two trivalent metal elements in the SrTiO 3 matrix, and the formula It is represented by Formula (2).
또한, 본 발명의 특징적인 형광 디스플레이용 형광체 제조방법은, 하기의 화학식 1 또는 화학식 2로 표현되는 조성에 따라, 스트론튬 산화물과, 티타늄 산화물과, Li, Na, K 중에서 선택된 적어도 1종의 1가 알카리금속의 산화물과, Ga, Al, In, B 중에서 선택된 적어도 1종 이상의 3가 금속의 산화물을 프라세오디뮴(Pr) 산화물 또는 프라세오디뮴염의 수용액에 소정의 용매를 가하여 혼합하는 제1 단계와, 상기 제2 단계에서 형성된 혼합물을 소성하는 제2 단계를 포함하여 이루어진다.In addition, the characteristic phosphor manufacturing method for a fluorescent display of the present invention, at least one monovalent selected from strontium oxide, titanium oxide, Li, Na, K according to the composition represented by the following formula (1) or (2) A first step of mixing an alkali metal oxide with at least one oxide of a trivalent metal selected from Ga, Al, In, and B by adding a predetermined solvent to an aqueous solution of praseodymium (Pr) oxide or praseodymium salt, and the second step. And a second step of firing the mixture formed in the step.
본 발명은 도판트(dopant)로 Ga3+, Li+을 첨가함으로써 초기 반응물인 SrCO3또는 SrO와 TiO2로부터 합성되는 SrTiO3의 구조를 변형시켜 활성제(activator)인 Pr3+의 여기 효율을 증가시키게 되며, 이에 따라 형광체의 휘도를 향상시킬 뿐 아니라 단일 방출 밴드를 갖게 하므로 우수한 색순도를 갖는 적색 형광체를 얻을 수 있다. 즉, 본 발명에 따르면, 초기 반응물인 SrCO3또는 SrO와 TiO2의 조성비를 기존의 1:1의 비율로 맞추는 대신에, Ga3+, Li+를 첨가하여 ABO3결정구조를 갖는 페로브스카이트(perovskite)의 A 또는 B 위치에 있는 Sr 또는 Ti의 일부를 Ga3+과 Li+로 치환하여 미세구조를 변형시켜 Pr3+의 여기 효율을 증가시키고, Li+의 첨가량과 반응온도를 조절하여 입도(입자의 크기)와 형상(입자의 모양)을 조절함으로써 휘도를 보다 향상 시킬 수 있다.The present invention relates to Ga as a dopant.3+, Li+By adding the initial reactant SrCO3Or SrO and TiO2Synthesized from SrTiO3Pr, an activator, by modifying its structure3+This increases the excitation efficiency of, thereby improving the luminance of the phosphor and having a single emission band, thereby obtaining a red phosphor having excellent color purity. That is, according to the present invention, the initial reactant SrCO3Or SrO and TiO2Instead of adjusting the composition ratio of to 1: 1 ratio, Ga3+, Li+By adding ABO3A portion of Sr or Ti at the A or B position of the perovskite having a crystal structure3+and Li+Pr by modifying the microstructure3+To increase the excitation efficiency of+The brightness can be further improved by adjusting the addition amount and the reaction temperature of the particle size (particle size) and the shape (particle shape).
이하, 본 발명의 바람직한 실시예에 따른 형광 디스플레이용 적색 형광체 제조방법과 이 제조방법으로부터 얻어진 형광체의 특성을 첨부도면을 참조하여 보다 상세히 설명한다.Hereinafter, a red for fluorescent display according to a preferred embodiment of the present invention The phosphor manufacturing method and the characteristics of the phosphor obtained from this manufacturing method will be described in more detail with reference to the accompanying drawings.
우선, 본 발명에 따른 형광 디스플레이용 적색 형광체는 하기의 화학식 1과 같이 나타낼 수 있다.First, the red phosphor for a fluorescent display according to the present invention can be represented by the following formula (1).
이때, M은 1가 알카리금속 원소, N은 3가 금속 원소, 0≤x≤0.3, 0≤y≤0.1, 0≤z≤0.1이다.In this case, M is a monovalent alkali metal element, N is a trivalent metal element, 0 ≦ x ≦ 0.3, 0 ≦ y ≦ 0.1, and 0 ≦ z ≦ 0.1.
본 실시예에 따른 형광 디스플레이용 적색 형광체 제조방법은, 우선 상기의 화학식 1로 표현되는 조성에 따라 일정량의 SrCO3,TiO2, ZnO, Ga2O3와 물에 용해된 PrCl3(H2O)7을 알코올이 담긴 막자 사발에 투입하고, 균일하게 잘 혼합시킨 후 건조시킨다.In the method of manufacturing a red phosphor for a fluorescent display according to the present embodiment, first, a predetermined amount of SrCO 3 , TiO 2 , ZnO, Ga 2 O 3 and PrCl 3 (H 2 O) dissolved in water according to the composition represented by Chemical Formula 1 ) 7 is poured into a mortar with alcohol, mixed well and dried.
다음으로, 건조된 혼합물을 알루미나 용기에 담고 전기 소성로에서1,000∼1300℃의 온도에서 10시간 이하로 소성시켜 SrTi1-x-yMxNyO3:zPr3+(SrTiO3:Pr3+, Ga3+, Li+)을 갖는 적색 형광체를 얻는다. 한편, 소성 온도를 다수의 구간으로 나누어 각 구간별(예컨대, 600℃에서 1∼4 시간 소성하고, 900℃에서 1~6 시간 소성한 후 1000∼1300℃의 온도에서 2∼6시간)로 소성을 실시할 수 있으며, 이러한 소성을 통해 최종 생성물인 형광체 분말의 표면 조성, 형광체 분말의 입도 및 형상을 최적화함으로써, SrTiO3계 형광체의 광특성을 극대화할 수 있다. 물론 소성은 600∼1300℃의 온도에서 일단계로 수행할 수도 있다.Next, the dried mixture was placed in an alumina container and fired in an electric sintering furnace at a temperature of 1,000 to 1300 ° C. for 10 hours or less. SrTi 1-xy M x N y O 3 : zPr 3+ (SrTiO 3 : Pr 3+ , Ga 3+ , Li + ) to obtain a red phosphor. On the other hand, the firing temperature is divided into a plurality of sections and fired at each section (for example, 1 to 4 hours at 600 ° C, 1 to 6 hours at 900 ° C, and 2 to 6 hours at a temperature of 1000 to 1300 ° C). Through such firing, the optical composition of the SrTiO 3 -based phosphor can be maximized by optimizing the surface composition of the final product, the particle size and shape of the phosphor powder. Of course, firing may be performed in one step at a temperature of 600 ~ 1300 ℃.
첨부된 도면 도 1은 SrTiO3에 (1 mol% Pr3+)와 (1 mol% Pr3++ 8 mol% Ga3+)이 첨가된 SrTiO3의 형광체에 대한 X-선 회절(XRD) 스펙트럼을 나타낸 것이다. 이를 참조하면 Ga3+을 8 mol% 첨가하였을 경우, 첨가하지 않았을 때와 비교하여 회절 스펙트럼의 변화가 없으며, 이로부터 Ga3+의 첨가에 따른 구조 변화가 일어나지 않은 것을 확인할 수 있었다.In the accompanying drawings Figure 1 is SrTiO 3 (1 mol% Pr 3+ ) and (1 mol% Pr 3+ + 8 mol% Ga 3+) X- ray diffraction (XRD) spectrum of the phosphor of the addition of SrTiO 3 It is shown. Referring to this, when 8 mol% of Ga 3+ was added, there was no change in the diffraction spectrum as compared with the case where no addition of Ga 3+ , and it was confirmed that no structural change occurred due to the addition of Ga 3+ .
첨부된 도면 도 2는 소성 온도에 따른 Li+첨가된 SrTi1-xGaxO3:Pr3+형광체의 광루미느센스(PL) 여기 및 방출 스펙트럼을 나타낸 것이다. 이를 참조하면 여기 밴드는 200∼388nm의 대역(A-대역)과 450∼500nm의 대역(B-대역)을 갖는 영역으로 나눌 수 있는데, A-대역은 SrTiO3모체가 여기되어 여기 에너지가 Pr3+이온에 전달하는 것에 기인한 것이고, B-대역은 Pr3+이온의 직접 여기에 기인한 것이다.FIG. 2 shows photoluminescence (PL) excitation and emission spectra of Li + added SrTi 1-x Ga x O 3 : Pr 3+ phosphors depending on firing temperature. Referring to this, the excitation band can be divided into a region having a band of 200 to 388 nm (A-band) and a band of 450 to 500 nm (B-band), where the SrTiO 3 matrix is excited and the excitation energy is Pr 3. It is due to the transfer to + ions, and the B-band is due to the direct excitation of Pr 3+ ions.
첨부된 도면 도 3은 본 발명의 일 실시예에 따라 제조된 Li+첨가된 SrTi1-xGaxO3:Pr3+형광체와 상용 CRT 형광체(Y2O2S:3+)의 음극선루미느센스 비교 스펙트럼을 도시한 것으로, 최적의 Pr3+, Ga3+, Li+를 첨가하여 얻은 SrTiO3:Pr3+, Ga3+, Li+형광체와 상용 CRT 적색 형광체인 Y2O2S:Eu를 가속전압을 800V로 조정하여 측정한 음극선 루미느센스(CL) 방출 스펙트럼을 나타내고 있다. 이를 참조하면 본 발명에 따른 형광체의 휘도 세기는 상용 CRT 형광체에 비해 약 2배인 것을 확인할 수 있다.3 is a cathode ray luminescence of Li + added SrTi 1-x Ga x O 3 : Pr 3+ phosphor and a commercial CRT phosphor (Y 2 O 2 S: 3+ ) prepared according to an embodiment of the present invention. that showing the slow sense compared spectra, the optimal Pr 3+, Ga 3+, SrTiO 3 is obtained by the addition of Li +: Pr 3+, Ga 3+, Li + is compatible with the CRT phosphors red phosphor Y 2 O 2 S : It shows cathode luminescence (CL) emission spectrum measured by adjusting Eu to acceleration voltage to 800V. Referring to this, it can be seen that the luminance intensity of the phosphor according to the present invention is about twice that of a commercial CRT phosphor.
한편, 색순도에 대한 실험을 수행한 결과, 색순도의 경우에도 상용 형광체가 x=0.642, y=0.345의 값을 갖는데 비해, 본 발명에 따라 제조된 형광체의 경우에는 x=0.660, y=0.336의 값을 나타내었다.On the other hand, as a result of the experiment on the color purity, even in the case of the color purity, the commercial phosphor has a value of x = 0.642, y = 0.345, whereas for the phosphor prepared according to the present invention x = 0.66, y = 0.336 Indicated.
이상에서 설명한 본 발명은 전술한 실시예 및 첨부된 도면에 의해 한정되는 것이 아니고, 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 여러 가지 치환, 변형 및 변경이 가능하다는 것이 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 있어 명백할 것이다.The present invention described above is not limited to the above-described embodiments and the accompanying drawings, and various substitutions, modifications, and changes can be made in the art without departing from the technical spirit of the present invention. It will be apparent to those of ordinary knowledge.
본 발명에 따른 형광체는 열적 자극이나 전자 주사 등의 기타 외부 자극에 대해 안전한 산화물계 형광체이므로, 본 발명에 따른 페로브스카이트 구조를 갖는 SrTiO3계 산화물 형광체를 형광디스플레이에 적용하거나 FED 형광체의 양극판으로 사용하게 되면 장시간의 전자 주사에 의한 형광체의 파괴를 방지할 수 있어 음극판과 양극판 사이에 있는 공간의 진공도를 깨뜨리지 않으므로 패널의 성능을 장시간 유지할 수 있다. 또한, 본 발명에 따른 형광체는 형광체 분말의 입도와 형상 조절이 가능하고, 저 전압에서도 휘도가 높고 당일 방출 밴드를 가져 색순도(방출 밴드 파장; 615nm: 색좌표; x=0.660, y=0.336)가 우수하므로 형광 디스플레이나 고성능 FED 패널 제조에 효과적으로 사용될 수 있다. 따라서, 본 발명에 따른 형광체는 형광 디스플레이에 적용하여 고휘도, 고선명도 등과 같은 우수한 성능을 발휘할 수 있으며, 저전압 FED의 상용화에도 기여할 것으로 기대된다.Since the phosphor according to the present invention is an oxide-based phosphor that is safe against thermal stimulation or other external stimuli such as electron scanning, the SrTiO 3 -based oxide phosphor having a perovskite structure according to the present invention may be applied to a fluorescent display or a cathode plate of an FED phosphor. In this case, it is possible to prevent the destruction of the phosphor by prolonged electron scanning, and thus to maintain the performance of the panel for a long time because it does not break the vacuum degree of the space between the negative electrode plate and the positive electrode plate. In addition, the phosphor according to the present invention is capable of controlling the particle size and shape of the phosphor powder, and has a high luminance even at low voltage, and has an emission band on the same day, thereby providing excellent color purity (emission band wavelength; 615 nm: color coordinate; x = 0.660, y = 0.336). Therefore, it can be effectively used for manufacturing fluorescent displays or high performance FED panels. Therefore, the phosphor according to the present invention can be applied to a fluorescent display can exhibit excellent performance, such as high brightness, high definition, etc., and is expected to contribute to the commercialization of low-voltage FED.
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