KR20020003886A - Fluorescent Material of Lanthanum Gallate and Method for Producing The Same - Google Patents

Fluorescent Material of Lanthanum Gallate and Method for Producing The Same Download PDF

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KR20020003886A
KR20020003886A KR1020000034031A KR20000034031A KR20020003886A KR 20020003886 A KR20020003886 A KR 20020003886A KR 1020000034031 A KR1020000034031 A KR 1020000034031A KR 20000034031 A KR20000034031 A KR 20000034031A KR 20020003886 A KR20020003886 A KR 20020003886A
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oxide
lanthanum
red phosphor
europium
phosphor
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KR100348207B1 (en
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박희동
김창해
박정규
김경화
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김충섭
한국화학연구원
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    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate

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Abstract

PURPOSE: A lanthanum gallate-based red fluorescent substance and its preparation method are provided, to improve the brightness at a low velocity electron ray and the stability under the high vacuum. CONSTITUTION: The lanthanum gallate-based red fluorescent substance is represented by La1-xGaO3;Eux, wherein x is a mole fraction of Eu to La and 0.0005<= x<=0.5, and preferably 0.05<= x <=0.2. The method comprises the steps of mixing lanthanum oxide(La2O3), gallium oxide(Ga2O3) and europium oxide(Eu2O3) with a mole fraction of Eu to La being 0.0005-0.5 to prepare a mixture; sintering the mixture at a temperature of 1,100-1,600 deg.C, preferably 1,200-1,400 deg.C at atmosphere to obtain a sintered one; and pulverizing the sintered one to obtain a red fluorescent substance.

Description

란탄갈레이트계 적색 형광체 및 그 제조방법{Fluorescent Material of Lanthanum Gallate and Method for Producing The Same}Lanthanum Gallate Red Phosphor and Method for Producing Them {Fluorescent Material of Lanthanum Gallate and Method for Producing The Same}

본 발명은 란탄갈레이트계 적색 형광체 및 그 제조방법에 관한 것으로서, 더욱 상세하게는 형광체 모체인 란탄갈레이트(LaGaO3)에 활성제로 유로피움옥사이드를 첨가함으로써 저속전자선에서 발광휘도가 우수하고 고진공에서도 안정한 물성을 가지며 저전압 전자선 여기에 의해 구동하는 전계 방출 디스플레이(Field Emission Display, FED)에 적합한 란탄갈레이트계 적색 형광체 및 그 제조방법에 관한 것이다.The present invention relates to a lanthanum gallate-based red phosphor and a method of manufacturing the same, and more particularly, by adding europium oxide as an activator to a lanthanide gallate (LaGaO 3 ), which is a phosphor matrix, excellent luminous luminance in a low-speed electron beam The present invention relates to a lanthanumate-based red phosphor suitable for field emission displays (FEDs) having stable physical properties and driven by low voltage electron beam excitation, and a method of manufacturing the same.

전계 방출 디스플레이(FED)는 정보표시용 디스플레이로 가장 많이 사용되어온 음극선관(CRT)의 단점을 보완, 대체할 수 있는 차세대 평판 디스플레이의 하나로서, 진공 평판 음극선 튜브를 사용한 새로운 형태의 디스플레이이며, 이는 1 ㎸ 이하의 저전압 음극선 여기를 기본으로 한다.Field emission displays (FEDs) are a new generation of flat panel displays that can supplement and replace the shortcomings of cathode ray tubes (CRTs), which are most often used as information displays, and are a new type of display using vacuum flat cathode tube. Based on low voltage cathode excitation below 1 kW.

그런데, 약 1 kV 이하의 양극 구동전압을 갖는 FED를 구동시키기 위해서는 FED용 형광체로서 저속 전자선용 형광체가 필요하다. 현재 사용되고 있는 FED용 형광체 중에서 대표적인 ZnO:Zn 형광체는 발광영역이 매우 넓어서 천연색 디스플레이로서 적용하기에는 부적합한 문제가 있다. 또한, 적색 형광체로서 (Zn, Cd)S:Ag, Cl 등과 같은 유화물 형광체는 황화합물이 함유되어 있어서 이를 사용하는 경우 음극으로부터 방출된 전자가 가속되어 황화물 형광체층에 충돌할 때 형광체층을 발광시키는 작용 외에 형광체층 표면을 분해하는 작용 및 형광체 자체의 분해로 인하여 디바이스의 여기원에 나쁜영향을 주는 것으로 알려져 있다.By the way, in order to drive FED which has an anode drive voltage of about 1 kV or less, fluorescent substance for low-speed electron beam is needed as fluorescent substance for FED. Representative ZnO: Zn phosphors among the currently used FED phosphors have a wide light emitting area, which is not suitable for application as a color display. In addition, as a red phosphor, sulfide phosphors such as (Zn, Cd) S: Ag, Cl, etc. contain sulfur compounds, and when used, the phosphor phosphor emits a phosphor layer when the electrons emitted from the cathode are accelerated and collide with the sulfide phosphor layer. In addition, it is known to adversely affect the excitation source of the device due to the decomposition of the surface of the phosphor layer and the decomposition of the phosphor itself.

현재 널리 알려져 있는 적색 형광체로는 Y2O3:Eu계 형광체가 있으나, 이는 절연성을 높이기 위하여 도전물질로 In2O3를 다량 혼합하여 사용함으로써 In2O3를 통하여 흐르는 무효전류가 많아져 저전압 구동영역에서의 발광 효율이 낮아지며, 신뢰성도 저하되는 문제점을 가지고 있다.Currently widely known red phosphors include Y 2 O 3 : Eu-based phosphors. However, in order to improve insulation, a large amount of In 2 O 3 is used as a conductive material to increase the reactive current flowing through In 2 O 3 . The luminous efficiency in the driving region is lowered and the reliability is also lowered.

이에 본 발명자들은 란탄옥사이드(La2O3)와 갈륨옥사이드(Ga2O3)를 형광체 원료로 사용한 란탄갈레이트(LaGaO3)를 새로운 모체로 사용하고 여기에 활성제로 유로피움옥사이드를 첨가함으로써 FED용으로 적합한 적색 형광체를 제조할 수 있음을 알게 되어 본 발명을 완성하였다.Therefore, the present inventors use lanthanum gallate (LaGaO 3 ) using lanthanum oxide (La 2 O 3 ) and gallium oxide (Ga 2 O 3 ) as phosphor raw materials as a new matrix and add europium oxide as an activator thereto. The present invention has been completed by knowing that a red phosphor suitable for the purpose can be prepared.

따라서, 본 발명은 저속전자관에서 발광휘도가 우수하고, 고진공에서도 안정한 물성을 가지며, 전계 방출 디스플레이에 적합한 새로운 란탄갈레이트계 적색 형광체 및 그 제조방법을 제공하는데 그 목적이 있다.Accordingly, an object of the present invention is to provide a novel lanthangalate-based red phosphor suitable for a field emission display, having excellent luminescence brightness in a low-speed electron tube, having stable physical properties even at high vacuum, and a method of manufacturing the same.

도 1은 본 발명의 란탄갈레이트계 적색 형광체에 있어서 소성온도에 따른 회절강도 및 회절각을 나타낸 그래프이고,1 is a graph showing the diffraction intensity and the diffraction angle according to the firing temperature in the lanthangalate-based red phosphor of the present invention,

도 2는 본 발명의 란탄갈레이트계 적색 형광체에 있어서 Eu의 첨가량에 따른 자외선 발광 스펙트럼 그래프이고,2 is an ultraviolet emission spectrum graph according to the amount of Eu added in the lanthangalate-based red phosphor of the present invention,

도 3은 본 발명의 란탄갈레이트계 적색 형광체에 있어서 Eu의 첨가량에 따른 음극선 발광 스펙트럼을 나타낸 그래프이다.3 is a graph showing a cathode emission spectrum according to the amount of Eu added in the lanthanide-based red phosphor of the present invention.

이와 같은 목적을 달성하기 위하여, 본 발명에 따르면, 일반식 La1-XGaO3:EuX(여기서, La에 대한 Eu의 몰분율 X는 0.0005≤X≤0.5 이다)로 표시되는 란탄갈레이트계 적색형광체가 제공된다.In order to achieve the above object, in accordance with the present invention, a lanthanumate red represented by the general formula La 1-X GaO 3 : Eu X (wherein the mole fraction X of Eu to La is 0.0005 ≦ X ≦ 0.5) Phosphors are provided.

또한, 본 발명에 따르면, 란탄옥사이드(La2O3), 갈륨옥사이드(Ga2O3) 및 유로피움옥사이드(Eu2O3)를 란탄에 대한 유로피움의 몰분율이 0.0005내지 0.5가 되도록 칭량, 혼합하여 혼합물을 얻는 단계, 상기 혼합체를 1100내지 1600℃의 대기중에서 1∼5시간 소성하여 소성물을 얻는 단계, 및 상기 소성물을 분쇄하여 적색형광체를 얻는 단계를 포함하는 것을 특징으로 하는 란탄갈레이트계 적색형광체의 제조방법이 제공된다.According to the present invention, lanthanum oxide (La 2 O 3 ), gallium oxide (Ga 2 O 3 ) and europium oxide (Eu 2 O 3 ) is weighed so that the mole fraction of europium to lanthanum is 0.0005 to 0.5, Mixing to obtain a mixture, calcination of the mixture in an atmosphere of 1100 to 1600 ° C. for 1 to 5 hours to obtain a fired product, and pulverizing the fired product to obtain a red phosphor. A method for producing a rate-based red phosphor is provided.

본 발명에서, 활성제로 첨가되는 유로피움옥사이드의 몰분율은 형광체 원료물질 중의 란탄옥사이드에 대하여 0.0005∼0.5몰, 바람직하기로는 0.05∼0.2몰로 첨가하는데, 만일 그 첨가량이 0.0005몰 미만이면 활성제로서의 기능을 하기에 충분한 양이 되지 못하여, 0.5몰을 초과하면 농도 소광 현상에 따른 휘도 저하가 일어난다.In the present invention, the mole fraction of europium oxide added as the activator is added in an amount of 0.0005 to 0.5 mol, preferably 0.05 to 0.2 mol, based on lanthanum oxide in the phosphor raw material. If the amount is not sufficient, it exceeds 0.5 mol, the luminance decreases due to the concentration quenching phenomenon occurs.

한편, 본 발명에 의한 란탄갈레이트계 적색형광체의 제조방법에 있어서는, 란탄옥사이드와 갈륨옥사이드를 형광체 원료로 사용하고, 여기에 활성제로서 유로피움옥사이드를 첨가하여 혼합한다. 이 혼합체는 100∼150℃에서 약 24시간 건조 후, 충분한 합성반응이 이루어질 수 있도록 1,100∼1,600℃, 바람직하기로는 1,200내지 1,400℃의 온도범위에서 1내지 5시간동안 소성을 한다.On the other hand, in the method for producing a lanthanum gallate red phosphor according to the present invention, lanthanum oxide and gallium oxide are used as phosphor raw materials, and europium oxide is added and mixed therein as an activator. The mixture is dried at 100 to 150 ° C. for about 24 hours, and then fired for 1 to 5 hours at a temperature range of 1,100 to 1,600 ° C., preferably 1,200 to 1,400 ° C., so that a sufficient synthesis reaction can be achieved.

본 발명에서 소성온도가 1100℃미만이면 La4Ga2O9와 같은 란탄갈레이트의 화합물 결정이 생성되어 발광효율이 감소하고 반면에, 1600℃를 초과하면 란탄갈레이트 결정이 불규칙적이며 조대한 입자로 성장하여 휘도가 저하하므로 바람직하지 않다.In the present invention, when the firing temperature is less than 1100 ° C., a compound crystal of lanthanide gallate such as La 4 Ga 2 O 9 is produced, and thus the luminous efficiency is reduced. It is not preferable because it grows to lower brightness.

이렇게 소성하여 얻어진 소성물은 냉각후 충분히 분쇄하여 분말상의 적생형광체를 얻는다.The calcined product thus obtained is pulverized sufficiently after cooling to obtain a powdery red phosphor.

이와 같은 본 발명을 실시예에 의거하여 상세하게 설명하겠는 바, 본 발명이 실시예에 한정되는 것은 아니다.Although this invention is demonstrated in detail based on an Example, this invention is not limited to an Example.

(실시예 1)(Example 1)

La0.875GaO3:Eu0.125형광체의 제조 La0.875GaO3: Eu0.125Preparation of Phosphor

란탄옥사이드(La2O3) 0.875mol,갈륨옥사이드(Ga2O3) 1mol, 유로피움옥사이드(Eu2O3) 0.125mol의 비율로 평량하고 이것을 마노 유발을사용하여아세톤 중에서 충분히 고르게 혼합하였다. 혼합한 시료를 오븐을 사용하여 130℃에서 24시간동안 건조하였다. 얻어진 혼합물을 고순도 알루미나 보트에 넣고 전기로를 사용하여 대기 중에서 1,100℃, 1,200℃, 1,300℃ 및 1,400℃로 3시간동안 각각 소성하였다. 소성 후에 얻어진 소성물을 충분히 분쇄처리하여 La0.875GaO3:Eu0.125로 표시되는 적색 형광체를 얻었다.Lanthanum oxide (La 2 O 3 ) 0.875 mol, gallium oxide (Ga 2 O 3 ) 1 mol, europium oxide (Eu 2 O 3 ) in a ratio of 0.125 mol and the basis weight was mixed evenly in acetone using agate mortar. The mixed samples were dried at 130 ° C. for 24 hours using an oven. The resulting mixture was placed in a high purity alumina boat and calcined at 1,100 ° C., 1,200 ° C., 1,300 ° C. and 1,400 ° C. for 3 hours in the air using an electric furnace. The fired product obtained after the firing was sufficiently milled to obtain a red phosphor represented by La 0.875 GaO 3 : Eu 0.125 .

얻어진 적색 형광체의 회절각에 따른 회절강도를 측정하고 그 결과를 도 1에 나타내었다.The diffraction intensity according to the diffraction angle of the obtained red phosphor was measured and the results are shown in FIG. 1.

도 1에 나타낸 바와 같이, 본 발명의 란탄갈레이트계 적색 형광체는 소성온도에 따라 La4Ga2O9상과 같은 다른 조성의 란탄갈레이트계 화합물이 생성되었다. 즉, 소성온도가 낮아질수록 LaGaO3와는 상이한 상이 출현하기 시작하여 1100℃이하에서는 La4Ga2O9의 피크빈도수가 점차 많아지게 됨을 알 수 있다.As shown in FIG. 1, the lanthanide gallate red phosphor of the present invention produced a lanthanide compound having a different composition, such as a La 4 Ga 2 O 9 phase, depending on the firing temperature. That is, as the firing temperature is lowered, a phase different from that of LaGaO 3 starts to appear, and the peak frequency of La 4 Ga 2 O 9 gradually increases at 1100 ° C. or lower.

(실시예 2)(Example 2)

Eu함량에 따른 적색형광체의 발광 스팩트럼 측정. Measurement of the emission spectrum of the red phosphor according to the Eu content.

란탄옥사이드에 대한 유로피움옥사이드의 몰분율을 각각 0.0005, 0.005, 0.125, 0.1, 0.2 0.3 및 0.4로 변화시키고, 소성온도를 1300℃로 한 것을 제외하고는 실시예 에서와 동일한 방법으로 La1-XGaO3:EuX적색형광체를 합성하였다.The molar fraction of europium oxide relative to lanthanum oxide was changed to 0.0005, 0.005, 0.125, 0.1, 0.2 0.3 and 0.4, respectively, and the la 1-X GaO was carried out in the same manner as in Example except that the calcination temperature was 1300 ° C. 3 : Eu X red phosphor was synthesized.

이렇게 하여 얻은 La1-XGaO3:EuX적색 형광체의 상대휘도를 254nm의 자외선으로 형광체를 여기시켜 발광 스펙트럼 측정하고 그 결과를 도 2에 나타내었다.The relative luminance of the thus obtained La 1-X GaO 3 : Eu X red phosphor was excited by 254 nm ultraviolet light to excite the phosphor, and the emission spectrum thereof was measured. The results are shown in FIG. 2.

도 2에서 보는 바와같이, 란탄에 대한 유로피움의 몰분율을 변화시킴에 따라 발광강도가 변화하게 되는데 유로피움의 몰분율이 0.125일 때 발광강도가 최고치를 나타냄을 알 수 있다.As shown in Figure 2, the emission intensity is changed by changing the mole fraction of europium to lanthanum, it can be seen that the emission intensity is the highest when the mole fraction of europium is 0.125.

도 3에 나타낸 바와 같이, 본 발명의 적색 형광체인 유로피움의 첨가량이 0.125mol이 될 때까지 발광휘도가 증가하며, 그 후에는 감소함을 알 수 있다.As shown in FIG. 3, the luminance of light emitted increases until the amount of europium, the red phosphor of the present invention, becomes 0.125 mol, and thereafter, decreases.

상술한 바와 같이 본 발명의 란탄갈레이트에 유로피움을 첨가한 적색 형광체는 음극선 발광소자의 새로운 모체로서 1 kV 이하의 저전압 전자선 여기 하에서 고휘도를 갖는다. 이는 황(S), 카드늄(Cd)을 포함하지 않는 산화물 형광체이므로 종래의 칼라 형광체에서 발생하는 유화물에 의한 음극의 오염 및 공해에 대한 문제점이 해결할 수 있는 효과가 있으므로 전계 방출 디스플레이에 적용할 수 있는 가능성이 매우 크다.As described above, the red phosphor in which europium is added to the lanthanumate of the present invention has a high luminance under excitation of a low voltage electron beam of 1 kV or less as a new matrix of cathode light emitting devices. Since it is an oxide phosphor that does not contain sulfur (S) and cadmium (Cd), there is an effect that can solve the problem of contamination and pollution of the cathode by the emulsion generated in the conventional color phosphor, which can be applied to the field emission display The possibilities are very large.

Claims (5)

일반식 La1-XGaO3:EuX(여기서, La에 대한 Eu의 몰분율 x는 0.0005≤X≤0.5 이다)로 표시되는 란탄갈레이트계 적색형광체.A lanthangalate-based red phosphor represented by general formula La 1-X GaO 3 : Eu X (wherein molar fraction x of Eu relative to La is 0.0005 ≦ X ≦ 0.5). 제 1항에 있어서, 상기 x는 0.05≤X≤0.2인 것을 특징으로 하는 란탄갈레이트계 적색형광체.The lanthanum gallate-based red phosphor of claim 1, wherein x is 0.05 ≦ X ≦ 0.2. 란탄옥사이드(La2O3), 갈륨옥사이드(Ga2O3) 및 유로피움옥사이드(Eu2O3)를 란탄에 대한 유로피움의 몰분율이 0.0005내지 0.5가 되도록 칭량, 혼합하여 혼합물을 얻는 단계, 상기 혼합체를 1100내지 1600℃의 대기중에서 소성하여 소성물을 얻는 단계, 및 상기 소성물을 분쇄하여 적색형광체를 얻는 단계를 포함하는 것을 특징으로 하는 란탄갈레이트계 적색형광체의 제조방법.Weighing and mixing lanthanum oxide (La 2 O 3 ), gallium oxide (Ga 2 O 3 ), and europium oxide (Eu 2 O 3 ) such that the mole fraction of europium to lanthanum is 0.0005 to 0.5, to obtain a mixture, Calcining the mixture in an air at 1100 to 1600 ° C. to obtain a fired product, and pulverizing the fired product to obtain a red phosphor. 제 3항에 있어서, 상기 소성온도는 1200내지 1400℃인 것을 특징으로 하는 란탄갈레이트계 적색형광체의 제조방법.The method of claim 3, wherein the firing temperature is 1200 to 1400 ℃. 제 3항에 있어서, 상기 유로피움의 몰분율은 0.05∼0.2인 것을 특징으로 하는 란탄갈레이트계 적색형광체의 제조방법.4. The method of claim 3, wherein the mole fraction of the europium is 0.05 to 0.2.
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US6761837B2 (en) * 2002-06-12 2004-07-13 General Electric Company Europium-activated phosphors containing oxides of rare-earth and group-IIIB metals and method of making the same
WO2011130926A1 (en) * 2010-04-23 2011-10-27 海洋王照明科技股份有限公司 Rare earth ion doped lanthanum gallate luminous material containing metal particles and preparation method thereof

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JP3425470B2 (en) * 1994-05-18 2003-07-14 化成オプトニクス株式会社 Red light emitting composition
US5601751A (en) * 1995-06-08 1997-02-11 Micron Display Technology, Inc. Manufacturing process for high-purity phosphors having utility in field emission displays
US5725801A (en) * 1995-07-05 1998-03-10 Adrian H. Kitai Doped amorphous and crystalline gallium oxides, alkaline earth gallates and doped zinc germanate phosphors as electroluminescent materials
KR20000008650A (en) * 1998-07-15 2000-02-07 김충섭 Method for preparing red fluorescent substance made of yttrium oxide derivatives

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6761837B2 (en) * 2002-06-12 2004-07-13 General Electric Company Europium-activated phosphors containing oxides of rare-earth and group-IIIB metals and method of making the same
WO2011130926A1 (en) * 2010-04-23 2011-10-27 海洋王照明科技股份有限公司 Rare earth ion doped lanthanum gallate luminous material containing metal particles and preparation method thereof
US8821759B2 (en) 2010-04-23 2014-09-02 Ocean's King Lighting Science & Technology Co., Ltd. Rare earth ion doped lanthanum gallate luminous material containing metal particles and preparation method thereof

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