KR930004373B1 - Preparation of geen fluorescent with excitation electron beam - Google Patents

Preparation of geen fluorescent with excitation electron beam Download PDF

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Publication number
KR930004373B1
KR930004373B1 KR1019890009620A KR890009620A KR930004373B1 KR 930004373 B1 KR930004373 B1 KR 930004373B1 KR 1019890009620 A KR1019890009620 A KR 1019890009620A KR 890009620 A KR890009620 A KR 890009620A KR 930004373 B1 KR930004373 B1 KR 930004373B1
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South Korea
Prior art keywords
electron beam
zinc oxide
firing
zno
phosphor
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KR1019890009620A
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Korean (ko)
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KR910003067A (en
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임익철
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삼성전관 주식회사
김정배
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/54—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing zinc or cadmium

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

The low speed excitation zinc-activated zinc oxide (ZnO:Zn) green light-emitting fluorescent material is mfd. by first-firing ZnO in the alumina crucible under the carbon atmosphere at 400-1100 deg.C for 0.5-6 hr, and second firing it at 500-1100 deg.C for 1-6 hr. The fluorescent material has a high luminance and long life.

Description

저속 전자선 여기 녹색형광체 제조방법Low speed electron beam excitation green phosphor manufacturing method

본 발명은 산화아연을 주제로 하는 저속 전자선 여기 녹색형광체의 제조방법에 관한 것으로서, 상세하게는 높은 휘도와 고른 결정입자를 가진 저속 전자선 여기 녹색형광체의 제조방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a method for producing a low speed electron beam-excited green phosphor based on zinc oxide, and more particularly, to a method for manufacturing a low-speed electron beam-excited green phosphor having high luminance and even crystal grains.

저속 전자선 여기 형광체로서는 황화물계 형광체와 산화아연 형광체를 예로 들 수 있는데, 상기 산화아연 형광체는 황화물계 형광체 보다 휘도나 수명에 있어서 우월한 특성이 있는 것으로 알려져 있다. 이러한 산화아연 형광체는 일반적으로 ZnO : Zn으로 표현되며 아연 부활 산화아연 형광체라고도 불리우는데, 산화아연(ZnO)을 환원성 분위기에서 소성하거나, 산화아연에 유화아연(ZnS)등의 아연 화합물을 미량 첨가하여 공기중에서 소성하도록 하는 것이 가장 일반적인 제법인 것이다.Examples of the low-speed electron beam excitation phosphor include sulfide-based phosphors and zinc oxide phosphors, which are known to have superior properties in brightness and lifetime than sulfide-based phosphors. These zinc oxide phosphors are generally expressed as ZnO: Zn and are also called zinc-activated zinc oxide phosphors. The zinc oxide (ZnO) is calcined in a reducing atmosphere, or a small amount of zinc compound such as zinc emulsion (ZnS) is added to zinc oxide. Firing in air is the most common recipe.

그러나 이러한 통상적인 방법에 의해서는 자기부활(自己復活)이 충분히 이루어지지 못하기 때문에 휘도가 절대적으로 부족하며, 이를 방지하기 위하여 고온에서 장시간 소성하게 될때에도 형광체 입자가 조대(粗大)해지고, 입도(粒度)가 불량해지기 때문에 형광막 형성시 막의 두께가 불균일하게 되며 나아가서는 막휘도가 크게 처리되는 등의 문제점이 발생된다.However, the conventional method does not sufficiently self-resilience (luminescence), so the brightness is absolutely insufficient, in order to prevent this, the phosphor particles become coarse even when baked for a long time at high temperature, and the particle size ( Since the film quality becomes poor, the thickness of the film becomes uneven when the fluorescent film is formed, and thus, the film brightness is largely processed.

본 발명의 목적은 아주 고른 입경과 입도 분포를 가지며 휘도가 크게 향상된 산화아연 형광체의 제조방법을 제공함에 있다.An object of the present invention is to provide a method for producing a zinc oxide phosphor having a very even particle size and particle size distribution and greatly improved brightness.

상기 목적을 달성하기 위하여 본 발명은, 산화아연(ZnO)을 탄소 분위기하에서 500-900℃ 정도로 30분 내지 6시간 동안 일차 소성하며, 다시 동일한 탄소 분위기하에서 500-1100℃ 정도로 이차 소성하도록 하여 산화아연 형광체를 얻도록 하는 점에 그 특징이 있다.In order to achieve the above object, the present invention, zinc oxide (ZnO) is first calcined for 30 minutes to 6 hours at 500-900 ℃ in a carbon atmosphere, and further zinc oxide to be baked at 500-1100 ℃ in the same carbon atmosphere again The characteristic is that the phosphor is obtained.

이하 실시예를 통하여 본 발명을 더욱 상세히 설명한다.The present invention will be described in more detail with reference to the following examples.

형광체 원료인 산화아연(ZnO)을 석영이나 알루미나 도가니등의 냉열성 용기에 충전한 다음 이 용기를 이보다 큰 용기에 집어 넣는다. 그리고 형광체 원료가 담긴 용기의 주위에 탄소(C)를 채워넣은 다음 큰 용기를 뚜껑으로써 밀폐한다. 이 때의 탄소 충전량은 용기의 크기에 따라서 차이가 있겠지만 바람직하게는 200-800g 정도로 한다.Zinc oxide (ZnO), which is a phosphor raw material, is filled in a cold-heating container such as quartz or alumina crucible and then placed in a larger container. Then, carbon (C) is filled around the container containing the phosphor raw material, and the large container is sealed by a lid. The amount of carbon at this time will vary depending on the size of the container, but preferably about 200-800 g.

이와같이 한 상태에서 소성을 실시하는데, 형광체의 채색과 입도 분포를 고려하여 소성온도를 400-1000℃ 정도로 하며, 바람직하게는 500-900℃ 정도로 하여 적정 시간 동안 소성한다. 이 때 소성시간은 통상의 소성용 도가니의 크기로 보아 30분에서 6시간 정도가 바람직하다. 이와같이 일차 소성이 완료된 후에는 재차 소성을 실시하게 되는데, 형광체의 발광 효율 및 입도 분포를 고려하여 소성온도는 일차 소성 온도 보다는 약간 높게 500-1100℃로 가열함이 좋으며, 총 소성시간은 1-6시간 정도로 하는 것이 바람직하다.In this state, the firing is carried out. The firing temperature is about 400-1000 ° C., preferably about 500-900 ° C. in consideration of the coloring of the phosphor and the particle size distribution. At this time, the firing time is preferably about 30 minutes to about 6 hours in view of the size of a conventional baking crucible. After the primary firing is completed, firing is performed again. In consideration of the luminous efficiency and particle size distribution of the phosphor, the firing temperature is preferably heated to 500-1100 ° C. slightly higher than the primary firing temperature, and the total firing time is 1-6. It is preferable to make it about time.

이상에서와 같이 본 발명은 형광체 원료를 탄소 분위기하에서 두번에 걸쳐 고온 소성 처리하도록 하는데, 일차 소성으로서는 소망하는 만큼의 휘도를 가진 형광체가 제조되지 못하기 때문에 재차 소성처리함으로써 완전한 자기 부활을 유도하도록 하는 것이다.As described above, the present invention allows the phosphor raw material to be subjected to high-temperature firing twice in a carbon atmosphere, but since the phosphor having the desired luminance is not manufactured as the primary firing, the firing process is performed again to induce complete self-activation. will be.

이러한 본 발명에 의하면, 환원성 분위기를 이용한 종래 제조방법을 통하여 제조된 녹색형광체보다 발광효율이 최대 10%가 높은 녹색형광체의 제조가 가능한데, 입도 분포가 고르고, 입경 또한 4-5㎛ 정도이어서 종래 형광체보다 매우 우수한 형광체를 제조할 수 있게 된다.According to the present invention, it is possible to manufacture a green phosphor having a luminous efficiency of up to 10% higher than the green phosphor manufactured by a conventional manufacturing method using a reducing atmosphere, the particle size distribution is even, the particle size is also about 4-5㎛ conventional phosphor More excellent phosphors can be produced.

Claims (2)

저속 전자선 여기 녹색형광체를 제조함에 있어서, 산화아연(ZnO)을 탄소 분위기하에서 400-1100℃의 소성 온도로 1차 소성하며, 이를 다시 탄소 분위기하에서 500-1100℃의 소성 온도로 2차 소성하도록 하는 공정을 포함하는 저속 전자선 여기 아연 부활 산화아연(ZnO : Zn) 녹색형광체의 제조방법.In preparing the low-speed electron beam-excited green phosphor, zinc oxide (ZnO) is first fired at a firing temperature of 400-1100 ° C. under a carbon atmosphere, and then secondly baked at a firing temperature of 500-1100 ° C. under a carbon atmosphere. A method for producing a low speed electron beam excited zinc activated zinc oxide (ZnO: Zn) green phosphor comprising a step. 제1항에 있어서, 상기 산화아연을 내열성 용기에 충전한 다음 이 용기를 탄소가 채워지는 내열성 용기에 밀폐 장입한 상태에서 소성 처리하도록 하는 것을 특징으로 하는 저속 전자선 여기 녹색형광체의 제조방법.The method for manufacturing a slow electron beam-excited green phosphor according to claim 1, wherein the zinc oxide is filled into a heat resistant container and then the container is calcined in a state where the container is enclosed in a heat resistant container filled with carbon.
KR1019890009620A 1989-07-06 1989-07-06 Preparation of geen fluorescent with excitation electron beam KR930004373B1 (en)

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KR930004373B1 true KR930004373B1 (en) 1993-05-26

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