KR100235404B1 - Sulfide phosphor and its production - Google Patents
Sulfide phosphor and its production Download PDFInfo
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- KR100235404B1 KR100235404B1 KR1019960008768A KR19960008768A KR100235404B1 KR 100235404 B1 KR100235404 B1 KR 100235404B1 KR 1019960008768 A KR1019960008768 A KR 1019960008768A KR 19960008768 A KR19960008768 A KR 19960008768A KR 100235404 B1 KR100235404 B1 KR 100235404B1
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Abstract
100V 정도의 제어전압으로 가속된 전자의 충돌에 의해서도 분해되기 어려운 황화물 형광체를 제공한다.It provides a sulfide phosphor that is difficult to decompose even by collision of electrons accelerated to a control voltage of about 100V.
ZnS 나 (Zn, Cd) S등을 모체로 하는 황화물 형광체의 표면은 Y2O3막으로 피복된다. 피복막을 형성하기 위해서는 프로피온산 이트륨을 아세틸 아세톤에 반응시켜서 얻을 수 있는 반응생성물을 에탄올로 희석한 막형성액을 황화물 형광체의 표면에 도포하여, 이것을 대기중에서 소성한다.The surface of the sulfide phosphor whose parent is ZnS or (Zn, Cd) S or the like is coated with a Y 2 O 3 film. In order to form a coating film, a film forming solution obtained by reacting yttrium propionate with acetyl acetone in ethanol is coated on the surface of the sulfide phosphor and calcined in the air.
황화물 형광체의 표면에는 Y2O2S 막을 사이로하여 Y2O3막이 형성되는 것으로 추정된다. Y2O2S는 안정된 물질이며, 황화물 형광체와 Y2O3막의 밀착성을 향상시킨다. Y2O2S막 상부에 있는 Y2O3는 안정된 물질이며, 고전압으로 가속된 전자의 충돌에 의해서도 분해되기 어렵다. 황화물 형광체는 Y2O3막으로 피복되어 있으므로, 100V 정도의 제어전압으로 가속된 전자의 충돌에 의해서도 거의 분해되지 않고, 발광휘도가 저하되지 않는다. 황화물 형광체의 휘도 잔존율은 향상되어 수명이 길어진다. 분해되기 어려우므로 인접하는 ZnO 형광체에 악영향을 미치지 않는다.It is estimated that a Y 2 O 3 film is formed on the surface of the sulfide phosphor with a Y 2 O 2 S film interposed therebetween. Y 2 O 2 S is a stable substance and improves the adhesion between the sulfide phosphor and the Y 2 O 3 film. Y 2 O 2 S film Y 2 O 3 is in the upper stable substance, it is difficult to decompose by the collision of accelerated electrons at a high voltage. Since the sulfide phosphor is coated with a Y 2 O 3 film, almost no decomposition is caused even by collision of electrons accelerated to a control voltage of about 100V, and the luminance of light emitted does not decrease. The luminance residual ratio of the sulfide phosphor is improved and the life is long. Since it is difficult to decompose, it does not adversely affect adjacent ZnO phosphors.
Description
제1도는 본 발명의 실시예의 효과를 확인하는 실험결과를 나타내는 일람표이다.1 is a table showing the experimental results confirming the effect of the embodiment of the present invention.
[산업상의 이용분야][Industrial use]
본 발명은 예컨대 100V 정도의 전압으로 가속된 전자의 충돌에 의해 발광하는 분해하기 어려운 황화물 형광체에 관한 것이다.The present invention relates to a sulfide phosphor that is difficult to decompose, for example, to emit light by collision of electrons accelerated to a voltage of about 100V.
[종래의 기술][Prior art]
일반적인 형광표시관은 고진공 분위기에 유지된 외위기(外圍器)의 내부에 전자를 방출하는 음극과 형광체층을 가지는 양극을 가지고 있다. 음극으로부터 방출된 전자는 양극에 충돌하여 형광체층을 발광시킨다.A typical fluorescent display tube has a cathode having a cathode layer and a phosphor layer emitting electrons inside an envelope maintained in a high vacuum atmosphere. Electrons emitted from the cathode collide with the anode to emit phosphor layers.
전자를 가속하는 형광표시관의 구동전압이 높을수록 전자가 충돌하는 형광체층은 분해가 용이해진다. 그래서, 형광체의 분해를 방지하기 위하여 형광체층의 표면에 보호를 위한 막을 형성하는 경우가 있었다. 예컨대, 산화아연 형광체의 경우에는 그 표면에 SiO2막을 형성하고, 그 SiO2의 양을 제어함으로써 저전압으로부터 고전압에 이르는 구동전압의 넓은 범위에 있어서 상기 형광체의 분해를 효과적으로 방지할 수 있다.The higher the driving voltage of the fluorescent display tube for accelerating electrons, the easier the phosphor layer to which electrons collide with. Thus, in order to prevent decomposition of the phosphor, a film for protection may be formed on the surface of the phosphor layer. For example, in the case of a zinc oxide phosphor, a SiO 2 film is formed on the surface thereof, and the decomposition of the phosphor can be effectively prevented in a wide range of driving voltages from low voltage to high voltage by controlling the amount of SiO 2 .
[발명이 해결하려고 하는 과제][Problems that the invention tries to solve]
형광표시관에 있어서는 발광표시를 다색으로 행하기 위하여 상기 산화아연 형광체 이외의 형광체의 이용이 추진되고 있다. 예컨대, 적색계나 청색계등의 발광이 얻어지는 황화물 형광체가 풀컬러 또는 멀티컬러의 그래픽 형광표시관에 사용되고 있다.In fluorescent display tubes, the use of phosphors other than the zinc oxide phosphors has been promoted in order to display light emission in multiple colors. For example, sulfide phosphors capable of emitting light such as red light or blue light are used for full color or multicolor graphic fluorescent display tubes.
그러나, 황화물 형광체는 그 표면에 SiO2막을 형성해 두어도, 예컨대 100V 전후의 고전압으로 가속된 전자가 충돌하면 분해되기 쉽다고 하는 문제가 있었다.However, even when a sulfide phosphor forms a SiO 2 film on its surface, there is a problem that, for example, electrons accelerated at high voltages around 100 V collide with each other and are easily decomposed.
그리고, 황화물 형광체가 분해되면 형광표시관의 외위기내에 유황이 비산하며, 유황은 음극에 피착하여 그 전자방출 능력을 저하시키고 만다.When the sulfide phosphor is decomposed, sulfur is scattered in the envelope of the fluorescent display tube, and the sulfur is deposited on the cathode to lower its electron emission ability.
이 때문에 형광표시관의 양극전류는 저하되어 표시 휘도의 저하가 빨라지고 만다고 하는 문제가 있었다. 또 황화물 형광체는 산화아연 형광체와 병용하여 사용되나, 황화물 형광체가 분해되면 인접하는 산화아연 형광체의 표면에 분해된 유황이 부착하여 산화아연 자체의 발광 특성도 저하시키고 만다고 하는 문제가 있었다.For this reason, there has been a problem that the anode current of the fluorescent display tube is lowered and the display luminance is lowered. In addition, sulfide phosphors are used in combination with zinc oxide phosphors, but when sulfide phosphors are decomposed, decomposed sulfur adheres to the surface of adjacent zinc oxide phosphors, thereby degrading the luminescence properties of zinc oxide itself.
본 발명은 고전압으로 가속된 전자의 충돌에 의해서도 분해되기 어려운 황화물 형광체와 그 제조방법을 제공하는 것을 목적으로 하고 있다.An object of the present invention is to provide a sulfide phosphor and a method for producing the sulfide phosphor, which are difficult to decompose even by collision of electrons accelerated at high voltage.
[과제를 해결하기 위한 수단][Means for solving the problem]
청구항 1에 기재된 황화물 형광체는 표면에 이트륨 산화물층이 형성된 것을 특징으로 하고 있다.The sulfide phosphor according to claim 1 has a yttrium oxide layer formed on its surface.
청구항 2에 기재된 황화물 형광체의 제조방법은 유기 이트륨을 함유하는 액체를 황화물 형광체의 표면에 도포하고, 이것을 소성하여 황화물 형광체의 표면에 이트륨 산화물층을 형성하는 것을 특징으로 하고 있다.The method for producing a sulfide phosphor according to claim 2 is characterized in that a liquid containing organic yttrium is applied to the surface of the sulfide phosphor, and then fired to form a yttrium oxide layer on the surface of the sulfide phosphor.
[작용][Action]
안정적이며 분해되기 어려운 이트륨 산화물층은 황화물 형광체와의 밀착성이 높은 Y2O2S 층을 통하여 황화물 형광체의 표면에 형성된다고 추정되어 있고, 황화물 형광체의 표면으로부터 박리되기 어렵다.The yttrium oxide layer that is stable and difficult to decompose is supposed to be formed on the surface of the sulfide phosphor through the Y 2 O 2 S layer having high adhesion to the sulfide phosphor, and is difficult to peel off from the surface of the sulfide phosphor.
[실시예]EXAMPLE
본 발명자들은 SiO2막을 황화물 형광체에 형성하여도 100V 정도의 제어전압으로 가속한 전자의 충돌에 의해 쉽게 분해되고마는 이유를 다음과 같이 고찰하였다. 먼저, ZnS 결정기판에 SiO2막을 조르겔법으로 형성하였으나, 밀착강도가 약하고, SiO2막은 극히 간단하게 형광체로부터 박리되고 말았다. 이 사실에서, ZnS 나 (Zn, Cd) S등을 모체로 하는 황화물 형광체는 SiO2와의 결정 격자의 미스매치가 크기 때문에 높은 밀착성을 얻을 수 없다고 생각하였다. 따라서, 황화물 형광체에 SiO2를 피복하여도, 전자충격이나 이온 충격등에 의해 간단히 박리되고마는 것으로 생각된다. 또, 피복하는 SiO2막의 양을 증가하면, 황화물 형광체와 SiO2막 사이의 왜곡이 증대하며, SiO2막의 양이 증가할수록 황화물 형광체 표면의 결정성이 열화하여 분해되기 쉽게되고마는 것으로 생각된다.The present inventors considered the reason why the SiO 2 film was easily decomposed by the collision of electrons accelerated to a control voltage of about 100V even when the SiO 2 film was formed on the sulfide phosphor as follows. First, a SiO 2 film was formed on the Z n S crystal substrate by the Zorgel method, but the adhesion strength was weak, and the SiO 2 film was very simply peeled off from the phosphor. In this fact, sulfide phosphors based on ZnS or (Zn, Cd) S and the like were considered to have a high mismatch in crystal lattice with SiO 2 , and thus could not obtain high adhesion. Therefore, even when SiO 2 is coated on the sulfide phosphor, it is considered that the film easily peels off due to an electron impact or an ion bombardment. In addition, when the amount of the SiO 2 film to be coated increases, the distortion between the sulfide phosphor and the SiO 2 film increases, and as the amount of the SiO 2 film increases, the crystallinity on the surface of the sulfide phosphor deteriorates and is liable to be degraded.
본 발명자들은 상기한 인식에 입각하여 예의 연구한 결과, 황화물 형광체와의 밀착성이 양호하며, 전자충격이나 이온충격등에 의한 분해가 되기 어려운 피복막을 개발하였다. 이 피복막은 ZnS나 (Zn, Cd) S등을 모체로하는 황화물 형광체의 표면에 형성된 Y2O3막으로 이루어진다.As a result of intensive studies based on the above-mentioned recognition, the present inventors have developed a coating film having good adhesion to sulfide phosphors and being hard to be decomposed by an electron shock or an ion shock. The coating film is composed of a Y 2 O 3 film formed on the surface of a sulfide phosphor having ZnS or (Zn, Cd) S as a parent.
황화물 형광체에 상기 피복막을 형성하는 방법을 설명한다. 유기 이트륨으로서의 프로피온산 이트륨 (CH3CH2COOY)을 함유하는 막형성액을 사용하였다. 더욱 구체적으로는 프로피온산이트륨을 아세틸아세톤에 반응시켜서 얻을 수 있는 반응생성물을 에탄올로 희석한 막형성액 (일반식 Y(OR)n, 단 R은 알킬기)을 사용하였다.A method of forming the coating film on the sulfide phosphor is described. A film formation liquid containing yttrium propionate (CH 3 CH 2 COOY) as organic yttrium was used. More specifically, a film-forming solution (General Formula Y (OR) n where R is an alkyl group) in which a reaction product obtained by reacting yttrium propionate with acetylacetone was diluted with ethanol.
상기 황화물 형광체의 표면에 상기 막형성액을 도포하고, 이것을 대기중에서 소성한다. 황화물 형광체의 표면에는 Y2O2S 막을 사이로하여 Y2O3막이 형성된다고 생각된다. 황화물 형광체와 Y2O3층 사이에 있는 Y2O2S 막은 황화물 형광체 표면의 S 와 막형성액의 성분이 소성 과정에 있어서 반응하여 생성된 것으로 생각된다. Y2O2S 는 안정된 물질이며, 황화물 형광체와 Y2O3막의 밀착성을 향상시킨다. Y2O2S 막의 상부에 있는 Y2O3는 대단히 안정된 물질이며, 100V 정도의 제어전압으로 가속된 전자의 충돌에 의해서도 분해되기 어렵다.The film-forming liquid is applied to the surface of the sulfide phosphor and calcined in the air. It is thought that a Y 2 O 3 film is formed on the surface of the sulfide phosphor with a Y 2 O 2 S film interposed therebetween. The Y 2 O 2 S film between the sulfide phosphor and the Y 2 O 3 layer is thought to be formed by the reaction of S on the surface of the sulfide phosphor with the components of the film forming solution during the calcination process. Y 2 O 2 S is a stable substance and improves the adhesion between the sulfide phosphor and the Y 2 O 3 film. Y 2 O 2 S film Y 2 O 3 in the upper part is a very stable substance, it is difficult to decompose by the acceleration of the electrons to a control voltage of about 100V collision.
상기와 같이하여 황화물 형광체에 형성한 Y2O3막이 박리되기 어려움을 스크래치테스터를 사용한 긁기 테스트로 확인하였다. 즉, 스크래치 테스터를 사용한 긁기 테스트에 있어서, ZnS 결정기판에 형성한 SiO2막의 수치가 30mN 였었던 것에 대하여, 본 실시예의 Y2O3막에 대해서는 50mN의 값을 얻었다.As described above, it was confirmed by the scratch test using a scratch tester that the Y 2 O 3 film formed on the sulfide phosphor was not easily peeled off. That is, in the scratch test using the scratch tester, the value of the SiO 2 film formed on the ZnS crystal substrate was 30 mN, and the value of 50 mN was obtained for the Y 2 O 3 film of the present example.
본 실시예의 Y2O3막을 형성한 황화물 형광체를 형광표시관의 양극 표시부에 실제 장착하여 연속점등 실험을 행한다. 실험결과를 제1도에 도시한다. 실험에 제공하는 실시예의 Y2O3막을 구비한 황화물 형광체의 샘플은 1, 10, 50g/ℓ의 3종류의 Y2O3농도의 막형성액과 200℃와 400℃ 2종류의 소성온도의 편성에 의해 6종류를 형성하였다.The sulfide phosphor in which the Y 2 O 3 film of the present embodiment was formed was actually mounted on the anode display portion of the fluorescent display tube to conduct continuous lighting experiments. The experimental results are shown in FIG. Samples of the sulfide phosphors with Y 2 O 3 membranes of the examples provided for the experiments were formed of three types of Y 2 O 3 concentrations of 1, 10, and 50 g / l, and two firing temperatures of 200 ° C. and 400 ° C. Six types were formed by knitting.
또, 인접하는 황화물 형광체의 분해에 의한 영향을 조사하기 위하여 실시예의 황화물 형광체 근방에 ZnO 형광체의 표시부를 설정해 두고, 이것은 연속점등 실험중에는 비점등으로 하였다. 또, 막에 의해 피복되어 있지 않는 황화물 형광체(코트않음)와 SiO2막으로 피복된 황화물 형광체(SiO2코트)를 양극 표시부에 가지는 형광표시관을 비교를 위하여 형성하였다.In order to investigate the effect of decomposition of adjacent sulfide phosphors, a display portion of the ZnO phosphor was set in the vicinity of the sulfide phosphor of the example, and this was set to non-lighting during the continuous lighting experiment. In addition, a fluorescent display tube having a sulfide phosphor (no coat) not covered with a film and a sulfide phosphor (SiO 2 coat) coated with a SiO 2 film was formed for comparison.
실시예의 황화물 형광체를 연속점등하고, 소정시간이 경과한 후의 휘도잔존율의 데이터로서 양극전류의 값(ib)과 동일하게 형광체의 휘도(L)를 초기치를 100%로 하여 측정한다. 또, 인접하는 ZnO 형광체의 표시부에 있어서의 양극 전류의 값(ib)과 형광체의 휘도(L)를 측정한다. 측정을 행한 것은 연속점등 140 시간후와 400 시간후 및 900 시간후이다. 구동조건은 양극전압 120V, 듀티비 1/70이다.The sulfide phosphors of Examples were continuously lit, and the luminance L of the phosphor was measured at an initial value of 100% in the same manner as the anode current value ib as data of the luminance residual ratio after a predetermined time had elapsed. In addition, the value (ib) of the anode current and the luminance (L) of the phosphor in the display section of the adjacent ZnO phosphor are measured. The measurement was carried out after 140 hours of continuous lighting and after 400 hours and 900 hours. The driving conditions are anode voltage 120V and duty ratio 1/70.
제1도에 도시한 바와같이 어떤 조건에 있어서도 본 실시예의 막에 의해 피복되어 있지 않는 황화물 형광체(코트않음) 나, SiO2막으로 피복된 황화물 형광체(SiO2코트)보다도, 본 실시예의 Y2O3막으로 피복된 황화물 형광체 쪽이 우수한 발광상태를 나타내고 있다.As shown in FIG. 1, the Y 2 of the present embodiment is better than the sulfide phosphor (not coated) or the sulfide phosphor (SiO 2 coat) coated with the SiO 2 film under any conditions. The sulfide phosphor coated with the O 3 film shows an excellent light emission state.
또, 인접하는 ZnO 형광체의 발광상태도, 본 실시예의 막에 의해 피복되어 있지 않는 황화물 형광체 (코트않음) 나, SiO2막으로 피복된 황화물 형광체(SiO2코트) 의 근방에 있는 ZnO 형광체 보다도 양호하다.In addition, the light emission state of adjacent ZnO phosphors is also better than that of a sulfide phosphor (not coated) not covered by the film of this embodiment or a ZnO phosphor in the vicinity of a sulfide phosphor (SiO 2 coat) coated with a SiO 2 film. Do.
이상의 실험결과로 부터 본 실시예의 황화물 형광체는 Y2O3막으로 피복되어 있으므로 100V 정도의 제어전압으로 가속된 전자의 충돌에 의해서도 거의 분해되지 않고, 자신의 발광휘도도 저하되지 않는다. 즉, 황화물 형광체의 휘도 잔존율이 향상하여 수명이 길어진다. 또, 분해되기 어려우므로 인접하는 ZnO 형광체에 악영향을 미치는 일도 없다.From the above experiment results, since the sulfide phosphor of the present example was coated with a Y 2 O 3 film, almost no decomposition was caused even by collision of electrons accelerated to a control voltage of about 100V, and its luminance was not lowered. That is, the luminance residual ratio of the sulfide phosphor is improved, and the life is long. Moreover, since it is hard to decompose | disassemble, it does not adversely affect adjacent ZnO fluorescent substance.
[발명의 효과][Effects of the Invention]
본 발명의 황화물 형광체는 그 표면에 이트륨 산화물층을 설정하였으므로, 전자의 충돌등에 의해서도 분해되기 어렵고, 휘도 잔존율이 향상하여 수명이 개선된다. 또, 인접하는 ZnO 형광체등에 악영향을 미치지 않는다.Since the yttrium oxide layer is set on the surface of the sulfide phosphor of the present invention, it is difficult to be decomposed by the collision of electrons or the like, the luminance residual ratio is improved, and the life is improved. Moreover, it does not adversely affect adjacent ZnO phosphors.
Claims (2)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07540495A JP3386622B2 (en) | 1995-03-31 | 1995-03-31 | Sulfide phosphor and method for producing the same |
| JP95-075404 | 1995-03-31 |
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| Publication Number | Publication Date |
|---|---|
| KR960034360A KR960034360A (en) | 1996-10-22 |
| KR100235404B1 true KR100235404B1 (en) | 1999-12-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1019960008768A KR100235404B1 (en) | 1995-03-31 | 1996-03-28 | Sulfide phosphor and its production |
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| Country | Link |
|---|---|
| JP (1) | JP3386622B2 (en) |
| KR (1) | KR100235404B1 (en) |
| TW (1) | TW310340B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100796703B1 (en) * | 2000-08-15 | 2008-01-21 | 소니 가부시끼 가이샤 | Method for manufacturing luminescent material, luminescent material manufactured by the same manufacturing method, and display substrate and display apparatus having the same luminescent material |
-
1995
- 1995-03-31 JP JP07540495A patent/JP3386622B2/en not_active Expired - Fee Related
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1996
- 1996-03-21 TW TW085103425A patent/TW310340B/zh active
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100796703B1 (en) * | 2000-08-15 | 2008-01-21 | 소니 가부시끼 가이샤 | Method for manufacturing luminescent material, luminescent material manufactured by the same manufacturing method, and display substrate and display apparatus having the same luminescent material |
| KR100811036B1 (en) * | 2000-08-15 | 2008-03-06 | 소니 가부시끼 가이샤 | Method for manufacturing luminescent material, luminescent material manufactured by the same manufacturing method, and display substrate and display apparatus having the same luminescent material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH08269447A (en) | 1996-10-15 |
| JP3386622B2 (en) | 2003-03-17 |
| TW310340B (en) | 1997-07-11 |
| KR960034360A (en) | 1996-10-22 |
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