KR930003704B1 - Production of red luminous fluorescent material - Google Patents
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- KR930003704B1 KR930003704B1 KR1019890019195A KR890019195A KR930003704B1 KR 930003704 B1 KR930003704 B1 KR 930003704B1 KR 1019890019195 A KR1019890019195 A KR 1019890019195A KR 890019195 A KR890019195 A KR 890019195A KR 930003704 B1 KR930003704 B1 KR 930003704B1
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Description
제 1 도는 종래의 형광체의 발광스팩트라와 본 발명의 형광체의 발광스펙트라를 나타낸 그래프.1 is a graph showing a light emission spectra of a conventional phosphor and a light emission spectra of the phosphor of the present invention.
제 2 도는 종래의 형광체와 본 발명의 형광체의 입도분포를 나타낸 그래프.2 is a graph showing a particle size distribution of a conventional phosphor and the phosphor of the present invention.
본 발명은 적색발광형광체의 제조방법에 관한 것으로서, 특히 칼라텔레비전에 사용되는 형광체로서 음극선관의 적색발광성분인 Y2O2S : Eu로 이루어진 적색발광 형광체의 제조방법에 관한 것이다.The present invention relates to a method of manufacturing a red light-emitting phosphor, and more particularly, to a method of manufacturing a red light-emitting phosphor consisting of Y 2 O 2 S: Eu which is a red light-emitting component of a cathode ray tube as a phosphor used in color television.
일반적으로 칼라텔레비전에 사용되고 있는 음극선관은 고휘도로 여기하고 고전류 밀도하에서 동작된다. 이와 같은 방식으로 스크린상에 충분한 밝은 화상을 얻기 위해서는 음극선관의 형광면상에 매우 밝은 고휘도화상을 표시하지 않으면 안된다.In general, cathode ray tubes used in color televisions are excited at high brightness and operated under high current density. In order to obtain a sufficient bright image on the screen in this manner, a very bright high luminance image must be displayed on the fluorescent surface of the cathode ray tube.
따라서 고휘도 화상을 표시하기 위한 형광체가 요구되고 있으며 이와 같은 형광체에 필요한 특성에는 다음의 3가지가 있다.Therefore, there is a need for a phosphor for displaying a high brightness image. There are three characteristics required for such a phosphor.
(1) 전자 비임전류의 증대에 따라 휘도가 포화하지 않는 것(즉, 휘도포화특성이 양호한 것)(1) The luminance does not saturate as the electron beam current increases (that is, the luminance saturation characteristic is good)
(2) 온도상승에 따라 온도소광이 작은 것(즉, 온도특성이 양호한 것)(2) Small temperature extinction due to temperature rise (that is, good temperature characteristics)
(3) 장시간 작동하여도 형광막이 손상하여 열화현상이 생기지 않는 것(즉, 휘도수명이 양호한 것)(3) The fluorescent film is not damaged by deterioration even after long time operation (that is, the luminance life is good)
상기 특성을 거의 만족하는 적색발광형광체로서 대표적으로 Y2O2S : Eu 형광체가 주목되고 있다.The Y 2 O 2 S: Eu phosphors are attracting attention as red luminescent phosphors substantially satisfying the above characteristics.
그러나 칼라음극선관을 더욱 밝게 하기 위해 전류밀도를 높여서 여기하려 해도 현재 사용되는 형광체는 반드시 고휘도와 우수한 전류휘도포화특성을 가지고 있다고 할 수 없다.However, even if the current density is increased to make the color cathode ray tube brighter and excited, the currently used phosphor does not necessarily have high luminance and excellent current luminance saturation characteristics.
따라서 본원 발명자는 적색발광형광체에 대해 꾸준히 연구한 끝에 Y2O2S : Eu 형광체가 갖는 색조와 전류휘도포화특성에 대한 결점을 신규한 방법으로 대폭 개선하였다.Therefore, the present inventors have steadily studied the red light-emitting phosphor, and greatly improved the defects in the color tone and current luminance saturation characteristics of the Y 2 O 2 S: Eu phosphor by a novel method.
본 발명의 목적은 고부하(고전압, 고밀도) 작동하에서도 고휘도 발광하고 우수한 발광휘도특성을 갖는 Y2O2S : Eu 적색발광형광체의 제조방법을 제공하는 것이다.An object of the present invention is to provide a method for producing a Y 2 O 2 S: Eu red light-emitting phosphor having high luminance and excellent emission luminance even under high load (high voltage, high density) operation.
상기 목적을 달성하기 위하여 본 발명은 Y2O2S : Eu 적색발광형광체의 제조방법에 있어서, 형광체 원료를 소성로에서 1100 내지 1200℃의 온도로 1차소성하는 공정과, 1300 내지 1500℃의 온도로 2차소성하는 공정을 포함하는 점에 특징이 있다.In order to achieve the above object, the present invention provides a method for producing a Y 2 O 2 S: Eu red light-emitting phosphor, the process of primary firing the phosphor raw material in a firing furnace at a temperature of 1100 to 1200 ℃, and a temperature of 1300 to 1500 ℃ It is characteristic in that it includes the process of secondary baking by furnace.
본 발명에 따른 적색발광형광체의 제조방법은 다음과 같다.The manufacturing method of the red light-emitting phosphor according to the present invention is as follows.
형광체 원료로는 이트륨원으로 산화이트륨등의 이트륨화합물, 유로피움원으로 산화유로피움등의 유로피움화합물을 사용한다.Yttrium compounds such as yttrium oxide are used as the yttrium source and europium compounds such as europium oxide as the europium source.
여기에 융제로서 탄산나트륨(Na2CO3), 인산수소칼륨(K2HPO4), 휘도증가제로 황(S)을 복합적으로 첨가하여 유봉이나 볼밀등의 혼합기로 충분히 혼합한다.To this, sodium carbonate (Na 2 CO 3 ), potassium hydrogen phosphate (K 2 HPO 4 ), and sulfur (S) are added as a brightness increasing agent, and mixed with a mixer such as a pestle or a ball mill.
이때 혼합은 고체인 상태로 혼합하는 건식법이나 적당한 용매를 사용하여 혼합하는 습식법으로 해도 무방하나 본 발명에서는 후자의 방법으로 하였다.At this time, the mixing may be a dry method of mixing in a solid state or a wet method of mixing using a suitable solvent, but in the present invention, the latter method is used.
또한, 첨가되는 형광체원료 혼합물이Y2O3100중량부에 대하여 산화유로피움은 4.0 내지 4.8중량부, 탄산나트륨은 30 내지 60중량부, 황은 50 내지 70중량부, 인산수소칼륨은 10 내지 30중량부가 바람직하다.In addition, the phosphor material mixture is added Y 2 O 3 100 weight of europium oxide with respect to the section is 4.0 to 4.8 parts by weight of sodium carbonate is 30 to 60 parts by weight of sulfur is from 50 to 70 parts by weight of a phosphoric acid potassium is from 10 to 30 wt. Addition is preferred.
그후 혼합물을 석영이나 알루니마 도가니등의 내열성 용기에 넣은 후 소성로에서 1100 내지 1200℃의 온도로 1 내지 4시간동안 1차 소성하고, 그후 얻어진 소성물을 분쇄, 수세여과, 건조등의 처리를 하여 Y2O2S : Eu 형광체를 얻었다.Thereafter, the mixture is placed in a heat-resistant container such as quartz or alumina crucible, and then first calcined in a firing furnace at a temperature of 1100 to 1200 ° C. for 1 to 4 hours, and then the resulting fired material is pulverized, washed with water, dried and treated. A Y 2 O 2 S: Eu phosphor was obtained.
상기에서 얻어진 Y2O2S : Eu 형광체를 다시 원료로 하여 상기와 동일한 방법으로 혼합기로 충분히 혼합한 후 수용액형태의 테르븀(Tb)을 첨가한다.The Y 2 O 2 S: Eu phosphor obtained above is used again as a raw material and sufficiently mixed with a mixer in the same manner as above, and then terbium (Tb) in the form of an aqueous solution is added.
이때 첨가되는 형광체원료 혼합물이 Y2O2S : Eu 형광체 100중량부에 대하여 산화유로피움은 3 내지 5중량부, 탄산나트륨은 20 내지 40중량부, 황은 30 내지 50중량부, 인산수소칼륨은 10 내지 30중량부, 테르븀은 20 내지 50PPM을 첨가한다.At this time, the phosphor raw material mixture added is 3 to 5 parts by weight of europium oxide, 20 to 40 parts by weight of sodium carbonate, 30 to 50 parts by weight of sulfur, and potassium hydrogen phosphate based on 100 parts by weight of Y 2 O 2 S: Eu phosphor. To 30 parts by weight, terbium is added from 20 to 50 PPM.
상기 혼합물을 석영이나 알루미나 도가니등의 내열성 용기에 넣은 후 소성로에서 1300 내지 1500℃의 온도로 1 내지 4시간동안 2차 소성하고, 그후 얻어진 소성물을 분쇄, 수세여과, 건조등의 처리를 하여 본 발명의 적색발광형광체를 얻었다.The mixture was placed in a heat-resistant container such as quartz or alumina crucible, and then calcined in a firing furnace at a temperature of 1300 to 1500 ° C. for 1 to 4 hours. The red light emitting phosphor of the invention was obtained.
본 발명의 따른 적색발광형광체를 다음의 실시예를 통해 상세히 설명한다.The red light emitting phosphor according to the present invention will be described in detail through the following examples.
[실시예 1]Example 1
형광체 원료로As phosphor raw material
Y2O2S : Eu : 100중량부Y 2 O 2 S: Eu: 100 parts by weight
Y2O3: 3중량부Y 2 O 3 : 3 parts by weight
Na2CO3: 20중량부Na 2 CO 3 : 20 parts by weight
S : 30중량부S: 30 parts by weight
K2HPO4: 10중량부K 2 HPO 4 : 10 parts by weight
Tb : 20PPMTb: 20PPM
를 칭량하여 볼밀로 충분히 혼합하고 얻어진 혼합물을 알루니마 도가니에 넣어 소성로에서 1500℃로 2시간동안 소성하여 얻어진 소성물을 수세여과, 건조등의 처리를 하여 본 발명의 형광체를 얻었다.Was weighed and sufficiently mixed in a ball mill, and the obtained mixture was placed in an alumina crucible and calcined at 1500 ° C. for 2 hours in a calcination furnace to obtain a phosphor of the present invention by performing washing with water and drying.
상기 테르븀(Tb)은 수용액상태로 첨가되므로 먼저 형광체에 습식 혼합한 후 건조하여 처리한다.Since terbium (Tb) is added in an aqueous solution, the mixture is first wet mixed with the phosphor and then dried.
[실시예 2]Example 2
형광체 원료로As phosphor raw material
Y2O2S : Eu : 100중량부Y 2 O 2 S: Eu: 100 parts by weight
Eu2O3: 4량부Eu 2 O 3 : 4 parts by weight
Na2CO3: 30중량부Na 2 CO 3 : 30 parts by weight
S : 40중량부S: 40 parts by weight
K2HPO4: 10중량부K 2 HPO 4 : 10 parts by weight
Tb : 15PPMTb: 15PPM
을 칭량하여 실시예 1과 동일한 방법으로 수행하되 1400℃에서 2시간동안 소성하여 얻어진 소성물을 수세여과, 건조등의 처리를 하여 본 발명의 형광체를 얻었다.Was carried out in the same manner as in Example 1, but the resulting fired product obtained by calcining at 1400 ℃ for 2 hours was washed with water, dried, etc. to obtain a phosphor of the present invention.
[실시예 3]Example 3
Y2O2S : Eu : 100중량부Y 2 O 2 S: Eu: 100 parts by weight
Eu2O3: 5중량부Eu 2 O 3 : 5 parts by weight
Na2CO3: 40중량부Na 2 CO 3 : 40 parts by weight
S : 50중량부S: 50 parts by weight
K2HPO4: 20중량부K 2 HPO 4 : 20 parts by weight
Tb : 20PPMTb: 20PPM
을 칭량하여 실시예 1과 동일한 방법으로 수행하되 1500℃에서 2시간동안 소성하여 얻어진 소성물을 수세여과, 건조등의 처리를 하여 본 발명의 형광체를 얻었다.Weighing was carried out in the same manner as in Example 1, but the calcined product obtained by calcining at 1500 ℃ for 2 hours was subjected to treatment such as water filtration, drying and the like to obtain the phosphor of the present invention.
본 발명의 형광체의 발광강도는 종래의 방법으로 제조된 형광체에 비하여 약 2 내지 7% 향상되었다. 그리고 발광피크파장은 626nm 부근에 있으며 발광색은 거의 일치하고 평균입자경도 크게 차이는 없었다.The luminous intensity of the phosphor of the present invention is improved by about 2 to 7% compared to the phosphor produced by the conventional method. The emission peak wavelength was around 626 nm and the emission color was almost identical and the average particle size was not significantly different.
이와 같은 제반특성을 상기 실시예 1, 2, 3으로부터 얻어진 형광체에 대하여 측정한 결과를 표 1에 나타내었고, 이때 기준은 종래의 제조방법으로 제조된 Y2O2S : Eu 형광체이다.The results obtained by measuring the various properties of the phosphors obtained in Examples 1, 2, and 3 are shown in Table 1, wherein the reference is a Y 2 O 2 S: Eu phosphor manufactured by a conventional manufacturing method.
[표 1]TABLE 1
표 1로부터 알 수 있는 바와 같이, 본 발명의 형광체의 발광광도는 종래의 형광체 보다 약 12 내지 17%향상되었다.As can be seen from Table 1, the luminous intensity of the phosphor of the present invention was improved by about 12 to 17% over the conventional phosphor.
제 1 도는 종래의 형광체의 발광스펙트라와 본 발명의 형광체의 발광스펙트라를 나타낸 그래프로서, 발광스펙트라에 있어서는 큰 차이가 없으므로 거의 영향이 없음을 알 수 있다.1 is a graph showing the light emission spectra of the conventional phosphor and the light emission spectra of the phosphor of the present invention, and it can be seen that there is almost no effect because there is no big difference in the light emission spectra.
제 2 도는 종래의 형광체와 본 발명의 형광체의 입도분포를 나타낸 그래프로서, 종래의 방법으로 제조된 형광체와 실시예 1, 2, 3에서 제조된 형광체의 입자분포를 비교하여 나타내었다. 그러나 종래의 형광체에 비해 큰 차이가 없었다.2 is a graph showing the particle size distribution of the conventional phosphor and the phosphor of the present invention, and is shown by comparing the particle distribution of the phosphor prepared by the conventional method and the phosphor prepared in Examples 1, 2, and 3. However, there was no significant difference compared with the conventional phosphor.
이상에서 설명한 바와 같이, 본 발명에 의하면 2회의 소성공정으로 제조된 Y2O2S : Eu 형광체로서, 고휘도로 발광하고 우수한 전류휘도포화특성 및 발광휘도특성을 갖는 적색발광형체를 얻었고 경제적인 측면에서 매우 실용적이었다.As described above, according to the present invention, as a Y 2 O 2 S: Eu phosphor prepared in two firing processes, a red light-emitting body having high luminance and excellent current luminance saturation characteristics and emission luminance characteristics was obtained. Was very practical.
Claims (3)
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| Application Number | Priority Date | Filing Date | Title |
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| KR1019890019195A KR930003704B1 (en) | 1989-12-22 | 1989-12-22 | Production of red luminous fluorescent material |
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| KR1019890019195A KR930003704B1 (en) | 1989-12-22 | 1989-12-22 | Production of red luminous fluorescent material |
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| KR930003704B1 true KR930003704B1 (en) | 1993-05-08 |
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