KR100373839B1 - Low-voltage red phosphor and method of preparing same - Google Patents
Low-voltage red phosphor and method of preparing same Download PDFInfo
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- KR100373839B1 KR100373839B1 KR10-2000-0051683A KR20000051683A KR100373839B1 KR 100373839 B1 KR100373839 B1 KR 100373839B1 KR 20000051683 A KR20000051683 A KR 20000051683A KR 100373839 B1 KR100373839 B1 KR 100373839B1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7701—Chalogenides
- C09K11/7703—Chalogenides with alkaline earth metals
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
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- C09K11/7718—Chalcogenides with alkaline earth metals
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7729—Chalcogenides
- C09K11/7731—Chalcogenides with alkaline earth metals
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
- C09K11/7744—Chalcogenides
- C09K11/7746—Chalcogenides with alkaline earth metals
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- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
본 발명은 저전압용 적색 형광체 및 그의 제조 방법에 관한 것으로서, 이 적색 형광체는 알칼리 토금속 및 티타늄의 산화물로 이루어진 모체 매트릭스 및 상기 모체 매트릭스에 첨가된 부활제로 희토류 원소 및 주기율표의 ⅢA족 원소를 포함하며, 상기 알칼리 토금속을 티타늄 1몰에 대하여 0.5 내지 0.9 몰의 양으로 포함한다.The present invention relates to a red phosphor for a low voltage and a method of manufacturing the same, the red phosphor comprising a rare earth element and a group IIIA element of the periodic table as a mother matrix composed of an alkaline earth metal and an oxide of titanium and an activator added to the matrix matrix, The alkaline earth metal is included in an amount of 0.5 to 0.9 moles with respect to 1 mole of titanium.
이 적색 형광체는 우수한 휘도 잔존율을 나타낸다.This red phosphor exhibits excellent luminance residual ratio.
Description
[산업상 이용 분야][Industrial use]
본 발명은 저전압용 적색 형광체 및 그의 제조 방법에 관한 것으로서, 상세하게는 휘도 잔존율이 우수한 저전압용 적색 형광체 및 그의 제조 방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a low voltage red phosphor and a method of manufacturing the same, and more particularly, to a low voltage red phosphor having excellent luminance residual ratio and a method of manufacturing the same.
[종래 기술][Prior art]
주로 1kV 이하의 저전압 디스플레이에는 진공 형광 디스플레이(Vaccumm Fluoresent Display: VFD), 전계 방출 디스플레이(Field Emission Display: FED) 등이 있다. VFD는 주로 가전, AV, 자동차 등의 각종 표시 소자로 사용되고 있고 FED는 차세대 소형 평판 표시 소자로 활발히 연구되고 있다.Low voltage displays of less than 1 kV include vacuum fluorescence displays (VFDs) and field emission displays (FEDs). VFD is mainly used for various display devices such as home appliances, AV, automobiles, etc., and FED is being actively researched as a next-generation small flat panel display device.
이러한 VFD 및 FED에 사용되는 적색 형광체로는 ZnS:Zn 등의 황화아연계 형광체, Y2O3:Eu 형광체 및 SrTiO3:Pr,Al 형광체가 있다. 이 형광체 중에서 SrTiO3:Pr,Al 형광체가 디스플레이 내부 및 환경 오염 문제가 발생하지 않으므로 최근 활발히 연구되고 있다.Red phosphors used in such VFD and FED include zinc sulfide-based phosphors such as ZnS: Zn, Y 2 O 3 : Eu phosphors, and SrTiO 3 : Pr, Al phosphors. Among these phosphors, SrTiO 3 : Pr, Al phosphors have been actively studied recently because they do not cause problems in the display and environmental pollution.
미국 특허 제 5,619,098 호에는 모체 SrTiO3와 부활제 Pr 및 공부활제 Al로 구성된 SrTiO3:Pr,Al 형광체가 기술되어 있다. 이 형광체는 스트론튬염과 티타늄염 및 부활제로 프라세오디뮴(Pr)염과 공부활제로 Al을 혼합하고 이 혼합물을 1100 내지 1400℃에서 소성하여 제조된다. 상기 스트론튬염과 티타늄염은 스트론튬 1몰에 대하여 티타늄 0.7 내지 0.9 몰이 되도록 사용한다.U. S. Patent No. 5,619, 098 describes SrTiO 3 : Pr, Al phosphors composed of parent SrTiO 3 and activator Pr and active agent Al. This phosphor is prepared by mixing strontium salt, titanium salt, praseodymium (Pr) salt as an activator, and Al as a activator and calcining the mixture at 1100 to 1400 ° C. The strontium salt and the titanium salt are used to be 0.7 to 0.9 mol of titanium per mol of strontium.
그러나 이 방법으로 제조된 형광체는 초기 휘도가 수십시간 만에 30∼60%로 그 휘도 잔존율이 떨어져 아직까지 상업적인 응용을 하지 못하고 있다.However, the phosphor produced by this method has an initial luminance of 30 to 60% in a few tens of hours and its luminance remaining rate is low, and thus commercial applications are not yet available.
본 발명은 상술한 문제점을 해결하기 위한 것으로서, 본 발명의 목적은 휘도 잔존율이 우수한 저전압용 적색 형광체를 제공하는 것이다.SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, and an object of the present invention is to provide a low voltage red phosphor having excellent luminance residual ratio.
본 발명의 다른 목적은 상기 물성을 갖는 저전압용 적색 형광체의 제조 방법을 제공하는 것이다.Another object of the present invention is to provide a method for producing a low phosphor red phosphor having the above physical properties.
상기 목적을 달성하기 위하여, 본 발명은 알칼리 토금속 및 티타늄의 산화물로 이루어진 모체 매트릭스; 및 상기 모체 매트릭스에 첨가된 부활제로 희토류 원소 및 주기율표의 ⅢA족 원소를 포함하는 저전압용 적색 형광체로서, 상기 티타늄 1몰에 대하여 상기 알칼리 토금속 0.5 내지 0.9 몰을 포함하는 것인 저전압용 적색 형광체를 제공한다.In order to achieve the above object, the present invention is a matrix matrix consisting of an alkaline earth metal and an oxide of titanium; And a low voltage red phosphor comprising a rare earth element and a group IIIA element of the periodic table as an activator added to the matrix matrix, wherein the red phosphor for low voltage comprises 0.5 to 0.9 moles of the alkaline earth metal per 1 mole of the titanium. do.
본 발명은 또한 알칼리 토금속염, 티타늄염, 희토류 원소 화합물 및 ⅢA족 원소 화합물을 혼합하고; 상기 혼합물을 1100 내지 1400℃에서 1 내지 6시간 동안 소성하는 공정을 포함하는 저전압용 적색 형광체의 제조 방법으로서, 상기 혼합 공정에서, 상기 알칼리 토금속염과 티타늄염의 사용양은 상기 적색 형광체에서 잔존하는 알칼리 토금속 양이 상기 티타늄 1몰에 대하여 0.5 내지 0.9몰이 되는 양으로 사용하는 것인 저전압용 적색 형광체의 제조 방법을 제공한다.The invention also mixes alkaline earth metal salts, titanium salts, rare earth element compounds and group IIIA element compounds; A method for producing a low phosphor red phosphor, comprising the step of baking the mixture at 1100 to 1400 ° C. for 1 to 6 hours, wherein in the mixing step, the amount of the alkaline earth metal salt and the titanium salt is used in the alkaline earth metal remaining in the red phosphor. It provides a method for producing a low-voltage red phosphor for use in an amount of 0.5 to 0.9 mole with respect to 1 mole of the titanium.
이하 본 발명을 더욱 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명의 저전압용 적색 형광체는 알칼리 토금속과 티타늄 산화물의 모체 매트릭스에 부활제로서 희토류 원소와 주기율표상의 ⅢA족 원소를 첨가시킨 것으로, MTiO3:R,B의 조성을 가진다. 상기 식에서 M은 Mg, Sr, Ca 또는 Ba의 알칼리 토금속이고, R은 Ce, Eu, Tb, Er, Tm, Pr 또는 Dy의 희토류 원소이고, B는 Al, Ga, In 또는 Tl의 ⅢA족 원소이다.In the low-voltage red phosphor of the present invention, a rare earth element and a group IIIA element on the periodic table are added to the matrix matrix of alkaline earth metal and titanium oxide, and have MTiO 3 : R, B composition. Wherein M is an alkaline earth metal of Mg, Sr, Ca or Ba, R is a rare earth element of Ce, Eu, Tb, Er, Tm, Pr or Dy, and B is a Group IIIA element of Al, Ga, In or Tl .
상기 저전압용 적색 형광체는 희토류 원소를 바람직하게 0.05 내지 5 몰% 포함하고, ⅢA족 원소를 바람직하게 0.05 내지 80 몰% 포함한다. 또한, 저전압용 적색 형광체는 티타늄 1몰에 대하여 0.5 내지 0.9 몰의 알칼리 토금속을 포함한다. 본 발명에서와 같이, 알칼리 토금속을 티타늄에 비하여 소량으로 사용하는 것이 티타늄보다 과량으로 사용하는 것보다 휘도 잔존율을 증가시킬 수 있다. 상기 희토류 원소, ⅢA족 원소 및 알칼리 토금속의 양이 상기 범위를 벗어나는 경우에는 최종 생성되는 형광체의 휘도가 저하되어 바람직하지 않다.The red phosphor for low voltage preferably contains 0.05 to 5 mol% of rare earth elements, and preferably 0.05 to 80 mol% of group IIIA elements. In addition, the red phosphor for low voltage contains 0.5 to 0.9 moles of alkaline earth metal per mole of titanium. As in the present invention, the use of an alkaline earth metal in a small amount compared to titanium can increase the luminance remaining ratio than the use in excess of titanium. When the amounts of the rare earth element, group IIIA element and alkaline earth metal are outside the above ranges, the luminance of the resulting phosphor is lowered, which is not preferable.
본 발명의 저전압용 적색 형광체는 알칼리 토금속 염과 티타늄염을 혼합한 다음, 희토류 원소 화합물과 ⅢA족 원소 화합물을 첨가한다. 이때, 상기 알칼리 토금속염과 티타늄염의 사용량은 최종 생성되는 형광체에서 알칼리 토금속과 티타늄의 몰비가 0.5 내지 9 : 1의 몰비가 되는 양으로 한다. 상기 알카리 토금속 염은 알칼리 토금속의 탄산염 또는 질산염을 사용할 수 있으며, 그 예로 SrCO3와 Sr(NO3)2를 들 수 있다. 상기 티타늄염으로는 티타늄 산화물을 사용할 수 있으며, 그 예로 TiO2를 들 수 있다. 또한, 상기 희토류 원소와 ⅢA족 원소를 포함하는 화합물로는 할로겐화물 또는 수산화물 등이 사용될 수 있으며, 그 예로는 PrCl3또는 Al(OH)3를 들 수 있다.In the low-voltage red phosphor of the present invention, an alkaline earth metal salt and a titanium salt are mixed, and then a rare earth element compound and a group IIIA element compound are added. In this case, the amount of the alkaline earth metal salt and the titanium salt is used in an amount such that the molar ratio of the alkaline earth metal and titanium is 0.5 to 9: 1 in the final phosphor. The alkaline earth metal salt may be a carbonate or nitrate of an alkaline earth metal, and examples thereof include SrCO 3 and Sr (NO 3 ) 2 . Titanium oxide may be used as the titanium salt, and examples thereof include TiO 2 . In addition, a halide or hydroxide may be used as the compound including the rare earth element and the group IIIA element, and examples thereof include PrCl 3 or Al (OH) 3 .
상기 희토류 원소 화합물은 최종 생성되는 적색 형광체에 잔존하는 희토류 원소가 0.05 내지 5 몰%가 되도록 첨가하며, 상기 ⅢA족 원소 화합물은 최종 생성되는 적색 형광체에 잔존하는 ⅢA족 원소가 0.05 내지 80 몰%가 되도록 첨가한다.The rare earth element compound is added so that the rare earth element remaining in the final red phosphor is 0.05 to 5 mol%, and the Group IIIA element compound contains 0.05 to 80 mol% of the Group IIIA element remaining in the final red phosphor. Add as much as possible.
상기 혼합물을 1100 내지 1400℃에서 1 내지 6시간동안 소성시켜 저전압용 적색 형광체를 제조한다. 소성 온도가 상기 범위보다 낮으면 결정이 잘 형성되지 않고, 상기 범위보다 높으면 소성 공정을 실시하여 제조된 너무 딱딱한 형광체가 형성되어 사용이 불가능하다. 상기 소성은 원료 물질에 따라 공기 분위기 하에서 이루어지거나 환원 분위기 하에서 이루어질 수도 있다. 이 소정 공정에서, MTiO3(M은 Mg, Sr, Ca 또는 Ba의 알칼리 토금속임)의 매트릭스가 형성되며, 적색 발광 영역을 갖는, 희토류 원소 및 ⅢA족 원소가 상기 매트릭스 내부로 도핑된다.The mixture is calcined at 1100 to 1400 ° C. for 1 to 6 hours to produce a low phosphor red phosphor. If the firing temperature is lower than the above range, crystals are hardly formed. If the firing temperature is higher than the above range, too hard phosphors produced by the firing process are formed and cannot be used. The firing may be performed under an air atmosphere or under a reducing atmosphere depending on the raw material. In this predetermined process, a matrix of MTiO 3 (M is an alkaline earth metal of Mg, Sr, Ca or Ba) is formed, and rare earth elements and group IIIA elements having a red light emitting region are doped into the matrix.
이하 본 발명의 바람직한 실시예 및 비교예를 기재한다. 그러나 하기한 본 발명의 실시예는 본 발명의 바람직한 일 실시예일 뿐 본 발명이 하기한 실시예에 한정되는 것은 아니다.Hereinafter, preferred examples and comparative examples of the present invention are described. However, the following examples of the present invention are only preferred embodiments of the present invention, and the present invention is not limited to the following examples.
(실시예 1-3과 비교예 1 및 대조예 1)(Examples 1-3, Comparative Example 1, and Comparative Example 1)
SrCO3과 TiO2를 혼합하고, PrCl3및 Al(OH)3를 하기 표 1에 기재된 양으로 첨가하여 잘 혼합하고 소성시켰다. SrCO3과 TiO2의 몰비, 상기 사용된 화합물의 첨가량 및 소성조건은 하기 표 1에 기재된 바와 같다.SrCO 3 and TiO 2 were mixed, PrCl 3 and Al (OH) 3 were added in the amounts shown in Table 1 below, mixed well and calcined. The molar ratio of SrCO 3 to TiO 2 , the amount of the compound used and the firing conditions are as shown in Table 1 below.
상기 실시예 1-3 및 비교예 1과 대조예 1의 형광체를 사용하여 제조된 VFD를 1000시간 동안 작동시킨 후, 휘도 잔존율을 측정하였다. 휘도 잔존율은 초기 휘도에 대하여 1000시간 작동시킨 후의 휘도 비율을 %로 계산하여 얻었다.After operating VFD prepared using the phosphors of Examples 1-3 and Comparative Example 1 and Comparative Example 1 for 1000 hours, the luminance residual ratio was measured. The luminance residual ratio was obtained by calculating the luminance ratio in% after the operation for 1000 hours with respect to the initial luminance.
상기 표 2에 나타낸 것과 같이, 알칼리 토금속염인 SrCO3를 티타늄염인 TiO2보다 소량으로 사용한 실시예 1 내지 3의 형광체가 SrCO3를 TiO2보다 과량으로 사용한 비교예 1의 형광체보다 휘도 잔존율이 우수함을 알 수 있다. 아울러, 알칼리 토금속염은 티타늄염 1몰에 대하여, 0.5몰 미만으로 사용한 대조예 1의 경우 휘도 잔존율이 떨어짐을 알 수 있다.As shown in Table 2, the phosphors of Examples 1 to 3 using SrCO 3 as an alkaline earth metal salt in a smaller amount than TiO 2 as titanium salts, have a luminance remaining ratio compared to the phosphor of Comparative Example 1 using SrCO 3 in excess of TiO 2. It can be seen that this is excellent. In addition, it can be seen that the alkaline residual metal salts have a lower luminance residual ratio in the case of Comparative Example 1, which is used at less than 0.5 mol with respect to 1 mol of titanium salts.
본 발명의 저전압용 적색 형광체는 휘도 잔존율이 매우 우수하다.The low phosphor red phosphor of the present invention is very excellent in luminance residual ratio.
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| JPH0885788A (en) * | 1994-09-16 | 1996-04-02 | Futaba Corp | Phosphor |
| KR19990085329A (en) * | 1998-05-15 | 1999-12-06 | 김충섭 | Strontium titanate-based red phosphor and its manufacturing method |
| KR20000059660A (en) * | 1999-03-06 | 2000-10-05 | 김충섭 | A red fluorescent body based SrTiO3and process for preparing them |
| KR20010011735A (en) * | 1999-07-30 | 2001-02-15 | 정선종 | A red phosphor for fluorescent display and a preparation method thereof |
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| JPH0885788A (en) * | 1994-09-16 | 1996-04-02 | Futaba Corp | Phosphor |
| US5619098A (en) * | 1994-09-16 | 1997-04-08 | Futaba Denshi Kogyo K.K. | Phosphor and fluorescent display device |
| KR0172005B1 (en) * | 1994-09-16 | 1999-03-20 | 호소야 레이지 | Phosphor and fluorescent display device |
| KR19990085329A (en) * | 1998-05-15 | 1999-12-06 | 김충섭 | Strontium titanate-based red phosphor and its manufacturing method |
| KR20000059660A (en) * | 1999-03-06 | 2000-10-05 | 김충섭 | A red fluorescent body based SrTiO3and process for preparing them |
| KR20010011735A (en) * | 1999-07-30 | 2001-02-15 | 정선종 | A red phosphor for fluorescent display and a preparation method thereof |
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