KR20010111834A - A blue emitting phosphor for low-voltage applications and a method of preparing the same - Google Patents

A blue emitting phosphor for low-voltage applications and a method of preparing the same Download PDF

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KR20010111834A
KR20010111834A KR1020000032518A KR20000032518A KR20010111834A KR 20010111834 A KR20010111834 A KR 20010111834A KR 1020000032518 A KR1020000032518 A KR 1020000032518A KR 20000032518 A KR20000032518 A KR 20000032518A KR 20010111834 A KR20010111834 A KR 20010111834A
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phosphor
low
blue phosphor
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flux
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KR100696678B1 (en
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유용찬
유일
유영철
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김순택
삼성에스디아이 주식회사
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Abstract

본 발명의 청색 형광체는 SrTiO3형광체 모체에 융제(flux)를 첨가한 후 1차 소성한 다음, 환원 분위기에서 2차 소성하여 제조된다. 스트론튬염과 티타늄 산화물(TiO2)의 혼합물에 융제를 첨가하여 혼합한 다음, 대기 분위기하에서 1100∼1400 ℃에서 1∼6시간 1차 소성시킨다. 상기 1차 소성된 물질을 환원 분위기하에서 1000∼1300 ℃에서 0.5∼2시간 2차 소성시켜 형광체에 도전성을 부여한다. 본 발명의 저전압용 SrTiO3청색 형광체는 In2O3, V2O5, WO3등과 같은 도전물질을 첨가하여 사용될 수도 있다.The blue phosphor of the present invention is prepared by adding a flux to a SrTiO 3 phosphor matrix, followed by primary firing, and then secondary firing in a reducing atmosphere. A flux is added to the mixture of strontium salt and titanium oxide (TiO 2 ), followed by mixing, followed by primary firing at 1100 to 1400 ° C. for 1 to 6 hours in an air atmosphere. The primary fired material is secondary fired at 1000 to 1300 ° C. for 0.5 to 2 hours in a reducing atmosphere to impart conductivity to the phosphor. The low-voltage SrTiO 3 blue phosphor of the present invention may be used by adding a conductive material such as In 2 O 3 , V 2 O 5 , WO 3, or the like.

Description

저전압용 청색 형광체 및 그 제조방법{A BLUE EMITTING PHOSPHOR FOR LOW-VOLTAGE APPLICATIONS AND A METHOD OF PREPARING THE SAME}Low voltage blue phosphor and its manufacturing method {A BLUE EMITTING PHOSPHOR FOR LOW-VOLTAGE APPLICATIONS AND A METHOD OF PREPARING THE SAME}

[산업상 이용 분야][Industrial use]

본 발명은 저전압용 청색 형광체 및 그 제조방법에 관한 것으로서, 더욱 상세하게는 VFD 또는 FED와 같은 저전압 표시장치에 적용될 수 있는 저전압 구동 가능한 청색 형광체 및 그 제조방법에 관한 것이다.The present invention relates to a low voltage blue phosphor and a method of manufacturing the same, and more particularly, to a low voltage driveable blue phosphor that can be applied to a low voltage display device such as VFD or FED and a method of manufacturing the same.

[종래 기술][Prior art]

주로 1㎸ 이하의 저전압 디스플레이에는 진공 형광 디스플레이(Vacuum Fluorescent 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. 이들 저전압용 표시 장치는 열선 등과 같은 전자 방출 장치(emitter)로부터 방출된 전자가 형광체를 발광시켜 원하는 화상을 재현하는 구조로 되어 있다.Low voltage displays of less than 1 kV include vacuum fluorescent display (VFD) and field emission display (FED). 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. These low voltage display devices have a structure in which electrons emitted from an electron emitter such as a hot wire emit light to emit a phosphor, thereby reproducing a desired image.

FED, VFD 등의 저전압 구동 장치용 형광체는 저저항이고, 발광 개시 전압이 낮아야 하고, 저가속 전압에서의 발광 효율이 높고 휘도 포화가 없으며, 형광체 입자 표면에 결함이 적고, 저속전자 여기 발광상태가 안정하고 분해가 일어나지 않아야 한다.Phosphors for low voltage drive devices such as FED and VFD should have low resistance, low emission start voltage, high luminous efficiency at low speed voltage, no luminance saturation, less defects on the surface of phosphor particles, and low electron excitation emission state. It should be stable and not degrade.

현재 저전압 구동 장치용 형광체로는 황화물계(sulfide) 형광체가 광범위하게 사용되고 있다. 저전압용 청색 형광체로 사용되고 있는 황화물계 형광체로는 ZnS:Zn이다. 이 형광체는 발광 효율은 우수하나 고전류의 저전압 조건에서 황화물이 분해되어 형광체 자체가 안정하지 못하여 수명이 짧다는 단점이 있다.Currently, sulfide phosphors are widely used as phosphors for low voltage driving devices. The sulfide-based phosphor used as the low voltage blue phosphor is ZnS: Zn. This phosphor is excellent in luminous efficiency but has a disadvantage in that the sulfide is decomposed under high current and low voltage conditions, so that the phosphor itself is not stable and the life is short.

황화물계 형광체는 모체(host material)의 저항이 높아서 저속 전자선 여기 발광을 행하기 때문에 저항을 낮추기 위한 방법으로 도전물질을 첨가하여 사용하고 있다. 그러나 전자선 여기시 황화물계 가스 방출과 형광체 물질이 분해비산에 의해 캐소드 필라민트의 오염과 형광체 효율을 저하시키는 문제점이 있기 때문에 비황화물계 형광체의 개발이 활발하게 진행되고 있다.Since sulfide-based phosphors have high resistance of a host material and emit low-speed electron beam excitation light emission, a conductive material is added and used as a method for lowering resistance. However, the development of non-sulfide-based phosphors has been actively progressed due to the problem of sulfide-based gas emission and phosphor material decomposing and scattering the electron beams during the electron beam excitation, thereby degrading the cathode filament and reducing phosphor efficiency.

본 발명의 목적은 화학적으로 안정하여 수명이 길고, 도전성이 우수한 저전압용 청색 형광체 및 그 제조방법을 제공하기 위한 것이다.An object of the present invention is to provide a low-voltage blue phosphor for chemical stability, long life and excellent conductivity, and a method of manufacturing the same.

본 발명의 다른 목적은 캐소드 필라민트를 오염시키지 않는 산화물계 청색 형광체를 제공하기 위한 것이다.It is another object of the present invention to provide an oxide-based blue phosphor that does not contaminate the cathode pilates.

상기한 목적을 달성하기 위하여, 본 발명에서는 SrTiO3형광체 모체에 융제를 첨가한 후 1차 소성한 다음, 환원 분위기에서 2차 소성시켜 저전압 청색 형광체를제조한다.In order to achieve the above object, in the present invention, the flux is added to the SrTiO 3 phosphor matrix, and then calcined first, and then calcined in a reducing atmosphere to prepare a low voltage blue phosphor.

이하 본 발명을 더욱 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.

본 발명의 청색 형광체의 제조공정중 첫 번째 단계로 스트론튬염과 티타늄 산화물(TiO2)의 혼합물에 융제를 첨가하여 혼합한다. 상기 스트론튬을 포함하는 염으로는 SrCO3또는 Sr(NO3)2등이 사용될 수 있으며, 스트론튬염과 티타늄 산화물의 몰비는 0.6 내지 1 : 1인 것이 바람직하며, 더욱 바람직하게는 0.8 내지 1 : 1, 가장 바람직하게는 0.8 : 1이다. 스트론튬염과 티타늄 산화물의 몰비가 상기 범위를 벗어나는 경우에는 제조되는 형광체의 휘도가 저하되므로 바람직하지 않다. 상기 융제로 사용되는 화합물로서는 Li3PO4, Li2CO3, Na3PO4, K2HPO4또는 KF 등이 사용될 수 있다. 이러한 화합물들은 입경을 성장시키거나 입형을 조절한다. 융제의 사용양은 10∼50 몰%가 바람직하며 이 범위를 초과하는 경우에는 제조되는 형광체의 휘도가 저하되는 문제점이 있다.As a first step in the process of manufacturing the blue phosphor of the present invention, a flux is added to the mixture of strontium salt and titanium oxide (TiO 2 ) and mixed. As the salt containing strontium, SrCO 3 or Sr (NO 3 ) 2 may be used, and the molar ratio of strontium salt and titanium oxide is preferably 0.6 to 1: 1, more preferably 0.8 to 1: 1. And most preferably 0.8: 1. If the molar ratio of strontium salt and titanium oxide is out of the above range, it is not preferable because the luminance of the produced phosphor is lowered. Li 3 PO 4 , Li 2 CO 3 , Na 3 PO 4 , K 2 HPO 4 or KF may be used as the compound used as the flux. These compounds grow or control particle size. The amount of the flux is preferably 10 to 50 mol%, and if it exceeds this range, there is a problem that the luminance of the phosphor to be produced is lowered.

두 번째 단계로 상기 혼합물을 대기 분위기 하에서 1100∼1400℃의 온도로 1∼6시간동안 1차 소성시킨다. 1차 소성 공정을 거쳐 SrTiO3매트릭스가 형성되며, 이때 융제는 휘발되어 제거된다.In a second step, the mixture is first calcined under an atmospheric atmosphere at a temperature of 1100-1400 ° C. for 1-6 hours. The SrTiO 3 matrix is formed through a primary firing process, in which the flux is removed by volatilization.

상기 1차 소성된 물질에 대하여 환원 분위기 하에서 1000∼1300℃의 온도로 0.5∼2시간동안 2차 소성을 실시한다. 이 2차 소성 공정을 통하여 형광체의 결정성을 증가시켜 휘도를 향상시킬 수 있다. 상기 1차 소성된 물질을 산소가 결핍된 환원 분위기에서 2차 소성시키게 되면 형광체가 도전성을 가지게 된다. 상기 환원분위기는 H25 부피%와 N295 부피%의 혼합 분위기이다.The primary fired material is subjected to secondary firing at a temperature of 1000 to 1300 ° C. for 0.5 to 2 hours under a reducing atmosphere. Through this secondary firing process, the crystallinity of the phosphor may be increased to improve luminance. When the first calcined material is secondarily calcined in a oxygen-deficient reducing atmosphere, the phosphor becomes conductive. The reducing atmosphere is a mixed atmosphere of H 2 5 vol% and N 2 95 vol%.

이와 같이 2차 소성된 물질을 시브(sieve)를 사용하여 분급함으로써 저전압 청색 형광체를 제조한다. 본 발명의 저전압용 SrTiO3청색 형광체는 In2O3, V2O5, WO3등과 같은 도전물질을 첨가하여 사용될 수도 있다. 상기 도전 물질은 형광체에 대하여 10∼20 중량%의 양으로 첨가되는 것이 바람직하다.The secondary calcined material is classified using a sieve to produce a low voltage blue phosphor. The low-voltage SrTiO 3 blue phosphor of the present invention may be used by adding a conductive material such as In 2 O 3 , V 2 O 5 , WO 3, or the like. The conductive material is preferably added in an amount of 10 to 20% by weight based on the phosphor.

다음은 본 발명의 이해를 돕기 위하여 바람직한 실시예를 제시한다. 그러나 하기의 실시예들은 본 발명을 보다 쉽게 이해하기 위하여 제공되는 것일 뿐 본 발명이 하기의 실시예에 한정되는 것은 아니다.The following presents a preferred embodiment to aid the understanding of the present invention. However, the following examples are merely provided to more easily understand the present invention, and the present invention is not limited to the following examples.

실시예 1-3Example 1-3

SrCO3, TiO2및 Li3PO4를 하기 표 1에 기재된 양으로 혼합하였다. 상기 혼합물을 대기 분위기하에서 1차 소성한 다음, 환원 분위기하에서 2차 소성시켜 청색 형광체인 SrTiO3를 제조하였다. 1차 소성과 2차 소성시의 온도와 시간은 하기 표 1에 기재된 바와 같다.SrCO 3 , TiO 2 and Li 3 PO 4 were mixed in the amounts shown in Table 1 below. The mixture was first calcined in an atmosphere and then calcined in a reducing atmosphere to prepare SrTiO 3 , which is a blue phosphor. Temperature and time at the time of primary baking and secondary baking are as Table 1 below.

실시예 4Example 4

청색 형광체인 SrTiO3에 15 중량%의 In2O3를 첨가시킨 것을 제외하고는 상기 실시예 1과 동일한 방법으로 형광체를 제조하였다.A phosphor was prepared in the same manner as in Example 1, except that 15 wt% of In 2 O 3 was added to SrTiO 3 , which is a blue phosphor.

비교예 1Comparative Example 1

SrCO3와 TiO2를 하기 표 1에 기재된 양으로 혼합하고 1차 소성시에 Li3PO4를첨가하지 않은 것을 제외하고 상기 실시예 1과 동일한 방법으로 청색 형광체를 제조하였다.A blue phosphor was prepared in the same manner as in Example 1 except that SrCO 3 and TiO 2 were mixed in the amounts shown in Table 1 and Li 3 PO 4 was not added during the first firing.

비교예 2Comparative Example 2

대기 분위기하에서 2차 소성시킨 것을 제외하고 상기 비교예 1과 동일한 방법으로 청색 형광체를 제조하였다.A blue phosphor was prepared in the same manner as in Comparative Example 1 except that the material was calcined in an air atmosphere for the second time.

SrCO3[g]SrCO 3 [g] TiO2[g]TiO 2 [g] SrCO3: TiO2몰비SrCO 3 : TiO 2 molar ratio Li3PO4[중량%]Li 3 PO 4 [% by weight] 1차소성조건Primary firing condition 2차소성조건Second firing condition 온도[℃]Temperature [℃] 시간[h]Time [h] 온도[℃]Temperature [℃] 시간[h]Time [h] 실시예Example 1One 147.63147.63 79.898679.8986 1 : 11: 1 1.51.5 13001300 66 11001100 1One 22 147.63147.63 63.9190463.91904 1 : 0.81: 0.8 1.51.5 13001300 66 11001100 1One 33 147.63147.63 47.7392847.73928 1 : 0.61: 0.6 1.51.5 13001300 66 11001100 1One 44 147.63147.63 79.898879.8988 1 : 11: 1 1.51.5 13001300 66 11001100 1One 비교예Comparative example 1One 147.63147.63 79.898879.8988 1 : 11: 1 00 13001300 66 11001100 1One 22 147.63147.63 63.9190463.91904 1 : 0.81: 0.8 00 13001300 66 11001100 1One

상기 실시예 1-4 및 비교예 1-2의 형광체에 대하여 27V의 구동전압에서 CIE 색좌표와 상대휘도를 측정하여 하기 표 2에 기재하였다.The CIE color coordinates and relative luminance of the phosphors of Examples 1-4 and Comparative Examples 1-2 were measured at a driving voltage of 27 V, and the results are shown in Table 2 below.

색좌표Color coordinates 상대휘도(%)Relative luminance (%) xx yy 실시예Example 1One 0.180.18 0.190.19 100100 22 0.190.19 0.200.20 120120 33 0.180.18 0.190.19 7070 44 0.190.19 0.210.21 200200 비교예Comparative example 1One 0.180.18 0.190.19 7070 22 0.190.19 0.200.20 8080

상기 표 2에 나타낸 것과 같이, 실시예 1 내지 4의 형광체의 상대 휘도가 비교예 1 내지 2보다 우수하게 나타남을 알 수 있다.As shown in Table 2, it can be seen that the relative luminance of the phosphors of Examples 1 to 4 is superior to Comparative Examples 1 to 2.

본 발명에 따른 저전압용 청색 형광체는 SrTiO3형광체 모체에 융제를 첨가한 후 1차 소성한 다음, 환원 분위기에서 2차 소성됨으로써 도전성이 증가되고 화학적으로 안정하여 수명이 길다. 또한 구동 전압이 낮아 VFD 또는 FED와 같은 저전압 표시장치에 적용될 수 있다.The blue phosphor for low voltage according to the present invention is first baked after adding a flux to the SrTiO 3 phosphor matrix, and then calcined in a reducing atmosphere to increase conductivity and to be chemically stable and thus have a long service life. In addition, the low driving voltage can be applied to low voltage display devices such as VFD or FED.

Claims (6)

스트론튬염과 티타늄 산화물(TiO2)의 혼합물에 융제를 첨가하여 혼합하는 공정;Adding a flux to a mixture of strontium salt and titanium oxide (TiO 2 ) and mixing the mixture; 상기 혼합물을 대기 분위기하에서 1100∼1400 ℃에서 1∼6시간 1차 소성시키는 공정; 및Firstly baking the mixture at 1100 to 1400 ° C. for 1 to 6 hours in an air atmosphere; And 상기 1차 소성된 물질을 환원 분위기하에서 1000∼1300 ℃에서 0.5∼2시간 2차 소성시키는 공정;Second firing the first calcined material at 1000 to 1300 ° C. for 0.5 to 2 hours in a reducing atmosphere; 을 포함하는 저전압용 청색 형광체의 제조방법.A low voltage blue phosphor manufacturing method comprising a. 제 1항에 있어서, 상기 스트론튬염 : 티타늄 산화물의 혼합 몰비는 0.6∼1 : 1인 저전압용 청색 형광체의 제조방법.The method of producing a blue phosphor for low voltage according to claim 1, wherein a mixing molar ratio of the strontium salt to titanium oxide is 0.6 to 1: 1. 제 1 항에 있어서, 상기 융제는 Li3PO4, Li2CO3, Na3PO4, K2HPO4및 KF로 이루어진 군으로부터 선택된 저전압용 청색 형광체의 제조방법.The method of claim 1, wherein the flux is selected from the group consisting of Li 3 PO 4 , Li 2 CO 3 , Na 3 PO 4 , K 2 HPO 4, and KF. 제 3 항에 있어서, 상기 융제의 첨가량은 10∼50 몰%인 저전압용 청색 형광체의 제조방법.The method for producing a low voltage blue phosphor according to claim 3, wherein the addition amount of the flux is 10 to 50 mol%. 제 1 항 내지 제 4 항의 어느 하나의 항에 따라 제조된 저전압용 SrTiO3청색 형광체.A low voltage SrTiO 3 blue phosphor prepared according to any one of claims 1 to 4. 제5항에 있어서, 상기 형광체에 In2O3, V2O5및 WO3으로 이루어진 군으로부터 선택된 도전물질을 더 첨가시켜 제조된 저전압용 SrTiO3청색 형광체.The low-voltage SrTiO 3 blue phosphor according to claim 5 , further prepared by adding a conductive material selected from the group consisting of In 2 O 3 , V 2 O 5, and WO 3 to the phosphor.
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CN105754597A (en) * 2016-03-31 2016-07-13 中南大学 Titanate host material for rare earth phosphors and preparing method thereof
CN105754597B (en) * 2016-03-31 2017-10-17 中南大学 A kind of fluorescent RE powder titanate host material and preparation method thereof

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