CN108165266B - 一种氟氮化物荧光粉及包含该荧光粉的发光器件 - Google Patents
一种氟氮化物荧光粉及包含该荧光粉的发光器件 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 22
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 14
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 10
- 239000011737 fluorine Substances 0.000 title claims abstract description 10
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 12
- 230000005284 excitation Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 abstract description 7
- 229910052712 strontium Inorganic materials 0.000 abstract description 6
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 4
- 150000001340 alkali metals Chemical class 0.000 abstract description 4
- 239000011572 manganese Substances 0.000 abstract description 4
- 229910052700 potassium Inorganic materials 0.000 abstract description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910052744 lithium Inorganic materials 0.000 abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 description 8
- 230000008901 benefit Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910020440 K2SiF6 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- -1 fluorine nitride Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000000243 photosynthetic effect Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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Abstract
本发明涉及一种氟氮化物荧光粉及包含该荧光粉的发光器件,该荧光粉的化学式组成为:Rx(My,Euz)Ala(Sib,Gec,Mnf)NdFe,式中,R选自Li,Na,K的至少一种元素,M选自Ca,Sr,Mg,Ba的至少一种元素;x,y,z,a,b,c,d为各组成元素的物质的量,其中,0<x≤0.2,0.9≤y≤1.0,0.001≤z≤0.1,0.9≤a≤0.99,0.8≤b≤1.0,0≤c≤0.1,2.5≤d≤3.0,0.01≤e≤1.2,0.01≤f≤0.1。本发明的荧光粉同时引入碱金属、氟元素和锰元素,发光效率高,合成工艺简单易行,其结构与CaAlSiN3结构相同,可单独用于或与其他荧光粉组合用于制作高性能的发光装置。
Description
技术领域
本发明涉及无机发光材料领域,尤其涉及主要由无机化合物组成的荧光粉及其应用,具体涉及一种氟氮化物荧光粉及包含该荧光粉的发光器件。
背景技术
白光LED具有高光效、低能耗、长寿命、无污染等优点,在照明和显示领域得到了广泛的应用。随着高品质照明和显示的快速发展,LED在追求显色指数的同时,对光效的要求越来越高。在白光LED实现过程中,荧光粉起着十分重要的作用,它决定着白光LED的光效、色温和显指等性能指标。
氮化物荧光粉因具有物理化学稳定性好、激发范围宽、发射光谱纯正可调等诸多优点,受到重点研究。由于氮化物荧光粉制备条件相对苛刻,亮度提升技术仍有很大空间。Intematix公司研制在MAlSiN3:Eu2+(M=Ca,Sr,Ba)氮化物荧光粉中引入卤族元素,荧光粉亮度有一定的提升(US 8274215)。博瑞光电(Ca,Sr)AlSiN3:Eu2+基础上通过引入一定量的碱金属元素,并通过微量的氧来平衡电荷,提高了光效(CN 201310285749.0)。这说明适当引进一定量的碱金属和卤族元素能够有效提升氮化物红粉的光效。Mn4+激活的K2TiF6,K2SiF6红色荧光体具有亮度高、半峰宽窄等优点(US 3576756,US 7497973,US 7648649),此类材料的光效相对氮化物红粉较高,但在稳定性方面仍然相对较差。如果能有效结合氮化物红粉稳定好和氟化物红粉亮度高的优点,将对LED光效提升具有非常重要的意义。
发明内容
为了解决以上问题,本发明的目的是:
(1)提供了一种高亮度和高稳定性的氟氮化物的红色荧光粉;
(2)提出了含有该荧光粉的发光装置。
本发明的技术方案中提供了一种氟氮化物荧光粉及包含该荧光粉的发光器件,具体为:
一种氟氮化物荧光粉,其化学组成如下:Rx(My,Euz)Ala(Sib,Gec,Mnf)NdFe,式中,R选自Li,Na,K的至少一种元素,M选自Ca,Sr,Mg,Ba的至少一种元素;x,y,z,a,b,c,d为各组成元素的物质的量,其中,0<x≤0.2,0.9≤y≤1.0,0.001≤z≤0.1,0.9≤a≤0.99,0.8≤b≤1.0,0≤c≤0.1,2.5≤d≤3.0,0.01≤e≤1.2,0.01≤f≤0.1,该物质结构同CaAlSiN3结构相同。
优选地,0.05≤x≤0.1,0.9≤y≤0.95,0.003≤z≤0.05,0.9≤a≤0.95,0.9≤b≤1.0,0.05≤c≤0.1,2.7≤d≤3.0,0.15≤e≤0.3,0.05≤f≤0.1。
优选地,所述R元素为K,M元素只含Ca、Sr两种元素。
优选地,1.0≤x+y≤1.1,且9≤y/x≤20。
优选地,1.05≤b/a≤1,12≤b/c≤18。
优选地,4.5≤d/e≤9.5。
优选地,M元素中锶钙比(Sr/Ca)介于5和15之间。
一种发光装置,包括激发光源和发光体,该发光体包含上述的所述的荧光粉。
优选地,所述激发光源为紫外或蓝光发射源。
本发明技术方案还公开了以上所述荧光粉的制备方法,其采用高温固相法和水热法共同制备,其制备步骤为:按照化学式组分称取相应元素的单质或化合物,研磨混合均匀后,在1600℃~1800℃下烧结4~10小时即得到中间体,将得到的中间体进行破碎和后处理,作为水热法前驱体;将前驱体作为原料,通过添加一些含有相应元素的试剂,在一定的温度下搅拌充分反应1~5小时,最后烘干即得到产品。
本发明的实施例提供的技术方案可以包括以下有益效果:
本发明的荧光粉同时引入碱金属、氟元素和锰元素,发光效率高,合成工艺简单易行,其结构与CaAlSiN3结构相同,可单独用于或与其他荧光粉组合用于制作高性能的发光装置。
本发明附加的方面和优点将在下面的描述中部分给出,部分将从下面的描述中变得明显,或通过本发明的实践了解到。应当理解的是,以上的一般描述和后文的细节描述仅是示例性和解释性的,并不能限制本发明。
附图说明
利用附图对本发明作进一步说明,但附图中的实施例不构成对本发明的任何限制,对于本领域的普通技术人员,在不付出创造性劳动的前提下,还可以根据以下附图获得其它的附图。
图1为实施例1的激发和发射光谱图;
图2为实施例1的XRD图谱。
具体实施方式
下面进一步例举实施例以详细说明本发明。同样应理解,以下实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例,即本领域技术人员可以通过本文的说明做合适的范围内选择,而并非要限定于下文示例的具体数值。
实施例1
实施例1在化学组成通式K0.1Ca0.886Eu0.004Al0.9Si0.95Mn0.01N2.7F0.3中,按照化学计量比先称取金属钙的化合物、金属铝的氮化物、金属硅的氮化物、金属铕的化合物,混合均匀后,在1600℃下烧结8小时得到中间体,将得到的中间体进行破碎和后处理,作为水热法前驱体,再在80℃条件下,添加金属钾的氟化物、金属硅的化合物及金属锰的化合物试剂,水热搅拌4小时,90度烘干后,对表面进行烘干即得到产品。所得到产品的荧光发光特性见表1,发射光谱见图1。
实施例2~15
在化学组成Rx(My,Euz)Ala(Sib,Gec,Mnf)NdFe,式中,R选自Li,Na,K的至少一种元素,M选自Ca,Sr,Mg,Ba的至少一种元素;x,y,z,a,b,c,d,e,f为各组成元素的物质的量;按照不同化学组成称取相应元素的化合物,制备过程同实施例1相同,所制得荧光粉的发光特性见表1。
表1荧光粉的发光特性
以上所述仅为本发明的较佳方式,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (3)
1.一种氟氮化物荧光粉,其特征在于,其化学组成如下:
K0.1Ca0.1Sr0.83Eu0.05Al0.9Si1.0Ge0.05Mn0.01N2.7F0.3或者K0.1Ca0.1Sr0.83Eu0.05Al0.9Si0.96Ge0.08Mn0.01N2.7F0.3或者K0.1Ca0.1Sr0.83Eu0.05Al0.9Si1.08Ge0.06Mn0.01N2.7F0.3或者K0.1Ca0.1Sr0.83Eu0.05Al0.9Si0.99Ge0.06Mn0.01N2.94F0.3或者K0.1Ca0.1Sr0.83Eu0.05Al0.9Si0.945Ge0.06Mn0.01N2.94F0.3或者K0.1Ca0.1Sr0.83Eu0.05Al0.9Si0.98Ge0.06Mn0.01N2.94F0.3或者K0.1Ca0.1Sr0.83Eu0.05Al0.9Si0.99Ge0.06Mn0.03N2.94F0.3或者K0.1Ca0.1Sr0.83Eu0.05Al0.9Si0.99Ge0.06Mn0.05N2.94F0.3。
2.一种发光装置,包括激发光源和发光体,其特征在于,所述发光体包含权利要求1所述的荧光粉。
3.根据权利要求2所述的发光装置,其特征在于,所述激发光源为紫外或蓝光发射源。
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WO2005019376A1 (ja) * | 2003-08-22 | 2005-03-03 | National Institute For Materials Science | 酸窒化物蛍光体と発光器具 |
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- 2018-03-23 CN CN201810247119.7A patent/CN108165266B/zh active Active
- 2018-04-26 JP JP2018085845A patent/JP6381845B1/ja active Active
- 2018-05-13 US US15/978,178 patent/US20190100693A1/en not_active Abandoned
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CN103555325A (zh) * | 2013-11-01 | 2014-02-05 | 江苏罗化新材料有限公司 | 一种氮化物红色荧光粉及其制备方法 |
CN105985772A (zh) * | 2015-02-11 | 2016-10-05 | 大连利德照明研发中心有限公司 | 固体光源用荧光材料、其制造方法及包含该荧光材料的组合物 |
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CN108165266A (zh) | 2018-06-15 |
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