WO2019120265A1 - 一种用于三基色暖白光led的蓝色荧光粉及其制备方法 - Google Patents

一种用于三基色暖白光led的蓝色荧光粉及其制备方法 Download PDF

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WO2019120265A1
WO2019120265A1 PCT/CN2018/122504 CN2018122504W WO2019120265A1 WO 2019120265 A1 WO2019120265 A1 WO 2019120265A1 CN 2018122504 W CN2018122504 W CN 2018122504W WO 2019120265 A1 WO2019120265 A1 WO 2019120265A1
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warm white
phosphor
white led
fluorescent powder
blue phosphor
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陈朝
杨星
陈佳超
李扬
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厦门大学
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    • C—CHEMISTRY; METALLURGY
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    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7759—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing samarium
    • C09K11/7762—Halogenides
    • C09K11/7763—Halogenides with alkali or alkaline earth metals
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • 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
    • C09K11/7737—Phosphates
    • C09K11/7738—Phosphates with alkaline earth metals
    • C09K11/7739—Phosphates with alkaline earth metals with halogens
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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
    • C09K11/774—Borates
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    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • H01L33/502—Wavelength conversion materials
    • H01L33/504—Elements with two or more wavelength conversion materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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  • the invention relates to a luminescent material and a preparation method thereof, in particular to a blue phosphor for a three-primary warm white LED and a preparation method thereof.
  • LED lighting is not only self-sufficient for the sustainable development of society and the environment, but also can drive related industries, enhance the competitiveness of China's lighting industry, and develop a number of emerging industries with independent intellectual property rights that are internationally competitive, and increase employment. Opportunities are the most potential competitors in the future to replace traditional lighting, and to promote the upgrading of the lighting industry and promote the development of new manufacturing industries.
  • white light emission is to use a blue chip to excite yellow phosphor.
  • the most mature yellow phosphor is mainly YAG:Ce3+, which can be effectively excited by 440-480nm blue LED chip and complemented by blue light.
  • White light however, such illuminating methods have defects such as poor color reproduction, low color rendering index, and difficulty in dispensing warm colors.
  • some single-substrate white phosphors have been reported as fluorescent materials for white LEDs, but most of them are cold white light. Even some bright white phosphors are doped with at least two rare earth ions in the matrix.
  • the element realizes luminescence, which not only increases the cost of the phosphor, but also causes the energy loss to be directly caused by the cascading excitation, and the final luminous efficiency of the phosphor is relatively low. It is very important to promote the development and promotion of warm white LEDs in the industry by exciting three-primary phosphors with near-ultraviolet or violet chips, and developing warm white phosphors with lower cost, higher luminous efficiency and better performance.
  • a blue phosphor for a warm white LED having a chemical formula of Sr (2-x) Eu x (BO 3 ) y (PO 4 ) (1-y) Cl, wherein 0.001 ⁇ x ⁇ 0.1, 0.001 ⁇ y ⁇ 0.5.
  • the chemical formula of the phosphor for warm white LEDs provided by the present invention is preferably Sr 1.95 Eu 0.05 (BO 3 ) 0.25 (PO 4 ) 0.75 Cl.
  • the phosphor of the present invention preferably has a chemical formula of Sr 1.99 Eu 0.01 (BO 3 ) 0.25 (PO 4 ) 0.75 Cl.
  • the invention also provides a preparation method of a phosphor for a warm white LED, comprising the following steps:
  • the red powder can be mixed with warm white light with high efficiency and high index.
  • the polishing time of the step (a) in the method for preparing a phosphor for a warm white LED provided by the present invention is 10-20 min.
  • the heating rate of the step (b) is 3-7 ° C / min.
  • the step (b) reducing atmosphere means a carbon dioxide-embedded or a reducing atmosphere formed by a mixed gas of H 2 and N 2 .
  • the step (b) is heated and heated to 900-1150 ° C for 5 h; preferably at 1050 ° C for 5 h.
  • step (a) weighs raw materials SrCO 3 (AR), NH 4 Cl (AR), H 3 BO 3 (AR), Eu 2 O 3 (99.99 Both %) and NH 4 H 2 PO 4 (AR) are commercially available products.
  • the luminescent material prepared by the invention has optical performance detection, and the color effect is up to 86.7 lm/W or even 104 m/W under the condition of a color rendering index of 90 or more.
  • Example 1 is an X-ray diffraction pattern (XRD) of blue phosphors prepared in Example 1 and Example 2.
  • Example 2 is an excitation spectrum and an emission spectrum of the blue phosphor prepared in Example 1.
  • Example 3 is an emission spectrum of a three-primary warm white phosphor prepared in Example 1.
  • the excitation wavelength was 395 nm.
  • Example 4 is a luminescence and color coordinate diagram of a three-primary warm white LED prepared in Example 1 under ultraviolet excitation.
  • the raw materials used in the examples of the present invention are SrCO 3 (AR), NH 4 Cl (AR), H 3 BO 3 (AR), Eu 2 O 3 (99.99%) and NH 4 H 2 PO 4 (AR). Commercial goods.
  • the prepared Sr 1.95 Eu 0.05 (BO 3 ) 0.25 (PO 4 ) 0.75 Cl phosphor was excited by violet light with CaAlSiN 3 :Eu 2+ red phosphor and (SrBa) 2 SiO 4 :Eu 2+ green phosphor A certain proportion of the mixture is coated on a 395 InGaN LED chip with an operating current of 350 mA to emit warm white light with a color temperature of 3153 K.
  • the optical properties of the luminescent materials prepared in the examples are tested.
  • the color rendering index is above 90, and the luminous efficacy is obtained. Up to 86.7lm/W.
  • Example 1 The same as Example 1 except that the phosphors produced were different in chemical formula. Its X-ray diffraction pattern (XRD) is shown in Figure 1.
  • strontium carbonate SrCO 3
  • anhydrous ammonium chloride NH 4 Cl
  • 0.268g boric acid
  • H 3 BO 3 boric acid
  • antimony trioxide Eu 2 O 3
  • ammonium dihydrogen phosphate NH 4 H 2 PO 4

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  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Luminescent Compositions (AREA)
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Abstract

本发明公开了一种用于三基色暖白光LED的蓝色荧光粉及其制备方法。以碳酸锶(SrCO3)、无水氯化铵(NH4Cl)、硼酸(H3BO3)、三氧化二铕(Eu2O3)和磷酸二氢铵(NH4H2PO4)为原料，在还原气氛中固相烧结法，得到化学式为Sr(2-x)Eux(BO3)y(PO4)(1-y)Cl，其中0.001≤x≤0.1、0.001≤y≤0.5的蓝色荧光粉。与CaAlSiN3：Eu2+红色荧光粉和(SrBa)2SiO4:Eu2+绿色荧光粉按一定比例配比可实现近紫外光激发高显指高光效的暖白光发射，具有非常广阔的应用前景。

Description

一种用于三基色暖白光LED的蓝色荧光粉及其制备方法 技术领域
本发明涉及发光材料及其制备方法，具体地说是一种用于三基色暖白光LED的蓝色荧光粉及其制备方法。
背景技术
世界性的能源危机使得白光LED照明成为国家发展的战略计划，随着国家半导体照明工程的启动，“十一五”计划予以的大量经费资助，加上我国白光LED用稀土荧光粉资源丰富，相关知识产权的建立，我国将迅速进入白光LED照明市场。
LED照明的提倡不仅自利于社会和环境的可持续性发展，还可以带动相关产业，提升我国照明产业的竞争力，并将发展一批具有自主知识产权的有国际竞争力的新兴产业，增加就业机会，是未来能够代替传统照明最具潜力的竞争者，对节约能源统照明产业升级，促进新型制造业发展意义。
目前实现高流明效率白光发射的一种方式是用蓝光芯片激发黄色荧光粉，其中最为成熟的黄色荧光粉主要是YAG:Ce3+，它能够被440-480nm的蓝光LED芯片有效激发，与蓝光互补形成白光；但是，这类发光方式存在色彩还原性差、显色指数低、很难配出暖色系等缺陷。近年来也出现了一些单一基质白光荧光粉作为白光LED的荧光粉材料的研究报道，但其大多为冷白光，即使有部分暖白光的荧光粉，也是在基质中掺杂了至少两种稀土离子或元素实现发光的，这不仅使得荧光粉的成本增加，而且这种间级联激发直接导致能量损耗比较严重，荧光粉最终的发光效率比较低。以近紫外光或紫光芯片激发三基色荧光粉，开发成本较低、 发光效率高、性能更加优异的暖白光荧光粉，这对促进行业内暖白光LED的发展和推广使用具有非常重要的意义。
发明内容
本发明的目的是提供一种用于暖白光LED的蓝色荧光粉及其制备方法。
本发明的目的是通过以下技术方案实现的：一种用于暖白光LED的蓝色荧光粉，该荧光粉的化学通式为Sr (2-x)Eu x(BO 3) y(PO 4) (1-y)Cl，其中0.001≤x≤0.1、0.001≤y≤0.5。
本发明提供的用于暖白光LED的荧光粉的化学式优选为Sr 1.95Eu 0.05(BO 3) 0.25(PO 4) 0.75Cl。
在另一实施例中，本发明提供的荧光粉的化学式优选为Sr 1.99Eu 0.01(BO 3) 0.25(PO 4) 0.75Cl。
本发明还提供了一种用于暖白光LED的荧光粉的制备方法，包括以下步骤：
(a)按照荧光粉的化学通式Sr (2-x)Eu x(BO 3) y(PO 4) (1-y)Cl中各元素的摩尔比称取原料SrCO 3、NH 4Cl、H 3BO 3、Eu 2O 3和NH 4H 2PO 4，混合，研磨，得混合物，所述化学通式中0.001≤x≤0.1、0.001≤y≤0.5；
(b)将所述混合物置于还原气氛中，加热升温至900-1150℃焙烧3-5h，得烧结体；
(c)将所述烧结体冷却至室温后研磨，得用于三基色暖白光LED的蓝色荧光粉。
本发明提供的用于暖白光LED的荧光粉的制备方法中步骤(a)化学通式中优选x＝0.05，y＝0.25；在优选条件下制备的荧光粉蓝光强度高、与商业绿粉与红粉可混合出高效率高显指的暖白光。
本发明提供的用于暖白光LED的荧光粉的制备方法中步骤(a)的研磨时间为10-20min。
本发明提供的用于暖白光LED的荧光粉的制备方法中步骤(b)加热速率为3-7℃/min。
本发明提供的用于暖白光LED的荧光粉的制备方法中步骤(b)还原气氛是指碳粉包埋或H 2、N 2混合气体形成的还原气氛。
本发明提供的用于暖白光LED的荧光粉的制备方法中步骤(b)加热升温至900-1150℃焙烧5h；优选1050℃焙烧5h。
本发明提供的用于暖白光LED的荧光粉的制备方法中步骤(a)称取原料SrCO 3(A.R.)、NH 4Cl(A.R.)、H 3BO 3(A.R.)、Eu 2O 3(99.99％)和NH 4H 2PO 4(A.R.)均为市售商品。
本发明的优点如下：
本发明所制备的发光材料经光学性能检测，显色指数在90以上的情况下，其光效高达86.7lm/W,甚至104m/W。
附图说明
图1为实施例1和实施例2制备的蓝色荧光粉的X射线衍射图谱(XRD)。
图2为实施例1制备的蓝色荧光粉的激发光谱图和发射光谱图。其中，激发波长λex＝395nm，发射波长λem＝446nm。
图3为实施例1制备的三基色暖白光荧光粉的发射光谱图。激发波长为395nm。
图4为实施例1制备的三基色暖白光LED在紫外激发下的发光及色坐标图。
具体实施方式
下面实施例用于进一步详细说明本发明，但实施例并不对本发明做任何形式的限定。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。但不以任何形式限制本发明。
实施例1：
分别称取碳酸锶(SrCO 3),1.406g、无水氯化铵(NH 4Cl),0.268g、硼酸(H 3BO 3),0.062g、三氧化二铕(Eu 2O 3),0.088g\磷酸二氢铵(NH 4H 2PO 4)0.371g，置于玛瑙研钵中充分研磨30min并混合均匀后；将研磨后的粉末置于还原气氛中焙烧，以加热速率为5℃/min升温至1000℃，在该温度下烧结6h，自然冷却到室温；将样品取出研磨，得到化学式为Sr 1.95Eu 0.05(BO 3) 0.25(PO 4) 0.75Cl的荧光粉。其X射线衍射图谱(XRD)见图1。
本发明的实施例中使用的原料SrCO 3(A.R.)、NH 4Cl(A.R.)、H 3BO 3(A.R.)、Eu 2O 3(99.99％)和NH 4H 2PO 4(A.R.)均为市售商品。
所制备的Sr 1.95Eu 0.05(BO 3) 0.25(PO 4) 0.75Cl荧光粉，在紫光激发下与CaAlSiN 3：Eu 2+红色荧光粉和(SrBa) 2SiO 4:Eu 2+绿色荧光粉按一定比例混匀涂覆在工作电流为350mA的395InGaN LED芯片上可发射色温3153K的暖白光，检测实施例所制备的发光材料的光学性能检测，显色指数在90以上的情况下，其光效高达86.7lm/W。
结果见图2至图4。
实施例2
同实施例1基本相同，所不同的是，制得的荧光粉化学式不同。其X射线衍射图谱(XRD)见图1。
分别称取碳酸锶(SrCO 3),1.465g、无水氯化铵(NH 4Cl),0.268g、硼酸(H 3BO 3),0.062g、三氧化二铕(Eu 2O 3),0.018g和磷酸二氢铵(NH 4H 2PO 4),0.371g，置于玛瑙研钵中充分研磨30min并混合均匀后；将研磨后的粉末置于还原气氛中焙烧，以加热速率为5℃/min升温至1000℃，在该温度下烧结6h，自然冷却到室温；将样品取出研磨，得到化学式为Sr 1.99Eu 0.01(BO 3) 0.25(PO 4) 0.75Cl的荧光粉。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受所述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (9)

  1. 一种用于三基色暖白光LED的蓝色荧光粉，其特征在于，该荧光粉的化学通式为Sr (2-x)Eu x(BO 3) y(PO 4) (1-y)Cl，其中0.001≤x≤0.1、0.001≤y≤0.5。
  2. 根据权利要求1所述的用于三基色暖白光LED的蓝色荧光粉，其特征在于，该荧光粉的化学式为Sr 1.95Eu 0.05(BO 3) 0.25(PO 4) 0.75Cl。
  3. 根据权利要求1所述的用于三基色暖白光LED的蓝色荧光粉，其特征在于，该荧光粉的化学式为Sr 1.99Eu 0.01(BO 3) 0.25(PO 4) 0.75Cl。
  4. 一种用于三基色暖白光LED的蓝色荧光粉的制备方法，包括以下步骤：
    (a)按照荧光粉的化学通式Sr (2-x)Eu x(BO 3) y(PO 4) (1-y)Cl中各元素的摩尔比称取原料SrCO 3、NH 4Cl、H 3BO 3、Eu 2O 3和NH 4H 2PO 4，混合，研磨，得混合物，所述化学通式中0.001≤x≤0.1，0.001≤y≤0.5；
    (b)将所述混合物置于还原气氛中，加热升温至900-1150℃焙烧4-5h，得烧结体；
    (c)将所述烧结体冷却至室温后研磨，得用于三基色暖白光LED的蓝色荧光粉。
  5. 根据权利要求4所述的用于三基色暖白光LED的蓝色荧光粉的制备方法，其特征在于，步骤(a)所述化学通式中x＝0.05，y＝0.25。
  6. 根据权利要求4所述的用于三基色暖白光LED的蓝色荧光粉的制备方法，其特征在于，步骤(a)所述的研磨时间为10-20min。
  7. 根据权利要求4所述的用于三基色暖白光LED的蓝色荧光粉的制备方法，其特征在于，步骤(b)加热速率为3-7℃/min。
  8. 根据权利要求4所述的用于三基色暖白光LED的蓝色荧光粉的制备方法，其特征在于，步骤(b)所述的还原气氛是指碳粉包埋或H2、N2混合气体形成的还 原气氛。
  9. 根据权利要求4-8任一项所述的用于三基色暖白光LED的蓝色荧光粉的制备方法，其特征在于，步骤(b)加热升温至900-1150℃焙烧5h。
PCT/CN2018/122504 2017-12-22 2018-12-21 一种用于三基色暖白光led的蓝色荧光粉及其制备方法 WO2019120265A1 (zh)

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CN109971477B (zh) * 2019-01-25 2022-02-08 云南大学 一种钐掺杂硼磷酸盐橙红色荧光粉及其制备方法和应用
CN110335935B (zh) * 2019-06-14 2021-07-13 厦门大学 一种近紫外激发单芯片全光谱led及其制备方法
CN116162457A (zh) * 2022-12-15 2023-05-26 上海应用技术大学 一种紫光/紫外激发的蓝光荧光粉及其制备方法与应用

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