CN108384534B - 一种铜铽共掺的CaSrSiO4纳米荧光粉末 - Google Patents
一种铜铽共掺的CaSrSiO4纳米荧光粉末 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 31
- HXRZOZRERHSWNW-UHFFFAOYSA-N copper terbium Chemical compound [Cu].[Cu].[Tb] HXRZOZRERHSWNW-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000010949 copper Substances 0.000 claims abstract description 25
- 239000002105 nanoparticle Substances 0.000 claims abstract description 11
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 4
- 239000007790 solid phase Substances 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 abstract description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 10
- 150000002910 rare earth metals Chemical class 0.000 abstract description 10
- 238000005424 photoluminescence Methods 0.000 abstract description 7
- 238000000103 photoluminescence spectrum Methods 0.000 abstract description 3
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 abstract description 3
- 230000005284 excitation Effects 0.000 abstract description 2
- 238000010791 quenching Methods 0.000 abstract description 2
- 230000000171 quenching effect Effects 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- -1 terbium ions Chemical class 0.000 description 3
- 150000001217 Terbium Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052918 calcium silicate Inorganic materials 0.000 description 2
- 239000000378 calcium silicate Substances 0.000 description 2
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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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
- C09K11/7749—Aluminates
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Abstract
本发明属于稀土发光材料领域。采用高温固相烧结法制备了系列铜铽共掺的CaSrSiO4纳米荧光粉。在245 nm紫外光激发下，系统测量了样品的光致发光谱，发现与未掺铜的CaSrSiO4:Tb3+纳米荧光粉末发光强度相比较，加入了铜纳米颗粒后，荧光粉发光强度发生明显改变，在掺铜浓度为0.3 mol%时，铜铽共掺的CaSrSiO4纳米荧光粉的发光性能得到明显改善，增强一倍左右。随着掺铜浓度的继续提高，将发生浓度淬灭，荧光粉的光致发光强度减弱。表明通过改变铜纳米颗粒的掺入量，可以对掺铽CaSrSiO4纳米荧光粉的光致发光性能起到调控作用。
Description
技术领域
本发明涉及稀土发光材料领域，具体公开一种在硅酸锶钙基质中掺杂三价铽离子的基础上加入了铜纳米颗粒具有优秀光致发光特性的金属--稀土纳米荧光粉。利用金属的局域表面等离子体共振效应，可显著提高稀土掺杂发光材料的发光效率。
背景技术
稀土掺杂发光材料具有发光效率高、波长丰富和性能稳定等诸多优点，广泛应用于工农业、医疗和军事等各个领域。特别是在光学领域，稀土掺杂纳米荧光粉在发光二极管、激光器、放大器和传感器等领域扮演了不可替代的角色。
稀土掺杂材料的发光主要属于稀土元素中电子的f-f和f-d跃迁。当前关于稀土发光材料的研究仍主要集中于发光效率的提升。常见的几种关于增强材料发光性质的方法为：改善制备工艺、优化工艺参数，包括掺杂浓度、反应时间等；选择低声子能量的晶体或玻璃作为基质；提高共掺稀土离子之间能量传递的效率；通过包覆等手段实现核壳结构的形成。近年来，在薄膜的表面加上贵金属元素（Au, Ag）技术设计已证明可提高稀土掺杂薄膜的发光效率。本发明特色是在纳米荧光粉中掺入Cu纳米颗粒，不仅可以显著改善稀土掺杂纳米荧光粉的发光效率，而且相对于贵金属Au、Ag而言，成本更低。即一种新的金属-稀土复合型材料被设计、制备和表征，并进行了系统的光致发光特性分析，证明该材料具有优异的下转换光致发光性能，可作为高效的荧光粉材料进行生产和应用。
发明内容
本发明是为了改善荧光粉的发光性能，提出一种在硅酸锶钙基质中掺杂三价铽离子的基础上加入了铜纳米颗粒具有优秀光致发光特性的金属--稀土纳米荧光粉。
本发明的方案是：一种铜铽共掺的CaSrSiO4纳米荧光粉末，其特征在于：所述的纳米荧光粉末由CaSrSiO4、Tb3+和Cu纳米颗粒经高温固相烧结法制备而成，且CaSrSiO4：0.7mol%Tb3+，xmol%Cu，其中x的取值范围是0.1至0.5。
本发明具有如下优点：本发明所公开的纳米荧光粉末，利用金属的局域表面等离子体共振效应，将稀土掺杂发光材料的发光效率进一步改善；具体表现在它通过铜纳米颗粒的加入及一系列工艺优化，让纳米荧光粉末的荧光性能得到大大提升。
附图说明
图1是是采用日本XRD-6000型X射线衍射仪测量的系列铽、铜单掺和共掺CaSrSiO4纳米荧光粉的XRD图谱，测量范围为2θ=10°-80°。与标准卡对比，可以看铽、铜的掺入并未明显改变CaSrSiO4基质的晶体结构，纳米荧光粉依然为纯相，无杂相产生。
图2是采用日立公司的SU8000扫描电子显微镜所测量的系列铽单掺和铜铽共掺CaSrSiO4纳米荧光粉的SEM图像，a-d图依次为0.7Tb3+，0.7Tb3+0.1Cu，0.7Tb3+0.3Cu和0.7Tb3 +0.5Cu（浓度单位均为mol%）。
图3是采用日立公司F-4600型荧光分光光度计测量的铜铽共掺CaSrSiO4纳米荧光粉随掺铜浓度的变化光致发光谱，并绘制出浓度折线图。可以发现优化的掺铜浓度为0.3mol%。可以看出，随掺铜颗粒浓度的增加，颗粒尺寸逐渐变大，分别为60-60-130-150 nm。
图4是同样采用日立公司F-4600型荧光分光光度计测量的铜铽共掺CaSrSiO4纳米荧光粉随掺铜浓度变化而引起的寿命变化。
具体实施方式
下面将结合附图说明本发明的具体实施方式，如图1至图4所示：采用高温固相烧结法制备了系列铜铽共掺的CaSrSiO4纳米荧光粉：CaSrSiO4:0.7mol%Tb3+, xmol%Cu (x=0.1~0.5)。
通过XRD和SEM确定了样品的晶体结构和表面形貌，并优化了制备工艺和参数。详细分析了系列铜铽共掺CaSrSiO4纳米荧光粉的光致发光特性，在245 nm紫外光激发下，可以获得强的紫外（381 nm）、蓝（415，437 nm）、绿（545 nm）、橙（585 nm）和红（624 nm）光发射，其中545 nm绿光最强。同时发现，相对于未掺杂铜纳米颗粒的CaSrSiO4:Tb3+纳米荧光粉，加入了铜纳米颗粒后，CaSrSiO4:Tb3+荧光粉发光强度随掺铜浓度增大而增强，最高可增强一倍。优化的掺铜浓度为0.3 mol%，随后继续铜掺杂量会发生浓度淬灭，发光强度减弱。这表明可以通过改变铜纳米颗粒的掺入量，对CaSrSiO4: Tb3+纳米荧光粉的发光性能起到调控作用。
Claims (1)
1.一种铜铽共掺的CaSrSiO4纳米荧光粉末，其特征在于：所述的纳米荧光粉末由CaSrSiO4、Tb3+和Cu纳米颗粒经高温固相烧结法制备而成，且CaSrSiO4：0.7mol%Tb3+，xmol%Cu，其中x的取值范围是0.1至0.5。
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| CN107557012A (zh) * | 2017-09-19 | 2018-01-09 | 贵州师范大学 | 一种制备金属离子共掺杂磷酸钇发光材料的方法 |
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| R3+:CaF2(R=Yb、Er、Tm、Ce)粉末发光特性及温度和激光退火对Tb3+:CaSrSiO4发光的影响;徐奇;《学位论文全文》;20170301;第1-50页 * |
| Soluble silica assisted synthesis and luminescent characteristics of yellow emitting CaSrSiO4:Eu2+ phosphors for warm white light production;Hyun-Joo Woo et al.;《Ceramics International》;20141231;第41卷;第1-22页 * |
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