近紫外光LED转换白光用红色荧光粉的制备、发光性质研究及应用
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摘要
本文以近紫外光激发红色荧光粉为研究对象，利用高温固相反应方法制备了发射波长位于616nm的LiEuMo_(2-x)Si_xO_8和Li_(1-3x)Tb_xEuMo_2O_8，发射波长位于591nmY_2Ti_2O_7:Eu~(3+)，和发射主峰位于620nm的Ba_3MgSi_2O_8: Eu~(2+), Tb~(3+), Mn~(2+)等多种高性能红色荧光粉，详细研究了基质晶格修饰、能量传递体系设计、电荷补偿、和助熔剂选择等对荧光粉发光性能的影响。在此基础上结合蓝、绿色荧光粉研制高显色性白光LED器件。具体研究内容如下：
对白钨矿结构的LiEuMo_2O_8荧光粉进行基质晶格修饰以改善红光发射性能。研究表明Si~(4+)替代部分Mo~(4+)可提高荧光粉在近紫外光395nm激发下的红光发射强度（616nm，5D0→7F2跃迁），在x=0.2时亮度最高，达到LiEuMo_2O_8亮度的1.3倍。激发和吸收光谱分析表明Si掺杂导致基质的电荷迁移吸收带边从420nm蓝移到360nm，减少了基质对紫外光区（360-420nm）的吸收，增强了Eu~(3+)在近紫外光激发下的激发和发射几率。用Tb~(3+)替代部分Li+制备Li_(1-3x)Tb_xEuMo_2O_8红色荧光粉。研究表明，微量的Tb~(3+)共激活剂的引入可显著增强荧光粉在近紫外激发下的红光发射强度；在x=0.04时，样品的红光发射提高了1.4倍。激发光谱和瞬态光谱测试表明Tb~(3+)和Eu~(3+)之间存在Tb~(3+)→Eu~(3+)的能量传递关系，可增强Eu~(3+)在近紫外光激发下的激发和发射几率。
利用高温固相反应方法制备了烧绿石结构的Y_(2-x)Ti_2O_7:xEu~(3+)新型荧光粉。研究表明，在近紫外光激发下荧光粉发出主峰位于591nm (5D0→7F1跃迁的)橙红色光，随Eu~(3+)浓度的提高616nm（5D0→7F2跃迁）贡献逐渐增大，在x=0.45橙红光发射强度达到最大。变温发光研究表明，Y1.55Ti2O7:0.45Eu~(3+)橙红色荧光粉发光猝灭温度（T50%）高达376摄氏度，显示出在高温发光材料领域的应用潜力。用H3BO3，NH4Cl，NaCl，NH4F，NaF，LiF等助熔剂优化Y_(2-x)Ti_2O_7:xEu~(3+)荧光粉的制备。研究表明NaF助熔剂效果最佳，能提高橙红光发射强度16倍以上。综合SEM、EDAX Mapping和微区阴极射线发光等分析表明NaF助熔剂存在下能形成类球形的、激活剂分布均匀的荧光粉颗粒，这与其制备温度相近的熔点和F-对晶体生长过程的影响相关。
利用微区阴极射线发光和EDAX Mapping详细表征Ba_3MgSi_2O_8:Eu~(2+), Mn~(2+)荧光粉的发光性质。研究表明，近紫外光激发下荧光粉本征发光位于620nm（Mn~(2+)：4T→6A1）和440nm（Eu~(2+)：5d→4f），但伴有疑似Ba_2SiO_4: Eu~(2+)杂相的505nm强绿光发射。在高温固相反应体系中加入Tb~(3+)制备Ba_3MgSi_2O_8: Eu~(2+), Tb~(3+), Mn~(2+)荧光粉。XRD和荧光显微分析表明，Tb~(3+)掺杂能抑制杂相生成，显著降低源于杂相的505nm绿光发射，这与Tb~(3+)在高温固相反应中起到电荷补偿剂作用有关。发光和激发光谱分析表明，掺杂Tb~(3+)能提高Mn~(2+)位于620nm红光发射强度；当x=0.1mol时，红光发射强度达到最大，色坐标为（0.52,0.31）。这与Eu~(2+)→Tb~(3+)→Mn~(2+)间形成有效的能量传递体系有关。
In this dissertation, we mainly focus on the red-emitting phosphos under excitation at nearultraviolet, and prepared various red-emitting phosphor with different emitting wavelength,e.g., LiEuMo_(2-x)Si_xO_8and Li_(1-3x)Tb_xEuMo_2O_8phosphor with strongest emitting wavelength at616nm, Y_2Ti_2O_7:Eu~(3+)phosphor with strongest emission wavelength at591nm, Ba_3MgSi_2O_8:Eu~(2+), Tb~(3+), Mn~(2+)phosphor with strongest emission620nm, and study in detail the influenceof modification of host crystal lattice, energy transfer design, charge compensation andchoose method of flux on photoluminescence properties of phosphor. Based on the abovework, we prepared high color rendering index (CRI) white lighting emitting diodes (WLEDs)device combination near ultraviolet LED chips () with green-emitting phosphors(Ba,Sr)2SiO4:Eu~(2+)and (Sr,Mg)4Si3O8Cl:Eu~(2+)blue-emitting, The main contents as follow:
For LiEuMo_2O_8phosphor with scheelite structure, we focus on modiy host crystal latticefor enhancement the red-emitting intensity. Results indicated that Si partly replace the Mo,red-emitting intensity can be improved1.3times at x=0.2. Excitation and absorpbtion spectraindicated that Si-doped result in the charge transfer band from420nm blue shift to360nm，reduce the absorbtion of host in near ultraviolet (360-420nm), increase the probablility ofexcitation and emission of phosphor. Tb~(3+)partly substitude for Li, results indicated thatintroduction of Tb~(3+)can significatntly improve the red-emitting intensiy under excitation atnerar ultraviolet, the luminous intensity can be increase1.4times at x=0.04. Excitation andlifetime spectra suggest that energy transfer from Tb~(3+)to Eu~(3+)can enhance the probability ofexcitation and emission.
Novel pyrochlore Y1.55Ti2O7:0.45Eu~(3+)orange-red emission phosphor has been synthesizedby high-temperature solid-state reaction. The results suggest that this phosphor showorange-red emitting at591nm (5D0→7F1) under NUV excitation. Luminous intensity ofred-emitting at616nm increases with increasing content of Eu-doped, and reach the maxmum.This orange–red phosphor Y1.55Ti2O7:0.45Eu~(3+)shows high thermal quenching temperature(T50%) even up to376°C, and be consider as a promising luminescence thermometry at hightemperature. In addition, we chose H3BO3，NH4Cl，NaCl，NH4F，NaF，LiF as flux tooptimize the condition of Y_(2-x)Ti_2O_7:xEu~(3+)phosphor. Experimental results show that NaF isthe best one among the five flux materials, can significantly improve the luminous intensityover16times. According to SEM, EDAX Mapping and CL spectra analysis result indicatedthat NaF flux can modify the paricle morphology and homogenize activator distribution,which is acctributed to the melting point of NaF much more approach to the synthesis temperature of Y_(2-x)Ti_2O_7:xEu~(3+)phosphor.
According to CL, EDAX Mapping, XRD analysis result of Ba_3MgSi_2O_8:Eu~(2+), Mn~(2+)phosphor indicated that green-emitting peak at505nm is ascribed to byproducts Ba_2SiO_4rather than Ba_3MgSi_2O_8:Eu~(2+), Mn~(2+)phosphor.Tb-doped can inhibit the formation ofbyproducts Ba_2SiO_4. Photoluminescence and flurescence microscope results suggest thatTb-dped not only reduce green-emitting intensity from byproducts but also can significantlyimprove the red-emitting intensity of phosphor, and luminous intensity reach maxmum at x=0.1. As a charge compensator, Tb~(3+)-doped can help the formation of a single phaseBa_3MgSi_2O_8, and improve the efficiency of energy transfer from Eu~(2+)-Mn~(2+). Enhanced redemission of Ba_3MgSi_2O_8:Eu~(2+), Tb~(3+)，Mn~(2+)was discussed in terms of Eu~(2+)→Tb~(3+)→Mn~(2+)energy transfer.
对白钨矿结构的LiEuMo_2O_8荧光粉进行基质晶格修饰以改善红光发射性能。研究表明Si~(4+)替代部分Mo~(4+)可提高荧光粉在近紫外光395nm激发下的红光发射强度（616nm，5D0→7F2跃迁），在x=0.2时亮度最高，达到LiEuMo_2O_8亮度的1.3倍。激发和吸收光谱分析表明Si掺杂导致基质的电荷迁移吸收带边从420nm蓝移到360nm，减少了基质对紫外光区（360-420nm）的吸收，增强了Eu~(3+)在近紫外光激发下的激发和发射几率。用Tb~(3+)替代部分Li+制备Li_(1-3x)Tb_xEuMo_2O_8红色荧光粉。研究表明，微量的Tb~(3+)共激活剂的引入可显著增强荧光粉在近紫外激发下的红光发射强度；在x=0.04时，样品的红光发射提高了1.4倍。激发光谱和瞬态光谱测试表明Tb~(3+)和Eu~(3+)之间存在Tb~(3+)→Eu~(3+)的能量传递关系，可增强Eu~(3+)在近紫外光激发下的激发和发射几率。
利用高温固相反应方法制备了烧绿石结构的Y_(2-x)Ti_2O_7:xEu~(3+)新型荧光粉。研究表明，在近紫外光激发下荧光粉发出主峰位于591nm (5D0→7F1跃迁的)橙红色光，随Eu~(3+)浓度的提高616nm（5D0→7F2跃迁）贡献逐渐增大，在x=0.45橙红光发射强度达到最大。变温发光研究表明，Y1.55Ti2O7:0.45Eu~(3+)橙红色荧光粉发光猝灭温度（T50%）高达376摄氏度，显示出在高温发光材料领域的应用潜力。用H3BO3，NH4Cl，NaCl，NH4F，NaF，LiF等助熔剂优化Y_(2-x)Ti_2O_7:xEu~(3+)荧光粉的制备。研究表明NaF助熔剂效果最佳，能提高橙红光发射强度16倍以上。综合SEM、EDAX Mapping和微区阴极射线发光等分析表明NaF助熔剂存在下能形成类球形的、激活剂分布均匀的荧光粉颗粒，这与其制备温度相近的熔点和F-对晶体生长过程的影响相关。
利用微区阴极射线发光和EDAX Mapping详细表征Ba_3MgSi_2O_8:Eu~(2+), Mn~(2+)荧光粉的发光性质。研究表明，近紫外光激发下荧光粉本征发光位于620nm（Mn~(2+)：4T→6A1）和440nm（Eu~(2+)：5d→4f），但伴有疑似Ba_2SiO_4: Eu~(2+)杂相的505nm强绿光发射。在高温固相反应体系中加入Tb~(3+)制备Ba_3MgSi_2O_8: Eu~(2+), Tb~(3+), Mn~(2+)荧光粉。XRD和荧光显微分析表明，Tb~(3+)掺杂能抑制杂相生成，显著降低源于杂相的505nm绿光发射，这与Tb~(3+)在高温固相反应中起到电荷补偿剂作用有关。发光和激发光谱分析表明，掺杂Tb~(3+)能提高Mn~(2+)位于620nm红光发射强度；当x=0.1mol时，红光发射强度达到最大，色坐标为（0.52,0.31）。这与Eu~(2+)→Tb~(3+)→Mn~(2+)间形成有效的能量传递体系有关。
In this dissertation, we mainly focus on the red-emitting phosphos under excitation at nearultraviolet, and prepared various red-emitting phosphor with different emitting wavelength,e.g., LiEuMo_(2-x)Si_xO_8and Li_(1-3x)Tb_xEuMo_2O_8phosphor with strongest emitting wavelength at616nm, Y_2Ti_2O_7:Eu~(3+)phosphor with strongest emission wavelength at591nm, Ba_3MgSi_2O_8:Eu~(2+), Tb~(3+), Mn~(2+)phosphor with strongest emission620nm, and study in detail the influenceof modification of host crystal lattice, energy transfer design, charge compensation andchoose method of flux on photoluminescence properties of phosphor. Based on the abovework, we prepared high color rendering index (CRI) white lighting emitting diodes (WLEDs)device combination near ultraviolet LED chips () with green-emitting phosphors(Ba,Sr)2SiO4:Eu~(2+)and (Sr,Mg)4Si3O8Cl:Eu~(2+)blue-emitting, The main contents as follow:
For LiEuMo_2O_8phosphor with scheelite structure, we focus on modiy host crystal latticefor enhancement the red-emitting intensity. Results indicated that Si partly replace the Mo,red-emitting intensity can be improved1.3times at x=0.2. Excitation and absorpbtion spectraindicated that Si-doped result in the charge transfer band from420nm blue shift to360nm，reduce the absorbtion of host in near ultraviolet (360-420nm), increase the probablility ofexcitation and emission of phosphor. Tb~(3+)partly substitude for Li, results indicated thatintroduction of Tb~(3+)can significatntly improve the red-emitting intensiy under excitation atnerar ultraviolet, the luminous intensity can be increase1.4times at x=0.04. Excitation andlifetime spectra suggest that energy transfer from Tb~(3+)to Eu~(3+)can enhance the probability ofexcitation and emission.
Novel pyrochlore Y1.55Ti2O7:0.45Eu~(3+)orange-red emission phosphor has been synthesizedby high-temperature solid-state reaction. The results suggest that this phosphor showorange-red emitting at591nm (5D0→7F1) under NUV excitation. Luminous intensity ofred-emitting at616nm increases with increasing content of Eu-doped, and reach the maxmum.This orange–red phosphor Y1.55Ti2O7:0.45Eu~(3+)shows high thermal quenching temperature(T50%) even up to376°C, and be consider as a promising luminescence thermometry at hightemperature. In addition, we chose H3BO3，NH4Cl，NaCl，NH4F，NaF，LiF as flux tooptimize the condition of Y_(2-x)Ti_2O_7:xEu~(3+)phosphor. Experimental results show that NaF isthe best one among the five flux materials, can significantly improve the luminous intensityover16times. According to SEM, EDAX Mapping and CL spectra analysis result indicatedthat NaF flux can modify the paricle morphology and homogenize activator distribution,which is acctributed to the melting point of NaF much more approach to the synthesis temperature of Y_(2-x)Ti_2O_7:xEu~(3+)phosphor.
According to CL, EDAX Mapping, XRD analysis result of Ba_3MgSi_2O_8:Eu~(2+), Mn~(2+)phosphor indicated that green-emitting peak at505nm is ascribed to byproducts Ba_2SiO_4rather than Ba_3MgSi_2O_8:Eu~(2+), Mn~(2+)phosphor.Tb-doped can inhibit the formation ofbyproducts Ba_2SiO_4. Photoluminescence and flurescence microscope results suggest thatTb-dped not only reduce green-emitting intensity from byproducts but also can significantlyimprove the red-emitting intensity of phosphor, and luminous intensity reach maxmum at x=0.1. As a charge compensator, Tb~(3+)-doped can help the formation of a single phaseBa_3MgSi_2O_8, and improve the efficiency of energy transfer from Eu~(2+)-Mn~(2+). Enhanced redemission of Ba_3MgSi_2O_8:Eu~(2+), Tb~(3+)，Mn~(2+)was discussed in terms of Eu~(2+)→Tb~(3+)→Mn~(2+)energy transfer.
引文
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