无汞荧光灯用荧光材料的制备及发光性能研究
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摘要
无汞荧光灯由于具有绿色环保、启动快等特点成为显示照明领域的研究热点。Y203:Eu3+以其优异的性能得到了广泛应用,但是由于其中高价位稀土元素的大量使用导致了其高成本的缺点,如何降低Y203:Eu3+真空紫外红色荧光粉的成本成为亟待解决的问题。真空紫外BaMgAl10O17:Eu2+,Mn2+蓝色发光材料表现出比BaMgAl10O17:Eu2+更好的色饱和度,但是其劣化机理还不清楚。另外,研究和开发新型真空紫外用荧光材料是无汞荧光灯研究的一个重要方面。本论文针对降低商用红色荧光粉Y2O3:Eu3+的生产成本、BaMgAl10O17:Eu2+,Mn2+蓝色发光材料的劣化问题和新型K3Gd(PO4)2基质真空紫外发光材料的开发,通过对Y2O3:Eu3+进行Ca2+离子共掺杂,制备Y2O3:Eu3+包覆Y2O3荧光粉等途径进行降低Y2O3:Eu3+生产成本的尝试,研究BaMgAl10O17:Eu2+,Mn2+蓝色发光材料在热处理、紫外辐照及真空紫外辐照下的劣化机理,并开发了新型的K3Gd(PO4)2:0.8Tb3+高亮度真空紫外用绿色发光材料。主要结果有：
1、使用燃烧法制备了Ca2+掺杂的Y2O3:Eu3+荧光粉,尿素的最佳加入量为理论计算量的100%,热处理温度为1400℃,Ca2+最佳掺杂浓度为0.6mol%。在254nm激发下,Y1.94-xCaxEu0.06O3(?)的发光强度随Ca2+掺杂浓度的增大而增大,这与Ca2+掺入后增强了对254nm激发光的吸收有关。在147nm激发下,Y1.94-xCaxEu0.06O3的发光强度随Ca2+掺杂浓度的增大而增大。
2、使用尿素辅助均匀沉淀法制备了Y2O3:Eu3+包覆的Y203颗粒,最佳反应条件为：(Y,Eu)(NO3)3浓度0.02mol/L,反应时间3小时。在254nm激发下,Y203:Eu3+包覆的Y203颗粒的发光强度是使用相同方法制备得到的Y203:Eu3+的86%,在147nm激发下,Y203:Eu3+包覆的Y203颗粒的发光强度是使用相同方法制备得到的Y203:Eu3+(?)的88%。
3、通过对比热处理、紫外辐照处理、真空紫外辐照处理前后的BaMgAl10O17: Eu2+,Mn2+紫外和真空紫外区的激发、发射光谱及发光强度的变化、Eu2+和Mn2+稳定性的变化、吸收光谱以热释曲线的变化,说明BAM:Eu2+,Mn2+热劣化的主要原因是Eu2+离子的氧化和迁移,紫外辐照劣化主要来源于Eu2+离子的亚稳态；真空紫外辐照劣化由Eu2+的迁移引起。紫外辐照处理后BAM:Eu2+,Mn2+在真空紫外激发下的光衰在一定程度上与陷阱对基质到激活剂之间能量传递的阻碍有关。BAM:Eu2+,Mn2+中Mn2+在热处理、紫外辐照处理和真空紫外辐照处理后没有发生变化,与BAM的劣化无关
4、使用固相方法合成了K3Gd1-x(PO4)2:Eux3+(0(?)x(?)1)和K3Gd1-x(PO4)2:Tbx3+(0≤y≤1)紫外激发和发射光谱测试结果说明,在K3Gd(PO4)2基质中由于最近邻Gd3+之间的距离相对较大,激发能不能在激活剂离子之间传递。在147nm激发下,当Eu或Tb的浓度为0.8mol时发光强度最高。浓度猝灭主要受K3Gd(PO4)2基质和P-O四面体中被激发电子数的影响。在147nm激发下,K3Gd0.2(PO4)2:0.8Tb3+的发光强度达到了商用荧光粉Zn1.96SiO4:0.04Mn2+的204%,色坐标为(0.340,0.561),衰减时间为5.09ms,说明K3Gd0.2(PO4)2:0.8Tb3+是一种有潜力的无汞荧光灯用绿色真空紫外荧光粉。
Mercury-free fluorescent lamp has been a research focus in lighting and display fields due to its characteristics of environment protection, quickly starting, and so on. Y2O3:Eu3+phosphor has been widely applied because of its excellent properties. But its cost is high because there is a mout of high price rare earth elements in it. So how to reduce the cost of vacuum ultra-violet (VUV) red phosphor Y2O3:Eu3+is an urgent problem to be solved. VUV blue phosphor BaMgAl10O17:Eu2+Mn2+has better color saturation than BaMgAl10O17:Eu2+phosphor, but the degradation mechanism of this phosphor has not been clearly clarified. Additionally, it is an important study field for mercury-free fluorescent lamp to research and develop new VUV phosphors. In this dissertation, the following aspects are chosen as researching objects: reducing the production cost of commercial red phosphor Y2O3:Eu3+, the degradation mechanism of BaMgAl10O17:Eu2+, Mn2+blue phosphor, and the development of new K3Gd(PO4)2based phosphors. Ca2+co-doping and Y2O3:Eu3+coated Y2O3phosphor are selected to reduce the production cost of Y2O3:Eu3+phosphor. The degradation mechanism of BaMgAl10O17:Eu2+, Mn2+under thermal treatment, UV radation and VUV radation is studied. The new K3Gd0.2(PO4)2:0.8Tb3+VUV green phosphor with high luminance is developed. The main results are listed below:
1. The Ca2+co-doped Y2O3:Eu3+phosphors are prepared by solution combustion method. The optimized amout of urea, temperature of thermal treatment, and the concentration of Ca2+are100%of theoretical amount,1400°C, and6mol%, respectively. Under254nm excitation, the intensity of Y1.94-xCaxEu0.06O3increases with the concentration of Ca2+, which is caused by the strengthening of adsorption of254nm by co-doping of Ca2+. Under147nm excitation, the intensity of Y1.94-xCaxEu0.06O3also increases with the concentration of Ca2+
2、The Y2O3:Eu3+coated Y2O3particles are prepared by urea assisted homogeneous precipitation. The optimized concentration of (Y, Eu)(NO3)3and reacting time are0.02mol/L and3hours respectively. Under254mm excitation, the intensity of Y2O3:Eu3+coated Y2O3particles equals86%of the intensity of Y2O3sampie prepared under same condition. Under147mm excitation, the intensity of Y2O3:Eu3+coated Y2O3particles equals88%of the intensity of Y2O3sample prepared under same condition.
3.The emission and excitation spectra under UV and VUV excitation, the stability of Eu3+and Mn2+. adsorption spectra and thermoluminesccnce of BaMgAl10O17:Eu2+,Mn2+before and alter thermal treatment, UV radiation and VUV radiation are investigated comparatively. The results indicate that the oxidation and migration of Eu2+are primarily responsible for the thermal degradation of BAM:Eu2+,Mn2+. The UV radiation degradation of samples are primarily involved in the metaslable state of Eu2+The migration of Eu2+resulted in VUV radiation degradation. The serious VUV luminous loss of samples after UV radiation can be partly linked to the interruption of energy transfer from host to activator by traps. The Mn2+in BAM:Eu2+,Mn2+did not alter during the thermal, UV and VUV radiation treatments and is not related to the degradations.
4.The K3Gd1-x(PO4)2:Eux3+(0≤x≤1) and K3Gd1-y(PO4)2:Tby3+(0≤y≤1) are prepared by solid stale reaction. The obtained UV excitation and emission spectra indicate that the excitation energy can not be migrated among the activator ions in the K3Gd(PO4)2matrix because of a relatively large distance between the nearest Gd3+neighbors. The strongest emission intensity under147nm excitation is obtained when Eu or Tb concentration is0.8mol. The concentration quenching is affected mainly by the K3Gd(PO4)2host and the number of excited electrons of P-O tetrahedrons. Under147nm excitation, the integrate emission intensity of K3Gd0.2(PO4)2:0.8Tb3+is about204%of commercial phosphor Zn1.96SiO4:0.04Mn2+the chromaticity coordinates of K3Gd0.2(PO4)2:0.8Tb3+is around (0.340,0.561), the decay time of K3Gd0.2(PO4)2:0.8Tb3+is about5.09ms. K3Gd0.2(PO4)2:0.8Tb3+is a potential VUV green phosphor for the mercury-free fluorescent lamps.
1、使用燃烧法制备了Ca2+掺杂的Y2O3:Eu3+荧光粉,尿素的最佳加入量为理论计算量的100%,热处理温度为1400℃,Ca2+最佳掺杂浓度为0.6mol%。在254nm激发下,Y1.94-xCaxEu0.06O3(?)的发光强度随Ca2+掺杂浓度的增大而增大,这与Ca2+掺入后增强了对254nm激发光的吸收有关。在147nm激发下,Y1.94-xCaxEu0.06O3的发光强度随Ca2+掺杂浓度的增大而增大。
2、使用尿素辅助均匀沉淀法制备了Y2O3:Eu3+包覆的Y203颗粒,最佳反应条件为：(Y,Eu)(NO3)3浓度0.02mol/L,反应时间3小时。在254nm激发下,Y203:Eu3+包覆的Y203颗粒的发光强度是使用相同方法制备得到的Y203:Eu3+的86%,在147nm激发下,Y203:Eu3+包覆的Y203颗粒的发光强度是使用相同方法制备得到的Y203:Eu3+(?)的88%。
3、通过对比热处理、紫外辐照处理、真空紫外辐照处理前后的BaMgAl10O17: Eu2+,Mn2+紫外和真空紫外区的激发、发射光谱及发光强度的变化、Eu2+和Mn2+稳定性的变化、吸收光谱以热释曲线的变化,说明BAM:Eu2+,Mn2+热劣化的主要原因是Eu2+离子的氧化和迁移,紫外辐照劣化主要来源于Eu2+离子的亚稳态；真空紫外辐照劣化由Eu2+的迁移引起。紫外辐照处理后BAM:Eu2+,Mn2+在真空紫外激发下的光衰在一定程度上与陷阱对基质到激活剂之间能量传递的阻碍有关。BAM:Eu2+,Mn2+中Mn2+在热处理、紫外辐照处理和真空紫外辐照处理后没有发生变化,与BAM的劣化无关
4、使用固相方法合成了K3Gd1-x(PO4)2:Eux3+(0(?)x(?)1)和K3Gd1-x(PO4)2:Tbx3+(0≤y≤1)紫外激发和发射光谱测试结果说明,在K3Gd(PO4)2基质中由于最近邻Gd3+之间的距离相对较大,激发能不能在激活剂离子之间传递。在147nm激发下,当Eu或Tb的浓度为0.8mol时发光强度最高。浓度猝灭主要受K3Gd(PO4)2基质和P-O四面体中被激发电子数的影响。在147nm激发下,K3Gd0.2(PO4)2:0.8Tb3+的发光强度达到了商用荧光粉Zn1.96SiO4:0.04Mn2+的204%,色坐标为(0.340,0.561),衰减时间为5.09ms,说明K3Gd0.2(PO4)2:0.8Tb3+是一种有潜力的无汞荧光灯用绿色真空紫外荧光粉。
Mercury-free fluorescent lamp has been a research focus in lighting and display fields due to its characteristics of environment protection, quickly starting, and so on. Y2O3:Eu3+phosphor has been widely applied because of its excellent properties. But its cost is high because there is a mout of high price rare earth elements in it. So how to reduce the cost of vacuum ultra-violet (VUV) red phosphor Y2O3:Eu3+is an urgent problem to be solved. VUV blue phosphor BaMgAl10O17:Eu2+Mn2+has better color saturation than BaMgAl10O17:Eu2+phosphor, but the degradation mechanism of this phosphor has not been clearly clarified. Additionally, it is an important study field for mercury-free fluorescent lamp to research and develop new VUV phosphors. In this dissertation, the following aspects are chosen as researching objects: reducing the production cost of commercial red phosphor Y2O3:Eu3+, the degradation mechanism of BaMgAl10O17:Eu2+, Mn2+blue phosphor, and the development of new K3Gd(PO4)2based phosphors. Ca2+co-doping and Y2O3:Eu3+coated Y2O3phosphor are selected to reduce the production cost of Y2O3:Eu3+phosphor. The degradation mechanism of BaMgAl10O17:Eu2+, Mn2+under thermal treatment, UV radation and VUV radation is studied. The new K3Gd0.2(PO4)2:0.8Tb3+VUV green phosphor with high luminance is developed. The main results are listed below:
1. The Ca2+co-doped Y2O3:Eu3+phosphors are prepared by solution combustion method. The optimized amout of urea, temperature of thermal treatment, and the concentration of Ca2+are100%of theoretical amount,1400°C, and6mol%, respectively. Under254nm excitation, the intensity of Y1.94-xCaxEu0.06O3increases with the concentration of Ca2+, which is caused by the strengthening of adsorption of254nm by co-doping of Ca2+. Under147nm excitation, the intensity of Y1.94-xCaxEu0.06O3also increases with the concentration of Ca2+
2、The Y2O3:Eu3+coated Y2O3particles are prepared by urea assisted homogeneous precipitation. The optimized concentration of (Y, Eu)(NO3)3and reacting time are0.02mol/L and3hours respectively. Under254mm excitation, the intensity of Y2O3:Eu3+coated Y2O3particles equals86%of the intensity of Y2O3sampie prepared under same condition. Under147mm excitation, the intensity of Y2O3:Eu3+coated Y2O3particles equals88%of the intensity of Y2O3sample prepared under same condition.
3.The emission and excitation spectra under UV and VUV excitation, the stability of Eu3+and Mn2+. adsorption spectra and thermoluminesccnce of BaMgAl10O17:Eu2+,Mn2+before and alter thermal treatment, UV radiation and VUV radiation are investigated comparatively. The results indicate that the oxidation and migration of Eu2+are primarily responsible for the thermal degradation of BAM:Eu2+,Mn2+. The UV radiation degradation of samples are primarily involved in the metaslable state of Eu2+The migration of Eu2+resulted in VUV radiation degradation. The serious VUV luminous loss of samples after UV radiation can be partly linked to the interruption of energy transfer from host to activator by traps. The Mn2+in BAM:Eu2+,Mn2+did not alter during the thermal, UV and VUV radiation treatments and is not related to the degradations.
4.The K3Gd1-x(PO4)2:Eux3+(0≤x≤1) and K3Gd1-y(PO4)2:Tby3+(0≤y≤1) are prepared by solid stale reaction. The obtained UV excitation and emission spectra indicate that the excitation energy can not be migrated among the activator ions in the K3Gd(PO4)2matrix because of a relatively large distance between the nearest Gd3+neighbors. The strongest emission intensity under147nm excitation is obtained when Eu or Tb concentration is0.8mol. The concentration quenching is affected mainly by the K3Gd(PO4)2host and the number of excited electrons of P-O tetrahedrons. Under147nm excitation, the integrate emission intensity of K3Gd0.2(PO4)2:0.8Tb3+is about204%of commercial phosphor Zn1.96SiO4:0.04Mn2+the chromaticity coordinates of K3Gd0.2(PO4)2:0.8Tb3+is around (0.340,0.561), the decay time of K3Gd0.2(PO4)2:0.8Tb3+is about5.09ms. K3Gd0.2(PO4)2:0.8Tb3+is a potential VUV green phosphor for the mercury-free fluorescent lamps.
引文
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