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非水性sol-gel法Er~(3+)+Y~(3+)共掺杂Al/_2O/_3的制备及其发光特性研究
Preparation and Photoluminescence of the Er~/(3+/)+Y~/(3+/) Doped Al/_2O/_3 Derived from the Non-aqueous Sol-gel Method

导  师: 雷明凯

学科专业: 080503

授予学位: 硕士

作  者: ;

机构地区: 大连理工大学

摘  要: 采用非水性sol-gel法制备Er~/(3+/)-Y~/(3+/)共掺杂Al/_2O/_3粉末,选取0.1和1mol/%两种Er~/(3+/)掺杂浓度,系统地研究了Y~/(3+/)、Er~/(3+/)浓度比例范围为/(1-10/)∶1的Y~/(3+/)共掺杂对900和1000℃烧结的掺Er~/(3+1/)∶Al/_2O/_3结构及其光致发光/(PL/)特性的影响。 900和1000℃烧结的掺0.1和1mol/%Er~/(3+/)∶Al/_2O/_3粉末,其相结构均为具有非晶化特征的γ和θ相混合结构。其中,掺0.1mol/%Er~/(3+/)粉末,随0.1-1mol/%Y~/(3+/)浓度增加其γ和θ相非晶化趋势更加显著。900和1000℃烧结的掺1.mol/%Er~/(3+/)浓度粉末,其γ和θ相结构的非晶化趋势分别随1-10和1-5mol/%Y~/(3+/)的共掺杂浓度增加而更加严重;1000℃烧结时,10mol/%Y~/(3+/)共掺杂粉末γ相消失,具有立方结构的/(Er,Y/)/_3Al/_5O/_/(12/)化合物析出。傅立叶变换红外光谱/(FTIR/)测量表明,相同温度烧结的不同比例Y~/(3+/)共掺杂的掺Er~/(3+/)∶Al/_2O/_3粉末中,O-H基团特征吸收峰波段范围/(4000-2500cm~/(-1/)/)和吸收峰强度均无明显差异,说明Y~/(3+/)共掺杂对其振动频率和含量无明显影响。 980nm激光泵浦下,掺Er~/(3+/)∶Al/_2O/_3粉末具有峰值波长在1.53μm、660nm/(红光/)和545、523nm/(绿光/)附近的PL特性,其中前者为斯托克斯/(Stokes/)发光,后者红光和绿光为上转换发光。Y~/(3+/)掺杂对其PL强度具有明显影响。一方面Y~/(3+/)共掺杂降低了掺Er~/(3+/)∶Al/_2O/_3粉末基体的声子能量,导致Er~/(3+4/)I/_/(11//2/)能级寿命增加,其Stokes发光和红光强度下降,绿光强度提高,红、绿光强度比随之降低:另一方面Y~/(3+/)共掺杂可有效提高Er~/(3+/)的分散度,减小Er~/(3+/)光致发光的浓度猝灭效应,提高掺杂Er~/(3+/)∶Al/_2O/_3粉末的PL强度。掺Er~/(3+/)浓度为0.1mol/%时,因其浓度猝灭效应较小,Y~/(3+/)共掺杂主要体现降低声子能量这一效应,其PL强度随Y~/(3+/)共掺杂发生相应变化;掺Er~/(3+/)浓度为1mol/%时,Y~/(3+/)共掺杂既降低了基体声子能量,又减小了Er~/(3+/)浓度猝灭,使得900和1000℃烧结粉末的Stokes发光和上转换发光强度均随1-10mol/%Y/(3+/)共掺杂浓度的增加而增大,同时红、绿光强度比随Y~/(3+/)浓度增加而降低。Y~/(3+/)共掺杂对掺Er~/(3+/)∶Al/_2O/_3粉末Stokes光谱半高宽/(FWHM/)亦有影响。掺Er~/(3+/)浓度为0.1mol/%时,900℃烧结粉末Stokes光谱的FWHM随Y~/(3+/)共掺杂无明显变化,1000℃烧结粉末的FWHM随Y~/(3+/)浓度增加有所增大;掺Er~/(3+/)浓度为1mol/%时,除1000℃烧结的10mol/%Y~/(3+/)共掺杂粉末,其光谱FWHM降低外,900和1000℃烧结粉末的光谱FWHM均随Y~/(3+/)浓度增加而增大。 The 0.1 and 1 mol/% Er~3+ doped Al/_2O/_3 powders by Y~3+ codoping with the molar ratio of /(0-10/) : 1 for Y~3+ and Er~3+ at the sintering temperature of 900 and 1000℃ were prepared by the non-aqueous sol-gel method. The effects of Y~3+ codoping on the structure and photoluminescence properties of the powders were investigated.The 0.1 and 1 mol/% Er~3+-doped Al/_2O/_3 powders sintered at 900 and 1000 ℃ are of the mixture of γ and θ phases, which are both non-crystallization. The 0.1-1 mol/% Y~3+ codoping promotes the non-crystallization of the γ and θ phases for the 0.1 mol/% Er~3+-doped Al/_2O/_3 powders. The non-crystallization is also promoted by the 1-10 and 1-5 mol/% Y~3+ codoping for the 1 mol/% Er~3+-doped powders sintered at 900 and 1000 ℃ respectively, while the γ phases disappeares and the /(Er,Y/)/_3Al/_5O/_12 compound appears for the 1 mol/% Er~3+-doped powders at the sintering temperature of 1000 ℃ by 10 mol/% Y~3+ codoping. The FTIR spectra shows that the wavenumber range and the intensity of the absorption peak for O-H have no evident changes for the powders by Y~3+ codoping sintered at same temperature, indicating that Y~3+ codoping has no influence on the oscillation frequency and content of the O-H for the Er~3+-doped Al/_2O/_3 powders.The Er~3+-doped Al/_2O/_3 powders are characteristic of the photoluminescence /(PL/) spectra peaked at 1.53 urn, 660 nm /(red emission/), 545 and 523 nm /(green emission/) pumping by the laser with wavelength of 980 nm, and the emission peaked at 1.53μm is of stokes emission while the other two are of up-conversion emission. Y~3+ codoping has evident effects on the PL properties of the powers. On the one hand, Y~3+ codoping decreases the phone energy of the powders and increases the lifetime of the ~4I/_11//2 level for Er~3+, leading to a decrease in the intensity of Stokes emission and red emission as well as a increase in the intensity of green emssion and a decrease in the intensity ratio for the red emission and green emission. On the other hand, Y~3+ codoping effectively decreases the concentration quenching effect of the Er~3+, leading to an increase in the intensity of both Stokes emission and upconversion emission. For the 0.1 mol/% Er~3+-doped Al/_2O/_3 powders, the concentration quenching has small effect on its PL, and the Y~3+ codoping only decreases its phone energy with a corresponding changes in its PL intensity. For the 1 mol/% Er~3+-doped powders, Y~3+ codoping decreases both the phone energy and the Er~3+ concentration quenching, leading to an increase in both the Stokes emission and the upconversion emission with a decrease in the intensity ratio for green emssion and red emission. Y3+ codoping also influence the full width at half maximum /(FWHM/) of the PL spectrum peaked at 1.53 um for the Er3+-doped AI2O3 powders. For the 0.1 mol/% Er3+-doped powders sintered at 900 °C, the FWHM of the PL spectra has no evident change with Y3+ codoping, for that sintered at 1000 °C, the FWHM increases slightly by Y3+ codoping. The FWHM of the PL spectra for the 1 mol/% Er3+-doped AI2O3 powders sintered at 900 and 1000 °C both increase with the increase of the Y3+ codoping concentration, except a decrease in the FWHM of the spectrum for the powders sintered at 1000 °C by 10 mol/%Y3+codoping.

关 键 词: 共掺杂 光致发光 浓度猝灭

分 类 号: [TB34]

领  域: [一般工业技术]

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