掺稀土碲酸盐玻璃与光纤应用基础问题研究
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摘要
21世纪信息量的爆炸式增长和信息交流需求的剧增,迫切需要对信息进行超高速率、超快响应和超大容量处理。传统的掺铒石英光纤放大器由于稀土掺杂浓度较低,带宽较窄(～30 nm),已不能满足通信传输发展的需要。因此,在波分复用技术的推动下,开发新型宽带光纤放大器,将光放大带宽开拓至L波段和S波段,成为目前光通信材料与器件研究的热点之一。本文以研究用于1.53μm宽带光纤放大器的掺稀土碲酸盐玻璃与玻璃光纤应用基础问题为主要目标。主要内容包括掺稀土多组分碲酸盐玻璃与玻璃光纤基础问题研究,碲酸盐玻璃与光纤材料的激发和发光、能量传递与转换、光放大特性等材料物理和光学基本问题研究和探讨,多组分碲酸盐玻璃基光纤激光器的关键技术等。
碲酸盐玻璃具有比氟化物和磷酸盐更好的稳定性和抗腐蚀性。与传统掺铒石英玻璃相比,掺铒碲酸盐玻璃具有熔制温度低、透光区域大(0.35-6μm)、稀土离子溶解度高、折射率高、声子能量低(～750 cm?1)等优点。利用稀土掺杂碲酸盐光学玻璃作为激光核心介质,能够获得较大的受激发射截面、较高的辐射量子效率和带宽(～70 nm),有利于器件的小型化,对扩大光通信系统的传输容量具有重要的意义。然而,目前碲酸盐玻璃尚存在一些缺点,例如,碲酸盐玻璃抗析晶热稳定性较差、玻璃脆性较大、机械强度较低等,导致光纤制备过程中容易出现析晶、微裂纹等缺陷,引起光纤损耗增加;其次,由于碲酸盐玻璃声子能量较低,使得在980 nm激光二极管泵浦下,上转换和激发态吸收成为两个主要的能量损失通道,导致Er~(3+)离子在1.53μm的发光效率降低。
针对上述难题,结合国内外最新发展和研究,本论文着重研究了掺稀土多组分碲酸盐玻璃与玻璃光纤的应用基础问题,探讨了碲酸盐玻璃与光纤材料的激发和发光、能量传递与转换、光放大机理,以及多组分碲酸盐玻璃基光纤激光器的关键技术等。根据拉曼光谱测试,分析了不同网络修饰体和混合形成体对Er~(3+)离子配位环境的影响,讨论了不同类型玻璃中结构基团振动引起玻璃基质声子能量的变化,指出结构特征的变化对玻璃抗析晶热稳定性和Er~(3+)离子光谱非均匀展宽的作用。采用适当的敏化离子和能量接受离子共掺的方法,提高Er~(3+)离子对泵浦光的吸收效率,降低上转换发光,改善了Er~(3+)离子在玻璃中的发光特性;依据这些结果进一步分析稀土离子间能量传递机制,在此基础上优化光放大介质的设计;最后从光学参数、热力学参数和流变特性等性能匹配的角度,确定了光纤预制棒的纤芯和包层组分,制备稀土掺杂碲酸盐玻璃光纤;初步探讨了碲酸盐玻璃光纤的宽带光放大特性。本论文取得的主要结论和创新点如下:
(1)通过在TeO2-ZnO-Na2O系统玻璃中引入声子能量约为900 cm-1的Nb2O5、WO3和GeO2等网络形成体或网络中间体氧化物,显著改善了碲酸盐玻璃的抗析晶热稳定性。其拉曼光谱、X射线衍射谱和差示扫描测试分析研究表明,与一般采用网络修饰体改善玻璃热稳定性的方法相比,利用重金属氧化物对网络的修复作用和对网络群体的牵制作用之间的平衡,强化了碲酸盐玻璃网络结构。同时,高声子能量重金属氧化物的引入产生了明显的混合形成体效应,增大了Er~(3+)离子光谱的非均匀展宽,提高了玻璃的最大声子能量或最大声子能量密度,导致Er~(3+)离子4I11/2→4I13/2无辐射跃迁的几率提高,有效降低了上转换发光强度。
(2)系统探讨了能量接受离子RE~(3+)(RE~(3+) =Ce~(3+), Eu~(3+), Tb~(3+), Dy~(3+), Ho~(3+)和Tm~(3+))对Er~(3+)/Yb~(3+)共掺碲酸盐玻璃发光特性的影响规律,根据稀土离子能级,上转换发光光谱和荧光发射光谱,分析了Er~(3+)、Yb~(3+)和RE~(3+)离子之间的能量传递机制。研究结果显示,通过Dexter能量共振转移,掺杂能量接受离子Ce~(3+), Eu~(3+), Tb~(3+)和Dy~(3+)可以有效降低Er~(3+)离子上转换发光。而且,共掺Ce~(3+)离子还可以增强Er~(3+)在1.53μm处的发光,使得Er~(3+)/Yb~(3+)共掺碲酸盐玻璃在1.53μm光纤放大器的应用更具吸引力。
(3)采用“改进的管棒法”制备碲酸盐玻璃预制棒,并成功拉制出掺铒和掺铥单模碲酸盐玻璃光纤,其荧光半高宽分别为60 nm和102 nm,将掺铒和掺铥碲酸盐玻璃光纤串接后,荧光半高宽达到128 nm,为传统石英光纤的3倍以上,基本覆盖E+S+C波段。
(4)采用单程后向超荧光实验结构,在mW级的泵浦功率下,在长仅几厘米的掺铒碲酸盐玻璃短光纤中实现了3 dB带宽为60～80 nm的放大自发辐射光谱。
上述研究结果为进一步研究研制掺稀土碲酸盐基光纤激光器和放大器提供了理论基础和技术支撑。
With the rapid development of computer networks and other data-transmitting services, the demand for the increase of capacity of communication system is urgent. The conventional silica based Er~(3+)-doped fiber amplifier (EDFA) can not meet this requirement because of its low rare earth ion solubility and intrinsic bandwidth limit (～30 nm). Therefore, wide bandwidth novel optical amplifier covering C-band, L-band and S-band for wavelength division multiplexing (WDM) system has been attracted a great deal of attention. The dissertation reports on research works in the subject of the Er~(3+)-doped multi-component tellurtie glass active fiber for 1.53μm broadband optical amplifiers. The fundamental investigations on the properties and fluorescence characteristics of glass materials and fiber, the glass fiber fabrication technology and the pertinent theory of energy transfer have been carried out.
Compared with conventional Er~(3+)-doped silica glasses, Er~(3+)-doped tellurite glasses combining the attribute of low melting temperature, wide bandwidth (~70 nm), wide transmission region (0.35-6μm), good glass stability, rare earth ion solubility, slow corrosion rate, lowest phonon energy spectrum among oxide glass formers, and high refractive index, are now promising candidates for use in fabricating novel optical amplifiers for WDM system. However, there are two important factors to be considered in developing efficient amplifiers using tellurite glasses. Firstly, the relatively poor thermal stability and low strength lead to crystallization processes at the moment of optical fiber drawing, as well as make the material easy damageable at high optical intensities. Secondly, due to their low phonon energy (～750 cm?1), under 980nm pump, up-conversion and excited state absorption (ESA) become two dominant loss mechanisms,significantly depleting the spectral gain of Er~(3+) ions.
Herein, based on the requirement of the development of optical communication, the optimization on thermal stability and luminescence properties of the rare-earth-doped multi-component tellurite glasses have been the goal of this dissertation. The Raman spectra results indicate that the local ligand environment of Er~(3+) in glasses changed by different modifiers and mixed formers. The variations of maximum phonon energies in different glasses with vibrations of different kinds of structural group were discussed. And the influence of the structural characteristics on thermal stability and inhomogeneous broaden of Er~(3+)emission spectrum were also pointed out. Moreover, the spectral properties of Er~(3+) ions in tellurite glasses have been improved by introducing donor ion and energy acceptor ions. And the possible energy transfer mechanisms involved have also been systemically analyzed and discussed. The cladding glasses and the core glasses were then selected considering their well match in refractive index, thermal properties and rheological properties. Finally, the rare- earth-doped optical fiber were fabricated and characterized optically with a single pass backward (SPB) configuration.
The novel and main results of the research works are as follows:
(1) The Raman spectra, XRD and DCS results indicate that the introducing network formers (Nb2O5、WO3 and GeO2) behaved better than other modifiers in improving the thermal stability of tellurite glasses. With appropriate phonon energy (900 cm-1), they are also helpful for lowering the up-conversion luminescence of Er~(3+)-doped tellurite glass, via speeding up the nonradiative relaxation of Er~(3+):4I11/2→4I13/2 transition without influencing the 1.53μm emission.
(2) The effect of energy acceptor RE~(3+) (RE~(3+) =Ce~(3+), Eu~(3+), Tb~(3+), Dy~(3+), Ho~(3+) and Tm~(3+)) ions on the fluorescence characteristics of tellurite glasses co-doped with Er~(3+)/Yb~(3+) is reported. The energy transfer dominated by Dexter mechanism between Er~(3+) and RE~(3+) were explored based on their energy level diagrams, up-conversion and infrared emission properties. It is found that the incorporation of energy acceptor into Er~(3+)/Yb~(3+)-codoped tellurite glass could effectively reduce up-conversion emission. Moreover, co-doping Ce~(3+) could also enhanced the 1.53μm emission, which makes Er~(3+)/Yb~(3+)-codoped tellurite glass more attractive for using in 1.53μm optical fiber amplifiers.
(3) A modified rod-in-tube technique is brought forward to prepared Er~(3+)-doped and Tm~(3+)-doped tellurite single-mode glass-fibers with the FWHM of 60 nm and 102 nm respectively. And broad emission spectra with bandwidth up to 128 nm (as 3 times of that in conventional Er~(3+)-doped silica glasses), which coveres E-, S- and C-bands simultaneously, is obtained based on an tandem structure with Er~(3+)-doped and Tm~(3+)-doped tellurite glass-fibers.
(4) A very broad erbium amplified spontaneous emission (60~80 nm) from erbium-doped single- mode tellurite glass-fiber is described in a single pass backward (SPB) configuration.The advantages of this EDTF are the short EDTF length and the small pumping power required in such an SPB configuration.
The investigation results of this work provide theoretical foundation and technical support for the further research on rare-earth-doped tellurite glass fiber amplifier and laser.
碲酸盐玻璃具有比氟化物和磷酸盐更好的稳定性和抗腐蚀性。与传统掺铒石英玻璃相比,掺铒碲酸盐玻璃具有熔制温度低、透光区域大(0.35-6μm)、稀土离子溶解度高、折射率高、声子能量低(～750 cm?1)等优点。利用稀土掺杂碲酸盐光学玻璃作为激光核心介质,能够获得较大的受激发射截面、较高的辐射量子效率和带宽(～70 nm),有利于器件的小型化,对扩大光通信系统的传输容量具有重要的意义。然而,目前碲酸盐玻璃尚存在一些缺点,例如,碲酸盐玻璃抗析晶热稳定性较差、玻璃脆性较大、机械强度较低等,导致光纤制备过程中容易出现析晶、微裂纹等缺陷,引起光纤损耗增加;其次,由于碲酸盐玻璃声子能量较低,使得在980 nm激光二极管泵浦下,上转换和激发态吸收成为两个主要的能量损失通道,导致Er~(3+)离子在1.53μm的发光效率降低。
针对上述难题,结合国内外最新发展和研究,本论文着重研究了掺稀土多组分碲酸盐玻璃与玻璃光纤的应用基础问题,探讨了碲酸盐玻璃与光纤材料的激发和发光、能量传递与转换、光放大机理,以及多组分碲酸盐玻璃基光纤激光器的关键技术等。根据拉曼光谱测试,分析了不同网络修饰体和混合形成体对Er~(3+)离子配位环境的影响,讨论了不同类型玻璃中结构基团振动引起玻璃基质声子能量的变化,指出结构特征的变化对玻璃抗析晶热稳定性和Er~(3+)离子光谱非均匀展宽的作用。采用适当的敏化离子和能量接受离子共掺的方法,提高Er~(3+)离子对泵浦光的吸收效率,降低上转换发光,改善了Er~(3+)离子在玻璃中的发光特性;依据这些结果进一步分析稀土离子间能量传递机制,在此基础上优化光放大介质的设计;最后从光学参数、热力学参数和流变特性等性能匹配的角度,确定了光纤预制棒的纤芯和包层组分,制备稀土掺杂碲酸盐玻璃光纤;初步探讨了碲酸盐玻璃光纤的宽带光放大特性。本论文取得的主要结论和创新点如下:
(1)通过在TeO2-ZnO-Na2O系统玻璃中引入声子能量约为900 cm-1的Nb2O5、WO3和GeO2等网络形成体或网络中间体氧化物,显著改善了碲酸盐玻璃的抗析晶热稳定性。其拉曼光谱、X射线衍射谱和差示扫描测试分析研究表明,与一般采用网络修饰体改善玻璃热稳定性的方法相比,利用重金属氧化物对网络的修复作用和对网络群体的牵制作用之间的平衡,强化了碲酸盐玻璃网络结构。同时,高声子能量重金属氧化物的引入产生了明显的混合形成体效应,增大了Er~(3+)离子光谱的非均匀展宽,提高了玻璃的最大声子能量或最大声子能量密度,导致Er~(3+)离子4I11/2→4I13/2无辐射跃迁的几率提高,有效降低了上转换发光强度。
(2)系统探讨了能量接受离子RE~(3+)(RE~(3+) =Ce~(3+), Eu~(3+), Tb~(3+), Dy~(3+), Ho~(3+)和Tm~(3+))对Er~(3+)/Yb~(3+)共掺碲酸盐玻璃发光特性的影响规律,根据稀土离子能级,上转换发光光谱和荧光发射光谱,分析了Er~(3+)、Yb~(3+)和RE~(3+)离子之间的能量传递机制。研究结果显示,通过Dexter能量共振转移,掺杂能量接受离子Ce~(3+), Eu~(3+), Tb~(3+)和Dy~(3+)可以有效降低Er~(3+)离子上转换发光。而且,共掺Ce~(3+)离子还可以增强Er~(3+)在1.53μm处的发光,使得Er~(3+)/Yb~(3+)共掺碲酸盐玻璃在1.53μm光纤放大器的应用更具吸引力。
(3)采用“改进的管棒法”制备碲酸盐玻璃预制棒,并成功拉制出掺铒和掺铥单模碲酸盐玻璃光纤,其荧光半高宽分别为60 nm和102 nm,将掺铒和掺铥碲酸盐玻璃光纤串接后,荧光半高宽达到128 nm,为传统石英光纤的3倍以上,基本覆盖E+S+C波段。
(4)采用单程后向超荧光实验结构,在mW级的泵浦功率下,在长仅几厘米的掺铒碲酸盐玻璃短光纤中实现了3 dB带宽为60～80 nm的放大自发辐射光谱。
上述研究结果为进一步研究研制掺稀土碲酸盐基光纤激光器和放大器提供了理论基础和技术支撑。
With the rapid development of computer networks and other data-transmitting services, the demand for the increase of capacity of communication system is urgent. The conventional silica based Er~(3+)-doped fiber amplifier (EDFA) can not meet this requirement because of its low rare earth ion solubility and intrinsic bandwidth limit (～30 nm). Therefore, wide bandwidth novel optical amplifier covering C-band, L-band and S-band for wavelength division multiplexing (WDM) system has been attracted a great deal of attention. The dissertation reports on research works in the subject of the Er~(3+)-doped multi-component tellurtie glass active fiber for 1.53μm broadband optical amplifiers. The fundamental investigations on the properties and fluorescence characteristics of glass materials and fiber, the glass fiber fabrication technology and the pertinent theory of energy transfer have been carried out.
Compared with conventional Er~(3+)-doped silica glasses, Er~(3+)-doped tellurite glasses combining the attribute of low melting temperature, wide bandwidth (~70 nm), wide transmission region (0.35-6μm), good glass stability, rare earth ion solubility, slow corrosion rate, lowest phonon energy spectrum among oxide glass formers, and high refractive index, are now promising candidates for use in fabricating novel optical amplifiers for WDM system. However, there are two important factors to be considered in developing efficient amplifiers using tellurite glasses. Firstly, the relatively poor thermal stability and low strength lead to crystallization processes at the moment of optical fiber drawing, as well as make the material easy damageable at high optical intensities. Secondly, due to their low phonon energy (～750 cm?1), under 980nm pump, up-conversion and excited state absorption (ESA) become two dominant loss mechanisms,significantly depleting the spectral gain of Er~(3+) ions.
Herein, based on the requirement of the development of optical communication, the optimization on thermal stability and luminescence properties of the rare-earth-doped multi-component tellurite glasses have been the goal of this dissertation. The Raman spectra results indicate that the local ligand environment of Er~(3+) in glasses changed by different modifiers and mixed formers. The variations of maximum phonon energies in different glasses with vibrations of different kinds of structural group were discussed. And the influence of the structural characteristics on thermal stability and inhomogeneous broaden of Er~(3+)emission spectrum were also pointed out. Moreover, the spectral properties of Er~(3+) ions in tellurite glasses have been improved by introducing donor ion and energy acceptor ions. And the possible energy transfer mechanisms involved have also been systemically analyzed and discussed. The cladding glasses and the core glasses were then selected considering their well match in refractive index, thermal properties and rheological properties. Finally, the rare- earth-doped optical fiber were fabricated and characterized optically with a single pass backward (SPB) configuration.
The novel and main results of the research works are as follows:
(1) The Raman spectra, XRD and DCS results indicate that the introducing network formers (Nb2O5、WO3 and GeO2) behaved better than other modifiers in improving the thermal stability of tellurite glasses. With appropriate phonon energy (900 cm-1), they are also helpful for lowering the up-conversion luminescence of Er~(3+)-doped tellurite glass, via speeding up the nonradiative relaxation of Er~(3+):4I11/2→4I13/2 transition without influencing the 1.53μm emission.
(2) The effect of energy acceptor RE~(3+) (RE~(3+) =Ce~(3+), Eu~(3+), Tb~(3+), Dy~(3+), Ho~(3+) and Tm~(3+)) ions on the fluorescence characteristics of tellurite glasses co-doped with Er~(3+)/Yb~(3+) is reported. The energy transfer dominated by Dexter mechanism between Er~(3+) and RE~(3+) were explored based on their energy level diagrams, up-conversion and infrared emission properties. It is found that the incorporation of energy acceptor into Er~(3+)/Yb~(3+)-codoped tellurite glass could effectively reduce up-conversion emission. Moreover, co-doping Ce~(3+) could also enhanced the 1.53μm emission, which makes Er~(3+)/Yb~(3+)-codoped tellurite glass more attractive for using in 1.53μm optical fiber amplifiers.
(3) A modified rod-in-tube technique is brought forward to prepared Er~(3+)-doped and Tm~(3+)-doped tellurite single-mode glass-fibers with the FWHM of 60 nm and 102 nm respectively. And broad emission spectra with bandwidth up to 128 nm (as 3 times of that in conventional Er~(3+)-doped silica glasses), which coveres E-, S- and C-bands simultaneously, is obtained based on an tandem structure with Er~(3+)-doped and Tm~(3+)-doped tellurite glass-fibers.
(4) A very broad erbium amplified spontaneous emission (60~80 nm) from erbium-doped single- mode tellurite glass-fiber is described in a single pass backward (SPB) configuration.The advantages of this EDTF are the short EDTF length and the small pumping power required in such an SPB configuration.
The investigation results of this work provide theoretical foundation and technical support for the further research on rare-earth-doped tellurite glass fiber amplifier and laser.
引文
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