稀土掺杂包埋纳米晶硅硅基薄膜光学性质研究
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摘要
随着科学技术的发展,现有的微电子技术已难以满足由其支撑的现代电了技术不断提出的更高要求。用光子代替电子作为信息的载体,从微电子技术向光集成或光电子集成技术发展,成为必然的趋势。虽然Ⅲ-Ⅴ族半导体材料非常适合制造光电子器件,但在Ⅲ-Ⅴ族化合物基片上制造大规模电子集成回路的技术还很不成熟,且造价太高,难以进入民用市场。相反,硅基微电子集成制造工艺相当成熟,己进入大规模工业化生产阶段。因此硅基光电集成成为研究的主要热点。然而硅基半导体材料不是好的发光体,限制了它们在光电子集成方面的应用。稀土离了具有丰富的电子能级和4f电子跃迁特性,可获得多种发光性能,能够为高科技领域特别是通信领域提供性能优越的发光材料。稀土掺杂包理纳米晶硅硅基发光材料在实现微电子技术向光电子集成技术发展中具有重要意义,因此一直是人们不懈追求的研究目标。
利用离子束溅射和离子注入技术,并辅以热氧化技术,制备了Er掺杂富硅SiO2薄膜材料和Ce掺杂SiO2薄膜材料。分别利用透射电子显微镜、拉曼光谱和光致发光谱研究了Er掺杂富硅SiO2薄膜材料的微结构和光致发光性质、Ce掺杂SiO2薄膜材料的光致发光性质。并利用CASTEP软件计算了各种SiO2结构的材料的光电性质。主要取得了以下研究结果：
对Er掺杂富硅SiO2薄膜样品在1100℃经10secs-5mins进行高温快速退火。研究了退火样品的微结构和光致发光性质。结果表明：经退火热处理后在SiO2薄膜基体中有Si-nc晶粒生成。在室温条件下,所有退火态样品中均观测到较强的Si-nc和Er3+离子发光。随退火时间增加,Si-nc颗粒尺寸增大,量子限制效应减弱,导致Si-nc发光强度减弱,发光峰位红移。对于Er3+离子,其发光峰峰位几乎不随退火时间增加而改变。但随退火时间增加,其发光强度明显改变,并且发光强度随退火时间的变化趋势与Si-nc相反,验证了Si-nc与Er3+离子之间确实存在能量传递。对样品施加不同的外加压强进行调制后,Si-nc的发光峰位波长在P=5.76GPa时明显减小,而发光强度也在该压强附近急剧减弱。这是由基体材料及纳米晶硅结构在外加压强作用下发生变化引起的。
利用不同的实验方法制备了两个系列Ce3+离子掺杂SiO2薄膜样品,并对样品在不同条件下进行退火热处理。室温条件下,在所有制备态和退火态样品中均观测到较强的Ce3+离子光致发光。详细讨论了Ce3+离子掺杂浓度、退火条件、制备方法等对样品发光性质的影响。研究发现Ce3+离子的发光性质强烈依赖于Ce3+离子掺杂浓度、退火温度、退火气氛以及制备方法。随Ce3+离子掺杂浓度增加,其发光强度几乎呈线性增加,发光峰峰位改变。当Ce3+离子掺杂浓度继续增加时,离了间距离减小,处于激发态的Ce3+离子将能量传递给近邻的其它Ce3+离子从而引起发光猝灭。在空气气氛中经较高温度退火后,基体中有更多的Ce3+离子存在并进入SiO2网格形成发光中心,导致材料发光强度增强。随退火温度继续增加,一方面Ce3+离子发生团簇引起发光猝灭或者直接从基体材料中析出；另一方面,更多的Ce3+离子被氧化为非光学活性的Ce4+离子。以上因素导致Ce3+离子发光强度显著减弱。另外通过分析不同气氛中退火样品的PL谱,发现N2气氛可有效保护Ce3+离了防止Ce3+离子被氧化为Ce4+离了,从而可以明显改善样品的发光性质。不同的制备方法对样品的发光性质也有影响,例如在B系列样品中随着Ce3+离子掺杂浓度增加到1.46at%,观察到Ce3+离子发光猝灭效应,而在A系列样品中却没有发现这种现象。
利用CASTEP软件计算了包埋纳米晶硅SiO2和Ce掺杂SiO2结构的材料的电子结构和光学性质。研究表明,与SiO2材料相比,包理纳米晶SiO2材料整个导带下移,并在费米面附近形成局域分离能级。禁带宽度由原来的5.742eV减小为1.05eV。吸收光谱中,在2.27eV处出现新的吸收峰,对应于费米面以下-1.01eV附近能级上的电子向由键角畸变引入的费米面以上1.05eV附近能级的跃迁。研究表明,用一个Ce原子代替Si原子形成Ce掺杂SiO2结构材料后,在SiO2禁带中引入Ce杂质能级,禁带宽度减小。与SiO2材料相比,吸收谱中2.96eV处出现新的吸收峰,对应于Ce的4f电子向5d能级跃迁,与实验测量结果一致。
With the development of science and technology, the existing microelectronic technology has been difficult to meet the higher requirements put forward by the modern electronic technology which was supported by microelectronic technology. Using photons to instead of electrons as the carrier of information, that microelectronic technology turn into photon integrated or optoelectronic integrated technology become an inevitable trend. The Ⅲ-Ⅴ semiconductor materials are suitable to use for optoelectronic devices, however the technology to manufacture large-scale electronic integrated circuit is still immature for the Ⅲ-Ⅴ compound materials and the cost too high to enter the civilian market. In contrast, the manufacturing process of silicon-based microelectronic integration is quite mature and it has reached the level of large-scale industrial production. So. the silicon-based optoelectronic integration becomes the main interest point of the study. The silicon semiconductor materials, however, is not good at luminescence which limits their application for the optoelectronic integration. Rare earth ions own a wealth of electronic energy levels and the4f electron transition characteristics. So. the rare earth ions can obtain a variety of luminescence properties to be able to be used as luminescence materials for high level technology especially the field of communication. The rare earth doped silicon-based luminescence materials embedded Si-nc have been the relentless pursuit of research goals for great significance shown in the development from microelectronic technology to photon integrated or optoelectronic integrated technology.
In this thesis, Er-doped Si-rich silicon oxide samples and Ce-doped silicon oxide samples were successfully prepared, respectively, by ion beam sputtering and ion implantation. The microstructure and photoluminescence (PL) properties of Er-doped Si-rich silicon oxide samples were investigated through transmission electron microscopy (TEM), Raman spectroscopy and PL spectroscopy, respectively. The PL properties of Ce-doped silicon oxide samples were also investigated via the PL spectroscopy. And the photoelectric properties of doped SiO2thin films were studied by CASTEP software package.
The Er-doped Si-rich silicon oxide samples were annealed at1100℃with annealing time from10sees to5mins. The investigations of the microstructure and PL properties show that Si nanocrystalline (Si-nc) was formed in annealed samples and PL of Si-nc and Er3+ions were observed at room temperature from all annealed samples. The size of Si-nc particle increases with increasing annealing time. So, the quantum confinement effect becomes weak leading to the decrease of PL intensity and red shift of PL peak wavelength. In contrast, there is no obvious change of the PL peak position of Er3+ions with increasing annealing time. However, the PL intensity changed as the annealing time increased, and the changing trend is contrary to that of Si-nc which verifies the energy transfer does exist between Si-nc and Er3ions. Different pressures were applied to the samples and the PL studies show the peak position changed sharply as the pressure reached5.76GPa, the PL intensity was also changed as the pressure value is around5.76GPa. All the changes may arise from the change of the structure of matrix materials.
Two series Ce-doped silicon oxide samples were successfully prepared via different processes. PL of Ce3+ions were observed at room temperature from all unannealed and annealed samples. PL of Ce3+ions were detected from all Ce-doped silicon oxide samples un-annealed and annealed and the effect of Ce ions concentrations, annealing conditions and fabricating process on the PL properties were investigated comprehensively. The results indicated that the PL properties were dependent strongly on Ce ions concentrations, annealing temperatures, annealing ambient and fabricating process. The PL intensity increases almost linearly and the peak position changes with increasing Ce concentrations. As the Ce concentrations further increased, the distance between Ce3+ions decreased, some excited Ce3+ions transfer their energy to other nearby Ce3+ion, which causes PL quenching. When the samples were annealed at high temperatures in air ambient, the amount of Ce3+ions increases and more Ce3+ions have enough energy to enter the network of silica to form the PL centers, so the PL intensity enhanced. However, the PL intensity decreases obviously as the annealing temperatures continue to increase. The Clustering or precipitation of Ce3+ions occurs and Ce3+ions can be oxidized to form inactive Ce4+ions at higher temperatures, which results in a decrease of PL intensity. Compared the PL spectroscopy of samples annealed in different ambient, the results indicated nitrogen gas can protect the Ce3+ions from being oxidized. Therefore, the PL intensity can be enhanced for the samples annealed in nitrogen gas. The fabricating processes also have an influence on the PL properties. The oxidation of the samples with Ce ions implanted into Si films likely produces more Ce4+, leading to a PL quenching which is not observed in the samples with Ce ions implanted into SiO2films.
The electronic structure and optical properties of Si-nc embedded in SiO2and Ce-doped SiO2were investigated by first-principles pseudopotential plane-wave method. The results show the whole conduction band moved down and the localized energy levels near the Fermi level were observed in the Si-nc embedded in SiO2. And the band gap changed from5.742eV to1.05eV. According to the absorption spectroscopy, the new absorption peak at about2.27eV is attributed to the transition of the electrons from-1.01eV energy level to1.05eV energy level generated by valence-band distortion. As for the Ce-doped SiO2structure, the results show the impurity levels of Ce were introduced leading to the decrease of band gap. The absorption peak at about2.96eV is attributed to the transition of electrons from4f energy level to5d energy level, which consisitent the measurement result.
利用离子束溅射和离子注入技术,并辅以热氧化技术,制备了Er掺杂富硅SiO2薄膜材料和Ce掺杂SiO2薄膜材料。分别利用透射电子显微镜、拉曼光谱和光致发光谱研究了Er掺杂富硅SiO2薄膜材料的微结构和光致发光性质、Ce掺杂SiO2薄膜材料的光致发光性质。并利用CASTEP软件计算了各种SiO2结构的材料的光电性质。主要取得了以下研究结果：
对Er掺杂富硅SiO2薄膜样品在1100℃经10secs-5mins进行高温快速退火。研究了退火样品的微结构和光致发光性质。结果表明：经退火热处理后在SiO2薄膜基体中有Si-nc晶粒生成。在室温条件下,所有退火态样品中均观测到较强的Si-nc和Er3+离子发光。随退火时间增加,Si-nc颗粒尺寸增大,量子限制效应减弱,导致Si-nc发光强度减弱,发光峰位红移。对于Er3+离子,其发光峰峰位几乎不随退火时间增加而改变。但随退火时间增加,其发光强度明显改变,并且发光强度随退火时间的变化趋势与Si-nc相反,验证了Si-nc与Er3+离子之间确实存在能量传递。对样品施加不同的外加压强进行调制后,Si-nc的发光峰位波长在P=5.76GPa时明显减小,而发光强度也在该压强附近急剧减弱。这是由基体材料及纳米晶硅结构在外加压强作用下发生变化引起的。
利用不同的实验方法制备了两个系列Ce3+离子掺杂SiO2薄膜样品,并对样品在不同条件下进行退火热处理。室温条件下,在所有制备态和退火态样品中均观测到较强的Ce3+离子光致发光。详细讨论了Ce3+离子掺杂浓度、退火条件、制备方法等对样品发光性质的影响。研究发现Ce3+离子的发光性质强烈依赖于Ce3+离子掺杂浓度、退火温度、退火气氛以及制备方法。随Ce3+离子掺杂浓度增加,其发光强度几乎呈线性增加,发光峰峰位改变。当Ce3+离子掺杂浓度继续增加时,离了间距离减小,处于激发态的Ce3+离子将能量传递给近邻的其它Ce3+离子从而引起发光猝灭。在空气气氛中经较高温度退火后,基体中有更多的Ce3+离子存在并进入SiO2网格形成发光中心,导致材料发光强度增强。随退火温度继续增加,一方面Ce3+离子发生团簇引起发光猝灭或者直接从基体材料中析出；另一方面,更多的Ce3+离子被氧化为非光学活性的Ce4+离子。以上因素导致Ce3+离子发光强度显著减弱。另外通过分析不同气氛中退火样品的PL谱,发现N2气氛可有效保护Ce3+离了防止Ce3+离子被氧化为Ce4+离了,从而可以明显改善样品的发光性质。不同的制备方法对样品的发光性质也有影响,例如在B系列样品中随着Ce3+离子掺杂浓度增加到1.46at%,观察到Ce3+离子发光猝灭效应,而在A系列样品中却没有发现这种现象。
利用CASTEP软件计算了包埋纳米晶硅SiO2和Ce掺杂SiO2结构的材料的电子结构和光学性质。研究表明,与SiO2材料相比,包理纳米晶SiO2材料整个导带下移,并在费米面附近形成局域分离能级。禁带宽度由原来的5.742eV减小为1.05eV。吸收光谱中,在2.27eV处出现新的吸收峰,对应于费米面以下-1.01eV附近能级上的电子向由键角畸变引入的费米面以上1.05eV附近能级的跃迁。研究表明,用一个Ce原子代替Si原子形成Ce掺杂SiO2结构材料后,在SiO2禁带中引入Ce杂质能级,禁带宽度减小。与SiO2材料相比,吸收谱中2.96eV处出现新的吸收峰,对应于Ce的4f电子向5d能级跃迁,与实验测量结果一致。
With the development of science and technology, the existing microelectronic technology has been difficult to meet the higher requirements put forward by the modern electronic technology which was supported by microelectronic technology. Using photons to instead of electrons as the carrier of information, that microelectronic technology turn into photon integrated or optoelectronic integrated technology become an inevitable trend. The Ⅲ-Ⅴ semiconductor materials are suitable to use for optoelectronic devices, however the technology to manufacture large-scale electronic integrated circuit is still immature for the Ⅲ-Ⅴ compound materials and the cost too high to enter the civilian market. In contrast, the manufacturing process of silicon-based microelectronic integration is quite mature and it has reached the level of large-scale industrial production. So. the silicon-based optoelectronic integration becomes the main interest point of the study. The silicon semiconductor materials, however, is not good at luminescence which limits their application for the optoelectronic integration. Rare earth ions own a wealth of electronic energy levels and the4f electron transition characteristics. So. the rare earth ions can obtain a variety of luminescence properties to be able to be used as luminescence materials for high level technology especially the field of communication. The rare earth doped silicon-based luminescence materials embedded Si-nc have been the relentless pursuit of research goals for great significance shown in the development from microelectronic technology to photon integrated or optoelectronic integrated technology.
In this thesis, Er-doped Si-rich silicon oxide samples and Ce-doped silicon oxide samples were successfully prepared, respectively, by ion beam sputtering and ion implantation. The microstructure and photoluminescence (PL) properties of Er-doped Si-rich silicon oxide samples were investigated through transmission electron microscopy (TEM), Raman spectroscopy and PL spectroscopy, respectively. The PL properties of Ce-doped silicon oxide samples were also investigated via the PL spectroscopy. And the photoelectric properties of doped SiO2thin films were studied by CASTEP software package.
The Er-doped Si-rich silicon oxide samples were annealed at1100℃with annealing time from10sees to5mins. The investigations of the microstructure and PL properties show that Si nanocrystalline (Si-nc) was formed in annealed samples and PL of Si-nc and Er3+ions were observed at room temperature from all annealed samples. The size of Si-nc particle increases with increasing annealing time. So, the quantum confinement effect becomes weak leading to the decrease of PL intensity and red shift of PL peak wavelength. In contrast, there is no obvious change of the PL peak position of Er3+ions with increasing annealing time. However, the PL intensity changed as the annealing time increased, and the changing trend is contrary to that of Si-nc which verifies the energy transfer does exist between Si-nc and Er3ions. Different pressures were applied to the samples and the PL studies show the peak position changed sharply as the pressure reached5.76GPa, the PL intensity was also changed as the pressure value is around5.76GPa. All the changes may arise from the change of the structure of matrix materials.
Two series Ce-doped silicon oxide samples were successfully prepared via different processes. PL of Ce3+ions were observed at room temperature from all unannealed and annealed samples. PL of Ce3+ions were detected from all Ce-doped silicon oxide samples un-annealed and annealed and the effect of Ce ions concentrations, annealing conditions and fabricating process on the PL properties were investigated comprehensively. The results indicated that the PL properties were dependent strongly on Ce ions concentrations, annealing temperatures, annealing ambient and fabricating process. The PL intensity increases almost linearly and the peak position changes with increasing Ce concentrations. As the Ce concentrations further increased, the distance between Ce3+ions decreased, some excited Ce3+ions transfer their energy to other nearby Ce3+ion, which causes PL quenching. When the samples were annealed at high temperatures in air ambient, the amount of Ce3+ions increases and more Ce3+ions have enough energy to enter the network of silica to form the PL centers, so the PL intensity enhanced. However, the PL intensity decreases obviously as the annealing temperatures continue to increase. The Clustering or precipitation of Ce3+ions occurs and Ce3+ions can be oxidized to form inactive Ce4+ions at higher temperatures, which results in a decrease of PL intensity. Compared the PL spectroscopy of samples annealed in different ambient, the results indicated nitrogen gas can protect the Ce3+ions from being oxidized. Therefore, the PL intensity can be enhanced for the samples annealed in nitrogen gas. The fabricating processes also have an influence on the PL properties. The oxidation of the samples with Ce ions implanted into Si films likely produces more Ce4+, leading to a PL quenching which is not observed in the samples with Ce ions implanted into SiO2films.
The electronic structure and optical properties of Si-nc embedded in SiO2and Ce-doped SiO2were investigated by first-principles pseudopotential plane-wave method. The results show the whole conduction band moved down and the localized energy levels near the Fermi level were observed in the Si-nc embedded in SiO2. And the band gap changed from5.742eV to1.05eV. According to the absorption spectroscopy, the new absorption peak at about2.27eV is attributed to the transition of the electrons from-1.01eV energy level to1.05eV energy level generated by valence-band distortion. As for the Ce-doped SiO2structure, the results show the impurity levels of Ce were introduced leading to the decrease of band gap. The absorption peak at about2.96eV is attributed to the transition of electrons from4f energy level to5d energy level, which consisitent the measurement result.
引文
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