电子束诱生硅中位错的发光性质及其物理结构研究
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摘要
硅作为最重要的半导体材料被广泛地用于微电子器件的制造,而基于硅集成电路工艺的硅基光电子,不仅能够为微电子器件提供大带宽的光互连,还可以降低光电子器件的制造成本,从而成为国际上半导体领域研究的热点之一。但是,与集成电路制造工艺兼容的硅基光源一直没有实现,是制约硅基光电子发展的首要问题。而硅中缺陷发光,尤其是基于硅中位错在红外波段的发光,已经成为实现硅基光源的重要路径之一
本文创新地提出并成功地运用了电子束辐照的方法,在硅晶体中诱生可控位错,系统研究了其生成机理及其物理结构性能,同时还对不同硅晶体(直拉单晶硅、区熔单晶硅和铸造准单晶硅)等样品中的诱生位错的光致发光及相应器件的电致发光性能进行了详细研究,取得了如下主要的创新结果：
(1)提出电子束辐照在硅片上引入可控位错的方法,位错密度可达107cm-2量级。该方法具有良好的可控性,通过控制电子束照射位置与角度,可以选择性地在硅片特定区域局域产生位错。研究指出,其显微结构为碎片化、局域化的位错结构；随着辐照时间的延长,宏观和微观的应变均会增大,使得位错与其他缺陷相互反应形成了较为复杂的结构。研究认为,电子束辐照所带来热应力所引起的硅晶格膨胀收缩是诱生位错的主要原因。电子束诱生位错的方法是一种新型的硅中引入位错的工具,为硅中缺陷研究提供了新方法,也为硅基位错提供了新的技术途径。
(2)通过调节温度与退火时间,实验发现,1050℃12h单步高温长时间热处理可以得到较好的电子束辐照硅中的位错发光,成功地增强并稳定了D1发光中心,大幅度提高了其淬灭温度,获得了室温D1发光。研究指出,D1发光中心的激活能在热处理前后几乎一致,为-86meV；另外,光致发光谱中的D1峰在170K-210K温度区间存在峰位反常移动现象,说明D1发光中心存在重构现象。研究表明,硅中点缺陷在高温长时间热处理中参与了位错结构的重构,从而形成了复杂的位错-点缺陷结构；而经重构的D1发光中心,能够大幅提高并稳定室温的D1发光。
(3)利用区熔单晶硅和直拉单晶硅诱生位错光致发光对比,对硅中位错发光谱线中的0.78eV峰来源做了系统深入的研究。其激活能为-13meV,远小于D1／D2峰的激活能。0.78eV峰独特的强度-温度衰减规律,说明它与D1／D2峰的来源是不同的。分析表明,0.78eV发光中心与硅中氧原子团簇,不论是热施主亦或是氧沉淀均没有关系。研究推测,该峰源自特定的经重构的位错结构,而该结构容易受点缺陷和温度的影响。
(4)通过电子束辐照硅晶体制备的硅基发光二极管,系统研究了电子束诱生位错在低温和室温变功率、变温度的电致发光谱,成功获得了1.6μm处的D1室温电致发光。研究表明,在15K时,D1发光中心容易被激活,而带边峰需要更高的注入水平才能出现,证明带边峰与D1峰存在相互竞争的关系。实验还发现,电致发光谱中D1峰相关的-0.86eV副峰仅在较大的注入功率下才会产生。变功率的电致发光谱研究表明,D1中心是由特定的位错引入的能级所组成。相比较于带边辐射复合,注入的电子和空穴更倾向于优先在D1发光中心附近复合发光。
(5)通过在铸造准单晶中运用电子束辐照的方法引入诱生位错,分别研究了铸造准单晶的原生位错、诱生位错、原生位错与诱生位错共存光致发光谱。研究发现：同一片准单晶上原生位错分布差异很大,不同区域光谱性质有显著差别,原生位错同样存在硅中位错发光的特征的D1-D4峰,D1/D2峰位随温度变化性质与单晶硅不一致；高温长时间热处理后,D1与D2合为大峰包,出现峰位先蓝移后红移的现象,这是因为在准单晶中,原生位错、辐照位错与杂质和点缺陷存在复杂反应,对D1发光中心产生影响。同时,研究认为热处理使得杂质与点缺陷在位错应力场周围形成气团；热处理温度升高,缺陷气团运动,从而可能造成D1峰位反常移动。
It is well known that silicon is one of the most important semiconductor materials which is widely used for microelectronic devices. The silicon photoelectric monolithic integration can provide a large bandwidth optical interconnects, inexpensive manufacturing for optoelectronic devices. These advantages make the silicon-based optoelectronics become one of the hotspots of the international semiconductor research. However, the lack of silicon-based light source which is compatible with the current IC manufacturing process has been the most important issue of silicon optoelectronics. The luminescence based on defects in silicon, especially the light-emitting in the infrared band based on silicon dislocations has become one of the most important paths to silicon-based light source.
In this dissertation, the electron beam irradiation technique has been creatively and successfully applied to inducing dislocations in silicon and its generation mechanism, physical structure and properties have been systemetically investigated. The photoluminescence and electroluminescence properties of different irradiated silicon samples (Czochralski silicon, float-zone silicon and cast quasi-single crystalline (QSC))silicon have been studied intensively. In the following, the primary achievements in this work are described.
(1) The method of electron beam irradiation can induce dislocations into silicon with densities up to～107cm-2. The method has good controllability, one can selectively generate localized dislocations at a specific area by controling the position and angle of the electron beam. The dislocation structure is fragmented and localized. By increasing of the irradiation time, the macro-and micro-strain increase. The dislocations and other defects will react with each other by forming more complex structures. We believe that the silicon lattice expansion and contraction caused by thermal stress introduced under the the electron beam irradiation is the main reason for the induced dislocations. The method of electron beam irradiation is a new method to induce dislocations in silicon, which offters the new option for the study of defects in silicon and the silicon-based light-emitting materials.
(2) The photoluminescence of dislocations in Czochralski silicon induced by electron beam irradiation are studied extensively by applying a wide range of temperature and time combinations. By applying the1050℃12h single step annealing, the Dl luminescence center has been successfully enhanced and stabilized and its quenching temperature has been substantially increased to room temperature. The D1peak activation energy is almost the same before and after heat treatment, which is-86meV. It is first reported that there is an abnormal energy movement of D1peak in the temperature range of170K-210K, which proves the existence of the reconstruction of D1luminescence center. Structural studies reveal that silicon point defects could participate in the reconstruction of the dislocation structure in the high temperature and long time annealing, thereby forming a complex dislocation-point defect structure. It is the reconstructed D1luminescence center which can strongly enhance and stabilize D1emitting at room temperature.
(3) The origin of the0.78eV line has been investigated systematically by comparing the photoluminescence of the electron irradiated float zone silicon and Czochralski silicon. The activation energy of0.78eV line is-13meV which is much smaller than that of D1/D2lines. The0.78eV line has its unique dependence of the intensity on temperature, which reveals its nature is different than that of D1/D2lines. It is shown that the0.78eV luminescence center has no relation with the silicon oxygen atoms in the clusters, neither in the form of the thermal donor nor the oxygen precipitates. The0.78eV line may come from specific reconstructed dislocation structure which is easily influenced by point defects and temperature.
(4) By preparing the silicon light emitting diodes, the power-dependent and temperature-dependent electroluminescence property of the electron irradiated silicon sample have been studied extensively. The strong Dl line around1.6μm is successfully achieved at room temperature. Studies show that the D1luminescence center is easily activated at15K, while the band-to-band luminescence requires a higher injection level. It reveals the competition of the Dl line and the band-to-band luminescence. It is also found that the～0.86eV peak beside the D1line in the electroluminescence spectra which only exist in the larger injected power. The power-dependent electroluminescence spectra study shows the D1center is composed by several dislocations induced energy levels. Compared to the band-to-band radiative recombination, the injected electron and hole will preferentially recombine near the D1luminescence center.
(5) The photoluminescence of as-grown dislocations and irradiated dislocations in the QSC silicon have been investigated extensity. It is found that the distribution of the native dislocations in the same QSC silicon wafer is widely varied, and the luminescence properties show significant differences in different regions. There are identical dislocation related D1～D4lines in the as-grown dislocations. The dependence of D1/D2peak positions on the temperature is different with the single crystalline silicon. The D1and D2lines envelope together as a large peak after the high temperature and long time annealing. There is a phenomenon that the peak position first blue shifts than redshifts with the increase of the temperature. In the QSC silicon, there is a complex reaction of as-grown dislocations and irradiated dislocations with the impurities and point defects, which exerts great effects on the D1luminescence center. The heat treatment will make the impurities and point defects form atmosphere bubbles around the dislocation stress field; when the temperature increases, the bubbles move, resulting in the abnormal peak movement of D1line. It reveals the fact that the dislocations luminescence centers is very susceptible to the influence of point defects.
本文创新地提出并成功地运用了电子束辐照的方法,在硅晶体中诱生可控位错,系统研究了其生成机理及其物理结构性能,同时还对不同硅晶体(直拉单晶硅、区熔单晶硅和铸造准单晶硅)等样品中的诱生位错的光致发光及相应器件的电致发光性能进行了详细研究,取得了如下主要的创新结果：
(1)提出电子束辐照在硅片上引入可控位错的方法,位错密度可达107cm-2量级。该方法具有良好的可控性,通过控制电子束照射位置与角度,可以选择性地在硅片特定区域局域产生位错。研究指出,其显微结构为碎片化、局域化的位错结构；随着辐照时间的延长,宏观和微观的应变均会增大,使得位错与其他缺陷相互反应形成了较为复杂的结构。研究认为,电子束辐照所带来热应力所引起的硅晶格膨胀收缩是诱生位错的主要原因。电子束诱生位错的方法是一种新型的硅中引入位错的工具,为硅中缺陷研究提供了新方法,也为硅基位错提供了新的技术途径。
(2)通过调节温度与退火时间,实验发现,1050℃12h单步高温长时间热处理可以得到较好的电子束辐照硅中的位错发光,成功地增强并稳定了D1发光中心,大幅度提高了其淬灭温度,获得了室温D1发光。研究指出,D1发光中心的激活能在热处理前后几乎一致,为-86meV；另外,光致发光谱中的D1峰在170K-210K温度区间存在峰位反常移动现象,说明D1发光中心存在重构现象。研究表明,硅中点缺陷在高温长时间热处理中参与了位错结构的重构,从而形成了复杂的位错-点缺陷结构；而经重构的D1发光中心,能够大幅提高并稳定室温的D1发光。
(3)利用区熔单晶硅和直拉单晶硅诱生位错光致发光对比,对硅中位错发光谱线中的0.78eV峰来源做了系统深入的研究。其激活能为-13meV,远小于D1／D2峰的激活能。0.78eV峰独特的强度-温度衰减规律,说明它与D1／D2峰的来源是不同的。分析表明,0.78eV发光中心与硅中氧原子团簇,不论是热施主亦或是氧沉淀均没有关系。研究推测,该峰源自特定的经重构的位错结构,而该结构容易受点缺陷和温度的影响。
(4)通过电子束辐照硅晶体制备的硅基发光二极管,系统研究了电子束诱生位错在低温和室温变功率、变温度的电致发光谱,成功获得了1.6μm处的D1室温电致发光。研究表明,在15K时,D1发光中心容易被激活,而带边峰需要更高的注入水平才能出现,证明带边峰与D1峰存在相互竞争的关系。实验还发现,电致发光谱中D1峰相关的-0.86eV副峰仅在较大的注入功率下才会产生。变功率的电致发光谱研究表明,D1中心是由特定的位错引入的能级所组成。相比较于带边辐射复合,注入的电子和空穴更倾向于优先在D1发光中心附近复合发光。
(5)通过在铸造准单晶中运用电子束辐照的方法引入诱生位错,分别研究了铸造准单晶的原生位错、诱生位错、原生位错与诱生位错共存光致发光谱。研究发现：同一片准单晶上原生位错分布差异很大,不同区域光谱性质有显著差别,原生位错同样存在硅中位错发光的特征的D1-D4峰,D1/D2峰位随温度变化性质与单晶硅不一致；高温长时间热处理后,D1与D2合为大峰包,出现峰位先蓝移后红移的现象,这是因为在准单晶中,原生位错、辐照位错与杂质和点缺陷存在复杂反应,对D1发光中心产生影响。同时,研究认为热处理使得杂质与点缺陷在位错应力场周围形成气团；热处理温度升高,缺陷气团运动,从而可能造成D1峰位反常移动。
It is well known that silicon is one of the most important semiconductor materials which is widely used for microelectronic devices. The silicon photoelectric monolithic integration can provide a large bandwidth optical interconnects, inexpensive manufacturing for optoelectronic devices. These advantages make the silicon-based optoelectronics become one of the hotspots of the international semiconductor research. However, the lack of silicon-based light source which is compatible with the current IC manufacturing process has been the most important issue of silicon optoelectronics. The luminescence based on defects in silicon, especially the light-emitting in the infrared band based on silicon dislocations has become one of the most important paths to silicon-based light source.
In this dissertation, the electron beam irradiation technique has been creatively and successfully applied to inducing dislocations in silicon and its generation mechanism, physical structure and properties have been systemetically investigated. The photoluminescence and electroluminescence properties of different irradiated silicon samples (Czochralski silicon, float-zone silicon and cast quasi-single crystalline (QSC))silicon have been studied intensively. In the following, the primary achievements in this work are described.
(1) The method of electron beam irradiation can induce dislocations into silicon with densities up to～107cm-2. The method has good controllability, one can selectively generate localized dislocations at a specific area by controling the position and angle of the electron beam. The dislocation structure is fragmented and localized. By increasing of the irradiation time, the macro-and micro-strain increase. The dislocations and other defects will react with each other by forming more complex structures. We believe that the silicon lattice expansion and contraction caused by thermal stress introduced under the the electron beam irradiation is the main reason for the induced dislocations. The method of electron beam irradiation is a new method to induce dislocations in silicon, which offters the new option for the study of defects in silicon and the silicon-based light-emitting materials.
(2) The photoluminescence of dislocations in Czochralski silicon induced by electron beam irradiation are studied extensively by applying a wide range of temperature and time combinations. By applying the1050℃12h single step annealing, the Dl luminescence center has been successfully enhanced and stabilized and its quenching temperature has been substantially increased to room temperature. The D1peak activation energy is almost the same before and after heat treatment, which is-86meV. It is first reported that there is an abnormal energy movement of D1peak in the temperature range of170K-210K, which proves the existence of the reconstruction of D1luminescence center. Structural studies reveal that silicon point defects could participate in the reconstruction of the dislocation structure in the high temperature and long time annealing, thereby forming a complex dislocation-point defect structure. It is the reconstructed D1luminescence center which can strongly enhance and stabilize D1emitting at room temperature.
(3) The origin of the0.78eV line has been investigated systematically by comparing the photoluminescence of the electron irradiated float zone silicon and Czochralski silicon. The activation energy of0.78eV line is-13meV which is much smaller than that of D1/D2lines. The0.78eV line has its unique dependence of the intensity on temperature, which reveals its nature is different than that of D1/D2lines. It is shown that the0.78eV luminescence center has no relation with the silicon oxygen atoms in the clusters, neither in the form of the thermal donor nor the oxygen precipitates. The0.78eV line may come from specific reconstructed dislocation structure which is easily influenced by point defects and temperature.
(4) By preparing the silicon light emitting diodes, the power-dependent and temperature-dependent electroluminescence property of the electron irradiated silicon sample have been studied extensively. The strong Dl line around1.6μm is successfully achieved at room temperature. Studies show that the D1luminescence center is easily activated at15K, while the band-to-band luminescence requires a higher injection level. It reveals the competition of the Dl line and the band-to-band luminescence. It is also found that the～0.86eV peak beside the D1line in the electroluminescence spectra which only exist in the larger injected power. The power-dependent electroluminescence spectra study shows the D1center is composed by several dislocations induced energy levels. Compared to the band-to-band radiative recombination, the injected electron and hole will preferentially recombine near the D1luminescence center.
(5) The photoluminescence of as-grown dislocations and irradiated dislocations in the QSC silicon have been investigated extensity. It is found that the distribution of the native dislocations in the same QSC silicon wafer is widely varied, and the luminescence properties show significant differences in different regions. There are identical dislocation related D1～D4lines in the as-grown dislocations. The dependence of D1/D2peak positions on the temperature is different with the single crystalline silicon. The D1and D2lines envelope together as a large peak after the high temperature and long time annealing. There is a phenomenon that the peak position first blue shifts than redshifts with the increase of the temperature. In the QSC silicon, there is a complex reaction of as-grown dislocations and irradiated dislocations with the impurities and point defects, which exerts great effects on the D1luminescence center. The heat treatment will make the impurities and point defects form atmosphere bubbles around the dislocation stress field; when the temperature increases, the bubbles move, resulting in the abnormal peak movement of D1line. It reveals the fact that the dislocations luminescence centers is very susceptible to the influence of point defects.
引文
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