氮和锗对直拉硅单晶机械性能的影响
摘要
集成电路的快速发展，要求硅单晶大直径、无缺陷，这对硅单晶晶体的生长、加工工艺及后继的集成电路工艺提出了全新的挑战。随着硅单晶直径的增大，籽晶承重不断增加，硅片加工过程中的损伤、集成电路工艺中不断增加的热应力和重应力引起翘曲等新的问题对硅单晶的机械性能提出了新的要求。因此对单晶硅材料的机械性能研究，提高其机械强度成为集成电路工业中一个不可忽视的方向。
掺杂是改善硅单品性能的一种重要方法。近年来，掺氮和掺锗的硅单晶可以抑制Void缺陷，并有很好的内吸杂能力，可以满足下一代集成电路工业的要求，逐渐受到产业界的重视。杂质原子不仅可以影响硅单晶的电学性能及微缺陷的形成，同时对硅单晶机械性能也有很大作用，但是相关的机械性能的研究很少。
本论文偏重于杂质原子对硅单晶机械性能的影响，阐述了杂质原子与位错的相互作用，杂质对硅单晶塑性变形及断裂的影响，及常见杂质对硅单晶机械性能的影响。在压痕法研究氮和锗对硅中位错运动的影响和室温三点弯法研究锗对直拉单晶硅室温断裂强度的影响的基础上，提出了氮和锗原子影响硅单晶机械性能的机理。
本论文首先系统的研究了压痕法研究硅单晶中位错运动的主要实验因素。研究了加载载荷、加载时间、热处理时间、热处理温度和样品晶向对位错运动的影响。结果表明位错滑移长度与加载载荷成正比，而与加载时间无关。并对热处理过程中位错的运动过程进行了理论的分析，发现位错运动过程中应力随热处理时间以指数的方式迅速衰减，相应的位错滑移距离与时间也存在指数关系；位错滑移距离与热处理温度正相关。在此实验的基础上，确定了实验的最佳条件。
通过对比掺氮和不掺氮重掺锑直拉单晶硅中的位错运动，实验发现与普通轻掺硅单晶不同，位错在重掺锑硅单晶中滑移需要一个孕育期，这主要是由于重掺锑硅单晶中存在大量的位错钉扎源(锑原子，氧沉淀核心等)，使得位错从杂质气氛下脱钉需要一定的时间。实验还发现，氮在重掺锑硅单晶中依然对位错运动有明显抑制作用：氮原子自身对位错的强烈钉扎作用和对氧沉淀产生的促进作用，使得含氮重掺硅单晶中的位错需要更长的孕育期，滑移距离也更短。
本文还系统的研究了锗对直拉硅单晶机械性能的影响。研究表明，仅当锗浓
浙江大学硕士生毕业论文
度达到lxlo’“cm一时，锗才表现出对硅中位错运动的抑制作用。经过对位错运动
过程的分析，认为锗的主要作用机理为在低应力阶段形成复合体和氧沉淀核心等
位错钉扎源，降低了位错滑移速度并提高了位错的滑移临界应力。
锗杂质对硅单晶的室温断裂强度的影响的实验研究表明:与普通直拉硅单晶
相比，锗浓度为1又10lscm一3的掺锗硅单晶原生硅片的室温断裂强度并无明显变
化;但含有氧沉淀的硅片断裂强度有明显提高。这说明锗原子本身对硅单晶断裂
强度的影响较小，主要通过改变氧沉淀的密度和尺寸，来影响直拉硅单晶的断裂
强度。当锗浓度为lx10‘“cm一3时，硅中氧沉淀的密度明显提高，尺寸变小，这些
氧沉淀可以阻止微裂纹扩展并改变裂纹扩展路径，从而可以提高硅单晶的断裂强
度。
总之，实验表明，氮和锗不仅可以抑制硅单晶中的缺陷，还可以提高直拉硅
单晶的机械性能，有望在下一代的集成电路中得到广泛的应用。这对于发展具有
我国自主知识产权的集成电路用硅材料有重要意义。
The development of ultra large-scale integrated (ULSI) circuit requires large diameter and defect free Czochralski (CZ) silicon wafers, which challenges the traditional crystal growth process and the 1C processing of silicon crystal. Especially nowadays, it is often the critical problems in ULSI devices fabrication that defects and dislocations generated in silicon caused by the increased crystal diameter. The enlarged wafer diameter that demanded silicon wafers suffered much higher thermal stress and gravitational stress as well as the seed bearing more weight. Therefore, it is desirable to investigate the mechanical property of silicon crystal and enhance its mechanical property.
It is well known that impurities influence not only the formation of microdefects and the electronic property, but also the mechanical property. In recent years, the nitrogen (N) doped and germanium (Ge) doped CZ silicon crystals have been received intensive attention due to their novel properties. Hence, it is worth to investigate the effect of N and Ge on the mechanical property from both the practical and theoretic purposes.
This paper was focused on the interaction between the impurities and dislocations by indentation. It was founded that the distance traveled of dislocations was related to the load, annealing temperature, and crystal orientation, but independent with the loading time. By this method, the effect of common impurity dopants in CZ silicon were investigated and summarized. Our experiments suggest that the N enhanced the mechanical property of silicon either in lightly or in heavily doped wafers. And it was interesting that an incubation of the dislocations slide in the HSb CZ silicon was founded. The incubation was attributed that dislocations needed more time to escape from the pinning of the large amount of impurity atoms or complexes.
On the other hand, the effect of N and Ge on the mechanical property of silicon crystal had been done systemically. For Ge doped wafers, the dislocation pinning
could be observed only when Ge concentration was high than 1018cm"3. And the further experiment proved that the individual Ge atom hardly increased the fracture strength of silicon at room temperature. The enhancement of Ge on silicon was obtained mainly by the formation of complex or clusters with oxygen.
In short, the better understanding on the mechanical property of silicon makes better use of the silicon material to ULSI industry. Also through the investigation on the N doped and Ge doped CZ silicon, it will greatly advance the development of our national intellectual property of the silicon material used for ULSI.
掺杂是改善硅单品性能的一种重要方法。近年来，掺氮和掺锗的硅单晶可以抑制Void缺陷，并有很好的内吸杂能力，可以满足下一代集成电路工业的要求，逐渐受到产业界的重视。杂质原子不仅可以影响硅单晶的电学性能及微缺陷的形成，同时对硅单晶机械性能也有很大作用，但是相关的机械性能的研究很少。
本论文偏重于杂质原子对硅单晶机械性能的影响，阐述了杂质原子与位错的相互作用，杂质对硅单晶塑性变形及断裂的影响，及常见杂质对硅单晶机械性能的影响。在压痕法研究氮和锗对硅中位错运动的影响和室温三点弯法研究锗对直拉单晶硅室温断裂强度的影响的基础上，提出了氮和锗原子影响硅单晶机械性能的机理。
本论文首先系统的研究了压痕法研究硅单晶中位错运动的主要实验因素。研究了加载载荷、加载时间、热处理时间、热处理温度和样品晶向对位错运动的影响。结果表明位错滑移长度与加载载荷成正比，而与加载时间无关。并对热处理过程中位错的运动过程进行了理论的分析，发现位错运动过程中应力随热处理时间以指数的方式迅速衰减，相应的位错滑移距离与时间也存在指数关系；位错滑移距离与热处理温度正相关。在此实验的基础上，确定了实验的最佳条件。
通过对比掺氮和不掺氮重掺锑直拉单晶硅中的位错运动，实验发现与普通轻掺硅单晶不同，位错在重掺锑硅单晶中滑移需要一个孕育期，这主要是由于重掺锑硅单晶中存在大量的位错钉扎源(锑原子，氧沉淀核心等)，使得位错从杂质气氛下脱钉需要一定的时间。实验还发现，氮在重掺锑硅单晶中依然对位错运动有明显抑制作用：氮原子自身对位错的强烈钉扎作用和对氧沉淀产生的促进作用，使得含氮重掺硅单晶中的位错需要更长的孕育期，滑移距离也更短。
本文还系统的研究了锗对直拉硅单晶机械性能的影响。研究表明，仅当锗浓
浙江大学硕士生毕业论文
度达到lxlo’“cm一时，锗才表现出对硅中位错运动的抑制作用。经过对位错运动
过程的分析，认为锗的主要作用机理为在低应力阶段形成复合体和氧沉淀核心等
位错钉扎源，降低了位错滑移速度并提高了位错的滑移临界应力。
锗杂质对硅单晶的室温断裂强度的影响的实验研究表明:与普通直拉硅单晶
相比，锗浓度为1又10lscm一3的掺锗硅单晶原生硅片的室温断裂强度并无明显变
化;但含有氧沉淀的硅片断裂强度有明显提高。这说明锗原子本身对硅单晶断裂
强度的影响较小，主要通过改变氧沉淀的密度和尺寸，来影响直拉硅单晶的断裂
强度。当锗浓度为lx10‘“cm一3时，硅中氧沉淀的密度明显提高，尺寸变小，这些
氧沉淀可以阻止微裂纹扩展并改变裂纹扩展路径，从而可以提高硅单晶的断裂强
度。
总之，实验表明，氮和锗不仅可以抑制硅单晶中的缺陷，还可以提高直拉硅
单晶的机械性能，有望在下一代的集成电路中得到广泛的应用。这对于发展具有
我国自主知识产权的集成电路用硅材料有重要意义。
The development of ultra large-scale integrated (ULSI) circuit requires large diameter and defect free Czochralski (CZ) silicon wafers, which challenges the traditional crystal growth process and the 1C processing of silicon crystal. Especially nowadays, it is often the critical problems in ULSI devices fabrication that defects and dislocations generated in silicon caused by the increased crystal diameter. The enlarged wafer diameter that demanded silicon wafers suffered much higher thermal stress and gravitational stress as well as the seed bearing more weight. Therefore, it is desirable to investigate the mechanical property of silicon crystal and enhance its mechanical property.
It is well known that impurities influence not only the formation of microdefects and the electronic property, but also the mechanical property. In recent years, the nitrogen (N) doped and germanium (Ge) doped CZ silicon crystals have been received intensive attention due to their novel properties. Hence, it is worth to investigate the effect of N and Ge on the mechanical property from both the practical and theoretic purposes.
This paper was focused on the interaction between the impurities and dislocations by indentation. It was founded that the distance traveled of dislocations was related to the load, annealing temperature, and crystal orientation, but independent with the loading time. By this method, the effect of common impurity dopants in CZ silicon were investigated and summarized. Our experiments suggest that the N enhanced the mechanical property of silicon either in lightly or in heavily doped wafers. And it was interesting that an incubation of the dislocations slide in the HSb CZ silicon was founded. The incubation was attributed that dislocations needed more time to escape from the pinning of the large amount of impurity atoms or complexes.
On the other hand, the effect of N and Ge on the mechanical property of silicon crystal had been done systemically. For Ge doped wafers, the dislocation pinning
could be observed only when Ge concentration was high than 1018cm"3. And the further experiment proved that the individual Ge atom hardly increased the fracture strength of silicon at room temperature. The enhancement of Ge on silicon was obtained mainly by the formation of complex or clusters with oxygen.
In short, the better understanding on the mechanical property of silicon makes better use of the silicon material to ULSI industry. Also through the investigation on the N doped and Ge doped CZ silicon, it will greatly advance the development of our national intellectual property of the silicon material used for ULSI.
引文
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