大规模集成电路用同族元素掺杂直拉硅单晶的微缺陷及其缺陷工程
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摘要
超大规模集成电路的高速发展对硅单晶材料提出了愈来愈严格的要求,控制和消除直拉硅中的微缺陷是硅材料开发面临的最关键的问题。随着直拉硅单晶的大直径化,硅中氧含量有所下降,而当代集成电路以超浅结为特征,其制造工艺的热预算显著降低,这两方面都不利于直拉硅中的氧沉淀,从而削弱了硅片的内吸杂能力,使得传统的内吸杂工艺受到了挑战。另一方面,在大直径直拉硅中形成的空洞型缺陷(Void)若得不到有效的控制,将会影响金属-氧化物-半导体(MOS)器件的栅极氧化层完整性(GOI),从而降低集成电路的成品率。利用共掺杂技术来调控硅中的微缺陷和增强硅片的内吸杂能力是目前硅材料研究的热点,开发新型共掺杂直拉硅单晶具有重要的理论意义和实用价值,是目前和今后国际硅材料界重要的研究领域之一。
本文在生长同族元素(锗、碳)掺杂的新型直拉硅单晶的基础上,系统的研究了掺锗直拉(GCZ)硅和高碳含量的直拉(H[C]CZ)硅中的氧沉淀行为以及Void产生和消除的规律,揭示了同族元素杂质影响直拉硅中微缺陷行为的机理;同时,研究了适用于这两种新型直拉硅片的内吸杂工艺,取得了如下所述的创新结果:
(1)研究了微量锗杂质影响直拉硅中氧沉淀的规律,发现掺锗可以促进原生氧沉淀的形成并在很宽的温度范围(650-1150℃)内促进后续退火过程中的氧沉淀。揭示了微量锗杂质影响直拉硅中氧沉淀的机理,指出GCZ硅中形成的Ge-V和Ge-V-O等锗关复合体可以作为氧沉淀的异质形核核心,从而促进氧沉淀的形成。同时,发现掺锗能显著降低直拉硅中氧沉淀的高温热稳定性,指出这是由于GCZ硅中形成了小尺寸的氧沉淀和片状氧沉淀所致。
(2)研究了基于普通炉退火(CFA)和快速热退火(RTA)处理的适用于GCZ硅片的内吸杂工艺。发现掺锗能促进直拉硅片在高-低-高三步退火过程中的氧沉淀从而提高体微缺陷(BMD)密度并同时减小洁净区(DZ)宽度。通过RTA预退火结合低-高两步退火或高温单步退火的热处理工艺,在GCZ硅片中形成高密度的BMD和宽度合适的DZ,这有助于减小集成电路制作过程中内吸杂工艺的热预算。同时,明确指出:通过上述两种工艺形成的DZ中不存在微小氧沉淀,并且GCZ硅片体内BMD区吸除金属沾污的能力优于普通直拉(CZ)硅片。
(3)研究了适用于H[C]CZ硅片的内吸杂工艺及其氧沉淀规律,发现高浓度碳杂质可以在内吸杂工艺过程中促进硅中的氧沉淀。揭示了碳影响氧沉淀的机理,指明H[C]CZ硅中形成的C(3)中心和C-V等碳关复合体会促进氧沉淀的生成。并且通过基于CFA和RTA处理的内吸杂工艺在H[C]CZ硅片中形成了没有微小氧沉淀的DZ和具有比CZ硅片更高密度的BMD。该结果为H[C]CZ硅片在集成电路制造中的可能应用提供了理论依据。
(4)研究了微量锗杂质和高浓度碳杂质对直拉硅中Void形成的影响。与CZ硅片相比,GCZ硅片中形成了更高密度的小尺寸Void和更低密度的大尺寸Void,而H[C]CZ硅片中具有更低密度的大尺寸Void,指出这是由于在晶体生长冷却过程中Void形成之前,锗和碳杂质与空位形成复合体从而降低了硅中空位浓度,使得Void形成温度降低所致。此外,微量锗杂质或高浓度碳杂质的引入都可以降低Void的高温热稳定性,这有助于消除硅片近表面区域中的Void,从而提高MOS器件的GOI。
(5)研究了微量锗杂质对直拉硅片机械性能的影响,发现掺锗有利于在硅中形成高密度的小尺寸氧沉淀,它们可以钉扎位错从而抑制位错攀移,并由此降低硅片在器件制造过程中的弯曲度和翘曲度,这有利于提高集成电路制造的成品率。
(6)根据第一性原理计算,指出直拉硅中的同族元素(锗、碳)杂质可以与空位和间隙氧原子形成复合体。基于实验提供的证据,认为这些复合体可以在晶体生长冷却过程中的高温阶段形成,这一方面消耗了部分空位从而促进高密度小尺寸Void的形成;另一方面,这些复合体在很宽的温度范围内可以作为异质形核核心而促进氧沉淀。同样的,这些复合体也可以在RTA处理的高温过程中形成,并促进后续退火过程中的氧沉淀。在理论和实验工作的基础上,建立了同族元素杂质影响直拉硅中微缺陷(氧沉淀和Void)形成的物理模型。
With the rapid development of ultra large-scale integrated circuits(ICs),the requirements on silicon materials become increasingly stringent.The control and elimination of microdefects in Czochralski(CZ)silicon is the most important issue for the development of silicon materials.For the larger diameter CZ silicon wafers, the oxygen concentration is reduced to a certain extent.Moreover,the thermal budget for the manufacturing of contemporary IC featuring super-shallow junction is significantly lowered.The two regards as mentioned above are not favorable for oxygen precipitation and therefore the internal gettering(IG)capability for CZ silicon wafers so that the traditional IG process is challenged.On the other hand,the gate oxide integrity(GOI)of metal-oxide-semiconductor(MOS)devices and furthermore the yield of IC will be deteriorated by the void defects commonly existing in large diameter silicon wafers.Addressing the control of microdefects and the enhancement of IG capability,the strategy of co-doping in CZ silicon has been developed.
In this dissertation,based on the growth of new type CZ silicon crystals doped with iso-group elements(germanium and carbon),the oxygen precipitation behavior and the formation and elimination of void defects in both the lightly germanium doped CZ(GCZ)silicon and high-carbon-content CZ(H[C]CZ)silicon have been intensively investigated.Moreover,the mechanisms for the effect of germanium and carbon on the oxygen precipitation and grown-in defects in CZ silicon have been reasonably exploited.Furthermore,the IG processes appropriate for GCZ and H[C] CZ silicon wafers have been well developed.Listed below are the most important results achieved in this work.
(1)The effects of germanium on oxygen precipitation in CZ silicon have been investigated.It is found that the formation of grown-in oxygen precipitates and oxygen precipitation during the post-growth anneals in a wide temperature range of 650-1150℃can be enhanced by the germanium-doping in CZ silicon.It is suggested that the germanium-related complexes generated during the crystal growth,such as Ge-V and Ge-V-O complexes,act as the heterogeneous nucleation centers for oxygen precipitates in GCZ silicon.Moreover,it is found that the thermal stability of oxygen precipitates at high temperature for GCZ silicon is remarkably weakened,which is attributed to the small precipitates and plate-like precipitates formed in GCZ silicon.
(2)The IG processes for GCZ silicon wafer based on the conventional furnace anneal(CFA)and rapid thermal anneal(RTA)have been developed.With the three-step of high-low-high anneal,the density of bulk microdefects(BMDs)is increased and the denuded zone(DZ)is narrowed in the GCZ silicon wafer with respect to the conventional CZ silicon wafer,which is ascribed to the enhancement of oxygen precipitation by the germanium doping.It is also found that a high density of BMDs and a DZ with a desirable width can be generated in GCZ silicon wafer subjected to the low-high two step anneal or a single high temperature anneal following a RTA at high temperature,meaning that the RTA-based IG processes feature substantially lower thermal budget.Note that it has been definitely clarified that there are hardly tiny oxygen precipitates existing in the DZ formed by the CFA- and RTA-based IG processes for GCZ silicon wafer and,moreover,the IG capability of GCZ silicon wafer is superior to that of CZ silicon wafer.
(3)The effects of high-content carbon on oxygen precipitation in H[C]CZ silicon have been investigated and,furthermore,the IG processes for H[C]CZ silicon wafers have been developed.It is found that oxygen precipitation occurring in the IG processes is enhanced by the high-content carbon,due to the formation of carbon-related complexes,including C(3)center and C-V complexes,in H[C]CZ silicon. On the other hand,both the DZ without tiny oxygen precipitates and a higher density of BMDs with respect to that of CZ wafer can be generated in H[C]CZ silicon wafer through the CFA- and RTA-based IG process,which sheds light on the application of H[C]CZ silicon wafer in the manufacturing of IC.
(4)The influences of the light germanium-doping and the heavy carbon-doping on the formation of void defects in CZ silicon have been investigated.It is found that the small-sized voids in a higher density and the large-sized voids in a lower density are generated in GCZ silicon wafer while the large-sized voids in a lower density are formed in H[C]CZ silicon wafer,with respect to those in CZ silicon wafer.It is believed that during the post-cooling of crystal growth the interaction of germanium or carbon and vacancy to form the complexes prior to the formation of voids consumes a number of vacancies,therefore,the formation of voids in GCZ and H[C]CZ silicon shifts to a lower temperature,thus leading to generating smaller but denser voids. Moreover,the voids in GCZ and H[C]CZ silicon wafers can be annihilated at lower temperatures with respect to those in CZ silicon wafer,which facilitates to increase the GOI of MOS devices.
(5)The effect of light germanium-doping on the mechanical properties of CZ silicon wafer has been tentatively investigated.Due to the high density of small-sized oxygen precipitates preformed in GCZ silicon,the climbing of dislocations can be suppressed by the pinning effect of small-sized oxygen precipitates on the dislocations.As a result,the warp and bow of CZ silicon wafer doped with the germanium can be significantly reduced during the thermal cycles of device fabrication, which is beneficial for the elimination of voids within the near-surface region of silicon wafer.
(6)According to the computation based on first principle,it is theoretically pointed out that the interaction among the germanium/carbon,oxygen and vacancy and therefore the formation of complexes in specific structures are thermodynamically favorable.Based on the experimental evidences,it is believed that such complexes can be formed in silicon during the post-crystal-growth cooling process.On one hand,the complexes consumes a part of vacancies in silicon involved during the crystal growth,thus leading to smaller voids in higher density;on the other hand, they can act as the heterogeneous nucleation centers for the enhanced oxygen precipitation. Likewise,the germanium and carbon related complexes can be also formed during the RTA process,which also promote oxygen precipitation during the subsequent anneals.With the theoretical and experimental works,a qualitative model for elucidating the mechanism for the effects of germanium and carbon on the behaviors of microdefects(oxygen precipitate and void)in CZ silicon has been tentatively developed.
本文在生长同族元素(锗、碳)掺杂的新型直拉硅单晶的基础上,系统的研究了掺锗直拉(GCZ)硅和高碳含量的直拉(H[C]CZ)硅中的氧沉淀行为以及Void产生和消除的规律,揭示了同族元素杂质影响直拉硅中微缺陷行为的机理;同时,研究了适用于这两种新型直拉硅片的内吸杂工艺,取得了如下所述的创新结果:
(1)研究了微量锗杂质影响直拉硅中氧沉淀的规律,发现掺锗可以促进原生氧沉淀的形成并在很宽的温度范围(650-1150℃)内促进后续退火过程中的氧沉淀。揭示了微量锗杂质影响直拉硅中氧沉淀的机理,指出GCZ硅中形成的Ge-V和Ge-V-O等锗关复合体可以作为氧沉淀的异质形核核心,从而促进氧沉淀的形成。同时,发现掺锗能显著降低直拉硅中氧沉淀的高温热稳定性,指出这是由于GCZ硅中形成了小尺寸的氧沉淀和片状氧沉淀所致。
(2)研究了基于普通炉退火(CFA)和快速热退火(RTA)处理的适用于GCZ硅片的内吸杂工艺。发现掺锗能促进直拉硅片在高-低-高三步退火过程中的氧沉淀从而提高体微缺陷(BMD)密度并同时减小洁净区(DZ)宽度。通过RTA预退火结合低-高两步退火或高温单步退火的热处理工艺,在GCZ硅片中形成高密度的BMD和宽度合适的DZ,这有助于减小集成电路制作过程中内吸杂工艺的热预算。同时,明确指出:通过上述两种工艺形成的DZ中不存在微小氧沉淀,并且GCZ硅片体内BMD区吸除金属沾污的能力优于普通直拉(CZ)硅片。
(3)研究了适用于H[C]CZ硅片的内吸杂工艺及其氧沉淀规律,发现高浓度碳杂质可以在内吸杂工艺过程中促进硅中的氧沉淀。揭示了碳影响氧沉淀的机理,指明H[C]CZ硅中形成的C(3)中心和C-V等碳关复合体会促进氧沉淀的生成。并且通过基于CFA和RTA处理的内吸杂工艺在H[C]CZ硅片中形成了没有微小氧沉淀的DZ和具有比CZ硅片更高密度的BMD。该结果为H[C]CZ硅片在集成电路制造中的可能应用提供了理论依据。
(4)研究了微量锗杂质和高浓度碳杂质对直拉硅中Void形成的影响。与CZ硅片相比,GCZ硅片中形成了更高密度的小尺寸Void和更低密度的大尺寸Void,而H[C]CZ硅片中具有更低密度的大尺寸Void,指出这是由于在晶体生长冷却过程中Void形成之前,锗和碳杂质与空位形成复合体从而降低了硅中空位浓度,使得Void形成温度降低所致。此外,微量锗杂质或高浓度碳杂质的引入都可以降低Void的高温热稳定性,这有助于消除硅片近表面区域中的Void,从而提高MOS器件的GOI。
(5)研究了微量锗杂质对直拉硅片机械性能的影响,发现掺锗有利于在硅中形成高密度的小尺寸氧沉淀,它们可以钉扎位错从而抑制位错攀移,并由此降低硅片在器件制造过程中的弯曲度和翘曲度,这有利于提高集成电路制造的成品率。
(6)根据第一性原理计算,指出直拉硅中的同族元素(锗、碳)杂质可以与空位和间隙氧原子形成复合体。基于实验提供的证据,认为这些复合体可以在晶体生长冷却过程中的高温阶段形成,这一方面消耗了部分空位从而促进高密度小尺寸Void的形成;另一方面,这些复合体在很宽的温度范围内可以作为异质形核核心而促进氧沉淀。同样的,这些复合体也可以在RTA处理的高温过程中形成,并促进后续退火过程中的氧沉淀。在理论和实验工作的基础上,建立了同族元素杂质影响直拉硅中微缺陷(氧沉淀和Void)形成的物理模型。
With the rapid development of ultra large-scale integrated circuits(ICs),the requirements on silicon materials become increasingly stringent.The control and elimination of microdefects in Czochralski(CZ)silicon is the most important issue for the development of silicon materials.For the larger diameter CZ silicon wafers, the oxygen concentration is reduced to a certain extent.Moreover,the thermal budget for the manufacturing of contemporary IC featuring super-shallow junction is significantly lowered.The two regards as mentioned above are not favorable for oxygen precipitation and therefore the internal gettering(IG)capability for CZ silicon wafers so that the traditional IG process is challenged.On the other hand,the gate oxide integrity(GOI)of metal-oxide-semiconductor(MOS)devices and furthermore the yield of IC will be deteriorated by the void defects commonly existing in large diameter silicon wafers.Addressing the control of microdefects and the enhancement of IG capability,the strategy of co-doping in CZ silicon has been developed.
In this dissertation,based on the growth of new type CZ silicon crystals doped with iso-group elements(germanium and carbon),the oxygen precipitation behavior and the formation and elimination of void defects in both the lightly germanium doped CZ(GCZ)silicon and high-carbon-content CZ(H[C]CZ)silicon have been intensively investigated.Moreover,the mechanisms for the effect of germanium and carbon on the oxygen precipitation and grown-in defects in CZ silicon have been reasonably exploited.Furthermore,the IG processes appropriate for GCZ and H[C] CZ silicon wafers have been well developed.Listed below are the most important results achieved in this work.
(1)The effects of germanium on oxygen precipitation in CZ silicon have been investigated.It is found that the formation of grown-in oxygen precipitates and oxygen precipitation during the post-growth anneals in a wide temperature range of 650-1150℃can be enhanced by the germanium-doping in CZ silicon.It is suggested that the germanium-related complexes generated during the crystal growth,such as Ge-V and Ge-V-O complexes,act as the heterogeneous nucleation centers for oxygen precipitates in GCZ silicon.Moreover,it is found that the thermal stability of oxygen precipitates at high temperature for GCZ silicon is remarkably weakened,which is attributed to the small precipitates and plate-like precipitates formed in GCZ silicon.
(2)The IG processes for GCZ silicon wafer based on the conventional furnace anneal(CFA)and rapid thermal anneal(RTA)have been developed.With the three-step of high-low-high anneal,the density of bulk microdefects(BMDs)is increased and the denuded zone(DZ)is narrowed in the GCZ silicon wafer with respect to the conventional CZ silicon wafer,which is ascribed to the enhancement of oxygen precipitation by the germanium doping.It is also found that a high density of BMDs and a DZ with a desirable width can be generated in GCZ silicon wafer subjected to the low-high two step anneal or a single high temperature anneal following a RTA at high temperature,meaning that the RTA-based IG processes feature substantially lower thermal budget.Note that it has been definitely clarified that there are hardly tiny oxygen precipitates existing in the DZ formed by the CFA- and RTA-based IG processes for GCZ silicon wafer and,moreover,the IG capability of GCZ silicon wafer is superior to that of CZ silicon wafer.
(3)The effects of high-content carbon on oxygen precipitation in H[C]CZ silicon have been investigated and,furthermore,the IG processes for H[C]CZ silicon wafers have been developed.It is found that oxygen precipitation occurring in the IG processes is enhanced by the high-content carbon,due to the formation of carbon-related complexes,including C(3)center and C-V complexes,in H[C]CZ silicon. On the other hand,both the DZ without tiny oxygen precipitates and a higher density of BMDs with respect to that of CZ wafer can be generated in H[C]CZ silicon wafer through the CFA- and RTA-based IG process,which sheds light on the application of H[C]CZ silicon wafer in the manufacturing of IC.
(4)The influences of the light germanium-doping and the heavy carbon-doping on the formation of void defects in CZ silicon have been investigated.It is found that the small-sized voids in a higher density and the large-sized voids in a lower density are generated in GCZ silicon wafer while the large-sized voids in a lower density are formed in H[C]CZ silicon wafer,with respect to those in CZ silicon wafer.It is believed that during the post-cooling of crystal growth the interaction of germanium or carbon and vacancy to form the complexes prior to the formation of voids consumes a number of vacancies,therefore,the formation of voids in GCZ and H[C]CZ silicon shifts to a lower temperature,thus leading to generating smaller but denser voids. Moreover,the voids in GCZ and H[C]CZ silicon wafers can be annihilated at lower temperatures with respect to those in CZ silicon wafer,which facilitates to increase the GOI of MOS devices.
(5)The effect of light germanium-doping on the mechanical properties of CZ silicon wafer has been tentatively investigated.Due to the high density of small-sized oxygen precipitates preformed in GCZ silicon,the climbing of dislocations can be suppressed by the pinning effect of small-sized oxygen precipitates on the dislocations.As a result,the warp and bow of CZ silicon wafer doped with the germanium can be significantly reduced during the thermal cycles of device fabrication, which is beneficial for the elimination of voids within the near-surface region of silicon wafer.
(6)According to the computation based on first principle,it is theoretically pointed out that the interaction among the germanium/carbon,oxygen and vacancy and therefore the formation of complexes in specific structures are thermodynamically favorable.Based on the experimental evidences,it is believed that such complexes can be formed in silicon during the post-crystal-growth cooling process.On one hand,the complexes consumes a part of vacancies in silicon involved during the crystal growth,thus leading to smaller voids in higher density;on the other hand, they can act as the heterogeneous nucleation centers for the enhanced oxygen precipitation. Likewise,the germanium and carbon related complexes can be also formed during the RTA process,which also promote oxygen precipitation during the subsequent anneals.With the theoretical and experimental works,a qualitative model for elucidating the mechanism for the effects of germanium and carbon on the behaviors of microdefects(oxygen precipitate and void)in CZ silicon has been tentatively developed.
引文
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