化学机械抛光试验及其材料去除机理的研究
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摘要
上世纪六十年代，化学机械抛光技术开始应用于半导体材料工业。从此，化学机械抛光技术一直伴随着半导体技术的发展、特别是微电子行业的集成电路的发展而不断发展。目前，化学机械抛光技术已经运用于多种不同材料的精细抛光，例如：半导体材料、宝石、特殊用途的高光洁度光学玻璃等硬脆性材料。但是，迄今为止的研究并没有充分认识化学机械抛光的材料去除机理，特别是纳米尺度的抛光磨粒的性能以及单晶硅晶圆表面的微纳尺度的摩擦磨损性能等因素与材料去除机理之间的关系尚不清楚，相关的研究亦处于初始阶段。深入研究化学机械抛光过程的材料去除机理，研究抛光工艺的各技术要素：抛光压力、速度、抛光液的化学成分、抛光液中的磨粒等对抛光过程中的材料去除的作用，将有助于优选抛光工艺参数，从而更好地控制抛光过程，获得高光洁、无损伤的表面。
首先，本论文建立了考虑磨粒变形的化学机械抛光材料去除模型。通过计算磨粒的变形量，更加精确地计算出磨粒压入晶圆表面的深度。由这个压入深度，计算出单位时间内磨粒在晶圆表面去除的材料体积。同时，磨粒压入晶圆表面的深度决定了抛光后的晶圆表面质量。进一步研究决定磨粒变形量的因素：施加在磨粒上的来自晶圆和抛光垫的力、以及磨粒自身的因素：磨粒的尺寸、硬度、弹性模量等，得出：①新的考虑磨粒变形因素的化学机械抛光材料去除模型可以更加准确地预测材料去除率；②在纳米级的材料去除研究中，磨粒本身的尺寸在纳米尺度，此时磨粒的变形量不可忽视；③硬度值低的磨粒，磨粒更易变形，磨粒在抛光表面形成的擦划沟槽的深度更浅，意味着抛光后表面粗糙度值更小。
其次，本论文研究不同润滑条件下的单晶硅晶圆化学机械抛光的材料去除机理。基于纳米划痕实验，研究了抛光力与摩擦系数之间的关系以及抛光速度与摩擦系数之间的关系。计算划痕的长度、宽度和深度得出材料的去除率，从而得出抛光力与材料去除率之间的关系以及抛光速度与材料去除率之间的关系。实验研究的结果表明：在纳米尺度条件下，抛光力与材料去除率成正比，而抛光速度的提高并不能一味提高材料去除率；抛光界面的不同润滑条件决定着材料去除机理的不同：在干摩擦条件下，单晶硅晶圆在化学机械抛光过程中表现出粘着磨损的材料去除机理；在过氧化氢润滑条件下，材料的去除表征出一种因微裂纹而导致剥落的材料去除机理；而在去离子水的润滑条件下，纳米划痕实验中的单次磨痕的最小深度为0.063nm，充分证明了此条件下的单分子层的材料去除机理。
再者，本论文研究了单晶硅晶圆化学机械抛光后表面层及亚表层的损伤。利用中国科学院苏州纳米技术研究所的先进设备条件，成功制备单晶硅晶圆表面纳米划痕的透射电子显微镜分析用试样，并对试样进行高分辨的透射电子显微分析。通过此项研究，掌握了水润滑和过氧化氢润滑条件下的单晶硅晶圆纳米划痕实验得到的划痕表面层及亚表层在不同的力的作用下以及在不同的材料去除速度下产生的晶格畸变、相变等晶体缺陷的规律。
进一步的研究，通过对比水润滑条件下和过氧化氢润滑条件下的划痕表面层及亚表层的晶体结构，得到：抛光液中的化学成分与被抛光材料的表面发生化学反应后，材料界面化学性能发生变化，易于被机械能去除；但是，过度的化学反应则将更易带来表面层及亚表层损伤。研究结果充分证明了化学机械抛光过程中抛光力和抛光液中的化学成分的相互影响关系亦即在此过程中的机械能和化学能的协同作用，以及这种协同作用的演变对化学机械抛光工艺结果的影响。在水润滑和过氧化氢润滑条件下的单晶硅晶圆表面的纳米划痕实验中，当材料去除速度保持不变，抛光力在30mN至70mN之间，摩擦界面发生摩擦化学反应，并产生具有润滑作用的润滑膜。由此可见，在这样的条件下机械作用可以实现加速或者说具有促进化学反应的作用。这样，在实现机械能与化学作用的平衡、机械能促进化学反应、机械能控制化学能的条件下，化学机械抛光的能量消耗将最少、材料消耗最低，而材料去除率则可以达到最大值，表面层及亚表层无损伤、少无化学污染。
在化学机械抛光过程中通过调整工艺的机械和化学参数可以实现机械能对化学能的控制。研究成果为少无化学污染的绿色无损伤精密抛光技术奠定了基础，为最终实现清洁的机械能为主导的、高效、绿色的精密抛光，获得理想的抛光表面提供了理论和实践依据。
Since1960s, the chemical mechanical polishing has been applied in the semiconductorindustry. From that time, the chemical mechanical polishing technology has been developingwith the development of the semiconductor industry, especially with the development ofintegrated circuit in the microelectronics industry. Currently, the chemical mechanicalpolishing technology has been widely used for precision polishing of many different materials,for example, hard and fragile material like: semiconductor material, jewel, optic glass withsuper cleanness requirements for special utilization. However, the research in this area by nowdoes not fully recognize the material removal mechanism of the chemical mechanicalpolishing, the relationship between the nanoscale sized abrasive particle, the micro-andnano-scale frictional and wear properties of single crystal silicon wafer and the materialremoval mechanism is not clearly understood, the related research is still in the beginningphase. Study on material removal mechanism in chemical mechanical polishing, study on thefunctions of these parameters of polishing load, speed, slurry chemical compositions, abrasiveparticles in the slurry, helps best select the polishing parameters, helps understand on thepolishing process deeply, it is conducive to well control and use this technology, to obtainhigh clean and non-damaged surface.
Firstly, this paper built the mathematic model on material removal with consideration ofthe deformation of abrasive particle. Through calculation of the deformation of the abrasiveparticle, it is possible to calculate more precisely the depth of the abrasive particle embeddinginto the surface of the silicon wafer. With this depth, the removed material per unit time by theabrasive particle can be obtained. Simultaneously, the depth of the abrasive particleembedding into the surface of the silicon wafer determines the surface quality of the polishedsilicon wafer. Further study on the elements which are influencing the deformation of theabrasive particle, like: the size of the particle, its hardness, its elastic Young’s modulus, etc.The following results can be achieved:①using the new model, the material removal ratecan be more precisely predicted, it is very close to the material removal rate obtained from theexperiments in this paper;②in the nanometer sized material removal research, the sizes ofthe particle itself is in nanoscale, its deformation can’t be neglected;③the particle which isin a less hardness is more easily deformed by the outside force, the ploughed groove on thepolished surface is more shallow, it means that the roughness of polished surface is more less.
Secondly, this paper studies the material removal mechanism of chemical mechanicalpolishing of single crystal silicon wafer under different lubrication conditions. By means ofnanoscale scratching experiments, the relationship between the polishing load and frictioncoefficient and the relationship between the polishing speed and the friction coefficient havebeen studied. The material removal rate is able to be obtained by calculation of the length,width and depth of the scratched groove, in this way, the relationship between the polishedload and the material removal rate and the relationship between the polishing speed and thematerial removal rate are obtained. The results from the experimental studies show that, in the nanoscale the material removal rate is direct proportional to the polishing load, but theincreasing of the polishing speed does not means that a higher material removal rate is surelyto be reached. At the same time, the different lubrication conditions in the polished interfacesinduce different material removal mechanisms: in the dry frictional condition, the singlecrystal silicon wafer presents a kind of material removal mechanism of adhesion wear in thechemical mechanical polishing; under the hydrogen peroxide lubrication, the materialremoval is a kind of material spalling which is induced by the micro cracks; under thedeionized water lubrication, the smallest scratching depth is0.0063nanometer in thenanoscale scratching experiments, it proves that the material removal mechanism is amolecular-scale material removal.
Moreover, the reseach work of this paper also explored a novel research method forstudy on the surface and subsurface damage of polished single crystal silicon wafer. Byutilizing the modern devices and equipments in Suzhou Nano Science and TechnologyResearch Institute of China Academy of Sciences, the specimen of the single crystal siliconwafer with the nanoscale scratching from the nanoscale scratching experiments aresuccessfully prepared for the further study by the Transmission Electron Microscopy, and thestudy in a high resolution scope has been successfully carried out. Through this study, the lawof the damages and disfigurements like aberration and phase changing of crystal lattice etc.which are caused in the nanoscale scratching experiments in the surface and subsurface ofsingle crystal silicon wafer under different loads and speeds in the deionized water lubricationand hydrogen peroxide lubrication conditions has been mastered.
Further study on the crystal structure of the nanoscale scratched surface and subsurfaceunder deionized water lubrication and hydrogen peroxide lubrication by comparison, reachesthat the chemical composition in the slurry reacts with the polishing surface material, thechemical features of the surface have been changed, the surface material becomes easy to beremoved by the mechanical effects; but, excessive chemical reactions will easily bring surfacedamage and subsurface damage also. The research results have proven that the synergiceffects of mechanical function and chemical function in the chemical mechanical polishing,and its influence to the outcome of the chemical mechanical polishing by the evolvement ofthe synergy of mechanical effects and chemical effects. In the nanoscale scratchingexperiments with deionized water lubrication and hydrogen peroxide lubrication, thefrictional chemical reactions happened in the frictional interface, and generate lubricatingfilms when the sliding speed unchanging and the load is between30mN and70mN. Hence,under this condition, mechanical effects can accelerate, or in other words, can expedite thechemical effects. Thus, the consumption of total energy and material will reach the minimumand the material removal rate may reach the maximum, no surface damage and no subsurfacedamage, less or no chemical pollution when the balance of mechanical energy and chemicaleffects, mechanical energy accelerating chemical effects, mechanical effects controlling thechemical effects are realized.
Through the adjustment of mechanical and chemical parameters in the chemicalmechanical polishing processes, the mechanical effects dominating chemical effects may berealized. This research result in this dissertation built the foundation of less/non chemical pollution, green, undamaged and precise polishing technology, and the results providedsupplied the theoretical and experimental foundation for the clean mechanical effectsdominated high efficient green precise polishing so as to obtain the ideal surface from thechemical mechanical polishing.
首先，本论文建立了考虑磨粒变形的化学机械抛光材料去除模型。通过计算磨粒的变形量，更加精确地计算出磨粒压入晶圆表面的深度。由这个压入深度，计算出单位时间内磨粒在晶圆表面去除的材料体积。同时，磨粒压入晶圆表面的深度决定了抛光后的晶圆表面质量。进一步研究决定磨粒变形量的因素：施加在磨粒上的来自晶圆和抛光垫的力、以及磨粒自身的因素：磨粒的尺寸、硬度、弹性模量等，得出：①新的考虑磨粒变形因素的化学机械抛光材料去除模型可以更加准确地预测材料去除率；②在纳米级的材料去除研究中，磨粒本身的尺寸在纳米尺度，此时磨粒的变形量不可忽视；③硬度值低的磨粒，磨粒更易变形，磨粒在抛光表面形成的擦划沟槽的深度更浅，意味着抛光后表面粗糙度值更小。
其次，本论文研究不同润滑条件下的单晶硅晶圆化学机械抛光的材料去除机理。基于纳米划痕实验，研究了抛光力与摩擦系数之间的关系以及抛光速度与摩擦系数之间的关系。计算划痕的长度、宽度和深度得出材料的去除率，从而得出抛光力与材料去除率之间的关系以及抛光速度与材料去除率之间的关系。实验研究的结果表明：在纳米尺度条件下，抛光力与材料去除率成正比，而抛光速度的提高并不能一味提高材料去除率；抛光界面的不同润滑条件决定着材料去除机理的不同：在干摩擦条件下，单晶硅晶圆在化学机械抛光过程中表现出粘着磨损的材料去除机理；在过氧化氢润滑条件下，材料的去除表征出一种因微裂纹而导致剥落的材料去除机理；而在去离子水的润滑条件下，纳米划痕实验中的单次磨痕的最小深度为0.063nm，充分证明了此条件下的单分子层的材料去除机理。
再者，本论文研究了单晶硅晶圆化学机械抛光后表面层及亚表层的损伤。利用中国科学院苏州纳米技术研究所的先进设备条件，成功制备单晶硅晶圆表面纳米划痕的透射电子显微镜分析用试样，并对试样进行高分辨的透射电子显微分析。通过此项研究，掌握了水润滑和过氧化氢润滑条件下的单晶硅晶圆纳米划痕实验得到的划痕表面层及亚表层在不同的力的作用下以及在不同的材料去除速度下产生的晶格畸变、相变等晶体缺陷的规律。
进一步的研究，通过对比水润滑条件下和过氧化氢润滑条件下的划痕表面层及亚表层的晶体结构，得到：抛光液中的化学成分与被抛光材料的表面发生化学反应后，材料界面化学性能发生变化，易于被机械能去除；但是，过度的化学反应则将更易带来表面层及亚表层损伤。研究结果充分证明了化学机械抛光过程中抛光力和抛光液中的化学成分的相互影响关系亦即在此过程中的机械能和化学能的协同作用，以及这种协同作用的演变对化学机械抛光工艺结果的影响。在水润滑和过氧化氢润滑条件下的单晶硅晶圆表面的纳米划痕实验中，当材料去除速度保持不变，抛光力在30mN至70mN之间，摩擦界面发生摩擦化学反应，并产生具有润滑作用的润滑膜。由此可见，在这样的条件下机械作用可以实现加速或者说具有促进化学反应的作用。这样，在实现机械能与化学作用的平衡、机械能促进化学反应、机械能控制化学能的条件下，化学机械抛光的能量消耗将最少、材料消耗最低，而材料去除率则可以达到最大值，表面层及亚表层无损伤、少无化学污染。
在化学机械抛光过程中通过调整工艺的机械和化学参数可以实现机械能对化学能的控制。研究成果为少无化学污染的绿色无损伤精密抛光技术奠定了基础，为最终实现清洁的机械能为主导的、高效、绿色的精密抛光，获得理想的抛光表面提供了理论和实践依据。
Since1960s, the chemical mechanical polishing has been applied in the semiconductorindustry. From that time, the chemical mechanical polishing technology has been developingwith the development of the semiconductor industry, especially with the development ofintegrated circuit in the microelectronics industry. Currently, the chemical mechanicalpolishing technology has been widely used for precision polishing of many different materials,for example, hard and fragile material like: semiconductor material, jewel, optic glass withsuper cleanness requirements for special utilization. However, the research in this area by nowdoes not fully recognize the material removal mechanism of the chemical mechanicalpolishing, the relationship between the nanoscale sized abrasive particle, the micro-andnano-scale frictional and wear properties of single crystal silicon wafer and the materialremoval mechanism is not clearly understood, the related research is still in the beginningphase. Study on material removal mechanism in chemical mechanical polishing, study on thefunctions of these parameters of polishing load, speed, slurry chemical compositions, abrasiveparticles in the slurry, helps best select the polishing parameters, helps understand on thepolishing process deeply, it is conducive to well control and use this technology, to obtainhigh clean and non-damaged surface.
Firstly, this paper built the mathematic model on material removal with consideration ofthe deformation of abrasive particle. Through calculation of the deformation of the abrasiveparticle, it is possible to calculate more precisely the depth of the abrasive particle embeddinginto the surface of the silicon wafer. With this depth, the removed material per unit time by theabrasive particle can be obtained. Simultaneously, the depth of the abrasive particleembedding into the surface of the silicon wafer determines the surface quality of the polishedsilicon wafer. Further study on the elements which are influencing the deformation of theabrasive particle, like: the size of the particle, its hardness, its elastic Young’s modulus, etc.The following results can be achieved:①using the new model, the material removal ratecan be more precisely predicted, it is very close to the material removal rate obtained from theexperiments in this paper;②in the nanometer sized material removal research, the sizes ofthe particle itself is in nanoscale, its deformation can’t be neglected;③the particle which isin a less hardness is more easily deformed by the outside force, the ploughed groove on thepolished surface is more shallow, it means that the roughness of polished surface is more less.
Secondly, this paper studies the material removal mechanism of chemical mechanicalpolishing of single crystal silicon wafer under different lubrication conditions. By means ofnanoscale scratching experiments, the relationship between the polishing load and frictioncoefficient and the relationship between the polishing speed and the friction coefficient havebeen studied. The material removal rate is able to be obtained by calculation of the length,width and depth of the scratched groove, in this way, the relationship between the polishedload and the material removal rate and the relationship between the polishing speed and thematerial removal rate are obtained. The results from the experimental studies show that, in the nanoscale the material removal rate is direct proportional to the polishing load, but theincreasing of the polishing speed does not means that a higher material removal rate is surelyto be reached. At the same time, the different lubrication conditions in the polished interfacesinduce different material removal mechanisms: in the dry frictional condition, the singlecrystal silicon wafer presents a kind of material removal mechanism of adhesion wear in thechemical mechanical polishing; under the hydrogen peroxide lubrication, the materialremoval is a kind of material spalling which is induced by the micro cracks; under thedeionized water lubrication, the smallest scratching depth is0.0063nanometer in thenanoscale scratching experiments, it proves that the material removal mechanism is amolecular-scale material removal.
Moreover, the reseach work of this paper also explored a novel research method forstudy on the surface and subsurface damage of polished single crystal silicon wafer. Byutilizing the modern devices and equipments in Suzhou Nano Science and TechnologyResearch Institute of China Academy of Sciences, the specimen of the single crystal siliconwafer with the nanoscale scratching from the nanoscale scratching experiments aresuccessfully prepared for the further study by the Transmission Electron Microscopy, and thestudy in a high resolution scope has been successfully carried out. Through this study, the lawof the damages and disfigurements like aberration and phase changing of crystal lattice etc.which are caused in the nanoscale scratching experiments in the surface and subsurface ofsingle crystal silicon wafer under different loads and speeds in the deionized water lubricationand hydrogen peroxide lubrication conditions has been mastered.
Further study on the crystal structure of the nanoscale scratched surface and subsurfaceunder deionized water lubrication and hydrogen peroxide lubrication by comparison, reachesthat the chemical composition in the slurry reacts with the polishing surface material, thechemical features of the surface have been changed, the surface material becomes easy to beremoved by the mechanical effects; but, excessive chemical reactions will easily bring surfacedamage and subsurface damage also. The research results have proven that the synergiceffects of mechanical function and chemical function in the chemical mechanical polishing,and its influence to the outcome of the chemical mechanical polishing by the evolvement ofthe synergy of mechanical effects and chemical effects. In the nanoscale scratchingexperiments with deionized water lubrication and hydrogen peroxide lubrication, thefrictional chemical reactions happened in the frictional interface, and generate lubricatingfilms when the sliding speed unchanging and the load is between30mN and70mN. Hence,under this condition, mechanical effects can accelerate, or in other words, can expedite thechemical effects. Thus, the consumption of total energy and material will reach the minimumand the material removal rate may reach the maximum, no surface damage and no subsurfacedamage, less or no chemical pollution when the balance of mechanical energy and chemicaleffects, mechanical energy accelerating chemical effects, mechanical effects controlling thechemical effects are realized.
Through the adjustment of mechanical and chemical parameters in the chemicalmechanical polishing processes, the mechanical effects dominating chemical effects may berealized. This research result in this dissertation built the foundation of less/non chemical pollution, green, undamaged and precise polishing technology, and the results providedsupplied the theoretical and experimental foundation for the clean mechanical effectsdominated high efficient green precise polishing so as to obtain the ideal surface from thechemical mechanical polishing.
引文
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