核壳结构SiO_2/CeO_2、PS/CeO_2复合微球的可控合成及其CMP性能研究
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摘要
化学机械抛光/平坦化(Chemical Mechanical Polishing/Planarization, CMP)技术被广泛应用于超大规模集成电路和精密光学系统制造过程中的平坦化工艺,其中磨料的性质对于CMP质量具有十分重要的影响。为了提高SiO2-CMP质量,本文设计并可控合成了具有核壳结构的SiO2/Ce02和聚苯乙烯(PS)/CeO2复合微球,并讨论了复合磨料CMP机理。具体研究内容和结果如下：
以TEOS水解得到的单分散SiO2微球为内核,分别采用浸渍工艺和化学原位沉淀工艺制备了SiO2/CeO2复合微球,整个制备过程无需对SiO2微球进行表面处理。TEM和FESEM结果表明所得复合微球具有核壳结构,CeO2纳米颗粒均匀包覆在SiO2内核表面。XPS分析结果显示,复合微球样品中Ols (O-Si)和Si2p的结合能发生了明显的化学位移,推断CeO2颗粒与SiO2内核之间形成了Si-O-Ce键,两者产生化学键结合。复合微球表面CeO2壳厚(包覆量)可分别通过调整铈溶胶和反应液中硝酸铈的浓度进行控制。
进一步采用化学原位沉淀工艺制备了以PS为核、CeO2为壳的复合微球。首先用阴离子引发剂(KPS),通过无皂乳液聚合的方法制备了表面带负电荷的PS微球,利用带负电荷的PS微球与反应液中Ce3+之间的静电作用,以及HMT的缓慢水解过程,制备了具有不同内核尺寸和/或不同壳厚的核壳结构PS/CeO2复合微球。制备过程中无需对PS微球进行特殊的表面改性,也不需要加入其他乳化剂或稳定剂。利用TEM、FESEM以及TGA等手段对样品进行表征。通过调节反应条件,可控制复合微球的粒径在100～300 nm,Ce02壳厚在5-20 nm,复合微球中氧化铈的含量在30～70 wt%。
利用AFM测定了PS微球和PS/CeO2复合微球的力-位移曲线,根据Hertzain接触模型计算了样品的弹性模量,考察了复合微球的PS内核尺寸和/或CeO2壳厚对样品弹性模量的影响规律。计算结果表明,PS微球的平均弹性模量为2.80 GPa,其数值略低于聚苯乙烯块体材料的弹性模量。当复合微球的CeO2壳厚相当时,其平均弹性模量随着PS内核尺寸的增大而增大；当复合微球中PS内核一定时,样品的平均弹性模量随着CeO2壳厚的增大而增大。与纯氧化铈相比,PS/CeO2复合微球的弹性模量明显更偏向于PS微球,整体上表现出了非刚性的力学特征。
与传统的纳米SiO2磨料和纳米CeO2磨料相比,SiO2/CeO2复合磨料对砷化镓晶片、石英玻璃以及二氧化硅介质层表现出更好的抛光性能,抛光后表面无明显划痕,表面粗糙度RMS值分别为1.09、0.346和0.428 nm。由于SiO2/CeO2复合磨料特殊的核壳包覆结构,能够保证壳层中粒径约5～10 nm的CeO2纳米颗粒与晶片表面直接接触,一定程度上避免了传统纳米磨料产生硬团聚从而造成抛光表面的机械损伤,使得抛光质量得以提高。
核壳结构PS/CeO2复合磨料能够有效地提高SiO2-CMP质量,且复合磨料的微观结构对抛光后表面形貌有明显影响。本实验范围内,当复合磨料中CeO2壳厚一定时,随着PS内核尺寸的减小,表面粗糙度随之降低,抛光后表面的微观轮廓曲线更趋于平缓；当复合磨料中PS内核尺寸一定时,随着CeO2壳厚的减小,表面粗糙度呈先降低后增大的趋势。SiO2-CMP质量的提高可能归因于复合微球的非刚性力学特性,PS/CeO2复合磨料与晶片表面接触过程中可能发生一定的弹性变形,增大磨料与晶片之间的接触面积,可以将抛光压力更加温和地传递给抛光表面,使得接触应力以及单个磨料在晶片表面的压入深度δW降低,因此不仅抛光表面粗糙度得以降低,而且还有利于减少划痕和亚表层损伤。考虑到抛光垫表面存在凹凸峰,复合磨料所特有的“弹簧状”状结构还有利于调节磨料粒子与晶片之间的接触状态,有利于提高抛光表面的平整度。
Chemical mechanical polishing/Planarization (CMP) is one of the most efficient planarization technologies in the manufacturing of ultra-large scale integration (ULSI) and precision optical devices. In CMP processes, abrasives in slurry play an important role in improving CMP performances, such as material removal rate (MRR), roughness, number of defects, and surface flatness. CMP performances depend on the choice of abrasives including type, morphology, size distribution and mechanical properties. In this dissertation, the silica/ceria (SiO2/CeO2) and polystyrene/ceria (PS/CeO2) composite microspheres with core-shell structure were synthesized by liquid phase method, and the SiO2-CMP performance were investigated. The obtained results are as follows.
SiO2/CeO2 composite microspheres with core-shell structure were prepared by immersion method and In-situ chemical precipitation method with tetraethyl orthosilicate (TEOS) as silica source and cerium nitrate hexahydrate as the cerium source, respectively. TEM and FESEM results showed the surfaces of SiO2 core were coated uniformly by CeO2 nanoparticles. XPS results showed the CeO2 (shell) was chemically bound with SiO2 (core), and as a result of Si—O—Ce was formed. The CeO2 shell thickness of composite microspheres could be controlled by adjusting the cerium ion concentration in the sol and the concentration of Ce(NO3)3·6H2O in the reaction solution, respectively.
A simple method was proposed to prepare PS/CeO2 composite microspheres without surface modification or addition of surfactant (stabilizer). Firstly, negative-charged polystyrene microspheres were prepared via soap-free emulsion polymerization by potassium peroxydisulfate (KPS, anionic) as initiator. Then, Ce3+ cations could be absorbed onto the surfaces of the negatively charged PS microspheres. Under slow hydrolyzing of HMT, the opposite-charged OH- was released in the solution. Ce3+ combined with OH- slowly hydrolyzed from HMT driven by electrostatic attraction. By using this method, PS/CeO2 composite microspheres with different core size and/or shell thickness could be obtained. The results indicated that the as-prepared core-shell structured composite microspheres (100-300 nm in diameter) possessed thin shell (5-20 nm) composed of CeO2 nanoparticles (particle diameter of 5-10 nm), and the final CeO2 contents of the composite microspheres ranged from 30 to 70 wt%.
Atomic force microscopy (AFM) was employed to probe the mechanical properties of PS microspheres and PS/CeO2 composite microspheres. On the basis of Hertz's theory of contact mechanics, elastic moduli were measured by the analysis of force-displacement curves captured on the microsphere samples. The average elastic modulus value of the PS microspheres was found to be approximately 2.8 GPa. The compressive modulus is slightly less than the moduli of polystyrene bulk materials. The PS core size and/or the CeO2 shell thickness affected the mechanical properties of composite microspheres. For a fixed PS core size or CeO2 shell thickness, the elastic modulus of composites increased with an increase of the CeO2 shell thickness or the PS core size, respectively. The elastic moduli of the composites displayed a significant shift from the value of pure CeO2 toward that of PS core. Compared with traditional inorganic particles, the as-prepared PS/CeO2 composite microspheres exhibited the especial non-rigid mechanical properties. This approach would provide fundamental insights into the actual role of organic/inorganic core/shell composite abrasives in CMP.
Compared with pure SiO2 and CeO2 abrasives, SiO2/CeO2 composite abrasives led to lower topographical variations as well as few scratches. The surface roughness (RMS) values of polished GaAs wafer, silica glass, and silicon oxide dielectric layer was 1.09, 0.346 and 0.428 nm, respectively. The as-prepared SiO2/CeO2 composite abrasives exhibited the core-shell structure, which could provide the direct contact between CeO2 nanoparticles and wafer. Such character could partially avoid the mechanical damage induced by hard agglomerates, which could improve the CMP performance.
The CMP results showed that the PS/CeO2 composite abrasives were beneficial to elimination of scratches and decrease surface roughness (RMS) in the process of SiO2-CMP. In addition, there was an obvious effect of core size and/or shell thickness of the composite abrasives on oxide CMP performance. At a fixed CeO2 shell thickness, the surface roughness values increased with an increase of PS core size. And for a given PS core, the surface roughness value decreased and then increased with the increase of CeO2 shell thickness. The improvement of CMP performance might be attributed to a synergistic effect of the core-shell structure. The spring-like effect coming from the elastic polymer core increased the contact area between wafer and abrasives and decreased the contact stress during CMP, which was in favor of reducing roughness and mechanical damage. Furthermore, assisted by the mechanical compliance coming from the elastic PS core, the planarity of wafer after CMP could also be enhanced. In addition, inorganic shell could improve the surface hardness of the polymer core and possessed an enhanced chemical activity of composite abrasives.
以TEOS水解得到的单分散SiO2微球为内核,分别采用浸渍工艺和化学原位沉淀工艺制备了SiO2/CeO2复合微球,整个制备过程无需对SiO2微球进行表面处理。TEM和FESEM结果表明所得复合微球具有核壳结构,CeO2纳米颗粒均匀包覆在SiO2内核表面。XPS分析结果显示,复合微球样品中Ols (O-Si)和Si2p的结合能发生了明显的化学位移,推断CeO2颗粒与SiO2内核之间形成了Si-O-Ce键,两者产生化学键结合。复合微球表面CeO2壳厚(包覆量)可分别通过调整铈溶胶和反应液中硝酸铈的浓度进行控制。
进一步采用化学原位沉淀工艺制备了以PS为核、CeO2为壳的复合微球。首先用阴离子引发剂(KPS),通过无皂乳液聚合的方法制备了表面带负电荷的PS微球,利用带负电荷的PS微球与反应液中Ce3+之间的静电作用,以及HMT的缓慢水解过程,制备了具有不同内核尺寸和/或不同壳厚的核壳结构PS/CeO2复合微球。制备过程中无需对PS微球进行特殊的表面改性,也不需要加入其他乳化剂或稳定剂。利用TEM、FESEM以及TGA等手段对样品进行表征。通过调节反应条件,可控制复合微球的粒径在100～300 nm,Ce02壳厚在5-20 nm,复合微球中氧化铈的含量在30～70 wt%。
利用AFM测定了PS微球和PS/CeO2复合微球的力-位移曲线,根据Hertzain接触模型计算了样品的弹性模量,考察了复合微球的PS内核尺寸和/或CeO2壳厚对样品弹性模量的影响规律。计算结果表明,PS微球的平均弹性模量为2.80 GPa,其数值略低于聚苯乙烯块体材料的弹性模量。当复合微球的CeO2壳厚相当时,其平均弹性模量随着PS内核尺寸的增大而增大；当复合微球中PS内核一定时,样品的平均弹性模量随着CeO2壳厚的增大而增大。与纯氧化铈相比,PS/CeO2复合微球的弹性模量明显更偏向于PS微球,整体上表现出了非刚性的力学特征。
与传统的纳米SiO2磨料和纳米CeO2磨料相比,SiO2/CeO2复合磨料对砷化镓晶片、石英玻璃以及二氧化硅介质层表现出更好的抛光性能,抛光后表面无明显划痕,表面粗糙度RMS值分别为1.09、0.346和0.428 nm。由于SiO2/CeO2复合磨料特殊的核壳包覆结构,能够保证壳层中粒径约5～10 nm的CeO2纳米颗粒与晶片表面直接接触,一定程度上避免了传统纳米磨料产生硬团聚从而造成抛光表面的机械损伤,使得抛光质量得以提高。
核壳结构PS/CeO2复合磨料能够有效地提高SiO2-CMP质量,且复合磨料的微观结构对抛光后表面形貌有明显影响。本实验范围内,当复合磨料中CeO2壳厚一定时,随着PS内核尺寸的减小,表面粗糙度随之降低,抛光后表面的微观轮廓曲线更趋于平缓；当复合磨料中PS内核尺寸一定时,随着CeO2壳厚的减小,表面粗糙度呈先降低后增大的趋势。SiO2-CMP质量的提高可能归因于复合微球的非刚性力学特性,PS/CeO2复合磨料与晶片表面接触过程中可能发生一定的弹性变形,增大磨料与晶片之间的接触面积,可以将抛光压力更加温和地传递给抛光表面,使得接触应力以及单个磨料在晶片表面的压入深度δW降低,因此不仅抛光表面粗糙度得以降低,而且还有利于减少划痕和亚表层损伤。考虑到抛光垫表面存在凹凸峰,复合磨料所特有的“弹簧状”状结构还有利于调节磨料粒子与晶片之间的接触状态,有利于提高抛光表面的平整度。
Chemical mechanical polishing/Planarization (CMP) is one of the most efficient planarization technologies in the manufacturing of ultra-large scale integration (ULSI) and precision optical devices. In CMP processes, abrasives in slurry play an important role in improving CMP performances, such as material removal rate (MRR), roughness, number of defects, and surface flatness. CMP performances depend on the choice of abrasives including type, morphology, size distribution and mechanical properties. In this dissertation, the silica/ceria (SiO2/CeO2) and polystyrene/ceria (PS/CeO2) composite microspheres with core-shell structure were synthesized by liquid phase method, and the SiO2-CMP performance were investigated. The obtained results are as follows.
SiO2/CeO2 composite microspheres with core-shell structure were prepared by immersion method and In-situ chemical precipitation method with tetraethyl orthosilicate (TEOS) as silica source and cerium nitrate hexahydrate as the cerium source, respectively. TEM and FESEM results showed the surfaces of SiO2 core were coated uniformly by CeO2 nanoparticles. XPS results showed the CeO2 (shell) was chemically bound with SiO2 (core), and as a result of Si—O—Ce was formed. The CeO2 shell thickness of composite microspheres could be controlled by adjusting the cerium ion concentration in the sol and the concentration of Ce(NO3)3·6H2O in the reaction solution, respectively.
A simple method was proposed to prepare PS/CeO2 composite microspheres without surface modification or addition of surfactant (stabilizer). Firstly, negative-charged polystyrene microspheres were prepared via soap-free emulsion polymerization by potassium peroxydisulfate (KPS, anionic) as initiator. Then, Ce3+ cations could be absorbed onto the surfaces of the negatively charged PS microspheres. Under slow hydrolyzing of HMT, the opposite-charged OH- was released in the solution. Ce3+ combined with OH- slowly hydrolyzed from HMT driven by electrostatic attraction. By using this method, PS/CeO2 composite microspheres with different core size and/or shell thickness could be obtained. The results indicated that the as-prepared core-shell structured composite microspheres (100-300 nm in diameter) possessed thin shell (5-20 nm) composed of CeO2 nanoparticles (particle diameter of 5-10 nm), and the final CeO2 contents of the composite microspheres ranged from 30 to 70 wt%.
Atomic force microscopy (AFM) was employed to probe the mechanical properties of PS microspheres and PS/CeO2 composite microspheres. On the basis of Hertz's theory of contact mechanics, elastic moduli were measured by the analysis of force-displacement curves captured on the microsphere samples. The average elastic modulus value of the PS microspheres was found to be approximately 2.8 GPa. The compressive modulus is slightly less than the moduli of polystyrene bulk materials. The PS core size and/or the CeO2 shell thickness affected the mechanical properties of composite microspheres. For a fixed PS core size or CeO2 shell thickness, the elastic modulus of composites increased with an increase of the CeO2 shell thickness or the PS core size, respectively. The elastic moduli of the composites displayed a significant shift from the value of pure CeO2 toward that of PS core. Compared with traditional inorganic particles, the as-prepared PS/CeO2 composite microspheres exhibited the especial non-rigid mechanical properties. This approach would provide fundamental insights into the actual role of organic/inorganic core/shell composite abrasives in CMP.
Compared with pure SiO2 and CeO2 abrasives, SiO2/CeO2 composite abrasives led to lower topographical variations as well as few scratches. The surface roughness (RMS) values of polished GaAs wafer, silica glass, and silicon oxide dielectric layer was 1.09, 0.346 and 0.428 nm, respectively. The as-prepared SiO2/CeO2 composite abrasives exhibited the core-shell structure, which could provide the direct contact between CeO2 nanoparticles and wafer. Such character could partially avoid the mechanical damage induced by hard agglomerates, which could improve the CMP performance.
The CMP results showed that the PS/CeO2 composite abrasives were beneficial to elimination of scratches and decrease surface roughness (RMS) in the process of SiO2-CMP. In addition, there was an obvious effect of core size and/or shell thickness of the composite abrasives on oxide CMP performance. At a fixed CeO2 shell thickness, the surface roughness values increased with an increase of PS core size. And for a given PS core, the surface roughness value decreased and then increased with the increase of CeO2 shell thickness. The improvement of CMP performance might be attributed to a synergistic effect of the core-shell structure. The spring-like effect coming from the elastic polymer core increased the contact area between wafer and abrasives and decreased the contact stress during CMP, which was in favor of reducing roughness and mechanical damage. Furthermore, assisted by the mechanical compliance coming from the elastic PS core, the planarity of wafer after CMP could also be enhanced. In addition, inorganic shell could improve the surface hardness of the polymer core and possessed an enhanced chemical activity of composite abrasives.
引文
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