Investigation of pad wear in CMP with swing-arm conditioning and uniformity of material removal

Chemical mechanical polishing (CMP) process plays the role of planarizing and smoothing the uneven layers after the material deposition process in the semiconductor industry. In this process, pad conditioning using a diamond disk is inevitable to attain a high material removal rate (MRR) and to ensure the stability of the process. Pad conditioning is performed for providing uniform surface roughness and opening up the glazed surfaces of the polishing pad. However, the uneven pad wear resulting from pad conditioning leads to changes in the uniformity of MRR and productivity of the device. In this study, we investigate the pad wear profile after swing-arm conditioning of the pad, based on measurements performed using a pad measurement system (PMS). Conditioning experiments are conducted with seven cases of profiles of the conditioner's duration time (PCDT). In all the cases, “W”-shaped pad profiles are generated through swing-arm conditioning. It is observed that a concave-shaped PCDT results in the lowest value of maximum pad wear rate. The average depth of pad wear (h_avg) is mainly related to the MRR, and the maximum depth of pad wear (h_max) and the horizontal distance from the wafer center to the position (e) where the maximum pad wear occurs affect the within-wafer non-uniformity (WIWNU). A concave-shaped PCDT results in longer life of the polishing pad by minimizing the variation in pad wear. This paper can provide a technical assistance in selecting the conditioning recipe and improving the lifetime of the polishing pad in the CMP process.     

Nature and removal of the modified layer in Cu CMP with ferric nitrate as oxidizer

Chemical mechanical polishing (CMP) has been introduced in the semiconductor manufacturing industry in order to achieve global planarization of wafer surfaces. Lately, copper has replaced aluminum for its better electrical and mechanical properties.Cu CMP consists in the transformation of the copper surface layer to copper oxide, which is then removed by alumina abrasive particles. The oxidizer is the chemical agent that transforms the copper into copper oxide.We have been studying the influence of ferric nitrate as oxidizer on the copper CMP.We evaluated the nature of the copper oxide with XPS observation. We found it was cuprous oxide (Cu₂O) that was actually removed by the abrasive particles.We observed that the removal rate increased with the oxidizer concentration for low concentrations, but was almost constant for higher concentrations.We also evaluated what becomes of the polishing residues for short time processes, once they are removed from the surface. The remaining copper particles are too small to be responsible for any posterior damage of the surface.     

Prediction of the surface roughness and material removal rate in chemical mechanical polishing of single-crystal SiC via a back-propagation neural network

Chemical mechanical polishing (CMP) is a common method for realising the global planarisation and polishing of single-crystal SiC and other semiconductor substrates. The strong oxidant hydroxyl radicals (·OH) generated by the Fenton reaction can effectively oxidise and corrode the SiC substrate, and are thus used to improve the material removal rate (MRR) and surface roughness (Ra) after polishing of SiC during CMP. Therefore, it is necessary to study the material removal mechanism in detail. Based on the modified Preston equation, the effects of the CMP process parameters on the MRR and Ra after polishing of SiC and their relationship were studied, and a prediction model of the CMP process parameters, MRR, and Ra after polishing was also established based on a back-propagation neural network. The MRR initially increased and then decreased, and the Ra after polishing initially decreased and then increased, with increasing FeSO₄ concentration, H₂O₂ concentration, and pH value. The MRR continuously increased with increasing abrasive particle size, abrasive concentration, polishing pressure, and polishing speed. However, the Ra continuously decreased with increasing abrasive particle size and abrasive concentration, increased with increasing polishing pressure, and initially decreased and then increased with increasing polishing speed. The established prediction model could accurately predict the relationship between the process parameters, MRR and Ra after polishing in CMP (relative prediction error of less than 10%), which could provide a theoretical basis for CMP of SiC.     

Electrochemical Analysis of the Slurry Composition for Chemical Mechanical Polishing of Flexible Stainless-Steel Substrates

The surface quality of the stainless steel affects the efficiency of flexible photovoltaics. Chemical mechanical polishing (CMP) is a finishing process that is used to prepare substrates for electronic devices. The CMP slurry composition is an important factor because additives in the slurry generally improve the polishing performance. However, it is limited to find the optimum conditions for the slurry by only experimental approaches. Thus, this study uses electrochemical analysis and friction monitoring to examine the effects of the abrasive, oxidizer, chelating agent, and pH. Electrochemical and monitoring analysis are useful for validating predictions and understanding interactions between the slurry and the stainless steel surface. Good correspondence was found between the predictions and the polishing results in more accurate. The corrosion rate (CR) obtained from the potentiodynamic polarization curve is proportional to the experimental results, as is the behavior of the curve and the coefficient of friction (COF). After only 3 min CMP, the best performing slurry (abrasive 39 wt %, oxalic acid 1 wt %, H₂O₂ 0.03 wt %, pH 1.5) improved the surface quality of 304 stainless steel by 4 nm. As a result, the proposed methods could help reduce the risks involved in stainless steel CMP slurry and these results could provide a reference for optimizing CMP slurry for flexible 304 stainless steel substrates.     

Polishing tool with phyllotactic distributed through-holes for photochemically combined mechanical polishing of N-type gallium nitride wafers

In this work, we further developed the photochemically combined mechanical polishing (PCMP) method for finishing N-type gallium nitride (GaN) wafers. A core improvement is to design a novel polishing tool with phyllotactic distributed through-holes, through which the wafer surface underneath through-holes can receive ultraviolet (UV)-light for the photochemical oxidation, while the rest parts undergo mechanical polishing. During PCMP, the co-rotation of the wafer and polishing tool allows the wafer surface to undergo the uniform and high-frequency conversion of oxidation and polishing. Based on the designed PCMP system and apparatus, the fundamental issues arising from such an alternate processing mode, which is different from the parallel mode of conventional chemical mechanical polishing (CMP), were investigated. Results show that the technical features of PCMP depend on the nature of the photochemical oxidation of wafers themselves if the mechanical polishing procedure can sufficiently remove oxides in time. The material removal rate (MRR) is inversely proportional to the dislocation density of wafers. Under acidic conditions, the oxidation proceeds by the GaN monocrystal step orientation, allowing PCMP to clear surface/subsurface damages (SSDs) and to prepare step-terrace structures on the wafer surface. When the polishing solution (pH = 1.5) includes 0.1 M K₂S₂O₈ oxidants and 10 wt% SiO₂ abrasives, the surface roughness Sa attains 0.21 nm in 10 × 10 μm², and the MRR reaches 275.3 nm/h. The present study shows that the phyllotactic distributed through-hole array structure designed for polishing tools offers rich possibilities for the innovation of polishing technologies combining with various oxidation approaches.     

超细氧化铝表面改性及其抛光特性

在化学机械抛光（CMP）中，为了提高氧化铝磨料分散稳定性和防止团聚，利用丙烯酰氯对超细氧化铝进行了表面改性，并用XPS、激光粒度仪、SEM对其进行表征，结果表明改性后的超细氧化铝分散性明显提高。研究了改性后超细氧化铝在数字光盘玻璃基片中的化学机械抛光特性，即外加压力、抛光时间和下盘转速对玻璃基片去除量的影响,并对其CMP机制进行了推断。结果表明，材料去除量随下盘转速、压力变化趋势相近，即随着压力的增加或下盘转速的提高，材料去除量先增大后减小；随抛光时间延长，抛光初期材料去除量增加较快，但在后段时间内去除量增加趋势趋于平缓。     

计算机硬磁盘CMP中抛光工艺参数对去除率的影响

对于计算机硬磁盘的生产,为了最大限度地提高盘片生产量,降低生产成本,要求化学机械抛光(chemieal mechanical polishing,简称CMP)中在保证优质表面质量情况下,实现最大去除量(Material Removal,简称MR)和去除率(Material Removal Rate,简称MRR)。本文讨论了硬盘片的化学机械抛光过程中的外加压力、转速和抛光时间对去除率的影响。实验采用含多种添加剂的纳米二氧化硅(SiO_2)胶体作为研磨液在双面抛光机上对镍磷敷镀铝镁合金基片进行精抛光。结果表明,不降低表面质量,MRR随着压力的增加而增大到一个最大值,随后随着压力继续增加而减小;增加抛光机下盘的转速将使MRR变大到一定值后再下降;增加抛光时间将使MR增大,而MRR变化是非线性的。     

Preparation of La-doped colloidal SiO2 composite abrasives and their chemical mechanical polishing behavior on sapphire substrates

Chemical mechanical polishing (CMP) has become a widely accepted global planarization technology. Abrasive is one of the key elements in CMP process. In order to enhance removal rate and improve surface quality of sapphire substrate, a series of novel La-doped colloidal SiO₂ composite abrasives were prepared by seed-induced growth method. The CMP performance of the La-doped colloidal SiO₂ composite abrasives on sapphire substrate were investigated using UNIPOL-1502 polishing equipment. The analyses on the surface of polished sapphire substrate indicate that slurries containing the La-doped colloidal SiO₂ composite abrasives achieve lower surface roughness, higher material removal rate than that of pure colloidal SiO₂ abrasive under the same testing conditions. Furthermore, the acting mechanism of the La-doped colloidal silica in sapphire CMP was investigated. X-ray photoelectron spectroscopy analysis shows that solid-state chemical reactions between La-doped colloidal SiO₂ abrasive and sapphire surface occur during CMP process, which can promote the chemical effect in CMP and lead to the improvement of material removal rate.     

The degradation of EBSD-patterns as a tool to investigate surface crystallized glasses and to identify glassy surface layers

Surface crystallized samples of glass-ceramics containing cordierite, rhombohedral BaAl₂B₂O₇ and fresnoite were analyzed using electron backscatter diffraction (EBSD). The first two materials were chosen because surface crystallized samples of these materials have previously been shown to contain crystals covered by a very thin layer of glass. In all materials, EBSD pattern degradation occurs if the step size of a scan is chosen to be small. It is shown that the minimum step size enabling an evaluable EBSD-scan increases notably, if the crystals are covered by a thin layer of glass. It is also shown that pattern degradation may be utilized to prove the existence of such a thin glass or otherwise thermally sensitive layer. This provides significant information concerning the nucleation process of glasses also with respect to nucleation theory of glass-ceramics. It is also possible to describe the quantity of crystalline surface covered by the thermally sensitive layer.     

Experimental investigation of process parameters for roll-type linear chemical mechanical polishing (Roll-CMP) system

The fabrication processes for electronic components are now demanding a higher degree of planarity for integration and multistacking, with chemical mechanical polishing (CMP) processes replacing conventional etching or mechanical polishing owing to their ability to attain global planarization. As CMP has been applied to more and more fields, new types of CMP machines have been developed. This study introduces a novel roll-type linear CMP (Roll-CMP) process that uses a line-contact material removal mechanism to for the polish flexible substrates, and examines the effect of the process parameters on the material removal rate (MRR) and its nonuniformity (NU). The parameters affecting the Roll-CMP process include down force, roll speed, table feed rate, slurry flow rate, slurry temperature, and the table oscillation length. Increasing the down force, roll speed, slurry flow rate, and slurry temperature resulted in a high average MRR (MRR_avg). Further, the MRR_avg was found to decrease with an increase in the oscillation length because of the effect of the polishing area. A large down force, high roll speed, high table feed rate, and high slurry flow rate were effective for reducing the NU. These results will be helpful for understanding the newly developed Roll-CMP process.     

High precision chemical mechanical polishing of highly-boron-doped Si wafer used for epitaxial substrate

The surface waviness with concentric circular pattern is generated on highly-boron-doped Si wafer by chemical–mechanical polishing (CMP) with amine system polishing slurry. To investigate the generation mechanism of the waviness, the mechanical and chemical characteristics were clarified using the silicon crystal samples with various boron concentration level ranging from 2.9 × 10¹⁷ cm⁻³ to 1.3 × 10²⁰ cm⁻³. The conventional silicon substrate used as epitaxial wafer has boron concentration of about 2.5 × 10¹⁸ cm⁻³, a region at which the radical change of etching rate is induced with amine system chemical reagent. The mechanical micro-hardness of highly-boron-doped Si is 30% higher than that of lightly-doped Si. It is found that SiB bond in crystal lattice is firmed up and stabilized for mechanical stress and chemical reaction. To cancel the difference in CMP rate based on boron concentration deviation, increasing the mechanical action in CMP was proposed and performed. The precision CMP was performed using the harder polishing pad and a smooth surface without waviness was obtained.     

Effects of pH and Oxidizer on Chemical Mechanical Polishing of AISI 1045 Steel

AISI 1045 steel has been widely used as the substrate for thin film deposition. In some cases, an ultra-smooth surface of AISI 1045 steel is needed and is even indispensible for the satisfactory deposition of thin film. In this paper, chemical mechanical polishing technique was employed to prepare the ultra-smooth surface of AISI 1045 steel. The effects of pH and H₂O₂ on the polishing performance of AISI 1045 steel were investigated. It is revealed that, with the increase of pH, the material removal rate (MRR) and the static etching rate (SER) of AISI 1045 steel gradually decrease due to the formation of passive iron oxides on the top surface, and thus the surface quality gradually improves. At pH 4.00, with the addition of H₂O₂, the SER of AISI 1045 steel is further suppressed; while the MRR of AISI 1045 steel first dramatically increases due to the formation of porous iron oxides with relatively low mechanical strength on the surface when the H₂O₂ concentration increases from 0 to 0.01 wt%, and then decreases since the porous iron oxides gradually grow compact when the H₂O₂ concentration further increases. The increase of the compactness of the iron oxides might be attributed to the crystallization of γ-FeOOH into α-FeOOH and even into α-Fe₂O₃ and the resulting polymerization of the amorphous iron oxides.     

TWO STEPS CHEMICAL-MECHANICAL POLISHING OF RIGID DISK SUBSTRATE TO GET ATOM-SCALE PLANARIZATION SURFACE

In order to get atomic smooth rigid disk substrate surface, ultra-fined alumina slurry and nanometer silica slurry are prepared, and two steps chemical-mechanical polishing (CMP) of rigid disk substrate in the two slurries are studied. The results show that, during the first step CMP in the alumina slurry, a high material removal rate is reached, and the average roughness (Ra) and the average waviness (Wa) of the polished surfaces can be decreased from previous 1.4 nm and 1.6 nm to about 0.6 nm and 0.7 nm, respectively. By using the nanometer silica slurry and optimized polishing process parameters in the second step CMP, the Ra and the Wa of the polished surfaces can be further reduced to 0.038 nm and 0.06 nm, respectively. Atom force microscopy (APM) analysis shows that the final polished surfaces are ultra-smooth without micro-defects.     

添加剂对电诱导GaN晶片化学机械抛光的影响

为研究添加剂对氮化镓(GaN)晶片化学机械抛光(CMP)材料去除率的影响,采用直流电源对n型GaN晶片进行电化学刻蚀,利用X射线光电子能谱(XPS)和原子力显微镜(AFM)研究电诱导辅助下GaN晶片CMP过程中,对苯二甲酸(PTA)和H 2O 2对其材料去除的影响。结果表明:在添加电流的条件下,随着H 2O 2体积分数增大,GaN材料去除率先升高后降低;随着PTA浓度的增加,GaN材料去除率先增加后减少;在H 2O 2体积分数为4%,PTA浓度为10 mmol/L条件下,GaN晶片的化学机械抛光材料去除率最高,为693.77 nm/h,抛光后GaN晶片表面粗糙度为0.674 nm;通过XPS分析,电诱导后GaN晶片表面的Ga 2O 3含量增加,表明电流作用促进了GaN材料表面的氧化腐蚀作用,进而提高了其CMP材料去除速率。     

Material removal mechanism of precision grinding of soft-brittle CdZnTe wafers

Cd_0.96Zn_0.04Te (111) wafers were precisely ground by #800, #1500, #3000, and #5000 diamond grinding wheel. For comparison, Cd_0.96Zn_0.04Te (110) wafers were machined by lapping, mechanical polishing, and chemical mechanical polishing. High-resolution environmental scanning electron microscopy equipped with energy dispersive spectroscopy and optical interference surface profiler both were employed to investigate the surface quality and material removal mechanism. The results show that the material removal mechanism of #800 grinding wheel is abrasive wear, fatigue wear, and adhesive wear, and that of #1500 is abrasive wear and fatigue wear. Both the material removal mechanism of #3000 and #5000 grinding wheel are abrasive wear, leading to the excellent ductile removal precision grinding. While the material removal mechanism of CMP on CdZnTe wafers is firstly chemical resolving reaction and secondly mechanical carrying action. Moreover, precision grinding exhibits high-efficiency character and eliminates the imbedding of free abrasives of Al₂O₃ and SiO₂.     

Reduction in wear of metakaolinite-based geopolymer composite through filling of PTFE

Metakaolinite-based geopolymer composite containing 5-30% (volume fraction) polytetra-fluoroethylene (PTFE) was synthesized using compound activator composed of aqueous NaOH and sodium silicate at room temperature. Flexural strength, compressive strength and elastic modulus of the composite were measured. Tribological behaviour of the composite sliding against AISI-1045 steel was investigated on an MM-200 friction and wear tester. SEM, EDS and XPS analysis were conducted on worn surfaces and wear debris. The results show that mechanical strength of the composite was lower than corresponding geopolymer while the wear model became mild. The friction process was stable and the wear rate was dramatically reducted by 86-99.4%. The improvement of tribological properties of the composite was attributed to form a brown soft thin layer on the worn surface of the composite containing Fe₂O₃ came from tribochemical reaction. EDS analysis on the worn surfaces indicate the content of Fe increase along with the increase of volume content of PTFE in the composite. Furthermore, the counterpart, the steel ring was also protected from terrible wear as occurred when friction with geopolymer without any filling of solid lubricant. There is a brown thin layer mainly composed of Fe₂O₃ on the steel ring.     

无抛光垫化学机械抛光技术研究

应用双电层理论分析了SiO2磨粒与聚苯乙烯粒子在溶液中的ζ电位及粒子间的相互作用机制,观察到SiO2磨粒吸附在聚苯乙烯粒子表面的现象.分析了基于复合粒子抛光液的无抛光垫化学机械抛光技术特点及其材料去除机理.比较试验表明,基于复合粒子抛光液的硅片无抛光垫化学机械抛光具有与传统化学机械抛光相接近的材料去除率和硅片表面粗糙度值,并可避免工件塌边现象的产生.     

Design of experiments approach to the study of tribological performance of Cu-concentrate-filled PPS composites

The tribological performance of copper-concentrate (CC) mineral deposit as the filler in polyphenylene sulfide (PPS) was studied as a function of the filler proportions and sliding test variables. CC is a complex mixture of CuS, Fe_xO_y, SiO₂, Al₂O₃, and other trace materials. The design of experiments based upon L₉ (3⁴) orthogonal arrays by Taguchi was used. Sliding tests were performed in the pin-on-disk configuration against a hardened tool steel (55-60 HRC) disk. The improvement in wear resistance of PPS was considerable with the use of fillers. The lowest steady state wear rate of 0.0030 mm³/km was obtained for PPS+20%CC+15%PTFE composition. It was two orders of magnitude lower than that of unfilled PPS. The variations in steady state coefficient of friction with the changes in filler proportions and sliding test variables were small. The transfer film was studied by atomic force microscopy (AFM) and scanning electron microscopy (SEM). X-ray photoelectron microscopy (XPS) was used to detect chemical reactive species developed during sliding, especially in the interface between transfer film and its counterface. Wear particles and the polymer worn surfaces were analyzed by energy dispersive spectroscopy (EDS) for elemental distribution.     

高浓度硼扩散硅片CMP工艺研究

"叉指式微加速度计"的研制,需要使用高浓度硼扩散硅片,而硅片经过高浓度硼扩散后,硅片双面生长了一层硼硅玻璃,很难将其去除,不能在高浓度硼扩散层上制作更好的"叉指式微加速度计"结构.针对上述问题,在CMP研磨抛光工艺中,针对上述问题,在CMP研磨抛光工艺中,选择合适的研磨料和抛光料以及研磨盘和抛光盘,通过对浆料浓度、流量大小、抛光温度进行改进,优化研磨抛光工艺流程及工艺参数,以完成高浓度硼扩散硅片的表面平坦化.     

Effect of abrasive grit shape on polishing of β-Ga2O3(100) substrate

β-Ga₂O₃ can be cleaved easily, where the (100) surface is the main cleavage surface. This surface encounters local stress concentration during ultra-precision machining and is prone to local fragmentation, resulting in formation of micro-cleavage pits. The effects of different abrasive grit shapes on polishing are studied in order to ensure smooth processing of β-Ga₂O₃(100). First, a contact mechanics model for different shapes of abrasive grits and crystal surfaces is established in accordance with the theory of elasticity. Then, the contact mechanism between the abrasive grits and the crystal surfaces is analyzed using a theoretical model. Finally, the feasibility of the theoretical model is verified in experiments. The results show that blunt spherical abrasive grits are more suitable for polishing of β-Ga₂O₃(100) than sharp diamond-shaped abrasive grits. Compared to sharp abrasive grits, the crystal surfaces processed using blunt abrasive grits are smoother, with surface roughness (Ra) of approximately 14 nm. During polishing, the sharp and blunt abrasive grits remove brittle and plastic material, respectively. Therefore, blunt abrasive grits are more suitable for the polishing of β-Ga₂O₃ than sharp abrasive grits.