Polishing Of SiC Research Articles

Preparation of CIP@Fe3O4 particles and their impact on the fenton reaction processing performance of single-crystal SiC

This study proposes the preparation of CIP@Fe3O4 composite magnetic particles, which maintain excellent magnetic properties while exhibiting superior Fenton reaction performance for the magnetorheological chemical polishing of single-crystal SiC. The CIP@Fe3O4 particles were prepared by coating a nanoscale layer of Fe3O4 onto micron-sized carbonyl iron powder (CIP) using the co-precipitation method. Their Fenton reaction performance and magnetic properties were characterized, and CIP@Fe3O4 was used as a solid-phase catalyst in Fenton reaction-induced etching, frictional wear, and polishing experiments on single-crystal SiC. The prepared CIP@Fe3O4 particles have a saturation magnetization of 184.3 emu/g, representing only an 8.7 % reduction compared to CIP, yet achieved a decolorization rate of 76.2 % for the methyl orange indicator (compared to only 17.2 % with CIP alone). The Fenton reaction using CIP@Fe3O4 resulted in a prominent corrosion layer on the surface of single-crystal SiC, with the oxygen atomic fraction reaching 22.15 %. The study examined material removal from SiC under Fenton reactions with different solid-phase catalysts: CIP, CIP@Fe3O4, and CIP + Fe3O4. Frictional wear results indicated that the maximum scratch cross-sectional removal area on the SiC surface under the Fenton reaction with CIP@Fe3O4 was 474.38 μm2, representing a 207.3 % increase compared to without the Fenton reaction. Additionally, Si-O compounds were identified in the debris. Polishing experiments showed that the material removal rate (MRR) with the Fenton reaction was 3295 nm/h, an increase of 220.2 % compared to without the Fenton reaction, and the surface roughness was reduced to Ra 0.895 nm, a 73.4 % reduction compared to without the Fenton reaction. This study provides additional evidence for the application of magnetorheological technology and the Fenton reaction in the polishing field of single-crystal SiC.

Piezocatalysis for Chemical-Mechanical Polishing of SiC: Dual Roles of t-BaTiO3 as a Piezocatalyst and an Abrasive.

Chemical mechanical polishing (CMP) offers a promising pathway to smooth third-generation semiconductors. However, it is still a challenge to reduce the use of additional oxidants or/and energy in current CMP processes. Here, a new and green atomically smoothing method: Piezocatalytic-CMP (Piezo-CMP) is reported. Investigation shows that the Piezo-CMP based on tetragonal BaTiO3 (t-BT) can polish the rough surface of a reaction sintering SiC (RS-SiC) to the ultra-smooth surface with an average surface roughness (Ra) of 0.45nm and the rough surface of a single-crystal 4H-SiC to the atomic planarization Si and C surfaces with Ra of 0.120 and 0.157nm, respectively. In these processes, t-BT plays a dual role of piezocatalyst and abrasive. That is, it piezo-catalytically generates in-situ active oxygen species to selectively oxidize protruding sites of SiC surface, yielding soft SiO2, and subsequently, it acts as a usual abrasive to mechanically remove these SiO2. This mechanism is further confirmed by density functional theory (DFT) calculation and molecular simulation. In this process, piezocatalytic oxidation is driven only by the original pressure and friction force of a conventional polishing process, thus, the piezo-CMP process do not require any additional oxidant and energy, being a green and effective polishing method.

Damage-free polishing of SiC by Slurryless Electrochemical Mechanical Polishing

Damage-free polishing of SiC by Slurryless Electrochemical Mechanical Polishing

The polishing properties of magnetorheological-elastomer polishing pad based on the heterogeneous Fenton reaction of single-crystal SiC

Magnetic particles (Fe3O4/CIP) in magnetorheological elastomer (MRE) were used as solid-phase catalysts in the heterogeneous Fenton reaction for chemical mechanical polishing (CMP) of single-crystal SiC. The polishing effect and polishing mechanism were investigated by experiments and polishing debris analysis. The results show that when using H2O2 polishing solution the material removal rate (MRR) was higher and the surface roughness (Ra) was lower at all stages of polishing than using deionized water polishing solution. The MRRs when polishing for 60 min with the deionized water and the H2O2 polishing debris were, respectively, 636.94 nm/h and 1194.27 nm/h (an increase by 87.5%), and the corresponding Ra values were, respectively, 12.445 nm and 4.420 nm (a decrease by 64.5%). From the analysis of the polishing debris after 60 min of polishing, it was found that the H2O2 polishing solution was polished with laminated loose chips, and the main elements of the chips were C, O, and Si, with O element accounting for 38.585 wt%. This indicates that a chemical reaction has occurred on the SiC surface during polishing, generating low hardness and low binding strength SiO2, and thus resulting in increased material removal; this phenomenon is confirmed by the profile morphology of SiC wafer by fixed-point polishing. It is shown that the use of Fe3O4/CIP in MRE as a solid-phase catalyst for the heterogeneous Fenton reaction of polishing SiC can substantially increase the material removal capacity of MRE polishing pads and improve the polishing quality at the same time.

A study of the magneto-controlled mechanical properties and polishing performance for single-crystal SiC used as a magnetorheological-elastomer polishing pad

Magnetorheological elastomers (MREs) are widely used in vibration control due to their excellent magneto-controlled mechanical properties. In this research, polyurethane-based MRE polishing pads were prepared and used for the polishing of single-crystal SiC to investigate the magneto-controlled mechanical properties, the magneto-polishing effect, and the mechanism of action thereof. The results show that the pre-structuring process is affected by parameters such as mass fraction and particle size of magnetic particles in MREs and curing magnetic field strength, different chain strings that demonstrate different magnetorheological effects are formed. The greater the mass fraction of magnetic particles and curing magnetic field strength, the more the MREs exhibit magnetorheological effects, especially so when the magnetic particles size of 3 μm. A series of 90 min polishing experiments on single-crystal SiC with original surface roughness (R a) 80 nm were conducted using an MRE pad. The results indicate that with the increase of polishing magnetic field strengths, the shear modulus of MRE polishing pads increases, the material removal rate (MRR) of the polishing process increases and R a decreases. As the magnetic field strength is increased from 0 mT to 335 mT, the shear modulus is increased from 1.392 MPa to 1.825 MPa (an increase of 31.1%), while MRR is increased from 706.3 nm h−1 to 835.3 nm h−1 (an increase of 18.3%), R a is decreased from 19.92 nm to 3.62 nm (an improvement in surface quality of 81.8%). The results show that the increase of the polishing magnetic field strengths changes the material modulus of the MRE polishing pads, which cause the decreases in the compressive and shear elastic deformation of the abrasive grains on the elastic substrate. This increases the positive pressure of the abrasive grains on the SiC wafer, which enhances the material-removal ability of the SiC wafer, thereby improving the surface quality of the wafer.

A Review on Precision Polishing Technology of Single-Crystal SiC

Single-crystal SiC is a typical third-generation semiconductor power-device material because of its excellent electronic and thermal properties. An ultrasmooth surface with atomic surface roughness that is scratch free and subsurface damage (SSD) free is indispensable before its application. As the last process to reduce the surface roughness and remove surface defects, precision polishing of single-crystal SiC is essential. In this paper, precision polishing technologies for 4H-SiC and 6H-SiC, which are the most commonly used polytypes of single-crystal SiC, such as chemical mechanical polishing (CMP), photocatalytic chemical mechanical polishing (PCMP), plasma-assisted polishing (PAP), electrochemical mechanical polishing (ECMP), and catalyst-referred etching (CARE), were reviewed and compared with emphasis on the experimental setup, polishing mechanism, material removal rate (MRR), and surface roughness. An atomically smooth surface without SSD can be obtained by CMP, PCMP, PAP, and CARE for single-crystal SiC. However, their MRRs are meager, and the waste treatment after CMP is difficult and expensive. Moreover, PAP’s operation is poor due to the complex polishing system, plasma generation, and irradiation devices. A high MRR can be achieved by ECMP. In addition, it is an environmentally friendly precision polishing process for single-crystal SiC since the neutral salt solution is generally used as the electrolyte in ECMP. However, the formation of the egglike protrusions at the oxide/SiC interface during anodic oxidation would lead to a bigger surface roughness after ECMP than that after PAP is processed. The HF solution used in CARE was toxic, and Pt was particularly expensive. Ultrasonic vibration-assisted single-crystal SiC polishing and electrolyte plasma polishing (EPP) were discussed; furthermore, the research direction of further improving the surface quality and MRR of single-crystal SiC was prospected.

Study on the Mechanism of Solid-Phase Oxidant Action in Tribochemical Mechanical Polishing of SiC Single Crystal Substrate.

Na2CO3—1.5 H2O2, KClO3, KMnO4, KIO3, and NaOH were selected for dry polishing tests with a 6H-SiC single crystal substrate on a polyurethane polishing pad. The research results showed that all the solid-phase oxidants, except NaOH, could decompose to produce oxygen under the frictional action. After polishing with the five solid-phase oxidants, oxygen was found on the surface of SiC, indicating that all five solid-phase oxidants can have complex tribochemical reactions with SiC. Their reaction products are mainly SiO2 and (SiO2)x. Under the action of friction, due to the high flash point temperature of the polishing interface, the oxygen generated by the decomposition of the solid-phase oxidant could oxidize the surface of SiC and generate a SiO2 oxide layer on the surface of SiC. On the other hand, SiC reacted with H2O and generated a SiO2 oxide layer on the surface of SiC. After polishing with NaOH, the SiO2 oxide layer and soluble Na2SiO3 could be generated on the SiC surface; therefore, the surface material removal rate (MRR) was the highest, and the surface roughness was the largest, after polishing. The lowest MRR was achieved after the dry polishing of SiC with KClO3.

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.

Basic research on chemical mechanical polishing of single-crystal SiC—Electro–Fenton: Reaction mechanism and modelling of hydroxyl radical generation using condition response modelling

Hydroxyl radicals (·OH) can effectively oxidise and corrode single-crystal SiC, and are used for chemical mechanical polishing (CMP). The generation rate of ·OH and its total concentration produced by a CMP process based on the Electro-Fenton reaction can be effectively controlled by regulating the electric field parameters, thereby improving the polishing effect of SiC. The effects of initial H2O2 concentration, Fe3O4 concentration, and voltage on ·OH were studied, and the reaction mechanism was also revealed. Moreover, a conditional-response mathematical model for ·OH generation was established. The generated ·OH first increased and then decreased with increasing initial H2O2 concentration, Fe3O4 concentration, and voltage. When these parameters were 7.5 wt%, 1.5 wt% and 0.75 V, respectively, a maximum total ·OH concentration of 9545.776μmol could be obtained. The conditional-response mathematical model established with initial H2O2 concentration, Fe3O4 concentration, and voltage can accurately predict the total generated ·OH concentration with a relative prediction error of less than 10%. Controlling the electric field parameters can accelerate the conversion of Fe3+ to Fe2+, increasing Fe2+ concentration and enhancing catalytic effect. On the other hand, it also generates a small amount of H2O2 in situ on the cathode, which slows down H2O2 consumption. Furthermore, the Pt anode oxidises water to generate a small amount of ·OH. These combined effects promote ·OH generation. Additionally, the total ·OH concentration achieved in this work was 48.69% greater than that produced by the Fenton reaction. This indicates that applying the Electro-Fenton reaction to CMP of SiC improves the polishing effect.

High efficient polishing of sliced 4H-SiC (0001) by molten KOH etching

Single-crystal silicon carbide (4H-SiC) is a promising third-generation semiconductor material because of its excellent electrical, mechanical and chemical properties. However, the high hardness of 4H-SiC makes it a typical difficult-to-machine material, which greatly restricts the development of SiC devices. In this work, molten KOH etching was first used to polish SiC. The perfect crystal surface and dislocation spots were studied separately. For the perfect crystal surface, a typical isotropic etching polishing behavior was observed. The speed of the polishing process was closely correlated with the temperature. An ultrafast polishing of sliced SiC was achieved, reducing the roughness from 246.5 nm to 16.06 nm within 2 min at 800 °C, and all subsurface damage was removed, as demonstrated by TEM. For the dislocation spot, a relationship between the etch pits angle and temperature was found, making it possible to remove the influence of the dislocation spot by increasing the etch pits angle to approach 180°. This study shows that molten KOH etching could be a very promising SiC polishing method and deserves further research. We anticipate that this approach will be applicable to ultrafast polishing of SiC at the industrial scale.

Special Issue on Precision Surface Finishing

Precision surface finishing plays an important role in product quality owing to its direct effects on product appearance. As a result, automated precision surface finishing processes (APSFPs) are key technologies for industrial products and molds for forming and shaping processes. APSFPs can be divided into three main categories, namely, mechanical processes, electrochemical processes, and high energy beam processes. The objective of this special issue is to collect the cutting-edge research works focused on APSFPs. This issue includes 11 papers on APSFPs covering the following topics: ===danraku===- Review of ultraprecision surface finishing processes. ===danraku===- Ultraprecision surface machining and finishing with compensated feeding mechanisms. ===danraku===- Ultrasonic assisted cutting of unidirectional wetting surfaces and polishing of mold steels. ===danraku===- Vibration-assisted polishing of glass lenses. ===danraku===- Magnetic-assisted polishing of mirror surfaces. ===danraku===- Chemical-mechanical polishing of single-crystal SiC and GaN wafers. ===danraku===- Direct transfer of smoothing Au surfaces. ===danraku===- Plasma surface finishing of narrow channel walls of X-ray crystal monochromators. ===danraku===- Analysis and characterization of finished surfaces. It is expected that this issue will be helpful for readers to understand the recent developments in APSFPs and will lead to further research on APSFPs. We deeply appreciate the contributions of all authors and thank the reviewers for their incisive efforts.

Polishing of SiC with natural zeolite

Polishing of SiC with natural zeolite

Investigation of anodic oxidation mechanism of 4H-SiC (0001) for electrochemical mechanical polishing

In an attempt to realize the high-quality and highly efficient polishing of SiC, the anodic oxidation mechanism of SiC was studied to enable the application of electrochemical mechanical polishing (ECMP). Through linear scanning voltammetry (LSV) and anodic oxidation experiments, the etch pits on the processed surface were found to be generated by oxidation on the sites where breakdown occurs in the anodic oxidation process. The origin of the etch pits was investigated through observing the same area on a SiC substrate during the oxidation process using atomic force microscopy (AFM), and they were confirmed to be atomic-scale pits mechanically introduced in the chemical mechanical polishing (CMP) process. The Deal-Grove model was used to model the growth process of the etch pits. It was found that their growth is controlled by a charge transfer process in the initial growth stage, which changes to a diffusion process in the late growth stage. The results of this research provide a reference for obtaining atomically smooth SiC surfaces by applying ECMP.

Abrasive-less polishing of SiC using friction of elastic pad

Abrasive-less polishing of SiC using friction of elastic pad

Experiment on Chemical Magnetorheological Finishing of SiC Single Crystal Wafer

Experiment was performed to examine the plane polishing of SiC single crystal wafer by using the chemical magnetorheological finishing (CMRF) technique. The influence of some process parameters such as the concentration of diamond abrasive particles, the concentration of carbonyl iron powder and the machining gap in CMRF were studied comparing with the magnetorheological finishing (MRF) method. The results show that the surface roughness of polished SiC single crystal by the CMRF is slightly lower than that by the MRF. Polishing liquid with different components and processing parameters affects the coupling effect of mechanical removal and chemical removal in CMRF, and a better coupling effect can produce a better surface quality in CMRP. In the MRF, the surface roughness of SiC single crystal is lower for a higher concentration of carbonyl iron powder (CIP). However, in the CMRF, the CIP’s concentration may change the contact state between the catalyst and SiC, and the CIP’s concentration of about 20% can produce a better surface roughness of SiC. The machining gap between the polishing disk and the workpiece surface determines the processing effect, and the machining gap of 1.0 mm is suitable for the polishing of SiC in the MRF and CMRF.

Smart Polishing of Hard-to-Machine Materials with an Innovative Dilatancy Pad under High-Pressure, High-Speed, Immersed Condition

An innovative dilatancy polishing pad of which characteristics are controlled with processing conditions is proposed to establish high-efficiency, high-quality polishing of hard-to-machine materials for next-generation high-power devices. To make the best use of the property of the dilatancy pad, a highly durable polishing machine which enables high-pressure, high-speed, and immersed polishing was developed. Dilatancy properties were evaluated for various viscoelastic materials to select appropriate materials for a pad. The selected viscoelastic material was mixed with a special filler and abrasive particles, and integrated into a conventional polishing pad to form a dilatancy pad. Application of the dilatancy pad to polishing of SiC realized a smart polishing which achieves both high efficiency and high quality in any processing conditions. In addition, it was demonstrated that the processing conditions could be selected for the purpose of each polishing step, i.e. mid- to high-speed conditions for high-efficiency polishing and low-speed condition for high-quality finishing. A newly developed highly durable polishing machine is capable of achieving wide range of processing conditions. To avoid overheating under high load conditions, the machine can polish a work piece in slurry fluid. The material removal rate using the dilatancy pad showed superlinear dependence on the rotation speed, which outperforms the conventional polishing following the Preston's law. This innovative process can significantly reduce the polishing time of hard-to-machine materials for next-generation semiconductor devices.

Competition between surface modification and abrasive polishing: a method of controlling the surface atomic structure of 4H-SiC (0001).

The surface atomic step-terrace structure of 4H-SiC greatly affects its performance in power device applications. On the basis of the crystal structure of 4H-SiC, we propose the generation mechanism of the a-b-a*-b* type, a-b type and a-a type step-terrace structures. We demonstrate that the step-terrace structure of SiC can be controlled by adjusting the balance between chemical modification and physical removal in CeO2 slurry polishing. When chemical modification plays the main role in the polishing of SiC, the a-b-a*-b* type step-terrace structure can be generated. When the roles of physical removal and chemical modification have similar importance, the a-b-a*-b* type step-terrace structure changes to the a-b type. When physical removal is dominant, the uniform a-a type step-terrace structure can be generated.

Comparison of Fe Catalyst Species in Chemical Mechanical Polishing Based on Fenton Reaction for SiC Wafer

Chemical reaction rate of SiC wafer surface usually determines the material removal rate (MRR) in chemical mechanical polishing (CMP). In this paper, systemic experiments are carried out to discover the relationship between Fe catalyst with different forms or valence and chemical reaction rate based on Fenton reaction. Experimental results show that the MRR changes little using Fe powder or hydrogen peroxide (H2O2) alone, but the MRR of SiC will increase largely by adding them both that will produce Fenton reaction. The MRR continues to increase slightly when Fe2+ ions is employ as catalyst, but that is much lower when utilizing Fe3+ ions. Moreover, SiC wafer with a smaller surface roughness and better quality can be obtained when using Fe powder as catalyst in Fenton reaction. The results indicate that the Fenton reaction can effectively improve the polishing efficiency of SiC substrate and Fe powder is more suitable for polishing of SiC than ferrous or ferric salt in CMP based on Fenton reaction.

Electrochemical Polishing of p-Type 4H SiC

This article discusses the electrochemical polishing of silicon-face p-type 4H SiC using diluted aqueous HF solution. Etchings on the silicon and carbon faces of SiC samples are performed and compared. The experimental results show that the RMS surface roughness of the electrochemically polished Si-face could be as low as about 2 nm. Carbon-face electrochemical polishing gives a rougher surface. Therefore, silicon-face 4H SiC is a better candidate for MEMS processing. The underlying mechanism is also discussed.

A study on surface polishing of SiC with a tribochemical reaction mechanism

This work investigates the surface polishing of silicon carbide SiC using the tribochemical reaction mechanism. Different metal discs – cast iron, AISI 304 stainless steel, S45C medium carbon steel plated chromium, brass and copper – are used to polish SiC in water and kerosene, respectively. The experimental results show that ferrous metal discs can effectively polish SiC in water. Also, no surface damage or scratches on the polished surface of SiC are observed by this method. The polishing debris was analyzed by electron spectroscopy for chemical analysis. The analyzed results indicate that the polishing surface of SiC is removed tribochemically with the aid of catalytic effect of iron oxide. Moreover, in this process the maximum material removal rate is about 0.06 μm/h.