Etching Area Research Articles

Advanced Techniques for the Fabrication of Nanostructured Porous Silicon Using Photoelectrochemical Etching and Ultrasonic Vibration

This study presents a novel method combining photoelectrochemical etching with ultrasonic vibration for the formation of nanocrystalline porous silicon (NC-PS). This combined process enhances the band gap energy absorption (BEA) by reducing bubble accumulation in the etching area. It is found that laser irradiation can decrease the etching rate, while ultrasonic vibration aids with bubble expulsion, preventing accumulation in the etching area, resulting in more uniform etching and increasing the porosity of the porous silicon (PS). High porosity in NC-PS structures enhances the surface area, thereby increasing electron mobility and improving the electron energy distribution. Our experiments demonstrate that this combined process leads to more uniform and deeper etching and the creation of well-defined porous structures. The more uniform PS size distribution (8–14 nm) achieved by photoelectrochemical etching combined with ultrasonic vibration enhances the optical properties of the material due to quantum confinement effects. Porosity measurements provide essential surface characterization information that is crucial for determining the performance of PS diode components in various applications. Our findings demonstrate that this combination technique improves the uniformity, efficiency, and precision of porous silicon etching, producing material for high-performance applications, including sensors, catalysts, and photonic devices.

Investigation of white etching area at non-carbides origin in M50 bearing steel under rolling contact fatigue

White etching areas (WEAs) were originated in regions free of carbides or non-metallic inclusions under rolling contact fatigue (RCF) in M50 bearing steel. Two types of WEAs with largely sheared and compact morphologies were observed. They were investigated using Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The results show that WEAs involve martensite-to-austenite phase transformation and amorphization, in contrast to the butterfly-winged WEAs consisting of only ferrite nanocrystallines. It is suggested that the nanocrystallines are the result of recrystallization. The high micro shear strain of 0.9–1.1 drives phase transformation. The solid-state amorphization occurs due to accumulation of high dislocation density. The dislocation density in the compact WEA is much higher than that in the sheared WEA.

Discovery of white etching areas in high nitrogen bearing steel X30CrMoN15-1: A novel finding in rolling contact fatigue analysis

White etching areas (WEA) and white etching cracks (WEC) are frequently linked to premature bearing failure in conventional high carbon bearing steels like 100Cr6 (SAE 52100). In contrast, no WEA/WEC has yet been reported for the high nitrogen bearing steel X30CrMoN15-1 (SAE AMS 5898). Thus, the present study proves for the first time that X30CrMoN15-1 is also susceptible to develop WEA/WEC under rolling contact fatigue (RCF) when pre-charged with hydrogen. RCF tests conducted in parallel without hydrogen pre-charging resulted in RCF damage only, which identifies hydrogen as an active agent for WEA/WEC formation in X30CrMoN15-1. These findings correspond to the fact that hydrogen diffusion during RCF is often considered to cause or accelerate the formation of WEA/WEC. Additionally, it is observed that the M2(C, N) and M23C6 precipitates of the martensitic microstructure of the X30CrMoN15-1 do not entirely decompose during the WEA formation process as observed for M3C precipitates in 100Cr6. In conclusion, the results for X30CrMoN15-1 strongly suggest that the formation of WEA is driven by a hydrogen-activated local severe plastic deformation process, which initiates continuous dynamic recrystallisation, leading to the characteristic nano-ferritic grains observed in WEA. Also, the highly stable and self-regenerating passive chromium-oxide layer of X30CrMoN15-1 mitigates the risk of WEA/WEC failure during typical RCF operation by hindering the formation and adsorption of ionic hydrogen. Hence, this study emphasises the importance of protecting the base material against hydrogen ingress to delay WEA/WEC formation.

Experimental Characterization of Common-Mode Voltages and Currents in Gearbox Bearings of a Doubly-Fed Induction Generator Wind Turbine on a Test Bench

Wind turbine (WT) drivetrain failures can lead to expensive repairs and downtime, significantly impacting the Levelized Costs of Electricity (LCOE). Gearbox failures are a major contributor to maintenance costs, with High-Speed-Shaft (HSS) bearings having the highest failure rate. Frequently occurring premature HSS bearing damage indicates design inadequacies. Currently, bearing design standards (DIN/ISO 281) are primarily based on fatigue. Other damage mechanisms like adhesion or damages due to electrical currents passing through the bearings are not considered. WT gearbox bearings are exposed to electrical currents, mainly caused by common-mode (CM) voltages. Bearing currents lead to surface damages and also may promote the formation of white etching areas (WEA) or cracks (WEC) and thus need to be investigated further. The CM voltage is an inherent feature of the power converter, which generates CM currents in the electrical machine. The resulting high voltages at the HSS bearings can lead to electrical discharge currents in the rolling contact, which damage the raceways of the bearing. This paper presents an experimental method for characterization of the currents and voltages that pass from the generator to the HSS of the gearbox in a multi-megawatt WT drivetrain on a test bench. CM currents and voltages measured at the converter are correlated with the shaft voltages at the HSS bearing. The results indicate, that the CM currents directly pass the HSS and its bearings into the gearbox housing. The CM currents show peaks indicating discharge events with over 100 A. Furthermore, at the discharge events, high-frequency oscillations with over 20 MHz are observed in CM current and bearing voltage.

A new fabrication method for enhancing the yield of linear micromirror arrays assisted by temporary anchors

As one of the most common spatial light modulators, linear micromirror arrays (MMAs) based on microelectromechanical system (MEMS) processes are currently utilized in many fields. However, two crucial challenges exist in the fabrication of such devices: the adhesion of silicon microstructures caused by anodic bonding and the destruction of the suspended silicon film due to residual stress. To solve these issues, an innovative processing method assisted by temporary anchors is presented. This approach effectively reduces the span of silicon microstructures and improves the Euler buckling limit of the silicon film. Importantly, these temporary anchors are strategically placed within the primary etching areas, enabling easy removal without additional processing steps. As a result, we successfully achieved wafer-level, high-yield manufacturing of linear MMAs with a filling factor as high as 95.1%. Demonstrating superior capabilities to those of original MMAs, our enhanced version boasts a total of 60 linear micromirror elements, each featuring a length-to-width ratio of 52.6, and the entire optical aperture measures 5 mm × 6 mm. The linear MMA exhibits an optical deflection angle of 20.4° at 110 Vdc while maintaining exceptional deflection flatness and uniformity. This study offers a viable approach for the design and fabrication of thin-film MEMS devices with high yields, and the proposed MMA is promising as a replacement for digital micromirror devices (DMDs, by TI Corp.) in fields such as spectral imaging and optical communication.

Determining rational parameters for the treatment of concentrated wastewater from etching site by using combined systems producing sediments of predefined composition

The object of this study is model solutions, spent sulfuric acid and chloride acid etching solutions, degreasing of metal products at enterprises. The paper reports results of research on the possibility of obtaining sediments of predefined composition and reducing the consumption of chemical reagents in comparison with conventional cleaning schemes. The systematization of the elements of the technological scheme has been shown, which provides for the treatment of concentrated wastewater of the etching area in combined systems with obtaining sediments of predefined composition and is the basis for the implementation of resource-saving technology. Rational parameters were established for the state (рН=3‒4, Eh=+0.3‒+0.33 V, and rH2=16.3–19.38 V) and technological parameters (degree of iron extraction ψ=0.8, reagent consumption from the stoichiometric norm of B=0.8). Such parameters provide the proper conditions for the oxidation of organic compounds and their co-precipitation with insoluble iron hydroxy compounds (the maximum degree of extraction of organic impurities is 86 %). The formed precipitate corresponds to the FeOOH.nH2O composition, contains 2‒3 % of organic impurities, and is subject to burial. As a result of studies on the treatment of concentrated iron-containing wastewater, the obtained sediment is ready for further utilization by processing. The composition of this sediment corresponds to the natural mineral limonite FeOOH (Fe2O3.nH2O) and is formed at pH values from 3.5 to 7.5 with rH2 values from 26 V to 21 V and at technological regeneration parameters of pH=4.0–4.6; rH2 =23.34–32.25 V. As a result of research into the deep purification of wastewater using a magnetic device, a suspension of sediment of ferromagnetic impurities (hydroxo compounds of iron) is obtained, which could be the basis for extraction or production of magnetically favorable dispersed material.

Investigations on Optical Absorption and the Pyro-phototronic Effect with Selectively Patterned Black Silicon for Advanced Photodetection.

A novel property existing in the stain-etching technique that eliminates the need for expensive etchant masks in the texturization process of silicon wafers was identified. Through the combination of grayscale lithography and stain-etching methodologies, selective patterning of silicon with AR-P 3510 T, a positive-photoresist mask, was carried out. The etch area ratio was varied in nine different patterns of various feature sizes ranging from 400 to 1500 μm. The optical characteristics of the patterned substrates were determined from diffuse reflectance spectroscopy analysis, and the results were supported with finite-difference time-domain simulations. Complimenting the improvement in optical properties, the electrical losses in microwell-patterned photodetector devices have been reduced with an electro-optic optimum value of the surface enhancement factor, γ. The photodetecting efficiency of a selectively patterned microwell photodetector device exceeded the planar and black silicon photodetector devices with a considerable improvement in the pyro-phototronic effect. This work suggests an alternative for black silicon optoelectronic devices providing a new route to fabricate selectively patterned substrates with an achieved detectivity 16- and 20-fold higher than black and planar silicon photodetector devices, respectively.

Microstructure alterations and white etching area formation in bearing steels under high-frequency dynamic loading

This article discusses the effects of various steels and lubricants on subsurface microstructural changes during a high-frequency dynamic pin-on-disc test under pure sliding and boundary lubrication conditions. Steel materials chosen for this study are 55SiMo8 steel, 100Cr6 steel, and 8 %Cr steel. Fully formulated polyalkylene glycols-based oil, synthetic hydrocarbon oil, and per-fluoro polyether base oil were selected as the lubricants. In 8 %Cr, the average roundness of large carbides was reduced by 33 % due to the deformation of carbides that occurred during severe cyclic loading. The outcomes showed that the material effect has a greater impact on the generation of white etching areas than the effect of lubricants under high-frequency dynamic loading.

Investigation on butterfly white etching area formation mechanism and crack source at different stages in M50 bearing steel

Rolling contact fatigue tests with different stresses and cycles have been conducted to study the formation mechanism and crack source of butterfly white etching area (WEA) in different stages of M50 bearing steel. The results suggest that the structural transformation is prior to cracks. The initial microstructure is the nanocrystalline α-Fe formed by dislocation assisted carbon migration. With the extension of cycles, unlike the previous studies, the butterfly-origin carbide is refined into Mo2C and M7C3 nanocrystalline by the accumulated dislocation clusters. Subsequently, the increase of interfacial energy drives the metal elements diffusion and thus the formation of amorphous structures. A new mechanism called diffusion-assisted dislocation has been proposed for butterfly WEA formation.

The influence of lubricants on white etching areas formation in DLC-coated bearing steel under severe boundary lubrication

White etching areas (WEAs) and white etching cracks (WECs) are the catastrophic premature failure modes associated with wind turbine gearbox bearings. Several drivers, including lubricant chemistry, influence the evolution of WEAs and WECs. This study investigated the performance of base oils with various lubricant chemistry against microstructural decay in DLC-coated AISI 52100 bearing steel. Tests were performed in sliding-dynamic loading conditions under severe boundary lubrication. The effect of base oils against WEAs formation in DLC-coated steel is explored by analysing the condition of oils, wear behaviour, and subsurface microstructural change. The study outcomes revealed that the selection of base oils plays a vital role against the WEAs formation in DLC-coated bearing steel subsurface.

High-precision and high-speed etching of diamond surfaces using Fe–Ni alloy catalyzed H–O plasma etching

Power devices with low losses are essential for achieving high-efficiency, low-cost, and miniaturized inverters and advance electronic technologies. Recently, diamond-based p-type groove semiconductor field-effect transistors have emerged as a hot research topic. Conventional method of fabricating surface grooves using inductively coupled plasma etching is costly and relatively slow. Here, we realized a novel diamond machining method using Fe–Ni alloy catalyzed H–O microwave plasma etching that can achieve high-rate and high-precision etching of diamond surfaces. Two major factors affecting the etching rate and pattern accuracy, wettability of diamond and carbon solubility with liquid metal, were identified. Oxygen added in H2 plasma allows the wetting increase, resulting in an improvement in uniformity of the etch area, while keeping the etch rate as high as 3 μm/min. The developed approached is promising for low-cost diamond patterning in electronic devices fabrication processes.

High sensitivity and optimum design of LSPR-based sensors by coupled nano-rings for cancer detection

Plasmonic RI sensors are widely used in various fields due to their high sensitivity and specificity; and is based on the change of the refractive index of the system. In this research work, we investigate an LSPR-based sensor consisting of two coupled silver nano-rings on a SiO2/Si substrate. The sensor's sensitivity, full width at half maximum (FWHM), and figure of merit (FOM) of the sensor are measured to be 393.14 nm/RIU, 53.2 nm, 7.39 RIU−1, respectively. The resonance peak is generated by the focused electric field in the elliptical area between the nano-rings. By assuming an etched area filled with the solution under the elliptical area between the nano-rings, we enhance the interaction between the solution and the penetrated electrical field in the SiO2 layer. This approach increases the sensitivity, FWHM, and FOM to 524.3 nm/RIU, 52.3 nm, 10.024 RIU−1, respectively. The designed sensor as a bio-sensor is capable of effectively detecting different types of cancerous cells from healthy cells, since the refractive index of a cell that affected by cancer, is higher than healthy cell. The simulation results show good selectivity for each type of cancer, with a FOM of approximately 9.5 RIU−1.

White etching area damage induced by shear localization in rolling contact fatigue of bearing steel

AbstractWhite etching area (WEA) is a primary damage in rolling contact fatigue (RCF) of bearing steels. In spite of extensive investigations, there is a large discrepancy in the existing mechanisms of WEA formation. We attempt to unify the mechanisms from the perspective of shear localization and plastic damage accumulation based on ductile damage. RCF tests were conducted to generate WEAs with various microstructures and compositions. A thermodynamically consistent model of the ductile damage evolution from an inclusion was established by developing the phase field damage coupled with the crystal elastic‐viscoplastic constitutive relationship under RCF. The model was implemented into the FE framework through a user materials subroutine. The results indicated that the WEA is the shear band resulting from shear localization. The large inhomogeneity and scatter in WEA's microstructure are due to the influence of the crystal orientation. The development and orientation of SBs predicted by the model and the experimental observation of the WEA are in good agreement. The large micro‐shear strain in the WEA provides the driving force for mechanically controlled austenite phase transformation. The shear band center, which has the largest strain and the least stress, is where cracks initiate. This demonstrates that contrary to earlier reports that WEA is induced by previously formed crack faces friction, cracks actually initiate from the interior of the WEA.

Effect of DLC film on the mitigation of white etching areas (WEAs) under dynamic loading

The premature failures in wind turbine gearbox bearings are primarily caused by the decay of subsurface microstructure called white etching areas and white etching cracks. Severe operating conditions of wind turbine gearbox bearings necessitated for tribological coatings to enhance the system performance. The current study investigated the performance of hydrogenated diamond-like‑carbon (DLC) coating against white etching areas formation under sliding-dynamic conditions. The dynamic loading experiments were carried out in the dynamic pin-on-disc tribometer with Polyalphaolefin base stock oil under a boundary lubrication regime. Prior to the dynamic load tests, detailed tribological characterisation of the deposited DLC coating was carried out. The post-test analysis results were compared with the uncoated AISI 52100 bearing steel tribopair to evaluate the performance of DLC-coated bearing steel against white etching areas formation under given conditions. The results obtained show the capability of the proposed coating to delay the formation of white etching areas in the bearing steel.

Selective mask deposition using SiCl4 plasma for highly selective etching process

We developed an area-selective deposition process for forming protective layers on top of masks generated using a microwave electron-cyclotron-resonance etching system. A deposition layer is formed only on SiO2 masks without forming an unnecessary deposition layer on the Si surfaces in the etching area, such as the bottoms of the patterns and isolated etching area. The protection layers were selectively formed on a SiO2 mask without forming on a Si etching area by using a SiCl4/H2/Cl2 plasma. The pretreatment to clean the Si and SiO2 surfaces before deposition was important for achieving selective deposition because selectivity appeared by nucleation delay on the cleaned Si surface. On the Si surface, adsorbed SiClx easily desorbed again by reacting with the Cl generated from the plasma. However, adsorbed SiClx on SiO2 was more difficult to desorb by reacting with Cl due to Si–O having a larger binding energy than Si–Si. After the deposition layer was selectively formed on the SiO2 mask, the layer was oxidized by using O2 plasma treatment to improve the etching resistance during the subsequent Si etching. We also investigated a Si etching process using selective deposition during the etching of a 25 nm-pitch line-and-space Si pattern with a SiO2 mask. Extremely highly selective etching was achieved using selective deposition without forming an unnecessary deposition on an isolated Si area.

The influence of fracture surface morphology on nonuniform etching in limestone acid fracturing

The success of acid fracturing in tight limestone reservoirs relies on the formation of nonuniform etching on the fracture wall. However, almost all acid fracturing models neglect the effect of fracture surface morphology on nonuniform etching. In this study, a three-dimensional acid fracturing mathematical model is developed to quantify and analyze the influence of rough fracture surface morphology on nonuniform etching for the first time by defining a morphology coefficient to describe the degree of local and overall morphological undulations of the fracture surface from a three-dimensional scale. The model uses the moving mesh partial differential equation (MMPDE) method to describe the flow field and spatial variation in the fracture as the fracture surface is continuously dissolved with the acid during acid fracturing, and the MMPDE moving mesh is coupled with the flow field, mass transfer, acid-rock reaction and fracture width variation. Based on the model, the effects of flow pattern, morphology coefficient, initial fracture width and fracture type on the nonuniform etching are studied. The simulation results demonstrate that the rough fracture surface can disturb the flow field and make the acid distribution more turbulent, which is conducive to the formation of nonuniform etching on the fracture surface. This phenomenon of flow rate differentiation can enhance the acid transfer distance. The local etching degree of the fracture surface decreases with the increase of the morphology coefficient of the area, and the strongly etching areas will appear around it. When the morphology coefficient of the local fracture area is larger than 1.2218, the area can appear obvious strongly etching areas and weakly etching areas after acid etching. The larger the initial fracture width is, the smaller the degree of nonuniform etching on the fracture surface. The prediction model constructed based on multiple linear regression was highly accurate (R2 = 0.9268) for the standard deviation of facture width (StdWidth) after acid etching. The critical value of StdWidth is recommended to be 0.6 as the criterion for judging the nonuniform etching ability. When the nonuniformity of the fracture surface is greater than this value, it is considered that the nonuniform etching ability is strong. In addition, the fracture with shear damage can produce relative sliding distance, which makes the fracture morphology on both sides of the fracture surface unevenly distributed and thus disturbs the flow field, which enhances the degree of nonuniform etching on the fracture surface. As the sliding distance increase, the magnitude of this enhancement also increases gradually. This study proposes a new three-dimensional characterization method for rough fracture surface morphology, solves the issue of mismatching flow field due to dynamic change in fracture width during acid fracturing.

New microstructure of butterfly white etching area in rolling contact fatigue of bearing steel

Butterfly white etching area (WEA) formed at subsurface inclusions under rolling contact fatigue (RCF) of bearing steel was investigated by using the Scanning Electronic Microscopy and Transmission Electron Microscopy. Two kinds of butterfly WEAs with different orientations were observed at non-metallic inclusions: largely sheared and narrow band morphologies. Both involve body-centered-cubic (bcc) to face-centered-cubic (fcc) transformation, which is opposed to the previously reported butterfly WEAs consisting of only ferrite nanocrystallines. The largely sheared WEA is composed of nanocrystallines with the grain size of 15 nm averagely. In contrast, apart from the nanocrystallines, the narrow band WEA also includes well-developed equiaxed dynamic recrystallization grains with the grain size ten times larger than the nanocrystallines. This indicates that the WEA involves not only grain refinement, which is commonly reported, but grain growth as well due to dynamic recrystallization. It was suggested that the bcc to fcc phase transformation in nanocrystallines is mechanically controlled, while the phase transformation in equiaxed dynamic recrystallization grains is governed by thermally-assisted plastic deformation.

The role of size and volume fraction of carbides on hydrogen embrittlement and white etching areas formation in bearing steel under dynamic loading

Despite of more than two decades of research in white etching areas (WEAs), this phenomenon still persists in wind turbine gearbox bearings leading to a reduction of L10 life by 90 percent. There are various drivers for WEAs formation among which hydrogen is considered one of the root causes which accelerates the microstructural degradation. Diffusible atomic hydrogen reduces the threshold for dislocation motion leading to localized strain accumulation. The tendency to form WEAs in bearing steel depends on the stability of carbide precipitates during plastic deformation and resistance to diffusible hydrogen. In this research work, the role of size and volume fraction of carbides on their relative stability against decomposition and hydrogen embrittlement is studied. The performance of bearing ball samples with different carbide sizes and distribution is tested in the presence of two different lubricants in the dynamic load pin-on-disc (PoD) test rig. The results from the study show that reducing the size of carbide precipitates improved their stability against plastic deformation leading to the stagnation of WEAs formation.

The origin of microstructural alterations in M50 bearing steel undergoing rolling contact fatigue

M50 bearing steel designed for aerospace applications exhibits unique microstructural alterations at the subsurface during rolling contact fatigue (RCF). In this work, three types of microstructural alterations, light etching region (LER), white etching band (WEB) and white etching area (WEA) are systematically studied. A hardness profile at the subsurface is obtained by microindentation with material softening being detected. It is found that the material softening is associated with the formation of WEBs. The microstructural nature of the three types of microstructural alterations is revealed by detailed characterisation using focused ion beam milling and transmission electron microscopy. It is found that LERs, WEBs and WEAs are a manifestation of the decay of the parent martensite and all consist of dislocation cells or fine grains, indicative of plastic deformation. Through subsurface stress field analysis, LER, WEBs and WEAs are found to be caused by different stress components. The similarities and differences of the microstructural alterations in M50 and in widely studied 100Cr6 are discussed where the stability of carbides is believed to play a key role. The difference in material response in the microstructural alterations in M50 is further analysed and modelled based on Kocks and Mecking theory, with different types of activated dislocation slip systems found to be the root cause for such difference. Based on the material response analysis for WEBs, a material softening model for M50 during RCF is established by considering residual plastic strain accumulation, yielding prediction results in agreement with experimental measurement.

Confirming Debonding of Non-Metallic Inclusions as an Important Factor in Damage Initiation in Bearing Steel

Damage in bearings is closely associated with the presence of microstructural alterations, known as white etching areas (WEAs) and white etching cracks (WECs). One of the main reasons for the creation of these microstructural alterations is the presence of defects in the material, such as non-metallic inclusions. Manganese sulfides and aluminum oxides are widely reported in the literature as the most common types of non-metallic inclusions found in bearing steels. This study classifies 280 non-metallic inclusions in an investigated bearing steel according to several criteria: bonded/debonded with the matrix, size, shape, orientation angle, depth below the raceway surface, and chemical composition. Contrary to the findings in the literature, this investigation reports that the chemical composition of the inclusion (MnS + Al2O3) is of secondary importance when considering factors for damage initiation. The orientation of the microstructural alterations is observed to coincide with the high-stress regions, indicating a relation between the formation of butterfly wings and the white etching crack. In our investigation, butterfly wings typically exhibit a 45-degree pattern originating from the non-metallic inclusions. Conversely, the white etching crack starts from the non-metallic inclusion at a shallower angle in correspondence to the raceway. This can be attributed to the stress state, which corresponds to a region where extensive white etching cracks are formed. In conclusion, the microstructural observations demonstrate that the state of non-metallic inclusion—i.e., whether they are bonded or not to the steel matrix—plays an essential role in initiating rolling contact fatigue damage.