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  1. Abstract

    The oxidation mechanism of atomically thin molybdenum disulfide (MoS2) plays a critical role in its nanoelectronics, optoelectronics, and catalytic applications, where devices often operate in an elevated thermal environment. In this study, we systematically investigate the oxidation of mono- and few-layer MoS2flakes in the air at temperatures ranging from 23 °C to 525 °C and relative humidities of 10%–60% by using atomic force microscopy (AFM), Raman spectroscopy and x-ray photoelectron spectroscopy. Our study reveals the formation of a uniform nanometer-thick physical adsorption layer on the surface of MoS2, which is attributed to the adsorption of ambient moisture. This physical adsorption layer acts as a thermal shield of the underlying MoS2lattice to enhance its thermal stability and can be effectively removed by an AFM tip scanning in contact mode or annealing at 400 °C. Our study shows that high-temperature thermal annealing and AFM tip-based cleaning result in chemical adsorption on sulfur vacancies in MoS2, leading to p-type doping. Our study highlights the importance of humidity control in ensuring reliable and optimal performance for MoS2-based electronic and electrochemical devices and provides crucial insights into the surface engineering of MoS2, which are relevant to the study of other two-dimensional transition metal dichalcogenide materials and their applications.

     
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  2. Atomic force microscope (AFM)-based nanomanufacturing offers an affordable and easily deployable method for fabricating high-resolution nanopatterns. This study employs a comprehensive design of experiment (DOE) approach to investigate the effects of various parameters, such as voltage, speed, and vibration axis, on the width and depth of lithography patterns using electrical field and vibration-assisted lithography on PEDOT: PSS films. The DOE explores the effect of voltage and speed on the process of electrical field and vibration-assisted AFM-based nanopatterning in two vibration trajectories: a circular trajectory employing X and Y axis vibration and a reciprocating trajectory employing Y axis vibration. The results indicate that using circular XY-vibration with a low stiffness contact probe and optimized speed and voltage factors results in higher depth and width of the lithography patterns compared to Y-vibration alone at the same parameters as expected. In both cases, pattern width was dominantly controlled by the voltage. Regarding depth, in XY-vibration, the speed of the tip is the most significant factor, while for Y-vibration, voltage plays the most significant role. It is noteworthy that there is a minimum threshold of speed that can produce a pattern; for example, the high-speed level that produced patterns in the circular trajectory (XY-vibration) did not produce patterns in reciprocating motion (Y-vibration). In conclusion, the study demonstrates the significant impact of voltage, speed, and axis on the width and depth of the lithography patterns. These findings can be instrumental in developing and understanding AFM-based high-resolution nanofabrication techniques. 
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    Free, publicly-accessible full text available October 15, 2025
  3. The atomic force microscopy (AFM) technology is a promising method for nanofabrication due to the high tunability of this affordable platform. The quality inspection and control significantly impact the manufacturing effectiveness for realizing the functionality of the achieved nanochannel. Particularly, the surface characteristics of nanochannel sidewalls, which play a significant role in determining the quality of the nanomachined products, can not be accurately captured using conventional surface integrity metrics (e.g., surface roughness). Therefore, it is necessary to propose a method to quantitatively characterize the surface morphology and detect the abnormal parts/regions of the nanochannel sidewall. This paper presents a statistical process control approach derived from the self-affine fractal model to detect the sidewall surface anomalies. It evaluates changes in the self-affine fractal model parameters (standard deviation, correlation length, and roughness exponent), which can be used to signify the changes on the sidewall surface; the statistical distributions of these parameters are derived and used to develop control charts to allow inspection of the sidewall morphology. The approach was tested on the AFM-based nanomachined samples. The results suggest that the presented approach can effectively reflect the abnormal regions on the machined parts, which opens up a new avenue toward guiding the quality control and rework for process improvement for AFM-based nanomachining. 
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    Free, publicly-accessible full text available October 15, 2025
  4. Understanding the kinetics of nanobubbles encapsulated by ultrathin two-dimensional (2D) layered van der Waals crystal membranes on atomically flat substrates is important to the applications of 2D materials and the pursuit of 2D nanobubble technologies. Here, we investigate the controlled motion of monolayer molybdenum disulfide (MoS2)-encapsulated nanobubbles on flat hexagonal boron nitride substrates using atomic force microscopy (AFM). Our study reveals a distinct transition from standstill bubble deformations to stable, stepwise bubble translations on flat substrates. The membrane tension-dominated 2D nanobubble behaves like an elastic soft body in its collision interaction with the AFM tip. This delicate motion-control technique enables neighboring 2D nanobubbles to move closer and eventually coalesce into larger nanobubbles. These findings pave the way for high-precision manipulation of nanobubbles and facilitate the exploration of their emerging applications.

     
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    Free, publicly-accessible full text available September 9, 2025
  5. Vibration-assisted atomic force microscopy (AFM)-based nanomachining is a promising method for the fabrication of nanostructures. During mechanical nanomachining, the geometry of the tooltip and workpiece interface is sensitive to variations in the depth of cut, the material grain size, and system vibrations; understanding the underlying uncertainties is essential to improve the process capability. This paper investigates process uncertainties and their impacts on the achieved surface geometries based on an experimental study of AFM-based nanomachining. The variations and biases of the achieved surface characteristics (compared to the theoretical geometries) are observed and identified as the torsional deflections on the AFM probe. A physical-based model combined with the Kriging method is reported to capture such uncertainties and estimate the surface finish based on different process parameters. 
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    Free, publicly-accessible full text available March 12, 2025
  6. The vibration-assisted atomic force microscope (AFM)-based nanomachining offers a promising opportunity for low-cost nanofabrication with high tunability. However, critical challenges reside in advancing the throughput and the quality assurance of the process due to extensive offline experimental investigations and characterizations, which in turn hinders the wide industry applications of current AFM-based nanomachining process. Hence, it is necessary to create an in-process monitoring for the nanomachining to allow real-time inspection and process characterizations. This paper reports a sensor-based analytic approach to allow real-time estimations of the AFM-based nanomachining process. The temporal-spectral features of collected acoustic emission (AE) sensor signals are applied to predict the depth morphology of nanomachined trenches under different machining conditions. The experimental case study suggests that the most significant frequency domain information from AE sensor can accurately predict (R-squared value around 92%) the nanomachined depth profile. It, therefore, breaks the current limitation of characterization tools at the nanoscale precision level, and opens up an opportunity to allow real-time estimation for quality inspection of vibration-assisted AFM-based nanofabrication process. 
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  7. Lakhtakia, Akhlesh ; Bukkapatnam, Satish T. (Ed.)
    The atomic force microscope (AFM)-based nanomachining has the potential for highly customized nanofabrication due to its low cost and tunability. However, the low productivity and issues related to the quality assurance for AFM-based nanomachining impede it from large-scale production due to the extensive experimental study for turning process parameters with time-consuming offline characterizations. This work reports an analytic approach to capturing the AE spectral frequency responses from the nanopatterning process using vibration-assisted AFM-based nanomachining. The experimental case study suggests the presented approach allows characterizations of subtle variations on the AE frequency responses during the nanomachining processes (with overall 93% accuracy), which opens up the chance to explain the variations of the nano-dynamics using the senor-based monitoring approach for vibration-assisted AFM-based nanomachining. 
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  8. Continuum mechanics break down in bending stiffness calculations of mono- and few-layered two-dimensional (2D) van der Waals crystal sheets, because their layered atomistic structures are uniquely characterized by strong in-plane bonding coupled with weak interlayer interactions. Here, we elucidate how the bending rigidities of pristine mono- and few-layered molybdenum disulfide (MoS 2 ), graphene, and hexagonal boron nitride (hBN) are governed by their structural geometry and intra- and inter-layer bonding interactions. Atomic force microscopy experiments on the self-folded conformations of these 2D materials on flat substrates show that the bending rigidity of MoS 2 significantly exceeds those of graphene or hBN of comparable layers, despite its much lower tensile modulus. Even on a per-thickness basis, MoS 2 is found to possess similar bending stiffness to hBN and is much stiffer than graphene. Density functional theory calculations suggest that this high bending rigidity of MoS 2 is due to its large interlayer thickness and strong interlayer shear, which prevail over its weak in-plane bonding. 
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