Atomic Force Microscopy Research Articles

Preparation of Atomically Smooth SrTiO₃ Substrates

SrTiO3 has been used as a substrate to grow thin films of materials including high-temperature superconductors such as cuprates, ferromagnetic oxides such as manganites, and ferroelectric oxides such as BaTiO3. The use of SrTiO3 as a substrate for the deposition of manganite thin films provides an excellent template for observing unique effects observed only in ferromagnets, such as the anomalous and planar Hall effects. The as-received SrTiO3 substrates require a process that prepares atomically smooth surfaces for thin film deposition. This study focuses on using ultrasonic cleaning, water annealing, and thermal annealing in air to prepare SrTiO3 substrate surfaces and verifying their smoothness at the atomic scale using atomic force microscopy.

Heteroepitaxial Growth of NiO Thin Films on (‐201) β‐Ga2O3 by Mist Chemical Vapor Deposition

The growth of NiO epitaxial thin films on (‐201) β‐Ga2O3 by mist chemical vapor deposition (CVD) and the effects of carrier gas selection (N2 and O2) and substrate preannealing treatment on the structural and morphological properties on the grown thin films are explored. X‐ray diffraction analysis reveals successful epitaxial growth with the orientation relationship (111) NiO [0‐11] || (‐201) β‐Ga2O3 [010]. As a carrier gas, O2 results in single‐domain NiO films while N2 leads to the formation of rotational domains. Atomic force microscopy and field‐emission scanning electron microscopy confirm the lateral growth of NiO films, thus highlighting the importance of substrate preannealing at 1200 °C in oxygen atmosphere to obtain flat, high‐quality films. The results demonstrate that the method of mist CVD combined with appropriate substrate preparation and carrier gas selection is effective for the growth of high‐quality NiO/β‐Ga2O3 heterostructures. This achievement opens new possibilities for the development of wide‐bandgap p–n heterojunctions, potentially advancing the field of high‐power oxide‐based electronic devices.

Electric Double Layer and Structure of the Li-ion Battery Separator/Liquid Electrolyte Interface Detected with the Atomic Force Microscope

Electric Double Layer and Structure of the Li-ion Battery Separator/Liquid Electrolyte Interface Detected with the Atomic Force Microscope

Reduction in Optical Feedback Noise of Atomic Force Microscopy by High-Frequency Current Modulation

Introduction: With the advancement of technology, nanotechnology has emerged as a prominent research field. The Atomic Force Microscope (AFM) serves as a vital tool in nanoscience and technology, playing an indispensable role across various domains. Method: However, in the AFM photoelectric sensing system, the optical feedback noise from the beam deflection method can lead to inaccuracies in signal identification and analysis, impacting the accuracy and reliability of AFM measurements. To mitigate this interference, this study proposes a highfrequency current superposition system aimed at reducing optical feedback noise. By superimposing high-frequency currents, the semiconductor laser transitions from a single-mode to a multi-mode operational state, thereby altering its mode of operation and consequently reducing optical feedback noise during sensing. Initially, mathematical modeling and simulation analysis were conducted on the high-frequency current superposition noise reduction system to examine the impact of high-frequency current on the intensity noise of the semiconductor laser. Subsequently, the design of the high-frequency current superposition noise reduction system was outlined, encompassing the development of a constant current drive circuit, a voltage-controlled oscillator circuit, and a biasing circuit. Finally, the high-frequency current superposition noise reduction system underwent testing. Results: During the high-frequency current superposition noise reduction test, the system's Signal-to-Noise Ratio (SNR) increased from 15.57 dB to 17.81 dB, and the system's noise peak-to-peak value decreased from 8 mV to 6 mV. Analysis of the superposition frequency and noise reduction effect determined the optimal superposition frequency of the AFM photoelectric sensor system to be 400 MHz. Characterization experiments of the high-frequency superposition noise reduction system compared the clarity of Escherichia coli images before and after noise reduction. Conclusion: The aforementioned experimental results demonstrated that high-frequency current superposition is an effective noise reduction method capable of mitigating optical noise in the AFM photoelectric sensing system.

Tuning the magnetic properties of ultrathin magnetic films with MgO as the buffer layer

To minimize the screening effect of a metallic ferromagnetic film and improve the effectiveness of electric field modulation, high-quality ultrathin magnetic film is one of the critical prerequisites. Here ultrathin magnetic films and synthetic antiferromagnetics (SAFs) are deposited on SiO2 substrates at room temperature using the magnetron sputtering. Atomic force microscopy is used to characterize the roughness of MgO, Nb, Ru, W, and CoFeB films, revealing their atomic-level flatness, with root mean square roughness values below 0.3 nm, which are crucial in the subsequent preparation of ultrathin SAF to achieve high-quality interfaces. The results from the magneto-optical Kerr microscopy suggest that when MgO is 1.48 nm, ultrathin 0.6 nm CoFeB exhibits stable room-temperature perpendicular magnetic anisotropy (PMA) and there is a correlation between room-temperature ferromagnetism and MgO thickness. For SAFs, ultrathin 0.6 nm CoFeB-based SAF exhibits room-temperature antiferromagnetism via the Ruderman-Kittel-Kasuya-Yosida interaction mechanism. The exchange coupling field demonstrates that the transition between ferromagnetic coupling and antiferromagnetic coupling can be regulated by adjusting both the thickness of the non-magnetic spacer layer and the CoFeB layer. This work lays the ground for the potential applications of high-density storage and efficient electric field modulation of ferromagnetic multilayers for improving energy efficiency.

Abnormal Response of Indirect Excitons to Non‐Uniform Elastic Strain in MoS2 Flakes

AbstractRegulating the electronic structures and carrier dynamics in 2D materials via elastic strain is a fascinating avenue for tailoring their optoelectronic properties at atomic scale. Here, the abnormal response of indirect excitons to non‐uniform elastic strain in MoS2 flakes is reported. The non‐uniform elastic strain in the MoS2 flakes is introduced by transferring them to pre‐prepared convex cross structures on a SiO2/Si substrate, where the topography and strain distribution are determined by atomic force microscopy and Raman spectroscopy, respectively. It is observed that the emission energy of the indirect excitons shows an unexpected blue‐shift followed by a red‐shift with increasing the local tensile strain, which is in sharp contrast to the linear red‐shift of the direct excitons. Density functional theory calculations reveal that the abnormal energy shift of the indirect excitons in the MoS2 flakes arises from the strain‐induced competition between two indirect bandgap transitions and the spatial exciton funnel effect in the non‐uniform strain field. This work provides new insights into the elastic strain effect on the indirect excitons in 2D semiconductors, which possesses potential applications in flexible optoelectronic devices.

The application of KMnO4 in reverse flotation separation of chalcopyrite and talc and its selective depression mechanism

Talc exhibits excellent floatability and, as a major silicate gangue mineral associated with chalcopyrite, significantly obstructs the purification and smelting of chalcopyrite. This study investigates the reverse flotation separation of chalcopyrite and talc using KMnO4 as a depressant and DDA (dodecylamine) as a collector within a reverse flotation system. Single mineral flotation experiments show that after adding KMnO4, the recovery of chalcopyrite in 38–74 μm is only 6.86 %, whereas the recovery of talc in 45–106 μm and 25–45 μm are 93.47 % and 89.25 %, respectively. Further experiments with artificially mixed ores demonstrate that KMnO4 effectively achieves the separation of chalcopyrite and talc. The depression mechanism of KMnO4 on chalcopyrite and talc was analyzed using Zeta potential, contact angle measurement, AFM (atomic force microscopy), FTIR (Fourier transform infrared spectroscopy), XPS (X-ray photoelectron spectroscopy), and DFT (density functional theory) calculations. Mechanistic analysis indicates that in an alkaline environment, chalcopyrite can undergo a redox reaction with KMnO4, forming hydrophilic hydroxide species (Cu(OH)2, Fe(OH)3) on the chalcopyrite surface, which depresses chalcopyrite flotation. In contrast, the surface properties of talc are relatively stable and difficult to react with KMnO4, which cannot depress the flotation of talc. Therefore, KMnO4 can be used as an efficient and selective depressant for the reverse flotation separation of chalcopyrite and talc.

The Influence of Temperature on the Spatial Distribution of AuNPs on a Ceramic Substrate for Biosensing Applications

In this study, we investigated the spatial distribution and homogeneity of gold nanoparticles (AuNPs) on an alumina (Al2O3; AAO) substrate for potential application as surface-enhanced Raman scattering (SERS) sensors. The AuNPs were synthesized through thermal treatment at 450 °C at varying times (5, 15, 30, and 60 min), and their distribution was characterized using field-emission scanning electron microscopy (FE-SEM) and scanning transmission electron microscopy (STEM). The FE-SEM and STEM analyses revealed that the size and interparticle distance of the AuNPs were significantly influenced by the duration of thermal treatment, with shorter times promoting smaller and more closely spaced nanoparticles, and longer times resulting in larger and more dispersed particles. Raman spectroscopy, using Rhodamine 6G (R6G) as a probe molecule, was employed to evaluate the SERS enhancement provided by the AuNPs on the AAO substrate. Raman mapping (5 µm × 5 µm) was conducted on five sections of each sample, demonstrating improved homogeneity in the SERS effect across the substrate. The topological features of the AuNPs before and after R6G incubation were analyzed using atomic force microscopy (AFM), confirming the correlation between a decrease in surface roughness and an increase in R6G adsorption. The reproducibility of the SERS effect was quantified using the maximum intensity deviation (D), which was found to be below 20% for all samples, indicating good reproducibility. Among the tested conditions, the sample synthesized for 15 min exhibited the most favorable characteristics, with the smallest average nanoparticle size and interparticle distance, as well as the most consistent SERS enhancement. These findings suggest that AuNPs on AAO substrates, particularly those synthesized under the optimized condition of 15 min at 450 °C, are promising candidates for use in SERS-based sensors for detecting cancer biomarkers. This could be attributed to temperature propagation promoted at the time of synthesis. The results also provide insights into the influence of thermal treatment on the spatial distribution of AuNPs and their subsequent impact on SERS performance.

Mitigation effect of a biodegradable surfactant N,N,N-trimethyl-2-(((hexadecyloxy)carbonyl)oxy)ethan-1-aminiumiodide for mild steel corrosion in 5% HCl: Experimental and theoretical insights

A cleavable cationic surfactant having carbonate linkage, N,N,N-trimethyl-2-(((hexadecyloxy)carbonyl)oxy)ethan-1-aminiumiodide referred to as THC was synthesised and characterized employing elemental analysis, FT-IR (Fourier Transform Infrared Spectroscopy), 1H NMR (Nuclear Magnetic Resonance) and 13C NMR. The extent of corrosion inhibition of THC was for the first time studied experimentally and theoretically on mild steel (MS) substrate in 5 % HCl solution at temperatures 303, 313, 323, 333, 343, 353 K. Experimental investigations include gravimetric analysis, potentiodynamic polarization (PDP) and electrochemical impedance analysis (EIS). THC provided maximum inhibition efficiency of 93.2 % at concentration of 1×10−4 M at 303 K which was further raised to 98.1 % at 353 K. PDP studies reveal that given surfactant is mixed type inhibitor. Surface studies such as contact angle measurement, AFM (Atomic Force Microscopy), SEM-EDX (Scanning Electron Microscope-Energy Dispersive X-ray Analysis), and XPS (X-ray Photoelectron Spectroscopy) were employed to justify the adsorption of inhibitor molecules on MS surface. Furthermore, biodegradability test on THC was done to support the environment friendly nature of the surfactant.

An optimisation of the internal roller burnishing process for magnesium composites using Taguchi Multi objective optimization method

Machining Metal Matrix Composites with conventional metal removal causes particle debonding and crack propagation. This paper has given enhancing results for magnesium silicon carbide Metal Matrix Composite using an internal roller burnishing process. The optimal process parameters are obtained using a full factorial design and Taguchi Multi Response optimization. The optimized parameters include a spindle speed of 500 rpm, a feed rate of 0.5 mm/rev, and a stock allowance of 0.03 mm. The resulting surface characteristics comprise a surface roughness of 0.1555 µm, an out of roundness of 0.0595 mm, and a surface hardness of 66.9 HV. Scanning electron and atomic force microscope, images analyze the surface topology. Auto parts like transfer case and steering components can use burnished components.

Low-Temperature Sintering of Colloidal Gold Nanoparticles by Salt Addition

AbstractGold nanoparticles synthetized by pulsed laser ablation in liquid with a mean diameter of 4 nm were joined together by adding potassium bromide solution at various concentrations. By increasing the salt concentration, there is a significant increase of the particle size up to a mean diameter of 18 nm. We have studied the nanoparticle merging by using atomic force and electron microscopy characterizations, also demonstrating that it is possible to deposit sintered nanoparticles on silanized substrates in a fast, simple, cost-effective, energy-saving method with relevance in industrial manufacturing.

Atomically Precise Control of Topological State Hybridization in Conjugated Polymers.

Realization of topological quantum states in carbon nanostructures has recently emerged as a promising platform for hosting highly coherent and controllable quantum dot spin qubits. However, their adjustable manipulation remains elusive. Here, we report the atomically accurate control of the hybridization level of topologically protected quantum edge states emerging from topological interfaces in bottom-up-fabricated π-conjugated polymers. Our investigation employed a combination of low-temperature scanning tunneling microscopy and spectroscopy, along with high-resolution atomic force microscopy, to effectively modify the hybridization level of neighboring edge states by the selective dehydrogenation reaction of molecular units in a pentacene-based polymer and demonstrate their reversible character. Density functional theory, tight binding, and complete active space calculations for the Hubbard model were employed to support our findings, revealing that the extent of orbital overlap between the topological edge states can be finely tuned based on the geometry and electronic bandgap of the interconnecting region. These results demonstrate the utility of topological edge states as components for designing complex quantum arrangements for advanced electronic devices.

Effects of copper on hydroxyapatite thin films by pulsed laser deposition on silicon

AbstractThis study deals with the effect of Cu on hydroxyapatite (HAp) thin films on silicon substrates prepared by pulsed laser deposition (PLD) technique for Cu concentrations ranging from 0 to 0.8 wt.%. Fourier transform infrared spectroscopy and Raman spectroscopy provide additional evidence of HAp in the films, which exhibit characteristic HAp bands such as the 960 cm−1 phosphate ion band. The X‐ray diffraction patterns confirm the presence of HAp, without copper‐related peaks, suggesting that it is not incorporated into the HAp lattice, which is present as an amorphous phase. X‐ray photoelectron spectroscopy confirms the presence of Cu on the HAp thin films, possibly related to the adsorption of Cu2+ on HAp surfaces through electrostatic or interactions with (PO4)3− groups. Atomic force microscopy shows that the roughness of the films varies depending on the presence or absence of copper ions. Finally, density functional theory and kinetic Monte Carlo simulations explain the effects of atomic diffusion on roughness and HAp clustering. These changes correlate with the contact angle values, indicating the formation of hydrophobic films due to copper inclusions.

Understanding AFM-IR Signal Dependence on Sample Thickness and Laser Excitation: Experimental and Theoretical Insights.

Photothermal induced resonance (PTIR), also known as atomic force microscopy-infrared (AFM-IR), enables nanoscale IR absorption spectroscopy by transducing the local photothermal expansion and contraction of a sample with the tip of an atomic force microscope. PTIR spectra enable material identification at the nanoscale and can measure sample composition at depths >1 μm. However, implementation of quantitative, multivariate, nanoscale IR analysis requires an improved understanding of PTIR signal transduction and of the intensity dependence on sample characteristics and measurement parameters. Here, PTIR spectra measured on three-dimensional printed conical structures up to 2.5 μm tall elucidate the signal dependence on sample thickness for different IR laser repetition rates and pulse lengths. Additionally, we develop a model linking sample thermal expansion dynamics to cantilever excitation amplitudes that includes samples that do not fully thermalize between consecutive pulses. Remarkable qualitative agreement between experiments and theory demonstrates a monotonic increase in the PTIR signal intensity with thickness, with decreasing sensitivities at higher repetition rates, while signal intensity is nearly unaffected by laser pulse length. Although we observe slight deviations from linearity over the entire 2.5 μm thickness range, the signal's approximate linearity for bands of sample thicknesses up to ≈500 nm suggests that samples with comparably low topographic variations are most amenable to quantitative analysis. Importantly, we measure absorptive undistorted profiles in PTIR spectra for strongly absorbing modes, up to ≈1650 nm, and >2500 nm for other modes. These insights are foundational toward quantitative nanoscale PTIR analyses and material identification, furthering their impact across many applications.

Air Fixation and AFM: A Comparative Study of Nanoparticle-Induced Topographical Changes in Lung Cells

Gold nanoparticles (AuNPs) have emerged as promising agents in biomedical applications due to their unique physicochemical properties. This study investigates the cellular interactions of AuNPs with A549 (non-small cell lung adenocarcinoma) and BEAS-2B (normal bronchial epithelial) cell lines. AuNPs were synthesized via the citrate reduction method, resulting in 20, 50, and 70 nm particles. Cells were incubated with AuNPs for increasing durations (30 minutes, 4 hours, and 24 hours). Post-incubation, cells were washed with PBS, air-fixed, and subsequently analyzed using Atomic Force Microscopy (AFM) to obtain detailed topographical maps. AFM imaging revealed distinct interactions between AuNPs and the two cell lines. A549 cells displayed darker regions on the cell surface, indicative of topographical depressions likely resulting from nanoparticle-induced membrane collapse. In contrast, BEAS-2B cells did not exhibit such depressions, which is consistent with the literature that suggests cancer cells are mechanically softer than normal cells. The surface roughness analysis results indicated that the preservation of surface integrity post-fixation validates the air-fixation methodology for obtaining reliable mechanical data from AFM analyses.

Study of the surface features of palladium-based alloys using atomic force microscopy and magnetic force microscopy

The surface state of palladium-based alloys, specifically Pd–6.0In–0.5Ru and Pd–7.0Y (the element content is given in wt.%) has been studied using magnetic force microscopy (MFM) and atomic force microscopy (AFM). The study was conducted within the framework of the current trend to enhance the safety of hydrogen separation and storage. The samples for the study were made of high-purity metals through arc alloying. They underwent reversible hydrogen alloying to investigate the impact of internal deformation of metal systems on their structure-sensitive properties. The study demonstrates the characteristics of the sample surface morphology and domain structure before and after hydrogenation. The local magnetic properties of alloy surfaces have been clarified, and their changes as a result of hydrogen exposure have been identified.

Enhanced hydrophobicity of polyurethane coating for steel protection through replication and nanomaterial integration

Polyurethanes (PU) are widely used in corrosion protection, anti-biofouling coatings, and self-cleaning glass, yet their low hydrophobicity poses durability challenges. This study addresses this by enhancing PU coatings’ hydrophobicity by refining surface roughness and forming tailored porous structures. Using drop, spin, dip, and spray coating techniques, hydrophobic PU coatings were fabricated on 304 steel plates. To further enhance hydrophobicity, 0.5 w/v% graphene nanoplatelets (GNP) were introduced into the coatings. Additionally, stainless-steel 500 mesh was incorporated to create patterned surfaces, increasing surface roughness and tailoring the porous structure. The analysis included optical and scanning electron microscopy, water contact angle (WCA) measurements, Fourier transform infrared spectroscopy, electrochemical corrosion tests, and atomic force microscopy. Incorporating GNP notably increased WCA by 20–23° and reduced corrosion rates in a 3.5% NaCl solution. Likewise, applying stainless-steel mesh improved surface roughness, raising WCA by 3-8° and decreasing corrosion rates. The study observed changes in porous structure, with pore size reduction correlating with increased roughness and decreased corrosion rates upon mesh application and GNP addition. This comprehensive examination highlights the potential of PU coatings for various applications and underlines the importance of tailored porous structures in enhancing their performance and versatility. Spin coating emerged as the optimal technique, yielding uniform, defect-free coatings with the highest WCA.

Effect of hybrid sizings on the surface morphology, mechanical behavior of basalt fibers, and fiber/epoxy composite properties

AbstractIn the present study, the basalt fibers (BFs) were treated with hybrid sizings consisting silane coupling agent (3‐Glycidoxypropyl)trimethoxysilane, and silicon dioxide nanoparticles (SNPs). Using acetone washing and heat treatment, the commercial sizing previously on the BFs was removed. Next, the fibers were dip‐coated, and silanes condensed on the surface of the fibers. Fiber samples were characterized using thermogravimetric analysis (TGA), atomic force microscopy (AFM), X‐ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). The test findings demonstrate that acetone extraction was an effective way to remove sizings. The AFM analysis and SEM micrographs demonstrate that SNP and silane particles were dispersed uniformly across the fiber surface. The single fiber tensile testing results indicated that the deposition of hybrid sizings enhanced the fibers strength. Because of the better adhesion between the fiber and epoxy, the hybrid sizings also improved the flexural strength by 22.28% and the interlaminar shear strength by 20.75%.Highlights Hybrid sizings (silanes and nano‐particles) on the basalt fiber surface. Characterization of the sizings and understanding of surface morphology. Hybrid sizings resulted in better tensile strength. Failure mechanisms of the fibers were observed using fractography. The effect of hybrid sizing on ILSS and flexural properties was observed.

Complement-mediated killing of Escherichia coli by mechanical destabilization of the cell envelope.

Complement proteins eliminate Gram-negative bacteria in the blood via the formation of membrane attack complex (MAC) pores in the outer membrane. However, it remains unclear how outer membrane poration leads to inner membrane permeation and cell lysis. Using atomic force microscopy (AFM) on living Escherichia coli (E. coli), we probed MAC-induced changes in the cell envelope and correlated these with subsequent cell death. Initially, bacteria survived despite the formation of hundreds of MACs that were randomly distributed over the cell surface. This was followed by larger-scale disruption of the outer membrane, including propagating defects and fractures, and by an overall swelling and stiffening of the bacterial surface, which precede inner membrane permeation. We conclude that bacterial cell lysis is only an indirect effect of MAC formation; outer membrane poration leads to mechanical destabilization of the cell envelope, reducing its ability to contain the turgor pressure, leading to inner membrane permeation and cell death.

Macroscopic perspective on phase transition behavior of natural single-crystal graphite under different pressure environments

Comprehensive understanding of the direct transformation pathway from graphite to diamond under high temperature and high pressure has long been one of the fundamental goals in materials science. Despite considerable experimental and theoretical progress, current experimental studies have mainly focused on the local microstructural characterizations of recovered samples, which has certain limitations for high-temperature and high-pressure products, which often exhibit diversity. Here, we report on the pressure-induced phase transition behavior of natural single-crystal graphite under three distinct pressure-transmitting media from a macroscopic perspective using in situ two-dimensional Raman spectroscopy, scanning electron microscopy, and atomic force microscopy. The surface evolution process of graphite before and after the phase transition is captured, revealing that pressure-induced surface textures can impede the continuity of the phase transition process across the entire single crystal. Our results provide a fresh perspective for studying the phase transition behavior of graphite and greatly deepen our understanding of this behavior, which will be helpful in guiding further high-temperature and high-pressure syntheses of carbon allotropes.