Characterization Of Micro Research Articles

Synthesis and characterization of micro-/nano-α-Fe2O3 for photocatalytic dye degradation.

Photocatalytic activity using micro-/nano-α-Fe2O3 on a large scale was carried out using a sol-gel autocombustion method. A degradation time of 60 min was noted for 50 mg of the catalyst. Post characterization, this catalyst system showed a degradation of about 53% (rate = 2.60 × 10-3 min-1) and 17% (rate = 1.38 × 10-2 min-1) under sunlight and up to 45% (rate = 1.13 × 10-3 min-1) and 7% (rate = 1.20 × 10-2 min-1) under a 400 W UV lamp for rhodamine 6G (R6G) and crystal violet (CV), respectively. Sunlight has a broad spectrum of light; it greatly accelerates the degradation process and creates ideal conditions for the reaction to occur. The rate of photocatalytic dye degradation of α-Fe2O3 without Fenton's reagent was found to be 7.84 × 10-3 min-1 in the presence of external air provided (in the photocatalytic setup) through a bubbler and 3.23 × 10-3 min-1 in the absence of the bubbler.

Analysis and Characterization of Micro–Nano Pores in Coal Reservoirs of Different Coal Ranks

Coalbed methane represents a promising source of clean and efficient unconventional energy. The intricate network of micro–nano pores within coal serves as the primary adsorption space for gas, contributing to the complexity of gas migration channels. In this study, based on the box-counting method, three coal samples representing low, medium, and high ranks were subjected to high-precision micro-CT scanning and nano-CT scanning to generate three-dimensional (3D) pore network models using Avizo visualization software. This facilitated the accurate and quantitative characterization of the micro–nano pore structures within coal reservoirs. The results indicated that the face rate distribution range of each sample was large, indicating relatively strong heterogeneity in each sample. The volume fractal dimension of each sample, determined through micro–nano-CT scanning, was around 2.5, while the surface fractal dimension exhibited oscillatory characteristics with moderate uniformity. The pore equivalent radius and throat equivalent radius distributions were unimodal across all the samples, with the micro-CT scanning revealing a concentration primarily within the range of 100–400 μm for the pore equivalent radius and within 200 μm for the throat equivalent radius. Conversely, the nano-CT scanning exhibited concentrations primarily within the range of 500–2500 nm for the pore equivalent radius and within 2000 nm for the throat equivalent radius. The analysis of the 3D reconstruction structures indicated that the middle-rank coal exhibited more developed large–medium pores compared with the low-rank and high-rank coal, while the low-rank and high-rank coal exhibited relatively more micro–small pores. Furthermore, the low-rank coal exhibited the fewest number of pores but the largest average pore equivalent radius and throat radius. Additionally, the middle–high-rank coal exhibited a relatively larger number of pores. Despite the complex topological structures observed in each sample, a significant proportion indicated a coordination number of 0–20, indicating excellent connectivity within the coal samples. This study is conducive to the optimization of coalbed methane surface development blocks and the formulation of reasonable development plans.

Quantum genetic algorithm assisted high speed and precision pump-probe thermoreflectance characterization of micro-/nano-structures

The rapid and precise extraction of thermophysical properties remains an enormous challenge in pump-probe thermoreflectance, and quantum algorithms present significant potential for addressing thermal transport problems. This paper introduces an innovative application of the quantum genetic algorithm to the fitting of experimental data from pump-probe thermoreflectance. Initially, a physical model based on the thermal transmission matrix is developed to compute the heat transport of multilayer micro-/nano-structures. The quantum genetic algorithm is then employed for multiparameter optimization in the extraction of thermophysical properties and tested on three samples. Both simulation and experimental results demonstrate that the quantum genetic algorithm assisted pump-probe thermoreflectance, capable of extracting thermophysical properties with high precision in just one minute, is approximately 30 times faster than the conventional method and 10 times faster than the genetic algorithm. Furthermore, measurement sensitivity and algorithmic randomness are analyzed. The reasons behind the phenomenon of equivalent fitting results and the indication of non-convex optimization are also presented.

Detection and characterization of micro‐ and nano‐plastics in wastewater: Current status of preparatory & analytical techniques

AbstractMicro‐ and nano‐plastics (MNPs) are ubiquitous emerging pollutants that have gained global traction due to their persistent nature and potential risks to the environment and human health. The physico‐chemical properties of MNPs such as size, shape, density, surface charge and hydrophobicity are quite different from macro‐plastics, which render them unique behavior exemplified by high rate of diffusion, high mobility, easy uptake by organisms, high toxicity, and potential of bioaccumulation. Human exposure to MNPs causes serious health impacts including apoptosis, necrosis, inflammation, oxidative stress, metabolic disorders, and hampered immune responses. The hazardous nature and high persistence of MNPs in the environment necessitates accelerated studies focused upon their detection, quantification, impact analysis, and risk assessment. All kinds of wastewaters whether municipal, agricultural, or industrial, consist of significant loads of MNPs and act as secondary source of MNP pollution in groundwater and soil. Wastewater is highly complex in composition and there are several impediments in the accurate detection and identification of MNPs in this matrix owing to the in‐efficient sampling methods, lack of standardized methodologies, and non‐reproducibility of data. This review provides an overview of currently available techniques for sampling, detection, identification, and characterization of MNPs in wastewater. A critical commentary on the challenges and limitations of these techniques has been given and strategic combinatorial methods have been suggested for efficient and reliable MNP analysis in wastewater samples. The article also highlights novel sensor‐based methods enabling rapid and accurate detection of MNPs in wastewater.

Scanning electrochemical probe microscopy: towards the characterization of micro- and nanostructured photocatalytic materials.

Platinum-black (Pt-B) has been demonstrated to be an excellent electrocatalytic material for the electrochemical oxidation of hydrogen peroxide (H2O2). As Pt-B films can be deposited electrochemically, micro- and nano-sized conductive transducers can be modified with Pt-B. Here, we present the potential of Pt-B micro- and sub-micro-sized sensors for the detection and quantification of hydrogen (H2) in solution. Using these microsensors, no sampling step for H2 determination is required and e.g., in photocatalysis, the onset of H2 evolution can be monitored in situ. We present Pt-B-based H2 micro- and sub-micro-sized sensors based on different electrochemical transducers such as microelectrodes and atomic force microscopy (AFM)-scanning electrochemical microscopy (SECM) probes, which enable local measurements e.g., at heterogenized photocatalytically active samples. The microsensors are characterized in terms of limits of detection (LOD), which ranges from 4.0 μM to 30 μM depending on the size of the sensors and the experimental conditions such as type of electrolyte and pH. The sensors were tested for the in situ H2 evolution by light-driven water-splitting, i.e., using ascorbic acid or triethanolamine solutions, showing a wide linear concentration range, good reproducibility, and high sensitivity. Proof-of-principle experiments using Pt-B-modified cantilever-based sensors were performed using a model sample platinum substrate to map the electrochemical H2 evolution along with the topography using AFM-SECM.

Characterization and quantification of microplastics and organic pollutants in mussels by microwave-assisted sample preparation and analytical pyrolysis

We developed a method to isolate and quantify various classes of both non-polymeric contaminants and polymers from mussel flour using microwave-assisted extraction/digestion and analytical pyrolysis-GC-MS.

Influence of electron beam irradiation on nanoscale adhesion during colloidal probe experiments inside the scanning electron microscope

Scanning electron microscope is not only a versatile visualization and characterization tool for nanomaterials, but it is also widely used for visual feedback during assembly and manipulation of micro- and nanoparticles, novel devices based on 2D and 1D materials, and microrobots. Due to increase in the surface-to-volume ratio, adhesion forces play a significant role in micro- and nanorobotic applications. We investigate the quantitative effect of electron beam irradiation on nanoscale adhesive interactions between different end effector types and plain substrates. For this purpose, we use an interferometry-based force measurement setup integrated into the chamber of a scanning electron microscope capable of a subnano Newton force resolution. We provide quantitative results for the influence of the electron beam on the adhesion forces depending on the exposure dose, geometrical configuration in which it is applied, as well as on the material of the end effector. Simulation results, atomic force microscope adhesion measurements, and measurements with piezoresistive cantilevers serve as references. Our findings indicate that the electron beam influences the adhesive interaction not only in the case of insulating probes but also for well-grounded conducting and semiconducting probes. Its influence can range from several 10% to several 100% in comparison to the adhesion values measured with an atomic force microscope in an ambient atmosphere and no charged particle beam is applied. Moreover, it is shown that the influence of a charged particle beam is a multidimensional phenomenon that depends on several factors such as end effector and substrate material, geometry and aspect ratio of the end effector, geometrical configuration between particle beam and probe–sample arrangement, as well as exposure dose and field of view. We provide recommendations for handling and characterization of micro- and nano-objects using end effectors under the influence of charged particle beams: not to rely on adhesion values acquired in different environmental and exposure conditions, not to expect the application of conductive materials and grounding to completely avoid the effect of charged particle beams, and to be aware that charged particle beams can lower or increase the adhesion force in vacuum depending on material properties, among others.

Role of a 3D Nanoskeleton in Hindering Electrical Tree Growth in Nanocomposites: Insights from in Situ Self-Fluorescence Imaging.

Despite the proposal of nanodielectrics in 1994, the impact of nano- and microstructures on composite performance is still not completely understood. A key reason for this knowledge gap is the lack of in situ characterization of micro- and nanoscale structures within materials. In this study, we observed the self-excited fluorescence of a microscale-damaged microchannel inside a composite under the influence of an electric field. Furthermore, we conducted in situ imaging of the internal microstructures and discharge channels in the composite utilizing external laser excitation. The imaging results reveal that the electrical treelike damage in the composites grows with a single channel under the guidance of the nanoskeleton embedded in the matrix, which demonstrates that the three-dimensional (3D) nano-order skeleton hinders the development of electrical trees. Furthermore, we analyzed the nanoskeleton intervention's enhancement mechanism on the insulation properties of the composites. This work aids in the precision imaging-guided structural design of nanodielectrics.

Size and environment: The effect of phonon localization on micro-Brillouin imaging

Specifically designed samples have been analyzed to test the ability of Brillouin spectroscopy to provide reliable mechanical characterization of micro and nano-objects. The selected samples are polymeric films, whose transversal sizes from hundreds of nano- to some micro-meters cover the entire range of length-scales relevant in Brillouin scattering process. The experimental data highlight how, the size of the extended collective oscillation (acoustic phonons, in brief) is the lowest spatial resolution reachable in Brillouin mechanical characterization. Conversely, in the limit condition of phonon confinement, the technique provides the mechanical properties of nano-objects whose characteristic size is comparable with the phonon wavelength (⁓300 nm). Investigating acoustically heterogeneous materials, both size of heterogeneity and acoustic mismatch between adjacent regions are shown to be relevant in shaping the Brillouin response. In particular, a transition from a confined to a non-confined condition is obtained modulating the acoustic mismatch between the micro-objects and their local environment. The provided results and the derived analytic models for the data analysis will guide the interpretation of Brillouin spectra acquired in complex nano-structured samples such as cells, tissues or biomimetic materials. Our analysis can therefore generate new insights to tackle fundamental problems in mechanobiology or to characterize new bioengineered materials.

Residual oil start-up mechanism of polymer/surface dual flooding after polymer flooding in medium-high permeability reservoir

The remaining oil distribution and displacement mechanism of poly/surface dual flooding stage in medium and high permeability reservoir are not clear. In this paper, the reservoir conditions in Gangxi Area 3 of Dagang Oilfield were taken as the research object. Based on nuclear magnetic resonance and large model physical simulation experiment, the characterization of micro and macro residual oil start-up mechanism and enhanced oil recovery experiment were carried out respectively after polymer flooding poly/surface binary flooding. The experimental results suggest that polymer-surfactant flooding could increase the oil displacement efficiency by 12-29% after polymer flooding, and the contribution of porous to recovery degree is in the order of medium pore, large pore, and small pore. When the surfactant concentration is higher than 0.25%, the increase of oil displacement efficiency tends to be stable, and further enhancing oil recovery requires the expansion of sweep volume. Physical model experiments results show that medium permeability layer has the highest contribution to the recovery degree in the chemical flooding stage, and the displacement mechanism is mainly based on the synergistic effect of expanding sweep volume and improving displacement efficiency. The contribution of low permeability layer to recovery degree is next, and the displacement mechanism is mainly to expand sweep volume. The high permeability layer has the lowest contribution to the recovery degree, and the oil displacement mechanism is mainly to improve the oil displacement efficiency.

An Overview of Micro(Nano)Plastics in the Environment: Sampling, Identification, Risk Assessment and Control

Advances in urban infrastructure, a flourishing polymer sector, and more traffic have all contributed to a rise in micro(nano)plastics in the environment. Researchers are exploring the production, fate, toxicity threshold, and severity of micro(nano)plastic exposure. Albeit, understanding sampling protocols, preservation of samples, and characterization of micro(nano)plastics obtained from the different mediums (e.g., soil, water, air, and living bodies) is still challenging. Particularly identification of micro(nano)plastics, on the other hand, is restricted and limited to the typical generic definition of contaminating sources. In addition, before micro(nano)plastics degrade naturally, many challenges must be overcome, enhancing the need for research on assisted degradation. Thus, a systematic review is presented, which begins by discussing micro(nano)plastic identification, sampling, and handling; then showcases the environmental and health consequences and how to control them; finally, it discusses environmental micro(nano)plastics management options. According to studies, biological and chemical methods to break down micro(nano)plastics have risen in popularity. However, these methods often only cover one type of plastic. Furthermore, these solutions can transform polymers into micro(nano)plastics and may also produce byproducts, increasing environmental contamination risk. Therefore, control, prevention, and management strategies are all investigated to generate more realistic and long-term solutions. The literature suggests a combination of different microorganisms (e.g., different bacterial species) and different approaches (e.g., filtration with degradation) could be more effective in the treatment of micro(nano)plastics. Furthermore, according to the literature, relevant health risks associated with micro(nano)plastics to humans from various exposure routes are currently unclear. Likewise, standardization of methods supported with sophisticated state-of-the-art apparatus for detecting micro(nano)plastics is required. Overall, precision in micro(nano)plastic identification and treatment strategy selection is critical, and their usage should be regulated if their environmental behavior is not properly addressed.

Site-specific N-glycosylation characterization of micro monoclonal immunoglobulins based on EThcD-sceHCD-MS/MS.

Monoclonal immunoglobulin produced by clonal plasma cells is the main cause in multiple myeloma and monoclonal gammopathy of renal significance. Because of the complicated purification method and the low stoichiometry of purified protein and glycans, site-specific N-glycosylation characterization for monoclonal immunoglobulin is still challenging. To profile the site-specific N-glycosylation of monoclonal immunoglobulins is of great interest. Therefore, in this study, we presented an integrated workflow for micro monoclonal IgA and IgG purification from patients with multiple myeloma in the HYDRASYS system, in-agarose-gel digestion, LC-MS/MS analysis without intact N-glycopeptide enrichment, and compared the identification performance of different mass spectrometry dissociation methods (EThcD-sceHCD, sceHCD, EThcD and sceHCD-pd-ETD). The results showed that EThcD-sceHCD was a better choice for site-specific N-glycosylation characterization of micro in-agarose-gel immunoglobulins (~2 μg) because it can cover more unique intact N-glycopeptides (37 and 50 intact N-glycopeptides from IgA1 and IgG2, respectively) and provide more high-quality spectra than sceHCD, EThcD and sceHCD-pd-ETD. We demonstrated the benefits of the alternative strategy in site-specific N-glycosylation characterizing micro monoclonal immunoglobulins obtained from bands separated by electrophoresis. This work could promote the development of clinical N-glycoproteomics and related immunology.

Identification and Characterization of Micro and Mesoplastics Isolated from Commercially Important Marine Fishes of Pulicat Lake, Tamil Nadu, India

The investigation of microplastics have been carried out among the commercially important marine fishes at Pulicat lake waters. The gastrointestinal tract of fishes were isolated and experimented for further analysis to detect the presence of microplastics. The fishes viz., Nemipterus japonicus, Mugil cephalus, Scomberomorus guttatus, Terapon puta, Sardinella longiceps, Caranx ignobilis, Stolephorus indicus, Rastrelliger kanagurta, Eleuthronema tetradactylum, Alectis indica, Leiognathus sp., Trichiurus lepturus, Trachurus lathamni, Selaroides leptolepis and Terapon jarbua were examined in this study. The microplastics samples were confirmed with BrukerAlpha FTIR ATR spectrophotometer in order to confirm plastics functional groups. Out of the 16 plastic particles isolated, 8 particles were mesoplastics and the rest of them were microplastics. The FTIR-ATR peaks were confirmed C-H stretching and N- H stretching (polyamide), C-H stretching, O-H stretching or N-H stretching (poly lactic acid), CH group (polythene) and C-H stretching, C=O stretching and C-O stretching (polyester). The presence of microplastics in the fish from the sampling locations may be due to unmonitored dumping of wastes in the water. The presence of microplastics may affect the growth of fish which leads to poor commercial value. The future research should be aimed to evaluate the impact and the risk of microplastics to the fishes, environment as well as human beings and to create awareness among the people, as well as the fishermen.

Terahertz scattering-type near-field microscopy quantitatively determines the conductivity and charge carrier density of optically doped and impurity-doped silicon

A terahertz scattering-type scanning near-field optical microscope is used for nano-scale non-invasive conductivity measurements on bulk silicon samples. We first investigate the case where the density of charge carriers is determined by optical interband excitation. We show that the amplitude and phase of the near-field signal are reproduced by simulations based on an established near-field interaction model, which takes the Drude conductivity, ambipolar carrier diffusion, and known recombination properties of photo-excited carrier pairs in Si into account. This study is then extended to impurity-doped Si. We demonstrate that the phase of the near-field signal, which can easily be measured in absolute terms, allows us to quantitatively determine the conductivity of the specimens, from which the carrier density is derived based on the known carrier momentum relaxation time. A measurement at a single properly chosen terahertz frequency is sufficient. The technique proposed here holds promise for the spatially resolved quantitative characterization of micro- and nanoelectronic materials and devices.

Birefringence and scattering characterization using polarization sensitive quantum optical coherence tomography.

Polarization sensitive quantum optical coherence tomography (PS-QOCT) is used to characterize birefringence, scattering/absorption and path length differences in a flat transparent plastic sample. In this Letter, we present the first, to the best of our knowledge, experimental technique of PS-QOCT imaging and characterization of a birefringent material. Polarization sensitive coincidence rate of the entangled photons measured for each pixel and the 2D cross-sectional images are reconstructed. The technique described in this work has many potential applications in the characterization of micro and nano structures, including biological samples.

BL-02: a versatile X-ray scattering and diffraction beamline for engineering applications at Indus-2 synchrotron source.

A hard X-ray engineering applications beamline (BL-02) was commissioned recently and started operation in March 2019 at the Indian synchrotron source, Indus-2. This bending-magnet-based beamline is capable of operating in various beam modes, viz. white, pink and monochromatic beam. The beamline utilizes the X-ray diffraction technique in energy-dispersive and angle-dispersive modes to carry out experiments mainly focused on engineering problems, viz. stress measurement, texture measurement and determination of elastic constants inavariety of bulk as well as thin-film samples. An open-cradle six-circle diffractometer with ∼12 kg load capacity allows accommodation of a wide variety of engineering samples and qualifies the beamline as a unique facility at Indus-2. The high-resolution mode of this beamline is suitably designed so as to carry out line profile analysis for characterization of micro- and nano-structures. In the present article the beamline is described starting from the beamline design, layout, optics involved, various operational modes and experimental stations. Experiments executed to validate the beamline design parameters and to demonstrate the capabilities of the beamline are also described. The future facilities to be incorporated to enhance the capabilities of the beamline are alsodiscussed.

Review of Several Experimental Methods for Characterization of Micro- and Nano-Scale Pores in Cement-Based Material

Mechanical properties and durability of cement-based materials are largely affected by pore structures. This paper provides an overview of several experimental techniques to characterize pore size distribution and specific surface area, with focus on pores in calcium silicate hydrates. The reviewed experimental techniques are nitrogen and water vapor sorption isotherm, proton nuclear magnetic resonance (1H-NMR) and small-angle scattering (SAS). Different pretreatment methods are compared for sorption measurements. Pore size distribution and specific surface area are analyzed using data from different methods to understand difference and consistency of these methods. It is found that pore size distribution calculated from sorption isotherm is very sensitive to adsorption model. Though specific surface areas from different techniques are quite different from each other, they are all able to detect the microstructural alteration due to long-term drying.

6-DoF Full Robotic Calibration Based on 1-D Interferometric Measurements for Microscale and Nanoscale Applications

This article proposes an original approach for robotic calibration that is based on measurements along a single direction (1-D). Among all applications, the field of microrobotics and nanorobotics has been chosen as case study because of the strong needs for high positioning accuracy (10–100 nm typically) while measuring with sufficient resolution along multi-degrees of freedom (DoF) is still a fully open question. The 1-D measurements relying on Fabry–Perot (FP) interferences is used, and the proposed modeling of a 6-DoF nanopositioning robot enables to derive the measurement strategy as well as the identification procedure for both extrinsic and intrinsic parameters. Experimental investigations demonstrate that the approach is easy to implement, low cost, and enables to understand what are the main influential parameters onto positioning accuracy. They also conduct to very high accuracy in 6-DoF positioning; a positioning accuracy estimate of 50 nm and 0.004° has notably been obtained for the full pose (position and orientation, respectively) and can be held during several hours after the measurements. <italic xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">Note to Practitioners</i> —The motivation of this work is to give an answer to the growing needs for micro nanopositioning robots having a very high precision for applications in microassembly, in the characterization of micro and nano components or biological elements, or for minimally invasive surgery. The key contribution of the proposed work relies on the method proposed that enables to efficiently calibrate a serial 6-degree-of-freedom (DoF) robot using only 1-D interferometric measurements, which overcomes the need for multi-DoF, small size, and high-resolution sensors missing in commercial offers. Moreover, the behavior of such novel robotic solutions is not well known, difficult to model, and there is a clear lack of knowledge about the main influential parameters. The method proposed in this article notably enables to achieve the full calibration of the robot (all intrinsic and extrinsic parameters identified) to reach the best positioning accuracy. This first part takes times, and this article shows that it is then possible to adopt a less time taking procedure by only reidentifying extrinsic parameters and thus to hold these performances over long periods, typically a week.

Recent developments in mass spectrometry for the characterization of micro- and nanoscale plastic debris in the environment.

Development of analytical methods for the characterization (particle size determination, identification, and quantification) of the micro- and nanoscale plastic debris in the environment is a quickly emerging field and has gained considerable attention, not only within the scientific community, but also on the part of policy makers and the general public. In this Trends paper, the importance of developing and further improving analytical methodologies for the detection and characterization of sub-20-μm-range microplastics and especially nanoplastics is highlighted. A short overview of analytical methodologies showing considerable promise for the detection and characterization of such micro- and nanoscale plastic debris is provided, with emphasis on recent developments in mass spectrometry (MS)-based analytical methods. Novel hyphenated techniques combining the strengths of different analytical methods, such as field flow fractionation and MS-based detection, may be a way to adequately address the smallest fractions in plastic debris analysis, making such approaches worthwhile to be further explored.

Isolation and characterization of micro and nanocrystalline cellulose fibers from the walnut shell, corncob and sugarcane bagasse

The present study aims to extract and characterize the microcrystalline cellulose (MCC) present in different agro-industrial wastes such as walnut shells, corncob, and sugarcane bagasse. Moreover, it is also the aim of this study to convert MCCs to nanocrystalline cellulose fiber (NCCF), to demonstrate the difference in morphological, structural, thermal, and chemical natures. Corncob cellulose was observed to possess a loosely bounded linear bundle structure. Nanocrystalline cellulose fiber yield from walnut shell and sugarcane bagasse cellulose were higher than corncob cellulose. The thermal stability of cellulose was noted to be high for walnut shell NCCF. Nanocrystalline cellulose fiber of corncob and sugarcane bagasse was estimated to have a low thermal degradation temperature. All the MCCs and NCCFs produced from investigated cellulose sources were found to have type I cellulose. Functional group compositions of cellulose were observed to be intact for converted agro-based NCCF's.