Magnification Scanning Electron Microscopy Research Articles

Utilization of spent bleaching earth as green filler and plasticizer in the manufacture of rubber compounds for solid tire production

This study utilized spent bleaching earth (SBE) as a single form of filler and plasticizer in the manufacture of rubber components for solid tire vulcanizate. SBE, an underutilized byproduct of vegetable oil purification, is abundantly available globally and can be used as a filler and plasticizer in rubber compounds. This aligns with environmental sustainability principles, reduces disposal costs, and lowers raw material expenses in rubber manufacturing. In this research, the SBE was applied for each formula from SBE-02 to SBE-05 at ratios of 15–30 per hundred rubber (phr). As a comparison, carbon black (CB) filler (65 phr), CaCO3 (35 phr), and plasticizer derived from petroleum in the form of paraffinic oil (PO) (6 phr) were used. Rubber components were produced by masticating natural and synthetic rubber in an open mill, followed by the addition of filler, plasticizer, accelerator, co-activator, anti-degradant, and vulcanization agent. The resulting compounds were vulcanized at 150 °C and 10 MPa for 17 minutes. The test results demonstrated that incorporating SBE at a ratio of 15 phr (SBE-02) significantly reduced the cure time (t90) to 8 minutes and 20 seconds, the shortest among all tested formulations. The mechanical properties of the SBE-02 vulcanizate rubber met the requirements for solid wheelchair tire applications, with a hardness of 70 Shore A. However, its abrasion resistance test result of 189.1 g/cm³ was the lowest among the formulations tested. Furthermore, the scorch time (ts2) of the SBE-02 was determined to be 2 minutes and 35 seconds. Results from a 1000x magnification scanning electron microscope (SEM) reveal air gaps on all sample surfaces of different sizes. The elements C, O, Zn, Si, Ca, and Pb dominate the SEM-EDX results for all rubber vulcanizate samples from all three spectra, in varying weight percentages. The identification of functional groups with FTIR on all rubber vulcanizate samples shows Si–O–Si bending at 2, 4, and 5 and Si–O–Al stretching at 3, 5 on the wave number spectrum of 680–413 cm−1 Si–O–Si on the wave number spectrum 1100–1050 cm−1 from the infrared spectrum.

Optimized Design of Material Preparation for Cotton Linters-Based Carbon Black Dispersion Stabilizers Based on Response Surface Methodology.

Carbon black particles possess dimensions on the nanometer or sub-nanometer scale. When utilized, these particles have a tendency to aggregate, which compromises their stability under storage conditions. To address this issue, a dispersant was prepared using cotton short fibers as raw materials through etherification and graft polymerization with acrylamide (AM) and 2-acrylamido-2-methylpropane sulfonic acid (AMPS) as raw materials. The dispersant was then used to disperse carbon black to test its dispersing performance. A response surface optimization test was utilized to ascertain the influence of AMPS monomer mass, AM monomer mass, and potassium persulfate (KPS) initiator mass on the dispersibility of carbon black during dispersant preparation, and a set of optimal preparation conditions were obtained. The dispersion stability of carbon black in water was assessed using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), elemental analysis (EA), thermogravimetric analysis (TG), zeta potential analysis, high magnification scanning electron microscopy (SEM), and contact angle measurements. Results revealed that the optimum mass ratio of carboxymethyl cellulose (CMC) to AMPS to AM was 1:0.69:1.67, with the KPS initiator comprising 1.56% of the total monomer mass. By incorporating the dispersant at a concentration of 37.50%, the particle size of carbon black particles was observed to decrease from 5.350 μm to 0.255 μm, and no agglomeration of carbon black particles occurred even after 3 weeks of storage.

Segmentation and Classification of Fission as Pores in Reactor Iirradiated Annular U[sbnd]10Zr Metallic Fuel Using Machine Learning Models

Metallic fuels, particularly U10Zr, are promising candidates for next-generation sodium-cooled fast reactors. Irradiation of nuclear fuels in reactors can lead to the formation of solid and gas fission product which subsequently forms microstructural pores, deteriorating fuel performance. Due to the massive amount of pores and complex phases formed, a quantitative description of fission gas pores is not yet available, preventing the development of microstructure-informed fuel performance modeling for fuel qualification. This paper applied a pre-trained deep learning model to ∼10,260 high magnification scanning electron microscopy images. This method increased the accuracy of fission gas pore segmentation and allows statistical features to be extracted which cannot be achieved manually. A pre-trained decision tree model worked on the segemenation resutls and further classified the pores into different categories to produce a correlation between the pores, movement of lanthanides, and temperature gradient during irradiation. This paper emphasizes the potentials of machine learning models to accelerate fuel research, development, and qualification for advanced reactors.

Histological Features of Neovaginal Epithelium after Vaginoplasty in Mayer-Rokitansky-Küster-Hauser Syndrome

To analyze the features of the epithelia coating neovaginas after vaginoplasty in women affected by Mayer-Rokitansky-Küster-Hauser syndrome STUDY DESIGN: We conducted a retrospective analysis of prospectively collected data. Women affected by Rokitansky syndrome who underwent neovaginal biopsy after vaginoplasty (McIndoe surgery, intestinal vaginoplasty, Vecchietti surgery, and Davydov surgery) were included. Macroscopic mucosal features were assessed through clinical examination and the Schilling test. Each biopsy specimen was prepared for examination by light microscopy and in some cases by scanning electron microscopy (SEM). Thirty-six patients (4 McIndoe, 2 intestinal vaginoplasty, 14 Vecchietti, and 16 Davydov) were included. All biopsies were performed without complications. In McIndoe's neovaginas, the mucosal microscopic features were similar to normal skin, with large areas of preserved epithelium, heterogeneous presence of dermal papillae, and superficial keratinization. The characteristics of the intestinal neovagina's surface were similar to those of a sigmoid colon, with well-shaped glands, cylindrical cells, and a secreting mucosa. In Vecchietti neovaginas, the surface the epithelium was flat and multilayered, highly similar to that of a normal vagina, with the presence of glycogen and superficial desquamation. On medium SEM magnification evaluation, the epithelium presented flattened polygonal cells. Finally, in Davydov neovaginas, none of the specimens had persistent mesothelial elements. The squamous neo-epithelium had regular aspects of differentiation with the presence of glycogen. At greater SEM magnification, microridges were evident, with a regular distribution. Each different technique of vaginoplasty leads to unique histological and structural features of the neovagina's mucosa. Knowledge of these elements must be the basis for the choice of the most appropriate intervention.

Pitch calibration of standard nanoscale for uncertainty reduction of certified reference materials for SEM image sharpness evaluation and magnification calibration

Scanning electron microscopy (SEM) is widely used to observe and analyze nanostructures on surfaces. To obtain accurate and sharp images by SEM, it is necessary to evaluate the sharpness of SEM images and calibrate the magnification simultaneously. The NMIJ-CRM 5207-a is a certified reference material for image sharpness evaluation and magnification calibration. The certified values of NMIJ-CRM 5207-a are the average pitches in the X- and Y- axes. The major source of uncertainty of the NMIJ-CRM 5207-a is the pitch calibration of the commercially available standard nanoscale. To reduce the uncertainty of the pitch calibration value of the standard nanoscale, the pitch calibration was performed using a metrological atomic force microscope and uncertainty was evaluated in this study.

Stress corrosion cracking of the slip-ring connectors of a 2 MW wind turbine

The failure of the connectors between the slip ring and rotor of a 2 MW wind turbine was investigated. Visual inspection, low magnification stereomicroscopy and scanning electron microscopy showed the presence of highly branched transgranular cracks. The cracks are in zones of increased stress, as demonstrated by finite elements. The observations show that the failure is caused by stress corrosion cracking (SCC). Fourier transform infrared spectroscopy (FTIR) was used to characterise the insulating varnish of the slip ring. Tropical climate conditions cause the wetting of the components and with a close-by livestock plant is a source of NH3 contamination. Corrections to the design and manufacturing process of the slip rings were suggested to increase the life expectancy of the generator, although the selection of an insulating varnish with higher resistance to environmental exposure is probably the most efficient manner to reduce the incidence of this phenomenon in the future.

Wet chemical synthesis of BiPO4 :Eu3+ phosphor for w-LED application.

The synthesis of BiPO4 :Eu3+ phosphors has been achieved via a wet chemical process. X-ray diffraction patterns show that the phase of the as-prepared samples matches very well with the standard BiPO4 structure. At 395 nm, the highest excitation intensity was observed. Following 395 nm excitation, two characteristic emission peaks at 592 nm and 616 nm were shown. At 0.5mol% of Eu3+ ions, concentration quenching occurred. The particle size is within the micrometre range, according to the scanning electron microscope magnification. The chromaticity coordinates for wavelengths 592 nm and 616 nm are (x = 0.586, y = 0.412) and (x = 0.682, y = 0.317), respectively. The findings imply that the prepared phosphor may be used to create white light-emitting diodes.

The Effect of Annealing Technique on ZnO Film Properties

ZnO films deposited on glass substrates by ultrasonically chemical spray pyrolysis technique have been investigated to establish the effect of the annealing technique on film properties. For this purpose, films have been exposed to standard thermal annealing and microwave annealing in an air atmosphere. It has been determined that the structural, morphological, compositional, and optical properties of the ZnO films correlate with each other. X-ray diffraction analyses have been revealed the highest crystallization level and changing preferred orientations for microwave annealed films. It has been identified that the optical band gap values of the films decreased from 3.27 eV to 3.23 eV and 3.21 eV after the standard and microwave thermal annealing, respectively. Scanning electron microscope images have been revealed homogeneous morphology at plan-view images of all films. Also, it has been determined that the root-like morphology from the higher magnification scanning electron microscopy images. Thicknesses of the films have been also determined from cross-sectional scanning electron microscope images as 1.04m, 0.92m, and 0.92m for ZnO, standard thermal annealed and microwave annealed ZnO films, respectively. Also, the O/Zn ratio revealed improved stoichiometry for annealed films according to as-deposited film for investigated regions. The dependence of photoluminescence intensity on annealing technique has also been investigated in the current study.

Simulation of chromatic and achromatic assessments for camouflage textiles and combat background

Chromatic and achromatic (AC) assessments of camouflage textiles have been critical to the defense researchers for concealment, detection, recognition, and identification (CDRI) of target signature against multidimensional combat background (CB). AC assessment and camouflage measurement techniques are simulated and experimented for assessment of camouflage textiles against CB. This model has been demonstrated for color measurement spectrophotometer, scanning electron microscopy (SEM), digital imaging, hyperspectral imaging, and image processing software (ImageJ) for the advancement and establishment of AC camouflage textiles assessment. The chromatic variations of 48 artificial target objects (TOBs) have been synthesized by image processing; the technique can be implemented for defense CB-CDRI assessment. Microstructural variation versus optical signal of woodland, desertland and stoneland CB materials have been elucidated by SEM magnification. The achromatic variation of CB materials have been demonstrated for the replacement of optical signal against modern remote sensing device to the imaging sensor. Color difference (Δ E), microstructural variations, pixel variations to imaging signal and standard deviation of CB materials have been represented for remote sensing surveillance of defense applications against TOB-CB-CDRI. Technical simulation of color, texture, gloss, and pixel intensity has been derived for AC-CDRI assessment of camouflage textiles in TOBs-CB environment.

Calibration of high magnification in the measurement of critical dimension by AFM and SEM

In the measurement of critical dimension (CD) by scanning electron microscopy (SEM) and atomic force microscopy (AFM), the measured linewidths of the CD patterns are different from the real values due to the edge effect of secondary electrons and the radius and half cone angle of the tips for AFM. In order to solve this problem, a certified reference material (CRM) with a series of CD lines having different linewidth from 20 nm to 60 nm was designed to calibrate the magnification. The linewidths of the CRM could be traceably certified by high resolution scanning transmission electron microscope from the lattice constant of Si(1 1 1) plane in the Si(1 0 0) substrate. As a result, the magnification of AFM and SEM can be calibrated from the certified linewidths of the CRM. The magnification correction factors of AFM and SEM showed the relative standard uncertainties of 1.3% and 0.9%, respectively. The linewidths of the CD lines in the target samples can be traceably determined from the calibrated magnification after calibrating the instruments using the CRM and a calibration program.

Features of the architectonics of the microstructure of the primary remex of Owls (Strigiformes) due to the specifics of the flight

Conducted electron microscopic investigation of the primary remex fine structure of thirteen species of Owls (Strigiformes), using a scanning electron microscope (SEM). It is shown that Owls (Strigiformes) have a number of specific primary remex microstructural characteristics. First of all, these are the features of the structure of the pennaceous barb: a cross section configuration, a pith architectonics on the cross section and longitudinal sections, a cuticular structur of the barb. A number of the unique features in the microstructure of the vanules of the pennaceous barb have been found for the first time (at the scanning electron microscope level, at a large SEM magnification). First of all, these are the structural features of the distal barbules and the structure of the apical portion of the barb with the elongated proximal barbules and the distal barbules tightly contiguous to the ramus and closed with each other. Mentioned characteristics make for the thick velvet-like dorsal surface of the vane and the presence of a complex of peculiar “bunches” (fringes) forming the cleft edge (a fringed edge) of the inner vane – exceptionally specific adaptive characteristics in Strigiformes. Рresentenced original research results suggest that Owls (Strigiformes) have a number specific microstructural characteristics of the primary remex and also a number of the unique features in the microstructure of the primary remex which reflecting the ecological and morphological adaptations conditioned by the flight specificity.

A new type of nanoscale reference grating manufactured by combined laser-focused atomic deposition and x-ray interference lithography and its use for calibrating a scanning electron microscope

Calibration of magnification and nonlinearity of scanning electron microscopy (SEM) is an essential task. In this paper, we proposed a new type of 1D grating sample fabricated by combining laser-focused atomic deposition and x-ray interference lithography as a lateral standard for calibrating SEMs. The calibrations of the grating pattern by a metrological large-range atomic force microscope indicate that the grating sample exhibits outstanding pattern uniformity that surpasses conventional samples fabricated by e-beam lithography: (1) the nonlinear deviation of the grating structures is below +/- 0.5 nm over a measurement range of 5 µm; (2) the maximal variation of the calibrated mean pitch values is lower than 0.01 nm at different locations randomly selected all over the pattern area. The proposed new sample is applied for accurately calibrating the magnification and nonlinearity of a commercial SEM, showing its advantages of easy-of-use and high accuracy. The influence of the defocus level of SEM on the calibration result is also demonstrated. This research offers a feasible solution for highly accurate SEM calibration needed for 3D nanometrology and hybrid metrology demanded in metrology of modern nanoelectronics devices and systems.

Effect of tool geometry in dissimilar Al-Steel Friction Stir Welding

Aluminum-Steel joining is an example of a multi-material design. An amalgamation of both the material is very beneficial, yet they pose their set of difficulties in joining due to a significant difference in properties. Solid-state joining processes such as friction stir welding are beneficial in avoiding fusion and formation of a thick intermetallic layer in the Al-steel joint. Critical control of process parameters and tool geometry is essential in friction stir welding to attain a reasonably sound joint. In present work, butt welding of low carbon steel with Aluminum 5052 alloy is performed with the use of three different tools. Progressive refinement in the geometry of tools was done to achieve the optimized dimensions of the tool. The weld joints obtained from various tools were compared based on heat generation. The joints were characterized based on peak temperature achieved, tensile strength, and the number of steel fragments in the Al matrix through micrographs. The weld joint was observed under an optical microscope and Field emission scanning electron microscope (FESEM) for quantification of intermetallic compounds (IMC) layer. Energy-dispersive X-ray spectroscopy (EDX) and XRD analysis were performed to investigate the phase and composition of the IMC layer. The fractured surface under tensile loading was observed under high magnification scanning electron microscope. The tool with a shoulder diameter of 13 mm and a cylindrical pin was found to be optimized for its minimum heat generation and strongest weld joint formation with a minimum number of void-causing steel fragments.

Imaging Software Programs for Reliable Mathematical Measurements in Orthodontics.

Aim: To evaluate the reliability of linear and angular measurements taken using different software programs in orthodontics. Materials and Methods: A sample of four software programs from different manufacturers, namely MicroDicom viewer, Photoshop® CS3, AutoCAD®, and Image-Pro®, were used for measuring the geometric features of four types of miniscrews from different manufacturers. Each miniscrew type presented a group: Group I, Tomas® (Dentaurum, Ispringen, Germany); Group II, HUBIT® (HUBIT, Gyeonggi-do, Korea); Group III, AbsoAnchor® (Dentos, Daegu, Korea); and Group IV, Creative (Creative, Zhejiang, China). Measurements of apical face angle, thread angle, lead angle, flank, pitch depth, and width were taken on 45 × magnification scanning electron microscope images of the shafts of the miniscrews. One assessor measured the seven geometric features for the four types of miniscrews using the four software programs twice in two sessions separated by a three week interval. Results: Pairwise comparisons, for each of the four miniscrew groups, showed that the only common result observed was the significant difference (p < 0.001) between measurements of flank taken by the four software programs. When measurements of the four types of miniscrews were pooled into one group, a high degree of intra-rater reliability (ICC range from 0.9 to 1.0) for all the seven geometric features was found with all the four software programs. The paired t-test showed insignificant difference (at p ≤ 0.05) between the first and second measurements, except for a few measurements including pitch width measured by Image-Pro® (p = 0.012), MicroDicom (p = 0.023), and Photoshop® (p = 0.001). Conclusions: Results did not give absolute superiority to one software program over the others and suggested an assessor effect. Assessor estimates could have been affected, among other factors, by the design of the miniscrews and the technical features of the software programs.

Effect of Gas Flow Rates on Quality of Aerosol Jet Printed Traces With Nanoparticle Conducting Ink

AbstractThis paper focuses on the influence of carrier gas flow rate (CGFR) and sheath gas flow rate (SGFR) on the quality of conductive traces printed with nanoparticle inks using aerosol jet printing (AJP). This investigation was motivated by previous results of two AJP specimens that were printed at different gas flow rates and yielded significantly different thermal cycling durability lifetimes. A parametric sensitivity study was executed by printing and examining serpentine trace structures at 15 different combinations of CGFRs and SGFRs. The analysis included quantifying the trace's macroscale geometry, electrical properties, and micromorphological features. Interesting macroscale results include an increase in effective conductivity with increasing CGFR. At the microscale, image processing of high magnification scanning electron microscope (SEM) images of the printed traces revealed that agglomerations of silver clusters on the surface of traces became coarser at higher CGFR and also that agglomerates in the bulk were finer than those on the surface. Crystalline silver deposits were observed at all flow rates. In addition, cross sectioning of the printed traces showed higher incidences of buried cohesive cracking at higher gas flow rates. These cohesive cracks reduce the robustness of the traces but may not always be visible from the surface. The degree of cohesive cracking was seen to be broadly correlated with the coarseness of the surface agglomerates, thus suggesting that the coarseness of surface agglomerates may provide a visible surrogate measure of the print quality. The results of this study suggest that print quality may degrade as gas flow rates increase.

A case study of identification and classification of microplastics using aluminium sulfate in wastewater treatment facility on the university campus

This study is to identify the Microplastics in the effluent of the treatment plant on the University campus. The plastic with less than 5 (five) mm size is universally considered as Microplastics. Volume reduced sampling method is used and for sample concentration, Aluminium sulfate as the coagulant is used. A sample was concentrated as the liquid and solid powder. One micron filter paper is used. Visual identification was done using the dissecting microscope, For particles smaller than 40X magnification scanning electron microscope (SEM) we used. For Identification of polymers Fourier Transform Infrared Spectroscopy (FT-IR) was used. In FT-IR test results all the liquid samples were negative in a result, and all the solid samples were positive that, it showed the presence of polymer in the sample, the plastics identified are Polyethylene, polystyrene, Polyvinyl chloride, Polyamide (nylon) in the solid sample.

Automated characterisation and analysis of large arrays of nanostructures fabricated at wafer scale

Large-area and dense arrays of nanometric scale structures are commonly fabricated for several applications. The characterisation of sub-micron structures (below 1 μm) at a large scale as well as the related data analysis are challenging tasks. Here, we present a method to address the image acquisition, the data extraction and the data analysis, applied to the evaluation of the uniformity of nanometric structures in a silicon master. Automated routines for both high and low magnification Scanning Electron Microscope (SEM) imaging have been successfully developed. SEM images have been automatically acquired by scripting routines, which collect large amounts of images of the nanometric structures covering multiple regions of the wafer in a few hours. Geometric parameters of the nanometric structures such as diameter, period and height have been extracted from the raw images using the developed image processing scripts. Finally, the data extracted from more than 4800 images acquired with three different characterisation scripts (1600 images for each study) have been analysed and plotted according to their position in the wafer.

Morphology and Structure of Ni/Zr0.84Sc0.16O1.92 Electrode Material Synthesized via Glycine-Nitrate Combustion Method for Solid Oxide Electrochemical Cell

Nickel oxide and Sc-doped ZrO2 electrode material with a 1:1 wt % composition of NiO and Zr0.84Sc0.16O1.92 was synthesized via a single-step glycine-nitrate combustion method. Different glycine to nitrate (g/n) molar ratios of 0.27, 0.54, and 1.1 were used to investigate its effect on the structural, morphological, and electrical properties of the heat-treated samples. X-ray diffraction (XRD) patterns of the as-sintered samples for all the g/n ratios were indexed to cubic phases of NiO and ScSZ. Upon reduction at 700 °C, NiO was fully reduced to Ni. In-situ XRD patterns showed that the composite Ni/Zr0.84Sc0.16O1.92 electrode material retains its cubic structure at intermediate temperatures from 500 °C to 800 °C. High magnification scanning electron microscopy (SEM) images revealed that nanoparticles of Ni are also formed and situated at the surfaces of ScSZ grains, apart from agglomerated submicron particles of Ni. SEM and electron-dispersive spectroscopy mapping revealed interconnected grains of ScSZ oxide-ion conducting phase. From the calculated conductivity based on electrochemical impedance spectroscopy results, the 0.27 g/n ratio showed an order of magnitude-higher total conductivity among the other prepared samples.

The electronic component authenticity verification

The article presents a brief insight into the university research of efficient methods aimed at revealing counterfeit electronic components. Methods like multichannel curve tracing, component internal structure X-raying, system on chip optical inspection with higher magnification microscopy and Scanning Electron Microscopy combined with Element Energy Dispersive Spectroscopy (EDS) are powerful means for authenticity verification. Comparative analysis results serve as an illustration of cases where various features differences can warn not to let a particular component delivery penetrate the assembly process.

Effect of Zinc Oxide nanoparticals preparation from Zinc Sulphate (ZnSo4) against gram negative or gram positive microorganisms in vitro

This research aims to prepare ZnO NPs by using chemical bath deposition way from ZnSO4 and NaOH as starting materials. It was examined by X-ray diffraction, Scanning Electron Microscopy, Zeta potential and Fourier Transformation Infrared. Scanning Electron Microscopy images showed various morphological changes of ZnO nanoparticles obtained by the above method and the different magnification Scanning Electron Microscopy images of the nanoparticle and confirms that the Nano flowers are grown with well-defined morphology and diameters varying between 60-110 nm. The effect of Zinc oxide nanoparticles against bacteria staphylococcus aureus, E.coli and Pseudomous aeruginosa showed the ability of this substance to inhibit the growth of all types of bacteria in different concentrations. The percentage of survival bacteria was (2, 3.7 and 6%) for E.coli bacteria and (1, 1.5 and 5 %) for Pseudomous aeruginosa bacteria, while the percentage was (0.8, 1 and 1.5 %) for staphylococcus aurous respectively for all concentration.