Search results for: scanning electron microscopy (sem)

Authors: Raghvendra Singh Yadav, Ivo Kuritka, Jarmila Vilcakova, Pavel Urbanek, Michal Machovsky, David Skoda, Milan Masar

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The elastomer nanocomposites were synthesized by solution mixing method with an elastomer as a matrix and in situ thermally reduced graphene oxide (RGO) and spinel ferrite NiFe₂O₄ nanoparticles as filler. Spinel ferrite NiFe₂O₄ nanoparticles were prepared by the starch-assisted sol-gel auto-combustion method. The influence of filler on the microstructure, morphology, dielectric, electrical and magnetic properties of Reduced Graphene Oxide-Nickel Ferrite-Elastomer nanocomposite was characterized by X-ray diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, X-ray photoelectron spectroscopy, the Dielectric Impedance analyzer, and vibrating sample magnetometer. Scanning electron microscopy study revealed that the fillers were incorporated in elastomer matrix homogeneously. The dielectric constant and dielectric tangent loss of nanocomposites was decreased with the increase of frequency, whereas, the dielectric constant increases with the addition of filler. Further, AC conductivity was increased with the increase of frequency and addition of fillers. Furthermore, the prepared nanocomposites exhibited ferromagnetic behavior. This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: polymer-matrix composites, nanoparticles as filler, dielectric property, magnetic property

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Authors: Gabi N. Nehme, Saeed Ghalambor

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The use of titanium fluoride and iron fluoride (TiF3/FeF3) catalysts in combination with polutetrafluoroethylene (PTFE) in plain zinc dialkyldithiophosphate (ZDDP) oil is important for the study of engine tribocomponents and is increasingly a strategy to improve the formation of tribofilm and to provide low friction and excellent wear protection in reduced phosphorus plain ZDDP oil. The influence of surface roughness and the concentration of TiF3/FeF3/PTFE were investigated using bearing steel samples dipped in lubricant solution @100°C for two different heating time durations. This paper addresses the effects of water drop contact angle using different surface finishes after treating them with different lubricant combination. The calculated water drop contact angles were analyzed using Design of Experiment software (DOE) and it was determined that a 0.05 μm Ra surface roughness would provide an excellent TiF3/FeF3/PTFE coating for antiwear resistance as reflected in the scanning electron microscopy (SEM) images and the tribological testing under extreme pressure conditions. Both friction and wear performance depend greatly on the PTFE/and catalysts in plain ZDDP oil with 0.05% phosphorous and on the surface finish of bearing steel. The friction and wear reducing effects, which was observed in the tribological tests, indicated a better micro lubrication effect of the 0.05 μm Ra surface roughness treated at 100°C for 24 hours when compared to the 0.1 μm Ra surface roughness with the same treatment.

Keywords: scanning electron microscopy, ZDDP, catalysts, PTFE, friction, wear

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Authors: Wan-Tzu Yen, Yu-Chen Luo, I-Ping Liu, Po-Hsuan Yeh, Sheng-Hsun Fu, Yuh-Lang Lee

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Self-assembled characteristics and adsorption performance of 1-dodecylamine molecules on gold (Au) (111) surfaces were characterized via cyclic voltammetry (CV), surface-enhanced infrared absorption spectroscopy (SEIRAS) and scanning tunneling microscopy (STM). The present study focused on the formation of 1-dodecylamine (DDA) on a gold surface with respect to the ex-situ arrangement of an adlayer on the Au(111) surface, and phase transition at potential dynamics carried out by EC-STM. This study reveals that alkyl amine molecules were formed an adsorption pattern with highly regular “lie down shape” on Au(111) surface, even in an extreme acid system (pH = 1). Acidic electrolyte (HClO₄) could protonate the surface of alkyl amine of a monolayer of the gold surface when potential shifts to negative. The quite stability of 1-dodecylamine on the gold surface maintained the monolayer across the potential window (0.1-0.8V). This transform model was confirmed by EC-STM. In addition, amine-modified Au(111) electrode adlayer used to examine how to affect an electron transfer across an interface using [Fe(CN)₆]³⁻/[Fe(CN)₆]⁴⁻ redox pair containing 0.1 M HClO₄ solution.

Keywords: cyclic voltammetry, dodecylamine, gold (Au)(111), scanning tunneling microscopy, self-assembled monolayer, surface-enhanced infrared absorption spectroscopy

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Authors: Temitope Olumide Olugbade

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Low resistance and delayed fracture to corrosion, especially in harsh environmental conditions, often limit the wide application of high-manganese (high-Mn) steels. To address this issue, the present work investigates the influence of microalloying on the corrosion properties of high-Mn steels. Microalloyed and base high-Mn steels were synthesized through an arc melting process under an argon atmosphere. To generate different microstructures, the temperature and duration were varied via thermal homogenization treatments. The electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization techniques were used to determine the corrosion properties in 0.6 M NaCl aqueous solution at room temperature. The relationship between the microstructures and corrosion properties was investigated via Scanning Kelvin Probe Microscopy (SKPFM), energy dispersive X-ray spectroscopy (EDX), and Scanning electron microscopy (SEM) techniques. The local corrosion properties were investigated via in situ atomic force spectroscopy (AFM), considering the homogenization treatments. The results indicate that microalloying is a successful technique for enhancing the corrosion behavior of high-Mn steels. Compared to other alloying elements, Vanadium has shown improvement in corrosion properties for both general and local corrosion in chloride environments.

Keywords: corrosion, high-manganese steel, homogenization, microalloying, vanadium

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Authors: S. Mohajeri

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Electrocodeposition of Ni-TiO2 nanocomposite single layers and Ni-TiO2/TiO2 multilayers from Watts bath containing TiO2 sol was carried out on copper substrate. Pulse plating and pulse reverse plating techniques were applied to facilitate higher incorporations of TiO2 nanoparticles in Ni-TiO2 nanocomposite single layers, and the results revealed that by prolongation of the current-off durations and the anodic cycles, deposits containing 11.58 wt.% and 13.16 wt.% TiO2 were produced, respectively. Multilayer coatings which consisted of Ni-TiO2 and TiO2-rich layers were deposited by pulse potential deposition through limiting the nickel deposition by diffusion control mechanism. The TiO2-rich layers thickness and accordingly, the content of TiO2 reinforcement reached 104 nm and 18.47 wt.%, respectively in the optimum condition. The phase structure and surface morphology of the nanocomposite coatings were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The cross sectional morphology and line scans of the layers were studied by field emission scanning electron microscopy (FESEM). It was confirmed that the preferred orientations and the crystallite sizes of nickel matrix were influenced by the deposition technique parameters, and higher contents of codeposited TiO2 nanoparticles refined the microstructure. The corrosion behavior of the coatings in 1M NaCl and 0.5M H2SO4 electrolytes were compared by means of potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. Increase of corrosion resistance and the passivation tendency were favored by TiO2 incorporation, while the degree of passivation declined as embedded particles disturbed the continuity of passive layer. The role of TiO2 incorporation on the improvement of mechanical properties including hardness, elasticity, scratch resistance and friction coefficient was investigated by the means of atomic force microscopy (AFM). Hydrophilicity and wettability of the composite coatings were investigated under UV illumination, and the water contact angle of the multilayer was reduced to 7.23° after 1 hour of UV irradiation.

Keywords: electrodeposition, hydrophilicity, multilayer, pulse-plating

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Authors: J. Marx, D. Smazna, R. Adelung, B. Fiedler

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Aerographite is a 3D interconnected carbon foam. Its tetrapodal morphology is based on the zinc oxide (ZnO) template structure, which is replicated in the chemical vapour deposition (CVD) into a hollow carbon structure. This replication process is analyzed in ex-situ studies via interrupted synthesis and the observation of the reaction progress by using scanning electron (SEM), transmission electron microscopy (TEM) and Raman spectroscopy techniques. Based on the epitaxial growth process, with a layer-by-layer growth behaviour of the wall thickness or number of layers and the catalytical graphitization of the deposited amorphous carbon into graphitic carbon by zinc, a growth model is created. The properties of aerographite, such as the electrical conductivity is dependent on the graphitization and number of layer (wall thickness). Wall thicknesses between 3 nm and 22 nm are achieved by a controlled stepwise reduction of the synthesis time on the basis of the developed growth model, and by a further thermal treatment at 1800 °C the graphitization of the presented carbon foam is modified. The variation of the wall thickness leads to an optimum defect density (ID/IG ratio) and the graphitization to an improvement in the electrical conductivity. Furthermore, a metallic conducting behaviour of untreated and 1800 °C treated aerographite can be observed. Due to these structural and defective modifications, a fundamental structural-property equation for the description of their influences on the electrical conductivity is developed.

Keywords: electrical conductivity, electron microscopy (SEM/TEM), graphitization, wall thickness

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Authors: Kumari Kajal, Muthu Kumar Sampath, Hare Ram Singh

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In this context, the formulation and characterization of collagen silver lipid nanoparticles (CSLNs) were studied for their capacity to serve as fillers/matrix materials used in cosmeceutical applications. The CSLNs were prepared following a series of studies, such as X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) coupled with energy-dispersive X-ray spectroscopy (EDS), Fourier-transform infrared spectroscopy FT-IR; thermogravimetric analysis (TGA); and differential scanning calorimetry (DSC). The studies confirmed the structural integrity of nanoparticles, their cargo and thermal stability. The biological functionality of CSLNs was studied by carrying out in vitro & in vivo studies. The antibacterial effect, hemocompatibility and anti-inflammatory characteristics of these fibers were systematically investigated. The toxicological assays included oral toxicity in mice and aquatic life tests with the fish Danio rerio model. The morphology of the nanoparticles was confirmed using high-resolution transmission electron microscopy (HR-TEM). The report found that CSLNs had strong antimicrobial effects, unmatched hemocompatibility, and low or absent inflammatory reactions, which makes them perfect candidates for cosmeceutical applications. The toxicological evaluations evinced a good safety record without any significant adverse effects in both murine and Danio rerio models. This research reveals the efficient way of CSLNs to the efficacy and safety of dermaceuticals.

Keywords: collagen silver lipid nanoparticles (CSLNs), cosmeceuticals, antimicrobial activity, hemocompatibility, in vitro assessment, in vivo assessment.

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Authors: Shalini Rajput, Dinesh Mohan

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Water is the most important and essential resources for existing of life on the earth. Water quality is gradually decreasing due to increasing urbanization and industrialization and various other developmental activities. It can pose a threat to the environment and public health therefore it is necessary to remove hazardous contaminants from wastewater prior to its discharge to the environment. Recently, magnetic iron oxide nanoparticles have been arise as significant materials due to its distinct properties. This article focuses on the synthesis method with a possible mechanism, structure and application of magnetic iron oxide nanoparticles. The various characterization techniques including X-ray diffraction, transmission electron microscopy, scanning electron microscopy with energy dispersive X-ray, Fourier transform infrared spectroscopy and vibrating sample magnetometer are useful to describe the physico-chemical properties of nanoparticles. Nanosized iron oxide particles utilized for remediation of contaminants from aqueous medium through adsorption process. Due to magnetic properties, nanoparticles can be easily separate from aqueous media. Considering the importance and emerging trend of nanotechnology, iron oxide nanoparticles as nano-adsorbent can be of great importance in the field of wastewater treatment.

Keywords: nanoparticles, adsorption, iron oxide, nanotechnology

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Authors: Seyedamirreza Shamsdini, Mohsen Mohammadi

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In this research, 18Ni-300 maraging steel powder particles are investigated by studying particle size distribution along with their morphology and grain structure. The powder analysis shows mostly spherical morphologies with cellular structures. A laser-based additive manufacturing process, selective laser melting (SLM) is used to produce samples for further investigation of mechanical properties and microstructure. Several uniaxial tensile tests are performed on the as-built parts to evaluate the mechanical properties. The macroscopic properties, as well as microscopic studies, are then investigated on the printed parts. Hardness measurements, as well as porosity levels, are measured for each sample and are correlated with microstructures through electron microscopy techniques such as Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The grain structure is studied for the as-printed specimens and compared to the powder particle microstructure. The cellular structure of the printed samples is observed to have dendritic forms with dendrite width dimensions similar to the powder particle cells. The process parameter is changed, and the study is performed for different powder layer thickness, and the resultant mechanical properties and grain structure are shown to be similar. A phase study is conducted both on the powder and the printed samples using X-Ray Diffraction (XRD) techniques, and the austenite phase is observed to at first decrease due to the manufacturing process and again during the uniaxial tensile deformation. The martensitic structure is formed in the first stage based on the heating cycles of the manufacturing process and the remaining austenite is shown to be transformed to martensite due to different deformation mechanisms.

Keywords: additive manufacturing, maraging steel, mechanical properties, microstructure

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Authors: Princess Stephanie P. Llanos, Rinlee Butch M. Cervera

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Lithium iron phosphate (LiFePO4) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, carbon-coated nanograined LiFePO4 is synthesized via wet chemistry method at a low temperature of 400 °C and investigated its performance as a cathode in Lithium battery. The X-ray diffraction pattern of the synthesized samples can be indexed to an orthorhombic LiFePO4 structure. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LiFePO4 and coating of amorphous carbon layer. Elemental mapping using Energy dispersive spectroscopy analysis revealed the homogeneous dispersion of Fe, P, O, and C elements. On the other hand, the electrochemical performances of the synthesized cathodes were investigated using cyclic voltammetry, galvanostatic charge/discharge tests with different C-rates, and cycling performances. Galvanostatic charge and discharge measurements revealed that the sample sintered at 400 °C for 3 hours with carbon coating demonstrated the highest capacity among the samples which reaches up to 160 mAhg⁻¹ at 0.1C rate.

Keywords: cathode, charge-discharge, electrochemical, lithium batteries

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Authors: Ainouna Bouziane

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The ability of Electron Tomography to recover the 3D structure of catalysts, with spatial resolution in the subnanometer scale, has been widely explored and reviewed in the last decades. A variety of experimental techniques, based either on Transmission Electron Microscopy (TEM) or Scanning Transmission Electron Microscopy (STEM) have been used to reveal different features of nanostructured catalysts in 3D, but High Angle Annular Dark Field imaging in STEM mode (HAADF-STEM) stands out as the most frequently used, given its chemical sensitivity and avoidance of imaging artifacts related to diffraction phenomena when dealing with crystalline materials. In this regard, our group has developed a methodology that combines image denoising by undecimated wavelet transforms (UWT) with automated, advanced segmentation procedures and parameter selection methods using CS-TVM (Compressed Sensing-total variation minimization) algorithms to reveal more reliable quantitative information out of the 3D characterization studies. However, evaluating the accuracy of the magnitudes estimated from the segmented volumes is also an important issue that has not been properly addressed yet, because a perfectly known reference is needed. The problem particularly complicates in the case of multicomponent material systems. To tackle this key question, we have developed a methodology that incorporates volume reconstruction/segmentation methods. In particular, we have established an approach to evaluate, in quantitative terms, the accuracy of TVM reconstructions, which considers the influence of relevant experimental parameters like the range of tilt angles, image noise level or object orientation. The approach is based on the analysis of material-realistic, 3D phantoms, which include the most relevant features of the system under analysis.

Keywords: electron tomography, supported catalysts, nanometrology, error assessment

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Authors: Rimzhim Gupta, Bhanupriya Boruah, Jayant M. Modak, Giridhar Madras

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Microbial contamination is one of the major concerns in the field of water treatment. AOP (advanced oxidation processes) is well-established method to resolve the issue of removal of contaminants in water. A Z-scheme composite g-C₃N₄/CuWO₄ was synthesized by sol-gel method for the photocatalytic inactivation of a mixed population of Gram-positive bacteria (S. aureus) and Gram-negative bacteria (E. coli). The photoinactivation was observed for different types of bacteria in the same medium together and individually in the absence of the nutrients. The lattice structures and phase purities were determined by X-ray diffraction. For morphological and topographical features, scanning electron microscopy and transmission electron microscopy analyses were carried out. The band edges of the semiconductor (valence band and conduction band) were determined by ultraviolet photoelectron microscopy. The lifetime of the charge carriers and band gap of the semiconductors were determined by time resolved florescence spectroscopy and diffused reflectance spectroscopy, respectively. The effect of weight ratio of C₃N₄ and CuWO₄ was observed by performing photocatalytic experiments. To investigate the exact mechanism and major responsible radicals for photocatalysis, scavenger studies were performed. The rate constants and order of the inactivation reactions were obtained by power law kinetics. For E. coli and S. aureus, the order of reaction and rate constants are 1.15, 0.9 and 1.39 ± 0.03 (CFU/mL)⁻⁰.¹⁵ h⁻¹, 47.95 ± 1.2 (CFU/mL)⁰.¹ h⁻¹, respectively.

Keywords: z-scheme, E. coli, S. aureus, sol-gel

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Authors: Eman Alzahrani

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Efficient extraction of proteins by removing interfering materials is necessary in proteomics, since most instruments cannot handle such contaminated sample matrices directly. In this study, chitosan-coated magnetic nanoparticles (CS-MNPs) for purification of myoglobin were successfully fabricated. First, chitosan (CS) was prepared by a deacetylation reaction during its extraction from shrimp-shell waste. Second, magnetic nanoparticles (MNPs) were synthesised, using the coprecipitation method, from aqueous Fe2+ and Fe3+ salt solutions by the addition of a base under an inert atmosphere, followed by modification of the surface of MNPs with chitosan. The morphology of the formed nanoparticles, which were about 23 nm in average diameter, was observed by transmission electron microscopy (TEM). In addition, nanoparticles were characterised using X-ray diffraction patterns (XRD), which showed the naked magnetic nanoparticles have a spinel structure and the surface modification did not result in phase change of the Fe3O4. The coating of MNPs was also demonstrated by scanning electron microscopy (SEM) analysis, energy dispersive analysis of X-ray spectroscopy (EDAX), and Fourier transform infrared (FT-IR) spectroscopy. The adsorption behaviour of MNPs and CS-MNPs towards myoglobin was investigated. It was found that the difference in adsorption capacity between MNPs and CS-MNPs was larger for CS-MNPs. This result makes CS-MNPs good adsorbents and attractive for using in protein extraction from biological samples.

Keywords: chitosan, magnetic nanoparticles, coprecipitation, adsorption

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Authors: Amine Mezni, Merfat Algethami, Ali Aldalbahi, Arwa Alrooqi, Abel Santos, Dusan Losic, Sarah Alharthi, Tariq Altalhi

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In situ synthesis of carbon nanotubes featuring different diameters (10-200 nm), lengths (1 to 100 µm) and periodically nanostructured shape was performed in a custom designed chemical vapor deposition (CVD) system using nanoporous anodic alumina (NAA) under different conditions. The morphology of the resulting CNTs/NAA composites and free-standing CNTs were analyzed by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The results confirm that highly ordered arrays of CNTs with precise control of nanotube dimensions in the range 20-200 nm with tube length in the range < 1 µm to > 100 μm and with periodically shaped morphology can be fabricated using nanostructured NAA templates prepared by anodization. This technique allows us to obtain tubes open at one / both ends with a uniform diameter along the pore length without using any metal catalyst. Our finding suggests that this fabrication strategy for designing new CNTs membranes and structures can be significant for emerging applications as molecular separation/transport, optical biosensing, and drug delivery.

Keywords: carbon nanotubes, CVD approach, composites membrane, nanoporous anodic alumina

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Authors: Josef Fládr, Jiří Němeček, Veronika Koudelková, Petr Bílý

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Mechanical parameters of cementitious composites differ quite significantly based on the composition of cement matrix. They are also influenced by mixing times and procedure. The research presented in this paper was aimed at identification of differences in microstructure of normal strength (NSC) and differently mixed high strength (HSC) cementitious composites. Scanning electron microscopy (SEM) investigation together with energy dispersive X-ray spectroscopy (EDX) phase analysis of NSC and HSC samples was conducted. Evaluation of interfacial transition zone (ITZ) between the aggregate and cement matrix was performed. Volume share, thickness, porosity and composition of ITZ were studied. In case of HSC, samples obtained by several different mixing procedures were compared in order to find the most suitable procedure. In case of NSC, ITZ was identified around 40-50% of aggregate grains and its thickness typically ranged between 10 and 40 µm. Higher porosity and lower share of clinker was observed in this area as a result of increased water-to-cement ratio (w/c) and the lack of fine particles improving the grading curve of the aggregate. Typical ITZ with lower content of Ca was observed only in one HSC sample, where it was developed around less than 15% of aggregate grains. The typical thickness of ITZ in this sample was similar to ITZ in NSC (between 5 and 40 µm). In the remaining four HSC samples, no ITZ was observed. In general, the share of ITZ in HSC samples was found to be significantly smaller than in NSC samples. As ITZ is the weakest part of the material, this result explains to large extent the improved mechanical properties of HSC compared to NSC. Based on the comparison of characteristics of ITZ in HSC samples prepared by different mixing procedures, the most suitable mixing procedure from the point of view of properties of ITZ was identified.

Keywords: electron diffraction spectroscopy, high strength concrete, interfacial transition zone, normal strength concrete, scanning electron microscopy

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Authors: Jiang-Bei Qin, Rui-Xia Miao, Wei Ren

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In this study, high crystalline gallium oxide microstructures (wires, belts, and sheets) were synthesized by catalyst-free thermal oxidation. Structural studies such as X-ray diffraction, Raman and transmission electron microscope (TEM) investigations on the microstructures showed monoclinic phase of gallium oxide and single crystalline structure. The scanning electron microscopy (SEM) observations revealed that a huge super microsheet even grows up to 450 µm in length and 206 µm in width. Gallium oxide microstructures exhibit high crystallinity along (002) and (401), respectively. The PL spectrum of these microstructures excites a blue light band centered at 441 and 489nm. The growth mechanism of gallium oxide microstructures is discussed. These gallium oxide microstructures have great potential in functional devices.

Keywords: catalyst-free, gallium oxide, microstructures, thermal oxide

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Authors: Navid Zanganeh, Hafez Balavi, Farbod Sharif, Mahla Zabet, Marzieh Bakhtiary Noodeh

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Cerium oxide (CeO2) also known as cerium dioxide or ceria is a pale yellow-white powder with various applications in the industry from wood coating to cosmetics, filtration, fuel cell electrolytes, gas sensors, hybrid solar cells and catalysts. In this research, attempts were made to synthesize and characterization of CeO2 nano-particles via sol-gel method. In addition, the effect of aging time on the size of particles was investigated. For this purpose, the aging times adjusted 48, 56, 64, and 72 min. The obtained particles were characterized by x-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM), transmitted electron microscopy (TEM), and Brunauer–Emmett–Teller (BET). As a result, XRD patterns confirmed the formation of CeO2 nanoparticles. SEM and TEM images illustrated the nano-particles with cluster shape, spherical and a nano-size range which was in agreement with XRD results. The finest particles (7.3 nm) was obtained at the optimum condition which was aging time of 48 min, calcination temperature at 400 ⁰C, and cerium concentration of 0.004 mol. Average specific surface area of the particles at optimum condition was measured by BET analysis and recorded as 47.57 m2/g.

Keywords: aging time, CeO2 nanoparticles, size distribution, sol-gel

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Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

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In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)₄ to titanium oxide, TiO₂ was investigated. The as-prepared Ti(OH)₄ precipitate was annealed at 800°C to obtain TiO₂ nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO₂ nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO₂ nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.

Keywords: TiO2 nanoparticles, chemical precipitation route, phase transition, Fourier Transform Infra-Red spectroscopy (FTIR), micro-Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence Spectroscopy (PL) and Field Effect Scanning electron microscopy (FESEM)

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Authors: Rabah Bensaha, Badreeddine Toubal

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Un-doped TiO2, Co single doped TiO2 and (Cu-Co) co-doped TiO2 thin films have been growth on silicon substrates by the sol-gel dip coating technique. We mainly investigated both effects of the dopants and annealing temperature on the structural, optical and electrical properties of TiO2 films using X-ray diffraction (XRD), Raman and FTIR spectroscopy, Atomic force microscopy (AFM), Scanning electron microscopy (SEM), UV–Vis spectroscopy. The chemical compositions of Co-doped and (Cu-Co) co-doped TiO2 films were confirmed by XRD, Raman and FTIR studies. The average grain sizes of CoTiO3-TiO2 nanocomposites were increased with annealing temperature. AFM and SEM reveal a completely the various nanostructures of CoTiO3-TiO2 nanocomposites thin films. The films exhibit a high optical reflectance with a large band gap. The highest electrical conductivity was obtained for the (Cu-Co) co-doped TiO2 films. The polyhedral surface morphology might possibly improve the surface contact between particle sizes and then contribute to better electron mobility as well as conductivity. The obtained results suggest that the prepared TiO2 films can be used for optoelectronic applications.

Keywords: sol-gel, TiO2 thin films, CoTiO3-TiO2 nanocomposites films, Electrical conductivity

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Authors: Samir El-Gendy, Doaa Zaghloul

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The current study dealt with the gross and microscopic anatomy of the integument of male ostrich in addition to the histological features of different areas of skin by light and SEM. The ostrich skin is characterized by prominent feather follicles and bristles. The number of feather follicles was determined per cm2 in different regions. The integument of ostrich had many modifications which appeared as callosities and scales, nail and toe pads. They were sternal, pubic and Achilles tendon callosities. The vacuolated epidermal cells were seen mainly in the skin of legs and to a lesser extent in the skin of back and Achilles areas. Higher lipogenic potential was expressed by epidermis from glabrous areas of ostrich skin. The dermal papillae were found in the skin of feathered area of neck and back and this was not a common finding in bird's skin which may give resistance against shearing forces in these regions of ostrich skin. The thickness of the keratin layer of ostrich varied, being thick and characteristically loose in the skin at legs, very thin and wavy at neck, while at Achilles skin area, scale and toe pad were thick and more compact, with the thickest very dense and wavy keratin layer at the nail. The dermis consisted of superficial layer of dense irregular connective tissue characterized by presence of many vacuoles of different sizes just under the basal lamina of the epithelium of epidermis and deep layer of dense regular connective tissue. This result suggested presence of fat droplets in this layer which may be to overcome the lack of good barrier of cutaneous water loss in epidermis.

Keywords: ostrich, light microscopy, scanning electron microscopy, integument, skin modifications

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Authors: Lee Chiau Yeng, Norhayani Othman

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Regenerated cellulose fiber is fabricated in the NaOH/urea aqueous solution. In this work, cellulose is dissolved in 7 .wt% NaOH/12 .wt% urea in the temperature of -12 °C to prepare regenerated cellulose. Thermal and structure properties of cellulose and regenerated cellulose was compared and investigated by Field Emission Scanning Electron Microscopy (FeSEM), Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), Thermogravimetric analysis (TGA), and Differential Scanning Calorimetry. Results of FeSEM revealed that the regenerated cellulose fibers showed a more circular shape with irregular size due to fiber agglomeration. FTIR showed the difference in between the structure of cellulose and the regenerated cellulose fibers. In this case, regenerated cellulose fibers have a cellulose II crystalline structure with lower degree of crystallinity. Regenerated cellulose exhibited better thermal stability than the cellulose.

Keywords: regenerated cellulose, cellulose, NaOH, urea

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Authors: Khamael M. Abualnaja, Lidija Šiller, Ben R. Horrocks

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Surface enhanced Raman spectroscopy (SERS) of Silicon nano crystals (SiNCs) were obtained using two different laser excitations: 488 nm and 514.5 nm. Silver nano particles were used as plasmonics metal nano particles due to a robust SERS effect that observed when they mixed with SiNCs. SiNCs have been characterized by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). It is found that the SiNCs are crystalline with an average diameter of 65 nm and FCC lattice. Silver nano particles (AgNPs) of two different sizes were synthesized using photo chemical reduction of AgNO3 with sodium dodecyl sulfate (SDS). The synthesized AgNPs have a polycrystalline structure with an average particle diameter of 100 nm and 30 nm, respectively. A significant enhancement in the SERS intensity was observed for AgNPs100/SiNCs and AgNPs30/SiNCs mixtures increasing up to 9 and 3 times respectively using 488 nm intensity; whereas the intensity of the SERS signal increased up to 7 and 2 times respectively, using 514.5 nm excitation source. The enhancement in SERS intensities occurs as a result of the coupling between the excitation laser light and the plasmon bands of AgNPs; thus this intense field at AgNPs surface couples strongly to SiNCs. The results provide good consensus between the wavelength of the laser excitation source and surface plasmon resonance absorption band of silver nano particles consider to be an important requirement in SERS experiments.

Keywords: silicon nanocrystals (SiNCs), silver nanoparticles (AgNPs), surface enhanced raman spectroscopy (SERS)

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Authors: Bertilia L. Bartley, Ledjane S. Barreto

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As a preliminary investigation on the control of microcracking in composite cement pastes, this study explores and compares the compatibility of Tetraethyl Orthosilicate (TEOS), Ethylene Glycol (EG) and Silicone Resin (SIL) in cement pastes cured at high temperature. Pastes were prepared by incorporating ordinary Portland cement (OPC) into an additive solution, using a solution/cement ratio of 0.45. Specimens were molded for 24h at 21 ± 2°C, then cured in deionized water for another 24h at 74 ± 1°C. TEOS and EG influence on fresh paste properties were similar to the reference OPC paste yet disintegration was observed in EG and SIL specimens after the first 12h of curing. X-Ray Diffraction analysis (XRD) coupled with thermogravimetric analysis (TGA/DTG) verified that SIL addition impedes portlandite formation significantly. Backscatter Scanning Electron Microscopy (SEM) techniques were therefore performed on selected areas of each sample to investigate the morphology of the hydration products detected. Various morphologies of portlandite crystals were observed in pastes with EG and TEOS addition, as well as dense morphologies of calcium silicate hydrate (C-S-H) gel and fibers, and ettringite needles. However, the formation of portlandite aggregate and clusters of C-S-H was highly favored by TEOS addition. Furthermore, the microstructural details of composite pastes were clearly visible at low magnifications i.e. 500x, as compared to the OPC paste. The results demonstrate accelerated hydration within composite pastes, a uniform distribution of hydration products, as well as an adhesive interaction with the products and polymer additive. Overall, TEOS demonstrated the most favorable influence, which indicates the potential of TEOS as a compatible polymer additive within the cement system at high temperature.

Keywords: accelerated curing, cement/polymer composite, hydration, microstructural properties, morphology, portlandite, scanning electron microscopy (sem)

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Authors: K. Tomolya, D. Janovszky, A. Sycheva, M. Sveda, A. Roosz

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CuZrAl amorphous alloys have attracted high interest due to unique physical and mechanical properties, which can be enhanced by adding of Ni and Ti elements. It is known that this properties can be enhanced by crystallization of amorphous alloys creating nanocrystallines in the matrix. The present work intends to produce nanosized crystalline parti-cle reinforced amorphous matrix composite powders by crystallization of amorphous powders. As the first step the amorphous powders were synthe-tized by ball-milling of crystalline powders. (Cu49Zr45Al6) 80Ni10Ti10 and (Cu49Zr44Al7) 80Ni10Ti10 (at%) alloys were ball-milled for 12 hours in order to reach the fully amorphous structure. The impact en-ergy of the balls during milling causes the change of the structure in the powders. Scanning electron microscopical (SEM) images shows that the phases mixed first and then changed into a fully amorphous matrix. Furthermore, nanosized particles in the amorphous matrix were crystallized by heat treatment of the amorphous powders that was confirmed by TEM measurement. It was of importance to define the tem-perature when the amorphous phase starts to crystal-lize. Amorphous alloys have a special heating curve and characteristic temperatures, which can be meas-ured by differential scanning calorimetry (DSC). A typical DSC curve of an amorphous alloy exhibits an endothermic event characteristic of the equilibrium glass transition (Tg) and a distinct undercooled liquid region, followed by one or two exothermic events corresponding to crystallization processes (Tp). After measuring the DSC traces of the amorphous powders, the annealing temperatures should be determined between Tx and Tp. In our experiments several temperatures from the annealing temperature range were selected and de-pendency of crystallized nanoparticles fraction on their hardness was investigated.

Keywords: amorphous structure, composite, mechanical milling, powder, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electronmocroscopy (TEM)

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Authors: M. P. S. Tomar, Neelam Bansal

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Histomorphological, histochemical and scanning electron microscopic observations were recorded in developing cornea of buffalo fetuses. The samples from fetal cornea were collected in appropriate fixative from slaughter house and Veterinary Clinics, GADVASU, Ludhiana. The microscopic slides were stained for detailed histomorphological and histochemical studies. The scanning electron microscopic studies were performed at Electron microscopy & Nanobiology Lab, PAU Ludhiana. In present study, it was observed that, in 36 days (d) fetus, the corneal epithelium was well marked single layered structure which was placed on stroma mesenchyme. Cornea appeared as the continuation of developing sclera. The thickness of cornea and its epithelium increased as well as the epithelium started becoming double layered in 47d fetus at corneo-scleral junction. The corneal thickness in this stage suddenly increased thus easily distinguished from developing sclera. The separation of corneal endothelium from stroma was evident as a single layered epithelium. The stroma possessed numerous fibroblasts in 49d stage eye. Descemet’s membrane was appeared at 52d stage. The limbus area was separated by a depression from the developing cornea in 61d stage. In 65d stage, the Bowman’s layer was more developed. Fibroblasts were arranged parallel to each other as well as parallel to the surface of developing cornea in superficial layers. These fibroblasts and fibers were arranged in wavy pattern in the center of stroma. Corneal epithelium started to be stratified as a double layered epithelium was present in this age of fetal eye. In group II (>120 Days), the corneal epithelium was stratified towards a well marked irido-corneal angle. The stromal fibroblasts followed a complete parallel arrangement in its entire thickness. In full term fetuses, a well developed cornea was observed. It was a fibrous layer which had five distinct layers. From outside to inwards were described as the outer most layer was the 7-8 layered corneal epithelial, subepithelial basement membrane (Bowman’s membrane), substantia propria or stroma, posterior limiting membrane (Descemet’s membrane) and the posterior epithelium (corneal endothelium). The corneal thickness and connective tissue elements were continued to be increased. It was 121.39 + 3.73µ at 36d stage which increased to 518.47 + 4.98 µ in group III fetuses. In fetal life, the basement membrane of corneal epithelium and endothelium depicted strong to intense periodic Acid Schiff’s (PAS) reaction. At the irido-corneal angle, the endothelium of blood vessels was also positive for PAS activity. However, cornea was found mild positive for alcian blue reaction. The developing cornea showed strong reaction for basic proteins in outer epithelium and the inner endothelium layers. Under low magnification scanning electron microscope, cornea showed two types of cells viz. light cells and dark cells. The light cells were smaller in size and had less number of microvilli in their surface than in the dark cells. Despite these surface differences between light and dark cells, the corneal surface showed the same general pattern of microvilli studding all exposed surfaces out to the cell margin. which were long (with variable height), slight tortuous slender and possessed a micro villus shaft with a very prominent knob.

Keywords: buffalo, cornea, eye, fetus, ontogeny, scanning electron microscopy

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Authors: Soheir Mohamed Fathey

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Biofilms are complex biological communities which are hard to be eliminated by conventional antibiotic administration and implemented in eighty percent of humans infections. Green remedies have been used for centuries and have shown obvious effects in hindering and combating microbial biofilm infections. Nowadays, there has been a growth in the number of researches on the anti-biofilm performance of natural agents such as plant essential oil (EOs) and propolis. In this study, we investigated the antibiofilm performance of various natural agents, including four essential oils (EOs), cinnamon (Cinnamomum cassia), tea tree (Melaleuca alternifolia), and clove (Syzygium aromaticum), as well as propolis versus the biofilm of both Gram-positive pathogenic bacterium Staphylococcus aureus and Gram-negative pathogenic bacterium Pseudomonas aeruginosa which are major human and animal pathogens rendering a high risk due to their biofilm development ability. The antibiofilm activity of the tested agents was evaluated by crystal violet staining assay and detected by scanning electron and fluorescent microscopy. Antibiofilm performance declared a potent effect of the tested products versus the tested bacterial biofilms.

Keywords: biofilm, essential oils, electron microscopy, fluorescent

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Authors: Jung-Hwan Oh, Rajesh Kumar, Il-Kwon Oh

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Porous graphene has extensive potential applications in variety of fields such as hydrogen storage, CO oxidation, gas separation, supercapacitors, fuel cells, nanoelectronics, oil adsorption, and so on. However, the generation of some carbon atoms vacancies for precise small holes have been not extensively studied to prevent the agglomerates of graphene sheets and to obtain porous graphene with high surface area. Recently, many research efforts have been presented to develop physical and chemical synthetic approaches for porous graphene. But physical method has very high cost of manufacture and chemical method consumes so many hours for porous graphene. Herein, we propose a porous graphene contained holes with atomic scale precision by embedding metal nano-particles through microwave irradiation for hydrogen storage and CO oxidation multi- functionalities. This proposed synthetic method is appropriate for fast and convenient production of three dimensional nanostructures, which have nanoholes on the graphene surface in consequence of microwave irradiation. The metal nanoparticles are dispersed quickly on the graphene surface and generated uniform nanoholes on the graphene nanosheets. The morphological and structural characterization of the porous graphene were examined by scanning electron microscopy (SEM), transmission scanning electron microscopy (TEM) and RAMAN spectroscopy, respectively. The metal nanoparticle-embedded porous graphene exhibits a microporous volume of 2.586cm3g-1 with an average pore radius of 0.75 nm. HR-TEM analysis was carried out to further characterize the microstructures. By investigating the RAMAN spectra, we can understand the structural changes of graphene. The results of this work demonstrate a possibility to produce a new class of porous graphene. Furthermore, the newly acquired knowledge for the diffusion into graphene can provide useful guidance for the development of the growth of nanostructure.

Keywords: CO oxidation, hydrogen storage, nanocomposites, porous graphene

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Authors: Ivaylo A. Todorov, Peter S. Boyadzhiev

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A new distinctive species of Stepanovia Kostjukov (Hymenoptera: Eulophidae: Tetrastichinae) was reared in laboratory from mature galls of Diplolepis rosae (Linnaeus) (Cynipidae). The galls were collected from Rosa sp. bushes growing in Osogovo Mt. in Western Bulgaria. The new species is close to Stepanovia rosae Boyadzhiev & Todorov but differs in POL and OOL characteristics, width of antennae, forewings and ovipositor sheaths characteristics, different U-shaped pale stripe above clypeus and the length of the ventral plaque on male antenna. The taxonomically important morphological features are illustrated and compared with the rest species of the genus using Scanning electron microscopy and light reflection by compound microscopy. Images of male genitalia are also prepared.

Keywords: Eulophidae, Diplolepis rosae, galls, Stepanovia osogoviensis, Bulgaria

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Authors: C. Busuioc, S. I. Jinga, E. Pavel

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The continuous need of more non-volatile memories with a higher storage capacity, smaller dimensions and weight, as well as lower costs, has led to the exploration of optical lithography on active media, as well as patterned magnetic composites. In this context, optical lithography is a technique that can provide a significant decrease of the information bit size to the nanometric scale. However, there are some restrictions that arise from the need of breaking the optical diffraction limit. Major achievements have been obtained by employing a vitoceramic material as active medium and a laser beam operated at low power for the direct writing procedure. Thus, optical discs with ultra-high density were fabricated by a conventional melt-quenching method starting from analytical purity reagents. They were subsequently used for 3D recording based on their photosensitive features. Naturally, the next step consists in the elucidation of the composition and structure of the active centers, in correlation with the use of silver and rare-earth compounds for the synthesis of the optical supports. This has been accomplished by modern characterization methods, namely transmission electron microscopy coupled with selected area electron diffraction, scanning transmission electron microscopy and electron energy loss spectroscopy. The influence of laser diode parameters, silver concentration and fluorescent compounds formation on the writing process and final material properties was investigated. The results indicate performances in terms of capacity with two order of magnitude higher than other reported information storage systems. Moreover, the fluorescent photosensitive vitroceramics may be integrated in other applications which appeal to nanofabrication as the driving force in electronics and photonics fields.

Keywords: data storage, fluorescent compounds, laser writing, vitroceramics

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Authors: Nazli Darkhal

Abstract:

The use of gems and ornaments has been common in Iran since the beginning of history. The prosperity of the country, the wealth, and the interest of the people of this land in luxurious and glorious life, combined with beauty, have always attracted the attention of the gems and ornaments of the Iranian people. Iranians are famous in the world for having a long history of collecting and recognizing precious stones. In this case, we can use the unique treasure of national jewelry. Raman spectroscopy method is one of the oscillating spectroscopy methods that is classified in the group of nondestructive study methods, and like other methods, in addition to several advantages, it also has disadvantages and problems. Micro Raman spectroscopy is one of the different types of Raman spectroscopy in which an optical microscope is combined with a Raman device to provide more capabilities and advantages than its original method. In this way, with the help of Raman spectroscopy and a light microscope, while observing more details from different parts of the historical sample, natural or artificial pigments can be identified in a small part of it. The EDX electron microscope also functions as the basis for the interaction of the electron beam with the matter. The beams emitted from this interaction can be used to examine samples. In this article, in addition to introducing the micro Raman spectroscopy method, studies have been conducted on the structure of three samples of existing stones in the historic citadel of Bam. Using this method of study on precious and semi-precious stones, in addition to requiring a short time, can provide us with complete information about the structure and theme of these samples. The results of experiments and gemology of the stones showed that the selected beads are agate and jasper, and they can be placed in the chalcedony group.

Keywords: bam citadel, precious and semi-precious stones, Raman spectroscopy, scanning electron microscope

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