Search results for: Rewati Raman

Authors: Radka Sefcu, Vaclava Antuskova, Ivana Turkova

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A growing market with modern artworks of a high price leads to the creation and selling of artwork counterfeits. Material analysis is an important part of the process of assessment of authenticity. Knowledge of materials and techniques used by original authors is also necessary. The contribution presents possibilities of non-invasive methods of structural analysis in research on paintings. It was proved that unambiguous identification of many art materials is feasible without sampling. The combination of Raman spectroscopy with FTIR-external reflection enabled the identification of pigments and binders on selected artworks of prominent Czech painters from the first half of the 20th century – Josef Čapek, Emil Filla, Václav Špála and Jan Zrzavý. Raman spectroscopy confirmed the presence of a wide range of white pigments - lead white, zinc white, titanium white, barium white and also Freeman's white as a special white pigment of painting. Good results were obtained for red, blue and most of the yellow areas. Identification of green pigments was often impossible due to strong fluorescence. Oil was confirmed as a binding medium on most of the analyzed artworks via FTIR - external reflection. Collected data present the valuable background for the determination of art materials characteristic for each painter (his palette) and its development over time. Obtained results will further serve as comparative material for the authentication of artworks. This work has been financially supported by the project of the Ministry of the Interior of the Czech Republic: The Development of a Strategic Cluster for Effective Instrumental Technological Methods of Forensic Authentication of Modern Artworks (VJ01010004).

Keywords: non-invasive analysis, Raman spectroscopy, FTIR-external reflection, forgeries

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Authors: M. Khalid Alamgir, Javed Ahsan Bhatti, M. Zafarullah Khan

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Thin film of amorphous carbon (DLC) was deposited on 316 steel using Nd: YAG laser having energy 300mJ. Pure graphite was used as a target. The vacuum in the deposition chamber was generated in the range of 10-6 mbar by turbo molecular pump. Ratio of sp3 to sp2 content shows amorphous nature of the film. This was confirmed by Raman spectra having two peaks around 1300 cm-1 i.e. D-band to 1700 cm-1 i.e. G-band. If sp3 bonding ratio is high, the films behave like diamond-like whereas, with high sp2, films are graphite-like. The ratio of sp3 and sp2 contents in the film depends upon the deposition method, hydrogen contents and system parameters. The structural study of the film was carried out by XRD. The hardness of the films as measured by Vickers hardness tester and was found to be 28 GPa. The EDX result shows the presence of carbon contents on the surface in high rate and optical microscopy result shows the smoothness of the film on substrate. The film possesses good adhesion and can be used to coat surgical instruments.

Keywords: DLC, thin film, Raman spectroscopy, XRD, EDX

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Authors: Touka Nassim, Tabli Dalila

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In this study, CuO thin films synthesized via simple sol-gel method, have been deposited on glass substrates by the spin coating technique and annealed at various temperatures. Samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier-transform infrared (FT-IR) and Raman spectroscopy, and UV-visible spectroscopy. The structural characterization by XRD reveals that the as prepared films were tenorite phase and have a high level of purity and crystallinity. The crystallite size of the CuO films was affected by the annealing temperature and was estimated in the range 20-31.5 nm. SEM images show a homogeneous distribution of spherical nanoparticles over the surface of the annealed films at 350 and 450 °C. Vibrational Spectroscopy revealed vibration modes specific to CuO with monolithic structure on the Raman spectra at 289 cm−1 and on FT-IR spectra around 430-580 cm−1. Electronic investigation performed by UV–Visible spectroscopy showed that the films have high absorbance in the visible region and their optical band gap increases from 2.40 to 2.66 eV (blue shift) with increasing annealing temperature from 350 to 550 °C.

Keywords: Sol-gel, Spin coating method, Copper oxide, Thin films

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

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Alkylated silicon nanocrystals (C11-SiNCs) were prepared successfully by galvanostatic etching of p-Si(100) wafers followed by a thermal hydrosilation reaction of 1-undecene in refluxing toluene in order to extract C11-SiNCs from porous silicon. Erbium trichloride was added to alkylated SiNCs using a simple mixing chemical route. To the best of our knowledge, this is the first investigation on mixing SiNCs with erbium ions (III) by this chemical method. The chemical characterization of C11-SiNCs and their mixtures with Er3+ (Er/C11-SiNCs) were carried out using X-ray photoemission spectroscopy (XPS). The optical properties of C11-SiNCs and their mixtures with Er3+ were investigated using Raman spectroscopy and photoluminescence (PL). The erbium-mixed alkylated SiNCs shows an orange PL emission peak at around 595 nm that originates from radiative recombination of Si. Er/C11-SiNCs mixture also exhibits a weak PL emission peak at 1536 nm that originates from the intra-4f transition in erbium ions (Er3+). The PL peak of Si in Er/C11-SiNCs mixture is increased in the intensity up to three times as compared to pure C11-SiNCs. The collected data suggest that this chemical mixing route leads instead to a transfer of energy from erbium ions to alkylated SiNCs.

Keywords: photoluminescence, silicon nanocrystals, erbium, Raman spectroscopy

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Authors: Ruolan Zhang, Ryo Imai, Naoko Senda, Tomoyuki Sakai

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Enzymes have attracted increasing attentions in industrial manufacturing for their applicability in catalyzing complex chemical reactions under mild conditions. Directed evolution has become a powerful approach to optimize enzymes and exploit their full potentials under the circumstance of insufficient structure-function knowledge. With the incorporation of cell-free synthetic biotechnology, rapid enzyme synthesis can be realized because no cloning procedure such as transfection is needed. Its open environment also enables direct enzyme measurement. These properties of cell-free biotechnology lead to excellent throughput of enzymes generation. However, the capabilities of current screening methods have limitations. Fluorescence-based assay needs applicable fluorescent label, and the reliability of acquired enzymatic activity is influenced by fluorescent label’s binding affinity and photostability. To acquire the natural activity of an enzyme, another method is to combine pre-screening step and high-performance liquid chromatography (HPLC) measurement. But its throughput is limited by necessary time investment. Hundreds of variants are selected from libraries, and their enzymatic activities are then identified one by one by HPLC. The turn-around-time is 30 minutes for one sample by HPLC, which limits the acquirable enzyme improvement within reasonable time. To achieve the real high-throughput enzyme screening, i.e., obtain reliable enzyme improvement within reasonable time, a widely applicable high-throughput measurement of enzymatic reactions is highly demanded. Here, a high-throughput screening method using broadband coherent anti-Stokes Raman spectroscopy (CARS) was proposed. CARS is one of coherent Raman spectroscopy, which can identify label-free chemical components specifically from their inherent molecular vibration. These characteristic vibrational signals are generated from different vibrational modes of chemical bonds. With the broadband CARS, chemicals in one sample can be identified from their signals in one broadband CARS spectrum. Moreover, it can magnify the signal levels to several orders of magnitude greater than spontaneous Raman systems, and therefore has the potential to evaluate chemical's concentration rapidly. As a demonstration of screening with CARS, alcohol dehydrogenase, which converts ethanol and nicotinamide adenine dinucleotide oxidized form (NAD+) to acetaldehyde and nicotinamide adenine dinucleotide reduced form (NADH), was used. The signal of NADH at 1660 cm⁻¹, which is generated from nicotinamide in NADH, was utilized to measure the concentration of it. The evaluation time for CARS signal of NADH was determined to be as short as 0.33 seconds while having a system sensitivity of 2.5 mM. The time course of alcohol dehydrogenase reaction was successfully measured from increasing signal intensity of NADH. This measurement result of CARS was consistent with the result of a conventional method, UV-Vis. CARS is expected to have application in high-throughput enzyme screening and realize more reliable enzyme improvement within reasonable time.

Keywords: Coherent Anti-Stokes Raman Spectroscopy, CARS, directed evolution, enzyme screening, Raman spectroscopy

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Authors: Astrid Tannert, Anuradha Ramoji, Christina Ebert, Frederike Gladigau, Lorena Tuchscherr, Jürgen Popp, Ute Neugebauer

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Staphylococcus aureus is a facultative intracellular pathogen, which by entering host cells may evade immunologic host response as well as antimicrobial treatment. In that way, S. aureus can cause persistent intracellular infections which are difficult to treat. Depending on the strain, S. aureus may persist at different intracellular locations like the phagolysosome. The first barrier invading pathogens from the blood stream that they have to cross are the endothelial cells lining the inner surface of blood and lymphatic vessels. Upon proceeding from an acute to a chronic infection, intracellular pathogens undergo certain biochemical and structural changes including a deceleration of metabolic processes to adopt for long-term intracellular survival and the development of a special phenotype designated as small colony variant. In this study, the endothelial cell line Ea.hy 926 was used as a model for acute and chronic S. aureus infection. To this end, Ea.hy 926 cells were cultured on QIAscout™ Microraft Arrays, a special graded cell culture substrate that contains around 12,000 microrafts of 200 µm edge length. After attachment to the substrate, the endothelial cells were infected with GFP-expressing S. aureus for 3 weeks. The acute infection and the development of persistent bacteria was followed by confocal laser scanning microscopy, scanning the whole Microraft Array for the presence and for detailed determination of the intracellular location of fluorescent intracellular bacteria every second day. After three weeks of infection representative microrafts containing infected cells, cells with protruded infections and cells that did never show any infection were isolated and fixed for Raman micro-spectroscopic investigation. For comparison, also microrafts with acute infection were isolated. The acquired Raman spectra are correlated with the fluorescence microscopic images to give hints about a) the molecular alterations in endothelial cells during acute and chronic infection compared to non-infected cells, and b) metabolic and structural changes within the pathogen when entering a mode of persistence within host cells. We thank Dr. Ruth Kläver from QIAGEN GmbH for her support regarding QIAscout technology. Financial support by the BMBF via the CSCC (FKZ 01EO1502) and from the DFG via the Jena Biophotonic and Imaging Laboratory (JBIL, FKZ PO 633/29-1, BA 1601/10-1) is highly acknowledged.

Keywords: correlative image analysis, intracellular infection, pathogen-host adaption, Raman micro-spectroscopy

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Authors: Jayashree Das, V. V. Srinivasu , D. K. Mishra, A. Maity

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Owing to the important potential applications over decades, transition metal (TM: Mn, Fe, Ni, Cu, Cr, V etc.) doped ZnO-based diluted magnetic semiconductors (DMS) always attract research attention for more and newer investigations. One of the interesting aspects of these materials is to study and understand the magnetic property at room temperature properly, which is very crucial to select a material for any related application. In this regard, Electron spin resonance (ESR) study has been proven to be a powerful technique to investigate the spin dynamics of electrons inside the system, which are responsible for the magnetic behaviour of any system. ESR as well as the Raman and Photoluminescence spectroscopy studies are also helpful to study the defects present or created inside the system in the form of oxygen vacancy or cluster instrumental in determining the room temperature ferromagnetic property of transition metal doped ZnO system, which can be controlled through varying dopant concentration, appropriate synthesis technique and sintering of the samples. For our investigation, we synthesised Cu-doped ZnO nanocrystalline samples with composition Zn1-xCux ( 0.005< x < 0.05) by pyrophoric method and sintered at a low temperature of 650 0C. The microwave absorption is studied by the Electron Spin Resonance (ESR) of X-band (9.46 GHz) at room temperature. Systematic analysis of the obtained ESR spectra reveals that all the compositions of Cu-doped ZnO samples exhibit resonance signals of appreciable line widths and g value ~ 2.2, typical characteristic of ferromagnetism in the sample. Raman scattering and the photoluminescence study performed on the samples clearly indicated the presence of pronounced defect related peaks in the respective spectra. Cu doping in ZnO with varying concentration also observed to affect the optical band gap and the respective absorption edges in the UV-Vis spectra. FTIR spectroscopy reveals the Cu doping effect on the stretching bonds of ZnO. To probe into the structural and morphological changes incurred by Cu doping, we have performed XRD, SEM and EDX study, which confirms adequate Cu substitution without any significant impurity phase formation or lattice disorder. With proper explanation, we attempt to correlate the results observed for the structural optical and magnetic behaviour of the Cu-doped ZnO samples. We also claim that our result can be instrumental for appropriate applications of transition metal doped ZnO based DMS in the field of optoelectronics and Spintronics.

Keywords: diluted magnetic semiconductors, electron spin resonance, raman scattering, spintronics.

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Authors: X. L. Zhou, S. Tunmee, I. Toda, K. Komatsu, S. Ohshio, H. Saitoh

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Hydrogenated amorphous carbon (a-C:H) films have been synthesized by a radio frequency plasma enhanced chemical vapor deposition (rf-PECVD) technique with different bias voltage from 0.0 to -0.5 kV. The Raman spectra displayed the polymer-like hydrogenated amorphous carbon (PLCH) film with 0.0 to -0.1 and a-C:H films with -0.2 to -0.5 kV of bias voltages. The surface chemical information of all films were studied by X-ray photo electron spectroscopy (XPS) technique, presented to C-C (sp2 and sp3) and C-O bonds, and relative carbon (C) and oxygen (O) atomics contents. The O contamination had affected on structure and optical properties. The true density of PLCH and a-C:H films were characterized by X-ray refractivity (XRR) method, showed the result as in the range of 1.16-1.73 g/cm3 that depending on an increasing of bias voltage. The hardness was proportional to the true density of films. In addition, the optical properties i.e. refractive index (n) and extinction coefficient (k) of these films were determined by a spectroscopic ellipsometry (SE) method that give formation to in 1.62-2.10 (n) and 0.04-0.15 (k) respectively. These results indicated that the optical properties confirmed the Raman results as presenting the structure changed with applied bias voltage increased.

Keywords: negative bias voltage, a-C:H film, oxygen contamination, optical properties

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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: G. Eom, H. Kim, A. Hwang, T. Kang, B. Kim

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Telomerase activity is overexpressed in over 85% of human cancers while suppressed in normal somatic cells. Telomerase has been attracted as a universal cancer biomarker. Therefore, the development of effective telomerase activity detection methods is urgently demanded in cancer diagnosis and therapy. Herein, we report a nanogap-rich Au nanowire (NW) surface-enhanced Raman scattering (SERS) sensor for detection of human telomerase activity. The nanogap-rich Au NW SERS sensors were prepared simply by uniformly depositing nanoparticles (NPs) on single-crystalline Au NWs. We measured SERS spectra of methylene blue (MB) from 60 different nanogap-rich Au NWs and obtained the relative standard deviation (RSD) of 4.80%, confirming the superb reproducibility of nanogap-rich Au NW SERS sensors. The nanogap-rich Au NW SERS sensors enable us to detect telomerase activity in 0.2 cancer cells/mL. Furthermore, telomerase activity is detectable in 7 different cancer cell lines whereas undetectable in normal cell lines, which suggest the potential applicability of nanogap-rich Au NW SERS sensor in cancer diagnosis. We expect that the present nanogap-rich Au NW SERS sensor can be useful in biomedical applications including a diverse biomarker sensing.

Keywords: cancer biomarker, nanowires, surface-enhanced Raman scattering, telomerase

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Authors: Alejandro Carrasco-Pena, Mahmoud Omer, Nina Orlovskaya

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The results of studies of microstructure, mechanical behavior, vibrational response, and flow field analysis of critically endangered staghorn coral (Acropora cervicornis) skeletons are reported. The CaCO₃ aragonite structure of a chemically-cleaned coral skeleton of A. cervicornis was studied by optical microscopy and computer tomography. The mechanical behavior was studied using uniaxial compression and Vickers hardness technique. The average maximum stress measured during skeleton uniaxial compression was 10.7 ± 2.24 MPa and Vickers hardness was 3.56 ± 0.31 GPa. The vibrational response of the aragonite structure was studied by micro-Raman spectroscopy, which showed a substantial dependence of the structure on applied compressive stress. The flow-field around a single coral skeleton forming vortices in the wake of the moving skeleton was measured using Particle Image Velocimetry (PIV). The results are important for further analysis of time-dependent mechanical fatigue behavior and predicting the lifetime of staghorn corals.

Keywords: failure, mechanical properties, microstructure, Raman spectroscopy

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Authors: T. H. Huang, C. Y. Gao, C. H. Lin, J. L. Kwo, Y. K. Tseng

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The design and reliability of solar photovoltaic modules are crucial to the development of solar energy, and efforts are still being made to extend the life of photovoltaic modules to improve their efficiency because natural aging is time-consuming and does not provide manufacturers and investors with timely information, accelerated aging is currently the best way to estimate the life of photovoltaic modules. In this study, the accelerated aging of different light sources was combined with spectral response measurements to understand the effect of light sources on aging tests. In this study, there are two types of experimental samples: packaged and unpackaged and then irradiated with full-spectrum and UVC light sources for accelerated aging, as well as a control group without aging. The full-spectrum aging was performed by irradiating the solar cell with a xenon lamp like the solar spectrum for two weeks, while the accelerated aging was performed by irradiating the solar cell with a UVC lamp for two weeks. The samples were first visually observed, and infrared thermal images were taken, and then the electrical (IV) and Spectral Responsivity (SR) data were obtained by measuring the spectral response of the samples, followed by Scanning Electron Microscopy (SEM), Raman spectroscopy (Raman), and X-ray Diffraction (XRD) analysis. The results of electrical (IV) and Spectral Responsivity (SR) and material analyses were used to compare the differences between packaged and unpackaged solar cells with full spectral aging, accelerated UVC aging, and unaged solar cells. The main objective of this study is to compare the difference in the aging of packaged and unpackaged solar cells by irradiating different light sources. We determined by infrared thermal imaging that both full-spectrum aging and UVC accelerated aging increase the defects of solar cells, and IV measurements demonstrated that the conversion efficiency of solar cells decreases after full-spectrum aging and UVC accelerated aging. SEM observed some scorch marks on both unpackaged UVC accelerated aging solar cells and unpackaged full-spectrum aging solar cells. Raman spectroscopy examines the Si intensity of solar cells, and XRD confirms the crystallinity of solar cells by the intensity of Si and Ag winding peaks.

Keywords: solar cell, aging, spectral response measurement

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Authors: A. L. R. Rangel, J. A. M. Chaves, A. P. R. Alves Claro

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Surface modification of titanium and its alloys using TiO2 nanotube growth has been widely studied for biomedical field due to excellent interaction between implant and biological environment. The success of this treatment is directly related to anatase phase formation (TiO2 phase) which affects the cells growth. The aim of this study was to evaluate the phases formed in the nanotubes growth on the Ti-15Mo surface. Nanotubes were grown by electrochemical anodization of the alloy in ammonium fluoride based glycerol electrolyte for 24 hours at 20V. Then, the samples were annealed at 200°,400°, 450°, 500°, 600°, and 800° C for 1 hour. Contact angles measurements, scanning electron microscopy images and X rays diffraction analysis (XRD) were carried out for all samples. Raman Spectroscopy was used to evaluate TiO2 phases transformation in nanotubes samples as well. The results of XRD showed anatase formation for lower temperatures, while at 800 ° C the rutile phase was observed all over the surface. Raman spectra indicate that this phase transition occurs between 500 and 600 °C. The different phases formed have influenced the nanotubes morphologies, since higher annealing temperatures induced agglutination of the TiO2 layer, disrupting the tubular structure. On the other hand, the nanotubes drastically reduced the contact angle, regardless the annealing temperature.

Keywords: nanotubes, TiO2, titanium alloys, Ti-15Mo

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Authors: Alaa Y. Ali, Natalie P. Holmes, John Holdsworth, Warwick Belcher, Paul Dastoor, Xiaojing Zhou

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Multi-layered graphene has been produced under low temperature chemical vapour deposition (CVD) growth conditions by utilizing an organic solvent and polymer film source. Poly(methylmethacrylate) (PMMA) was dissolved in chlorobenzene solvent and used as a drop-cast film carbon source on a quartz slide. A source temperature (T_source) of 180 °C provided sufficient carbon to grow graphene, as identified by Raman spectroscopy, on clean copper foil catalytic surfaces.  Systematic variation of hydrogen gas (H₂) flow rate from 25 standard cubic centimeters per minute (sccm) to 100 sccm and CVD temperature (T_growth) from 400 to 800 °C, yielded graphene films of varying quality as characterized by Raman spectroscopy. The optimal graphene growth parameters were found to occur with a hydrogen flow rate of 75 sccm sweeping the 180 °C source carbon past the Cu foil at 600 °C for 1 min. The deposition at 600 °C with a H₂ flow rate of 75 sccm yielded a 2D band peak with ~53.4 cm^-1 FWHM and a relative intensity ratio of the G to 2D bands (I_G/I_2D) of 0.21. This recipe fabricated a few layers of good quality graphene.

Keywords: graphene, chemical vapor deposition, carbon source, low temperature growth

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Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, M. Hajdúchová, V. Enev, J. Wasserbauer

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In this work, the effect of particle size on the structural and magnetic properties of CoFe2-xGdxO4 (x =0.1) spinel ferrite nanoparticles synthesized by starch-assisted sol-gel auto combustion method was investigated. The different sized CoFe2-xGdxO4 (x =0.1) spinel ferrite nanoparticles were achieved after annealing at different temperature 500, 700 and 900 oC. The structural phases, crystallite size and lattice parameter of synthesized ferrite nanoparticles were estimated from X-ray diffraction studies. The field emission scanning electron microscopy study demonstrated increase in particle size with increase of annealing temperature. Raman spectroscopy study indicated the change in octahedral and tetrahedral site related Raman modes in Gd3+ ions doped cobalt ferrite nanoparticles. An infrared spectroscopy study showed the presence of two absorption bands in the frequency range around 580 cm-1 (ν1) and around 340 cm-1 (ν2); which indicated the presence of tetrahedral and octahedral group complexes, respectively, within the spinel ferrite nanoparticles. Vibrating Sample magnetometer study showed that the saturation magnetization and coercivity changes with particle size of CoFe2-xGdxO4 (x =0.1) spinel ferrite.

Keywords: magnetic properties, spinel ferrite, nanoparticles, sol-gel synthesis

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Authors: Mourad Makhlouf, Bouabdellah Benaicha, Zoubir Benmaamar, Didier Villemin

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The addition of combustion catalysts to ammonium perchlorate-based composite fuels can indeed significantly enhance their performance. In this work, a nanocomposite was synthesized using graphene oxide (GO) and hematite nanoparticles grafted onto graphene oxide as a catalyst support.To characterize the nanocomposite, several experimental techniques were employed, including Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, and scanning electron microscopy (SEM). FTIR is useful for analyzing chemical bonding and functional groups, while Raman spectroscopy provides information about the vibrational modes of the materials. SEM allows for visualizing the surface morphology and structure.The thermal analysis of two mixtures, one based on AP/GO and the other on AP/GO-Fe2O3, was conducted with varying percentages. The results indicated that the nanocomposite GO-Fe2O3 acted as a catalyst, significantly accelerating the thermal decomposition process of AP. This catalytic effect ultimately led to an improvement in the energy performance of the composite fuel.Overall, the synthesis and characterization of the nanocomposite, as well as the thermal analysis, demonstrated the effectiveness of GO-Fe2O3 as a combustion catalyst in enhancing the performance of ammonium perchlorate-based composite fuels.

Keywords: composite propellants, ammonium perchlorate, nanocomposite, catalytic support, hematite nanoparticles, graphene oxide, thermal decomposition

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Authors: C. Fornacelli, P. Colomban, E. Mugnaioli, I. Memmi Turbanti

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When semiconductor particles are reduced in scale to nanometer dimension, their optical and electro-optical properties strongly differ from those of bulk crystals of the same composition. Since sampling is often not allowed concerning cultural heritage artefacts, the potentialities of two non-invasive techniques, such as Raman and Fiber Optic Reflectance Spectroscopy (FORS), have been investigated and the results of the analysis on some original glasses of different colours (from yellow to orange and deep red) and periods (from the second decade of the 20th century to present days) are reported in the present study. In order to evaluate the potentialities of the application of non-invasive techniques to the investigation of the structure and distribution of nanoparticles dispersed in a glass matrix, Scanning Electron Microscopy (SEM) and energy-disperse spectroscopy (EDS) mapping, together with Transmission Electron Microscopy (TEM) and Electron Diffraction Tomography (EDT) have also been used. Raman spectroscopy allows a fast and non-destructive measure of the quantum dots composition and size, thanks to the evaluation of the frequencies and the broadening/asymmetry of the LO phonons bands, respectively, though the important role of the compressive strain arising from the glass matrix and the possible diffusion of zinc from the matrix to the nanocrystals should be taken into account when considering the optical-phonons frequency values. The incorporation of Zn has been assumed by an upward shifting of the LO band related to the most abundant anion (S or Se), while the role of the surface phonons as well as the confinement-induced scattering by phonons with a non-zero wavevectors on the Raman peaks broadening has been verified. The optical band gap varies from 2.42 eV (pure CdS) to 1.70 eV (CdSe). For the compositional range between 0.5≤x≤0.2, the presence of two absorption edges has been related to the contribution of both pure CdS and the CdSxSe1-x solid solution; this particular feature is probably due to the presence of unaltered cubic zinc blende structures of CdS that is not taking part to the formation of the solid solution occurring only between hexagonal CdS and CdSe. Moreover, the band edge tailing originating from the disorder due to the formation of weak bonds and characterized by the Urbach edge energy has been studied and, together with the FWHM of the Raman signal, has been assumed as a good parameter to evaluate the degree of topological disorder. SEM-EDS mapping showed a peculiar distribution of the major constituents of the glass matrix (fluxes and stabilizers), especially concerning those samples where a layered structure has been assumed thanks to the spectroscopic study. Finally, TEM-EDS and EDT were used to get high-resolution information about nanocrystals (NCs) and heterogeneous glass layers. The presence of ZnO NCs (< 4 nm) dispersed in the matrix has been verified for most of the samples, while, for those samples where a disorder due to a more complex distribution of the size and/or composition of the NCs has been assumed, the TEM clearly verified most of the assumption made by the spectroscopic techniques.

Keywords: CdSxSe1-x, EDT, glass, spectroscopy, TEM-EDS

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Authors: Nipin Kohli, Ravi Chand Singh

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Diabetes mellitus is a serious illness and can be life-threatening if left untreated. Acetone present in the exhaled breath of a diabetic person is a biomarker of patients suffering from diabetes mellitus and is higher than its usual concentration present in the breath of healthy people. In the present work, a portable gas sensor system based on chromium oxide (Cr₂O₃) nanoparticles has been developed that can analyze diabetic patient’s breath. Undoped and indium (In) doped Cr₂O₃ nanoparticles were synthesized by a chemical route and characterized by X-ray diffraction, scanning electron microscopy, Raman spectroscopy, UV-visible spectroscopy, and photoluminescence spectroscopy for their structural, morphological and optical properties. Thick film gas sensors were fabricated out of synthesized samples. To diagnose diabetes, the sensors’ response to low concentrations of acetone was measured, and it was found that the addition of indium dramatically enhances the acetone gas sensing response. Moreover, the fabricated sensors were highly stable, reproducible and resistant to humidity. Enhancement of sensor response of doped sensors towards acetone can be ascribed to increase in defects due to addition of a dopant, and it was found that in-doped Cr₂O₃ sensors are more useful for analysis of breath of diabetic patients.

Keywords: Diabetes mellitus, nanoparticles, raman spectroscopy, sensor

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Authors: Iuliia Riabenko, Konstantin Beloshenko, Sergey Shulga, Valeriy Shulga

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An optical system has been developed consisting of a TIR lens and an aspherical surface designed to collect Stokes radiation from biomolecules. The freeform material is SYLGARD-184, which provides a low level of noise associated with the luminescence of the substrate. The refractive index of SYLGARD-184 is 1.4028 for a wavelength of 632 nm, the Abbe number is 72, these material parameters make it possible to design the desired shape for the wavelength range of 640-700 nm. The system consists of a TIR lens, inside which is placed a high-quality resonant system consisting of a biomolecule and a metal colloid. This system can be described using the coupled oscillator model. The laser excitation radiation was fed through the base of the TIR lens. The sample was mounted inside the TIR lens at a distance of 8 mm from the base. As a result of Raman scattering of laser radiation, a Stokes bend appeared from the biolayer. The task of this work was that it was necessary to collect this radiation emitted at a 4π steradian angle. For this, an internal aspherical surface was used, which made it possible to defocus the beam emanating from the biolayer and direct its radiation to the borders of the TIR lens at the Brewster angle. The collated beam of Stokes radiation contains 97% of the energy scattered by the biolayer. Thus, a simple scheme was proposed for collecting and collimating the Stokes radiation of biomolecules.

Keywords: TIR lens, freeform material, raman scattering, biolayer, brewster angle

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Authors: Srijitra Khanpakdee, Teera Butburee, Jung-Ho Yun, Miaoqiang Lyu, Supphasin Thaweesak, Piangjai Peerakiatkhajohn

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The synthesis of titanium dioxide (TiO₂) nanorods (NRs) on fluorine-doped tin oxide (FTO) glass via hydrothermal methods was investigated to determine the optimal reaction time for enhanced photocatalytic and optical performance. Reaction times of 4, 6, and 8 hours were studied. Characterization through SEM, UV-vis, XRD, FTIR, Raman spectroscopy and photoelectrochemical (PEC) techniques revealed significant differences in the properties of the TiO₂ NRs based on the reaction duration. XRD and Raman spectroscopy analysis confirmed the formation of the rutile phase of TiO₂. As photoanodes in PEC cells, TiO₂ NRs synthesized for 4 hours exhibited the best photocatalytic activity, with the highest photocurrent density and superior charge transport properties, attributed to their densely packed vertical structure. Longer reaction times resulted in less optimal morphological and photoelectrochemical characteristics. The bandgap of the TiO₂ NRs remained consistent around 3.06 eV, with only slight variations observed. This study highlights the critical role of reaction time in hydrothermal synthesis, identifying 4 hours as the optimal duration for producing TiO₂ NRs with superior photoelectrochemical performance. These findings provide valuable insights for optimizing TiO₂-based materials for solar energy conversion and renewable energy applications.

Keywords: titanium dioxide, nanorods, hydrothermal, photocatalytic, photoelectrochemical

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Authors: El Mehdi Haily, Lahcen Bih, Mohammed Azrour, Bouchaib Manoun

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The effects of xBi₂O₃-yBaO-zP₂O₅ (BBP) glass addition on the sintering, structural, and dielectric properties of BaTiO₃ ceramic (BT) are studied. The BT ceramic was synthesized by the conventional solid-state reaction method while the glasses BaO-Bi₂O₃-P₂O₅ (BBP) were elaborated by melting and quenching process. Different composites BT-xBBP were formed by mixing the BBP glasses with BT ceramic. For each glass composition, where the ratio (x:y:z) is maintained constant, we have developed three composites with different glass weight percentage (x = 2.5, 5, and 7.5 wt %). Addition of the glass helps in better sintering at lower temperatures with the presence of liquid phase at the respective sintering temperatures. The results showed that the sintering temperature decreased from more than 1300°C to 900°C. Density measurements of the composites are performed using the standard Archimedean method with water as medium liquid. It is found that their density and molar volume decrease and increase with glass content, respectively. Raman spectroscopy is used to characterize their structural approach. This technique has allowed the identification of different structural units of phosphate and the characteristic vibration modes of the BT. The electrical properties of the composite samples are carried out by impedance spectroscopy in the frequency range of 10 Hz to 1 MHz under various temperatures from 300 to 473 K. The obtained results show that their dielectric properties depend both on the content of the glass in the composite and the Bi/P ratio in the glasses.

Keywords: phosphate, glasses, composite, Raman spectroscopy, dielectric properties

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Authors: Vedanki Khandenwal, Pawan Srivastava, Kartick Tarafder, Subhasis Ghosh

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We present here the experimental realization of controlled doping of graphene monolayers through charge transfer by trapping selected organic molecules between the graphene layer and underlying substrates. This charge transfer between graphene and trapped molecule leads to controlled n-type or p-type doping in monolayer graphene (MLG), depending on whether the trapped molecule acts as an electron donor or an electron acceptor. Doping controllability has been validated by a shift in corresponding Raman peak positions and a shift in Dirac points. In the transfer characteristics of field effect transistors, a significant shift of Dirac point towards positive or negative gate voltage region provides the signature of p-type or n-type doping of graphene, respectively, as a result of the charge transfer between graphene and the organic molecules trapped within it. In order to facilitate the charge transfer interaction, it is crucial for the trapped molecules to be situated in close proximity to the graphene surface, as demonstrated by findings in Raman and infrared spectroscopies. However, the mechanism responsible for this charge transfer interaction has remained unclear at the microscopic level. Generally, it is accepted that the dipole moment of adsorbed molecules plays a crucial role in determining the charge-transfer interaction between molecules and graphene. However, our findings clearly illustrate that the doping effect primarily depends on the reactivity of the constituent atoms in the adsorbed molecules rather than just their dipole moment. This has been illustrated by trapping various molecules at the graphene−substrate interface. Dopant molecules such as acetone (containing highly reactive oxygen atoms) promote adsorption across the entire graphene surface. In contrast, molecules with less reactive atoms, such as acetonitrile, tend to adsorb at the edges due to the presence of reactive dangling bonds. In the case of low-dipole moment molecules like toluene, there is a lack of substantial adsorption anywhere on the graphene surface. Observation of (i) the emergence of the Raman D peak exclusively at the edges for trapped molecules without reactive atoms and throughout the entire basal plane for those with reactive atoms, and (ii) variations in the density of attached molecules (with and without reactive atoms) to graphene with their respective dipole moments provides compelling evidence to support our claim. Additionally, these observations were supported by first principle density functional calculations.

Keywords: graphene, doping, charge transfer, liquid phase exfoliation

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Authors: Ravish K. Jain, Jatinder Kaur, Shaira Arora, Arun Kumar, Amit K. Chawla, Atul Khanna

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Surface-dependent properties such as hydrophobicity can be modified significantly by oblique angle deposition technique. Bi thin films were studied for their hydrophobic nature. The effects of oblique angle deposition on structural, surface morphology, electrical and wettability properties of Bi thin films have been studied and a comparison of these physical properties of normally deposited and obliquely deposited Bi films has been carried out in this study. X-ray diffraction studies found that films have highly oriented hexagonal crystal structure and crystallite size is smaller for obliquely deposited (70 nm) film as compared to that of the normally deposited film (111 nm). Raman spectra of the films consist of peaks corresponding to E_g and A_1g first-order Raman modes of bismuth. The atomic force and scanning electron microscopy studies show that the surface roughness of obliquely deposited film is higher as compared to that of normally deposited film. Contact angle measurements revealed that both films are strongly hydrophobic in nature with the contact angles of 105ᵒ and 119ᵒ for normally and obliquely deposited films respectively. Oblique angle deposition enhances the hydrophobicity of the film. The electrical conductivity of the film is significantly reduced by oblique angle deposition. The activation energies for electrical conduction were determined by four-probe measurements and are 0.016 eV and 0.018 eV for normally and obliquely deposited films respectively.

Keywords: bi thin films, hydrophobicity, oblique angle deposition, surface morphology

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Authors: Zuzana Chaloupková, Zdeňka Marková, Václav Ranc, Radek Zbořil

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Prostate cancer is now one of the most serious oncological diseases in men with an incidence higher than that of all other solid tumors combined. Diagnosis of prostate cancer usually involves detection of related genes or detection of marker proteins, such as PSA. One of the new potential markers is PSMA (prostate specific membrane antigen). PSMA is a unique membrane bound glycoprotein, which is considerably overexpressed on prostate cancer as well as neovasculature of most of the solid tumors. Commonly applied methods for a detection of proteins include techniques based on immunochemical approaches, including ELISA and RIA. Magnetically assisted surface enhanced Raman spectroscopy (MA-SERS) can be considered as an interesting alternative to generally accepted approaches. This work describes a utilization of MA-SERS in a detection of PSMA in human blood. This analytical platform is based on magnetic nanocomposites Fe3O4@Ag, functionalized by a low-molecular selector labeled as JB303. The system allows isolating the marker from the complex sample using application of magnetic force. Detection of PSMA is than performed by SERS effect given by a presence of silver nanoparticles. This system allowed us to analyze PSMA in clinical samples with limits of detection lower than 1 ng/mL.

Keywords: diagnosis, cancer, PSMA, MA-SERS, Ag nanoparticles

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Authors: Pawel Albrycht, Monika Ksiezopolska-Gocalska, Robert Holyst

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Surface Enhanced Raman Spectroscopy (SERS) is a technique of growing importance not only in purely scientific research related to analytical chemistry. It finds more and more applications in broadly understood testing - medical, forensic, pharmaceutical, food - and everywhere works perfectly, on one condition that SERS substrates used for testing give adequate enhancement, repeatability, and homogeneity of SERS signal. This is a problem that has existed since the invention of this technique. Some laboratories use as SERS amplifiers colloids with silver or gold nanoparticles, others form rough silver or gold surfaces, but results are generally either weak or unrepeatable. Furthermore, these structures are very often highly specific - they amplify the signal only of a small group of compounds. It means that they work with some kinds of analytes but only with those which were used at a developer’s laboratory. When it comes to research on different compounds, completely new SERS 'substrates' are required. That underlay our decision to develop universal substrates for the SERS spectroscopy. Generally, each compound has different affinity for both silver and gold, which have the best SERS properties, and that's what depends on what signal we get in the SERS spectrum. Our task was to create the platform that gives a characteristic 'fingerprint' of the largest number of compounds with very high repeatability - even at the expense of the intensity of the enhancement factor (EF) (possibility to repeat research results is of the uttermost importance). As specified above SERS substrates are offered by SERSitive company. Applied method is based on cyclic potentiodynamic electrodeposition of silver or silver-gold nanoparticles on the conductive surface of ITO-coated glass at controlled temperature of the reaction solution. Silver nanoparticles are supplied in the form of silver nitrate (AgNO₃, 10 mM), gold nanoparticles are derived from tetrachloroauric acid (10 mM) while sodium sulfite (Na₂O₃, 5 mM) is used as a reductor. To limit and standardize the size of the SERS surface on which nanoparticles are deposited, photolithography is used. We secure the desired ITO-coated glass surface, and then etch the unprotected ITO layer which prevents nanoparticles from settling at these sites. On the prepared surface, we carry out the process described above, obtaining SERS surface with nanoparticles of sizes 50-400 nm. The SERSitive platforms present highly sensitivity (EF = 10⁵-10⁶), homogeneity and repeatability (70-80%).

Keywords: electrodeposition, nanoparticles, Raman spectroscopy, SERS, SERSitive, SERS platforms, SERS substrates

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Authors: Aurea C. L. Lacerda, Paulo R. H. Moreno, Bruna M. P. Vianna, Cristina H. R. Serra, Airton Martin, André R. Baby, Vladi O. Consiglieri, Telma M. Kaneko

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The modified Franz cell is the most widely used model for in vitro permeation studies, however it still presents some disadvantages. Thus, some alternative methods have been developed such as Skin PAMPA, which is a bio- artificial membrane that has been applied for skin penetration estimation of xenobiotics based on HT permeability model consisting. Skin PAMPA greatest advantage is to carry out more tests, in a fast and inexpensive way. The membrane system mimics the stratum corneum characteristics, which is the primary skin barrier. The barrier properties are given by corneocytes embedded in a multilamellar lipid matrix. This layer is the main penetration route through the paracellular permeation pathway and it consists of a mixture of cholesterol, ceramides, and fatty acids as the dominant components. However, there is no consensus on the membrane composition. The objective of this work was to compare the performance among different bio-artificial membranes for studying the permeation in skin PAMPA system. Material and methods: In order to mimetize the lipid composition`s present in the human stratum corneum six membranes were developed. The membrane composition was equimolar mixture of cholesterol, ceramides 1-O-C18:1, C22, and C20, plus fatty acids C20 and C24. The membrane integrity assay was based on the transport of Brilliant Cresyl Blue, which has a low permeability; and Lucifer Yellow with very poor permeability and should effectively be completely rejected. The membrane characterization was performed using Confocal Laser Raman Spectroscopy, using stabilized laser at 785 nm with 10 second integration time and 2 accumulations. The membrane behaviour results on the PAMPA system were statistically evaluated and all of the compositions have shown integrity and permeability. The confocal Raman spectra were obtained in the region of 800-1200 cm-1 that is associated with the C-C stretches of the carbon scaffold from the stratum corneum lipids showed similar pattern for all the membranes. The ceramides, long chain fatty acids and cholesterol in equimolar ratio permitted to obtain lipid mixtures with self-organization capability, similar to that occurring into the stratum corneum. Conclusion: The artificial biological membranes studied for Skin PAMPA showed to be similar and with comparable properties to the stratum corneum.

Keywords: bio-artificial membranes, comparison, confocal Raman, skin PAMPA

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Authors: Hasnaa Benchorfi

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The Tellurite glasses exhibit interesting properties, notably their low melting point (700-900°C), high refractive index (≈2), high transparency in the infrared region (up to 5−6 μm), interesting linear and non-linear optical properties and high rare earth ions solubility. These properties give tellurite glasses a great interest in various optical applications. Transparent ceramics present advantages compared to glasses, such as improved mechanical, thermal and optical properties. But, the elaboration process of these ceramics requires complex sintering conditions. The full crystallization of glass into transparent ceramics is an alternative to circumvent the technical challenges related to the ceramics obtained by conventional processing. In this work, a crystallization study of a specific glass composition in the system TeO2-Ta2O5-Bi2O3 shows structural transitions from the glass to the stabilization of an unreported anti-glass phase to a transparent ceramic upon heating. An anti-glass is a material with a cationic long-range order and a disordered anion sublattice. Thus, the X-ray diffraction patterns show sharp peaks, while the Raman bands are broad and similar to those of the parent glass. The structure and microstructure of the anti-glass and corresponding ceramic were characterized by Powder X-Ray Diffraction, Electron Back Scattered Diffraction, Transmission Electron Microscopy and Raman spectroscopy. The optical properties of the Er3+-doped samples are also discussed.

Keywords: glass, congruent crystallization, anti-glass, glass-ceramic, optics

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Authors: Anjana Jain, S. Jayanth Kumar

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Polyvinylidene fluoride (PVDF) is a well-known material for remarkable mechanical properties, resistance to chemicals and superior ferroelectric performances. This endows PVDF the potential for application in supercapacitor devices. The dielectric properties of PVDF, however, are not very high. To improve the dielectric properties of Polyvinylidene fluoride (PVDF), Piezoelectric polymer nanocomposites are prepared without affecting the other useful properties of PVDF. Polyaniline (PANI) was chosen as a filler material to prepare the nanocomposites. PVDF-PANI nanocomposite films were prepared using solvent cast method with different volume fractions of PANI varying from 0.04% to 0.048% of PANI content. The films are characterized for structural, mechanical, and surface morphological properties using X-ray diffraction, differential scanning calorimeter, Raman spectra, Infrared spectra, tensile testing, and scanning electron microscopy. The X-ray diffraction analysis shows that, prepared films were in β-phase. The DSC scans indicated that the degree of crystallinity in PVDF-PANI is improved. Raman and Infrared spectrum further confirm the presence of β-phase of PVDF-PANI film. Tensile properties of PVDF-PANI films were in good agreement with those reported in literature. The surface feature shows that PANI is uniformly distributed in PVDF and also results in disappearance of spherulites. The influence of volume fraction of PANI in PVDF on dielectric properties was analyzed. The results showed that the dielectric permittivity of PVDF-PANI (120) was much higher than that of PVDF (12). The sensitivity of these films was studied on application of a pressure and a constant output voltage was obtained.

Keywords: dielectric Properties, PANI, PVDF, smart materials

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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: Pola Goldberg Oppenheimer, Stephan Hofmann, Sumeet Mahajan

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Owing to its fingerprint molecular specificity and high sensitivity, surface-enhanced Raman scattering (SERS) is an established analytical tool for chemical and biological sensing capable of single-molecule detection. A strong Raman signal can be generated from SERS-active platforms given the analyte is within the enhanced plasmon field generated near a noble-metal nanostructured substrate. The key requirement for generating strong plasmon resonances to provide this electromagnetic enhancement is an appropriate metal surface roughness. Controlling nanoscale features for generating these regions of high electromagnetic enhancement, the so-called SERS ‘hot-spots’, is still a challenge. Significant advances have been made in SERS research, with wide-ranging techniques to generate substrates with tunable size and shape of the nanoscale roughness features. Nevertheless, the development and application of SERS has been inhibited by the irreproducibility and complexity of fabrication routes. The ability to generate straightforward, cost-effective, multiplex-able and addressable SERS substrates with high enhancements is of profound interest for miniaturised sensing devices. Carbon nanotubes (CNTs) have been concurrently, a topic of extensive research however, their applications for plasmonics has been only recently beginning to gain interest. CNTs can provide low-cost, large-active-area patternable substrates which, coupled with appropriate functionalization capable to provide advanced SERS-platforms. Herein, advanced methods to generate CNT-based SERS active detection platforms will be discussed. First, a novel electrohydrodynamic (EHD) lithographic technique will be introduced for patterning CNT-polymer composites, providing a straightforward, single-step approach for generating high-fidelity sub-micron-sized nanocomposite structures within which anisotropic CNTs are vertically aligned. The created structures are readily fine-tuned, which is an important requirement for optimizing SERS to obtain the highest enhancements with each of the EHD-CNTs individual structural units functioning as an isolated sensor. Further, gold-functionalized VACNTFs are fabricated as SERS micro-platforms. The dependence on the VACNTs’ diameters and density play an important role in the Raman signal strength, thus highlighting the importance of structural parameters, previously overlooked in designing and fabricating optimized CNTs-based SERS nanoprobes. VACNTs forests patterned into predesigned pillar structures are further utilized for multiplex detection of bio-analytes. Since CNTs exhibit electrical conductivity and unique adsorption properties, these are further harnessed in the development of novel chemical and bio-sensing platforms.

Keywords: carbon nanotubes (CNTs), EHD patterning, SERS, vertically aligned carbon nanotube forests (VACNTF)

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