RESUMO
[This corrects the article DOI: 10.1039/D2RA06050G.].
RESUMO
The article presents the method of producing gold nanoparticles using a high voltage arc discharge of alternating current with a frequency of 50 Hz in distilled water. The equipment necessary to carry out the process is described, including the construction of the reactor and the power source of a very simple design necessary to generate a high-voltage arc discharge between the electrodes. Arc discharge processes were carried out two times for 2 and 5 minutes, respectively, in ambient conditions without thermostating the reactor, at medium temperature varying in the range of 25-70 °C. The obtained gold nanoparticles were examined by means of various analytical techniques such as UV-vis spectroscopy, zeta potential measurement, energy dispersive X-ray analysis (EDS), X-ray diffraction (XRD). The morphology, surface, and size of the obtained nanoparticles were carried out using transmission electron microscopy (HRTEM) and dynamic light scattering (DLS). The concentration of the obtained colloids were determined using the mass spectrometry ICP-MS technique. The results show that high-voltage AC arc discharge is a simple and effective way to obtain stable gold nanoparticles under environmentally friendly conditions at relatively low production costs, and can be considered as an alternative to arc discharge nanoparticles synthesis by means of direct current (DC) methods.
RESUMO
Conventional metal wires suffer from a significant degradation or complete failure in their electrical performance, when subjected to harsh oxidizing environments, however wires constructed from Carbon Nanotubes (CNTs) have been found to actually improve in their electrical performance when subjected to these environments. These opposing reactions may provide new and interesting applications for CNT wires. Yet, before attempting to move to any real-world harsh environment applications, for the CNT wires, it is essential that this area of their operation be thoroughly examined. To investigate this, CNT wires were treated with multiple combinations of the strongest acids and halogens. The wires were then subjected to conductivity measurements, current carrying capacity tests, as well as Raman, microscopy and thermogravimetric analysis to enable the identification of both the limits of oxidative conductivity boosting and the onset of physical damage to the wires. These experiments have led to two main conclusions. Firstly, that CNT wires may operate effectively in harsh oxidizing environments where metal wires would easily fail and secondly, that the highest conductivity increase of the CNT wires can be achieved through a process of annealing, acetone and HCl purification followed by either H2O2 and HClO4 or Br2 treatment.
Assuntos
Bromo/química , Condutividade Elétrica , Peróxido de Hidrogênio/química , Nanotubos de Carbono/química , Oxidantes/química , Percloratos/química , OxirreduçãoRESUMO
The titanyl phthalocyanine (TiOPc) thin film deposited on glass, silicon and gold substrate have been studied using Raman spectroscopy, atomic force microscopy (AFM), absorption and profilometry measurements. The TiOPc thin layers have been deposited at room temperature by the quasi-molecular beam evaporation technique. The Raman spectra have been recorded using micro Raman system equipped with a confocal microscope. Using surface Raman mapping techni que with polarized Raman spectra the polymorphic forms of the TiOPc thin films distribution have been obtained. The AFM height and phase image were examined in order to find surface features and morphology of the thin films. Additionally to compare experimental results, structure optimization and vibrational spectra calculation of single TiOPc molecule were performed using DFT calculations. The received results showed that the parameters like polymorphic form, grain size, roughness of the surface in TiOPc thin films can well characterize the obtained organic thin films structures in terms of their use in optoelectronics and photovoltaics devices.
RESUMO
The paper deals with spectroscopic characterization of metallic phthalocyanines (Pc's) (indium and gallium) complexed with chlorine and substituted with four benzyloxyphenoxy peripheral groups in bulk systems, 2D Langmuir monolayers and Langmuir-Blodgett nanolayers. An influence of the molecular structure of dyes (the presence of metal and of substitutes attached to the phthalocyanine macroring) on the in situ measurements of light absorption is reported. Molecular arrangement of the phthalocyanine molecular skeleton in the Langmuir monolayers on water substrate and in the Langmuir-Blodgett nanolayers is evaluated. A comparison of the light absorption spectra of the phthalocyanine monolayers with the spectra of the dyes in solution supports the existence of dye aggregates in the monolayer. It was shown that the type of dye aggregates (oblique and H types) depends markedly on the dye molecular structures. The NIR-IR, IR reflection-absorption and Raman spectra are also monitored for Langmuir-Blodgett nanolayers in non-polarized and polarized light. It was shown that the dye molecules in the Langmuir-Blodgett layers are oriented nearly vertically with respect to a gold substrate.
Assuntos
Corantes Fluorescentes/química , Índio/química , Indóis/química , Compostos Organometálicos/química , Espectrofotometria/métodosRESUMO
The aim of this study was the surface modification of hydroxyapatite and ß-tricalcium phosphate by poly(3-hydroxybutyrate) grafting and characterization of modificates. The bioactivity examination was carried out by the determination to grow an apatite layer on modified materials during incubation in simulated body fluid at 37°C. The additional issue taken up in this paper was to investigate the influence of fluid replacement. The process of the surface modification of biomaterials was evaluated by means of infrared and Raman spectroscopy. Formation of the apatite layer was assessed by means of scanning electron microscopy and confirmed by energy dispersive, Raman and Fourier transformed infrared spectroscopy. During exposure in simulated body fluid, the variation of the zeta potential, pH measurement and relative weight was monitored. Examination of scanning electron microscopy micrographs suggests that modification of hydroxyapatite and ß-tricalcium phosphate by poly(3-hydroxybutyrate) significantly increases apatite layer formation. Raman spectroscopy evaluation revealed that the formation of the apatite layer was more significant in the case of hydroxyapatite modificate, when compared to the ß-tricalcium phosphate modificate. Both modificates were characterized by stable pH, close to the natural pH of human body fluids. Furthermore, we have shown that a weekly changed, simulated body fluid solution increases apatite layer formation.
Assuntos
Fosfatos de Cálcio/química , Durapatita/química , Hidroxibutiratos/química , Poliésteres/química , Materiais Biocompatíveis/química , Líquidos Corporais/química , Cálcio/análise , Humanos , Concentração de Íons de Hidrogênio , Microscopia Eletrônica de Varredura , Peso Molecular , Fosfatos/análise , Espectroscopia de Infravermelho com Transformada de Fourier , Análise Espectral Raman , Eletricidade Estática , Propriedades de SuperfícieRESUMO
Biomechanical properties of bone depend on the composition and organization of collagen fibers. In this study, Raman microspectroscopy was employed to determine the content of mineral and organic constituents and orientation of collagen fibers in spongy bone in the human head of femur at the microstructural level. Changes in composition and structure of trabecula were illustrated using Raman spectral mapping. The polarized Raman spectra permit separate analysis of local variations in orientation and composition. The ratios of ν2PO4³â»/Amide III, ν4PO4³â»/Amide III and ν1CO3²â»/ν2PO4³â» are used to describe relative amounts of spongy bone components. The ν1PO4³â»/Amide I ratio is quite susceptible to orientation effect and brings information on collagen fibers orientation. The results presented illustrate the versatility of the Raman method in the study of bone tissue. The study permits better understanding of bone physiology and evaluation of the biomechanical properties of bone.
Assuntos
Osso e Ossos/química , Osso e Ossos/fisiologia , Cabeça do Fêmur/química , Cabeça do Fêmur/fisiologia , Análise Espectral Raman , Idoso , Apatitas , Fenômenos Biomecânicos , Cálcio , Colágeno , Feminino , Humanos , FosfatosRESUMO
In this article, we present orientation study of metallophthalocyanine (MPcs) (CoPc, ZnPc, CuPc, and MgPc) thin films deposited on silicon substrate. The MPc's thin layers were obtained by the quasi-molecular beam evaporation. The micro-Raman scattering spectra of MPc's thin films were investigated in the spectral range 550-1650 cm-1 using 488 nm excitation wavelength. Raman scattering studies were performed at room temperature before and after annealing process. Annealing process of thin layers was carried out at 200 °C for 6 h. From polarized Raman spectra using surface Raman mapping, the information on polymorphic phase of MPc's layers has been obtained. The chosen Raman modes A1g and B1g are connected with different polymorphic phases of MPc (α and ß form) thin layers. Moreover, the obtained results showed the influence of the annealing process on the ordering of the molecular structure. Following the annealing process, it was observed arrangement of the thin layers structure being revealed in Raman spectra. The obtained results indicate that the annealing process has a significant influence on the structure of thin layers being under study.