RESUMO
In this study, ZnO nanostructures with different types of morphologies and particle sizes were evaluated and applied for the development of an immunosensor. The first material was composed of spherical, polydisperse nanostructures with a particle size in the range of 10-160 nm. The second was made up of more compact rod-like spherical nanostructures with the diameter of these rods in the range of 50-400 nm, and approximately 98% of the particles were in the range of 20-70 nm. The last sample of ZnO was made up of rod-shaped particles with a diameter of 10-80 nm. These ZnO nanostructures were mixed with Nafion solution and drop-casted onto screen-printed carbon electrodes (SPCE), followed by a further immobilization of the prostate-specific antigen (PSA). The affinity interaction of PSA with monoclonal antibodies against PSA (anti-PSA) was evaluated using the differential pulse voltammetry technique. The limit of detection and limit of quantification of anti-PSA were determined as 1.35 nM and 4.08 nM for compact rod-shaped spherical ZnO nanostructures, and 2.36 nM and 7.15 nM for rod-shaped ZnO nanostructures, respectively.
Assuntos
Técnicas Biossensoriais , Óxido de Zinco , Humanos , Masculino , Anticorpos Monoclonais , Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas , Eletrodos , Ouro/química , Imunoensaio/métodos , Limite de Detecção , Antígeno Prostático Específico/química , Óxido de Zinco/química , Nanopartículas MetálicasRESUMO
The solid-state 1H, 31P NMR spectra and cross-polarization (CP MAS) kinetics in the series of samples containing amorphous phosphate phase (AMP), composite of AMP + nano-structured calcium hydroxyapatite (nano-CaHA) and high-crystalline nano-CaHA were studied under moderate spinning rates (5-30 kHz). The combined analysis of the solid-state 1H and 31P NMR spectra provides the possibility to determine the hydration numbers of the components and the phase composition index. A broad set of spin dynamics models (isotropic/anisotropic, relaxing/non-relaxing, secular/semi-non-secular) was applied and fitted to the experimental CP MAS data. The anisotropic model with the angular averaging of dipolar coupling was applied for AMP and nano-CaHA for the first time. It was deduced that the spin diffusion in AMP is close to isotropic, whereas it is highly anisotropic in nano-CaHA being close to the Ising-type. This can be caused by the different number of internuclear interactions that must be explicitly considered in the spin system for AMP (I-S spin pair) and nano-CaHA (IN-S spin system with N ≥ 2). The P-H distance in nano-CaHA was found to be significantly shorter than its crystallographic value. An underestimation can be caused by several factors, among those - proton conductivity via a large-amplitude motion of protons (O-H tumbling and the short-range diffusion) that occurs along OH- chains. The P-H distance deduced for AMP, i.e. the compound with HPO42- as the dominant structure, is fairly well matched to the crystallographic data. This means that the CP MAS kinetics is a capable technique to obtain complementary information on the proton localization in H-bonds and the proton transfer in the cases where traditional structure determination methods fail.
Assuntos
Durapatita , Prótons , Monofosfato de Adenosina , Cristalografia , Espectroscopia de Ressonância Magnética/métodosRESUMO
Polypropylene (PP), a promising engineering thermoplastic, possesses the advantages of light weight, chemical resistance, and flexible processability, yet preserving insulative properties. For the rising demand for cost-effective electronic devices and system hardware protections, these applications require the proper conductive properties of PP, which can be easily modified. This study investigates the thermal and electrical properties of isotactic polypropylene/copper nanowires (i-PP/CuNWs). The CuNWs were harvested by chemical reduction of CuCl2 using a reducing agent of glucose, capping agent of hexadecylamine (HDA), and surfactant of PEG-7 glyceryl cocoate. Their morphology, light absorbance, and solution homogeneity were investigated by SEM, UV-visible spectrophotometry, and optical microscopy. The averaged diameters and the length of the CuNWs were 66.4 ± 16.1 nm and 32.4 ± 11.8 µm, respectively. The estimated aspect ratio (L/D, length-to-diameter) was 488 ± 215 which can be recognized as 1-D nanomaterials. Conductive i-PP/CuNWs composites were prepared by solution blending using p-xylene, then melt blending. The thermal analysis and morphology of CuNWs were characterized by DSC, polarized optical microscopy (POM), and SEM, respectively. The melting temperature decreased, but the crystallization temperature increasing of i-PP/CuNWs composites were observed when increasing the content of CuNWs by the melt blending process. The WAXD data reveal the coexistence of Cu2O and Cu in melt-blended i-PP/CuNWs composites. The fit of the electrical volume resistivity (ρ) with the modified power law equation: ρ = ρo (V - Vc)-t based on the percolation theory was used to find the percolation concentration. A low percolation threshold value of 0.237 vol% and high critical exponent t of 2.96 for i-PP/CuNWs composites were obtained. The volume resistivity for i-PP/CuNWs composite was 1.57 × 107 Ω-cm at 1 vol% of CuNWs as a potential candidate for future conductive materials.
RESUMO
In this study, an aqueous sol-gel synthesis method and subsequent dip-coating technique were applied for the preparation of yttrium iron garnet (YIG), yttrium iron perovskite (YIP), and terbium iron perovskite (TIP) bulk and thin films. The monophasic highly crystalline different iron ferrite powders have been synthesized using this simple aqueous sol-gel process displaying the suitability of the method. In the next step, the same sol-gel solution was used for the fabrication of coatings on monocrystalline silicon (100) using a dip-coating procedure. This resulted, likely due to substrate surface influence, in all coatings having mixed phases of both garnet and perovskite. Thermogravimetric (TG) analysis of the precursor gels was carried out. All the samples were investigated by X-ray powder diffraction (XRD) analysis. The coatings were also investigated by scanning electron microscopy (SEM), atomic force microscopy (AFM) and Mössbauer spectroscopy. Magnetic measurements were also carried out.
RESUMO
Interest in magnetic nanoparticles is primarily due to their practical use. In this work, for the production of nanocrystalline powders of pure and gadolinium doped iron oxides, the extraction-pyrolytic method (EPM) was used. As a precursor, either iron-containing extract (iron (III) caproate in caproic acid) or its mixture with gadolinium-containing extract (gadolinium (III) valerate in valeric acid) was used. The mixed precursor contained 0.5 mol %, 2.5 mol %, 12.5 mol %, 50 mol %, and 75 mol % gadolinium in relation to the iron content. The formation of iron oxide phases, depending on the preparation conditions, was investigated. According to the results obtained, it was demonstrated that the presence of more than 2.5 mol % gadolinium additive in the mixed precursor inhibits the magnetite-to-hematite transformation process during thermal treatment. Produced samples were characterized by XRD and SEM methods, and the magnetic properties were studied.