993 resultados para Microstructure Characterization


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Effect of MnO addition on microstructure and ionic transport properties of nanocrystalline cubic(c)-ZrO2 is reported. Monoclinic (m) ZrO2 powders with 10-30 mol% MnO powder are mechanically alloyed in a planetary ball mill at room temperature for 10 h and annealed at 550 degrees C for 6 h. In all compositions m-ZrO2 transforms completely to nanocrystalline c-ZrO2 phase and MnO is fully incorporated into c-ZrO2 lattice. Rietveld's refinement technique is employed for detailed microstructure analysis by analyzing XRD patterns. High resolution transmission electron microscopy (HRTEM) analysis confirms the complete formation of c-ZrO2 phase. Presence of stoichiometric Mn in c-ZrO2 powder is confirmed by Electron Probe Microscopy analysis. XPS analysis reveals that Mn is mostly in Mn2+ oxidation state. A correlation between lattice parameter and oxygen vacancy is established. A detailed ionic conductivity measurement in the 250 degrees-575 degrees C temperature range describes the effect of MnO on conductivity of c-ZrO2. The ionic conductivity (s) of 30 mol% MnO alloyed ZrO2 at 550 degrees C is 0.04 s cm(-1). Electrical relaxation studies are carried out by impedance and modulus spectroscopy. Relaxation frequency is found to increase with temperature and MnO mol fraction. Electrical characterization predicts that these compounds have potentials for use as solid oxide fuel cell electrolyte material. (C) 2015 Elsevier Ltd. All rights reserved.

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Damage not only degrades the mechanical properties of explosives, but also influences the shock sensitivity, combustion and even detonation behavior of explosives. The study of impact damage is crucial in the vulnerability evaluation of explosives. A long-pulse low-velocity gas gun with a gas buffer was developed and used to induce impact damage in a hot pressed plastic bonded explosive. Various methods were used to detect and characterize the impact damage of the explosive. The microstructure was examined by use of polarized light microscopy. Fractal analysis of the micrographs was conducted by use of box counting method. The correlation between the fractal dimensions and microstructures was analyzed. Ultrasonic testing was conducted using a pulse through-transmission method to obtain the ultrasonic velocity and ultrasonic attenuation. Spectra analyses were carried out for recorded ultrasonic signals using fast Fourier transform. The correlations between the impact damage and ultrasonic parameters including ultrasonic velocities and attenuation coefficients were also analyzed. To quantitatively assess the impact induced explosive crystal fractures, particle size distribution analyses of explosive crystals were conducted by using a thorough etching technique, in which the explosives samples were soaked in a solution for enough time that the binder was totally removed. Impact induces a large extent of explosive crystal fractures and a large number of microcracks. The ultrasonic velocity decreases and attenuation coefficients increase with the presence of impact damage. Both ultrasonic parameters and fractal dimension can be used to quantitatively assess the impact damage of plastic bonded explosives.

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A laser-discrete quenched steel (LDQS) substrate/as-deposited chromium (top high-contraction (HC) and underlying low-contraction (LC) chromium) system was investigated by dissolving coatings in order to reveal the mechanism that the service life of the coated parts is largely improved using the hybrid technique of laser pre-quenching plus chromium post-depositing. It was found that the surface characteristics of the substrate, LC and HC chromium layer can be simultaneously revealed owing to the dissolution edge effect of chromium coatings. Moreover, the periodical gradient morphologies of the LDQS substrate are clearly shown: the surfaces of laser transformation-hardened regions are rather smooth; a lot of fine micro-holes exist in the transition zones; there are many micro-dimples in the original substrate. Furthermore, the novel method of dissolving coatings with sharp interfaces may be used to reveal the structural features of a substrate/coating system, explore the effect of the substrate on the initial microstructure and morphologies of coatings, and check the quality of the coated-parts.

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Viscoelastic deformation and creep behavior of La- and Ce-based bulk metallic glasses (BMGs) with low glass transition temperature are investigated through nanoindentation at room temperature. Creep compliance and retardation spectra are derived to study the creep mechanism. The time-dependent displacement can be well described by a generalized Kelvin model. A modification is proposed to determine the elastic modulus from the generalized Kelvin model. The results are in excellent agreement with the elastic modulus determined by uniaxial compression tests. (c) 2007 Published by Elsevier B.V.

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Zr48.5Cu46.5Al5 bulk metallic glass (BMG) composites with diameters of 3 and,4 mm were prepared through suction casting in an arc melting furnace by modulating the alloy composition around the monothetic BMG composition of the high glass forming ability. Microstructural characterization reveals that the composites contain micron-sized CuZr phase with martensite structure, as well as nano-sized Zr2Cu crystalline particles and Cu10Zr7 plate-like phase embedded in an amorphous matrix. Room temperature compression tests showed that the composites exhibited significant strain hardening and obvious plastic strain of 7.7% for 3 nun and 6.4% for 4 nun diameter samples, respectively.

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A process of laser cladding Ni-CF-C-CaF2 mixed powders to form a multifunctional composite coatingd on gamma-TiAl substrate was carried out. The microstructure of the coating was examined using XRD, SEM and EDS. The coating has a unique microstructure consisting of primary dendrite or short-stick TiC and block Al4C3 carbides reinforcement as well as fine isolated spherical CaF2 solid lubrication particles uniformly dispersed in the NiCrAlTi (gamma) matrix. The average microhardness of the composite coatings is approximately HV 650 and it is 2-factor greater than that of the TiAl substrate. (C) 2008 Elsevier B.V. All rights reserved.

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Acceptor-doped ceria has been recognized as a promising intermediate temperature solid oxide fuel cell electrode/electrolyte material. For practical implementation of ceria as a fuel cell electrolyte and for designing model experiments for electrochemical activity, it is necessary to fabricate thin films of ceria. Here, metal-organic chemical vapor deposition was carried out in a homemade reactor to grow ceria films for further electrical, electrochemical, and optical characterization. Doped/undoped ceria films are grown on single crystalline oxide wafers with/without Pt line pattern or Pt solid layer. Deposition conditions were varied to see the effect on the resultant film property. Recently, proton conduction in nanograined polycrystalline pellets of ceria drew much interest. Thickness-mode (through-plane, z-direction) electrical measurements were made to confirm the existence of proton conductivity and investigate the nature of the conduction pathway: exposed grain surfaces and parallel grain boundaries. Columnar structure presumably favors proton conduction, and we have found measurable proton conductivity enhancement. Electrochemical property of gas-columnar ceria interface on the hydrogen electrooxidation is studied by AC impedance spectroscopy. Isothermal gas composition dependence of the electrode resistance was studied to elucidate Sm doping level effect and microstructure effect. Significantly, preferred orientation is shown to affect the gas dependence and performance of the fuel cell anode. A hypothesis is proposed to explain the origin of this behavior. Lastly, an optical transmittance based methodology was developed to obtain reference refractive index and microstructural parameters (thickness, roughness, porosity) of ceria films via subsequent fitting procedure.

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Current technological advances in fabrication methods have provided pathways to creating architected structural meta-materials similar to those found in natural organisms that are structurally robust and lightweight, such as diatoms. Structural meta-materials are materials with mechanical properties that are determined by material properties at various length scales, which range from the material microstructure (nm) to the macro-scale architecture (μm – mm). It is now possible to exploit material size effect, which emerge at the nanometer length scale, as well as structural effects to tune the material properties and failure mechanisms of small-scale cellular solids, such as nanolattices. This work demonstrates the fabrication and mechanical properties of 3-dimensional hollow nanolattices in both tension and compression. Hollow gold nanolattices loaded in uniaxial compression demonstrate that strength and stiffness vary as a function of geometry and tube wall thickness. Structural effects were explored by increasing the unit cell angle from 30° to 60° while keeping all other parameters constant; material size effects were probed by varying the tube wall thickness, t, from 200nm to 635nm, at a constant relative density and grain size. In-situ uniaxial compression experiments reveal an order-of-magnitude increase in yield stress and modulus in nanolattices with greater lattice angles, and a 150% increase in the yield strength without a concomitant change in modulus in thicker-walled nanolattices for fixed lattice angles. These results imply that independent control of structural and material size effects enables tunability of mechanical properties of 3-dimensional architected meta-materials and highlight the importance of material, geometric, and microstructural effects in small-scale mechanics. This work also explores the flaw tolerance of 3D hollow-tube alumina kagome nanolattices with and without pre-fabricated notches, both in experiment and simulation. Experiments demonstrate that the hollow kagome nanolattices in uniaxial tension always fail at the same load when the ratio of notch length (a) to sample width (w) is no greater than 1/3, with no correlation between failure occurring at or away from the notch. For notches with (a/w) > 1/3, the samples fail at lower peak loads and this is attributed to the increased compliance as fewer unit cells span the un-notched region. Finite element simulations of the kagome tension samples show that the failure is governed by tensile loading for (a/w) < 1/3 but as (a/w) increases, bending begins to play a significant role in the failure. This work explores the flaw sensitivity of hollow alumina kagome nanolattices in tension, using experiments and simulations, and demonstrates that the discrete-continuum duality of architected structural meta-materials gives rise to their flaw insensitivity even when made entirely of intrinsically brittle materials.

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Hybrid ZnO/ormosils Elms are prepared by the sol-gel method. A FT-IR spectrometer, 900 UV/VIS/NIR spectrophotometer, atomic force microscope, and ellipsometer are employed to investigate microstructure and optical properties of the films fired at different temperatures. The results show that the films with high transmittance and low surface roughness could be obtained at the heat-treatment temperature of 150 degrees C, the refractive index and thickness of the film are 1.413, 2.11 mu m, respectively. Higher temperatures (350 degrees C, 550 degrees C) change the Elm microstructure severely, and then decrease the transmittance of the films.

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Four kinds of Y2O3 stabilized ZrO2 (YSZ) thin films with different Y2O3 content have been prepared on BK7 substrates by electron-beam evaporation method. Structural properties and surface morphology of thin films were investigated by X-ray diffraction (XRD) spectra and scanning probe microscope. Laser induced damage threshold (LIDT) was determined. It was found that crystalline phase and microstructure of YSZ thin films was dependent on Y2O3 molar content. YSZ thin films changed from monoclinic phase to high temperature phase (tetragonal and cubic) with the increase of Y2O3 content. The LIDT of stabilized thin film is more than that of unstabilized thin films. The reason is that ZrO2 material undergoes phase transition during the course of e-beam evaporation resulting in more numbers of defects compared to that of YSZ thin films. These defects act as absorptive center and the original breakdown points. (c) 2006 Elsevier B.V. All rights reserved.

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Thin films of nano-composite Y-Ba-Cu-O (YBCO) superconductors containing nano-sized, non-superconducting particles of Y2Ba 4CuMOx (M-2411 with M = Ag and Nb) have been prepared by the PLD technique. Electron backscatter diffraction (EBSD) has been used to analyze the crystallographic orientation of nano-particles embedded in the film microstructure. The superconducting YBa2Cu3O7 (Y-123) phase matrix is textured with a dominant (001) orientation for all samples, whereas the M-2411 phase exhibits a random orientation. Angular critical current measurements at various temperature (T) and applied magnetic field (B) have been performed on thin films containing different concentration of the M-2411 second phase. An increase in critical current density J c at T < 77 K and B < 6 T is observed for samples with low concentration of the second phase (2 mol % M-2411). Films containing 5 mol % Ag-2411 exhibit lower Jc than pure Y-123 thin films at all fields and temperatures. Samples with 5 mol % Nb-2411 show higher Jc(B) than phase pure Y-123 thin films for T < 77 K. © 2010 IOP Publishing Ltd.

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Upon heating, hydrated magnesium carbonates (HMCs) undergo a continuous sequence of decomposition reactions. This study aims to investigate the thermal decomposition of various commercially produced HMCs classified as light and heavy, highlight their differences, and provide an insight into their compositions in accordance with the results obtained from thermal analysis and microstructure studies. An understanding of the chemical compositions and microstructures, and a better knowledge of the reactions that take place during the decomposition of HMCs were achieved through the use of SEM, XRD, and TG/differential thermal analysis (DTA). The quantification of their CO 2 contents was provided by TG and dissolving the samples in HCl acid. Results show that variations exist within the microstructure and decomposition patterns of the two groups of HMCs, which do not exactly fit into the fixed stoichiometry of the known HMCs in the MgO-CO2-H2O system. The occurrence of an exothermic DTA peak was only observed for the heavy HMCs, which was attributed to their high CO2 contents and the relatively delayed decomposition pattern. © 2013 Akadémiai Kiadó, Budapest, Hungary.

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Polymorphous silicon (pm-Si:H) films have been prepared by a new regime of plasma enhanced chemical vapour deposition in the region adjacent of phase transition from amorphous to microcrystalline state. Comparing to the conventional amorphous silicon (a-Si:H), the pm-Si:H has higher photoconductivity (sigma(ph)), better stability, and a broader light spectral response range in the longer wavelength range. It can be found from Raman spectra that there is a notable improvement in the medium range order. There are a blue shift for the stretching mode of IR spectra and a red shift for the wagging mode. The shifts are attributed to the variation of the microstructure. By using pm-Si:H film as intrinsic layer, a p-i-n junction solar cell was prepared with the initial efficiency of 8.51% and a stabilized efficiency of 8.01% (AM1.5, 100mw/cm(2)) at room temperature (T-R).

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High-quality nc-Si/a-Si:H diphasic films with improved stability were prepared by using the plasma-enhanced chemical vapor deposition technology. In comparison with typical amorphous silicon, the diphasic silicon films possess higher photoconductivity (two orders larger than that of the amorphous silicon film) and fairly good photosensitivity(the ratio of the photo-to dark-conductivity is about 10) and higher stability (the degradation of the photoconductivity is less than 10% after 24h long light soaking with 50 mW/cm(2) intensity at room temperature). In addition, the diphasic silicon film has a better light spectra response in the longer wavelength range. The improvement in photoelectronic properties may be attributed to: the existence of the disorder within the amorphous matrix, which breaks the momentum selection rule in the optical transition and, consequently, results in the large light absorption coefficient and high photosensitivity; the improved medium range order and low gap states density. Excess carriers generated in the amorphous matrix tend to recombine in the embedded crystallites, which suppresses nonradiative recombination within the amorphous matrix and reduces the subsequent defect creation.

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A kind of hydrogenated diphasic, silicon films has been prepared by a new regime of plasma enhanced chemical vapor deposition (PECVD) in the region adjacent to the phase transition from amorphous to crystalline state. The photoelectronic and microstructural properties of the films have been investigated by the constant photocurrent method (CPM), Raman scattering and nuclear magnetic resonance (NMR). Our experimental results and corresponding analyses showed that the diphasic films, incorporated with a subtle boron compensation, could gain both the fine photosensitivity and high stability, provided the crystalline fraction (f) was controlled in the range of 0 < f < 0.3. When compared with the conventional hydrogenated amorphous silicon (a-Si:H), the diphasic films are more ordered and robust in the microstructure, and have a less clustered phase in the Si-H bond configurations. (C) 2002 Elsevier Science Ltd. All rights reserved.