Rock porosity quantification by dual-energy X-ray computed microtomography

Porous media investigation by X-ray microtomography allows obtaining valuable quantitative and qualitative information, while preserving sample integrity. Modern X-ray nanotomography or Synchrotron radiation systems may distinguish structures sized only hundreds of nanometers. However, pores sized less than a few microns (microporosity) may be undetectable due to the system’s spatial resolution and noise in microfocus sources, compromising the quality of the measurement. In this study a dual-energy methodology was developed to generate density-based images from two scans made at two different voltages (80 kV and 130 KV) with a microfocus bench-top microtomography system. The images obtained were quantized in 256 gray levels, where the lowest value (zero) corresponded to voids and the highest value (255) corresponded to the densest regions mapped. From density images and single energy images, porosity was evaluated and compared. Results indicate that density images present better results than single energy images when both are compared with porosity obtained by the helium injection method. In addition, images acquired in dual-energy show good agreement with the sample’s real density values.     

Effective atomic number and density determination of rocks by X-ray microtomography

Microtomography, as a non-destructive technique, has become an important tool in studies of internal properties of materials. Recently, interest using this methodology in characterizing the samples with respect to their compositions, especially rocks, has grown. Two physical properties, density and effective atomic number, are important in determining the composition of rocks. In this work, six samples of materials with densities that varied from 2.42 to 6.84 g/cm³ and effective atomic numbers from 15.0 to 77.3 were studied. The measurements were made using a SkyScan-Bruker 1172 microtomography apparatus operating in voltages at 50, 60, 70, 80, 90 and 100 kV with a resolution of 13.1 μm. Through micro-CT images, an average gray scale was calculated for the samples and correlation studies of this value with the density and the effective atomic number of samples were made. Linear fits were obtained for each energy value. The obtained functions were tested with samples of Amazonite, Gabbro, Sandstone and Sodalite.     

Quantification of fluids injection in a glass-bead matrix using X-ray microtomography

Several daily activities involve the accumulation or percolation of fluids through porous media. X-ray microtomography is a non-invasive technique capable of providing images of the internal microstructure of materials showing the different phases of fluid distribution present in the sample directly or at the pore-scale. This methodology was used to qualitatively and quantitatively assess samples consisting with glass beads of standard size, which contained fluid filling a porous region. Three samples were prepared with 0.6 mm or 0.8 mm diameter glass beads inserted into a glass tube with an inner diameter of 6.7 mm and 1.0 mm wall thickness. The fluids injected were dopant salt–water solution, industrial oil and commercial oil. The samples were scanned using a Skyscan-1172 microtomographic system. All phases present in the sample were differentiated. The values of injected fluids were determined through 2D and 3D analyses. Two types of solutions were used, one doped with KI, and the other with BaCl₂·2H₂O. The percentage of KI used allowed the individualization of the solution and, therefore, the direct quantification of this phase through 2D and 3D images.     

Annealing temperature dependent on structural,optical and electrical properties of indium oxide thin films deposited by electron beam evaporation method

In the present work the influence of annealing temperature on the structural and optical properties of the In₂O₃ films deposited by electron beam evaporation technique in the presence of oxygen was studied. The deposited films were annealed from 350 to 550 °C in air. The chemical compositions of In₂O₃ films were carried out by X-ray photoelectron spectroscopy (XPS). The film structure and surface morphologies were investigated as a function of annealing temperature by X-ray diffraction (XRD) and atomic force microscopy (AFM). The structural studies by XRD reveal that films exhibit preferential orientation along (2 2 2) plane. The refractive index (n), packing density and porosity (%) of films were arrived from transmittance spectral data obtained in the range 250–1000 nm by UV–vis-spectrometer. The optical band gap of In₂O₃ film was observed and found to be varying from 3.67 to 3.85 eV with the annealing temperature.     

Focused electron beam induced deposition as a tool to create electron vortices

Focused electron beam induced deposition (FEBID) is a microscopic technique that allows geometrically controlled material deposition with very high spatial resolution. This technique was used to create a spiral aperture capable of generating electron vortex beams in a transmission electron microscope (TEM). The vortex was then fully characterized using different TEM techniques, estimating the average orbital angular momentum to be ∼0.8ℏ per electron with almost 60% of the beam ending up in the ℓ = 1 state.     

Characterization of NiO–yttria stabilised zirconia (YSZ) hollow fibres for use as SOFC anodes

NiO–yttria stabilised zirconia (YSZ) hollow fibres with varying NiO content and a desired microstructure were prepared using a phase inversion technique and sintering. By controlling the fabrication parameters, microstructures with predominately finger-like pores near the inner and outer surfaces and a denser central layer with sponge-like pores were produced, for use as substrates for anode-supported hollow fibre solid oxide fuel cells (HF-SOFC). The NiO–YSZ fibres were reduced to Ni–YSZ at 250–700 °C in hydrogen flowing at 20 cm³ min^? 1 to produce Ni–YSZ hollow fibres, the mechanical and electrical properties of which were determined subsequently, reduction to Ni being verified by X-ray diffraction. The effects of NiO concentration and sintering temperature of the fibre precursors on the conductivity, strength and porosity of the reduced hollow fibres were investigated to assess their suitability for use as anode substrates. As expected, increasing Ni concentration increased electrical conductivities and decreased mechanical strength. Sintering temperature had a critical effect in producing axially conductive hollow fibres of sufficient mechanical strength for use as SOFC anodes. The hollow fibres retained their initial microstructure through the reduction process, though ca. 41% volume contraction is predicted on reduction of NiO to Ni, producing increased porosity in the reduced fibres. The mean porosity of the Ni–YSZ hollow fibres was ca. 60% and ca. 40% after sintered at 1250 °C and 1400 °C, respectively. The mean pore sizes for all the fibres after reduction varied between ca. 0.3 and 1 µm. The hollow fibres produced with 60% NiO, of length ca. 300 mm, electrical conductivities of ca. (1–2.25) × 10⁵ S m^? 1 and a porosity of ca. 43% are being used currently to construct and test the electrical behaviour of an anode-supported HF-SOFC.     

Mechanical properties of polycrystalline RuSr2GdCu2O8 superconductor

The main objective of this paper is to report the room temperature hardness and elastic modulus of the RuSr₂GdCu₂O₈ superconductor phase by instrumented indentation. Polycrystalline samples were produced by a solid state reaction technique. The samples were also characterized by scanning electron microscopy, X-ray diffraction and electrical resistivity measurements. The influence of porosity on the mechanical properties was avoided by considering only those indentations inside the grains. The hardness and elastic modulus were 8.6 GPa and 145 GPa, respectively. These values are comparable with those of Y-123. The indentation fracture toughness evaluated after conventional Vickers indentation was 1.9 MPa m^1/2.     

Structure and electrochemical performance of Y(III) and Al(III) codoped amorphous nickel hydroxide

Amorphous nickel hydroxide codoped with rare earths Y(III) and Al(III) has been synthesized by the chemical precipitation method combined with the rapid freezing technique. The microstructure and morphology of the prepared sample were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectra. The electrochemical performance of the sample was characterized by the charge/discharge test and cyclic voltammetry. The results show that this amorphous nickel hydroxide codoped with Y(III) and Al(III) has many structural defects and therefore results in a relatively high specific capacity (351.83 mA h g^?1 at a charge/discharge rate of 0.2 C) and good electrochemical reversibility.     

Linear and nonlinear optical properties of N-(3-nitrophenyl) acetamide single crystals

Optically transparent nonlinear optical bulk single crystal of N-(3-nitrophenyl) acetamide (3NAA) of dimension 7 mm × 6 mm × 5 mm has been grown from its aqueous solution by slow solvent evaporation technique. The grown crystal was characterized by powder X-ray diffraction to confirm the crystal structure. Investigation has been carried out to assign the vibrational frequencies of the grown crystals by Fourier Transform Infrared Spectroscopy and FT-NMR technique. Thermal behaviour of the grown crystals was studied by thermogravimetric analysis. The second harmonic generation efficiency of 3NAA was determined by Kurtz and Perry powder technique. The optical absorption study confirms the suitability of the crystal for device applications. The mechanical properties of the grown crystals have been studied using Vickers microhardness tester. Dielectric, microhardness and photoconductivity studies also carried out for the grown sample.     

Characterisations of CoCu films electrodeposited at different cathode potentials

Structural and magnetic properties of CoCu films electrodeposited on polycrystalline Cu substrates were investigated as a function of cathode potential used for their deposition. The compositional analysis, performed by energy dispersive X-ray spectroscopy, demonstrated that an increase in the deposition potential results in an increase in Co content of CoCu films. The crystal structure of the films was studied using the X-ray diffraction (XRD) technique. It was observed that they have a face centred cubic (fcc) structure, but also contain partly hexagonal close-packed phase. XRD results revealed that the (1 1 1) peak of fcc structure splits into two as Co (1 1 1) and Cu (1 1 1) peaks and the peak intensities change depending on the deposition potential and hence the film composition. The magnetic measurements were carried out at room temperature using a vibrating sample magnetometer. The magnetic findings indicated that coercivity decreases and saturation magnetisation increases with the increase of Co:Cu ratio caused by the deposition potential and also all films have planar magnetisation.     

Magnetic properties and structures of Fe/MgF2 multilayered films

Multilayers composed of Fe and MgF₂ with layer thicknesses between 9 Å and 100 Å and of 30 Å, respectively, were prepared with an ultrahigh-vacuum deposition technique. Medium-angle X-ray data show that the Fe layers in the BCC phase have considerable (1 1 0) texture. Periodicity due to multilayered structures was confirmed by a small-angle X-ray diffraction study and cross-section transmission electron microscope for films with Fe layer thicknesses >45 Å. In an Fe/MgF₂(9 Å/30 Å) sample, an island structure for the Fe layers was suggested by the existence of superparamagnetism in a film. At 4.2 K, enhancements of both magnetization and hyperfine field were observed in films having Fe layers thinner than 40 Å. The maxima in the magnetization (233 emu/g of Fe) and in the average hyperfine field (390 kOe) at 4.2 K were found in an Fe/MgF₂(9 Å/30 Å) film and were approximately 105% and 115% that of the bulk α-Fe, respectively. The thickness dependence suggests a 12% enhancement in the magnetic moment of interface Fe atoms. No exchange bias was found in the films, implying that antiferromagnetic fluorides are not formed at the interface, which is different from the case of Fe/LiF and Fe/CaF₂ multilayers.     

Infrared absorption and Raman spectroscopy studies of InSbBi layers grown by liquid phase epitaxy

We report on the results of optical absorption and Raman spectroscopy measurements on InSbBi layers grown by liquid phase technique. A maximum Bi content of 0.4 at.%, as measured by energy dispersive X-ray (EDX) technique, is used in the experiments. Optical absorption measurements made on the samples indicate a room temperature energy band gap reduction up to about 6 meV with respect to undoped InSb layers grown by the same technique. Bi content calculated from this band gap reduction agrees with that obtained from EDX. A weak peak obtained at 152 cm^?1 in the Raman spectrum of the material is identified with the longitudinal optical phonon mode of InBi. Further a mode at 140 cm^?1 is observed due to isolated Bi atoms at the interstitial sites.     

Effect of Fe doping on the room temperature ferromagnetism in chemically synthesized (In1−xFex)2O3 (0 ⩽ x ⩽ 0.07) magnetic semiconductors

Observation of room temperature ferromagnetism in Fe doped In₂O₃ samples (In_1−xFe_x)₂O₃ (0 ⩽ x ⩽ 0.07) prepared by co-precipitation technique is reported. Lattice parameter obtained from powder X software shows distinct shrinkage of the lattice constant indicating an actual incorporation of Fe ions into the In₂O₃ lattice. X-ray diffraction data measurements show that the entire sample exhibits single phase polycrystalline behavior. SEM micrographs showed the prepared powder was in the range 25–36 nm. SEM EDS mapping showed the presence of Fe and In ions in the Fe doped In₂O₃ sample. The highest remanence magnetization moment (6.624 × 10⁻⁴ emu/g) is reached in the sample with x = 0.03.     

Luminescence and Scintillation Characterization of Cs2NaGdBr6: Ce3+ Single Crystal

Luminescence and scintillation properties of newly discovered bromo-elpasolites Cs₂NaGdBr₆: Ce³⁺ (CNGB: Ce³⁺) are presented. Single crystals of CNGB: Ce³⁺ with dimensions up to Ø7×10 mm³ are successfully grown by the Bridgman technique. X-ray excited luminescence measurements of the grown samples showed a broad emission band in the wavelength range from 365 to 470 nm. It offered an energy resolution of 5.1% (FWHM) at 662 keV for 10% Ce sample. The light output of the investigated samples increases along with cerium concentration. A maximum light yield of ～36,800 ph/MeV is measured for the 10% Ce sample crystal. Under γ-ray excitation, CNGB: Ce³⁺ crystals showed three exponential decay time components. The scintillation mechanism in the sample crystal is presented.     

Luminescence behaviour of beryl (aquamarine variety) from Turkey

Natural blue-green beryl from Turkey has been investigated using scanning electron microscopy-energy-dispersive spectroscopy (SEM-EDS), X-ray diffraction (XRD) and Cathodoluminescence (CL). Beryl has the chemical formula Be₃Al₂Si₆O₁₈ and is hexagonal with space group P6/mcc. Chemical analyses of the beryl sample utilised inductively coupled plasma-atomic emission spectroscopy (ICP-AES) for major oxides and trace elements. It shows that the beryl sample is rich in Cs (531 ppm) and contains low concentrations of transition-metal ions, in total 2.29 wt.% Fe, 269 ppm Mn, V<5 ppm and Cr 20 ppm. Ideas on the origin of the green colour of this mineral are presented. The CL spectrum of the bulk sample display intense broad band emission from ～360 to ～800 nm.     

Flame spread along a thin solid randomly distributed combustible and noncombustible areas

Flame spread route in fire strongly depends on distribution of combustible materials. Two types of scenario are considered in flame spread when combustible materials randomly distributed; one case is that flame spreads and combustible materials burn out, and the other case is that flame self-extinguishes on the way. The threshold of burning out or self-extinguishing may be determined by quantity of combustible materials and their placement in space. Our objectives are to clarify the characteristics and threshold of flame spread. In this paper, we examine non-uniform flame spread in open air along a thin combustible solid with randomly distributed pores, which are considered as noncombustible space. Experimental results show that the flame spread rate for S ≦ 1 (S ≡ d/L_h, S: scale ratio, d: pore-scale, L_h: pre-heat length ahead of flame leading edge measured by using a shadowgraph method) increases with increasing the porosity and reaches maximum value approximately at 20–30% of porosity, while the flame spread rate for S > 1 is almost constant. Over 40% of porosity, the flame spread rate for both S ≦ 1 and S > 1 decreases. The flame cannot spread and completely self-extinguish over 60% of porosity independently with pore-scale and shape. The threshold of flame spread is related with the average-number of slit, N_s, which is made by connecting each pores. The N_s as the threshold of flame spread is unity for S > 1, while the modified average-number of slit (N_s × S) becomes two for S ≦ 1.     

Large-scale synthesis and growth habit of 3-D flower-like crystal of PbTe

In this paper, 3-D flower-like crystal of PbTe was successfully synthesized using Pb(CH₃COO)₂·3H₂O and Na₂TeO₃ as precursors under hydrothermal conditions, and characterized by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction pattern (XRD). The reaction parameters that influenced the evolution of PbTe synthesis and morphology were investigated. It was shown that the flower-like crystal of PbTe was composed of a nucleus with eight pods. A possible growth mechanism was proposed based on the calculation of the surface energies of PbTe and the SEM observation. Furthermore, the temperature-dependent transport properties of 3-D flower-like crystal of PbTe specimen have been evaluated with an average thermoelectric power of 120 S cm^?1 and electrical conductivity of 220 μV K^?1 at 740 K.     

Application of indium tin oxide (ITO) thin film as a low emissivity film on Ni-based alloy at high temperature

Indium tin oxide (ITO) films as the low emissivity coatings of Ni-based alloy at high temperature were studies. ITO films were deposited on the polished surface of alloy K424 by direct current magnetron sputtering. These ITO-coated samples were heat-treated in air at 600–900 °C for 150 h to explore the effect of high temperature environment on the emissivity. The samples were analyzed by X-ray diffraction (XRD), SEM and EDS. The results show that the surface of sample is integrity after heat processing at 700 °C and below it. A small amount of fine crack is observed on the surface of sample heated at 800 °C and Ti oxide appears. There are lots of fine cracks on the sample annealed at 900 °C and a large number of various oxides are detected. The average infrared emissivities at 3–5 μm and 8–14 μm wavebands were tested by an infrared emissivity measurement instrument. The results show the emissivity of the sample after annealed at 600 and 700 °C is still kept at a low value as the sample before annealed. The ITO film can be used as a low emissivity coating of super alloy K424 up to 700 °C.     

Fire safety distances for open pool fires

Fire accidents that carry huge loss with them have increased in the previous two decades than at any time in the history. Hence, there is a need for understanding the safety distances from different fires with different fuels. Fire safety distances are computed for different open pool fires. Diesel, gasoline and hexane are used as fuels for circular pool diameters of 0.5 m, 0.7 m and 1.0 m. A large square pool fire of 4 m × 4 m is also conducted with diesel as a fuel. All the prescribed distances in this study are purely based on the thermal analysis. IR camera is used to get the thermal images of pool fires and there by the irradiance at different locations is computed. The computed irradiance is presented with the threshold heat flux limits for human beings.     

Synthesis of oligomeric poly[(1, 2-propanediamine)-alt-(oxalic acid)] and anomalous proton conductivities of the thin films

New proton-conductive polyamide oligomers, oligomeric poly[(1, 2-propanediamine)-alt-(oxalic acid)], were synthesized to investigate the proton transport properties of bulk and thin films. The obtained oligomers were characterized by the X-ray diffraction, FT-IR spectra, ¹H NMR, Matrix Assisted Laser Desorption/Ionization Time of Flight (MALDI-TOF) mass spectrum, and electrical conductivity measurements. The bulk proton conductivity is 3.0 × 10^? 4 S cm^? 1 at the relative humidity (RH) of 80%. The proton conductivity of thin film is relatively higher than that of bulk sample. Thickness dependence of the proton conductivity was observed in these thin films. The maximum proton conductivity of the thin film is 4.0 × 10^? 3 S cm^? 1 at the relative humidity (RH) of 80%, which is higher one order magnitude than that of the bulk sample. The activation energies of bulk and 200 nm thick film are 1.0 and 0.69 eV at the RH of 60%, respectively.