Anatomical descriptions of silicified woods from Madagascar and Indonesia by scanning electron microscopy

Fine structure and tissue substitution by minerals were investigated in silicified woods from Madagascar and Indonesia by scanning electron microscopy and X-ray microanalysis. The silicified woods maintained the exterior morphology of once grown trees and showed typical inner structures of conifers. Radial planes of the silicified wood from Madagascar revealed tracheids as a major component of the axial system in the secondary xylem. Tracheids were mainly characterized by numerous bordered pits where a thickening in the middle (torus) was surrounded with the membrane (margo). The torus appeared to contrast with the fibrillar network of the margo. As a component of the axial system in the secondary phloem, sieve elements were found to have many sieve pores that were filled with seemingly crystalline materials. To correlate the colors of the silicified wood from Indonesia with elemental composition, energy-dispersive X-ray spectrometry was employed in this study. Silicon was present as a basic component of the silicified wood. Calcium and iron were detected from red-colored regions, whereas magnesium was found in blue-colored regions. These results suggest that tissues of silicified woods had been substituted by minerals over the past period, while retaining the inherent morphology of the tree species. Scanning electron microscopy and X-ray microanalysis could be applied to unravel structural details and composition of plant fossils in palaeobotany.     

Luminescence and micro-Raman investigations on inclusions of unusual habit in chrysoprase from Turkey

Chemical analyses performed on chrysoprase from Turkey have shown many trace elements as well as rare earth impurities. Quantitative chemical analyses of inclusions in minerals can improve our understanding of the chemistry of surface. The environmental scanning electron microscope (ESEM) with an attached X-ray energy dispersive system (EDS) is capable of producing rapid and accurate major element chemical analyses of individual inclusions in crystals larger than about 30 μm in diameter. The samples were examined with lifetime-resolved and spatially-resolved cathodoluminescence (CL), and inductively coupled plasma-atomic emission spectrometry (ICP-AES). Spatially resolved CL results at room temperature were recorded for two different areas. Bulk area displays with low CL emission and pores contain iron phases such as chromite, hematite and anatase which cause the green color. For the raw data in the lifetime resolved CL spectrum, at least three broad emission bands were detected in a yellow band of the highest intensity at about 550 nm, a weaker orange band at about 650 nm, and a red band at 720 nm. It is assumed that there are links between the CL emissions and the presence of some transition metal and REE elements, but it is obvious that all trace elements do not play a direct role. Micro-Raman measurements were performed on chrysoprase and these showed a characteristic intensive Raman band peaked at 464 cm^?1 which can be inferred to ν₂ doubly symmetric bending mode of [SiO₄/M] centers. Raman spectrum of all inclusions found in the material are also given and discussed in detail.     

Stabilization of high spin FCC Fe in (Fe/Pd)n multilayers

Polycrystalline (Fe/Pd)_n multilayers are grown onto sapphire substrates at room temperature in a UHV system. The number of periods n=40 and the thickness of Pd layers of t_Pd=4 nm are kept constant, whereas the thickness of the Fe layers is varied from 1.5 to 5 nm. Structural properties are studied by in situ reflection high energy diffraction (RHEED), scanning tunnelling microscopy (STM) and ex situ by X-ray diffraction at small angles and large angles. Analyzing the experimental data using the program SUPREX we obtain interplanar distances of d_Fe=2.03±0.01 Å for an Fe layer thickness larger than about 2.5 nm as expected for (1 1 0) planes of BCC Fe. For Fe layers with thicknesses less than about 2.5 nm the interplanar distance is d_Fe=2.1±0.01 Å, which is close to the distance between (1 1 1) planes of FCC Fe with a lattice parameter of a=3.64 Å. Magnetic susceptibility measurements at temperatures between 1.5 and 300 K for (Fe/Pd)_n multilayers with FCC Fe yield a magnetic moment per Fe atom of μ=2.7±0.1 μ_B, which is about 20% larger compared to μ=2.2 μ_B for BCC Fe. We show that the occurrence of the large magnetic moment originates from FCC Fe being in the high spin (HS) state rather than from polarization effects of Pd at Fe/Pd interfaces.     

Feasibility study of iron mineral separation from red mud by high gradient superconducting magnetic separation

The disposal of bayer red mud tailings now seriously threats the environment safety. Reduction and recycling of red mud is now an urgent work in aluminum industry. High gradient superconducting magnetic separation (HGSMS) system was applied to separate the extreme fine RM particles (<100 μm) into high iron content part and low iron content part. Two sorts of RM were fed in the HGSMS. The iron oxide contents in concentrates were about 65% and 45% when RM 1# and RM 2# were fed respectively. Meanwhile, the residues contained 52.0% or 14.1% iron oxide in residues after eight separation stages when RM 1# and RM 2# were fed respectively. The mass recovery of iron concentrates was about 10% after once separation process regardless of RM 1# or RM 2# was fed. Extreme fine particles (<10 μm) could be captured in the HGSMS. Intergrowth of Fe and other elements is disadvantages for iron mineral separation from RM by HGSMS. Some improvement should be studied to enhance the efficiency of iron separation. It is possible for HGSMS to separate RM into high iron content part and low iron content part, the former part could be used in iron-making furnace and the later part could be recycling to sintering process for alumina production or used as construction material.     

EHD flow in a wide electrode spacing spike–plate electrostatic precipitator under positive polarity

In this work, results of two- and three-dimensional particle image velocimetry (PIV) measurements of the flow velocity fields in a wide spacing spike–plate electrostatic precipitator (ESP) under positive polarity are presented. A DC voltage of positive polarity (up to 28 kV) was applied to the spike electrode. The average gas flow velocity was 0.6 m/s. The PIV measurements were carried out in four planes perpendicular to the plate electrodes. Three parallel planes passed along the ESP while one plane passed across the ESP duct. The results show that electrohydrodynamic (EHD) secondary flow with relatively strong vortices exist in the ESP. The EHD secondary flow pattern depends on applied voltage and measuring plane position in respect to the spike tip. The strongest vortices occur in the plane passing through the tip of the upstream-directed spike. These relatively strong EHD vortices may hinder collection of the particles in the diameter range of 0.1–1 μm in the wide electrode spacing spike–plate ESPs.     

A method for quantitative analysis of clump thickness in cervical cytology slides

Knowledge of the spatial distribution and thickness of cytology specimens is critical to the development of digital slide acquisition techniques that minimise both scan times and image file size. In this paper, we evaluate a novel method to achieve this goal utilising an exhaustive high-resolution scan, an over-complete wavelet transform across multi-focal planes and a clump segmentation of all cellular materials on the slide. The method is demonstrated with a quantitative analysis of ten normal, but difficult to scan Pap stained, Thin-prep, cervical cytology slides. We show that with this method the top and bottom of the specimen can be estimated to an accuracy of 1 μm in 88% and 97% of the fields of view respectively. Overall, cellular material can be over 30 μm thick and the distribution of cells is skewed towards the cover-slip (top of the slide). However, the median clump thickness is 10 μm and only 31% of clumps contain more than three nuclei. Therefore, by finding a focal map of the specimen the number of 1 μm spaced focal planes that are required to be scanned to acquire 95% of the in-focus material can be reduced from 25.4 to 21.4 on average. In addition, we show that by considering the thickness of the specimen, an improved focal map can be produced which further reduces the required number of 1 μm spaced focal planes to 18.6. This has the potential to reduce scan times and raw image data by over 25%.     

Preparation and characterization of iron/titanium-oxide composite particles

The iron/titanium-oxide composite particles have been prepared using “in-situ” hydrogen-thermal reduction method. The composites were characterized by X-ray diffraction, physical property measurement system and Mössbauer spectroscopy. The powder X-ray diffraction patterns reveal the presence of crystalline α-iron and titanium-oxide (FeTiO₃/TiO₂). The Mössbauer spectra of powders have been measured at room temperature, which indicated that the α-iron and the high-spin iron(II/III) components were observed. The complex permittivity and permeability of the composites have been measured using vector network analyzers. Reflection loss of the iron/titanium-oxide composite powders dispersing in epoxy resin has been calculated using measured values of complex permittivity and permeability in the frequency range of 2–12 GHz. The maximum reflection loss of ?36 dB was observed at 5.0 GHz. This study shows the possibility to obtain the novel dielectric and magnetic based microwave absorbers.     

Microwave-assisted synthesis of iron(III) oxyhydroxides/oxides characterized using transmission electron microscopy,X-ray diffraction,and X-ray absorption spectroscopy

Microwave-assisted synthesis of iron oxide/oxyhydroxide nanophases was conducted using iron(III) chloride titrated with sodium hydroxide at seven different temperatures from 100 to 250 °C with pulsed microwaves. From the X-ray diffraction (XRD) results, it was determined that there were two different phases synthesized during the reactions which were temperature dependent. At the lower temperatures, 100 and 125 °C, it was determined that an iron oxyhydroxide chloride was synthesized. Whereas, at higher temperatures, at 150 °C and above, iron(III) oxide was synthesized. From the XRD, we also determined the FWHM and the average size of the nanoparticles using the Scherrer equation. The average size of the nanoparticles synthesized using the experimental conditions were 17, 21, 12, 22, 26, 33, 28 nm, respectively, for the reactions from 100 to 250 °C. The particles also had low anisotropy indicating spherical nanoparticles, which was later confirmed using transmission electron microscopy (TEM). Finally, X-ray absorption spectroscopy (XAS) studies show that the iron present in the nanophase was present as iron(III) coordinated to six oxygen atoms in the first coordination shell. The higher coordination shells also conform very closely to the ideal or bulk crystal structures.     

Submicrometer tomographic resolution examined using a micro-fabricated test object

To estimate the spatial resolution of microtomographs, a test object on the submicrometer scale was prepared by focused ion beam milling and subjected to microtomographic analysis. Since human tissues are composed of cells and extracellular matrices with micrometer and submicrometer structures, it is important to investigate the three-dimensional spatial resolution of microtomographs used to visualize microstructures of human tissues. The resolutions along the direction within the tomographic slice plane (in-plane resolution) and perpendicular to it (through-plane resolution) were determined from the modulation transfer function of square-wave patterns. The in-plane resolution was estimated to be 1.2 μm from the modulation transfer function of the non-zoom image. In contrast, the zoom image gave the in-plane resolution of 0.8 μm. This in-plane resolution is comparable to the through-plane resolution, which was estimated to be 0.8 μm. Although the two-dimensional radiographs were taken with the pixel width of half the X-ray optics resolution, these three-dimensional resolution analyses indicated that the zoom reconstruction should be performed to achieve the in-plane resolution comparable to the X-ray optics resolution. The submicrometer three-dimensional analysis was applied in the structural study of human cerebral tissue stained with high-Z elements and the obtained tomograms revealed that the microtomographic analysis allows visualization of the subcellular structures of the cerebral tissue.     

Template-free sonochemical synthesis of hierarchically porous NiO microsphere

A novel template-free sonochemical synthesis technique was used to prepare NiO microspheres combined with calcination of NiO_2.45C_0.74N_0.25H_2.90 precursor at 500 °C. The NiO microspheres samples were systematically investigated by the thermograviometric/differential scanning calorimetry (TG/DSC), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), fourier-transformed infrared spectroscopy (FT-IR), Brunnauer–Emmett–Teller (BET) nitrogen adsorption–desorption isotherms, laser particle size analyzer, and ultraviolet–visible spectroscopy (UV–Vis). The morphology of the precursor was retained even after the calcination process, and exhibited hierarchically porous sphericity. The morphology changed over the ultrasonic radiation time, and the shortest reaction time was 70 min, which was much less than 4 h for the mechanical stirring process. The mechanical stirring was difficult to form the complete hierarchically porous microsphere structure. The BET specific surface area and the median diameter of the hierarchically porous NiO microspheres were 103.20 m²/g and 3.436 μm, respectively. The synthesized NiO microspheres were mesoporous materials with a high fraction of macropores. The pores were resulted from the intergranular accumulation. The ultraviolet absorption spectrum showed a broad emission at the center of 475 nm, and the band gap energy was estimated to be 3.63 eV.     

Inversion recovery ultrashort echo time magnetic resonance imaging: A method for simultaneous direct detection of myelin and high signal demonstration of iron deposition in the brain – A feasibility study

Multiple sclerosis (MS) causes demyelinating lesions in the white matter and increased iron deposition in the subcortical gray matter. Myelin protons have an extremely short T2* (< 1 ms) and are not directly detected with conventional clinical magnetic resonance (MR) imaging sequences. Iron deposition also reduces T2*, leading to reduced signal on clinical sequences. In this study we tested the hypothesis that the inversion recovery ultrashort echo time (IR-UTE) pulse sequence can directly and simultaneously image myelin and iron deposition using a clinical 3 T scanner. The technique was first validated on a synthetic myelin phantom (myelin powder in D₂O) and a Feridex iron phantom. This was followed by studies of cadaveric MS specimens, healthy volunteers and MS patients. UTE imaging of the synthetic myelin phantom showed an excellent bi-component signal decay with two populations of protons, one with a T2* of 1.2 ms (residual water protons) and the other with a T2* of 290 μs (myelin protons). IR-UTE imaging shows sensitivity to a wide range of iron concentrations from 0.5 to ~ 30 mM. The IR-UTE signal from white matter of the brain of healthy volunteers shows a rapid signal decay with a short T2* of ~ 300 μs, consistent with the T2* values of myelin protons in the synthetic myelin phantom. IR-UTE imaging in MS brain specimens and patients showed multiple white matter lesions as well as areas of high signal in subcortical gray matter. This in specimens corresponded in position to Perl's diaminobenzide staining results, consistent with increased iron deposition. IR-UTE imaging simultaneously detects lesions with myelin loss in the white matter and iron deposition in the gray matter.     

Mechanical characteristics of solution grown potassium zinc chloride crystals doped with lithium ions

Results of indentation-induced hardness testing studies on potassium zinc chloride crystals doped with Li⁺ ions, leading to an understanding of their mechanical behaviour, are presented. The Vickers hardness of these crystals for (1 0 0), (0 1 0) and (0 0 1) planes in the load range 20–160 g were studied. Load-independent values of hardness are estimated for the three crystallographic planes by applying Hays-Kendall’s and Li-Bradt models. The results showed that: (1) for the three crystallographic planes the load-independent hardness obtained by Li-Bradt model is higher than that predicted by Hays-Kendall’s, approach; (2) the load independent hardness of the (0 0 1) plane is higher than that of both (1 0 0) and (0 1 0) planes, (3) the values of load-independent hardness depend on Li⁺ concentrations in the K₂ZnCl₄ crystals, (4) the variations of crack length and crack morphology are described for studied crystal planes.     

Polycrystalline lead iodide films produced by solution evaporation and tested in the mammography X-ray energy range

Lead iodide polycrystalline films have been deposited on corning glass substrates using solution evaporation in oven. Films 6 μm-thick were obtained with full coverage of the substrates as verified by scanning electron microscopy. Some pin-holes were observable. X-ray diffraction revealed a crystalline structure corresponding to the 4 H–PbI₂ polytype formation. Polarized Raman scattering experiments indicated a lamellar structure. Anisotropy was also investigated using depolarization ratio calculations. The optical and electrical properties of the samples were investigated using photoluminescence and dark conductivity as a function of temperature, respectively. Activation energies of 0.10 up to 0.89 eV were related to two main electrical transport mechanisms. Films were also exposed to X-ray irradiation in the mammography X-ray energy range. The detector produced was also exposed to X-ray from 5 mR up to 1450 mR. A linear response was observed as a function of dose with a slope of 0.52 nA/mm² per mR.     

Preparation,surface state and band structure studies of SrTi(1 − x)Fe(x)O(3 − δ) (x = 0–1) perovskite-type nano structure by X-ray and ultraviolet photoelectron spectroscopy

In this report, SrTi_(1 ? x)Fe_(x)O_(3 ? δ) photocatalyst powder was synthesized by a high temperature solid state reaction method. The morphology, crystalline structures of obtained samples, was characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscopy (TEM), respectively. The electronic properties and local structure of the perovskite STF_x (0 ≤ x ≤ 1) systems have been probed by extended X-ray absorption fine structure (EXAFS) spectroscopy. The effects of iron doping level x (x = 0–1) on the crystal structure and chemical state of the STF_x have been investigated by X-ray photoelectron spectroscopy and the valence band edges for electronic band gaps were obtained for STF_x by ultraviolet photoelectron spectroscopy (UPS). A single cubic perovskite phase of STF_x oxide was successfully obtained at 1200 °C for 24 h by the solid state reaction method. The XPS results showed that the iron present in the STF_x perovskite structure is composed of a mixture of Fe³⁺ and Fe⁴⁺ (SrTi_(1 ? x)[Fe³⁺, Fe⁴⁺]_(x)O_(3 ? δ)). When the content x of iron doping was increased, the amount of Fe³⁺ and Fe⁴⁺ increased significantly and the oxygen lattice decreased on the surface of STF_x oxide. The UPS data has confirmed that with more substitution of iron, the position of the valence band decreased.     

10.6 μm Infrared light photoinduced insulator-to-metal transition in vanadium dioxide

Vanadium dioxide has excellent phase transition characteristic. Before or after phase transition, its optical, electrical, magnetic characteristic hangs hugely. It has a wide application prospect in many areas. Now, the light which can make vanadium dioxide come to pass photoinduced phase transition range from soft X-ray to medium infrared light (6.9 μm, 180 meV). However, whether 10.6 μm (117 meV) long wave infrared light can make vanadium dioxide generate photoinduced phase transition has been not studied. In this paper, we researched the response characteristic of vanadium dioxide excited by 10.6 μm infrared light. We prepared the vanadium dioxide and test the changes of vanadium dioxide thin film’s transmittance to 632.8 nm infrared light when the thin film is irradiate by CO₂ laser. We also test the resistivity of vanadium dioxide. Excluding the effect of thermal induced phase transition, we find that the transmittance of vanadium dioxide thin film to 632.8 nm light and resistivity both changes when irradiating by 10.6 μm laser. This indicates that 10.6 μm infrared light can make the vanadium dioxide come to pass photoinduced phase transition. The finding makes vanadium has a potential application in recording the long-wave infrared hologram and making infrared detector with high resolution.     

Study of resonant modes in a 700 nm pitch macroporous silicon photonic crystal

In this study the modes produced by a defect inserted in a macroporous silicon (MP) photonic crystal (PC) have been studied theoretical and experimentally. In particular, the transmitted and reflected spectra have been analyzed for variations in the defect’s length and width. The performed simulations show that the resonant frequency is more easily adjusted for the fabricated samples by length tuning rather than width. The optimum resonance peak results when centered in the PC bandgap. The changes in the defect geometry result in small variations of the optical response of the PC. The resonance frequency is most sensitive to length variations, while the mode linewidth shows greater change with the defect width variation. Several MPS photonic crystals were fabricated by the electrochemical etching (EE) process with optical response in the range of 5.8 μm to 6.5 μm. Results of the characterization are in good agreement with simulations. Further samples were fabricated consisting of ordered modulated pores with a pitch of 700 nm. This allowed to reduce the vertical periodicity and therefore to have the optical response in the range of 4.4 μm to 4.8 μm. To our knowledge, modes working in this range of wavelengths have not been previously reported in 3-d MPS structures. Experimental results match with simulations, showing a linear relationship between the defect’s length and working frequency inside the bandgap. We demonstrate the possibility of tailoring the resonance peak in both ranges of wavelengths, where the principal absorption lines of different gases in the mid infrared are placed. This makes these structures very promising for their application to compact gas sensors.     

Spatial coherence on micrometer scale measured by a nanohole array

For microscopic interference setups like an arrangement for in-line holographic microscopy a partially coherent illumination with volumes of coherence in the micrometer scale is sufficient and helpful. For the sensitive measurement of the area of spatial coherence, we use a 125 × 125 nanohole array with aperture diameters of 530 nm and periodic distances of 4 μm. In contrast to Young's double pinhole, multiple beams interfere with each other and a peak intensity enhancement by more than a factor of 1000 can be reached. From the diameter of interference spots, which are located in the Talbot planes, we determine the diameter of the area of spatial coherence in the range of 5–50 μm. Limitations of this technique are given by the numerical aperture of the used imaging lens (100×/0.75) as well as the periodic distance of the apertures within the array.     

Patterned growth of ZnO nanorods and their field emission properties

Patterned zinc oxide (ZnO) nanorods were fabricated on the different patterned silicon nanocrystallite (SiNC) substrates via a simple thermal evaporation method without any catalyst. The as-synthesized products were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), respectively. The efficient field emission with low turn-on and threshold field, 3.5 V/μm and 8.1 V/μm, was obtained. The experimental results demonstrate that these products could be one of the promising candidates for field emission displays.     

Microstructures and nano mechanical properties of the metal tungsten film

The W film was prepared on 1045 steel by magnetron sputtering, with the thickness of 2 μm, its surface and cross-section morphologies were investigated with SEM, and the phase structure was analyzed with XRD. X-ray stress determinator was utilized to measure its residual stress, and the nano-hardness and elastic modulus of the film were surveyed by nano-indentation tester. The results show that the surface of W film is very compact and smooth; the particles arranged regularly, the granularity of the thin film is about 1 μm. The microcracks, cavities and desquamation were not found in the film and interface, and the bonding between the W film and substrate is well. The XRD results showed that the W film had a body-centered cubic structure, the lattice constant: a = 0.316 nm, the growth preferred orientations are (1 1 0) and (2 2 0). The compressive stress (−169 MPa) was found on the surface. The average nano-hardness and elastic modulus of W film are 15.22 GPa, 176.64 GPa, respectively, and the mechanical properties of W film are well.     

Formation of the (Bi, Pb)2Sr2Ca2Cu3O10+δphase: reaction mechanism and kinetics

In order to elucidate the formation mechanism of the Bi, Pb(2223) phase, extensive investigations have been performed by means of combined differential thermal analysis and thermo-gravimetric measurements, X-ray diffraction as well as scanning electron microscopy and energy dispersive X-ray microanalysis.Starting from co-precipitated oxalate powders, the transformations leading to the formation of the Bi, Pb(2223) phase were studied. Based on these investigations the Bi,  Pb(2223) phase formation process, involving the Bi, Pb(2212), Ca₂PbO₄and alkaline-earth cuprate phases as precursors has been separated into elemental steps. A new model for the formation mechanism of the Bi, Pb(2223) phase will be presented.The Bi, Pb(2223) phase formation kinetics has been studied using the Avrami relation for isothermal phase transformations. The analysis of the Bi, Pb(2223) phase evolution revealed a marked change of the Avrami exponent during the course of the Bi, Pb(2223) phase formation after about 12 hours sintering at 857 ° C.The activation energy for the formation of the Bi, Pb(2223) phase has been determined under various experimental conditions. The nominal composition of the precursor powders, the temperature at which they were calcined as well as the size of their constituents were found to have a significant influence on the value of the activation energy.