A spectroscopic study of some high-temperature superconductors using a low-temperature STM

We used a scanning tunnelling microscope (STM) to measure both the tunnel current, I, and the dynamic conductance, dI/dV, at 4·2 K for a number of high-transition temperature oxide superconductors. Large spatial variations in the tunnelling characteristics are observed. At low tunnel resistances, all samples show evidence of single electron tunnelling and incremental charging. Results on BiSrCaCu₂O_x show the coexistence of charging with Josephson coupling between grains within the sample. Results on both the Bi sample and a single crystal of YBa₂Cu₃O_6·5+x reveal possible energy gap (2A) values of 17 and 20 meV, respectively. A very sharp 5 meV gap, observed in ceramic samples of YBa₂Cu₃O_6·5+x and Y_0·5Al_0·05Ba₂Cu₃O_6·5+x, may indicate the presence of a lower temperature phase in these samples.     

Morphometric analysis of cryofixed muscular tissue for intraoperative consultation

For diagnostic purposes, cryofixation of tissues is a daily routine technique to investigate rapidly about the presence of tumours during a surgical procedure in patients. We performed morphometric analysis of cryofixed muscular tissues according to different techniques. About 1,000 muscle fibers and 1,493 nuclei, were automatically examined. After freezing, ice tissue interfaces shrinkage of the cells were present. Liquid isopentane or liquid nitrogen produced a statistical increase of fractal dimension, D, of the ice‐tissue interfaces, P < 0.001 respect to the formalin‐fixed samples, cryofixation performed inside the cryostat chamber at t = ?20°C produced a D value close to the formalin‐fixed samples. Shrinkage of the muscle fibers was higher in the samples cryofixed inside the cryostat chamber (P < 0.001). Cryofixation inside cryostat or by liquid nitrogen caused decreases of the nuclei dimensions and altered nuclear morphology (P < 0.01), liquid isopentane appeared not affecting the nuclei of the fibers. Cryofixation inside the cryostat chamber produced the highest shrinkage but it was reduced performing cryofixation in liquid nitrogen or isopentane. Freezing damage inside the muscle cells was absent in the samples cryofixed inside the cryostat, it was present after cryofixation by liquid nitrogen or isopentane. Subcellular components like the nuclei were preserved by isopentane. This paper present, for the first time, an objective method able to quantify and characterize the damages produced by cryofixation in biological sample for intraoperative consultation. Microsc. Res. Tech. 79:155–161, 2016. © 2016 Wiley Periodicals, Inc.     

Baseline correction of AFM force curves in the force–time representation

This note reports on the proper correction of force data acquired with an atomic force microscope (AFM). The force–time representation is hereby used to obtain the correction factors for the overall offset and slope for a single force–time curve, as the initial force, F₀ = F(t₀), and the rate of change in the force per unit of time, dF/dt, respectively. The report shows that a complete set of force data, including the approach, delay and retraction regions, can be simultaneously corrected in the force–time representation by subtracting the line CL_t = F₀ + dF/dt·t to the experimental data. The method described here outperforms the one commonly employed in the correction of AFM force curves and highlights the convenience of using the force–time representation for force data processing wherein the artifactual behavior can be expressed as a single, differentiable function of time.     

Automated Microscope-Absorption-Spectrophotometry Of Rock-Forming Minerals In The Range 40,000–5000 Cm−1 (250–2000 Nm)

To measure polarized absorption spectra of microcrystals of 3dⁿ-ion bearing silicate minerals, computer processed, microscope-spectrophotometric methods have been developed. Absorbance, log (I₀/I), can be measured with high relative accuracy (near u.v. and vis: ±0·002 to 0·001; n.i.r.: ±0·004 to 0·002), and relatively small spectral band widths are available. Hence, weak spin-forbidden dd-bands of 3dⁿ-ions can be recognized alongside spin-allowed dd-transitions without artificial broadening of absorption bands due to finite resolution. The smallest area from which absorption spectra can be taken is 8 μm in diameter. As one example of the many applications in mineralogy and material sciences, absorption spectra of a natural spessartine garnet, Spess_69·7Alm_30·0Gross_0·05, containing Mn²⁺, Fe²⁺, and traces of Fe³⁺ as 3dⁿ-ions, and of a pure Mn²⁺-garnet, Spess₆₇Gross₃₃, are presented. From these it is evident that bands in natural spessartines at ～ 26,900, 23,200 cm^?1 which were assigned to dd-transitions in Fe³⁺⁽⁶⁾, have to be reassigned to Mn²⁺⁽⁸⁾. Comparison of spectra obtained with the microscopic equipment described with those obtained by means of conventional macroscopic equipment prove that the methods described produce true spectra.     

Determining Generation–Recombination Characteristics of a Semiconductor–Dielectric Interface from the Current Kinetics of Surface Minority Carrier Generation

Conditions for the one-to-one characterization of the generation (G _s) and surface recombination (R _s) rates of minority charge carriers (MCCs) in a metal–oxide–semiconductor (MOS) structure (in the case of strong nonequilibrium depletion) by the MCC surface generation current (I(t)) flowing in an external circuit of this structure are revealed. These conditions are the following: (1) the generation current I is independent of the time t (until the structure enters an equilibrium state) and the voltage V _{g 0} corresponding to the initial nonequilibrium depletion and (2) the duration of current steps I(V _{g 0}) = const and, consequently, the equilibrium surface charge increase with increasing V _{g 0}. The observed kinetics of the MCC generation current for the MCCs induced in an n-Si MOS structure at 293 K experimentally confirms the realization of these conditions. The values of the generation and recombination rates G _s = 2.84 × 10¹⁰ cm^–2s^–1 and R _s = 6.82 cm s^–1 obtained from current levels I(V _{g 0}) = const are typical of high-quality Si MOS structure. Additionally measured capacitance–voltage characteristics were used to determine the interface state density at the Si/SiO₂ contact near the middle of the Si gap (N _ss(E) 6.4 × 10¹⁰ cm^–2eV^–1), which allowed the estimation of the effective capture cross section of these states _eff 1.4 × 10^–16 cm².     

Elimination of Systematic Measurement Inaccuracy in Voltage–Capacitance Spectroscopy of Semiconductor/Insulator Interface

An improved algorithm for measurements of quasi-static voltage–capacitance characteristics (VCC) of metal–insulator–semiconductor (MIS) structures is suggested. This algorithm includes the following stages: high-temperature depolarization of a MIS structure, its cooling at a constant depolarization voltage, measurement of the MIS current I(V _g) upon the linearly time-swept (increasing or decreasing) gate potential, and averaging of the dependences I(V _g) obtained in the modes of sweep rate _v > 0 and _v < 0 ( _v = 0). The method allows the systematic error of the VCC C(V _g) measurement caused by the relaxation polarization of the insulator, leakage current, and shift of the electrometer zero to be eliminated. As a result, the accuracy and reliability of the determination of the interface state (IS) density N _ss(E) are increased, and the energy range of the IS spectra is extended. To test the efficiency of the algorithm developed, it was used for determining the function N _ss(E) in the system SiO₂/(100)Si : P.     

Determining the Surface Electrostatic Potential Ψ s of a Dielectric-Bordering Semiconductor Using the Method of Ψ s "/Ψ s Diagrams

A quantitative approach to determining the integration constant _s0(V _{g 0}) in an expression relating the semiconductor surface potential _s to the voltage V _g applied to the metal–insulator–semiconductor (MIS) structure and its quasi-static capacitance–voltage characteristic C _v(V _g) (normalized to the dielectric capacitance) is described. The method is based on the analysis of experimental functions _s ^"( _s ), where _s ^" = d _s /dV _g, and the same functions calculated for an ideal MIS structure. The obtained function _s (V _g) is a rather exact and complete characteristic of electron properties of the MIS-structure phase boundary (the integrated interface state density, flat-band voltage V _FB, sign and density of the dielectric fixed charge, and variations of these parameters under the action of various factors). Using the example of a particular n-Si MIS structure, it is shown that the method of _s ^"/ _s diagrams ensures a noticeable (up to 0.93 eV) widening of the Si gap sounding region and observation (by the value of the V _FB shift) of very small ( 1 × 10⁷ cm^–2) variations in the charge density at the Si/SiO₂ phase boundary.     

The effect of different cleaning agents and resin cement materials on the bond strength of contaminated zirconia

The purpose of this study was to examine the effect of different cleaning methods and resin cements on the shear bond strength (SBS) of contaminated zirconia. A total of 92 disc-shaped zirconia specimens were contaminated with different procedures. Then, the specimens were grouped according to cleaning methods and resin cements: no cleaning + Variolink Esthetic DC (CN_V), no cleaning + Panavia V5 (CN_P), sandblasted + Variolink Esthetic DC (SB_V), sandblasted + Panavia V5 (SB_P), Ivoclean + Variolink Esthetic DC (IC_V), Ivoclean + Panavia V5 (IC_P), Katana Cleaner + Variolink Esthetic DC (KC_V), and Katana Cleaner + Panavia V5 (KC_P). Following an aging protocol in a 37°C for 1 week, SBS analysis was performed with a universal test machine. For the surface topography and elemental analysis, scanning electron microscopy and energy-dispersive X-ray spectroscopy (EDS) were used. Significance was evaluated as p < .05 and p < .01. The highest SBS results were found in the SB_P group, showing a statistically significant difference from all other groups (p < .05). For the same cleaning method, Panavia V5 showed statistically significantly higher SBS values than Variolink Esthetic DC (p < .01), except the CN_P–CN_V (p = .880) and KC_P–KC_V (p = .082) groups. The most detected surface elements by EDS were Zr, O, C, and N, respectively. The contaminated zirconia surfaces must be cleaned for successful adhesion. The use of phosphate-containing adhesives in combination with sandblasting will increase the adhesion strength, and universal cleaning agents can be a good alternative to sandblasting.     

Estimation of length and surface of anisotropic capillaries

Surface density (S_V) and length density (L_V) of myocardial capillaries have hitherto been estimated from their profile boundary length (B_A) and their numerical density (Q_A) on transverse sections by the simplifying assumptions of the Krogh model (perfectly anisotropic, straight, unbranched capillaries with constant cross-sectional area). As the capillaries actually are partially anisotropic, curved, branching cylinders with variable cross-sectional area, a geometrical bias arises from the model-reality discrepancies. We have applied and compared two methods to overcome these inconsistencies: (1) estimation of L_V and S_V by a more realistic model (the Dimroth-Watson distribution); (2) estimation of L_V and S_V from isotropic uniform random (IUR) sections. Twelve male Wistar rats were fixed by retrograde vascular perfusion. One pair of longitudinal and transverse sections, and six IUR sections per animal were selected at random from the left ventricular papillary muscles. Ultrathin sections were silver-impregnated and studied by light microscopic morphometry. Nearly identical estimates of L_V and S_V were found by both methods. The model-based estimation provides biologically meaningful anisotropy constants, but it presupposes knowledge of the anisotropy axis. The IUR method provides no measure of anisotropy, but it can be applied in tissues where the anisotropy axis is not known. Both methods are equally efficient and practically unbiased in S_V estimation, but the model-based estimation is far more efficient in L_V estimation.     

An electron microscopy study of the phase Al3Fe

The phase Al₃Fe (monoclinic C2/m, a = 1·549 nm, b = 0·808 nm, c = 1·248 nm, β = 107·8°) has been studied by transmission electron microscopy (TEM) and high resolution electron microscopy (HREM). Crystals were obtained from a direct chill-cast ingot of an Al-0·25 wt% Fe-0·13 wt% Si alloy. Extracted crystals were prepared by dissolving the aluminium phase in butanol and filtering off the particles. The extracted Al₃Fe crystals were mainly (100) platelets. The monclinic lattice was confirmed by tilt experiments and the mirror plane was confirmed by convergent beam electron diffraction. Experimental HREM images from the [100] and [110] projection agreed with images calculated by the multislice method. The interpretation of images in terms of a projected crystal structure is discussed. Common defects in Al₃Fe crystals were: twins on (100) and faults on (001). The (001) faults could be described by a displacement 1/2·[100] on a fault plane at z = 0·5 in the unit cell. A model for (001) faults, based on multiple twinning, is proposed.     

A geometric theory of form, profile, and orientation tolerances

This article develops a geometric theory which unifies the formulation and computation of form (straightness, flatness, cylindricity, and circularity), profile and orientation tolerances stipulated in ANSI Y14.5M standard. The theory rests on an important observation that a toleranced feature exhibits a symmetry subgroup G₀ under the action of the Euclidean group, SE(3). Thus, the configuration space of a toleranced (or a symmetric) feature can be identified with the homogeneous space SE(3)/G₀ of the Euclidean group. Geometric properties of SE(3)/G₀, especially its exponential coordinates carried over from that of SE(3), are analyzed. We show that all cases of form, profile and orientation tolerances can be formulated as a minimization or constrained minimization problem on the space SE(3)/G₀, with G₀ being the symmetry subgroup of the underlying feature. We develop a simple geometric algorithm, called the Symmetric Minimum Zone (SMZ) algorithm, to unify the computation of form, profile, and orientation tolerances. Finally, we use numerical simulation results comparing the performances of the SMZ algorithm against the best known algorithms in the literature.     

Loading strategies for a class of just-in-time manufacturing system

In this paper, based on the group technology and the just-in-time manufacturing concepts, two loading models for optimal utilisation of the processing capabilities of an integrated manufacturing system consisting of a set of heterogeneous workstations are developed. These loading models are developed to integrate and utilise the available information from both the bill of materials and the process plans. The objective functions for these models are: the maximum tardiness and the makespan. In these models, the production quantity of each customer order for any part or product always equals its corresponding demand quantity; each part requires a finite number of aggregated stages of operation; job splitting is allowed; and the processing priorities of all the jobs during the planning time horizon are specified based on a desirable dispatching rule. The proposed mathematical programming models are fixed charge problems which are solved by compatible mixed integer programming algorithms. Finally, to provide additional decision-making capabilities, based on these models and their corresponding solution algorithms, a compatible decision support system is suggested.Notation l(1 toL) the product index - t(1 toN) the component (e.g., job type) index - i(1 toN) the job type priority index - j(1 toM) the workstation index - r(1 toR) the processing stage priority index - k(1 toK) the due date priority index - J _i,j,r,k the job with the job type priority indexi of the customer with the processing stage priority indexr and the due date priority indexk which has to be processed at the workstationj - L _i,r,k the number of units of the job with the job type priority indexi of the customer with processing stage priority indexr and the due date priority indexk (e.g. demand quantities) - t _i,j,r the required time to perform the processing stage priority indexr of each unit of the job with the job type priority indexi at the workstationj - D _i,r,k the due date of the job with the job type priority indexi of the customer with the processing stage priority indexr and the due date priority indexk - s _i,j,r the required time for setting up the workstationj for processing the job with the processing stage priority indexr, and the job type priority indexi - X _i,j,r,k the number of units of the job with job type priority indexi of the customer with the processing stage priority indexr, and the due date priority indexk to be produced at the workstationj - l _i,j,r,k the idle time at the workstationj prior to processing the job with the job type priority indexi and the processing stage priority indexr with the due date priority indexk - V the maximum tardiness - W the makespan of the operation - Y _i,j,r,k=1 ifX _i,j,r,k>0 - Y _i,j,r,k=0 ifX _i,j,r,k=0 - _i,j,r,k a sufficiently large constant (e.g. _i,j,r,kL _i,r,k)     

Tunnelling spectroscopy of high-temperature superconductors

We measured samples of La_1·85Sr_0·15CuO_4-y and YBa₂Cu₃O_7-y with a UHV low-temperature scanning tunnelling microscope using tips made out of tungsten, aluminium and indium. The samples are either sintered pellets, single crystals, or thin films. A wide variety of I-V curves were obtained ranging from nearly ideal S-I-N and S-I-S characteristics, to strongly asymmetric and multiple-peaked characteristics. The best data are obtained with thin film samples and indium tips. Large values of 2δ/kT_c (～ 11) are observed in most cases. We discuss possible explanations for these large values. New data are presented obtained with thin films of Y-Ba-Cu-O made by e-beam evaporation in our laboratory. A system of loadlocks is used to ensure that these films are never exposed to the atmosphere.     

The electron energy-loss near-edge structure (ELNES) on the N K-edges from the transition metal mononitrides with the rock-salt structure and its comparison with that on the C K-edges from the corresponding transition metal monocarbides

This paper presents the shapes of the electron energy-loss near-edges structure (ELNES) on the N K-edge of the group IV_A (Ti, Zr, Hf) and group V_A (V, Nb, Ta) transition metal mononitrides close to stoichiometry. With the exceptions of NbN and TaN, these compounds have the rock-salt (B1) structure when close to stoichiometry. NbN exists with both the rock-salt structure and a hexagonal structure. Two distinct ELNES shapes were observed from it, one of which corresponds closely with previously published data from the rock-salt structure. Under normal conditions, TaN is considered to exist only in the hexagonal form, the rock-salt form being a high-temperature/high-pressure phase although it has been reported as the result of plasma jet heating of the hexagonal form. Again two distinct ELNES shapes were observed, one of which appeared to fit into the pattern of the shapes from the other compounds with the rock-salt structure. The systematic changes of shape observed are very similar to those observed in the equivalent carbides and qualitatively follow the behaviour expected from theoretical band structures. The change in the chemical shift of the N K-edge on going from a group IV_A nitride to a group V_A nitride is ～-0·8 eV while that on going from a group IV_A carbide to a group V_A carbide is ～+0·8 eV. This difference in behaviour is explained as the result of differences in the densities of states at the Fermi levels of the compounds. The position of the first peak in the ELNES also shows a systematic change in its energy relative to the core state as the number of valence electrons in the compound increases and also as the transition series of the metal species changes. The energies, E_r, of the peaks in the ELNES relative to the threshold follow a relationship similar to that predicted by Natoli, i.e. (E_r - V)a = const. where V is the ‘muffin tin’ potential and a is the lattice parameter. The first peak gives a negative constant in the relationship. The value of constant increases for each subsequent peak up to the sixth becoming positive for the fourth and higher peaks but drops slightly on going from the sixth to the seventh peak. Each peak gives a different value of V in the relationship. The data sets for the carbides and the nitrides are systematically different in a similar way for each peak and there are deviations from linearity within each set. The systematic difference is minimized and the linearity significantly improved if the difference in the energies of two prominent peaks is used instead of E_r. This systematic variation of peak energy with lattice parameter can be used to predict the lattice parameter. If both the nitride and the carbide data for the energy of a prominent peak relative to the threshold are used, this results in a maximum deviation of 4% (or ～0·02 nm). However, if the differences in the energies of two prominent peaks are used and the data for the carbides and the nitrides are treated independently, the maximum deviation drops to 0·4% (or ～0·002 nm). At this level, uncertainties in the lattice parameters themselves come into play and better characterized materials are required to set true limits to the accuracy of the predictions. Finally some applications in the microanalysis of materials are outlined briefly.     

Effect of two medium chain triglycerides‐supplemented diets on synaptic morphology in the cerebellar cortex of late‐adult rats

Ketogenic diets (KDs) have shown beneficial effects in experimental models of neurodegeneration, designating aged individuals as possible recipients. However, few studies have investigated their consequences on aging brain. Here, late‐adult rats (19 months of age) were fed for 8 weeks with two medium chain triglycerides‐supplemented diets (MCT‐SDs) and the average area (S), numeric density (Nv_s), and surface density (S_v) of synapses, as well as the average volume (V), numeric density (Nv_m), and volume density (V_v) of synaptic mitochondria were evaluated in granule cell layer of the cerebellar cortex (GCL‐CCx) by computer‐assisted morphometric methods. MCT content was 10 or 20%. About 10%MCT‐SD induced the early appearance of senescent patterns (decreased Nv_s and Nv_m; increased V), whereas 20%MCT‐SD caused no changes. Recently, we have shown that both MCT‐SDs accelerate aging in the stratum moleculare of CA1 (SM CA1), but are “antiaging” in the outer molecular layer of dentate gyrus (OML DG). Since GCL‐CCx is more vulnerable to age than OML DG but less than SM CA1, present and previous results suggest that the effects of MCT‐SDs in the aging brain critically depend on neuronal vulnerability to age, besides MCT percentage. Microsc. Res. Tech. 2009. © 2009 Wiley‐Liss, Inc.     

Investigation of Tool Wear and Surface Finish by Analyzing Vibration Signals in Turning Assab-705 Steel

Various occurrences in machining influence the machining dynamics and thus produce vibration in the cutting tool-workpiece arrangement. In this investigation, with tri-axial accelerometer mounted on the tool-holder in turning ASSAB-705 steel, vibration signals have been captured with and without cutting. The nature of vibrations arising in the cutting tool at different cutting conditions has been investigated. It has been observed that the RMS amplitude of vibration along all three axes for the increasing cutting speed was mixed in nature; however, an increasing trend was noticed in the vibrations along the feed, V_x and radial, V_y directions. The vibration along the main cutting direction, V_z was mixed, initiated by large vibration and then decreased until a particular cutting speed was reached and finally increased steadily. The feed vibration component, V_x has a similar response to the change of the workpiece surface roughness, while the other two components, V_y and V_z have the more coherent response to the rate of flank wear progression throughout the tool life. The natural frequency of different machine parts vibration has been found to be within the band of 0 Hz – 4.2 kHz, whereas the frequencies of different occurrences in turning varied between 98 Hz and 42 kHz.     

Parallel schemes of certain discrete orthogonal transformations

The paper describes parallel transformations of the Walsh and Haar transforms with a time complexity O(log₂ N), as well as the fast wavelet and saw-tooth transforms. The parallel calculation of the basis of the discrete Fourier transform is performed with a time complexity O(1); the parallel algorithm of the fast wavelet transform is estimated as having a time complexity O(log₂ log₂ N × log₂ N).     

The expected volume of a random polytope in a ball*

For any convex body K in d-dimensional Euclidean space E^d(d≥2) and for integers n and i, n ≥ d + 1,1 ≤ i ≤ n, let V^(d)_n-ii(K) be the expected volume of the convex hull H_{n-i, i} of n independent random points, of which n-i are uniformly distributed in the interior, the other i on the boundary of K. We develop an integral formula for V^(d)_{n-i, i}(K) for the case that K is a d-dimensional unit ball by considering an adequate decomposition of V^(d)_n-i, i into d-dimensional simplices. To solve the important case i = 0, that is the case in which all points are chosen at random from the interior of B_d, we require in addition Crofton's theorem on mean values. We illustrate the usefulness of our results by treating some special cases and by giving numerical values for the planar and the three-dimensional cases.