Bone micro-damage assessment using non-linear resonant ultrasound spectroscopy (NRUS) techniques: a feasibility study

Non-linear resonant ultrasound spectroscopy (NRUS) is a technique exploiting the significant non-linear behavior of damaged materials, related to the presence of damage. This study shows for the first time the feasibility of this technique for damage assessment in bone. Two samples of bovine cortical bone were subjected to a progressive damage experiment. Damage accumulation was progressively induced in the samples by mechanical testing. For independent assessment of damage, X-ray CT imaging was performed at each damage step, but only helped in the detection of the prominent cracks. Synchrotron micro-CT imaging and histology using epifluorescence microscopy were performed in one of the two samples at the last damage step and allowed detection of micro-cracks for this step. As the quantity of damage accumulation increased, NRUS revealed a corresponding increase in the non-linear response. The measured change in non-linear response is much more sensitive than the change in elastic modulus. The results suggest that NRUS could be a potential tool for micro-damage assessment in bone. Further work has to be carried out for a better understanding of the physical nature of damaged bone, and for the ultimate goal of in vivo implementation of the technique where bone access will be a challenging problem.     

Applying nonlinear resonant ultrasound spectroscopy to improving thermal damage assessment in concrete

Nonlinear resonant ultrasound spectroscopy (NRUS) consists of evaluating one or more resonant frequency peak shifts while increasing excitation amplitude. NRUS exhibits high sensitivity to global damage in a large group of materials. Most studies conducted to date are aimed at interrogating the mechanical damage influence on the nonlinear response, applying bending, or longitudinal modes. The sensitivity of NRUS using longitudinal modes and the comparison of the results with a classical linear method to monitor progressive thermal damage (isotropic) of concrete are studied in this paper. In addition, feasibility and sensitivity of applying shear modes for the NRUS method are explored.     

Modal resonant ultrasound spectroscopy for ferroelastics

Recent experimental and theoretical improvements of resonant ultrasound spectroscopy (RUS) are summarized to investigate elastic constants of phases in shape memory alloys. The proposed inversion procedure, described in this work, is particularly suitable to reliable evaluation of the temperature dependence of elastic constants of low-symmetry ferroelastic materials which may be strongly elastically anisotropic and tend to exist in twinned forms. The method is applicable even for the evaluation of single-crystal elastic constants from RUS measurements on microtwinned crystals, since it involves a homogenization algorithm based on the macroscopic deformation response of the layered structure. This potentially allows performing meaningful acoustic studies on samples with a general submicron-size layered structure.     

Sensitivity of the resonant ultrasound spectroscopy to weak gradients of elastic properties

The applicability of resonant ultrasound spectroscopy on materials with weak spatial gradients in elastic coefficients and density is analyzed. It is shown that such gradients do not affect measurably the resonant spectrum but have a significant impact on the modal shapes. A numerical inverse procedure is proposed to explore the possibility of reconstructing the gradients from experimentally obtained modal shapes. This procedure is tested on synthetic data and applied to determine the gradient of the shear modulus in a continuously graded silicon nitride ceramic material. The results are in a good agreement with the gradient calculated for the examined material theoretically as well as with the results of other experimental methods.     

Nonlinear spectroscopy of resonant levels by the photon-echo technique

A new method to measure the relaxation times of population, orientation and alignment of the resonant level is proposed.     

On the use of hollow tube geometries for resonant ultrasound spectroscopy

Resonant ultrasound spectroscopy (RUS) can nondestructively obtain the elastic constants of compact specimens, however many materials have hollow cross-sections and frequency analysis of such geometries is required before inclusion in the RUS methodology. Resonant mode shapes of tubes with length equal to diameter and varying ratios of tube inner to outer diameter (Λ) as well as Poisson's ratio (ν) were identified by eigenvalue analysis using a commercial finite element code. Longitudinal and shear RUS experiments were conducted on tubes with Λ varying between 0 and 0.95 and compared to the numerical results. Simulations predict that the fundamental mode transitions from pure torsion to symmetric or antisymmetric ring bending at Λ = 0.3. The frequency of the first torsion mode is invariant to Λ and unequivocal identification of this mode is obscured by overlap of bending harmonics as Λ approaches 0.95. In the context of rapid calculation of isotropic elastic constants, shear moduli were calculated from the first torsional mode and Poisson's ratio was inferred from the Demarest maps of the mode structure's dependence upon Poisson's ratio. An average shear modulus of 27.5 + 1.5 ∕ -0.6 GPa, about 5% larger than literature values for 6061 aluminum, and ν of 0.33 were inferred. Errors are attributed to tube aspect ratios slightly greater than 1 and weak material anisotropy. Existing analytical solutions for ring bending modes derived from shell approximations and for infinitely long tubes under plane strain assumptions do not adequately describe the fundamental modes for short tubes. The shear modulus can be calculated for all Λ using the existing analytical solution.     

Measuring elastic constants of arbitrarily shaped samples using resonant ultrasound spectroscopy

One of the most important undertakings for materials is the measurement of the elastic behavior. As derivatives of the free energy with respect to atomic displacements, the elastic properties are closely connected to the thermodynamic properties of the material. Elastic behavior is a sensitive probe of the lattice environment in which all solid state phenomena occur, particularly in the vicinity of a phase transition. A useful method for measuring elastic properties is resonant ultrasound spectroscopy (RUS). Some novel materials to which RUS might be applied are often fragile or chemically reactive so that they cannot be polished into the shapes required by conventional RUS; for such cases a finite element method may be used. In this paper a discussion and test of a finite element method for RUS with arbitrarily shaped samples is provided.     

Wood elastic characterization from a single sample by resonant ultrasound spectroscopy

The goal of this paper is to propose an experimental method allowing the identification of the complete elastic tensor of anisotropic biological materials such as wood using only one sample. To do so, two complementary methods are used. First, the wood eigen-directions are defined from a sample of spherical shape that is then cut into a cube in a way to perform resonant ultrasound spectroscopy (RUS). The method is successfully applied on a reference beech sample with known orthotropic directions. A comparison of the identified elastic constants with those from the literature and some inferred from ultrasonic transmission measurements is given.     

Determination of elastic moduli of rock samples using resonant ultrasound spectroscopy

Resonant ultrasound spectroscopy (RUS) is a method whereby the elastic tensor of a sample is extracted from a set of measured resonance frequencies. RUS has been used successfully to determine the elastic properties of single crystals and homogeneous samples. In this paper, we study the application of RUS to macroscopic samples of mesoscopically inhomogeneous materials, specifically rock. Particular attention is paid to five issues: the scale of mesoscopic inhomogeneity, imprecision in the figure of the sample, the effects of low Q, optimizing the data sets to extract the elastic tensor reliably, and sensitivity to anisotropy. Using modeling and empirical testing, we find that many of the difficulties associated with using RUS on mesoscopically inhomogeneous materials can be mitigated through the judicious choice of sample size and sample aspect ratio.     

FTIR spectroscopy applied to woodflour

The features of infrared spectra of woodflour obtained by transmission and diffuse reflectance (DRIFT) are discussed. Intrinsic differences between the two techniques, as well as differences in sample preparation for transmission (pressed pellet) or DRIFT (simple mixing with powered KBr), affect the appearance of the spectra recorded. Other important differences arise from the water content in the sample, as well as in the KBr powder utilized as reference and dilution. Some of these differences are discussed since they occur in regions usually utilized to check modifications in the wood. The effect of sample concentration is investigated for both techniques. In transmission, the opacity of the pellet limits the sample concentration to about 2 wt% in KBr in order to obtain useful spectra. While no concentration limitations are present for DRIFT, distortion of the intensities of bands occur, mainly at low wavelengths. Finally, the use of DRIFT subtraction to detect small surface variations in the woodflour (chemical and physical adsorption of a modifier) is illustrated.     

Sub-gigahertz laser resonant ultrasound spectroscopy for the evaluation of elastic properties of micrometric fibers

The cross-section eigenmodes of micrometric cylinders were measured in the range of several tens of MHz to about 0.5 GHz. The vibrations were excited using subnanosecond laser pulses. The cross-section eigenmodes were simulated using finite element modeling in a 2D geometry. Using the method of resonant ultrasound spectroscopy, the vibration spectrum of an aluminum wire of diameter 33μm served to determine Young’s modulus and Poisson’s ratio with a precision of 0.7% and 0.3%, respectively. The calculated and measured frequencies of cross-section eigenmodes were fitted with a precision better than 0.5% in the 50–500 MHz range.     

Nonlinear spectroscopy with a vertical-cavity surface-emitting laser (VCSEL)

We have evaluated the suitability of a vertical-cavity surface-emitting laser diode (VCSEL) for spectroscopic applications. Despite its low output power it is possible to observe narrow resonances in a saturated absorption spectroscopy experiment on the cesium D ₂ transition at 852 nm, limited in width by the laser linewidth of several tens of MHz. High modulation efficiency of the VCSEL allows us to create modulation sidebands at 9.2 GHz frequency via direct modulation of the laser injection current. Using the carrier and either one of the sidebands coherent population trapping (CPT) resonances in a buffered cesium vapor can be prepared with linewidths below 130 Hz. With this very compact setup we have studied the dependence of CPT resonance position and linewidth as a function of optical detuning and find evidence of the influence of the excited state hyperfine structure. Received: 30 April 1999 / Revised version: 25 June 1999 / Published online: 30 November 1999     

Fluorescence spectroscopy applied to orange trees

In this work, we have applied laser-induced fluorescence spectroscopy to investigate biological processes in orange trees (Citrus aurantium L.). We have chosen to investigate water stress and Citrus Canker, which is a disease caused by the Xanthomonas axonopodis pv. citri bacteria. The fluorescence spectroscopy was investigated by using as an excitation source a 442-nm 15-mW HeCd gas multimode discharge laser and a 532-nm 10-mW Nd³⁺:YAG laser. The stress manifestation was detected by the variation of fluorescence ratios of the leaves at different wavelengths. The fluorescence ratios present a significant variation, showing the possibility to observe water stress by fluorescence spectrum. The Citrus Canker’s contaminated leaves were discriminated from the healthy leaves using a more complex analysis of the fluorescence spectra. However, we were unable to discriminate it from another disease, and new fluorescence experiments are planned for the future.     

Electron energy-loss spectroscopy applied to solids

Several illustrating examples of recent electron energy-loss investigations of the electronic structure of solids are reviewed. In particular, studies on rare-gas bubbles in metals, on conducting polymers, and onL _2,3 edges of 3d transition metals are reported. Moreover, the electron energy-loss spectrometer, which was used for these investigations, is described briefly.     

Nonlinear resonant tunneling diode (RTD) circuits for microwave A/D conversion

Short-duration electrical pulses play important roles in ultrafast time-domain metrology: they are used to sample rapidly varying signals or as probe signals in ranging radars, time-domain reflectometry and in communication. In this work, we design a nonlinear transmission, which is loaded with resonant tunneling diode to be suitable for microwave A/D conversion. A resonant tunneling diode (RTD) has a negative differential resistance that means when the voltage increases the current decreases. The equivalent circuit of monostable line is given. The simulation is performed by using OrCad program. Results show that a spike is produced and after a charging time constant, another switching occurs. Hence – similar to a relaxation oscillator – the spiking period is determined by the amplitude and frequency of the input current. The transmission line itself ensures the generation and propagation of identical spikes, such as solitons formed after few diodes.     

Interference approach applied to dual-grating dielectric resonant grating reflection filters

The resonant mechanisms associated with dual-grating dielectric resonant grating reflection filters are described by use of an interference approach. These structures consist of two modulated regions of equal period separated by a higher-index film region. We show that the spectral linewidth is dependent on the separation between the modulated regions and can range from theoretically zero to approximately four times what would be obtained by use of a single-grating geometry.     

X-ray photoelectron spectroscopy applied to insular films

For a given experimental arrangement, X-ray photoelectron spectra measured at different points on a sample surface may show fluctuations which cannot be attributed to counting statistics. These fluctuations are caused by overlayers having an insular structure. The XPS information obtained can be evaluated by a statistical method to yield the dimensions of the islands.     

Exchange-mediated anisotropy of (ga,mn)as valence-band probed by resonant tunneling spectroscopy

We report on experiments and theory of resonant tunneling anisotropic magnetoresistance (TAMR) in AlAs/GaAs/AlAs quantum wells (QW) contacted by a (Ga,Mn)As ferromagnetic electrode. Such resonance effects manifest themselves by bias-dependent oscillations of the TAMR signal correlated to the successive positions of heavy (HH) and light (LH) quantized hole energy levels in GaAs QW. We have modeled the experimental data by calculating the spin-dependent resonant tunneling transmission in the frame of the 6 x 6 valence-band k.p theory. The calculations emphasize the opposite contributions of the (Ga,Mn)As HH and LH subbands near the Gamma point, unraveling the anatomy of the diluted magnetic semiconductor valence band.