The authors would like to acknowledge the contributions made by Michael Behrens and Damith Abeywardana in designing and implementing several sensing hardware components. Research supervision roles played by Alen Alempijevic, Teresa Vidal-Calleja, Gamini Dissanayake, and Sarath Kodagoda, as well as contributions made by all persons and organizations who funded and partnered with the Critical Pipes Project, are also acknowledged.

1. Extracting the decay rate &#946; from an available detector coil-based PEC signal
<ol>
	<li>Express an available experimentally captured PEC signal (i.e., a time domain detector coil voltage (denoted as V(t))) in the logarithmic form of ln[V(t)]. A typical PEC signal expressed in the form of ln[V(t)] is shown in Figure 1.</li>
	<li>Find a linear region in the form of <img align="center" alt="Equation 2" src="/files/ftp_upload/59618/59618eq2g.jpg" /> such that the signal satisfies the condition <img align="center" alt="Equation 3" src="/files/ftp_upload/59618/59618eq3g.jpg" /> where <img align="center" alt="Equation 4" src="/files/ftp_upload/59618/59618eq4g.jpg" />. As per the signal in Figure 1, <img align="center" alt="Equation 5" src="/files/ftp_upload/59618/59618eq5g.jpg" /> happens to be a satisfactory and practicable linear region.</li>
	<li>As illustrated in Figure 2, fit the straight-line model <img align="center" alt="Equation 6" src="/files/ftp_upload/59618/59618eq6g.jpg" /> to the experimental signal data within the identified linear region and estimate the value of &#946;.</li>
</ol>
2. Quantification of relative thickness
<ol>
	<li>Suppose there are multiple signals (Figure 3) acquired from an NDE task performed on a conductive ferromagnetic test piece having varying thickness. First, identify a linear region common to all signals and extract &#946; values. As per the signals in Figure 3, <img align="center" alt="Equation 8" src="/files/ftp_upload/59618/59618eq8g.jpg" /> seems to be an adequate and practicable linear region.</li>
	<li>Select the maximum &#946; value and label it as &#946;ref since the maximum &#946; value should in principle correspond to the maximum thickness according to the &#946; <img align="center" alt="Equation 7" src="/files/ftp_upload/59618/59618eq7a.jpg" /> &#956;&#963;d2 proportionality6,7,8.</li>
	<li>Express relative thickness percentage in the form <img align="center" alt="Equation 9" src="/files/ftp_upload/59618/59618eq9g.jpg" />, where the index <img align="center" alt="Equation 10" src="/files/ftp_upload/59618/59618eq10g.jpg" /> corresponds to the <img align="center" src="/files/ftp_upload/59618/59618eq11d.jpg" />th measurement.</li>
</ol>
3. PEC_Signal_Processor installation
<ol>
	<li>Locate the file PEC_Signal_Processor.exe. Double click the file and allow to execute.</li>
	<li>When the interface below appears, click Next. When the interface pops up, specify the file location for installation, and tick the checkbox Add a shortcut to the desktop to add the software icon to the desktop. Then click Next.</li>
	<li>Specify the installation location for the required Runtime Environment, then click Next. If the required Runtime Environment is already installed, just click Next.</li>
	<li>Read, and agree to prompted license terms and conditions. Then click Install.</li>
	<li>Click Finish when installation is complete. The desktop icon will appear.</li>
</ol>
4. Preparation of signals
<ol>
	<li>Ensure the PEC sensor outputs [raw signals, i.e., V(t)] are arranged as a table.</li>
	<li>Copy the table containing signals to the desktop (or to a folder contained within the parent directory where the application is installed). For convenience, the desktop is recommended.</li>
</ol>
5. Executing the application
<ol>
	<li>Double click the desktop icon to run the application. The interface will open.</li>
	<li>Load signals by clicking on the Load Signals tab and select the file containing the signals in order to import the signals to the software interface.</li>
	<li>Wait until the number of signals which is contained within the table containing raw signals appear in front of Number of Signals =.</li>
	<li>Click on Plot Signals and observe the signals plotted in logarithmic scale.</li>
	<li>Click on the Zoom tab and adjust the plot window for the linear region to be clearly visible.</li>
	<li>After observation, decide on reasonable lower and upper margins for the linear region and enter the values in the editable text spaces.</li>
	<li>Click on Plot Margins and wait for the margins to be plotted in green.</li>
	<li>Click on Extract Features and observe how straight-line segments are plotted in red.</li>
	<li>Click on Calculate Relative Thickness and observe how a histogram of calculated relative thickness values is plotted.</li>
	<li>Click on Save Relative Thickness to save the calculated relative thickness values. Provide a filename and click OK.</li>
	<li>Confirm filename by clicking OK again to confirm the filename. The relative thickness values will be saved as a table on the desktop.</li>
</ol>

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Authors have no conflicts of interest to disclose. Authors would like to recommend works2,6,7,8,9,10,11 as additional reading material.

A protocol to quantify the relative thickness (i.e., thickness as a percentage with respect to a reference) of conductive ferromagnetic materials using detector coil-based PEC sensors was presented. The main advantage of this method is the ability to overcome the calibration requirement (i.e., overcome the need to measure or estimate the magnetic permeability and electrical conductivity of the material being inspected to enable thickness quantification). The protocol involves logarithmic representation of the time domain...

The pulsed eddy current (PEC) sensing technique is perhaps the most versatile member of the family of eddy current (EC) non-destructive evaluation (NDE) techniques and has many applications in detection and quantification of defects, and the geometry of metals and metallic structures1. Thickness quantification of conductive ferromagnetic wall-like structures, having wall thicknesses of no more than a few millimeters to a few tens of millimeters, is a high demand engineering service in the field of structural health monitoring of infrastructure. Critical infrastructure made of ferromagnetic alloys that require this service are commonly available in the energy, water, oil, and gas industries. While PEC sensors can be designed following several architectures, the detector coil-based architecture was determined to be the most effective and commonly used in condition assessment of ferromagnetic materials2,3,4,5. Therefore, it is the detector coil-based PEC sensor architecture that sets the foundation to the problem of thickness quantification of conductive ferromagnetic materials.
The detector coil-based PEC sensor architecture is typically comprised of two concentrically wound, air cored, conductive coils2,3,4,5,6 (typically copper coils). It is quite common to wind these coils to be circular in shape2,3,4,5,6, but occasionally, rectangular shaped coils6 have been used. From the two coils in the sensor, one behaves as an exciter coil while the other acts as the detector coil. In a PEC sensor, the exciter coil is excited by a voltage pulse - something that can be characterized as a Heaviside step function in principle. This pulsed excitation generates a transient magnetic field (called the primary field) around the sensor. When the sensor is placed adjacent to a conductive test piece (e.g., a conductive ferromagnetic wall-like structure), this transient magnetic field induces time varying eddy currents in the test piece. These eddy currents generate a secondary magnetic field (called the secondary field) that opposes the primary field. In response to the resultant effect of the primary and secondary fields, a transient voltage is induced in the detector coil - which becomes the time domain PEC signal of interest for this work.
The PEC sensor detector coil voltage decay rate (denoted as &#946;) has been reported6,7,8 to show the proportionality &#946; <img align="center" alt="Equation 7" src="/files/ftp_upload/59618/59618eq7a.jpg" /> &#956;&#963;d2, when a signal is acquired placing a PEC sensor above a conductive ferromagnetic layer of magnetic permeability &#956;, electrical conductivity &#963;, and thickness d. Although this decay rate signal feature has considerable immunity to parameters such as sensor size, sensor shape, and lift-off6,7,8, which makes the decay rate highly desirable for challenging NDE scenarios such as in situ pipe condition assessment9,10,11, this feature must be calibrated (i.e., &#956;, &#963; of the material being inspected be estimated) to enable thickness (i.e., d) quantification. To enable conventional methods of decay rate-based thickness quantification6,8, this calibration must be done by extracting calibration samples6,8 or by involving eddy current-based material property characterization methods12,13. Alternatively, the complexity of calibration can be avoided by representing thickness in the form of relative thickness. Suppose an NDE exercise is carried out and &#946; values are extracted from signals, then, the &#946; value qualitatively representative of the maximum thickness point in the test piece is considered as a reference (i.e., &#946;ref <img align="center" alt="Equation 7" src="/files/ftp_upload/59618/59618eq7a.jpg" /> &#956;&#963;dmax2); then, the thickness of any other location can be represented as a percentage of the maximum thickness in the form <img align="center" alt="Equation 1" src="/files/ftp_upload/59618/59618eq1g.jpg" />, presenting a relative thickness as the output, which is still useful qualitative information as an NDE output that also carries the simplicity of not having to calibrate for &#956;, &#963;. The protocol presented herein describes the steps to be followed to accomplish this.
Since the decay rate &#946; shows generality to the detector coil-based PEC sensor architecture while showing immunity to parameters of the sensor design as well as lift-off6,7,8,14, practitioners may use any detector coil-based PEC sensing system of their choice on a suitable conductive ferromagnetic material to perform relative thickness quantification following the protocol here. A PEC sensor design example for a conductive ferromagnetic material is available for interested readers15. The signals and results presented in this work were acquired using the PEC system developed by University of Technology Sydney6,8. The conductive ferromagnetic material used for representative results acquired by the PEC system is grey cast iron extracted from a pipe test-bed9,10,11 in Sydney Australia.
It should be noted that the methods, results, and discussions presented in this publication explicitly focus on the use of the detector coil-based PEC sensor architecture&#39;s time domain signal&#39;s decay rate for thickness quantification of conductive ferromagnetic materials. The publication does not include a broader discussion on general conventions of PEC sensing principles and sensor configurations. Other published work16,17,18 can be useful for readers to gain more insight about PEC sensor configurations other than the detector coil-based sensor architecture.

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>A Detector Coil-based PEC Sensing System.</td>
			<td>N/A</td>
			<td></td>
			<td>The representative results in this work were generated using the PEC system developed by University of Technology Sydney (UTS), Australia and published in works 6,8. This system may be accessible to readers via collaborating with UTS.</td>
		</tr>
		<tr>
			<td>A suitable conductive ferromagnetic material of varying thickness.</td>
			<td>N/A</td>
			<td></td>
			<td>The representative results in this work were generated by acquiring PEC measurements on grey cast iron test pieces extracted from a pipe test-bed located in Sydney Australia, whose location and vintage details are available in references 9-11. The pipe test-bed as well as the extracted calibration samples may be accessible to readers via collaborating with UTS.</td>
		</tr>
		<tr>
			<td>A computation platform for PEC signal processing</td>
			<td>MathWorks, Natick, MA, USA.</td>
			<td></td>
			<td>A computation platform in which the PEC signal processing algorithm can be coded and executed is required. In this publication, PEC signal processing was done using a software executable named &#34;PEC_Signal_Processor&#34;, produced using MATLAB R2017b, Publisher: MathWorks, Natick, MA, USA.</td>
		</tr>
		<tr>
			<td>An application that can produce a table containing raw PEC signals (e.g., Microsoft Office Excel).</td>
			<td>Microsoft Corporation, One Microsoft Way, Redmond, Washington, USA.</td>
			<td></td>
			<td>Microsoft Office Excel (Office 16) was used for the work of this publication.</td>
		</tr>
	</tbody>
</table>

quantifying the relative thickness of conductive ferromagnetic materials using detector coil-based pulsed eddy current sensors

Thickness quantification of conductive ferromagnetic materials by means of non-destructive evaluation (NDE) is a crucial component of structural health monitoring of infrastructure, especially for assessing the condition of large diameter conductive ferromagnetic pipes found in the energy, water, oil, and gas sectors. Pulsed eddy current (PEC) sensing, especially detector coil-based PEC sensor architecture, has established itself over the years as an effective means for serving this purpose. Approaches for designing PEC sensors as well as processing signals have been presented in previous works. In recent years, the use of the decay rate of the detector coil-based time domain PEC signal for the purpose of thickness quantification has been studied. Such works have established that the decay rate-based method holds generality to the detector coil-based sensor architecture, with a degree of immunity to factors such as sensor shape and size, number of coil turns, and excitation current. Moreover, this method has shown its effectiveness in NDE of large pipes made of grey cast iron. Following such literature, the focus of this work is explicitly PEC sensor detector coil voltage decay rate-based conductive ferromagnetic material thickness quantification. However, the challenge faced by this method is the difficulty of calibration, especially when it comes to applications such as in situ pipe condition assessment since measuring electrical and magnetic properties of certain pipe materials or obtaining calibration samples is difficult in practice. Motivated by that challenge, in contrast to estimating actual thickness as done by some previous works, this work presents a protocol for using the decay rate-based method to quantify relative thickness (i.e., thickness of a particular location with respect to a maximum thickness), without the requirement for calibration.

Representative results within this section have been generated using the PEC signals provided as supplementary material with reference8; as mentioned above, the signals have been captured on grey cast iron samples extracted from the pipe test bed in Sydney Australia, whose location and vintage details are provided in references9,10,11.
Figure 1 sho...

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Quantifying the Relative Thickness of Conductive Ferromagnetic Materials Using Detector Coil-Based Pulsed Eddy Current Sensors

Here, we present a protocol to quantify the relative thickness (i.e., thickness as a percentage with respect to a reference) of conductive ferromagnetic materials using detector coil-based pulsed eddy current sensors, while overcoming the calibration requirement.

Thickness quantification of conductive ferromagnetic materials by means of non-destructive evaluation (NDE) is a crucial component of structural health ...

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5.6K Views.  University of Melbourne. Here, we present a protocol to quantify the relative thickness (i.e., thickness as a percentage with respect to a reference) of conductive ferromagnetic materials using detector coil-based pulsed eddy current sensors, while overcoming the calibration requirement.

Video: Quantifying the Relative Thickness of Conductive Ferromagnetic Materials Using Detector Coil-Based Pulsed Eddy Current Sensors

Fabrication of Nano-engineered Transparent Conducting Oxides by Pulsed Laser Deposition

Nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas allows the deposition of metal oxides with tunable morphology, structure, density and stoichiometry by a proper control of the plasma plume expansion dynamics. Such versatility can be exploited to produce nanostructured films from compact and dense to nanoporous characterized by a hierarchical assembly of nano-sized clusters. In particular we describe the detailed methodology to fabricate two types of Al-doped ZnO (AZO) films as transparent electrodes in photovoltaic devices: 1) at low O2 pressure, compact films with electrical conductivity and optical transparency close to the state of the art transparent conducting oxides (TCO) can be deposited at room temperature, to be compatible with thermally sensitive materials such as polymers used in organic photovoltaics (OPVs); 2) highly light scattering hierarchical structures resembling a forest of nano-trees are produced at higher pressures. Such structures show high Haze factor (&gt;80%) and may be exploited to enhance the light trapping capability. The method here described for AZO films can be applied to other metal oxides relevant for technological applications such as TiO2, Al2O3, WO3 and Ag4O4.

We describe the experimental method to deposit nanostructured oxide thin films by nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas. By using this method Al-doped ZnO (AZO) films, from compact to hierarchically structured as nano-tree forests, can be deposited.

Nanosecond Pulsed  Laser Deposition (PLD) in the presence of a background gas allows the deposition  of metal oxides with tunable morphology, structure, ...

Using Neutron Spin Echo Resolved Grazing Incidence Scattering to Investigate Organic Solar Cell Materials

The spin echo resolved grazing incidence scattering (SERGIS) technique has been used to probe the length-scales associated with irregularly shaped crystallites. Neutrons are passed through two well defined regions of magnetic field; one before and one after the sample. The two magnetic field regions have opposite polarity and are tuned such that neutrons travelling through both regions, without being perturbed, will undergo the same number of precessions in opposing directions. In this case the neutron precession in the second arm is said to &#34;echo&#34; the first, and the original polarization of the beam is preserved. If the neutron interacts with a sample and scatters elastically the path through the second arm is not the same as the first and the original polarization is not recovered. Depolarization of the neutron beam is a highly sensitive probe at very small angles (&#60;50&#160;&#956;rad) but still allows a high intensity, divergent beam to be used. The decrease in polarization of the beam reflected from the sample as compared to that from the reference sample can be directly related to structure within the sample.
In comparison to scattering observed in neutron reflection measurements the SERGIS signals are often weak and are unlikely to be observed if the in-plane structures within the sample under investigation are dilute, disordered, small in size and polydisperse or the neutron scattering contrast is low. Therefore, good results will most likely be obtained using the SERGIS technique if the sample being measured consist of thin films on a flat substrate and contain scattering features that contains a high density of moderately sized features (30 nm to 5 &#181;m) which scatter neutrons strongly or the features are arranged on a lattice. An advantage of the SERGIS technique is that it can probe structures in the plane of the sample.

Progress has been made in utilizing spin echo resolved grazing incidence scattering (SERGIS) as a neutron scattering technique to probe the length-scales in irregular samples. Crystallites of [6,6]-phenyl-C61-butyric acid methyl ester have been probed using the SERGIS technique and the results confirmed by optical and atomic force microscopy.

The spin echo resolved grazing incidence scattering (SERGIS) technique has been used to probe the length-scales associated with irregularly shaped ...

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and reduction half reactions, and fast electron (hole) diffusion and charge separation. Nanowires present suitable architectures to meet these requirements. Axially segmented Ag|ZnO and radially segmented (coaxial) TiO2-Ag nanowires with a diameter of 200 nm and a length of 6-20 &#181;m were made by templated electrodeposition within the pores of polycarbonate track-etched (PCTE) or anodized aluminum oxide (AAO) membranes, respectively. In the photocatalytic experiments, the ZnO and TiO2 phases acted as photoanodes, and Ag as cathode. No external circuit is needed to connect both electrodes, which is a key advantage over conventional photo-electrochemical cells. For making segmented Ag|ZnO nanowires, the Ag salt electrolyte was replaced after formation of the Ag segment to form a ZnO segment attached to the Ag segment. For making coaxial TiO2-Ag nanowires, a TiO2 gel was first formed by the electrochemically induced sol-gel method. Drying and thermal annealing of the as-formed TiO2 gel resulted in the formation of crystalline TiO2 nanotubes. A subsequent Ag electrodeposition step inside the TiO2 nanotubes resulted in formation of coaxial TiO2-Ag nanowires. Due to the combination of an n-type semiconductor (ZnO or TiO2) and a metal (Ag) within the same nanowire, a Schottky barrier was created at the interface between the phases. To demonstrate the photocatalytic activity of these nanowires, the Ag|ZnO nanowires were used in a photocatalytic experiment in which H2 gas was detected upon UV illumination of the nanowires dispersed in a methanol/water mixture. After 17 min&#160;of illumination, approximately 0.2 vol% H2 gas was detected from a suspension of ~0.1 g of Ag|ZnO nanowires in a 50 ml 80 vol% aqueous methanol solution.

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Procedures are outlined to prepare segmented and coaxial nanowires via templated electrodeposition in nanopores. As examples, segmented nanowires consisting of Ag and ZnO segments, and coaxial nanowires consisting of a TiO2 shell and a Ag core were made. The nanowires were used in photocatalytic hydrogen formation experiments.

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and ...

Using Microwave and Macroscopic Samples of Dielectric Solids to Study the Photonic Properties of Disordered Photonic Bandgap Materials

Recently, disordered photonic materials have been suggested as an alternative to periodic crystals for the formation of a complete photonic bandgap (PBG). In this article we will describe the methods for constructing and characterizing macroscopic disordered photonic structures using microwaves. The microwave regime offers the most convenient experimental sample size to build and test PBG media. Easily manipulated dielectric lattice components extend flexibility in building various 2D structures on top of pre-printed plastic templates. Once built, the structures could be quickly modified with point and line defects to make freeform waveguides and filters. Testing is done using a widely available Vector Network Analyzer and pairs of microwave horn antennas. Due to the scale invariance property of electromagnetic fields, the results we obtained in the microwave region can be directly applied to infrared and optical regions. Our approach is simple but delivers exciting new insight into the nature of light and disordered matter interaction.

Our representative results include the first experimental demonstration of the existence of a complete and isotropic PBG in a two-dimensional (2D) hyperuniform disordered dielectric structure. Additionally we demonstrate experimentally the ability of this novel photonic structure to guide electromagnetic waves (EM) through freeform waveguides of arbitrary shape.

Disordered structures offer new mechanisms for forming photonic bandgaps and unprecedented freedom in functional-defect designs. To circumvent the computational challenges of disordered systems, we construct modular macroscopic samples of the new class of PBG materials and use microwaves to characterize their scale-invariant photonic properties, in an easy and inexpensive manner.

Recently, disordered photonic materials have been suggested as an alternative to periodic crystals for the formation of a complete photonic bandgap (PBG). ...

Formation of Thick Dense Yttrium Iron Garnet Films Using Aerosol Deposition

Aerosol deposition (AD) is a thick-film deposition process that can produce layers up to several hundred micrometers thick with densities greater than 95% of the bulk. The primary advantage of AD is that the deposition takes place entirely at ambient temperature; thereby enabling film growth in material systems with disparate melting temperatures. This report describes in detail the processing steps for preparing the powder and for performing AD using the custom-built system. Representative characterization results are presented from scanning electron microscopy, profilometry, and ferromagnetic resonance for films grown in this system. As a representative overview of the capabilities of the system, focus is given to a sample produced following the described protocol and system setup. Results indicate that this system can successfully deposit 11 &#181;m thick yttrium iron garnet films that are &#160;&#62; 90% of the bulk density during a single 5 min deposition run. A discussion of methods to afford better control of the aerosol and particle selection for improved thickness and roughness variations in the film is provided.

This report describes the use of a custom-built system to perform aerosol deposition of thick films of yttrium iron garnet onto sapphire substrates at RT. The deposited films are characterized using scanning electron microscopy, profilometry, and ferromagnetic resonance to give a representative overview of the capabilities of the technique.

Aerosol deposition (AD) is a thick-film deposition process that can produce layers up to several hundred micrometers thick with densities greater than 95% ...

Detection and Recovery of Palladium, Gold and Cobalt Metals from the Urban Mine Using Novel Sensors/Adsorbents Designated with Nanoscale Wagon-wheel-shaped Pores

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in industrialized countries. Here, the development of optical mesosensors/adsorbents (MSAs) for efficient recognition and selective recovery of Pd(II), Au(III), and Co(II) from urban mine was achieved. A simple, general method for preparing MSAs based on using high-order mesoporous monolithic scaffolds was described. Hierarchical cubic Ia3d wagon-wheel-shaped MSAs were fabricated by anchoring chelating agents (colorants) into three-dimensional pores and micrometric particle surfaces of the mesoporous monolithic scaffolds. Findings show, for the first time, evidence of controlled optical recognition of Pd(II), Au(III), and Co(II) ions and a highly selective system for recovery of Pd(II) ions (up to ~95%) in ores and industrial wastes. Furthermore, the controlled assessment processes described herein involve evaluation of intrinsic properties (e.g., visual signal change, long-term stability, adsorption efficiency, extraordinary sensitivity, selectivity, and reusability); thus, expensive, sophisticated instruments are not required. Results show evidence that MSAs will attract worldwide attention as a promising technological means of recovering and recycling palladium, gold and cobalt metals.

Because of the importance and extensive use of palladium, gold and cobalt metals in high-technology equipment, their recovery and recycling constitute an important industrial challenge. The metal recovery system described herein is a simple, low-cost means for the effective detection, removal, and recovery of these metals from the urban mine.

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in ...

Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis

Nuclear reaction analysis (NRA) via the resonant 1H(15N,&#945;&#947;)12C reaction is a highly effective method of depth profiling that quantitatively and non-destructively reveals the hydrogen density distribution at surfaces, at interfaces, and in the volume of solid materials with high depth resolution. The technique applies a 15N ion beam of 6.385 MeV provided by an electrostatic accelerator and specifically detects the 1H isotope in depths up to about 2 &#956;m from the target surface. Surface H coverages are measured with a sensitivity in the order of ~1013 cm-2 (~1% of a typical atomic monolayer density) and H volume concentrations with a detection limit of ~1018 cm-3 (~100 at. ppm). The near-surface depth resolution is 2-5 nm for surface-normal 15N ion incidence onto the target and can be enhanced to values below 1 nm for very flat targets by adopting a surface-grazing incidence geometry. The method is versatile and readily applied to any high vacuum compatible homogeneous material with a smooth surface (no pores). Electrically conductive targets usually tolerate the ion beam irradiation with negligible degradation. Hydrogen quantitation and correct depth analysis require knowledge of the elementary composition (besides hydrogen) and mass density of the target material. Especially in combination with ultra-high vacuum methods for in-situ target preparation and characterization, 1H(15N,&#945;&#947;)12C NRA is ideally suited for hydrogen analysis at atomically controlled surfaces and nanostructured interfaces. We exemplarily demonstrate here the application of 15N NRA at the MALT Tandem accelerator facility of the University of Tokyo to (1) quantitatively measure the surface coverage and the bulk concentration of hydrogen in the near-surface region of a H2 exposed Pd(110) single crystal, and (2) to determine the depth location and layer density of hydrogen near the interfaces of thin SiO2 films on Si(100).

We illustrate the application of 1H(15N,&#945;&#947;)12C resonant nuclear reaction analysis (NRA) to quantitatively evaluate the density of hydrogen atoms on the surface, in the volume, and at an interfacial layer of solid materials. The near-surface hydrogen depth profiling of a Pd(110) single crystal and of SiO2/Si(100) stacks is described.

Nuclear reaction analysis (NRA) via the resonant 1H(15N,&#945;&#947;)12C reaction is a highly effective method of depth profiling that quantitatively and ...

Characterization of Full Set Material Constants and Their Temperature Dependence for Piezoelectric Materials Using Resonant Ultrasound Spectroscopy

During the operation of high power electromechanical devices, a temperature rise is unavoidable due to mechanical and electrical losses, causing the degradation of device performance. In order to evaluate such degradations using computer simulations, full matrix material properties at elevated temperatures are needed as inputs. It is extremely difficult to measure such data for ferroelectric materials due to their strong anisotropic nature and property variation among samples of different geometries. Because the degree of depolarization is boundary condition dependent, data obtained by the IEEE (Institute of Electrical and Electronics Engineers) impedance resonance technique, which requires several samples with drastically different geometries, usually lack self-consistency. The resonant ultrasound spectroscopy (RUS) technique allows the full set material constants to be measured using only one sample, which can eliminate errors caused by sample to sample variation. A detailed RUS procedure is demonstrated here using a lead zirconate titanate (PZT-4) piezoceramic sample. In the example, the complete set of material constants was measured from room temperature to 120 &#176;C. Measured free dielectric constants <img alt="Equation 1" src="/files/ftp_upload/53461/image001.jpg" /> and&#160;<img alt="Equation 2" src="/files/ftp_upload/53461/image002.jpg" /> were compared with calculated ones based on the measured full set data, and piezoelectric constants d15 and d33 were also calculated using different formulas. Excellent agreement was found in the entire range of temperatures, which confirmed the self-consistency of the data set obtained by the RUS.

This protocol describes the procedure of measuring the temperature dependence of the full set material constants of piezoelectric materials using resonant ultrasound spectroscopy (RUS).

During the operation of high power electromechanical devices, a temperature rise is unavoidable due to mechanical and electrical losses, causing the ...

Electrospray Deposition of Uniform Thickness Ge23Sb7S70 and As40S60 Chalcogenide Glass Films

Solution-based electrospray film deposition, which is compatible with continuous, roll-to-roll processing, is applied to chalcogenide glasses. Two chalcogenide compositions are demonstrated: Ge23Sb7S70 and As40S60, which have both been studied extensively for planar mid-infrared (mid-IR) microphotonic devices. In this approach, uniform thickness films are fabricated through the use of computer numerical controlled (CNC) motion. Chalcogenide glass (ChG) is written over the substrate by a single nozzle along a serpentine path. Films were subjected to a series of heat treatments between 100 &#176;C and 200 &#176;C under vacuum to drive off residual solvent and densify the films. Based on transmission Fourier transform infrared (FTIR) spectroscopy and surface roughness measurements, both compositions were found to be suitable for the fabrication of planar devices operating in the mid-IR region. Residual solvent removal was found to be much quicker for the As40S60 film as compared to Ge23Sb7S70. Based on the advantages of electrospray, direct printing of a gradient refractive index (GRIN) mid-IR transparent coating is envisioned, given the difference in refractive index of the two compositions in this study.

Electrospray Deposition of Uniform Thickness Ge23Sb7S70 and As40S60 Chalcogenide Glass Films

A method of uniform thickness solution-derived chalcogenide glass film deposition is demonstrated using computer numerical controlled motion of a single-nozzle electrospray.

Solution-based electrospray film deposition, which is compatible with continuous, roll-to-roll processing, is applied to chalcogenide glasses. Two ...

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

This paper provides a detailed method to characterize the microstructure of ultra-fine grained and nanocrystalline materials using a scanning electron microscope equipped with a standard electron backscatter diffraction system. Metal alloys and minerals presenting refined microstructures are analyzed using this technique, showing the diversity of its possible applications.