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DOE OSTI2014

Ultrasound guided fluorescence molecular tomography with improved quantification by an attenuation compensated born-normalization and in vivo preclinical study of cancer

Ultrasound imaging, having the advantages of low-cost and non-invasiveness over MRI and X-ray CT, was reported by several studies as an adequate complement to fluorescence molecular tomography with the perspective of improving localization and quantification of fluorescent molecular targets in vivo. Based on the previous work, an improved dual-modality Fluorescence-Ultrasound imaging system was developed and then validated in imaging study with preclinical tumor model. Ultrasound imaging and a profilometer were used to obtain the anatomical prior information and 3D surface, separately, to precisely extract the tissue boundary on both sides of sample in order to achieve improved fluorescence reconstruction. Furthermore, a pattern-based fluorescence reconstruction on the detection side was incorporated to enable dimensional reduction of the dataset while keeping the useful information for reconstruction. Due to its putative role in the current imaging geometry and the chosen reconstruction technique, we developed an attenuation compensated Born-normalization method to reduce the attenuation effects and cancel off experimental factors when collecting quantitative fluorescence datasets over large area. Results of both simulation and phantom study demonstrated that fluorescent targets could be recovered accurately and quantitatively using this reconstruction mechanism. Finally, in vivo experiment confirms that the imaging system associated with the proposed image reconstruction approach was able to extract both functional and anatomical information, thereby improving quantification and localization of molecular targets.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2019

Optimization of the size and shape of the scanning aperture in autocollimator-based deflectometric profilometers

Deflectometric profilometers based on industrial electronic autocollimators (ACs), as the ELCOMAT-3000, have become indispensable tools for precision form measurements of optical surfaces. A growing number of labs at synchrotron and free electron laser x-ray facilities are going for BESSY-II NOM-like versions of the AC-based profilometers. These tools have proven capable of characterizing state-of-the-art aspherical x-ray optics with an accuracy on the level of 100 nrad (root-mean-square) over the spatial frequency range limited by the size of the aperture used in the profilometer. Normally, a round aperture with a diameter of about 2.5 mm is used. Previous investigations have shown that with the optimally aligned 2.5-mm aperture, the spatial resolution of a NOM-like profilometer corresponding to the first zero-crossing of the optical transform function (OTF) is ~1.2 mm. In this paper, we investigate the performance of an AC ELCOMAT-3000 for a slope profilometer with different aperture sizes and shapes. The results of angular calibration of the AC equipped with circular and rectangular apertures placed at different distances from the AC are discussed. The calibration was performed at the Physikalisch-Technische Bundesanstalt using the original experimental arrangements, also discussed in the paper. The OTF measurements with the specially developed test sample with chirped surface slope profiles were performed at the Advanced Light Source X-Ray Optics Laboratory (XROL) in application to a new optical surface measuring system under development at the XROL. In the OTF measurements, we have shown that application of a rectangular aperture with dimensions of 1.5 mm × 3 mm improves the spatial resolution in the tangential direction by a factor of ~1.4 compared to that of the standard circular aperture of 2.5-mm diameter. We postulate that the conclusions of our investigations are crucial for reaching fundamental metrological limits in deflectometric profilometry utilizing state-of-the-art electronic autocollimators.

47 OTHER INSTRUMENTATION↗

DOE OSTI2016

Solvent effect on polystyrene surface roughness on top of QCM sensor

Quartz Crystal Microbalance (QCM) has been used as a basis for many chemical sensors and biosensor. Its sensitivity to mass change which can detect a mass change on its surface down to sub ng/cm2 is one of its interesting aspects. Another interesting feature is its ability to work in liquid environment. However, there are many aspects which influence QCM sensor properties in contact with liquid. One of the aspects is surface roughness of the matrix layer where on top of it a biological sensitive layer will be immobilized. One of matrix layers in the immobilizing biological sensitive layer was polystyrene. Polystyrene was coated on the QCM sensor by using the spin coating method. During the coating process, polystyrene was solved using non-polar solvent. It is known that the physical and chemical properties of the solvent affect a transition process from soluble polymer becoming rigid polymer layer. In this work, we show that polystyrene solved in chloroform has a higher surface roughness compare to one solved in toluene, xylene, or tetrahydrofuran. Surface roughness of the polystyrene coating were measured using a non-contact profilometer. However, we also found that there is no difference on the electrical impedance of the QCM sensor coated with polystyrene resulted from differing solvent when the sensor was in contact with air and water. Thus, all of the mentioned solvent can be used to solve the polystyrene as a coating material for QCM sensor without affecting the electrical performance of the sensor, but the choice of the solution can be used as a simple method to control the difference roughness of the polystyrene coating.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Comparative In Vitro Evaluation Between Zirconia and Veneer Ceramic Materials Using Different Techniques

Zirconia surface treatment using different techniques could be employed to overcome the delamination issue reported between veneering ceramic materials and the corresponding zirconia core. The study subjected yttria partially stabilized zirconia core material to grinding and sandblasting as a first surface treatment. An airbrush gun spraying technique was used to coat a uniform thin layer of veneering ceramic (IPS e.max Ceram and Noritake Cerabien ZR) on the core materials followed by performing laser scanning as a second surface treatment. The specimens were investigated for surface topography, interface analysis, elemental compositions, phase transformation, and fracture mode patterns using profilometer, SEM, EDS, XRD, and stereomicroscope. The impact of laser scanning on the shear bond strength before and after storage of specimens in artificial saliva was also studied. Transformable tetragonal phase to monoclinic was predominant in sandblasted specimens followed by laser scanning with observation of micro-cracks at interface. The grinding followed by laser scanning yielded satisfactory outcomes in terms of the presence of coating property. The phase transformation was not detected through the latter technique. The technique greatly enhanced the roughness property and bond strength values which might be considered as a reliable application to improve the longevity of fixed dental crowns in load bearing areas.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Pulsed laser deposition to synthesize the bridge structure of artificial nacre: Comparison of nano- and femtosecond lasers

Nature offers inspiration to new adaptive technologies that allow us to build amazing shapes and structures such as nacre using synthetic materials. Consequently, we have designed a pulsed laser ablation manufacturing process involving thin film deposition and micro-machining to create hard/soft layered 'brick-bridge-mortar' nacre of AlMgB{sub 14} (hard phase) with Ti (soft phase). In this paper, we report pulsed laser deposition (PLD) to mimic brick and bridge structures of natural nacre in AlMgB{sub 14}. Particulate formation inherent in PLD is exploited to develop the bridge structure. Mechanical behavior analysis of the AlMgB{sub 14}/Ti system revealed that the brick is to be 250 nm thick, 9 {mu}m lateral dimensions while the bridge (particle) is to have a diameter of 500 nm for a performance equivalent to natural nacre. Both nanosecond (ns) and femtosecond (fs) pulsed lasers were employed for PLD in an iterative approach that involves varying pulse energy, pulse repetition rate, and target-to-substrate distance to achieve the desired brick and bridge characteristics. Scanning electron microscopy, x-ray photoelectron spectroscopy, and optical profilometer were used to evaluate the film thickness, particle size and density, stoichiometry, and surface roughness of thin films. Results indicated that both ns-pulsed and fs-pulsed lasers produce the desired nacre features. However, each laser may be chosen for different reasons: fs-pulsed laser is preferred for much shorter deposition time, better stoichiometry, uniform-sized particles, and uniform film thickness, while ns-pulsed laser is favored for industrial acceptance, reliability, ease of handling, and low cost.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

Dendrite-free Al recycling via electrodeposition using ionic liquid electrolytes: The effects of deposition temperature and cathode surface roughness

In this report, the electrodeposition of Al from aluminum scrap alloys (A2020) on copper cathode substrates with varied surface roughness under different deposition temperatures was studied using low-temperature AlCl 3 -1-butyl-3-methyl-imidazolium chloride (BMIC) ionic liquid electrolytes. The bulk electrodeposition of Al was carried out under a voltage of 1.5 V at a stirring rate of 120 rpm using a fixed ionic liquid electrolyte concentration (molar ratio AlCl 3 : BMIC = 2:1). The effects of deposition temperature (range from 80 °C to 140 °C) and surface roughness of Cu cathode substrates (polished by 320, 600, 800, 1200 grits SiC sandpapers and mirror polishing process) on the morphology of deposited Al, current density, current efficiency and energy consumption, were investigated. The Al deposits were characterized using scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), profilometer, and electrochemical measurements for current density, current efficiency, and energy consumption. It is demonstrated that the deposition temperature and surface roughness of Cu electrodes play a critical role in the nucleation and growth of Al deposits. Higher deposition temperature promotes the diffusion and/or migration of Al 2 Cl 7 - ions and then enhances the current density and efficiency during the electrodeposition of Al. Smoother surface of Cu electrodes is preferred for the formation of dendrite-free Al deposits. Typically, on the mirror polished Cu electrode, no Al dendrite structure was observed, and only plate-like Al deposits were formed at the deposition temperature of 100 °C. Pure metallic Al was successfully deposited on Cu electrodes in AlCl 3 + BMIC ionic liquid electrolytes for all experiments with a current efficiency range from 72% to 99% and energy consumption of 4.6–6.3 kW h/kg Al.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2021

A digital holography ex situ measurement characterization of plasma-exposed surface erosion from an electrothermal arc source

Digital holography has been proposed to fulfill a need for an imaging diagnostic capable of in situ monitoring of surface erosion caused by plasma–material interaction in nuclear fusion devices. A digital holography diagnostic for 3D surface erosion measurement has been developed at Oak Ridge National Laboratory with the goal of deployment on a plasma device. A proof-of-concept in situ demonstration is planned which would involve measurement of plasma erosion on targets exposed to an electrothermal arc source. This work presents the results of an ex situ characterization of the capability and limitations of holographic imaging of targets exposed to the arc source. Targets were designed to provide a fiducial for comparison of deformed and unaffected areas. The results indicated that the average net erosion was ~150 nm/plasma exposure, which is expected to be within the diagnostic’s measurement capacity. Surface roughness averages determined by holographic image analysis showed good agreement with measurements taken with a profilometer. Finally, the limit of the holography diagnostic’s x–y spatial resolution was characterized by comparison with scanning electron microscope imaging.

47 OTHER INSTRUMENTATION↗

DOE OSTI2016

Development of a mobile toolmark characterization/comparison system [Development of a mobile, automated toolmark characterization/comparison system]

Since the development of the striagraph, various attempts have been made to enhance forensic investigation through the use of measuring and imaging equipment. This study describes the development of a prototype system employing an easy-to-use software interface designed to provide forensic examiners with the ability to measure topography of a toolmarked surface and then conduct various comparisons using a statistical algorithm. Acquisition of the data is carried out using a portable 3D optical profilometer, and comparison of the resulting data files is made using software named “MANTIS” (Mark and Tool Inspection Suite). The system has been tested on laboratory-produced markings that include fully striated marks (e.g., screwdriver markings), quasistriated markings produced by shear-cut pliers, impression marks left by chisels, rifling marks on bullets, and cut marks produced by knives. Using the system, an examiner has the potential to (i) visually compare two toolmarked surfaces in a manner similar to a comparison microscope and (ii) use the quantitative information embedded within the acquired data to obtain an objective statistical comparison of the data files. Finally, this study shows that, based on the results from laboratory samples, the system has great potential for aiding examiners in conducting comparisons of toolmarks.

47 OTHER INSTRUMENTATION↗

DOE OSTI2015

Formation of conductive copper lines by femtosecond laser irradiation of copper nitride film on plastic substrates

In this paper, we report a simple method to form conductive copper lines by scanning a single-beam femtosecond pulse laser on a plastic substrate covered with copper nitride (Cu{sub 3}N) film. The Cu{sub 3}N films were prepared by DC magnetron sputtering in the presence of an Ar + N{sub 2} atmosphere at 100 °C. The influence of the laser power and scanning speed on the formed copper line width, surface features, and morphology was analyzed by means of optical microscopy, X-ray diffraction, non-contact 3D profilometer, and scanning electron microscopy. The experimental results demonstrate that low laser power and low scanning speed favor the formation of uniform and flat Cu lines. After process optimization, copper lines with a width less than 5 μm were obtained, which provides an attractive application prospect in the field of flexible electronic devices.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Cyclic Thermal Oxidation Evaluation to Improve Ti6Al4V Surface in Applications as Biomaterial

Thermal oxidation treatments are widely used to modify titanium surfaces. Thermally oxidized titanium alloys are used as biomaterials due to their better surface properties, such as corrosion resistance. However, the use of cyclic thermal treatment for this purpose has not yet been reported. This paper’s objective was to compare roughness, microhardness and corrosion resistance after cyclic and conventional isothermal heat treatments in a Ti6Al4V alloy. The heat treatments were performed over a period of 24 h with a maximum temperature of 650 °C, and cyclic conditions were executed from 200 to 400 °C for 48 cycles, each lasting 0.5 h. After the thermal treatments, roughness was measured through profilometer and atomic force microscopy, Vickers microhardness was evaluated, and polarization corrosion tests were performed in simulated body fluid. All treatments increased surface roughness, microhardness and corrosion resistance at 500 mV above open-circuit potential in polarization tests, compared to the material without oxidation. These results are associated with rutile formation, observed through XRD analysis. Although the isothermal and cyclic treatments presented similar behaviors, the 650-200 °C cyclic heat treatment provided an intermediate roughness and produced a slightly better corrosion resistance, demonstrating that cyclic thermal treatments are a viable alternative for improving titanium alloy surface properties.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Organofunctional Silane Modification of Aluminum-Doped Zinc Oxide Surfaces as a Route to Stabilization

Aluminum-doped zinc oxide (AZO) is a low-temperature processed transparent conductive oxide (TCO) made of earth abundant elements; its applications are currently limited by instability to heat, moisture, and acidic conditions. We demonstrate that the application of an organofunctional silane modifier mitigates AZO degradation, and explore the interplay between performance and material composition and morphology. Specifically, we evaluate degradation of bare AZO and APTES (3-aminopropyltriethoxysilane)-modified AZO in response to damp heat (DH, 85 °C, 85 % relative humidity) exposure over 1000 h, then demonstrate how surface modification impacts changes in electrical and optical properties, and chemical composition in one of the most thorough studies to date. Hall measurements show that the resistivity of AZO increases due to a decrease in electron mobility, with no commensurate change in carrier concentration. APTES decelerates this electrical degradation, without affecting AZO optical properties. Percent transmission and yellowness index of an ensemble of bare and modified AZO are stable upon DH exposure, but haze increases slightly for a discrete sample of modified AZO. Atomic force microscopy (AFM) and optical profilometer (OP) measurements do not show evidence of pitting or delamination after 1000 h DH exposure, but indicate a slight increase in surface roughness on both the nanometer and micron length scales. X-ray photoelectron spectroscopy data (XPS) reveal that the surface composition of bare and silanized AZO is stable over this time frame; oxygen vacancies, as measured by XPS, are also stable with DH exposure, which, together with transmission and Hall measurements, indicate stable carrier concentrations. However, after 1500 h of DH exposure, only bare AZO shows signs of catastrophic destruction. Comparison of the data presented herein to previous reports indicates that the initial AZO composition and microstructure dictate the degradation profile. Furthermore, this work demonstrates that surface modification slows the bulk degradation of AZO, and provides insight into how the material can be more widely used as a transparent electrode in the next generation of optoelectronic devices.

14 SOLAR ENERGY↗

DOE OSTI2018

The effect of engine operating conditions on exhaust gas recirculation cooler fouling

Exhaust gas recirculation (EGR) cooler fouling occurs when particulate matter (PM) and hydrocarbons (HC) in diesel exhaust form a deposit on the walls of the EGR cooler through thermophoresis and condensation. To better understand the mechanisms controlling deposit formation and removal and how operating conditions can affect cooler performance, 20 identical tube-in-shell EGR coolers with sinusoidal fins were fouled using a 5-factor, 3-level experimental design. The deposit thickness was measured using two methods: (1) epoxy-mounting and polishing cooler cross-sections and comparing deposit thicknesses on the primary (outer tube) to the secondary (fins) heat transfer surfaces, and (2) milling tube sections such that the surface of a fin could be observed and measuring the deposit thickness across the fin using a 3D profilometer. Near the cooler inlet, high inlet gas temperatures reduced deposit thickness by promoting mud-cracking and spallation. Near the middle of the cooler, the flow rate had the largest impact on the deposit thickness through the effect on residence time of the PM. The HC concentration along with flow rate had the largest effects near the cooler outlet where the lower temperatures allows for more HC condensation. Furthermore, these insights into how engine operating conditions influence the development of fouling layers in EGR coolers learned through this study will aid in the development of more fouling resistant coolers in the future.

42 ENGINEERING↗

DOE OSTI2013

Dry etching techniques for active devices based on hexagonal boron nitride epilayers

Hexagonal boron nitride (hBN) has emerged as a fundamentally and technologically important material system owing to its unique physical properties including layered structure, wide energy bandgap, large optical absorption, and neutron capture cross section. As for any materials under development, it is necessary to establish device processing techniques to realize active devices based on hBN. The authors report on the advancements in dry etching techniques for active devices based on hBN epilayers via inductively coupled plasma (ICP). The effect of ICP radio frequency (RF) power on the etch rate and vertical side wall profile was studied. The etching depth and angle with respect to the surface were measured using atomic force microscopy showing that an etching rate ∼1.25 μm/min and etching angles >80° were obtained. Profilometer data and scanning electron microscope images confirmed these results. This work demonstrates that SF{sub 6} is very suitable for etching hBN epilayers in RF plasma environments and can serve as a guide for future hBN device processing.

36 MATERIALS SCIENCE↗

DOE OSTI2015

X-ray microtomography and laser ablation in the analysis of ink distribution in coated paper

A novel method was developed for studying the ink-paper interface and the structural variations of a deposited layer of ink. Combining high-resolution x-ray tomography with laser ablation, the depth profile of ink (toner), i.e., its varying thickness, could be determined in a paper substrate. X-ray tomography was used to produce the 3D structure of paper with about 1 μm spatial resolution. Laser ablation combined with optical imaging was used to produce the 3D structure of the printed layer of ink on top of that paper with about 70 nm depth resolution. Ablation depth was calibrated with an optical profilometer. It can be concluded that a toner layer on a light-weight-coated paper substrate was strongly perturbed by protruding fibers of the base paper. Such fibers together with the surface topography of the base paper seem to be the major factors that control the leveling of toner and its penetration into a thinly coated paper substrate.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2019

Defect Characterization Through Automated Laser Track Trace Identification in SLM Processes Using Laser Profilometer Data

This paper presents recent developments in statistical image processing to demonstrate feasibility of layer-by-layer nondestructive inspection for selective laser melting (SLM) of metallic parts. A matrix of 10 mm × 10 mm stainless 316 squares was deposited with the first row consisting of just the sintered surface, Row 2 a single layer, Row 3 with 2 layers and so on. These layers were scanned to emulate the layer-by-layer collection of top surface geometry using a laser sensor. The resultant data were utilized to generate ISO 25718 roughness parameters and subsequently to perform track identification. This calculation consisted of two salient steps: (1) computing the gradients of surface roughness, which vanish at the peaks and pits, and (2) extracting the scanning direction by taking Hough transform of the geometry. This algorithm was repeated for all layers, and the alignment of the roughness with the rotating scan was observed to be persistent for all layers. Correlation between surface properties obtained along various scan directions and defect probability is explored.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Experimental and numerical study of plastic shear instability under high-speed loading conditions

The behavior of specimens dynamically loaded during the split Hopkinson (Kolsky) bar tests in a regime close to simple shear conditions was studied. The lateral surface of the specimens was investigated in a real-time mode with the aid of a high-speed infra-red camera CEDIP Silver 450M. The temperature field distribution obtained at different time made it possible to trace the evolution of plastic strain localization. The process of target perforation involving plug formation and ejection was examined using a high-speed infra-red camera and a VISAR velocity measurement system. The microstructure of tested specimens was analyzed using an optical interferometer-profilometer and a scanning electron microscope. The development of plastic shear instability regions has been simulated numerically.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effect of the Laser Scan Rate on the Microstructure, Magnetic Properties, and Microhardness of Selective Laser-Melted FeSiB

FeSiB alloys have been fabricated by selective laser melting (SLM) using a laser scan rate of 0.1–1.5 m/s, laser power of 90 W, scan line spacing of 40 μ m, and layer thickness of 50 μ m. X-ray diffraction, scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy, atomic force microscopy, profilometer, microdurometer, and vibrating sample magnetometer have been used to investigate the structural, microstructural, roughness, microhardness, and magnetic property changes during the laser melting process. The produced samples exhibit a nanocomposite structure consisting of nanocrystalline α-Fe{sub 0.95}Si{sub 0.05} and Fe{sub 2}B phases embedded into an amorphous ε-FeSi-type matrix. The selective laser-melted samples show high density, low surface roughness, higher microhardness values (1654–2273 Hv), and soft magnetic properties (M{sub s} = 188.6–199 emu/g and H{sub c} = 43.8–73 Oe).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Measurement of Piston Deposit Thickness Using Laser Profilometer

In this work, a novel method of measuring the thickness of deposits on engine pistons, including within ring grooves, is described. A laser profilometer is used in conjunction with a rotary stage to measure a continuous profile of the piston with deposits, and the measurement is repeated after cleaning the deposits from the piston. Algorithms for aligning the scans and determining the differential thickness are described, and results are compared to deposit thickness measurements using a contact-type magnetic induction coating thickness gauge. This method allows continuous measurement of deposit thickness across the entire surface including lands and ring grooves as well as quantification of the volume of the deposits.

42 ENGINEERING↗