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At least 1,675 records · Page 93

Method for nanoscale spatial registration of scanning probes with substrates and surfaces

Embodiments in accordance with the present invention relate to methods and apparatuses for aligning a scanning probe used to pattern a substrate, by comparing the position of the probe to a reference location or spot on the substrate. A first light beam is focused on a surface of the substrate as a spatial reference point. A second light beam then illuminates the scanning probe being used for patterning. An optical microscope images both the focused light beam, and a diffraction pattern, shadow, or light backscattered by the illuminated scanning probe tip of a scanning probe microscope (SPM), which is typically the tip of the scanning probe on an atomic force microscope (AFM). Alignment of the scanning probe tip relative to the mark is then determined by visual observation of the microscope image. This alignment process may be repeated to allow for modification or changing of the scanning probe microscope tip.

Wade, Lawrence A.↗

Aligning Arrays of Lenses and Single-Mode Optical Fibers

A procedure now under development is intended to enable the precise alignment of sheet arrays of microscopic lenses with the end faces of a coherent bundle of as many as 1,000 single-mode optical fibers packed closely in a regular array (see Figure 1). In the original application that prompted this development, the precise assembly of lenses and optical fibers serves as a single-mode spatial filter for a visible-light nulling interferometer. The precision of alignment must be sufficient to limit any remaining wavefront error to a root-mean-square value of less than 1/10 of a wavelength of light. This wavefront-error limit translates to requirements to (1) ensure uniformity of both the lens and fiber arrays, (2) ensure that the lateral distance from the central axis of each lens and the corresponding optical fiber is no more than a fraction of a micron, (3) angularly align the lens-sheet planes and the fiber-bundle end faces to within a few arc seconds, and (4) axially align the lenses and the fiber-bundle end faces to within tens of microns of the focal distance. Figure 2 depicts the apparatus used in the alignment procedure. The beam of light from a Zygo (or equivalent) interferometer is first compressed by a ratio of 20:1 so that upon its return to the interferometer, the beam will be magnified enough to enable measurement of wavefront quality. The apparatus includes relay lenses that enable imaging of the arrays of microscopic lenses in a charge-coupled-device (CCD) camera that is part of the interferometer. One of the arrays of microscopic lenses is mounted on a 6-axis stage, in proximity to the front face of the bundle of optical fibers. The bundle is mounted on a separate stage. A mirror is attached to the back face of the bundle of optical fibers for retroreflection of light. When a microscopic lens and a fiber are aligned with each other, the affected portion of the light is reflected back by the mirror, recollimated by the microscopic lens, transmitted through the relay lenses and the beam compressor/expander, then split so that half goes to a detector and half to the interferometer. The output of the detector is used as a feedback control signal for the six-axis stage to effect alignment.

Liu, Duncan↗

General Mode Scanning Probe Microscopy

A critical part of SPM measurements is the information transfer from the probe-sample junction to the measurement system. Current information transfer methods heavily compress the information-rich data stream by averaging the data over a time interval, or via heterodyne detection approaches such as lock-in amplifiers and phase-locked loops. As a consequence, highly valuable information at the sub-microsecond time scales or information from frequencies outside the measurement band is lost. We have developed a fundamentally new approach called General Mode (G-mode), where we can capture the complete information stream from the detectors in the microscope. The availability of the complete information allows the microscope operator to analyze the data via information-theory analysis or comprehensive physical models. Furthermore, the complete data stream enables advanced data-driven filtering algorithms, multi-resolution imaging, ultrafast spectroscropic imaging, spatial mapping of multidimensional variability in material properties, etc. Though we applied this approach to scanning probe microscopy, the general philosophy of G-mode can be applied to many other modes of microscopy. G-mode data is captured by completely custom software written in LabVIEW and Matlab. The software generates the waveforms to electrically, thermally, or mechanically excite the SPM probe. It handles real-time communications with the microscope software for operations such as moving the SPM probe position and also controls other instrumentation hardware. The software also controls multiple variants of high-speed data acquisition cards to excite the SPM probe with the excitation waveform and simultaneously measure multiple channels of information from the microscope detectors at sampling rates of 1-100 MHz. The software also saves the raw data to the computer and allows the microscope operator to visualize processed or filtered data during the experiment. The software performs all these features while offering a user-friendly interface.

Somnath, Suhas↗

Closed-looped in situ nano processing on a culturing cell using an inverted electron beam lithography system

Highlights: ► An electron beam lithography (EBL) was used as an in situ nano processing for a living cell. ► A synchronized optics was containing an inverted EBL and an optical microscope. ► This system visualized real-time images of the EB-induced nano processing. ► We demonstrated the nano processing for a culturing cell with 200–300 nm resolution. ► Our system would be able to provide high resolution display of virtual environments. -- Abstract: The beam profile of an electron beam (EB) can be focused onto less than a nanometer spot and scanned over a wide field with extremely high speed sweeping. Thus, EB is employed for nano scale lithography in applied physics research studies and in fabrication of semiconductors. We applied a scanning EB as a control system for a living cell membrane which is representative of large scale complex systems containing nanometer size components. First, we designed the opposed co-axial dual optics containing inverted electron beam lithography (I-EBL) system and a fluorescent optical microscope. This system could provide in situ nano processing for a culturing living cell on a 100-nm-thick SiN nanomembrane, which was placed between the I-EBL and the fluorescent optical microscope. Then we demonstrated the EB-induced chemical direct nano processing for a culturing cell with hundreds of nanometer resolution and visualized real-time images of the scanning spot of the EB-induced luminescent emission and chemical processing using a high sensitive camera mounted on the optical microscope. We concluded that our closed-loop in situ nano processing would be able to provide a nanometer resolution display of virtual molecule environments to study functional changes of bio-molecule systems.

60 APPLIED LIFE SCIENCES↗

Gas mixing system for imaging of nanomaterials under dynamic environments by environmental transmission electron microscopy

A gas mixing manifold system that is capable of delivering a stable pressure stream of a desired composition of gases into an environmental transmission electron microscope has been developed. The system is designed to provide a stable imaging environment upon changes of either the composition of the gas mixture or upon switching from one gas to another. The design of the system is described and the response of the pressure inside the microscope, the sample temperature, and sample drift in response to flow and composition changes of the system are reported.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Monopole antenna in quantitative near-field microwave microscopy of planar structures

We have developed an analytical model of a near-field microwave microscope based on a coaxial resonator with a sharpened tip probe. The probe interacts with a layered sample that features an arbitrary depth distribution of permittivity. The microscopic tip end with the accumulated charge is regarded as a monopole antenna radiating an electric field in near zone. The impedance of such an antenna is determined within a quasi-static approximation. The proposed model is used for calculating the sample-sensitive parameters of the microscope, specifically, resonance frequency f{sub 0} and quality factor Q{sub 0}, as a function of probe-sample distance h. The theory has been verified experimentally in studies of semiconductor structures, both bulk and thin films. For measurements, we built a ∼2.1 GHz microscope with an effective tip radius of about 100 μm. The theoretical and experimental dependences f{sub 0}(h) and Q{sub 0}(h) were found to be in a good agreement. The developed theory underlies the method for determining sheet resistance R{sub sh} of a semiconductor film on a dielectric substrate proposed in this article. Studies were performed on doped n-GaN films on an Al{sub 2}O{sub 3} substrate. The effective radius and height of the probe determined from calibration measurements of etalon samples were used as the model fitting parameters. For etalon samples, we employed homogeneous sapphire and doped silicon plates. We also performed four-probe dc measurements of R{sub sh}. The corresponding values for samples with R{sub sh} > 1 kΩ were found to be 50% to 100% higher than the microwave results, which are attributed to the presence of microdefects in semiconductor films.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

SISGR: Atom chip microscopy: A novel probe for strongly correlated materials

Microscopy techniques co-opted from nonlinear optics and high energy physics have complemented solid-state probes in elucidating the order manifest in condensed matter materials. Up until now, however, no attempts have been made to use modern techniques of ultracold atomic physics to directly explore properties of strongly correlated or topologically protected materials. Our current program is focused on introducing a novel magnetic field microscopy technique into the toolbox of imaging probes. Our prior DOE ESPM program funded the development of a novel instrument using a dilute gas Bose-Einstein condensate (BEC) as a scanning probe capable of measuring tiny magnetic (and electric) DC and AC fields above materials. We successfully built the world's first “scanning cryogenic atom chip microscope”, and we now are in the process of characterizing its performance before using the instrument to take the first wide-area images of transport flow within unconventional superconductors, pnictides and oxide interfaces (LAO/STO), topological insulators, and colossal magnetoresistive manganites. We will do so at temperatures outside the capability of scanning SQUIDs, with ~10x better resolution and without 1/f-noise. A notable goal will be to measure the surface-to-bulk conductivity ratio in topological insulators in a relatively model-independent fashion. We have completed the construction of this magnetic microscope. The instrument uses atom chips—substrates supporting micron-sized current-carrying wires that create magnetic microtraps near surfaces for ultracold thermal gases and BECs—to enable single-shot and raster-scanned large-field-of-view detection of magnetic fields. The fields emanating from electronic transport may be detected at the 10 -7 flux quantum (Φ0) level and below; that is, few to sub-micron resolution of sub-nanotesla fields over single-shot, millimeter-long detection lengths. By harnessing the extreme sensitivity of atomic clocks and BECs to external perturbations, we are now in a position to use atom chips for imaging transport in new regimes. Scanning quantum gas atom chip microscopy introduces three very important features to the toolbox of high-resolution scanning microscopy of strongly correlated or topological materials: simultaneous detection of magnetic and electric fields (down to the sub-single electron charge level; no invasive large magnetic fields or gradients; simultaneous micro- and macroscopic spatial resolution; DC to MHz detection bandwidth; freedom from 1/ƒ flicker noise at low frequencies; and, perhaps most importantly, the complete decoupling of probe and sample temperatures. The atom chip microscope can operate at maximum sensitivity and resolution without regard to the substrate temperature. While the BEC is among the coldest objects realizable (100 nK temperatures are typical), the atom chip substrate can be positioned 1 μm away from the BEC and be as hot as 400 K or as cold as the cryostat can cool. This is because unlike superconducting probes, whose temperature is closely coupled to nearby materials, quantum gases are immune to radiative heating. The energy gap between a Rb atom’s ground state and first excited state far exceeds the typical energy of room-temperature blackbody radiation; such atoms are therefore transparent to radiation heating by materials at room temperature or below. We experimentally demonstrated a new atom chip trapping system that allows the placement and high-resolution imaging of ultracold atoms within microns from any ≤100 μm-thin, UHV-compatible material, while also allowing sample exchange with minimal experimental downtime. The sample is not connected to the atom chip, allowing rapid exchange without perturbing the atom chip or laser cooling apparatus. Exchange of the sample and retrapping of atoms has been performed within a week turnaround, limited only by chamber baking. Moreover, the decoupling of sample and atom chip provides the ability to independently tune the sample temperature and its position with respect to the trapped ultracold gas, which itself may remain in the focus of a high-resolution imaging system. We confine 100-nK BECs of 104 87Rb atoms near a gold-mirrored 100-μm-thick silicon substrate. The substrate can be cooled to 35 K without use of a heat shield, while the atom chip, 120-μm away, remains at room temperature. Atoms may be imaged with 1-μm resolution and retrapped every 16 s, allowing rapid data collection. Straightforward improvements will allow us to push sample temperatures close to 4 K, and improve imaging resolution from 1 μm down to a few-100 nm, thereby providing 10 -9 Φ0 detection sensitivity. We will test the utility of this technique by imaging the magnetic fields emanating from electronic transport and domain percolation in several interesting examples of strongly correlated or topologically protected materials. STM, transport, and x-ray scattering experiments have, among others, revealed the existence of a quantum liquid crystal state in iron (pnictide) and cuprate superconductors. This strongly correlated state of matter could also be detected by imaging the fluctuating transport (spatially and in time) of electrons as the phase/regime boundary is crossed between the pnictide non-Fermi liquid (cuprate strange metal) and the pnictide magnetic phase (cuprate pseudogap regime). Our ability to image wide-area inhomogeneous current flow from room-temperature to <10 K will allow us to study the developing domain structure and transport near twin boundary interfaces through the T N ≈50–150 K nematic transition recently identified in bulk transport experiments by Ian Fisher's group in underdoped Fe-arsinide superconductors. Again, this highlights a main feature of our cryogenic atom chip microscope: the ability to image transport regardless of the sample temperature since the BEC, at nK temperatures, is transparent to blackbody radiation, even when held a microns from the surface.

36 MATERIALS SCIENCE↗

Isothermal oxidation of zirconium using steam

Oxidation of zirconium and its alloys under any atmosphere is generally characterised by a protective and non-protective stage. During the protective stage, the kinetics of oxidation are quasi-parabolic, while the oxide scale formed on the surface of the metal is black, compact, and protective in nature. For the non-protective stage, the oxidation rate becomes linear, while the protective oxide film turns into a deteriorated white scale. Breakaway is known as the transition point from protective to non-protective stage. The actual mechanism leading to breakaway of zirconium is still a matter of controversy, however some of the most common factors affecting breakaway are the following: - Impurities on the metal (Carbon, Oxygen, Nitrogen); - Oxidizing atmosphere (Presence of H{sub 2}O (g) or N{sub 2} (g)); - Sample preparation (Chemically etched or polished); - Temperature (LWR, LOCA). This research investigates the effect of temperature on 'breakaway' when zirconium is oxidized isothermally in steam for 60 min at 800 and 900 deg. C using thermogravimetric and optical microscopic imaging techniques. 1. Steam isothermal oxidations were performed on zirconium at 800 and 900 deg. C using a Thermogravimetric Analyzer (TGA). 2. Log-log plots of mass gain vs time were obtained from thermogravimetric results to calculate the reaction orders (n) and reaction rate constants (K) during oxidation. 3. Results of the kinetics of reaction were correlated with optical microscopic images form Light Microscope (LM) and Scanning Electron Microscope (SEM). Breakaway depends very strongly on temperature. At 800 deg. C, the weight gain followed a cubic-parabolic behaviour with evidence of a protective oxide film. On the other hand, oxidation at 900 deg. C showed signs of breakaway since the oxide film was cracked and oxidation rate was almost linear throughout the reaction.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Nuclear ground-state masses and deformations: FRDM(2012)

We tabulate the atomic mass excesses and binding energies, ground-state shell-plus-pairing corrections, ground-state microscopic corrections, and nuclear ground-state deformations of 9318 nuclei ranging from {sup 16}O to A=339. The calculations are based on the finite-range droplet macroscopic and the folded-Yukawa single-particle microscopic nuclear-structure models, which are completely specified. Relative to our FRDM(1992) mass table in Möller et al. (1995), the results are obtained in the same model, but with considerably improved treatment of deformation and fewer of the approximations that were necessary earlier, due to limitations in computer power. The more accurate execution of the model and the more extensive and more accurate experimental mass data base now available allow us to determine one additional macroscopic-model parameter, the density-symmetry coefficient L, which was not varied in the previous calculation, but set to zero. Because we now realize that the FRDM is inaccurate for some highly deformed shapes occurring in fission, because some effects are derived in terms of perturbations around a sphere, we only adjust its macroscopic parameters to ground-state masses. The values of ten constants are determined directly from an optimization to fit ground-state masses of 2149 nuclei ranging from {sup 16}O to {sub 106}{sup 265}Sg and {sub 108}{sup 264}Hs. The error of the mass model is 0.5595 MeV for the entire region of nuclei included in the adjustment, but is only 0.3549 MeV for the region N≥65. We also provide masses in the FRLDM, which in the more accurate treatments now has an error of 0.6618 MeV, with 0.5181 MeV for nuclei with N≥65, both somewhat larger than in the FRDM. But in contrast to the FRDM, it is suitable for studies of fission and has been extensively so applied elsewhere, with FRLDM(2002) constants. The FRLDM(2012) fits 31 fission-barrier heights from {sup 70}Se to {sup 252}Cf with a root-mean-square deviation of 1.052 MeV.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Application of deoxygenation-aeration cycling to control the predatory bacterium Vampirovibrio chlorellavorus in Chlorella sorokiniana cultures

A previously untested approach was evaluated to enable management of the predatory bacterium, Vampirovibrio chlorellavorus, a pathogen of Chlorella sorokiniana, in suspension cultures grown in a laboratory test reactor. Because V. chlorellavorus is an obligate aerobic bacterium, whereas C. sorokiniana grows under aerobic and anaerobic conditions, deoxygenation of the culture was expected to be detrimental to the pathogen, but not to the algal host. The effect of deoxygenation on the uninfected (healthy) C. sorokiniana suspension cells, compared to the C. sorokiniana-V. chlorellavorus co-culture, was studied in relation to biomass, dissolved oxygen, ratio of C. sorokiniana to V. chlorellavorus DNA, and visual and light microscopic observations. Preliminary experiments were conducted to test the effects of different deoxygenation-aeration cycling regimes on performance of V. chlorellavorus-free C. sorokiniana cultures. To an aerobic culture, pure nitrogen gas was introduced to create anoxic conditions, followed by the injection of ambient air to re-establish an aerobic environment. Under this repeated cycling regime, C. sorokiniana was shown to tolerate the anoxic conditions for extended timespans that ranged from 2 to 8 h over a 5-day test period. The analogous aerobic-anoxic cycling with the C. sorokiniana-V. chlorellavorus co-cultures resulted in ‘near-normal’ growth cycle and harvestable biomass, whereas the continuously-aerated (aerobic) co-cultures that were grown without the deoxygenation step in the cycle collapsed in 3 days. Visual and light microscopic observations revealed intact C. sorokiniana cells were present in the deoxygenated cultures, compared to the aerobically-grown, brown-colored algal cultures consisting of collapsed cells. Quantitative polymerase chain reaction analysis showed continuous increases in the ratio of V. chlorellavorus (16S rDNA) to C. sorokiniana (18S rDNA) DNA in the aerated co-cultures, with greater increases during dark periods, while the pathogen-to-host DNA ratio in the deoxygenated co-cultures was relatively low and algal cells did not collapse, as would be expected following pathogen attack.

Algae, Anoxic, Bomass, Infection, Nitrogen, Quanti↗

Combined Recipe for Clinical Target Volume and Planning Target Volume Margins

Purpose: To develop a combined recipe for clinical target volume (CTV) and planning target volume (PTV) margins. Methods and Materials: A widely accepted PTV margin recipe is M{sub geo} = aΣ{sub geo} + bσ{sub geo}, with Σ{sub geo} and σ{sub geo} standard deviations (SDs) representing systematic and random geometric uncertainties, respectively. On the basis of histopathology data of breast and lung tumors, we suggest describing the distribution of microscopic islets around the gross tumor volume (GTV) by a half-Gaussian with SD Σ{sub micro}, yielding as possible CTV margin recipe: M{sub micro} = ƒ(N{sub i}) × Σ{sub micro}, with N{sub i} the average number of microscopic islets per patient. To determine ƒ(N{sub i}), a computer model was developed that simulated radiation therapy of a spherical GTV with isotropic distribution of microscopic disease in a large group of virtual patients. The minimal margin that yielded D{sub min} <95% in maximally 10% of patients was calculated for various Σ{sub micro} and N{sub i}. Because Σ{sub micro} is independent of Σ{sub geo}, we propose they should be added quadratically, yielding for a combined GTV-to-PTV margin recipe: M{sub GTV-PTV} = √([aΣ{sub geo}]{sup 2} + [ƒ(N{sub i})Σ{sub micro}]{sup 2}) + bσ{sub geo}. This was validated by the computer model through numerous simultaneous simulations of microscopic and geometric uncertainties. Results: The margin factor ƒ(N{sub i}) in a relevant range of Σ{sub micro} and N{sub i} can be given by: ƒ(N{sub i}) = 1.4 + 0.8log(N{sub i}). Filling in the other factors found in our simulations (a = 2.1 and b = 0.8) yields for the combined recipe: M{sub GTV-PTV} = √((2.1Σ{sub geo}){sup 2} + ([1.4 + 0.8log(N{sub i})] × Σ{sub micro}){sup 2}) + 0.8σ{sub geo}. The average margin difference between the simultaneous simulations and the above recipe was 0.2 ± 0.8 mm (1 SD). Calculating M{sub geo} and M{sub micro} separately and adding them linearly overestimated PTVs by on average 5 mm. Margin recipes based on tumor control probability (TCP) instead of D{sub min} criteria yielded similar results. Conclusions: A general recipe for GTV-to-PTV margins is proposed, which shows that CTV and PTV margins should be added in quadrature instead of linearly.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Residual Tumor After Neoadjuvant Chemoradiation Outside the Radiation Therapy Target Volume: A New Prognostic Factor for Survival in Esophageal Cancer

Purpose/Objective(s): The aim of this study was to analyze the accuracy of gross tumor volume (GTV) delineation and clinical target volume (CTV) margins for neoadjuvant chemoradiation therapy (neo-CRT) in esophageal carcinoma at pathologic examination and to determine the impact on survival. Methods and Materials: The study population consisted of 63 esophageal cancer patients treated with neo-CRT. GTV and CTV borders were demarcated in situ during surgery on the esophagus, using anatomical reference points to provide accurate information regarding tumor location at pathologic evaluation. To identify prognostic factors for disease-free survival (DFS) and overall survival (OS), a Cox regression analysis was performed. Results: After resection, macroscopic residual tumor was found outside the GTV in 7 patients (11%). Microscopic residual tumor was located outside the CTV in 9 patients (14%). The median follow-up was 15.6 months. With multivariate analysis, only microscopic tumor outside the CTV (hazard ratio [HR], 4.96; 95% confidence interval [CI], 1.03-15.36), and perineural growth (HR, 5.77; 95% CI, 1.27-26.13) were identified as independent prognostic factors for OS. The 1-year OS was 20% for patients with tumor outside the CTV and 86% for those without (P<.01). For DFS, microscopic tumor outside the CTV (HR, 5.92; 95% CI, 1.89-18.54) and ypN+ (HR, 3.36; 95% CI, 1.33-8.48) were identified as independent adverse prognostic factors. The 1-year DFS was 23% versus 77% for patients with or without tumor outside the CTV (P<.01). Conclusions: Microscopic tumor outside the CTV is associated with markedly worse OS after neo-CRT. This may either stress the importance of accurate tumor delineation or reflect aggressive tumor behavior requiring new adjuvant treatment modalities.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

AM metal substrates for inkjet-printing of smart devices

Highlights: • An experimental study to characterize 3D-printed metal substrates and their surfaces for inkjet-printing is presented. • Multilayer structures composed of an insulating layer and a superposed conductive layer, inkjet-printed onto various metallic substrates. • Characterization based on microscopic and Focused Ion Beam (FIB) images, profilometer and contact angle measurements of the substrates. • Microscopic images and four-point-probe resistance- and profilometer measurements to gain insight into the quality of the multilayer print. - Abstract: A study to characterize surface and structural properties of 3D-printed metal substrates for multilayer inkjet-printing is presented. Such substrates can enable and alleviate the fabrication of smart and functional packages, implants or spare parts. For the characterization, a multilayer structure composed of an insulating layer and a superposed conductive layer is inkjet-printed onto the various 3D-printed metallic substrates. The printing is done using equivalent settings for all substrates. The characterization is based on microscopic and Focused Ion Beam (FIB) images, as well as profilometer and contact angle measurements of the substrates. Furthermore, microscopic images and four-point-probe resistance- and profilometer measurements are carried out, to gain insight into the quality of the multilayer print. We show the diversity in surface and structural properties of 3D-printed substrates, also for those fabricated using the same process. Also, the 3D-printed samples exhibit different wettability properties than metals processed using standard processes. Finally, we can also demonstrate the suitability of selected substrates for inkjet-printing.

36 MATERIALS SCIENCE↗

Effect of Nb micro-alloying on microstructure and properties of thermo-mechanically processed high carbon pearlitic steel

Highlights: • Effect of Nb micro-alloying on high carbon steels has been established. • Fine and degenerated pearlite with fine PAGS is achieved due to Nb micro-alloying. • AFM study indicates true interlamellar spacing which conforms well to TEM study. • Hardness and yield strength have been obviously improved with the addition of Nb. - Abstract: Two C-Mn-Si steels with and without Nb micro-alloying are selected in the present study. Both these high carbon steels have been thermo-mechanically processed using Gleeble 3800 simulator. Optical microscope (OM), scanning electron microscope (SEM), transmission electron microscope (TEM), atomic force microscope (AFM) were utilised for microstructural characterisation. The austenitising temperature was varied from 1150 °C to 1200 °C followed by hot compression and subjected to free cooling to evaluate the influence of austenite grain size on transformed microstructure and mechanical properties. It is evident that higher austenite grain size is obtained for both types of steels subjected to higher austenitising temperature. The refinement of pearlite interlamellar spacing (<0.20 μm) with degenerated morphology as well as finer prior austenite grain size (<40 μm) is found to be more prominent for Nb micro-alloyed sample. The average hardness values of both the steels are higher for the specimens, treated at a higher austenitising temperature which is attributed to finer interlamellar spacing. Finally, the correlation between the evolving microstructure and resulting mechanical properties (hardness and yield strength) has been made.

36 MATERIALS SCIENCE↗

Magneto acoustical emission in nanocrystalline Mn–Zn ferrites

Graphical abstract: Mn{sub 0.4}Zn{sub 0.6}Fe{sub 2}O{sub 4} powders were prepared by microwave hydrothermal method. The powders were characterized by X-ray diffraction, transmission electron microscope. The powders were sintered at different temperatures 400, 500, 600, 700, 800 and 900 °C/30 min using microwave sintering method. The grain size was estimated by scanning electron microscope. The room temperature dielectric and magnetic properties were studied in the frequency range (100 kHz–1.8 GHz). The magnetization properties were measured upto 1.5 T. The acoustic emission has been measured along the hysteresis loops from 80 K to Curie temperature. It is found that the magneto-acoustic emission (MAE) activity along hysteresis loop is proportional to the hysteresis losses during the same loop. This law has been verified on series of polycrystalline ferrites and found that the law is valid whatever the composition, the grain size and temperature. It is also found that the domain wall creation/or annihilation processes are the origin of the MAE. - Highlights: • The AE been measured along the hysteresis loops from 80 K to Curie temperature. • The MAE activity along hysteresis loop is proportional to P{sub h} during the same loop. • It is found that the domain wall creation/or annihilation processes are the origin of the MAE. - Abstract: Mn{sub 0.4}Zn{sub 0.6}Fe{sub 2}O{sub 4} powders were prepared by microwave hydrothermal method. The powders were characterized by X-ray diffraction, transmission electron microscope. The powders were sintered at different temperatures 400, 500, 600, 700, 800 and 900 °C/30 min using microwave sintering method. The grain size was estimated by scanning electron microscope. The room temperature dielectric and magnetic properties were studied in the frequency range (100 kHz–1.8 GHz). The magnetization properties were measured upto 1.5 T. The acoustic emission has been measured along the hysteresis loops from 80 K to Curie temperature. It is found that the magneto-acoustic emission (MAE) activity along hysteresis loop is proportional to the hysteresis losses during the same loop. This law has been verified on series of polycrystalline ferrites and found that the law is valid whatever the composition, the grain size and temperature. It is also found that the domain wall creation/or annihilation processes are the origin of the MAE.

36 MATERIALS SCIENCE↗

Multicolor Three-Dimensional Tracking for Single-Molecule Fluorescence Resonance Energy Transfer Measurements

Single-molecule fluorescence resonance energy transfer (smFRET) remains a widely utilized and powerful tool for quantifying heterogeneous interactions and conformational dynamics of biomolecules. However, traditional smFRET experiments either are limited to short observation times (typically less than 1 ms) in the case of “burst” confocal measurements or require surface immobilization which usually has a temporal resolution limited by the camera framing rate. We developed a smFRET 3D tracking microscope that is capable of observing single particles for extended periods of time with high temporal resolution. The confocal tracking microscope utilizes closed-loop feedback to follow the particle in solution by recentering it within two overlapping tetrahedral detection elements, corresponding to donor and acceptor channels. We demonstrated the microscope’s multicolor tracking capability via random walk simulations and experimental tracking of 200 nm fluorescent beads in water with a range of apparent smFRET efficiency values, 0.45-0.69. We also demonstrated the microscope’s capability to track and quantify double-stranded DNA undergoing intramolecular smFRET in a viscous glycerol solution. In future experiments, the smFRET 3D tracking system will be used to study protein conformational dynamics while diffusing in solution and native biological environments with high temporal resolution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Connecting Hindered Transport in Porous Media across Length Scales: From Single-Pore to Macroscopic

Hindered mass transport is widely observed in various porous media, including filtration membranes and porous rocks. However, there is no universal model capable of predicting transport in porous media due to the heterogeneity of porous structures and the complexity of the underlying microscopic mechanisms, including electrostatic and hydrodynamic effects. Here, we used a highly ordered porous medium (i.e. a silica inverse opal film) as a model system to directly explore the effects of geometric parameters (i.e. pore size, pore throat size and tracer particle size) and microscopic interaction parameters (e.g. controlled by ionic strength) on nanoparticle transport in porous environments using three-dimensional single-particle tracking. We found a linear scaling relation between the macroscopic diffusion coefficient and microscopic diffusion behaviors and a combination of parameters associated with microscopic features and phenomena, including both geometric effects and particle-level interactions. The proportionality coefficient relating micro and macro behaviors was complex and related to the connectivity of the matrix and pore-size variation, which could lead to tortuous diffusion pathways, hindering macroscopic transport. Furthermore, these findings provide important insights into nanoparticles and macromolecules transport in various porous media.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Improved Coarse-Grained Modeling of Cholesterol-Containing Lipid Bilayers

In mammalian cells cholesterol is essential for membrane function, but in excess can be cytototoxic. The cellular response to acute cholesterol loading involves biophysical-based mechanisms that regulate cholesterol levels, through modulation of the “activity” or accessibility of cholesterol to extra-membrane acceptors. Experiments and united atom (UA) simulations show that at high concentrations of cholesterol, lipid bilayers thin significantly and cholesterol availability to external acceptors increases substantially. Such cholesterol activation is critical to its trafficking within cells. Here we aim to reduce the computational cost to enable simulation of large and complex systems involved in cholesterol regulation, such as those including oxysterols and cholesterol-sensing proteins. To accomplish this, we have modified the published MARTINI coarse-grained force field to improve its predictions of cholesterol-induced changes in both macroscopic and microscopic properties of membranes. Most notably, MARTINI fails to capture both the (macroscopic) area condensation and membrane thickening seen at less than 30% cholesterol and the thinning seen above 40% cholesterol. The thinning at high concentration is critical to cholesterol activation. Microscopic properties of interest include cholesterol-cholesterol radial distribution functions (RDFs), tilt angle, and accessible surface area. First, we develop an “angle-corrected” model wherein we modify the coarse-grained bond angle potentials based on atomistic simulations. This modification significantly improves prediction of macroscopic properties, most notably the thickening/thinning behavior, and also slightly improves microscopic property prediction relative to MARTINI. Second, we add to the angle correction a “volume correction” by also adjusting phospholipid bond lengths to achieve a more accurate volume per molecule. The angle + volume correction substantially further improves the quantitative agreement of the macroscopic properties (area per molecule and thickness) with united atom simulations. However, this improvement also reduces the accuracy of microscopic predictions like radial distribution functions and cholesterol tilt below that of either MARTINI or the angle-corrected model. Thus, while both of our forcefield corrections improve MARTINI, the combined angle and volume correction should be used for problems involving sterol effects on the overall structure of the membrane, while our angle-corrected model should be used in cases where the properties of individual lipid and sterol models are critically important.

biomembrane↗