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DOE OSTI2016

Experimental stand for studying the impact of laser-accelerated protons on biological objects

An original experimental stand is presented, aimed at studying the impact of high-energy protons, produced by the laser-plasma interaction at a petawatt power level, on biological objects. In the course of pilot experiments with the energy of laser-accelerated protons up to 25 MeV, the possibility is demonstrated of transferring doses up to 10 Gy to the object of study in a single shot with the magnetic separation of protons from parasitic X-ray radiation and fast electrons. The technique of irradiating the cell culture HeLa Kyoto and measuring the fraction of survived cells is developed. The ways of optimising the parameters of proton beams and the suitable methods of their separation with respect to energy and transporting to the studied living objects are discussed. The construction of the stand is intended for the improvement of laser technologies for hadron therapy of malignant neoplasms. (extreme laser radiation: physics and fundamental applications)

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2023

Influencing Bonding Interactions of the Neptunyl (V, VI) Cations with Electron-donating and -withdrawing Groups

Neptunium makes up the largest percentage of minor actinides found in spent nuclear fuel, yet separations of this element have proven difficult due to its rich redox chemistry. Developing new reprocessing techniques should rely on understanding how to control the Np oxidation state and its interactions with different ligands. Designing new ligands for separations requires understanding how to properly tune a system toward a desired trait through functionalization. Emerging technologies for minor actinide separations focus on ligands containing carboxylate or pyridine functional groups, which are desirable due to their high degree of functionalization. So we use DFT calculations to study the interactions of carboxylate and polypyridine ligands with the neptunyl cation [Np(V/VI)O2] +/2+ . A systematic study is performed by varying the electronic properties of the carboxylate and polypyridine ligands through the inclusion of different electron-withdrawing and electron-donating R groups. We focus on how these groups can affect geometric properties, electronic structure, and bonding characterization as a function of the metal oxidation state and ligand character and discuss how these factors can play a role in neptunium ligand design principles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2013

On-Chip Microfluidic Components for In Situ Analysis, Separation, and Detection of Amino Acids

The Astrobiology Analytical Laboratory at GSFC has identified amino acids in meteorites and returned cometary samples by using liquid chromatography-electrospray ionization time-of-flight mass spectrometry (LCMS). These organic species are key markers for life, having the property of chirality that can be used to distinguish biological from non-biological amino acids. One of the critical components in the benchtop instrument is liquid chromatography (LC) analytical column. The commercial LC analytical column is an over- 250-mm-long and 4.6-mm-diameter stainless steel tube filled with functionized microbeads as stationary phase to separate the molecular species based on their chemistry. Miniaturization of this technique for spaceflight is compelling for future payloads for landed missions targeting astrobiology objectives. A commercial liquid chromatography analytical column consists of an inert cylindrical tube filled with a stationary phase, i.e., microbeads, that has been functionalized with a targeted chemistry. When analyte is sent through the column by a pressurized carrier fluid (typically a methanol/ water mixture), compounds are separated in time due to differences in chemical interactions with the stationary phase. Different species of analyte molecules will interact more strongly with the column chemistry, and will therefore take longer to traverse the column. In this way, the column will separate molecular species based on their chemistry. A lab-on-chip liquid analysis tool was developed. The microfluidic analytical column is capable of chromatographically separating biologically relevant classes of molecules based on their chemistry. For this analytical column, fabrication, low leak rate, and stationary phase incorporation of a serpentine microchannel were demonstrated that mimic the dimensions of a commercial LC column within a 5 10 1 mm chip. The microchannel in the chip has a 75- micrometer-diameter oval-shaped cross section. The serpentine microchannel has four different lengths: 40, 60, 80, and 100 mm. Functionized microbeads were filled inside the microchannel to separate molecular species based on their chemistry.

Zheng, Yun↗

NASA NTRS1989

Modal, ray, and beam techniques for analyzing the EM scattering by open-ended waveguide cavities

The problem of high-frequency electromagnetic (EM) scattering by open-ended waveguide cavities with an interior termination is analyzed via three different approaches. When cavities can be adequately modeled by joining together piecewise separable waveguide sections, a hybrid combination of asymptotic high-frequency and modal techniques is employed. In the case of more arbitrarily shaped waveguide cavities for which modes cannot even be defined in the conventional sense, the geometrical optics ray approach proves to be highly useful. However, at sufficiently high frequencies, both of these approaches tend to become inefficient. Hence, a paraxial Gaussian batch technique, which retains much of the simplicity of the ray approximation but is potentially more efficient, is investigated. Typical numerical results based on the different approaches are discussed.

Pathak, Prabhakar H.↗

NASA NTRS2002

Flow Control Research at NASA Langley in Support of High-Lift Augmentation

The paper describes the efforts at NASA Langley to apply active and passive flow control techniques for improved high-lift systems, and advanced vehicle concepts utilizing powered high-lift techniques. The development of simplified high-lift systems utilizing active flow control is shown to provide significant weight and drag reduction benefits based on system studies. Active flow control that focuses on separation, and the development of advanced circulation control wings (CCW) utilizing unsteady excitation techniques will be discussed. The advanced CCW airfoils can provide multifunctional controls throughout the flight envelope. Computational and experimental data are shown to illustrate the benefits and issues with implementation of the technology.

Sellers, William L., III↗

NASA NTRS1976

A numerical comparison of discrete Kalman filtering algorithms - An orbit determination case study

An improved Kalman filter algorithm based on a modified Givens matrix triangularization technique is proposed for solving a nonstationary discrete-time linear filtering problem. The proposed U-D covariance factorization filter uses orthogonal transformation technique; measurement and time updating of the U-D factors involve separate application of Gentleman's fast square-root-free Givens rotations. Numerical stability and accuracy of the algorithm are compared with those of the conventional and stabilized Kalman filters and the Potter-Schmidt square-root filter, by applying these techniques to a realistic planetary navigation problem (orbit determination for the Saturn approach phase of the Mariner Jupiter-Saturn Mission, 1977). The new algorithm is shown to combine the numerical precision of square root filtering with the efficiency of the original Kalman algorithm.

Thornton, C. L.↗

NASA NTRS1987

Free wake analysis of helicopter rotor blades in hover using a finite volume technique

A fully compressible method for determining helicopter rotor wake effects is described which computes the wake without requiring external specification of the wake, or separate computations for the wake and blade region. The method is a modification of a compressible finite volume Potential Flow technique, and it has been implemented in a program, HELIX I, for computing compressible rotor flow fields in hover with free wakes. Wake positions in substantial agreement with experiment have been calculated for cases including subsonic and transonic flows, high and low aspect ratios, and two- and four-bladed rotors.

Ramachandran, K.↗

NASA NTRS1983

Computational technique for three-dimensional compressible flow past wings at high angles of attack

A computational technique, based on the integral solution of the full potential equation, has been developed for the solution of three-dimensional high-subsonic flows past wings at high angles of attack. The problem includes two sources of nonlinearities: a boundary oriented nonlinearity (separated flow roll up) and a region oriented nonlinearity (flow compressibility). The former is represented by a nonlinear vortex lattice while the latter is represented by a source distribution inside a finite volume. The solution is obtained by using double iteration cycles; a separated flow (wake) iteration cycle and a compressibility iteration cycle. The computational technique is applied to a delta wing. The results show that the technique is very promising and efficient.

Kandil, O. A.↗

DOE OSTI2016

Fresh-slice multicolour X-ray free-electron lasers

X-ray free-electron lasers (XFELs) provide femtosecond X-ray pulses with a narrow energy bandwidth and unprecedented brightness. Ultrafast physical and chemical dynamics, initiated with a site-specific X-ray pulse, can be explored using XFELs with a second ultrashort X-ray probe pulse. However, existing double-pulse schemes are complicated, difficult to customize or provide only low-intensity pulses. Here we present the novel fresh-slice technique for multicolour pulse production, wherein different temporal slices of an electron bunch lase to saturation in separate undulator sections. This method combines electron bunch tailoring from a passive wakefield device with trajectory control to provide multicolour pulses. The fresh-slice scheme outperforms existing techniques at soft X-ray wavelengths. It produces femtosecond pulses with a power of tens of gigawatts and flexible colour separation. The pulse delay can be varied from temporal overlap to almost one picosecond. As a result, we also demonstrate the first three-colour XFEL and variably polarized two-colour pulses.

43 PARTICLE ACCELERATORS↗

DOE OSTI2016

Fabrication of MCM-41 fibers with well-ordered hexagonal mesostructure controlled in acidic and alkaline media

In this paper, synthesis and characterization of two type morphologies of the MCM-41mesoporous material, nano and microfibers, were investigated by electrospinning technique. The synthesis was performed in acidic and alkaline media, separately. The MCM-41 morphologies were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray powder diffraction (XRD), and nitrogen adsorption–desorption measurement. Tetraethylorthosilicate (TEOS) and cetyltrimethylammonium bromide (CTAB) were used as silica and template sources for the synthesis of MCM-41 morphologies, respectively. The SEM results showed that MCM-41 nanofibers were spun in acidic media and microfibers of MCM-41 were produced in alkaline media. The XRD study revealed a long range structural ordering of mesoporous materials. The TEM results indicated rough surfaces with uniform average diameter 200 nm for nanofibers and 2 µm for microfibers. The pore diameter and surface area of calcined MCM-41 nanofibers were 2.2 nm and 970 m{sup 2}/g, respectively. For the MCM-41 microfibers, pore sizes of 2.7 nm and surface areas 420 m{sup 2}/g was measured. - Graphical abstract: Electrospinning method was used for fabricating of MCM-41 microfibers from TEOS in alkaline media (top) and MCM-41 nanofibers in acidic media (bottom). - Highlights: • Synthesis of MCM-41 nanofibers and microfibers by electrospinning technique. • MCM-41 nanofibers were synthesized in acidic media. • MCM-41 manofibers spun in alkaline media. • Electrospinning was a simple method for preparing of fibers with respect to chemical method.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Low-order multiphysics coupling techniques for nuclear reactor applications

The accurate modeling and simulation of nuclear reactor designs depends greatly on the ability to couple differing sets of physics together. Current coupling techniques most often use a fixed-point, or Picard, iteration scheme in which each set of physics is solved separately, and the resulting solutions are passed between each solver. In the work presented here, two different coupling techniques are investigated: a Jacobian-Free Newton-Krylov (JFNK) approach and a new methodology called Coarse Mesh Finite Difference Coupling (CMFD-Coupling). In this work, both techniques were applied to the low-order CMFD system of equations. This allows for the multiphysics feedback effects to be captured on the low-order system without having to perform a neutron transport solve. The JFNK and CMFD-Coupling approaches were implemented in the MPACT neutron transport code, which is being developed for the Consortium for Advanced Simulation of Light Water Reactors (CASL). These methods were tested on a wide range of practical reactor physics problems, from a single 3D fuel pin to a massively parallel 3D full core problem. When coupled neutronics-thermal hydraulics problems were investigated with both JFNK and CMFD-Coupling, it was concluded that CMFD-Coupling outperformed JFNK in terms of both accuracy and runtime for every problem. When applied to large full core problems with multiple sources of strong feedback enabled, CMFD-Coupling reduced the overall number of transport sweeps required for convergence.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2025

Developing aqueous solubilizing agents as an alternative to solvent extraction

Here, advancing separations science is important for the entire field of chemistry. One partitioning technique that would benefit from improvement is solvent extraction. Despite its effective and widespread use, the method suffers from some problems: generation of flammable organic waste, lengthy process times, and safety concerns associated with contacting organic solvents with acidic aqueous solutions. We developed an alternative separation method inspired by solvent extraction that side-steps those issues. Toward this end, we identified that the functionality of an extractant (an agent used in solvent extraction to pull analytes from the aqueous phase into the organic phase) would change if it was modified for water solubility. In this alternative scenario, the extractant transforms into an “aqueous solubilizing agent.” We discovered that adding this aqueous solubilizing agent alongside a precipitating agent caused the contaminants to precipitate, but not the analyte. This separation concept was demonstrated within the bounds of one of the most difficult partitioning problems, separating minor actinides (Am 3+ ) from lanthanides (Ln 3+ ). We discovered that the (HSO 3 Ph) 4 BTP (aq) aqueous solubilizing agent prevented Am 3+ (aq) from precipitating with Ln 3+ (aq) when f-element precipitating agents (NaF (aq) or HF (aq) ) were added. This separation boasts impressive Am 3+ (aq) recovery yield (90 ± 2 %), near quantitative Ln 3+ (aq) removal, and high separation factors [>3000, Am 3+ (aq) vs. Nd 3+ (aq) ]. It seems likely – given the large number of candidate extractants that could be modified for aqueous solubility and the numerous combinations of existing solubilizing and precipitating agents – that this alternative approach could be used broadly in place of solvent extraction and solve other important separation problems.

(HSO3Ph)4BTP(aq)↗

DOE OSTI2026

Paramagnetic Properties of Rare Earth Hydroxides, Oxalates, and Dibutyl Phosphates

Magnetic separations present a promising approach for the recovery of rare earth (RE) elements from mixtures, particularly when coupled with precipitation techniques that enhance process efficiency and selectivity. However, the magnetic properties of RE materials typically encountered in the separations industry are not well characterized. Here, we synthesized a series of RE materials, combining four REs – praseodymium (Pr), neodymium (Nd), terbium (Tb), and dysprosium (Dy) – with three precipitating agents – hydroxide, oxalate, and dibutyl phosphate. All materials showed typical paramagnetic behavior consistent with the Curie-Weiss law. At low temperatures, we observed weak antiferromagnetic correlations, which were more pronounced for the lighter RE ions (Pr, Nd). Particle morphology and crystallography analyses showed that the dibutyl phosphates were well-ordered metal-organic frameworks, the oxalates were crystals with mixed hydration states, and the hydroxides were mostly amorphous. Regardless of the degree of crystallinity, the effective magnetic moments aligned well with theoretical estimates based on Hund's rules and 4f electron configurations of the corresponding RE ions. For a given RE ion, the magnetophoretic response was thus determined by the size of the particles rather than specific metal-ligand coupling, with dibutyl phosphate promoting the formation of larger crystals that were the most strongly attracted to magnets.

Wang, Qingpu (ORCID:0000000156041571)↗

DOE OSTI2017

Dramatically improve the Safety Performance of Li ion Battery Separators and Reduce the Manufacturing Cost Using Ultraviolet Curing and High Precision Coating Technologies

The objective of this project was to improve the safety of operation of Lithium ion batteries (LIB)and at the same time significantly reduce the manufacturing cost of LIB separators. The project was very successful in demonstrating the improved performance and reduced cost attributed to using UV curable binder and high speed printing technology to place a very thin and precisely controlled ceramic layer on the surface of base separators made of polyolefins such as Polyethylene, Polypropylene and combinations of the two as well as cellulosic base separators. The underlying need for this new technology is the recently identified potential of fire in large format Lithium ion batteries used in hybrid, plug-in hybrid and electric vehicles. The primary potential cause of battery fire is thermal runaway caused by several different electrical or mechanical mechanisms; such as, overcharge, puncture, overheating, compaction, and internal short circuit. During thermal runaway, the ideal separator prevents ion flow and continues to physically separate the anode from the cathode. If the temperature of the battery gets higher, the separator may melt and partially clog the pores and help prevent ion flows but it also can shrink which can result in physical contact of the electrodes and accelerate thermal run-away even further. Ceramic coated separators eliminate many of the problems related to the usage of traditional separators. The ceramic coating provides an electrically insulating layer that retains its physical integrity at high temperature, allows for more efficient thermal heat transfer, helps reduce thermal shrinkage, and inhibits dendrite growth that could create a potential short circuit. The use of Ultraviolet (UV) chemistry to bind fine ceramic particles on separators is a unique and innovative approach primarily because of the instant curing of the UV curable binder upon exposure to UV light. This significant reduction in drying/curing time significantly reduces the cost of a ceramic coating. Another innovation is high precision, high speed, printing techniques that can apply a unique pattern of ceramic particles on base separators. The pattern will maximize ionic conductivity and minimize ceramic coating weight and thickness, while retaining the benefits of increased puncture strength, reduced thermal shrinkage and no decomposition. This project has met all of its goals and has been successfully completed. This successful completion has enabled Miltec UV to take the final steps leading to the commercialization of an innovative technology that will result in ceramic coated separators that can be manufactured and sold from the US, with increased production capacity, reduced cost, and improved battery safety.

25 ENERGY STORAGE↗

NASA NTRS2005

Closed Loop Active Flow Separation Detection and Control in a Multistage Compressor

Active closed loop flow control was successfully demonstrated on a full annulus of stator vanes in a low speed axial compressor. Two independent methods of detecting separated flow conditions on the vane suction surface were developed. The first technique detects changes in static pressure along the vane suction surface, while the second method monitors variation in the potential field of the downstream rotor. Both methods may feasibly be used in future engines employing embedded flow control technology. In response to the detection of separated conditions, injection along the suction surface of each vane was used. Injected mass flow on the suction surface of stator vanes is known to reduce separation and the resulting limitation on static pressure rise due to lowered diffusion in the vane passage. A control algorithm was developed which provided a proportional response of the injected mass flow to the degree of separation, thereby minimizing the performance penalty on the compressor system.

Bright, Michelle M.↗

DOE OSTI2019

Design and optimization of a fused-silica microfluidic device for separation of trivalent lanthanides by isotachophoresis

Abstract Elemental analysis of rare earths is essential in a variety of fields including environmental monitoring and nuclear safeguards; however, current techniques are often labor intensive, time consuming and/or costly to perform. The difficulty arises in preparing samples, which requires separating the very chemically and physically similar lanthanides. However, by transitioning these separations to the microscale, the speed, cost, and simplicity of sample preparation can be drastically reduced. Here, all fourteen non radioactive lanthanides (lanthanum through lutetium minus promethium) are separated by ITP in a serpentine fused silica microchannel in < 10 minutes with limits of detection on the order of picomoles. Electrophoretic electrodes are embedded in the microchip reservoirs so that voltage can be quickly applied and switched during operation. The limits of detection are quantified using a commercial C4D to calculate ITP zone lengths in combination with ITP theory. Optimization of experimental procedures and reproducibility based on statistical analysis of subsequent experimental results are addressed.

Bottenus, Daniel R.↗

DOE OSTI2019

Highly Efficient Separation/Recycling Palladium(II) Ions from Aqueous Solutions by Silica Gel-Coated Graphene Oxide Modified with Mercapto Groups

The separation and recovery of precious metals from secondary resources is an extremely important and challenging task. Herein, a novel sorbent is successfully prepared by chemical grafting and utilized for the extraction and separation of Pd(II) ions from aqueous solutions. Various characterization techniques, including Fourier transform infrared spectroscopy, scanning electron microscopy, Brunauer–Emmett–Teller, X-ray photoelectron spectroscopy, and element analysis, are employed to study the structure, morphology, porous nature, and chemical composition of the as-prepared SiO{sub 2}@GO-SH nanocomposites. The adsorption of Pd(II) ions on the SiO{sub 2}@GO-SH can be described by the pseudo-second-order model and Langmuir isotherm model. The adsorption equilibrium has been attained within 90 min and the maximum adsorption capacity of 423.2 mg g{sup −1} was attained at pH 3.5 and T = 308 K. The results reveal that SiO{sub 2}@GO-SH exhibits an excellent adsorption performance towards Pd(II) ions. In addition, we have proposed the adsorption mechanism for Pd(II) ions on the SiO{sub 2}@GO-SH surface. The adsorption of Pd(II) in SiO{sub 2}@GO-SH is a chemisorption process, where partial adsorbed Pd(II) ions are reduced to Pd(0) by functional groups (-SH) in the SiO{sub 2}@GO-SH. The results indicate that SiO{sub 2}@GO-SH can serve as a promising sorbent for the efficient separation and recovery of palladium from the palladium-containing secondary resources.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Wafer-Free Crystalline Silicon Solar Cells (CRADA Final Report)

This CRADA project, based on the DOE Solar Energy Technologies Office (SETO) Solar Prize Voucher program, helped Leap Photovoltaics to develop methodologies to immobilize Si particles by permanently attaching them to an Al-coated substrate and thereby forming carrier-selective electrical contacts to the Si particles. The bigger goal was to help Leap Photovoltaics develop these immobilized and contacted particle arrays into relatively efficient, inexpensive, and industrially relevant solar cells. By using Si particles instead of wafers in a solar cell absorber layer, one can avoid costs associated with growing monocrystalline Si ingots, then diamond-sawing them into wafers, then processing wafers into cells – a mainstream practice in today's high-efficiency Si cell and module technology. Monocrystalline or polycrystalline Si particles can be obtained in various ways: for example, Si kerf from wafer sawing is monocrystalline; recycled Si cell wafers can be ball-milled into particles; particles can be grown using various gas-phase techniques (mostly from SiH4). These Si particles can be assembled onto a substrate and serve as an absorber layer for the solar cell, absorbing photons to generate photocarriers. The challenge with this technique is to collect photocarriers from individual Si particles, with separation of photogenerated electrons to the negative cell’s electrode and positive photogenerated holes to the positive electrode. Therefore, each particle must have two isolated, carrier-selective contacts: one for electrons and one for holes. Plus, particles need to be immobilized onto a solid substrate. The goal of this work was focused on the immobilization of Si particles and creating hole-selective contact to them at the same time, using industrially relevant Si photovoltaic (PV) cell technology: screen printing of Al back-surface field electrodes. This is used in the mainstream Propane Education and Research Council (PERC) technology for hole-collecting contacts at the back of the cell. The work performed at NREL consisted of screen printing of Al metal paste on substrates, spreading Si particles onto it, and thermally processing the structures to form hole-collecting contacts. The final structures were investigated by scanning electron microscopy (SEM) after focused ion beam (FIB) cross-sectioning and polishing. The work was done jointly by NREL staff and Leap Photovoltaics (Leap PV) employees stationed at NREL. The samples were then taken to Leap PV for further processing. Training the Leap PV employee on various NREL techniques (laser cutting, screen printing, thermal processing, characterization) was part of the scope.

14 SOLAR ENERGY↗