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At least 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Coupling Interfacial Redox‐Reactions with In Situ Proton Generation for the Photoelectrochemical Separation of Rare‐Earth Elements

Abstract A dual‐function photoelectrochemical (PEC) separation system is demonstrated for rare‐earth element (REE) recovery. The sustainable release of the captured REEs is promoted through the synergistic integration of a redox‐reaction for electrostatic repulsion, and in situ proton generation for ion‐exchange, all driven by photoelectrochemistry. The platform consists of a redox‐copolymer, poly(ferrocenylpropyl methacrylamide‐ co ‐methacrylic acid) (P(FPMAm‐ co ‐MAA)) (PFM), conjugated with carbon nanotubes (CNTs) and coated onto titanium dioxide nanorods (TNRs). The (PFM‐CNT)/TNR spontaneously adsorbs up to 214.2 mg of Yttrium/g PFM by ion‐exchange, and demonstrates broad applicability for other REEs. The adsorbed REEs are released through the PEC oxidation of ferrocene (Fc) to ferrocenium (Fc + ), and the simultaneous PEC water splitting reactions at the TNRs that protonate the carboxylate binding groups. This dual photoelectrochemically‐driven mechanism for REE release is investigated by in situ pH measurements, as well as vibrational and X‐ray photoelectron spectroscopy. Through PEC approaches, a 68.8% reduction in energy consumption during REE recovery has been achieved compared to purely electrochemical systems, with a regeneration efficiency close to 100%. For NdFeB magnets from waste hard disk drives, Nd and Dy recovery efficiencies of 59.2 and 61.1% are achieved. The dual‐functionality of these copolymer PEC systems offers a sustainable platform for modulating critical element recovery.

Cho, Ki‐Hyun [Department of Chemical and Biomolecu↗
DOE OSTI2022

Interfacial Exchange Phenomena Driven by Ferromagnetic Domains

Abstract Interfacial proximity effects in antiferromagnetic/ferromagnetic (AFM/FM) bilayers control the exchange‐bias (EB) phenomena exploited in most spintronic devices, although still is lack of full understanding. Discordant results, including different exchange‐bias field ( H E ), coercivity ( H C ), or blocking temperature ( T B ) found even in similar systems, are usually ascribed to uncontrolled parameters, namely dissimilar interfacial defects, structure, and thicknesses. Here, it is shown in the very same sample that the magnetic domain structure during the magnetization reversal of the FM layer controls those mentioned effects. Simultaneous transport and vectorial‐resolved magnetic measurements performed in a V 2 O 3 /Co system during warming after different field cooling (FC) procedures exhibit a strong dependence on the FC angle and the domain structure of the FM layer. Remarkably, magnetization reversal analysis reveals 35 K of variation in T B and up to a factor of two in H E . These observations can be explained within the random‐field model for the interfacial exchange coupling with a fixed AFM domain structure in contact with a variable (angle‐dependent) FM domain structure. The results highlight the importance of the domain structure and magnetization reversal of the FM layer (not previously considered) in the EB phenomena, with potential to tailor interfacial effects in future spintronic devices.

36 MATERIALS SCIENCE↗
DOE OSTI2023

pH‐ and Redox‐Responsive Pickering Emulsions Based on Cellulose Nanocrystal Surfactants

Abstract Nanoparticle surfactants (NPSs), formed by using dynamic interactions between nanoparticles and complementary ligands at the liquid‐liquid interface, have emerged as “smart emulsifiers” with attributes of high emulsification efficiency, long‐term stability, and on‐demand emulsification/demulsification capabilities. However, only pH‐responsiveness can be adopted for the assembly of reported NPSs formed by electrostatic interactions. Here, we propose an alternative design strategy, by taking advantage of the ferrocenium (Fc + ) sulfate ion pair, to develop a new type of cellulose nanocrystal (CNC) surfactant. The Fc + groups are sensitive to pH, redox reagents and voltage, imparting the CNC surfactants and derived Pickering emulsions with multi‐stimuli‐responsiveness, and showing promising applications in controllable delivery, release, and biphasic biocatalysis.

Yang, Yang↗
DOE OSTI2023

pH- and Redox-Responsive Pickering Emulsions Based on Cellulose Nanocrystal Surfactants

Nanoparticle surfactants (NPSs), formed by using dynamic interactions between nanoparticles and complementary ligands at the liquid-liquid interface, have emerged as “smart emulsifiers” with attributes of high emulsification efficiency, long-term stability, and on-demand emulsification/demulsification capabilities. However, only pH-responsiveness can be adopted for the assembly of reported NPSs formed by electrostatic interactions. Here, we propose an alternative design strategy, by taking advantage of the ferrocenium (Fc + ) sulfate ion pair, to develop a new type of cellulose nanocrystal (CNC) surfactant. In conclusion, the Fc + groups are sensitive to pH, redox reagents and voltage, imparting the CNC surfactants and derived Pickering emulsions with multi-stimuli-responsiveness, and showing promising applications in controllable delivery, release, and biphasic biocatalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Divalent Titanium via Reductive N−C Coupling of a Ti IV Nitrido with π ‐Acids

The nitrido-ate complex [(PN) 2 Ti(N){μ 2 -K(OEt 2 )}] 2 (1) (PN − =(N-(2-P i Pr 2 -4-methylphenyl)-2,4,6-Me 3 C 6 H 2 ) reductively couples CO and isocyanides in the presence of DME or cryptand (Kryptofix222), to form rare, five-coordinate Ti II complexes having a linear cumulene motif, [K(L)][(PN) 2 Ti(NCE)] (E=O, L=Kryptofix222, (2); E=NAd, L=3 DME, (3); E=N t Bu, L=3 DME, (4); E=NAd, L=Kryptofix222, (5)). Oxidation of 2–5 with [Fc][OTf] afforded an isostructural Ti III center containing a neutral cumulene, [(PN) 2 Ti(NCE)] (E=O, (6); E=NAd (7), N t Bu (8)) and characterization by CW X-band EPR spectroscopy, revealed unpaired electron to be metal centric. Moreover, 1e − reduction of 6 and 7 in the presence of Kryptofix222cleanly reformed corresponding discrete Ti II complexes 2 and 5, which were further characterized by solution magnetization measurements and high-frequency and -field EPR (HFEPR) spectroscopy. Furthermore, oxidation of 7 with [Fc*][B(C 6 F 5 ) 4 ] resulted in a ligand disproportionated Ti IV complex having transoid carbodiimides, [(PN) 2 Ti(NCNAd) 2 ] (9). Comparison of spectroscopic, structural, and computational data for the divalent, trivalent, and tetravalent systems, including their 15 N enriched isotopomers demonstrate these cumulenes to decrease in order of backbonding as Ti II →Ti III →Ti IV and increasing order of π-donation as Ti II →Ti III →Ti IV , thus displaying more covalency in Ti III species. Lastly, we show a synthetic cycle whereby complex 1 can deliver an N-atom to CO and CNAd.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Theoretical and Experimental Investigation of Functionalized Cyanopyridines Yield an Anolyte with an Extremely Low Reduction Potential for Nonaqueous Redox Flow Batteries

Abstract Cyanopyridines and cyanophenylpyridines were investigated as anolytes for nonaqueous redox flow batteries (RFBs). The three isomers of cyanopyridine are reduced at potentials of −2.2 V or lower vs. ferrocene +/0 (Fc +/0 ), but the 3‐CNPy⋅ − radical anion forms a sigma‐dimer that is re‐oxidized at E ≈−1.1 V, which would lead to poor voltaic efficiency in a RFB. Bulk electrochemical charge‐discharge cycling of the cyanopyridines in acetonitrile and 0.50 M [NBu 4 ][PF 6 ] shows that 2‐CNPy and 4‐CNPy lose capacity quickly under these conditions, due to irreversible chemical reaction/decomposition of the radical anions. Density‐functional theory (DFT) calculations indicated that adding a phenyl group to the cyanopyridines would, for some isomers, limit dimerization and improve the stability of the radical anions, while shifting their E 1/2 only about +0.10 V relative to the parent cyanopyridines. Among the cyanophenylpyridines, 3‐CN‐6‐PhPy and 3‐CN‐4‐PhPy are the most promising as anolytes. They exhibit reversible reductions at E 1/2 =−2.19 and −2.22 V vs. ferrocene +/0 , respectively, and retain about half of their capacity after 30 bulk charge‐discharge cycles. An improved version of 3‐CN‐6‐PhPy with three methyl groups (3‐cyano‐4‐methyl‐6‐(3,5‐dimethylphenyl)pyridine) has an extremely low reduction potential of −2.50 V vs. Fc +/0 (the lowest reported for a nonaqueous RFB anolyte) and loses only 0.21 % of capacity per cycle during charge‐discharge cycling in acetonitrile.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Lanthanide Sulfate Recovery by Synergistic Dimethyl Ether and Na 2 SO 4 Fractional Crystallization

Lanthanides (Lns) are important to many technologies including magnets used in high-efficiency traction motors and generators. While commonly occurring in the environment and industrial waste streams, Ln are generally present at low concentrations. This work demonstrates synergistic Ln recovery from an aqueous magnet leachate to single ppm concentrations using Na 2 SO 4 addition and subsequent dimethyl ether-driven fractional crystallization (DME-FC) treatment. It is found that combining DME-FC with low concentrations of Na 2 SO 4 (≈0.1 M) results in synergistic isolation of Lns while making use of Na 2 SO 4 , an excessive byproduct of hydrometallurgical metal production. Combined Na 2 SO 4 + DME reduces Ln metal ion (Pr, Nd, Sm, Gd, Dy, and Ho) solubilities by 700–27,000x with final concentrations ranging from 2 ppm to 200 ppm. Separately, Na 2 SO 4 0.1 M provides a 10–200x reduction and DME provides a 90–1,400x reduction in Ln solubilities. Final Ln concentrations of the combined process are 99.8% lower than what is achieved with each individual process.

dimethyl ether↗
DOE OSTI2019

Evolution of photoresist layer structure and surface morphology under fluorocarbon‐based plasma exposure

Abstract Ion bombardment of photoresist materials during plasma etching results in the formation of a surface dense amorphous carbon (DAC) layer that contributes to both etch resistance and the development of surface roughness. Real‐time ellipsometric measurements/analysis reveals that a C 4 F 8 ‐containing plasma interacts with an Ar‐plasma‐formed DAC layer to produce a modified DAC/fluorocarbon (FC) layer by FC deposition/diffusion of fluorine into the surface. The depletion of the DAC layer via modification and ion bombardment causes the etch rate of the bulk layer to increase. As the modified surface layer is formed, a noticeable decrease in surface roughness decrease is observed. These findings provide an understanding of the mechanisms of atomic layer etching processes in photoresist materials.

Pranda, Adam↗
DOE OSTI2019

Fabrication and Magnetic Characterization of CFO/NiO and CFO/NiS Heterostructures

Magnetic analysis of different magnetic bilayers and multilayers is an important step for designing next-generation multiferroic heterostructures. In this study, we have investigated the magnetic interaction at the interface in CFO/NiO hetero-structures grown by pulsed laser deposition on sapphire substrates. The thin film heterostructure samples were characterized by means of X-ray diffraction, scanning electron microscopy (SEM), energy disruptive X-ray spectroscopy (EDS), and superconducting quantum interference device (SQUID) for magnetic measurements. The XRD analysis on different samples shows the crystalline growth of the thin films. The SEM-EDS analysis provides information about structural and elemental compositions of the heterostructure films. A SQUID magnetometer was used to investigate the temperature and field-dependent magnetic properties. To better understand the magnetic properties of the thin film heterostructure samples, zero field cool (ZFC) and field cool (FC) magnetization data were analyzed. At low temperature, ferromagnetic hysteresis loop was observed. A shift in the M-H hysteresis curve was observed for the FC data from the ZFC data, which indicates the presence of exchange bias effect. In addition, we have examined the effect of antiferromagnetic NiS thin films on ferromagnetism of CFO. This study on the magnetic interaction between a ferromagnetic layer and an antiferromagnetic layer can advance the frontier for applications in spin valves, magnetic sensors, and magnetic random access memory.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Magnetic Relaxation Experiments in CNT-Based Magnetic Nanocomposite

In this work, we discuss the relaxation of the magnetic moments in a novel carbon nanotube (CNT)-based nanocomposite synthesized by using chemical vapor deposition process. The material consists of a matrix of CNT filled by Fe-based nanoparticles. This structure is seen clearly by scanning and transmission. X-ray diffraction and Raman spectroscopy are used to detect the predominant Fe{sub 3}C phase and the CNT presence in the sample, respectively. The results obtained from both hysteresis cycles, M(H), and zero field cooled-field cooled (ZFC-FC) measurements confirm that the material is characterized by both a strong ferromagnetic exchange and random magnetic anisotropy. For the first time, we have been able to fit the magnetic relaxation data, M(t), by using both the two distributions of nanoparticles data deduced from the ZFC-FC data and the temperature dependence of the magnetic anisotropy obtained from the law of approach to saturation in random magnets. .

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Microstructural and Textural Evolutions during β → α/ω Transformation in Biomedical Ti-15Mo Alloy and Its Effects on Mechanical Performance

This study investigated the precipitation behaviors and mechanical performance of Ti-15Mo alloy subjected to different treatment conditions. The microstructures were analyzed via scanning electron microscopy and transmission electron microscopy. The tensile properties and resultant fracture surfaces were investigated to determine the relationship between the phase transformation and mechanical performance. The Ti-15Mo alloy had a notable elongation due to no observable precipitation during solution treatment plus quenching (STQ). A high ultimate tensile strength (UTS) was obtained with a considerable amount of ω precipitates transformed during air cooling after solution treatment (ST). The coarse precipitates and additional precipitation free zones in the Ti-15Mo alloy treated with furnace cooling (FC) after ST induced a decrease in UTS. Furthermore, the absence of a continuous grain boundary α phase resulted in a lower strength in the specimen annealed at 600 °C after hot rolling. The alloy iso-aged after STQ exhibited good tensile properties with a UTS of 920 MPa and an elongation of 15%. The texture and variant relationship of the precipitates was analyzed with x-ray diffraction and electron backscatter diffraction. The common variants of the β matrix influenced the nucleation of precipitates in the Ti-15Mo alloy annealed after hot rolling, and the precipitates showed an obvious {01-10}α main texture. The variant selection of α precipitates at the grain boundary was caused by the two adjacent β grains in the alloy treated by FC after ST.

36 MATERIALS SCIENCE↗
DOE OSTI2018

NK cell and IFN signatures are positive prognostic biomarkers for resectable pancreatic cancer

Highlights: • Integrative immunomonitoring was undertaken in resected pancreatic cancer patients. • Immunomonitoring employed flow cytometry, multiplex-bead assays and RMA-Seq. • Higher NK cell % in peripheral blood are associated with better prognosis. • Type I and II IFN signatures in the tumor are associated with better prognosis. • Epithelial mesenchymal transition is associated with early recurrence. To establish prognostic biomarkers and to identify potential novel therapeutic targets, we performed integrative immunomonitoring of blood and tumor in patients with resectable pancreatic cancer. Flow cytometry (FC) was employed for phenotyping immune cells, multiplex bead assays for plasma cytokine and chemokine determination, and RNA-Seq for the analysis of gene expression in the tumor. Nineteen pancreatic cancer patients were stratified into those with longer or shorter than median recurrence-free survival after surgery (median, 426 days). There were no significant differences between the two groups for clinical parameters including age, sex, surgical procedure, stage, or postoperative adjuvant therapy. However, we found that the percentages of NK cells as assessed by FC in peripheral blood mononuclear cells were higher in patients with late recurrence (P = .037). RNA-Seq data indicated no differences in the amount of immune cells or stromal cells between the two groups, although NK cells in the tumor did tend to be higher in patients with late recurrence (P = .058). Type I and II IFN signatures were enriched in late-recurring tumors (FDR q-value <0.001), while genes related to KRAS signaling and the epithelial mesenchymal transition (EMT) were enriched in early recurrence. We conclude that tumor-intrinsic properties of metastasis and recurrence influence prognosis, whereas NK cells that might contribute to prevent metastasis are associated with longer recurrence-free survival. Therefore, enhancement of NK cell activity and inhibition of the EMT and KRAS signaling might represent appropriate therapeutic targets following surgical resection of pancreatic cancer.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2013

Biaxial Flexural Strength of Poled Lead Zirconate Titanate under High Electric Field with Extended Field Range

In the present work, as-received poled lead zirconate titanate, or PZT 5A, was examined using ball-on-ring (BoR) mechanical testing coupled with an electric field. Electric fields in the range of 4Ec (Ec, coercive field) with controlled loading paths were applied, and mechanical tests at a substantial number of characteristic electric field levels were conducted. Commercial electronic liquid FC-40 was used to prevent the setup from dielectric breakdown under a high electric field. Weibull strength distribution was used to interpret the mechanical strength data. The data showed that the strength levels of the PZT-5A tested under OC (open circuit) in air and in FC-40 were almost the same. It was further revealed that , for the studied cases, the effect of loading history on the biaxial flexural strength of the PZT was significant in -Ec, but not in OC or zero field as well as 4Ec . An asymmetry V curve was observed for the characteristic strength-electric field graph, and the bottom of V curve was located near the negative coercive field. Microscopy analysis showed that surface-located volume-distributed flaws were the strength limiter and responsible for the failure of the tested PZT under electromechanical loadings.

Zhang, Kewei↗
DOE OSTI2024

Experimental study of mechanistic factors influencing solvent-driven fractional crystallization of calcium sulfate

To advance dimethyl ether-driven fractional crystallization (DME-FC), a more sustainable method of water treatment and mineral recovery, a range of chemical equilibria were measured. These include varying concentrations of miscible organic solvents (MOS) used to experimentally measure the solvent-induced solid-liquid equilibrium (SLE) of calcium sulfate (CaSO 4 ) in water. Seven MOS, including dimethyl ether (DME), acetonitrile (MeCN), 1,4-dioxane, tetrahydrofuran (THF), acetone, ethanol, and diethylamine, were screened to establish trends associated with molecular volume, functional groups, and physical properties. The effect of MOS on CaSO 4 removal differed at concentrations <0.15 mol fraction MOS; MOS with greater molecular volume (THF, 1,4-dioxane, and diethylamine) induced greater CaSO 4 precipitation on a per mole basis. The solvent-induced SLE for all MOS converged between 0.15 and 0.2 mol fraction MOS, reaching a CaSO 4 concentration consistent with a water to MOS hydration ratio of 5:1 to 6:1, which may correspond to the solvent generating a solution-based pseudo-clathrate structure with continuity within the solution. Finally, solution pseudo-clathrate structures provide a mechanistic basis for DME-FC.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Structural and magnetic properties of the M{sub 2}Ga{sub 2}Fe{sub 2}O{sub 9} (M=In, Sc) oxides

We report on the structural and magnetic properties of In{sub 2}Ga{sub 2}Fe{sub 2}O{sub 9} and Sc{sub 2}Ga{sub 2}Fe{sub 2}O{sub 9}. X-ray diffraction measurements confirmed the presence of a single orthorhombic phase, corresponding to the expected structure for M{sub 2}Ga{sub 2}Fe{sub 2}O{sub 9} (M=In, Sc). Neutron diffraction measurements show considerable cation disorder at different lattice sites, and suggest that there is no long range magnetic ordering down to T=10 K. Temperature dependent magnetization measurements show a separation between field-cooled and zero-field-cooled curves near T{sub f}≈19 K. Below this temperature the M(H) curves also exhibit history dependent behavior. The temperature dependent ac susceptibility shows a peak in the magnetic dissipation, with the temperature of the peak varying systematically with frequency suggesting that this feature may be associated with a glassy relaxation. Zero-field specific heat measurements down to 4 K do not reveal any long range magnetic ordering of these compounds, nor is there any transition to an ordered state under the application of a 7 T field. - Graphical abstract: Temperature variation of magnetization (ZFC and FC) of M{sub 2}Ga{sub 2}Fe{sub 2}O{sub 9} (M=In, Sc) samples at 0.01 T. The magnetization has a history dependence with a bifurcation between ZFC and FC data at the freezing temperature T{sub f}=19 K. The inset shows the enlargement for both oxides for temperatures below 30 K. Highlights: ► Chemical disorder study of the M{sub 2}Ga{sub 2}Fe{sub 2}O{sub 9} (M=In, Sc) compounds. ► Our study indicates for the first time a glassy magnetic ground state of this system. ► The glassy-like-behavior is due to magnetic frustration created by the site disorder.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Microstructural Progression of Shear-Induced Mixing in a CuNi Alloy

Shear deformation has been highlighted in multiple research efforts for its ability to impart mechanical properties improvements and unique microstructures. When used to process and densify powdered material, these shear-based consolidation techniques are commonly referred to as friction consolidation (FC). In this paper, we have examined the microstructural evolution from compacted Cu and Ni powders to a consolidated Cu0.5Ni0.5 alloy. We have shown various stages of porosity reduction and preferential deformation being accommodated by the more ductile material early in the process, leading to formation of a tortuous microstructural zone. Porosity reduction was extensive, decreasing from ~65% in the unprocessed powder to ~1% in the fully consolidated alloy. The final consolidated alloy showed roughly a 2X hardness improvement over the unalloyed, compacted material. Unique aspects of this work include demonstration of the ability to use FC processing to produce a submicron and equiaxed grain size in samples within a 0.5 to 2 minute processing time.

Overman, Nicole R.↗
DOE OSTI2019

Front-end ASIC for spectroscopic readout of virtual Frisch-grid CZT bar sensors

Compact multi-channel radiation detectors rely on low noise front-end application specific integrated circuits (ASICs) to achieve high spectral resolution. Here, a new ASIC developed to readout virtual Frisch-grid cadmium zinc telluride (VFG CZT) detectors for gamma ray spectroscopy is presented. Corresponding to each ionizing event in the detector, the ASIC measures the amplitude and timing at the anode, the cathode and four pad sense electrodes associated with each sensor in a detector array. The ASIC is comprised of 52 channels of which there are 4 cathode channels and 48 channels which can be configured as either anode channels with a baseline of 250 mV or pad sense channels to process induced signals with a baseline of 1.2 V. With a static power dissipation of 3 mW, each channel performs low-noise charge amplification, high-order shaping, peak and timing detection along with analog storage and multiplexing. The overall channel linearity was better than ± 1% with timing resolution down to 700 ps for charges greater than 8 fC in the 3 MeV range. With a 4 × 4 array of 6 mm × 6 mm × 20 mm virtual Frisch-grid bar sensors connected and biased, an electronic resolution of ≈270 e - rms for charges up to 100 fC in the 3.2 MeV range was measured. Spectral measurements obtained with the 3D correction technique demonstrated resolutions of 1.8% FWHM at 238 keV and 0.9% FWHM at 662 keV.

3D↗