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1. Importance of multimodal characterization and influence of residual Li ₂ S impurity in amorphous Li ₃ PS ₄ inorganic electrolytes

   https://doi.org/10.1039/d1ta02754a  

   Mirmira, Priyadarshini ; Zheng, Jin ; Ma, Peiyuan ; Amanchukwu, Chibueze V. ( September 2021 , Journal of Materials Chemistry A)

   Amorphous Li 3 PS 4 (LPS) solid-state electrolytes are promising for energy-dense lithium metal batteries. LPS glass, synthesized from a 3 : 1 mol ratio of Li 2 S and P 2 S 5 , has high ionic conductivity and can be synthesized by ball milling or solution processing. Ball milling has been attractive because it provides the easiest route to access amorphous LPS with a conductivity of 3.5 × 10 −4 S cm −1 (20 °C). However, achieving the complete reaction of precursors via ball milling can be difficult, and most literature reports use X-ray diffraction (XRD) or Raman spectroscopy to confirm sample purity, both of which have limitations. Furthermore, the effect of residual precursors on ionic conductivity and lithium metal cycling is unknown. In this work, we illustrate the importance of multimodal characterization to determine LPS phase and chemical purity. To determine the residual Li 2 S content in LPS, we show that (1) XRD and 31 P solid state nuclear magnetic resonance (ssNMR) are insufficient and (2) Raman loses sensitivity at concentrations below 12 mol% Li 2 S. Most importantly, we show that 7 Li ssNMR is highly sensitive. Using 7 Li ssNMR, we investigate the effect of ballmore »milling parameters and develop a robust and highly reproducible procedure for pure LPS synthesis. We find that as the residual Li 2 S precursor content increases, LPS conductivity decreases and lithium metal batteries exhibit higher overpotentials and poor cycle life. Our work reveals the importance of multimodal characterization techniques for amorphous solid-state electrolyte characterization and will enable better synthetic strategies for highly conductive electrolytes for efficient energy-dense solid-state lithium metal batteries.« less
2. Strengthened relaxor behavior in (1− x )Pb(Fe _0.5 Nb _0.5 )O ₃ – x BiFeO ₃

   https://doi.org/10.1039/C9TC05883D  

   Prah, Uroš ; Dragomir, Mirela ; Rojac, Tadej ; Benčan, Andreja ; Broughton, Rachel ; Chung, Ching-Chang ; Jones, Jacob L. ; Sherbondy, Rachel ; Brennecka, Geoff ; Uršič, Hana ( March 2020 , Journal of Materials Chemistry C)

   A systematic study of (1− x )Pb(Fe 0.5 Nb 0.5 )O 3 – x BiFeO 3 ( x = 0–0.5) was performed by combining dielectric and electromechanical measurements with structural and microstructural characterization in order to investigate the strengthening of the relaxor properties when adding BiFeO 3 into Pb(Fe 0.5 Nb 0.5 )O 3 and forming a solid solution. Pb(Fe 0.5 Nb 0.5 )O 3 crystalizes in monoclinic symmetry exhibiting ferroelectric-like polarization versus electric field ( P–E ) hysteresis loop and sub-micron-sized ferroelectric domains. Adding BiFeO 3 to Pb(Fe 0.5 Nb 0.5 )O 3 favors a pseudocubic phase and a gradual strengthening of the relaxor behavior of the prepared ceramics. This is indicated by a broadening of the peak in temperature-dependent permittivity, narrowing of P–E hysteresis loops and decreasing size of ferroelectric domains resulting in polar nanodomains for x = 0.20 composition. The relaxor behavior was additionally confirmed by Vogel–Fulcher analysis. For the x ≥ 0.30 compositions, broad high-temperature anomalies are observed in dielectric permittivity versus temperature measurements in addition to the frequency-dispersive peak located close to room temperature. These samples also exhibit pinched P–E hysteresis loops. The observed pinching is most probably related to the reorganization of polar nanoregionsmore »under the electric field as shown by synchrotron X-ray diffraction measurements as well as by piezo-response force microscopy analysis, while in part affected by the presence of charged point defects and anti-ferroelectric order, as indicated from rapid cooling experiments and high-resolution transmission electron microscopy, respectively.« less
3. Corrosion Behavior and Hardness of Binary Mg Alloys Produced via High-Energy Ball-Milling and Subsequent Spark Plasma Sintering

   https://doi.org/10.5006/3633  

   Farooq Khan, Mohammad Umar ; Larimian, Taban ; Borkar, T. ; Gupta, R.K. ( November 2020 , Corrosion)

   In this work, nine nanocrystalline binary Mg alloys were synthesized by high-energy ball milling. The compositions, Mg-5 wt% M (M-Cr, Ge, Mn, Mo, Ta, Ti, V, Y, and Zn), were milled with the objective of achieving non-equilibrium alloying. The milled alloys were consolidated via cold compaction (CC) at 25°C and spark plasma sintering (SPS) at 300°C. X-ray diffraction (XRD) analysis indicated grain refinement below 100 nm, and the scanning electron microscopy revealed homogeneous microstructures for all compositions. XRD analysis revealed that most of the alloys showed a change in the lattice parameter, which indicates the formation of a solid solution. A significant increase in the hardness compared to unmilled Mg was observed for all of the alloys. The corrosion behavior was improved in all of the binary alloys compared to milled Mg. A significant decrease in the cathodic kinetics was evident due to Ge and Zn additions. The influence of the alloying elements on corrosion behavior has been categorized and discussed based on the electrochemical response of their respective binary Mg alloys.
4. Regional and Local Stratigraphic Markers in Three Hudson River Cores Taken Near Peekskill, New York: Core LWB 4-5

   Abdul, B. ; Adeghe, S. ; Diallo, M. B. ; McCann, B. ; Abbott, D. H. ; Bostick, B. C. ; Chang, C. ; Block, K. A. ( December 2018 , American Geophysical Union, Fall Meeting 2018, abstract #B53I-2167)

   We have been studying the stratigraphy of core LWB 4-5 taken in 2001 in the Hudson River 1.5 km north of the transit of the Peekskill meteorite in October 1992. We measured magnetic susceptibility and elemental composition at 1 cm intervals down to 50 cm and then at 5 cm intervals down to 108 cm. Magnetic susceptibilities are unusually high (above 20 cgs units) from 12-19 cm and again at 31 cm. The level at 31 cm contains mm-sized fragments of Fe oxide. X-Ray Fluorescence spectroscopy revealed high Ni/Cr levels concentrated from 9-11 cm and again below 97 cm. We found tektite-like spheroids, dumbbells and teardrops from 8-15 cm depth. They are glasses and they contain appreciable K, consistent with an origin as true tektites but we have not identified the source. Overall, we interpret the high susceptibility, high Ni/Cr and possibly tektite bearing layer as a resulting from the fall of one of the bodies postulated to have fallen with the Peekskill meteorite in 1992. A 1992 age for the top of the Peekskill layer at 8-9 cm depth is consistent with a uniform sedimentation rate in the core and the occurrence of the base of modern Pb atmore »97 cm depth. From previous work on cores from Central Park Lake, the base of modern Pb represents the year 1880 A.D. We also found other prominent horizons whose ages fit a linear sedimentation rate model. We found a step change in As/Pb ratio whose inferred age matches 1988, the year when Pb and Cu arsenide were banned as pesticides. Our core exhibits peaks in Ca and Sr content and a minor susceptibility peak at 17.5 depth that may represent the 1980 "Great Catskill Toilet Flush" Hudson River flood event. The Catskills contain abundant marine limestone that could serve as a source for Ca and Sr. A prominent susceptibility peak at 37.5 cm could represent a flood in 1955. We also found a peak in Pb at 50 cm depth whose inferred age matches that of the cessation of incinerator burning in 1938. 137Cs and 210Pb ages are in progress and may be available by the time of the meeting. The high Pb and As levels in parts of LWB 4-5 are supported by examination of the coarse fraction. We found two bright orange grains, both with carbon rich coatings. One grain analyses on the X-ray analyzer of an SEM as 8%C, 70% Pb, 17%As and 2% Cu. The second grain analyzes as 10% C, 43% Pb, 1% Ca, 2% P, 27% As, 4% Fe, 2% Ni, 1% Si, and 6% Zn. All analyses are in wt.% on an oxygen free basis.« less
5. The Effect of Bulk Residual Stress on Milling-Induced Residual Stress and Distortion

   https://doi.org/10.1007/s11340-022-00843-9  

   Chighizola, C. R. ; D’Elia, C. R. ; Jonsson, J. E. ; Weber, D. ; Kirsch, B. ; Aurich, J. C. ; Linke, B. S. ; Hill, M. R. ( April 2022 , Experimental Mechanics)

   Distortion arises during machining of metallic parts from two main mechanisms: 1) release of bulk residual stress (BRS) in the pre-form, and 2) permanent deformation induced by cut tools. Interaction between these mechanisms is unexplored.

   Assess this interaction using aluminum samples that have a flat surface with variations of BRS, where that surface is subsequently milled, and we observe milling-induced residual stress (MIRS) and distortion.

   Plate samples are cut from two kinds of large blocks, one kind stress-relieved by stretching and a second kind solution heat treated, quenched and aged. The BRS field in the plates is known from a recent series of measurements, being small in the stress relieved plates (within ±20 MPa) and large (±100 MPa) in the quenched plates, varying from tension to compression over the surface that is milled. MIRS is measured following milling using hole-drilling. Distortions of thin wafers cut at the milled surfaces are used to elucidate BRS/MIRS interactions. A finite element (FE) model and a strength of materials model are each used to assess consistency between wafer distortion and measured MIRS.

   Milling in samples with high BRS magnitude changes the directions of MIRS and distortion relative to the milling direction, with the direction ofmore »maximum curvature rotating toward or away from the milling direction depending on the sign and direction of BRS. High magnitude BRS was also found to increase the wafer peak arc height, nearly doubling the amount found in low BRS samples.

   Measured residual stress and observed wafer distortion both show interactions between MIRS and BRS. Stress analysis models show that the differences in measured MIRS are consistent with the differences in observed distortion.

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