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DOE OSTI2023

Ultrafast Optomechanical Strain in Layered GeS

Strong coupling between light and mechanical strain forms the foundation for next-generation optical micro- and nano-electromechanical systems. Such optomechanical responses in two-dimensional materials present novel types of functionalities arising from the weak van der Waals bond between atomic layers. In this paper, by using structure-sensitive megaelectronvolt ultrafast electron diffraction, we report the experimental observation of optically driven ultrafast in-plane strain in the layered group IV monochalcogenide germanium sulfide (GeS). Surprisingly, the photoinduced structural deformation exhibits strain amplitudes of order 0.1% with a 10 ps fast response time and a significant in-plane anisotropy between zigzag and armchair crystallographic directions. Rather than arising due to heating, experimental and theoretical investigations suggest deformation potentials caused by electronic density redistribution and converse piezoelectric effects generated by photoinduced electric fields are the dominant contributors to the observed dynamic anisotropic strains. Our observations define new avenues for ultrafast optomechanical control and strain engineering within functional devices.

2D materials↗

DOE OSTI2015

Investigations of the optical and EPR properties of LiGa{sub 5}O{sub 8}:Cr{sup 3+} phosphor

Highlights: • Cr{sup 3+} doped LiGa{sub 5}O{sub 8} phosphor was synthesized by solution combustion synthesis. • Morphological studies show the non-uniform distribution of particles. • Photoluminescence spectra of Cr{sup 3+} doped LiGa{sub 5}O{sub 8} showed the characteristic Cr{sup 3+} peaks. • EPR spectrum showed Cr{sup 3+} ions in tetragonally distorted octahedral symmetry. - Abstract: Red emitting LiGa{sub 5}O{sub 8} doped with Cr{sup 3+} ions has been prepared by a low temperature solution combustion route. The as-prepared phosphor was studied using X-ray diffraction and scanning electron microscopic techniques. The optical spectrum exhibits two broad bands characteristic of Cr{sup 3+} ions in an octahedral symmetry. Upon excitation at 590 nm, the material displays narrow red emission line centered at 715 nm due to the {sup 2}E{sub g} → {sup 4}A{sub 2g} transition of Cr{sup 3+} ions. Electron paramagnetic resonance analyses of the sample confirm the presence of Cr{sup 3+} in the LiGa{sub 5}O{sub 8} matrix.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Ultrasound resolution beats the diffraction limit

With an acoustic analogue of a Nobel Prize–winning optical technique, researchers can acquire detailed images quickly.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2018

One-Step Synthesis of Hybrid Core-Shell Metal-Organic Frameworks

Epitaxial growth of MOF-on-MOF composite is an evolving research topic in the quest for multifunctional materials. During prior approaches, the core–shell MOFs were synthesized via a stepwise strategy that involved growing the shell-MOFs on top of the preformed core-MOFs with matched lattice parameters. Yet, the inconvenient stepwise synthesis and the strict lattice-matching requirement have limited the preparation of core–shell MOFs. Herein, we demonstrate that hybrid core–shell MOFs with mismatching lattices can be synthesized under the guidance of nucleation kinetic analysis. A series of MOF composites with mesoporous core and microporous shell were constructed and characterized by optical microscopy, powder X-ray diffraction, gas sorption measurement, and scanning electron microscopy. Isoreticular expansion of microporous shells and orthogonal modification of the core was realized to produce multifunctional MOF composites, which acted as size selective catalysts for olefin epoxidation with high activity and selectivity.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Effect of SO 2 on oxidation of metallic materials in CO 2 /H 2 O-rich gases relevant to oxyfuel environments: Effect of SO 2 on oxidation of metallic materials

In an oxyfuel plant, heat exchanging metallic components will be exposed to a flue gas that contains substantially higher contents of CO2, water vapor, and SO2 than conventionalflue gases. In the present study, the oxidation behavior of the martensitic steel P92 was studied in CO2-and/or H2O-rich gas mixtures with and without addition of SO2. For this purpose, the corrosion of P92 at 550 8C up to 1000 h in Ar–H2O–SO2, Ar–CO2–SO2, Ar–CO2–O2–SO2 and simulated oxyfuel gas (Ar–CO2–H2O–O2–SO2) was compared with the behavior in selected SO2-free gases. The oxidation kinetics were estimated by a number of methods such as optical microscopy, scanning electron microscopy with energy and wave length dispersive X-ray analysis, glow discharge optical emission spectroscopy, X-ray diffraction as well as transmission electron microscopy. The experimental results revealed that the effect of SO2 addition on the materials behavior substantially differed, depending on the prevailing base gas atmosphere. The various types of corrosion attack affected by SO2 could not be explained by solely comparing equilibrium activities of the gas atmospheres with thermodynamic stabilities of possible corrosion products. The results were found to be strongly affected by relative rates of reactions of the various gas species occurring within the frequently porous corrosion scales as well as at the scale/gas-and scale/alloy interfaces.Whereas SO2 addition to Ar–CO2 resulted in formation of an external mixed oxide/sulflde layer, the presence of SO2 in oxyfuel gas and in Ar–H2O–SO2 resulted in Fe-sulflde formation near the interface between inner and outer oxide layer as well as Cr-sulflde formation in the alloy. In the latter gases, the presence of SO2 seemed to have no dramatic effect on oxide scale growth rates.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effect of Rolling Temperature on Fracture Properties of INRAFMS at Different Temperatures

Two heats of Indian reduced activation ferritic / martensitic steel have been produced with similar chemical composition and identical process parameters except the start and final rolling temperature referred as P950 and P1050, respectively. Fracture behaviours of both the heats have been evaluated, and it was found that quasistatic fracture properties are better for P1050 than P950. An attempt is made to establish the reasons for the observed behaviour through optical, scanning electron microscopic, electron backscatter diffraction and transmission electron microscopic studies. These variations are attributed to the difference in rolling temperature of both heats. P1050 meets the acceptance criteria as per Indian specifications, and it compares favourably with the international grades of equivalent RAFM steels.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Structure/property (constitutive and spallation response) of additively manufactured 316L stainless steel

For additive manufacturing (AM) of metallic materials, the certification and qualification paradigm needs to evolve as there is currently no broadly accepted “ASTM- or DIN-type” additive manufacturing certification process or AM-produced material specifications. Accordingly, design, manufacture, and subsequent implementation and insertion of AM materials to meet engineering applications requires detailed quantification of the constitutive (strength and damage) properties of these evolving materials, across the spectrum of metallic AM methods, in comparison/contrast to conventionally-manufactured metals and alloys. For this paper, cylindrical samples of 316L SS were produced using a LENS MR-7 laser additive manufacturing system from Optomec (Albuquerque, NM) equipped with a 1 kW Yb-fiber laser. The microstructure of the AM-316L SS was characterized in both the “as-built” AM state and following a heat-treatment designed to obtain full recrystallization to facilitate comparison with annealed wrought 316L SS. The constitutive behavior as a function of strain rate and temperature was characterized and is compared to that of annealed wrought 316L SS plate material. The dynamic shock-loading-induced damage evolution and failure response of all three 316L SS materials was quantified using flyer-plate impact driven spallation experiments at peak stresses of 4.7 and 6.5 GPa. The spall strength of AM-produced 316L SS and the recrystallized-AM-316L SS were found to decrease with increasing peak shock stress while the annealed wrought 316L SS spall strength remained essentially constant. Finally, the damage evolution, characterized using optical metallography and electron-backscatter diffraction (EBSD), was found to vary significantly across the three 316L SS microstructures while the three samples loaded to a peak shock stress of 6.5 GPa displayed only ~12% differences in spall strength.

316L SS↗

DOE OSTI2024

Infrared nanoimaging and nanospectroscopy of electrochemical energy storage materials and interfaces

Electrochemical interfaces are central to the function and performance of energy storage devices. Thus, the development of new methods to characterize these interfaces, in conjunction with electrochemical performance, is essential for bridging the existing knowledge gaps and accelerating the development of energy storage technologies. Of particular need is the ability to characterize surfaces or interfaces in a non-destructive way with adequate resolution to discern individual structural and chemical building blocks. To this end, sub-diffraction-limit low-energy infrared optical probes that exploit near-field interactions within atomic force microscopy platforms, such as pseudoheterodyne nanoimaging, photothermal nanoimaging and nanospectroscopy, and nanoscale Fourier transform infrared spectroscopy, are all powerful emerging techniques. These are capable of non-destructive surface probing and imaging at nanometer resolution. This review outlines recent efforts to characterize ex situ, in situ, and operando electrode materials and electrochemical interfaces in rechargeable batteries with these advanced infrared near-field probes.

25 ENERGY STORAGE↗

DOE OSTI2014

Highly transparent ammonothermal bulk GaN substrates

A novel apparatus has been employed to grow ammonothermal (0001) gallium nitride (GaN) with diameters up to 2 in The crystals have been characterized by x-ray diffraction rocking-curve (XRC) analysis, optical and scanning electron microscopy (SEM), cathodoluminescence (CL), and optical spectroscopy. High crystallinity GaN with FWHM values about 20-50 arcsec and dislocation densities below 1 x 10(5) cm(-2) have been obtained. High optical transmission was achieved with an optical absorption coefficient below 1 cm(-1) at a wavelength of 450 nm. (C) 2014 Elsevier B.V. All rights reserved.

Jiang, WK↗

DOE OSTI2018

Effect of Ce addition on the microstructure and properties of Al-Cu-Mn-Mg-Fe lithium battery shell alloy

Highlights: • Al{sub 6}(Mn, Fe) particles could be remarkably refined by Ce alloying. • Ce addition to the alloy promoted precipitation of S' phase. • Ce-containing alloy had higher tensile strength than that of Ce-free alloy. • Ce-containing alloy had positive corrosion potential and lower corrosion current density. - Abstract: Effect of Ce addition on the microstructures, mechanical properties and electrochemical properties of Al-Cu-Mn-Mg-Fe lithium battery alloy was investigated by optical microscope (OM), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), tensile testing and electrochemical testing. Experimental results indicate that Ce addition resulted in the formation of Al{sub 8}Cu{sub 4}Ce phase in the Al-Cu-Mn-Mg-Fe alloy. The Ce-containing precipitates nucleated and grew up along the surface of Al{sub 6}(Mn, Fe) precipitates. Al{sub 6}(Mn, Fe) precipitates could be remarkably refined by Ce alloying. The aging precipitation behavior of S' phases could be promoted after Ce addition to the alloy. In comparison with Ce-free alloy, the Ce-containing alloy had higher tensile strength at both low temperature and elevated temperature. Especially at 200 °C, the yield strength and tensile strength of Ce-containing alloy substantially increased by 23.4% and 27.08%, respectively. Potentiodynamic polarization testing indicated that the Ce-containing alloy had a more positive corrosion potential and a lower corrosion current density.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Formation of {332}<113>β twins from parent {130}<310>α″ plastic twins in a full α″ Ti-Nb alloy by annealing

Highlights: • The solution-treated, deformed and annealed structures of a full α″ martensitic Ti-23Nb (at.%) alloy have been investigated. • The self-accommodated feature of the α″ martensites is presented by EBSD. • The martensites transform into β phase after annealing and the β phase is retained to room temperature by furnace-cooling. • Direct evidence is given for the formation of {332}{sub β} twins from {130}{sub α″} plastic twins by ex-situ EBSD observations. • A possible {351}<1 1-bar 2>{sub α″} twinning in α″ phase that corresponds to {332}<11 3-bar >{sub β} is proposed. - Abstract: The solution-treated (ST), deformed and subsequently annealed microstructures of a full α″ martensitic Ti-23Nb at.% alloy have been investigated by optical micrograph (OM), X-ray diffraction (XRD) and electron back-scattered diffraction (EBSD). The results show that both the self-accommodated α″ martensites in ST sample and re-orientated martensitic structure and plastic {130}{sub α″} twins in the Deformed sample fully transformed into the β phase with a small amount of the ω phase by annealing. The ex-situ EBSD measurements showed that the {332}{sub β} twins occur in the Annealed sample, which correspond to the {130}{sub α″} plastic twins of the α″ phase in the Deformed sample, and thus give a direct evidence that the {332}{sub β} twins in the β phase form from the reverse martensitic transformation of the {130}{sub α″} plastic twins in the α″ phase. Moreover, it's also expected from EBSD results that in addition to {130}<3 1-bar 0>{sub α″}, the possible <{351}<1 1-bar 2>{sub α″} twinning system of the α″ phase corresponds to the {332}<11 3-bar >{sub β} twinning of the β phase.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Reaction of Pb(II) and Zn(II) with Ethyl Linoleate To Form Structured Hybrid Inorganic–Organic Complexes: A Model for Degradation in Historic Paint Films

To investigate soap formation in drying oils in historic paints, the reaction between metal acetates (K + , Zn 2+ , Pb 2+ ) and ethyl linoleate (EL) was studied using optical microscopy, X-ray powder diffraction, and electron microscopy. Pb(II) and Zn(II) react rapidly with EL to form highly structured, spherulitic, luminescent crystallites that aggregate. Evidence from Fourier transform infrared (FTIR) and scanning electron microscopy/energy dispersive X-ray analysis and high-resolution synchrotron powder X-ray diffraction indicates that these are organic–inorganic hybrid complexes or coordination polymers. FTIR absorbance peaks at ca. 1540 cm –1 for Pb(II) and ca. 1580 cm –1 for Zn(II) are consistent with the formation of carboxylate complexes. The complexes formed offer insight into the degradation processes observed in oil paint films, suggesting that soap formation is rapid when metal ions are solubilized and can occur with unsaturated fatty acids that are present in fresh oils. These complexes may account for the atypical luminescence observed in lead-containing cured oil paint films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Naphthalene Bis(4,8-diamino-1,5-dicarboxyl)amide Building Block for Semiconducting Polymers

We report a new naphthalene bis(4,8-diamino-1,5-dicarboxyl)amide (NBA) building block for polymeric semiconductors. Computational modeling suggests that regio-connectivity at the 2,6- or 3,7-NBA positions strongly modulates polymer backbone torsion and, therefore, intramolecular π-conjugation and aggregation. Optical, electrochemical, and X-ray diffraction characterization of 3,7- and 2,6-dithienyl-substituted NBA molecules and corresponding isomeric NBA-bithiophene copolymers P1 and P2, respectively, reveals the key role of regio-connectivity. Charge transport measurements demonstrate that while the twisted 3,7-NDA-based P1 is a poor semiconductor, the planar 2,6-functionalized NBA polymers (P2–P4) exhibit ambipolarity, with μe and μh of up to 0.39 and 0.32 cm2/(V·s), respectively.

Eckstein, Brian J.↗

DOE OSTI2014

Modified chemical route for deposition of molybdenum disulphide thin films

Molybdenum disulphide (MoS{sub 2}) thin films were deposited on quartz substrates using a modified chemical route. Sodium molybdate and sodium sulphide were used as precursors for molybdenum and sulphur respectively. The route involves formation of tetrathiomolybdate ions (MoS{sub 4}{sup 2−}) and further reduction by sodium borohydride to form MoS{sub 2}. The deposition was performed at room temperature. The deposited films were annealed in argon atmosphere at 1073 K for 1 hour to improve its crystallinity. The deposited films were characterized using scanning electron microscopy (SEM) for morphology, UV-Vis absorption spectroscopy for optical studies and X-ray diffraction (XRD) for structure determination.