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All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Structural and magnetic characterization of three tetranuclear Cu(II) complexes with face-sharing-dicubane/double-open-cubane like core framework

Three novel tetranuclear copper(II) complexes namely [Cu{sub 4}(L{sup 1}){sub 4}]∙2(dmf) (1), [Cu{sub 4}(L{sup 1}){sub 4}] (2) and [Cu{sub 4}(L{sup 2}){sub 2}(HL{sup 2}){sub 2}(H{sub 2}O){sub 2}]∙2(ClO{sub 4})·6(H{sub 2}O) (3) (H{sub 2}L{sup 1}, (E)−2-((1-hydroxybutan-2-ylimino)methyl)phenol; H{sub 2}L{sup 2}, (E)−2-((1-hydroxybutan-2-ylimino)methyl)−6-methoxyphenol)) were synthesized from the self-assembly of copper(II) perchlorate and the tridentate Schiff base ligands. The structural determination reveals that crystallizes in the monoclinic system with space group C2/c, whereas both the and crystallize in the triclinic system with space group P-1. and possess face-sharing dicubane core, on the other hand complex 3 has double open cubane core structure. The copper(II) ions in the cubane core are in distorted square planar geometries, and weak π…π and C–H…π interactions lead to formation of a 2D supramolecular architecture for and . At room temperature and , exhibit fluorescence with a quantum yield (Φ{sub s}) of 0.47, 0.49 and 0.38, respectively. Variable temperature magnetic susceptibility measurements in the range 2–300 K indicate an overall weak antiferromagnetic exchange coupling in all complexes. The PHI program was used to study their magnetic behaviour. In agreement with their face-sharing dicubane structure, a Hamiltonian of the type H =– J{sub 1}(S{sub 1}S{sub 2}+S{sub 1}S{sub 2’}+S{sub 1'}S{sub 2}+S{sub 1'}S{sub 2’}) – J{sub 2}S{sub 1}S{sub 1’}, where S{sub 1} = S{sub 1’} = S{sub 2} = S{sub 2’} = S{sub Cu} =1/2, was used for studying and . Simulations performed suggest magnetic exchange constants with values close to J{sub 1} =−20 cm{sup −1} and J{sub 2} =0 cm{sup -1} for these complexes. On the other hand, the spin Hamiltonian H =– J{sub 1}(S{sub 1}S{sub 4}+S{sub 2}S{sub 3}) – J{sub 2}(S{sub 1}S{sub 3}+S{sub 2}S{sub 4}) – J{sub 3}S{sub 1}S{sub 2}, where S{sub 1} = S{sub 2} = S{sub 3} = S{sub 4} = S{sub Cu} =1/2, was used to study the magnetic behaviour of the double open cubane core of and a good agreement between the experimental and simulated results was found by using the parameters g{sub 1} = g{sub 2} =2.20, g{sub 3} = g{sub 4} =2.18, J{sub 1} =−36 cm{sup -1}, J{sub 2} =−44 cm{sup -1} and J{sub 3} =0 cm{sup -1}. - Graphical abstract: Tetranuclear Cu(II) complexes with face-sharing-dicubane / double-open-cubane like core frameworks were synthesized and characterized by crystal structure and magnetic analysis. Variable temperature magnetic properties corroborate with their structural arrangement. - Highlights: • Novel tetranuclear copper(II) complexes have been structurally characterized. • Complexes possess face-sharing dicubane/double open cubane core structures. • Variable temperature magnetic measurements reveal antiferromagnetic coupling. • PHI program was used to explain the observed magnetic properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Syntheses and structural characterization of vanado-tellurites and vanadyl-selenites: SrVTeO{sub 5}(OH), Cd{sub 2}V{sub 2}Te{sub 2}O{sub 11}, Ca{sub 3}VSe{sub 4}O{sub 13}·H{sub 2}O and Ba{sub 2}VSe{sub 3}O{sub 10}

Four new quaternary vanado-tellurites and vanadyl-selenites, namely, SrVTeO{sub 5}(OH)(1), Cd{sub 2}V{sub 2}Te{sub 2}O{sub 11}(2), Ca{sub 3}VSe{sub 4}O{sub 13}·H{sub 2}O(3) and Ba{sub 2}VSe{sub 3}O{sub 10}(4) have been synthesized and structurally characterized by single crystal X-ray diffraction. The oxidation state of vanadium is +5 in tellurites 1 and 2 and +4 in selenites 3 and 4. The structures of SrVTeO{sub 5}(OH)(1) and Cd{sub 2}V{sub 2}Te{sub 2}O{sub 11}(2) compounds consist of (VTeO{sub 5}(OH)){sup 2-} and (V{sub 2}Te{sub 2}O{sub 11}){sup 4-}anionic chains respectively, which are built from tetrahedral VO{sub 4} and disphenoidal TeO{sub 4} moieties. Similarly the structures of Ca{sub 3}VSe{sub 4}O{sub 13}·H{sub 2}O(3) and Ba{sub 2}VSe{sub 3}O{sub 10}(4) respectively contain (VSe{sub 2}O{sub 7}){sup 2-} and (VSe{sub 3}O{sub 10}){sup 4-} anionic chains, which are made up of octahedral VO{sub 6} and pyramidal SeO{sub 3} units. Compounds 1 and 3 have been characterized by thermogravimetric and infrared spectroscopic methods. Compounds 1 and 2 are wide band gap semiconductors. - Graphical abstract: Ca{sub 3}VSe{sub 4}O{sub 13}·H{sub 2}O and Ba{sub 2}VSe{sub 3}O{sub 10} compounds contain (VSe{sub 2}O{sub 7}){sup 2-} and (VSe{sub 3}O{sub 10}){sup 4-} chains. - Highlights: • Four new vanado-tellurites and vanadyl-selenites are synthesized. • Their structural features are different. • The vanado-tellurites are wide band gap semiconductors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Synthesis and characterization of heterometallic uranyl pyridinedicarboxylate compounds

The incorporation of transition metals into hybrid uranyl materials can result in more diverse structural topologies and variations in physical and chemical properties. To explore the impact of transition metals on the uranyl cation, five uranium containing bimetallic chain compounds, [(UO{sub 2})M(PDC){sub 2}(H{sub 2}O){sub 4}]·4(H{sub 2}O) (PDC = 2,6 pyridinedicarboxylate; M = Ni{sup 2+}, Co{sup 2+}, Fe{sup 2+}, Zn{sup 2+,} and Cu{sup 2+}) were synthesized by evaporation of aqueous solutions at room temperature. The uranyl cation is complex by two PDC ligands and the transition metal cations bond to the complex to form a one-dimensional chain topology. The presence of the transition metal leads to the presence of a stronger uranyl oxo bonds as shown by the single-crystal X-ray diffraction data and the Raman spectra. Solid state diffuse reflectance UV/Visible spectra confirmed the presence of the transition metals in the structure by the broad bands that appeared at relevant wavelengths. - Graphical abstract: Synthesis and characterization of [(UO{sub 2})M(2,6 pyridinedicarboxylate)(H{sub 2}O){sub 4}]·4(H{sub 2}O) [M = Ni{sup 2+}, Co{sup 2+}, Fe{sup 2+}, Zn{sup 2+}, and Cu{sup 2+}] compounds reveals impact of transition metals in uranyl hybrid systems. Display Omitted - Highlights: • 5 heterometallic uranyl PDC compounds were synthesized and characterized by X-ray diffraction and spectroscopic techniques. • Uranyl PDC 1-D chain complexes that were linked via transition metal cations were further linked through π- πinteractions. • Structural data denotes shorter uranyl bonds in the presence of the transition metals and this is confirmed by Raman shifts. • Solid-state UV/Vis spectroscopy confirms the presence of transition metals in this system.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Perspective on identifying and characterizing the processes controlling iron speciation and residence time at the atmosphere-ocean interface

It is well recognized that the atmospheric deposition of iron (Fe) affects ocean productivity, atmospheric CO 2 uptake, ecosystem diversity, and overall climate. Despite significant advances in measurement techniques and modeling efforts, discrepancies persist between observations and models that hinder accurate predictions of processes and their global effects. Here, we provide an assessment report on where the current state of knowledge is and where future research emphasis would have the highest impact in furthering the field of Fe atmosphere-ocean biogeochemical cycle. These results were determined through consensus reached by diverse researchers from the oceanographic and atmospheric science communities with backgrounds in laboratory and in situ measurements, modeling, and remote sensing. We discuss i) novel measurement methodologies and instrumentation that allow detection and speciation of different forms and oxidation states of Fe in deliquesced mineral aerosol, cloud/rainwater, and seawater; ii) oceanic models that treat Fe cycling with several external sources and sinks, dissolved, colloidal, particulate, inorganic, and organic ligand-complexed forms of Fe, as well as Fe in detritus and phytoplankton; and iii) atmospheric models that consider natural and anthropogenic sources of Fe, mobilization of Fe in mineral aerosols due to the dissolution of Fe-oxides and Fe-substituted aluminosilicates through proton-promoted, organic ligand-promoted, and photo-reductive mechanisms. In addition, the study identifies existing challenges and disconnects (both fundamental and methodological) such as i) inconsistencies in Fe nomenclature and the definition of bioavailable Fe between oceanic and atmospheric disciplines, and ii) the lack of characterization of the processes controlling Fe speciation and residence time at the atmosphere-ocean interface. Such challenges are undoubtedly caused by extremely low concentrations, short lifetime, and the myriad of physical, (photo)chemical, and biological processes affecting global biogeochemical cycling of Fe. However, we also argue that the historical division (separate treatment of Fe biogeochemistry in oceanic and atmospheric disciplines) and the classical funding structures (that often create obstacles for transdisciplinary collaboration) are also hampering the advancement of knowledge in the field. Finally, the study provides some specific ideas and guidelines for laboratory studies, field measurements, and modeling research required for improved characterization of global biogeochemical cycling of Fe in relationship with other trace elements and essential nutrients. In conclusion, the report is intended to aid scientists in their work related to Fe biogeochemistry as well as program managers at the relevant funding agencies

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Mechanical and structural characterizations of gamma- and alpha-alumina nanofibers

We investigate the applicability of alumina nanofibers as a potential reinforcement material in ceramic matrix compounds by comparing the mechanical properties of individual nanofibers before and after annealing at 1400 °C. Mechanical testing is performed inside a scanning electron microscope (SEM), which enables observation in real time of the deformation and fracture of the fibers under loading, thereby providing a close-up inspection of the freshly fractured area in vacuum. Improvement of both the Young's modulus and the breaking strength for annealed nanofibers is demonstrated. Mechanical testing is supplemented with the structural characterization of the fibers before and after annealing using SEM, transmission electron microscopy and X-ray diffraction methods. - Highlights: • Mechanical properties of individual alumina nanofibers were measured using in situ SEM cantilevered beam bending technique. • Improvement of mechanical properties of the alumina fibers after annealing at 1400 °C is demonstrated. • Formation of branched structures is demonstrated and their mechanical properties are studied. • XRD and electron microscopy were used for structural characterization of untreated and annealed nanofibers.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

The stress, surface spin and dipolar interaction in the diluted NiFe{sub 2}O{sub 4} nanoparticles by the SiO{sub 2} matrix: Characterization and analyses

Well-dispersed uniform NiFe{sub 2}O{sub 4} nanoparticles (NPs) with an average particle size of 15.4 nm were synthesized by thermal decomposition of a metal–organic salt, and then were diluted in a SiO{sub 2} matrix via a sol–gel method with different concentration. The magnetization (M) dependence of NiFe{sub 2}O{sub 4}/SiO{sub 2} on the temperature (T) and on the applied magnetic field (H) was systematically characterized by the Quantum Design superconducting quantum interference device (SQUID) PPMS system. The results of M ~ H/T divide the magnetic properties between 10 K and 300 K into two regions: the low temperature blocked-particle regime below the blocking temperature T{sub B} and the interacting superparamagnetic (ISP) regime above T{sub B}. In the ISP regime, all samples deviate from the ideal Langevin superparamagnetic behavior due to the effective anisotropy induced by the stress, surface spins and interparticle dipolar interaction. The Raman spectra indicate that the stress in all samples exhibits the vibration behavior, which leads to the effective anisotropy and hence coercivity vibration. - Graphical abstract: Display Omitted - Highlights: • Increase of NiFe{sub 2}O{sub 4} NPs' concentration elevates T{sub B} and broadens ZFC peak. • NiFe{sub 2}O{sub 4}/SiO{sub 2} samples do not exhibit the ideal superparamagnetism above T{sub B}. • Stress leads to the effective anisotropy and hence H{sub c} vibration. • Stress vibration was characterized in detail by the Raman spectra.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Microstructure characterization of LAE442 magnesium alloy processed by extrusion and ECAP

The magnesium alloy LAE442 was processed by extrusion and equal channel angular pressing (ECAP) to achieve ultrafine grained microstructure. Detailed characterization of the microstructure was performed by scanning electron microscope, electron back scattered diffraction (EBSD) and transmission electron microscope. The initial, as-cast, microstructure consisted of large grains of ~ 1 mm. The grain refinement due to the processing by severe plastic deformation led to a decrease of the average grain size to ~ 1.7 μm after the final step of ECAP. A detailed characterization of secondary phases showed the precipitation of Al{sub 11}RE{sub 3}, Al{sub 2}Ca and Al{sub 10}RE{sub 2}Mn{sub 7} intermetallic phases. X-ray diffraction measurements proved that Li is dissolved within the magnesium matrix in the as-cast condition. Newly formed Al{sub 3}Li phase was observed after ECAP. The texture formation due to the extrusion and ECAP was different from that in the other magnesium alloys due to the activation of non-basal slip systems as a result of the decrease of the c/a ratio. - Highlights: • Combined extrusion and equal channel angular pressing results in significant grain refinement by factor 1000 approximately. • Al{sub 11}RE{sub 3}, Al{sub 2}Ca and Al{sub 10}RE{sub 2}Mn{sub 7} secondary phases are present in the as-cast material while Li was dissolved in the Mg matrix. • Extrusion and ECAP have no effect on the composition of the secondary phases but they influence strongly their distribution. • Texture evolution is affected by decrease of c/a ratio due to the presence of Li and resulting activation of non-basal slip.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Characterization of intermetallics in aluminum to zinc coated interstitial free steel joining by pulsed MIG brazing for automotive application

In order to meet the demand for lighter and more fuel efficient vehicles, a significant attempt is currently being focused toward the substitution of aluminum for steel in the car body structure. It generates vital challenge with respect to the methods of joining to be used for fabrication. However, the conventional fusion joining has its own difficulty owing to formation of the brittle intermetallic phases. In this present study AA6061-T6 of 2 mm and HIF-GA steel sheet of 1 mm thick are metal inert gas (MIG) brazed with 0.8 mm Al–5Si filler wire under three different heat inputs. The effect of the heat inputs on bead geometry, microstructure and joint properties of MIG brazed Al-steel joints were exclusively studied and characterized by X-ray diffraction, field emission scanning electron microscopy (FESEM), electron probe micro analyzer (EPMA) and high resolution transmission electron microscopy (HRTEM) assisted X-ray spectroscopy (EDS) and selective area diffraction pattern. Finally microstructures were correlated with the performance of the joint. Diffusion induced intermetallic thickness measured by FESEM image and concentration profile agreed well with the numerically calculated one. HRTEM assisted EDS study was used to identify the large size FeAl{sub 3} and small size Fe{sub 2}Al{sub 5} type intermetallic compounds at the interface. The growth of these two phases in A2 (heat input: 182 J mm{sup −1}) is attributed to the slower cooling rate with higher diffusion time (~ 61 s) along the interface in comparison to the same for A1 (heat input: 155 J mm{sup −1}) with faster cooling rate and shorter diffusion time (~ 24 s). The joint efficiency as high as 65% of steel base metal is achieved for A2 which is the optimized parameter in the present study. - Highlights: • AA 6061 and HIF-GA could be successfully joined by MIG brazing. • Intermetallics are exclusively studied and characterized by XRD, FESEM and EPMA. • Intermetallic formation by diffusion is worth considering or not. • HRTEM-EDS, SAD pattern identifies the morphologies and size of intermetallics. • A compromise concerning formation of IMC is necessary.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Investigation and characterization of ZnO single crystal microtubes

Morphological, structural, and optical characterization of microwave synthesized ZnO single crystal microtubes were investigated in this work. The structure and morphology of the ZnO microtubes are characterized using X-ray diffraction (XRD), single crystal diffraction (SCD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM). The results reveal that the as-synthesized ZnO microtube has a highly regular hexagonal cross section and smooth surfaces with an average length of 650–700 μm, an average outer diameter of 50 μm and wall thickness of 1–3 μm, possessing a single crystal wurtzite hexagonal structure. Optical properties of ZnO single crystal microtubes were investigated by photoluminescence (PL) and ultraviolet-visible (UV-vis) absorption techniques. Room-temperature PL spectrum of the microtube reveal a strong UV emission peak at around 375.89 nm and broad and a weak visible emission with a main peak identified at 577 nm, which was assigned to the nearest band-edge emission and the deep-level emission, respectively. The band gap energy of ZnO microtube was found to be 3.27 eV. - Highlights: • ZnO microtube length of 650–700 μm, diameter of 50 μm, wall thickness of 1–3 μm • ZnO microtube possesses a single crystal wurtzite hexagonal structure. • The crystal system is hexahedral oriented along a-axis with indices of (100). • A strong and sharp UV emission at 375.89 nm (3.29 eV) • One prominent absorption band around 378.88 nm (3.27 eV)

36 MATERIALS SCIENCE↗
DOE OSTI2016

Direct comparison of Fe-Cr unmixing characterization by atom probe tomography and small angle scattering

The fine microstructure obtained by unmixing of a solid solution either by classical precipitation or spinodal decomposition is often characterized either by small angle scattering or atom probe tomography. This article shows that a common data analysis framework can be used to analyze data obtained from these two techniques. An example of the application of this common analysis is given for characterization of the unmixing of the Fe-Cr matrix of a 15-5 PH stainless steel during long-term ageing at 350 °C and 400 °C. A direct comparison of the Cr composition fluctuations amplitudes and characteristic lengths obtained with both techniques is made showing a quantitative agreement for the fluctuation amplitudes. The origin of the discrepancy remaining for the characteristic lengths is discussed. - Highlights: •Common analysis framework for atom probe tomography and small angle scattering •Comparison of same microstructural characteristics obtained using both techniques •Good correlation of Cr composition fluctuations amplitudes from both techniques •Good correlation of Cr composition fluctuations amplitudes with classic V parameter.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Characterization of yttrium-rich precipitates in a titanium alloy weld

The yttrium-rich (Y-rich) precipitates that form in the fusion zone (FZ) of a Ti–5Al–1Sn–1Zr–1V–0.8Mo (wt.%) alloy, or Ti-5111, gas-tungsten arc welds (GTAW) were characterized. The filler metal was modified by a small concentration of Y in order to refine the microstructure and thus improve the FZ ductility. A high number density of nanoscale Y-rich precipitates were characterized in the weld FZ by atom probe tomography (APT) and scanning transmission electron microscopy (STEM). - Highlights: •A high number density of nanoscale precipitates were observed in the FZ matrix. •The nanoscale precipitates are enriched in yttrium. •Oxygen and sulfur are also present in the Y-rich precipitates and their interfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2017

X-ray micro computed tomography characterization of cellular SiC foams for their applications in chemical engineering

Open-cell SiC foams clearly are promising materials for continuous-flow chemical applications such as heterogeneous catalysis and distillation. X-ray micro computed tomography characterization of cellular β-SiC foams at a spatial voxel size of 13.6{sup 3} μm{sup 3} and the interpretation of morphological properties of SiC open-cell foams with implications to their transport properties are presented. Static liquid hold-up in SiC foams was investigated through in-situ draining experiments for the first time using the μ-CT technique providing thorough 3D information about the amount and distribution of liquid hold-up inside the foam. This will enable better modeling and design of structured reactors based on SiC foams in the future. In order to see more practical uses, μ-CT data of cellular foams must be exploited to optimize the design of the morphology of foams for a specific application. - Highlights: •Characterization of SiC foams using novel X-ray micro computed tomography. •Interpretation of structural properties of SiC foams regarding to their transport properties. •Static liquid hold-up analysis of SiC foams through in-situ draining experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Atomic scale characterization of white etching area and its adjacent matrix in a martensitic 100Cr6 bearing steel

Atom probe tomography was employed to characterize the microstructure and C distribution in the white etching area (WEA) of a martensitic 100Cr6 bearing steel subjected to rolling contact fatigue. Different from its surrounding matrix where a plate-like martensitic structure prevails, the WEA exhibits equiaxed grains with a uniform grain size of about 10 nm. Significant C grain boundary enrichment (>7.5at.%) and an overall higher C concentration than the nominal value are observed in the WEA. These results suggest that the formation of WEA results from severe local plastic deformation that causes dissolution of carbides and the redistribution of C. - Highlights: •APT has been applied to characterize the microstructure of white etching area (WEA). •Quantitative analyses of C distribution indicate that carbides are dissolved on the WEA. •WEA contains equiaxed grains with a uniform grain size of 10 nm. •C segregation at grain boundaries stabilizes the nanosized grain structure. •Formation of WEA is explained by severe local plastic deformation introduced by cyclic contact loading.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructure characterization of recycled IN718 powder and resulting laser clad material

Highlights: • A simple and efficient recycling procedure of IN718 powder has been defined for the laser cladding process. • Characterization of wasted and cleaned powder and comparison with new IN718 powder pointed out a slight diameter increase. • Microstructure characterization of clad builds showed differences between builds with new and recycled powders. • Clad microstructure and porosity increase remain constant static properties but decrease rupture strain after 3 reuses. • Without special precautions for cladding, the recycled powder can be reused twice without modifying the properties of IN718. - Abstract: The possibility to reuse the metal powder wasted in Laser Material Deposition (LMD) process has been evaluated and a simple procedure developed. LMD uses metal powder which is fed through a nozzle into the focal point of a laser, where it melts the powder and the substrate material. During the process, a high ratio of particles hits against an unmelted area and directly bounces off the deposited area. The efficiency ratio of deposition can drop to 40% depending on the configuration and spot size. This work deals with the design of a procedure to recollect and reuse the wasted powder of a nickel based superalloy IN718. After usage, powder is recollected, undesired fractions are magnetically segregated and aggregates are removed by sieving. The particles are mixed again and ready for reuse. In order to study the effectiveness of the process, no new powder has been added to the recovered fraction, and this procedure has been repeated five times. Experimental tests show that deposited material present similar properties than those obtained with new powder grains. But, after 3 reuses, the porosity content increases consequently and the rupture strain decreases strongly. The implementation of this process allows the improvement of the final efficiency, reducing costs and decreasing the hazardous powder amount.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Characterizing dislocation configurations and their evolution during creep of a new 12% Cr steel

Highlights: • Applicability of different techniques to characterize particular dislocation configuration. • XRD models in combination with TEM and EBSD to measure the dislocation density. • Substructure evolution during creep of a new 12% Cr steel is discussed. - Abstract: In this research, different types of dislocations are characterized and quantified in a newly developed 12% Cr steel in as-received as well as in crept conditions. X-ray diffraction (XRD) patterns are analyzed using three different models. The dislocation densities are determined employing the Convolution Multiple Whole Profile (CMWP) fitting, the analysis of the asymptotic part of the X-ray line profile (Groma's method), and the Rietveld refinement coupling Popa's and Williamson-Smallman approaches. CMWP method is used to measure the internal dislocation density inside the subgrains consisting of mobile and dipole dislocations, and the results show good agreement with Transmission Electron Microscopy (TEM) measurements. Groma's method is used to evaluate the total dislocation density, with results comparable to those obtained from the combination of Electron Backscatter Diffraction (EBSD) and TEM. Rietveld method gives the internal dislocation density or mobile dislocation density depending on the model chosen. The experimentally determined results such as creep strain, dislocation densities and subgrain size are compared with theoretical predictions and they are found in good agreement.

36 MATERIALS SCIENCE↗
DOE OSTI2018

EBSD characterization of the eutectic microstructure in hypoeutectic Fe-C and Fe-C-Si alloys

Highlights: • EBSD investigation of eutectic cementite and austenite in as-solidified low-alloy cast iron • Crystallographically independent growth of rapidly solidified cementite/austenite eutectic • Epitaxial growth of eutectic austenite from primary dendrites • Eutectic cementite and eutectoid ferrite frequently obey Bagaryatsky or Pitsch-Petch orientation relationship. - Abstract: Hypoeutectic Fe-C and Fe-C-Si model alloys were produced at different solidification conditions. Copper mold casting yields low cooling rates promoting the formation of a eutectic microstructure, which is characterized by two morphologies: elongated cementite plates and a rod structure growing perpendicular to the plates, i.e. austenite rods in a cementite matrix. Electron beam surface remelting generates a mainly plate-like eutectic due to rapid solidification. The microstructures were characterized by light-optical microscopy and electron backscatter diffraction (EBSD). The latter allows for a spatially resolved investigation of the growth crystallography of the eutectic phases. Thereby, a possible existence of crystallographic orientations relationships between cementite and austenite within the plate-like eutectic was assessed experimentally. The eutectic phases were found to grow largely crystallographically independently. Moreover, ferrite and eutectic cementite within the decomposed eutectic microstructure frequently comply with the Bagaryatsky or the Pitsch-Petch orientation relationship. Complementary X-ray diffraction (XRD) analysis reveals a pronounced cementite {002} texture in the microstructure produced by mold casting. Characteristic changes in the lattice parameters indicate that as-cast cementite is non-stoichiometric.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural characterization and comparison of Ti-6Al-4V manufactured with different additive manufacturing processes

In this work, the microstructures of Ti-6Al-4V manufactured by different additive manufacturing (AM) processes have been characterized and compared. The microstructural features that were characterized are the α lath thickness, grain boundary α (GB-α) thickness, prior β grain size and α colony size. In addition, the microhardnesses were also measured and compared. The microstructure of shaped metal deposited (SMD) Ti-6Al-4V material showed the smallest variations in α lath size, whereas the material manufactured with laser metal wire deposition-0 (LMwD-0) showed the largest variation. The prior β grain size was found to be smaller in material manufactured with powder bed fusion (PBF) as compared with corresponding material manufactured with the directed energy deposition (DED) processes. Parallel bands were only observed in materials manufactured with DED processes while being non-present in material manufactured with PBF processes.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Characterization of martensite-austenite constituents and micro-hardness in intercritical reheated and coarse-grained heat affected zones of API X70 HSLA steel

Highlights: • The influence of cold wire addition to the tandem submerged arc welding process on the ICRCGHAZ is investigated. • Comprehensive characterization of the microstructure and micro-hardness in the ICRCGHAZ of a HSLA steel is performed. • A lower fraction of finely distributed M-A formed in the ICRCGHAZ of TSAW + cold wire steel, leading to lower micro-hardness. • The aspect ratio and inter-particle spacing of M-A constituents decreased in the ICRCGHAZ through cold wire addition. - Abstract: The thermal cycles that high strength low alloy (HSLA) low carbon steels experience during welding inevitably affect the microstructure and mechanical properties of the weld joints. It is generally agreed that the coarse-grained heat affected zone (CGHAZ) and the intercritical reheated coarse-grained heat affected zone (ICRCGHAZ) in one-pass and multi-pass welding, respectively, have the poorest microstructure and mechanical properties relative to the rest of the steel joint. The martensite-austenite (M-A) constituents formed in the HAZ regions predominantly govern property deterioration in the CGHAZ and the ICRCGHAZ by promoting the initiation and propagation of micro-cracks. However, the characteristics of the M-A constituents, i.e., fraction, size, shape and aspect ratio, are strongly affected by the welding heat input. Accordingly, in this study, the aim was to evaluate the influence of a cold wire addition in conventional tandem submerged arc welding (TSAW + cold-wire) on the microstructure and micro-hardness in the CGHAZ and ICRCGHAZ. Microstructural characterization showed that a lower fraction of finely distributed M-A constituents associated with smaller prior austenite grains (PAGs) formed in the CGHAZ of the steel welded by the TSAW + cold-wire process (CW-OD weld) relative to that welded by the conventional TSAW process (TW-OD weld). Furthermore, the fraction of M-A constituents in the ICRCGHAZ of the CW-OD weld was decreased. A higher fraction of slender shaped M-A constituents in the ICRCGHAZ of the TW-OD weld resulted in an increase in the micro-hardness. The microstructure and micro-hardness changes associated with cold wire addition were attributed to the lower welding heat input and, consequently, the faster cooling rate with a corresponding reduction in the retention time in the austenitic region and ferrite/austenite region in the CGHAZ and ICRCGHAZ regions, respectively.

36 MATERIALS SCIENCE↗