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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 721 records · Page 40
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Microstructural characterization of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint

The microstructure of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint was characterized in this work by optical microscopy, scanning electron microscopy (with electron back scattering diffraction) and micro-hardness testing. Epitaxial growth and competitive growth are evident in the 308L–316L fusion boundary regions. A martensite layer, carbon-depleted zones, and type-II and type-I boundaries are found in the SA508–309L fusion boundary regions, while only martensite and austenite mixed zones are observed in the SA508–308L fusion boundary regions. The microstructure near the fusion boundary and the microstructure transition in the SA508 heat affected zone are quite complex. Both for SA508–309L/308L and 308L–316L, the highest residual strain is located on the outside of the weldment. The residual strain and the grain boundary character distribution change with increasing distance from the fusion boundary in the heat affected zone of 316L. Micro-hardness measurements also reveal non-uniform mechanical properties across the weldment. - Highlights: • The microstructure of SA508 HAZ, especially near the FB, is very complex. • The outside of the dissimilar metal welded joint has the highest residual. • The micro-hardness distributions along the DMWJ are non-uniform.

36 MATERIALS SCIENCE↗
DOE OSTI2015

The effect of postprocessing on tensile property and microstructure evolution of friction stir welding aluminum alloy joint

Friction stir welding is an efficient manufacturing method for joining aluminum alloy and can dramatically reduce grain size conferring excellent plastic deformation properties. Consequently, friction stir welding is used to manufacture tailor welded blanks to optimize weight or performance in the final component. In the study, the microstructural evolution and mechanical properties of friction stir welding joint during plastic forming and subsequent heat treatment were investigated. The microstructural characteristics of the friction stir welding joints were studied by Electron Backscattered Diffraction and Transmission Electron Microscopy. The mechanical properties were evaluated by tensile and microhardness tests. It is found that the tensile and yield strengths of friction stir welding joints are significantly improved after severe plastic deformation due to the grain refinement. Following heat treatment, the strength of the friction stir welding joints significantly decrease due to the obvious abnormal grain growth. Careful attention must be given to the processing route of any friction stir welding joint intended for plastic forming, especially the annealing between forming passes. Severe plastic deforming of the friction stir welding joint leads to a high level of stored energy/dislocation density, which causes the abnormal grain growth during subsequent heat treatment, and consequently reduce the mechanical properties of the friction stir welding joint. - Highlights: • Great changes are observed in the microstructure of FSW joint after postprocessing. • Postprocessing shows great effect on the microstructure stability of FSW joint. • The weld shows more significant decrease in strength than the BM due to the AGG. • Attention must be given to the processing route of FSW joint for plastic forming.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Microstructure evolution and mechanical behavior of a high strength dual-phase steel under monotonic loading

Transmission electron microscopy (TEM) microstructures of a high-strength dual-phase steel DP800 have been examined after moderate plastic deformations in simple shear and uniaxial tension. Special attention has been paid to the effect of the intergranular hard phase (martensite) on the microstructure evolution in the near-grain boundary regions. Quantitative parameters of dislocation patterning have been determined and compared with the similar characteristics of previously examined single-phase steels. The dislocation patterning in the interiors of the ferrite grains in DP800 steel is found to be similar to that already observed in the single-phase IF (Interstitial Free) steel whereas the martensite-affected zones present a delay in patterning and display very high gradients of continuous (gradual) disorientations associated with local internal stresses. The above stresses are shown to control the work-hardening of dual-phase materials at moderate strains for monotonic loading and are assumed to influence their microstructure evolution and mechanical behavior under strain-path changes. - Highlights: • The microstructure evolution has been studied by TEM in a DP800 steel. • It is influenced by both martensite and dislocations in the initial state. • The DP800 steel presents a high work-hardening rate due to internal stresses.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Thermal Microstructural Stability of AZ31 Magnesium after Severe Plastic Deformation

Both equal channel angular pressing and friction stir processing have the ability to refine the grain size of twin roll cast AZ31 magnesium and potentially improve its superplastic properties. This work used isochronal and isothermal heat treatments to investigate the microstructural stability of twin roll cast, equal channel angular pressed and friction stir processed AZ31 magnesium. For both heat treatment conditions, it was found that the twin roll casted and equal channel angular pressed materials were more stable than the friction stir processed material. Calculations of the grain growth kinetics showed that severe plastic deformation processing decreased the activation energy for grain boundary motion with the equal channel angular pressed material having the greatest Q value of the severely plastically deformed materials and that increasing the tool travel speed of the friction stir processed material improved microstructural stability. The Hollomon-Jaffe parameter was found to be an accurate means of identifying the annealing conditions that will result in substantial grain growth and loss of potential superplastic properties in the severely plastically deformed materials. In addition, Humphreys’s model of cellular microstructural stability accurately predicted the relative microstructural stability of the severely plastically deformed materials and with some modification, closely predicted the maximum grain size ratio achieved by the severely plastically deformed materials.

FSW↗
DOE OSTI2015

Microstructure, texture evolution and magnetic properties of strip-casting non-oriented 6.5 wt.% Si electrical steel doped with cerium

A 0.3 mm thick non-oriented 6.5 wt.% Si electrical steel sheet doped with cerium is produced by twin-roll strip casting, hot rolling, warm rolling and annealing. A detailed study of the cerium precipitates in the as-cast strip, microstructure and texture evolution at different processing stages is carried out by electron probe micro-analysis, optical microscopy, X-ray diffraction and electron backscattered diffraction analysis. Grain interior distributing precipitates identified as Ce-oxides, Ce-oxysulfides and Ce-phosphides, and boundary distributing Ce-oxides and Ce-phosphides are observed in the as-cast strip. The initial as-cast strip is characterized by a much finer solidification microstructure and dominated by obvious < 001 >//ND texture through the strip thickness. After hot and warm rolling, inhomogeneous microstructure containing large amounts of in-grain shear bands is characterized by mixed < 110 >//RD and < 111 >//ND textures. The texture of the annealed sheet with a relatively large average grain size is far more optimized by the domination of the beneficial cube, rotated cube, (001)< 120 > to (001)< 130 > and Goss texture components, and the elimination of the detrimental γ-fiber texture, leading to a superior magnetic induction and improved iron loss. - Highlights: • An Fe–6.5 wt.% Si as-cast strip doped with cerium was produced. • A thin warm rolled sheet with limited edge cracks was obtained. • Microstructure and texture evolution at each stage were investigated. • Strong λ-fiber and Goss recrystallization textures were formed. • The magnetic properties of the annealed sheet were significantly improved.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Microstructures and microhardness at fusion boundary of 316 stainless steel/Inconel 182 dissimilar welding

Microstructures and microhardness at fusion boundary of a weld joint were investigated in a 316 stainless steel/Inconel 182 dissimilar weldment. The results showed that there were two alternately distributed typical fusion boundaries, a narrow random boundary (possessed 15% in length) with a clear sharp interface and an epitaxial fusion one with (100){sub BM}//(100){sub WM} at the joint interface. The composition transition, microstructure and hardness across the fusion boundary strongly depended on the type of the fusion boundary. For the random boundary, there was a clear sharp interface and the composition transition with a width of 100 μm took place symmetrically across the grain boundary. For the epitaxial fusion one, however, there were Type-I and Type-II grain boundaries perpendicular and parallel to the epitaxial fusion boundary, respectively. The composition transition took place in the Inconel 182 weld side. Σ3 boundaries in the HAZ of 316SS side and Σ5 grain boundaries in weld metal were usually observed, despite the type of fusion boundary, however the former was much more in epitaxial fusion boundary. Microhardness was continuously decreased across the random fusion boundary from the side of Inconel 182 to 316SS, but a hardening phenomenon appeared in the epitaxial fusion boundary zone because of its fine cellular microstructure. - Highlights: • Two typical fusion boundaries alternately distributed in the fusion interface • The microstructure, composition and hardness across fusion boundary depended on its type. • Different regions in welded joint have different special CSL value boundaries. • Hardening phenomenon only appeared in the epitaxial fusion boundary.

36 MATERIALS SCIENCE↗
DOE OSTI2015

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of the material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructure and mechanical behavior of direct metal laser sintered Inconel alloy 718

In this paper, we investigate microstructure and quasi-static mechanical behavior of the direct metal laser sintered Inconel 718 superalloy as a function of build direction (BD). The printed material was further processed by annealing and double-aging, hot isostatic pressing (HIP), and machining. We characterize porosity fraction and distribution using micro X-ray computed tomography (μXCT), grain structure and crystallographic texture using electron backscattered diffraction (EBSD), and mechanical response in quasi-static tension and compression using standard mechanical testing at room temperature. Analysis of the μXCT imaging shows that majority of porosity develops in the outer layer of the printed material. However, porosity inside the material is also present. The EBSD measurements reveal formation of columnar grains, which favor < 001 > fiber texture components along the BD. These measurements also show evidence of coarse-grained microstructure present in the samples treated by HIP. Finally, analysis of grain boundaries reveal that HIP results in a large number of annealing twins compared to that in samples that underwent annealing and double-aging. The yield strength varies with the testing direction by approximately 7%, which is governed by a combination of grain morphology and crystallographic texture. In particular, we determine tension–compression asymmetry in the yield stress as well as anisotropy of the material flow during compression. We find that HIP lowers yield stress but improves ductility relative to the annealed and aged material. These results are discussed and critically compared with the data reported for wrought material in the same condition. - Highlights: • Microstructure and mechanical properties of DMLS Inconel 718 are studied in function of build direction. • Inhomogeneity of microstructure in the material in several conditions is quantified by μXCT and EBSD. • Anisotropy and asymmetry in the mechanical response are determined by tension and compression testing.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructural evolution and mechanical properties on an ARB processed IF steel studied by X-ray diffraction and EBSD

Accumulative Roll Bonding (ARB) is one of the so-called severe plastic deformation (SPD) processes, allowing the production of metals and alloys with ultrafine (micro-nano) structures. Materials with ultrafine grains present attractive properties like the simultaneous increase in strength and ductility. Our interest in these materials is focused on their microstructural evolution during ARB processing, eventually responsible for the enhancement of those mechanical properties. In the current work we follow the evolution of the microstructure in an interstitial-free (IF) steel deformed by ARB after consecutive processing cycles, by means of Electron BackScatter Diffraction (EBSD) and X-ray diffraction (XRD). Particularly, we present results related to texture, grain (GS) and domain sizes, grain boundary character, density of Geometrically Necessary Dislocations (GND), Grain Orientation Spread (GOS), lattice parameters, microstrain, dislocation density and their spatial arrangement. After 5 ARB cycles the system shows a microstructure constituted mainly by submicrometric grains with high angle boundaries and low presence of dislocations inside the grains. - Highlights: •The evolution of microstructure is followed simultaneously by using GAM, GOS and GND (EBSD) and XRD. •LAGBs and subgrains disappear after few cycles SSDs and HAGBs persist at the end. •Dynamic recrystallization counterbalances dislocation arrays and diminishes hardening rate. •Grain size stabilization is revealed as a mechanism for increasing ductility after few ARB cycles.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructure, texture, and mechanical properties of friction stir welded commercial brass alloy

Microstructural evolution during friction stir welding of single-phase brass and corresponding mechanical properties were investigated. For this purpose, 2 mm thick brass plate was friction stir welded at a rotational speed of 450 rpm and traverse speed of 100 mm/min. The microstructure of the joint was studied using optical microscopy, scanning electron microscopy equipped with electron back scattered diffraction system, and scanning transmission electron microscopy. The mechanical properties were measured using hardness and tensile tests. The formation of subgrains and their transformation into new grains in conjunction with existence of A{sub 1}{sup ⁎}, A{sub 2}{sup ⁎} and C texture components revealed that the continuous dynamic recrystallization plays a dominant role in the microstructural evolution. However, grain boundary bulging, along with the formation of twin boundaries, and presence of the G texture component showed that the discontinues dynamic recrystallization may participate in the new grain formation. Furthermore, the different strengthening mechanisms, which caused the higher strength of the joint, were discussed. - Highlights: •Microstructural evolution during FSW of a single phase brass was investigated. •CDRX and DDRX were the main mechanisms of the grain structure formation during FSW. •GDRX and SRX were not contributed in grain structure formation. •The lamellas TBs were formed in the SZ of the joints. •Grain boundary, dislocation, and texture effects resulted in higher strength.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructure evolution and mechanical performance of copper processed by equal channel angular rolling

Highlights: • Copper was processed by equal channel angular rolling (ECAR) up to 33 passes. • A very fine grained microstructure with high dislocation density was developed. • A decrease of dislocation density was observed for high numbers of passes. • The proof stress saturated at a value of about 400 MPa. • ECAR is a possible way of commercialization of ultrafine-grained materials. - Abstract: Ultrafine-grained (UFG) oxygen free high conductivity (OFHC) Cu samples were processed by severe plastic deformation (SPD) using the method of equal channel angular rolling (ECAR) up to 33 passes at room temperature. It was found that the grain size gradually decreased from ~ 40 μm to ~ 250 nm with increasing the number of passes. A maximum dislocation density of ~ 21 × 10{sup 14} m{sup − 2} was achieved after 13 passes of ECAR. For large numbers of passes (between 23 and 33), the dislocation density decreased to ~ 14 × 10{sup 14} m{sup − 2}. The proof stress was saturated at the value of about 400 MPa. The stored energy was measured by calorimetry and compared with the values calculated from the parameters of the microstructure. The reduction of the released heat after 13 and 33 passes suggested structural relaxation of the UFG microstructure. For these numbers of passes, the reduction of area in tensile testing was improved without decreasing the proof stress. The correlation between the microstructure and the mechanical behavior was discussed in detail. It was found that ECAR is capable for the mass-production of UFG metallic materials with high strength, therefore this method is a possible way of commercialization of SPD-processed materials.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Ultrafine gradient microstructure induced by severe plastic deformation under sliding contact conditions in copper

Highlights: • Sliding contact produces a gradient microstructure by severe plastic deformation. • Nanohardness is increased strongly by grain size and dislocation hardening. • The texture components in the deformed layer correspond to pure shear. • Grain size distribution, boundary misorientation and KAM were analysed. • Strain induced effects compete with crystallisation to determine the microstructure. - Abstract: Sliding contact induces severe plastic deformation (SPD) at the surface of ductile materials and induces a microstructural gradient associated to a significant increase of hardness toward the surface. This gradient allows observing all stages of grain refinement in SPD, as illustrated here by the analysis of polycrystalline electrolytic copper tested in a coaxial tribometer. Materials tested in the cold-rolled state and after annealing were characterised by high-resolution electron backscattering diffraction and nano-indentation. The incremental plastic strain produces an ultrafine microstructure in the top layers, which gradually changes to the original size in unaffected material. In cold-rolled material, an intermediate recrystallised layer is observed. The separation of the Misorientation Angle Distribution (MAD) in a low-angle portion and a high angle portion allows characterising the accumulation of strain induced misorientation, while the Kernel Average Misorientation (KAM) provides information on the evolution of substructure at the finest levels. The results point toward a process where strain-induced effects compete continuously with recrystallisation, except for the surface layer in the cold-rolled material, where dynamic recrystallisation is dominant. Combining the information from KAM and subgrain size distribution, the measured hardness can be explained as a combination of grain size and dislocation hardening.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural characterization of SiO2/Ni nanocomposites electrodeposited from a sulphate bath modified by PEI

Highlights: • SiO{sub 2}/Ni + PEI nanocomposites are deposited from the sulphate bath containing PEI. • PEI allows incorporation of higher SiO{sub 2} vol% in SiO{sub 2}/Ni + PEI nanocomposites. • PEI in the form of a thin layer surrounds spherical Ni nanograins and SiO{sub 2} clusters. • PEI action ensures high hardness, tribological properties and corrosion resistance. - Abstract: SiO{sub 2}/Ni nanocomposite coatings containing well-dispersed SiO{sub 2} nanoparticles were electrodeposited from a sulphate bath with and without the addition of polyethylenimine (PEI) as a cationic surfactant. The surface morphology and microstructure in the cross-sections of the deposited nanocomposites were examined by scanning electron microscopy. More detailed microstructure characterization was performed using transmission, scanning-transmission and high resolution transmission electron microscopy. It was determined that the addition of 0.05 g/L and 0.1 g/L of PEI allows the incorporation of SiO{sub 2} nanoparticles in the nickel matrix to be increased in comparison with the nanocomposite deposited without a surfactant. Based on high spatial resolution microanalysis, performed using high count rate energy dispersive spectroscopy of characteristic X-rays in the scanning-transmission mode, the distribution of SiO{sub 2} nanoparticles in the nanocomposite was visualized on elemental maps. Image analysis of the electron microscopy images enabled the mean equivalent circle diameters of grains in the nickel matrix to be determined, together with the volume fraction of SiO{sub 2} nanoparticles in the nanocomposites. The volume fraction of SiO{sub 2} clusters in the SiO{sub 2}/Ni + PEI nanocomposites with the addition of 0.05 g/L and 0.1 g/L of PEI is equal to 18.4% and 13.3%, respectively. Furthermore, the PEI addition allows the nickel grain size in the matrix to be reduced. The combination of different imaging techniques confirmed that PEI is not only present as a surfactant in the electrolytic bath, but also incorporates into the microstructure of the nanocomposite. Nanocomposites electrodeposited in the presence of 0.05 g/L of PEI exhibit higher hardness, good tribological properties and improved corrosion resistance. Although increasing the PEI concentration in the bath up to 0.1 g/L strongly promotes grain size reduction and increase of the SiO{sub 2} volume fraction, it also causes an increase in the PEI fraction embedded in the microstructure, which results in deterioration of the properties of the SiO{sub 2}/Ni + PEI nanocomposites.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Densification, microstructure and properties of TiB2 ceramics fabricated by spark plasma sintering

Highlights: • Nearly full densification of in-house processed TiB{sub 2} ceramic powders at 1500 °C. • Microstructures revealing the size and shape of TiB{sub 2} grains after SPS. • The effect of sub-micron particles on the densification during SPS. • The effect of sintering pressure on the microstructure. • Microhardness and nano-indentation measurements along with oxidation studies. - Abstract: This study reports the fabrication of high-density TiB{sub 2} ceramics at reduced temperatures (1500 °C) by using field assisted sintering technology/spark plasma sintering (FAST/SPS) technique. In-house processed TiB{sub 2} powders with high purity were employed as starting materials. The effects of SPS conditions on the sintering behavior and microstructure of TiB{sub 2} were investigated. Sub-micron character of TiB{sub 2} particles has a strong influence on the densification during SPS. Microstructural analyses revealed that the high pressure affected both the grain size and the shape of TiB{sub 2} crystallites. Elongated grains with average size of 6 μm were perceived in TiB{sub 2} sample fabricated by SPS at 1500 °C under 60 MPa pressure with a relative density of 96.7%. The microhardness and elastic modulus were measured as 27.4 GPa and 685.2 GPa, respectively. This sample revealed an improved oxidation resistance due to the formation of a thin oxidation layer on the surface when heated up to 1200 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Data clustering for the high-resolution alignment of microstructure and strain fields

The emergence of small-scale deformation mapping by a combination of scanning electron microscopy and digital image correlation (SEM-DIC) has enabled full-field investigations into the complex roles of microstructure on microscale deformation mechanisms. However, these investigations are hindered by errors in alignment between the microstructure data, generally acquired by electron backscatter diffraction (EBSD), and the microscale strain data obtained by SEM-DIC. Distortions, stitching artifacts, and spatial resolution differences between microstructure and strain fields can lead to misalignments on the order of μms. This alignment uncertainty introduces error into microstructure-strain localization analyses and precludes the examination of deformation mechanisms near grain boundaries. To improve alignment between EBSD-obtained grain boundaries and SEM-DIC strain data, an approach was created wherein a mantle was first established around the EBSD-acquired grain boundaries. Strain data was then clustered within this mantle using a k-means algorithm to identify grain boundary strain localization, and these boundary points were fit to obtain a continuous curve for each individual boundary. Clustered point outliers, such as those due to grain boundary-local dislocation slip, were statistically identified by using an absolute error threshold and removed from the grain boundary fit. The ending identification of grain boundaries in the microscale strain data is significantly improved from EBSD-identified boundaries.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Strain rate sensitivity, microstructure variations, and stress-assisted β → α" phase transformation investigation on the mechanical behavior of dual-phase titanium alloys

In this study, the microstructures of three widely used dual-phase titanium alloys: Ti-6Al-4V, Ti-6Al-2Sn-4Zr-2Mo, and Ti-6Al-2Sn-4Zr-6Mo are characterized using backscatter electron imaging and the deformation behaviors in their individual α and β phases are investigated using in situ high-energy X-ray diffraction during uniaxial tension experiments. This is accompanied by calculation of the strain rate sensitivity (SRS) in these alloys, as a function of applied loading. The results of the calculated SRS and the mechanical response (in terms of lattice strains and hardening behaviors) are rationalized based on the local microstructure, composition, and texture of the alloy. A stress-induced β (BCC) to α" (orthorhombic) phase transformation is observed during the in-situ diffraction experiment, which permitted analysis of the lattice strain evolution during the phase transformation. Results from this study provide insights into the relationship between microstructure, composition, applied loading, and the deformation behavior, including effects on loading with time holds. Specifically, the results show that the microstructure, and not necessarily the chemical composition (Mo content), along with the applied loading have a dominant role in the observed SRS variation in titanium alloys. Further, the evolution of the α" (orthorhombic) phase is observed for the first time during deformation of an industrially relevant titanium alloy, Ti-6246.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Microstructural stability of irradiated yttrium hydride under thermal cycles

Hydrides that retain their hydrogen in service are critical for advanced microreactor and space nuclear systems. Hydrogen retention is affected by evolving microstructure under temperature and irradiation extremes. This study investigated microstructural features in neutron-irradiated yttrium hydride and the stability of these features under thermal cycles. Differential scanning calorimetry was used to determine hydrogen desorption and temperatures at which significant phase changes are occurring, and transmission electron microscopy was used for microstructural analysis after each thermal cycle. Cyclic heating led to crystallization and epitaxial growth of surface oxidation and dehydriding of the matrix. Other features such as the bulk matrix crystal structure, irradiation-induced cavities, and matrix precipitation remained constant after thermal cycling. Results allow us to design better hydride alloys through microstructure tailoring and potential irradiation conditioning treatments.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Three-dimensional interconnected nickel phosphide networks with hollow microstructures and desulfurization performance

Graphical abstract: Three-dimensional interconnected nickel phosphide networks with hollow microstructures and desulfurization performance. - Highlights: • Three-dimensional Ni{sub 2}P has been prepared using foam nickel as a template. • The microstructures interconnected and formed sponge-like porous networks. • Three-dimensional Ni{sub 2}P shows superior hydrodesulfurization activity. - Abstract: Three-dimensional microstructured nickel phosphide (Ni{sub 2}P) was fabricated by the reaction between foam nickel (Ni) and phosphorus red. The as-prepared Ni{sub 2}P samples, as interconnected networks, maintained the original mesh structure of foamed nickel. The crystal structure and morphology of the as-synthesized Ni{sub 2}P were characterized by X-ray diffraction, scanning electron microscopy, automatic mercury porosimetry and X-ray photoelectron spectroscopy. The SEM study showed adjacent hollow branches were mutually interconnected to form sponge-like networks. The investigation on pore structure provided detailed information for the hollow microstructures. The growth mechanism for the three-dimensionally structured Ni{sub 2}P was postulated and discussed in detail. To investigate its catalytic properties, SiO{sub 2} supported three-dimensional Ni{sub 2}P was prepared successfully and evaluated for the hydrodesulfurization (HDS) of dibenzothiophene (DBT). DBT molecules were mostly hydrogenated and then desulfurized by Ni{sub 2}P/SiO{sub 2}.

36 MATERIALS SCIENCE↗