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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 1,711 records · Page 95
All sourcesNASA NTRSDOE OSTI
DOE OSTI2012

High-throughput and in situ EDXRD investigation on the formation of two new metal aminoethylphosphonates - Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) and Ca(OH)(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3}){center_dot}2H{sub 2}O

The system Ca{sup 2+}/2-aminoethylphosphonic acid/H{sub 2}O/NaOH was systematically investigated using high-throughput methods. The experiments led to one new compound Ca(O{sub 3}PC{sub 2} H{sub 4}NH{sub 2}) (1) and the crystal structure was determined using in house X-ray powder diffraction data (monoclinic, P2{sub 1}/c, a=9.7753(3), b=6.4931(2), c=8.4473(2) A, {beta}=106.46(2) Degree-Sign , V=514.20(2) A{sup 3}, Z=4). The formation of 1 was investigated by in situ energy dispersive X-ray diffraction measurements (EDXRD) at beamline F3 at HASYLAB (light source DORIS III), DESY, Hamburg. An intermediate, Ca(OH)(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3}){center_dot}2H{sub 2}O (2), was observed and could be isolated from the reaction mixture at ambient temperatures by quenching the reaction. The crystal structure of 2 was determined from XRPD data using synchrotron radiation (monoclinic, P2{sub 1}/m, a=11.2193(7), b=7.1488(3), c=5.0635(2) A, {beta}=100.13(4) Degree-Sign , V=399.78(3) A{sup 3}, Z=2). - Graphical abstarct: The detailed in situ energy dispersive X-ray diffraction (EDXRD) investigation on the formation of the new inorganic-organic hybrid compound Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) leads to the discovery of a new crystalline intermediate phase. Both crystal structures were elucidated using X-ray powder diffraction data. Highlights: Black-Right-Pointing-Pointer High-throughput investigation led to new metal aminoethylphosphonate Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}). Black-Right-Pointing-Pointer The formation of Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) was followed by in situ EDXRD measurements. Black-Right-Pointing-Pointer The crystalline intermediate Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3})(OH){center_dot}2H{sub 2}O was discovered. Black-Right-Pointing-Pointer Isolation of Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3})(OH){center_dot}2H{sub 2}O was accomplished by quenching experiments. Black-Right-Pointing-Pointer The structures were determined using X-ray powder diffraction data.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Formation of Mg{sub 2}Ni with enhanced kinetics: Using MgH{sub 2} instead of Mg as a starting material

At a temperature over the decomposition point (375 Degree-Sign C) of MgH{sub 2}, the formation of Mg{sub 2}Ni is greatly enhanced from the 2MgH{sub 2}+Ni system, as compared to the 2Mg+Ni system. In support of this finding, in-situ observation of X-ray absorption fine structure of the two systems indicates that Mg---Ni bonds form faster in the 2MgH{sub 2}+Ni system than in the 2Mg+Ni system. Furthermore, theoretical modeling also shows that Mg atoms are readily released from MgH{sub 2} using much less energy and thus are more available to react with Ni once the dehydrogenation of MgH{sub 2} occurs, as compared to normal Mg. - Graphical Abstract: The formation of Mg{sub 2}Ni is greatly enhanced by using MgH{sub 2} instead of Mg at a temperature higher than the MgH{sub 2} decomposition point. Highlights: Black-Right-Pointing-Pointer A new and efficient synthesis of Mg-based compounds at a reduced temperature. Black-Right-Pointing-Pointer Mg{sub 2}Ni formation is enhanced by using MgH{sub 2} instead of Mg as a starting material. Black-Right-Pointing-Pointer XAFS results show that Mg---Ni bonds are formed faster in 4MgH{sub 2}+Ni than in 4Mg+Ni. Black-Right-Pointing-Pointer DFT calculations show that Mg atoms are released from MgH{sub 2} more readily than from Mg. Black-Right-Pointing-Pointer Mg formed by MgH{sub 2} dehydrogenation is more available to react with Ni than normal Mg.

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

Controlled synthesis and formation mechanism of monodispersive lanthanum vanadate nanowires with monoclinic structure

Monodisperse LaVO{sub 4} nanowires with relatively high aspect ratio larger than 50 have been prepared by a one-step solvothermal synthesis. This method provides a simple, inexpensive, controllable and reproducible process to produce LaVO{sub 4} nanowires with an average diameter of 15 nm and a high aspect ratio. The as-synthesized products have been characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and fast Fourier transform spectroscopy (FFT), indicative of a well-crystalline monoclinic structure and ascendant nanowire-morphology. The formation mechanism is suggested that oriented attachment plays a vital role in the growth of LaVO{sub 4} nanowires, which recommends a favorable route to fabricate similar morphological and structural nanometer materials. - Graphical abstract: The formation of LaVO{sub 4} nanowires is attributed to oriented attachment, a combination of nanocrystallites through their suitable surface planes, that is, with the same crystallographic orientations of [−120]. Highlights: ► Monodisperse LaVO{sub 4} nanowires with high aspect ratio have been prepared solvothermally without any templates. ► The morphology and structure of LaVO{sub 4} nanowires were characterized by XRD, SEM, TEM techniques. ► The formation mechanism of LaVO{sub 4} nanowires is suggested that oriented attachment plays a vital role.

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

Control of Y₂O₃ phase and its nanostructure formation through a very high energy mechanical milling

The formation behavior of Y₂O₃ ceramic particles was studied by employing a very high energy ball milling (milling energy: ~165 kJ/g·hit, milling speed: 1000 rpm). Both the XRD and HRTEM studies revealed that the high impact strain energy generated during the milling caused a drastic phase transition from the original C-type cubic (space group Ia3, a=10.58 Å) to the metastable B-type monoclinic (space group C2/m, a=13.89 Å), finally followed by a partial solid-state amorphization. The cubic phase was difficult to be reduced down to smaller than 10 nm, while the monoclinic phase was stabilized at sizes smaller than 10 nm with a mean crystallite size of 7.57 nm. Consequently, the existence of Y₂O₃ at a nanoscale smaller than 10 nm is possible by forming metastable monoclinic crystals, which are strain-induced. - Graphical abstract: The fig shows the solid-state phase formation of Y₂O₃ by very high energy input into the particles during milling: ordered body-centered cubic phase (space group Ia3, a=10.58 Å) nanocrystalline monoclinic phase (space group C2/m, a=13.89 Å) disordered monoclinic phase partial amorphous phase. The formation of Y₂O₃ smaller than 10 nm was strongly dependent on whether the phase transition from cubic to monoclinic occurred. Highlights: • This paper analyses very high energy milling behavior of coarse Y₂O₃ particles. • A drastic phase transition from cubic to monoclinic occurred with a partial amorphization. • An existence of Y₂O₃ smaller than 10 nm is possible by forming strain-induced monoclinic crystals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Conditions and mechanisms for the formation of nano-sized Delafossite (CuFeO{sub 2}) at temperatures ≤90 °C in aqueous solution

In this study, we present the mechanism of CuFeO{sub 2} formation in aqueous solution at low temperatures ≤90 °C, using sulfate salts as reactants. Furthermore, we demonstrate the influence of experimental conditions (alkalization, reaction and ageing temperature and time) on the synthesized nanoparticles. In all cases, GR–SO{sub 4}, a Fe(II–III) layered double hydroxysulphate (Fe{sup 2+}{sub 4}Fe{sup 3+}{sub 2}(OH){sub 12}·SO{sub 4}) and Cu{sub 2}O precipitate first. During further OH{sup −} supply GR–SO{sub 4} oxidizes and forms Fe{sub 10}O{sub 14}(OH){sub 2}, Cu{sub 2}O and CuFeO{sub 2} crystals. Due to the high pH further CuFeO{sub 2} crystals grow at the cost of the unstable intermediate products. The reaction rate increases with increasing ageing temperature, reaction pH and, in particular, NaOH concentrations in the solution. As a result, highly crystalline CuFeO{sub 2} (3R and 2H polytypes) nanoparticles showing hexagonal morphology can be synthesized at 70 °C within 10 h or at 50 °C within 1 week. The formation of 2H polytype is favored by additional OH{sup −} supply during the pH-stat time and rather low temperatures. - Highlights: • We solve the formation mechanism of pure CuFeO{sub 2} using sulfates as reactants. • CuFeO{sub 2} nanoparticles crystallize on cost of green rust, Fe{sub 10}O{sub 14}(OH){sub 2} and Cu{sub 2}O. • The reaction rate increases with increasing temperature and OH- concentration. • CuFeO{sub 2} nanoparticles form at 50 °C within one week and at 70 °C within 10 h. • 2H-polytype of CuFeO{sub 2} is favored by additional NaOH supply during pH-stat-time.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Understanding the formation and growth of Ag nanoparticles on silver chromate induced by electron irradiation in electron microscope: A combined experimental and theoretical study

Ag{sub 2}CrO{sub 4} microcrystals were synthesized using the co-precipitation method. These microcrystals were characterized through X-ray diffraction (XRD) with Rietveld analysis, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) with energy-dispersive spectroscopy (EDS), micro-Raman (MR). XRD patterns and Rietveld refinement data showed that the material exhibits an orthorhombic structure without any deleterious phases. FE-SEM and TEM micrographs revealed the morphology and the growth of Ag nanoparticles on Ag{sub 2}CrO{sub 4} microcrystals during electron beam irradiation. These events were directly monitored in real-time. Their optical properties were investigated using ultraviolet-visible (UV–vis) diffuse reflectance spectroscopy that allowed the calculation of the optical band gap energy. Theoretical analyses based on the density functional theory level indicate that the incorporation of electrons is responsible for structural modifications and formation of defects on the [AgO{sub 6}] and [AgO{sub 4}] clusters, generating ideal conditions for the growth of Ag nanoparticles. - Graphical abstract: Theoretical representation of the Ag{sub 2}CrO{sub 4} orthorhombic structure. Display Omitted - Highlights: • The Ag{sub 2}CrO{sub 4} microcrystals indicate an orthorhombic structure. • The formation of Ag{sup 0} promotes Ag-nanoparticle growth on the surface of the Ag{sub 2}CrO{sub 4}. • Electron irradiation of the material induces the formation of Ag vacancies.

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

Gold nano-particle formation from crystalline AuCN: Comparison of thermal, plasma- and ion-beam activated decomposition

In this work, in addition to the conventional thermal process, two non-conventional ways, the plasma and ion beam activations are described for preparing gold nanoparticles from microcrystalline AuCN precursor. The phase formation at plasma and ion beam treatments was compared with that at thermal treatments and the products and transformations were characterized by thermogravimetry-mass-spectrometry (TG-MS), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). TG-MS measurements in Ar atmosphere revealed that AuCN decomposition starts at 400 °C and completes at ≈700 °C with evolution of gaseous (CN){sub 2}. XPS and TEM show that in heat treatment at 450 °C for 1 h in Ar, loss of nitrogen and carbon occurs and small, 5–30 nm gold particles forms. Heating at 450 °C for 10 h in sealed ampoule, much larger, 60–200 nm size and well faceted Au particles develop together with a fibrous (CN){sub n} polymer phase, and the Au crystallites are covered by a 3–5 nm thick polymer shell. Low pressure Ar plasma treatment at 300 eV energy results in 4–20 nm size Au particles and removes most of the nitrogen and part of carbon. During Ar{sup +} ion bombardment with 2500 eV energy, 5–30 nm size Au crystallites form already in 10 min, with preferential loss of nitrogen and with increased amount of carbon residue. The results suggest that plasma and ion beam activation, acting similarly to thermal treatment, may be used to prepare Au nanoparticles from AuCN on selected surface areas either by depositing AuCN precursors on selected regions or by focusing the applied ionized radiation. Thus they may offer alternative ways for preparing tailor-made catalysts, electronic devices and sensors for different applications. - Graphical abstract: Proposed scheme of the decomposition mechanism of AuCN samples: heat treatment in Ar flow (a) and in sealed ampoule (b); Ar{sup +} ion treatment at 300 eV (c) and at 2500 eV (d). Cross section sketches illustrate the Au phase formation and the corresponding TEM micrographs are shown as top views. The dotted lines represent the original boundaries of the AuCN crystals. - Highlights: • AuCN decomposes between 400 and 700 °C with evolution of gaseous (CN){sub 2}. • Epitaxial relationship is established between Au and parent AuCN crystals. • Ar plasma treatment results in similar phase transition than the thermal treatment. • Plasma and ion-beam activation offer alternative way for preparing Au nanocrystals. • Reaction mechanisms of Au particle formation at the three treatments are proposed.

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

Phase formation in the (1-y)BiFeO{sub 3}-yBiScO{sub 3} system under ambient and high pressure

Formation and thermal stability of perovskite phases in the BiFe{sub 1-y}Sc{sub y}O{sub 3} system (0≤y≤0.70) were studied. When the iron-to-scandium substitution rate does not exceed about 15 at%, the single-phase perovskite ceramics with the rhombohedral R3c symmetry (as that of the parent compound, BiFeO{sub 3}) can be prepared from the stoichiometric mixture of the respective oxides at ambient pressure. Thermal treatment of the oxide mixtures with a higher content of scandium results in formation of two main phases, namely a BiFeO{sub 3}-like R3c phase and a cubic (I23) sillenite-type phase based on γ-Bi{sub 2}O{sub 3}. Single-phase perovskite ceramics of the BiFe{sub 1-y}Sc{sub y}O{sub 3} composition were synthesized under high pressure from the thermally treated oxide mixtures. When y is between 0 and 0.25 the high-pressure prepared phase is the rhombohedral R3c with the √2a{sub p}×√2a{sub p}×2√3a{sub p} superstructure (a{sub p} ~ 4 Å is the pseudocubic perovskite unit-cell parameter). The orthorhombic Pnma phase (√2a{sub p}×4a{sub p}×2√2a{sub p}) was obtained in the range of 0.30≤y≤0.60, while the monoclinic C2/c phase (√6a{sub p}×√2a{sub p}×√6a{sub p}) is formed when y=0.70. The normalized unit-cell volume drops at the crossover from the rhombohedral to the orthorhombic composition range. The perovskite BiFe{sub 1-y}Sc{sub y}O{sub 3} phases prepared under high pressure are metastable regardless of their symmetry. At ambient pressure, the phases with the compositions in the ranges of 0.20≤y≤0.25, 0.30≤y<0.50 and 0.50≤y≤0.70 start to decompose above 970, 920 and 870 K, respectively. - Graphical abstract: Formation of perovskite phases in the BiFe{sub 1-y}Sc{sub y}O{sub 3} system when y≥0.15 requires application of pressure of several GPa. The phases formed under high pressure: R3c (0.20≤y≤0.25), Pnma (0.30≤y≤0.60) and C2/c (y≥0.70) are metastable. - Highlights: • Maximal Fe-to-Sc substitution rate in BiFeO{sub 3} at ambient pressure is about 15 at%. • R3c → Pnma → C2/c phase sequence in high-pressure prepared BiFe{sub 1-y}Sc{sub y}O{sub 3} ceramics. • The perovskite BiFe{sub 1-y}Sc{sub y}O{sub 3} phases formed under high pressure are metastable.

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

Conditions for the formation of pure birnessite during the oxidation of Mn(II) cations in aqueous alkaline medium

Birnessite was synthetized through redox reaction by mixing MnO{sub 4}{sup -}, Mn{sup 2+} and OH{sup -} solutions. The Mn(VII): Mn(II) ratio of 0.33 was chosen and three methods were used consisting in a quick mixing under vigorous stirring of two of the three reagents and then on the dropwise addition of the third one. The obtained solids were characterized by XRD, FTIR and XPS spectroscopies. Their average oxidation states were determined from ICP and CEC measurements while their surface properties were investigated by XPS. This study provides an increased understanding of the importance of dissolved oxygen in the formation of birnessite and hausmannite and shows the ways to obtain pure birnessite. The role of counter-ion ie. Na{sup +} or K{sup +} was also examined. - Graphical abstract: Pathways of birnessite formation. - Highlights: • Pure birnessite is prepared through a redox reaction. • Hausmannite formation is prevented by controlling dissolved O2. • The employed counterion influences the purity of birnessite. • Initial Mn(OH){sub 2} is oxidized by both MnO{sub 4}{sup -} and dissolved O{sub 2}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Understanding the formation of nanocomposites consisting of silver sulfide and platinum hollow nanostructures

Highlights: • Reacting core-shell [email protected] particles with Na{sub 2}S leads to hollow Pt nanostructures. • Reacting core-shell [email protected] particles with sulfur leads to Ag{sub 2}S-hPt nanocomposites. • The mechanism determining the formation of Ag{sub 2}S-hPt nanocomposites was elucidated. • Additional experiments were designed to rationalize the formation mechanism. - Abstract: Structural conversion using core-shell silver (Ag)-platinum (Pt) nanoparticles as starting materials is a promising way to produce nanocomposites consisting of silver sulfide (Ag{sub 2}S) and hollow Pt nanostructures (Ag{sub 2}S-hPtNCs). However, the mechanism behind the structural conversion process is yet to be understood. In this study, we use transmission electron microscope (TEM) as a typical tool to characterize the products formed in different structural conversion processes, and interpret the experimental observations by proposing mechanisms behind the reactions between core-shell Ag-Pt nanoparticles and sulfur precursors from different sources. We then design additional experiments to rationalize the formation mechanism we proposed. The mechanistic understanding of the structural conversion from bimetallic core-shell nanostructures to heterogeneous nanocomposites may extend the fabrication of heterogeneous nanocomposites for a given technological application.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

The sequence of intermetallic formation and solidification pathway of an Al–13Mg–7Si–2Cu in-situ composite

The phase transformation sequence and solidification behaviour of an Al–13Mg–7Si–2Cu in-situ composite was examined using a combination of computer-aided cooling curve thermal analysis and interrupted quenching techniques. Five different phases were identified by analysing the derivative cooling curves, the X-ray diffraction profile, optical and scanning electron microscopy images and the corresponding energy dispersive spectroscopy. It has been found that the solidification of this alloy begins with primary Mg{sub 2}Si precipitation and continues with the formation of eutectic Al–Mg{sub 2}Si, followed by Al{sub 5}FeSi and simultaneous precipitation of Al{sub 5}Cu{sub 2}Mg{sub 8}Si{sub 6} and Al{sub 2}Cu complex intermetallic phases. The formation of the last three intermetallic compounds changes the solidification behaviour of these composites remarkably due to their complex eutectic formation reactions. The solidification of the alloy, calculated using the Factsage thermochemical analysis software, has demonstrated a good agreement with the experiments in terms of compound prediction, their weight fractions and reaction temperatures. - Highlights: • Solidification path of a commercial Al-13Mg-7Si-2Cu composite was characterized. • Five different phases were identified and then confirmed with EDS and XRD results. • Mg{sub 2}Si, Al-Mg{sub 2}Si,Al{sub 5}FeSi (β),Al{sub 5}Cu{sub 2}Mg{sub 8}Si{sub 6} (Q) and Al{sub 2}Cu(θ) precipitated respectively. • Solidification was predicted using the Factsage thermochemical analysis software.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Oxidation and alpha-case formation in Ti–6Al–2Sn–4Zr–2Mo alloy

Isothermal heat treatments in ambient air were performed on wrought Ti–6Al–2Sn–4Zr–2Mo (Ti-6242) material at 500, 593 and 700°C for times up to 500 h. In the presence of oxygen at elevated temperatures simultaneous reactions occurred in Ti-6242 alloy, which resulted in the formation of an oxide scale and a layer with higher oxygen concentration (termed as alpha-case). Total weight gain analysis showed that there was a transition in the oxidation kinetics. At 500°C, the oxidation kinetics obeyed a cubic relationship up to 200 h and thereafter changed to parabolic at prolonged exposure times. At 593°C, it followed a parabolic relationship. After heat treatment at 700°C, the oxidation obeyed a parabolic relationship up to 200 h and thereafter changed to linear at prolonged exposure times. The observed transition is believed to be due to the differences observed in the oxide scale. The activation energy for parabolic oxidation was estimated to be 157 kJ/mol. In addition, alpha-case layer was evaluated using optical microscope, electron probe micro-analyser and microhardness tester. The thickness of the alpha-case layer was found to be a function of temperature and time, increasing proportionally, and following a parabolic relationship. The activation energy for the formation of alpha-case layer was estimated to be 153 kJ/mol. - Highlights: • Transition in oxidation kinetics was observed in Ti–6Al–2Sn–4Zr–2Mo alloy in the temperature range 500–700°C. • The activation energy for parabolic oxidation and for alpha-case formation is about 157 kJ/mol and 153 kJ/mol. • Thickness of alpha-case layer estimated by optical microscopy and electron probe microanalysis is comparable.

36 MATERIALS SCIENCE↗
DOE OSTI2015

On the formation of Mo{sub 2}C nanocrystals by a novel system through microwave assisted combustion synthesis

This research is devoted to microwave assisted combustion synthesis of Mo{sub 2}C nanoparticles. The ternary system of MoO{sub 3}–Zn–C was used as a novel approach for the in-situ synthesis of Mo{sub 2}C in which the zincothermic reduction of MoO{sub 3} was responsible for the combustion to take place. Results showed that the formation of Mo{sub 2}C was assisted by the zincothermic reaction, although further microwave heating up to 6 min was necessary to complete the reaction. The effects of the microwave heating and mechanical activation on the reaction progress were investigated. X-ray powder diffraction was used to examine the synthesis progress. Final products (Mo{sub 2}C and ZnO) were successfully separated from each other and the synthesized carbide was characterized by transmission electron microscopy (TEM), showing the formation of Mo{sub 2}C hexagonal nanocrystals during combustion process. - Highlights: • Hexagonal β-Mo{sub 2}C nanocrystals were successfully synthesized. • MoO{sub 3}–Zn–C powder mixture was selected as the initial mixture for the in-situ synthesis of Mo{sub 2}C. • 30 min of mechanical activation was necessary for the carbide formation to be completed. • The zincothermic reduction of MoO{sub 3} by Zn was responsible for the combustion. • The final products included of Mo{sub 2}C and ZnO in which ZnO was removed by acid leaching.

36 MATERIALS SCIENCE↗
DOE OSTI2016

The distribution and mechanism of pore formation in copper foams fabricated by Lost Carbonate Sintering method

In this research, utilizing X-ray computed tomography (XCT), geometrical characterization, and pore formation mechanisms of highly porous copper foams manufactured by powder metallurgical (PM) process are investigated. Open-cell copper foams with porosity percentages of 60% and 80% and with a pore size within the range of 300–600 μm were manufactured by using potassium carbonate as a space holder agent via the Lost Carbonate Sintering (LCS) technique. XCT and SEM were also employed to investigate the three-dimensional structure of foams and to find the effect of the parameters of the space holders on the structural properties of copper foams. The result showed an excellent correlation between the structural properties of the foams including the size and shape of the pores, porosity percentage, volume percentage, particle size, and the shape of the sacrificial agent used. Also, the advanced image analysis of XCT images indicated fluctuations up to ± 10% in porosity distribution across different cross-sections of the foams. Simultaneous thermal analysis (STA: DTA–TG) was also used to study the thermal history of the powders used during the manufacturing process of the foams. The results indicated that the melting and thermal decomposition of the potassium carbonate occurred simultaneously at 920 °C and created the porous structure of the foams. By combining the STA result with the result of the tension analysis of cell walls, the mechanisms of open-pore formation were suggested. In fact, most open pores in the samples were formed due to the direct contact of potassium carbonate particles with each other in green compact. Also, it was found that the thermal decomposition of potassium carbonate particles into gaseous CO{sub 2} led to the production of gas pressure inside the closed pores, which eventually caused the creation of cracks on the cell walls and the opening of the pores in foam's structure. - Highlights: • Structural characterization of copper foam produced by LCS method is investigated by tomography images. • The ability of LCS technique to control structural features of produced foams was proved. • The mechanisms of open pores formation were presented.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Effect of Ag additions on the lengthening rate of Ω plates and formation of σ phase in Al-Cu-Mg alloys during thermal exposure

Effect of Ag additions on the mechanical properties and microstructures of the peak-aged Al-Cu-Mg alloys during prolonged thermal exposure at 150 °C, was investigated by tensile testing, conventional transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). The results showed that after exposure for 500 h, > 85% of the peak strength remained. Microstructure observations indicated that increasing the Ag content from 0.14 to 0.57% promoted the precipitation of a fine and uniform Ω phase and suppressed the formation of the θ′ phase, leading to a notable improvement of the strength properties and thermal stability of the studied alloys. Quantitative TEM analysis showed that the coarsening of Ω phase was predominated by plate lengthening rather than thickening, while its lengthening rate was independent of various Ag additions during exposure at 150 °C. In addition, an increase of Ag also facilitated the formation of a cubic σ phase, which was further supported by STEM results. - Highlights: •Increasing Ag improved strength properties and thermal stability of the alloys. •After exposure for 500 h, > 85% of the peak strength remained. •The lengthening rate of Ω plates remained constant as Ag increased at 150 °C. •Increasing Ag content facilitated the formation of σ phase.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influence of strain on the formation of cold-rolling and grain growth textures of an equiatomic HfZrTiTaNb refractory high entropy alloy

Highlights: • Effect of strain on Texture formation is reported in HfZrTiTaNb for the first time. • Cold-rolled microstructure shows high density of deformation heterogeneities. • Weak texture compared to other BCC phases in HEAs • Imposed strain does not affect texture significantly unlike other BCC materials. - Abstract: The effect of cold-rolling strain on the evolution of deformation and grain growth textures in an equiatomic HfZrTiTaNb refractory high entropy alloy (RHEA) was investigated. For this purpose, the development of microstructure and texture was compared in 50% and 90% cold-rolled materials. The development of deformation microstructure was accompanied by the formation of extensive deformation heterogeneities. The 90% cold-rolled material showed ultrafine lamellar regions as well as regions severely fragmented by the fine scale deformation heterogeneities. The 50% cold-rolled material showed dominant ND-fiber (ND//), while the 90% cold-rolled material showed presence of both RD (RD//) and ND-fiber components. Profuse deformation heterogeneities presumably weakened the deformation texture considerably. The annealing texture of the 50% and 90% cold-rolled material showed stronger {111} component. Comparison of the annealing texture of the 50% and 90% cold-rolled materials with other BCC HEA phases indicated much weaker texture. The annealing texture of the RHEA was not significantly strengthened by increasing cold-rolling strain, presumably due to the high density of deformation heterogeneities in the cold-rolled microstructure. Thus, deformation heterogeneities significantly influenced the formation of cold-rolling and annealing textures of the equiatomic HfZrTiTaNb RHEA.

36 MATERIALS SCIENCE↗
DOE OSTI2018

On the formation mechanism of solid-solution Cu-to-Cu joints in the Cu/Ni/Ga/Ni/Cu system

Highlights: • The mechanism of Cu/(Ni,Cu,Ga)/Cu solid-solution joint formation is elaborated. • Ga is the dominant diffusion species in the Cu/Ni/Ga/Ni/Cu bonding system. • Loose and columnar Ni{sub 3}Ga{sub 7} layer is formed by the (001)-textured Ni/Ga reactions. • Cu significantly accelerates the growth of Ni{sub 3}Ga{sub 7} layer by enhancing Ga diffusion. • Supersaturated Cu in Ni{sub 2}Ga{sub 3} phase promotes the formation of the final fcc phase. - Abstract: Copper (Cu)-to-Cu interconnection is crucial in electronic packaging for applications ranging from three-dimensional integrated circuits to die-attachment in wide band-gap devices. Solid-solution phases are innate with better ductility and electrical and thermal conductivity over intermetallic compounds, which are brittle, electrical resistant, and unstable; yet are commonly seen in electronic joints. The desired solid-solution Cu-to-Cu joints have recently been demonstrated using transient-liquid-phase bonding with gallium (Ga) as the filler material to bond Cu substrates with electroplated nickel (Ni) as under-bump-metallurgy. The Cu/Ni/Ga/Ni/Cu couples can fully transform into the Cu/face-centered cubic (fcc)-(Ni,Cu,Ga)/Cu solid-solution joints. However, why and how the solid-solution joints were formed remains unclear. Here we proposed the formation mechanism of the fcc-(Ni,Cu,Ga) solid-solution joints based on five sets of Cu-Ni-Ga couples, namely the Ni/Ga, Ni/Cu/Ga, Ni/Ni/Ga, (Cu,Ni)/Ga, and Cu/Ni/Ni{sub 3}Ga{sub 7}/Ni{sub 3}Ga{sub 7}/Ni/Cu reactions. The roles of each element in the Cu-Ga-Ni interactions as well as the reaction progressions are elaborated.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Formation of intermetallic structures at the interface of steel-to-aluminium explosive welds

Highlights: • The interface of Fe-Al explosive welds was characterised by SEM/EDS and EBSD. • The intermetallics formed at the weld interface are rich in Al (Fe{sub 4}Al{sub 13}, Fe{sub 2}Al{sub 5}). • The presence of intermetallic phases on the interface deeply affects the weldability. • Al-rich intermetallics increase the solidification time of the weld interface. - Abstract: The formation of intermetallic structures at the interface of carbon steel to 6082 aluminium alloy explosive welds and their influence on the weldability of these two materials were studied. The morphology, the microstructure, the chemical and phase compositions of the welds were characterised by several types of microscopy techniques. The interface characterisation proved that explosive mixtures with a lower detonation velocity were revealed as being more suitable for achieving consistent welds since jet entrapment was prevented and continuous molten layers were not formed at the weld interface. It was also found that the physical properties of the intermetallic phases generated at the weld interface have a strong influence on the weldability of steel-to-aluminium explosive welds. Specifically, it was shown that the formation of aluminium-rich intermetallic phases at the weld interface increases the solidification time of the interfacial molten material, decreasing the weldability of these two materials. The formation of these intermetallic compounds should be avoided by reducing the interaction between the flyer and the baseplate as well as by avoiding excessive molten layers.

36 MATERIALS SCIENCE↗