SEARCH · Engineering Papers

Results for “dissolution”

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.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,747 records · Page 97

All sources NASA NTRS DOE OSTI

DOE OSTI2020

Vertical effective stress and temperature as controls of quartz cementation in sandstones: Evidence from North Sea Fulmar and Gulf of Mexico Wilcox sandstones

Here we present quantitative petrographic data, high spatial resolution oxygen isotope analyses of quartz cement, basin modelling and a kinetic model for quartz precipitation for two Paleocene-Eocene Wilcox Group sandstones from Texas and two Jurassic Fulmar Formation sandstones from the Central North Sea. At each location, one sandstone has been buried to ca. 145 °C and one to ca. 185 °C. A key difference between the Wilcox and Fulmar burial histories is that the Wilcox sandstones are currently at higher vertical effective stresses and, from basin modelling studies, have been subjected to generally higher vertical effective stresses through their burial history. The amounts of quartz cement in the Wilcox sandstones are between 12 and 18%, and between 2 and 6% in the Fulmar sandstones. High-spatial-resolution oxygen isotope data obtained from the quartz cements suggest temperature ranges for quartz precipitation from 60 to 80 °C to values approaching maximum burial temperature. Factors such as grain coatings or the timing of petroleum emplacement cannot explain the differences in the amounts of quartz cement. Petrographic data show that most of the silica for quartz cement can be derived from intergranular pressure dissolution. Although the sample set is small, we interpret the results to suggest that the differences in quartz cementation in Fulmar and Wilcox sandstones can be explained better by differences in their vertical effective stress history than their temperature history; in this case, the supply of silica rather than the precipitation of quartz becomes an important control on the rate and extent of cementation.

58 GEOSCIENCES↗

DOE OSTI2014

The role of local strains from prior cold work on stress corrosion cracking of α-brass in Mattsson's solution

The dynamic strain rate ahead of a crack tip formed during stress corrosion cracking (SCC) under a static load is assumed to arise from the crack propagation. The strain surrounding the crack tip would be redistributed as the crack grows, thereby having the effect of dynamic strain. Recently, several studies have shown cold work to cause accelerated crack growth rates during SCC, and the slip-dissolution mechanism has been widely applied to account for this via a supposedly increased crack-tip strain rate in cold worked material. While these interpretations consider cold work as a homogeneous effect, dislocations are generated inhomogeneously within the microstructure during cold work. The presence of grain boundaries results in dislocation pile-ups that cause local strain concentrations. The local strains generated from cold working α-brass by tensile elongation were characterized using electron backscatter diffraction (EBSD). The role of these local strains in SCC was studied by measuring the strain distributions from the same regions of the sample before cold work, after cold work, and after SCC. Though, the cracks did not always initiate or propagate along boundaries with pre-existing local strains from the applied cold work, the local strains surrounding the cracked boundaries had contributions from both the crack propagation and the prior cold work. - Highlights: • Plastic strain localization has a complex relationship with SCC susceptibility. • Surface relief created by cold work creates its own granular strain localization. • Cold work promotes crack growth but several other factors are involved.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Microstructural, mechanical and electrochemical behaviour of a 7017 Al–Zn–Mg alloy of different tempers

The aim of the investigation is to assess the microstructural features and associated physical, mechanical and electrochemical properties of a 7017 Al–Zn–Mg alloy of various tempers. A 7017 Al–Zn–Mg alloy was subjected to different ageing schedules to produce under-(T4), peak-(T6), over-(T7) and highly over-aged tempers. Optical microscopy, hardness measurement, electrical conductivity measurement, tensile testing and SEM fractographs, differential scanning calorimetry (DSC), transmission electron microscopy (TEM), and electrochemical polarization studies have been used to characterize the alloy tempers. Hardness measurement and tensile testing showed the characteristic age hardening phenomenon of aluminium alloys. Optical and TEM micrographs have revealed the variation in size of matrix strengthening η′ (MgZn{sub 2}) and also the size and distribution of grain boundary η (MgZn{sub 2}) precipitate with ageing time. DSC thermograms exhibiting exothermic and endothermic peaks indicated the characteristic solid state reaction sequence of the 7017 alloy. Potentiodynamic polarization study of the 7017 alloy of various tempers in 3.5 wt.% NaCl solution at near neutral pH showed typical active metal dissolution behaviour, but at pH 12 an active–passive–transpassive transition behaviour has been observed. - Graphical abstract: TEM micrograph of the 7017 aluminium alloy of various tempers (a, b) under aged (T4), (c, d) peak aged (T6), (e, f) over aged (T7) and (g, h) highly over-aged. Display Omitted - Highlights: • 7017 Al-Zn-Mg alloy was subjected to different artificial ageing treatments. • Characterization of 7017 alloy tempers by hardness, tensile, DSC, TEM and electrochemical behaviour. • Structure-properties relationship of the 7017 Al-Zn-Mg alloy of various tempers.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2016

Sample preparation methods for scanning electron microscopy of homogenized Al-Mg-Si billets: A comparative study

Characterization of Mg-Si precipitates is crucial for optimizing the homogenization heat treatment of Al-Mg-Si alloys. Although sample preparation is key for high quality scanning electron microscopy imaging, most common methods lead to dealloying of Mg-Si precipitates. In this article we systematically evaluate different sample preparation methods: mechanical polishing, etching with various reagents, and electropolishing using different electrolytes. We demonstrate that the use of a nitric acid and methanol electrolyte for electropolishing a homogenized Al-Mg-Si alloy prevents the dissolution of Mg-Si precipitates, resulting in micrographs of higher quality. This preparation method is investigated in depth and the obtained scanning electron microscopy images are compared with transmission electron micrographs: the shape and size of Mg-Si precipitates appear very similar in either method. The scanning electron micrographs allow proper identification and measurement of the Mg-Si phases including needles with lengths of roughly 200 nm. These needles are β″ precipitates as confirmed by high resolution transmission electron microscopy. - Highlights: •Secondary precipitation in homogenized 6xxx Al alloys is crucial for extrudability. •Existing sample preparation methods for SEM are improvable. •Electropolishing with nitric acid/methanol yields superior quality in SEM. •The obtained micrographs are compared to TEM micrographs.

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

Microstructural and microchemical studies of phase stability in V-O solid solution

Over the last couple of decades vanadium and V-based alloys have received significant attention as a potential structural material for fusion power applications because of their favourable mechanical properties under irradiation and at elevated temperatures. They are also considered as the advanced options of storage materials for hydrogen and its isotopes. However, the higher affinity of V for O, C and N poses critical challenges in its engineering applications since they lead to degradation of mechanical properties. They can further interact with the matrix to produce metallic oxy-carbo-nitride precipitates. To a certain limit, these precipitates are beneficial and can be exploited to enhance the mechanical behaviour of the alloy through suitable microstructural design. However, this requires a prior knowledge of the interaction between the alloy and the impurity solutes. In the present work vanadium specific experiments have been designed and carried out to bring out the V-interstitial solute interaction by charging oxygen in the near surface region of vanadium. Microstructural and microchemical behaviour of the V-O solid solution has been studied through HRTEM (high resolution transmission electron microscopy) and HAADF (high angle annular dark field) coupled with EELS. Quantitative electron microscopy has been carried out to study structural modification of the alloy in atomic level caused by O charging. - Highlights: •Controlled experiments were carried out in pulsed laser ablation set-up to promote V-O interaction. • As a consequence of O dissolution, V transformed into a bct structure which is otherwise a bcc structure. •In V-O solid solution, dissolved O in the V matrix introduces significant amount of lattice strain. • Present work can be extended for introducing interstitial O in other pure transition metals and their alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2017

A quasi-in-situ EBSD observation of the transformation from rolling texture to recrystallization texture in V-4Cr-4Ti alloy

Recrystallization texture evolution of rolled V-4Cr-4Ti alloy has been investigated by quasi-in-situ EBSD (electron back-scattering diffraction) method. Concurrently, the precipitates were characterized by SEM (Scanning Electron Microscopy). It was found that both the initial rolling textures and the distribution of the precipitates affected the formation of the recrystallization texture. It was revealed that the texture transformations of (558) 〈110〉 + (665) 〈110〉 to (334) 〈483〉 + (665) 〈1 1 2.4〉 were possibly attributed to the selective drag induced by the sparsely dispersed Ti-rich precipitates. While the densely distributed Ti-rich precipitates were responsible for the randomized recrystallization texture. Finally, when the precipitates were absent, the orientation changes from (112) 〈110〉 and (558) 〈110〉 to (111) 〈112〉 and (001) <110> to (001) <520> were observed. - Highlights: • Micro recrystallization texture evolution in V-4Cr-4Ti alloys is reported for the first time. • The volume fraction of Ti-rich precipitates has significant effect on the recrystallization texture evolution. • The dissolution of the Ti-rich precipitates above 1100 °C induces the strengthening of (111) <112> texture.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Characterisation of ODS Fe-14Cr-2W-0.3Ti before and after high temperature triple and low temperature single ion irradiations

Highlights: • Nanoparticles stable after high temperature triple-beam and low temperature single-beam irradiation • Samples appear to have maintained the composition after both irradiations. • Slight decrease of the nanoparticle sizes below 5 nm after both irradiations • There appears to be incomplete dissolution of smaller nanoparticles after both irradiations. - Abstract: Oxide dispersion strengthened reduced activation ferritic steels are being considered as structural materials for future fusion reactors and Gen IV fission reactors. In this work, the stability of the nanometric oxides after being irradiated at different conditions and temperatures has been investigated. A Fe-14Cr-2W-0.3Ti-0.3Y{sub 2}O{sub 3} alloy was simultaneously triple-beam irradiated at 600 °C with Fe, He and H ions. The same alloy was irradiated with Fe ions at − 80 °C. The microstructure of this alloy was investigated using Transmission Electron Microscopy, Atom Probe Tomography and nanoindentation before and after the irradiations. There were no significant changes in the morphology and chemical composition of the nanoparticles after the irradiations, although the size of the smaller ones tends to decrease for both irradiation conditions. Small irradiation-induced bubbles were present after the triple simultaneous irradiation at high temperature. Nanoindentation also shows no significant differences with a slight increase in hardness for the sample irradiated at low temperature, while softening appears in the high temperature irradiation.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effect of interfacial reaction on Young's modulus in CNT/Al nanocomposite: A quantitative analysis

Highlights: • Effect of interfacial reaction on Young’s modulus of CNT/Al composite was quantitatively revealed. • Both qualitative and quantitative characterizations of CNT/Al interfacial reaction were conducted. • Volume expansion induced by CNTs-Al{sub 4}C{sub 3} transformation was the key to modulus increase with greater reaction degree. • The significant role of raw CNTs quality in “Young’s modulus-interfacial reaction” relationship was uncovered. - Abstract: 1.5 wt% CNT/Al nanocomposite with limited, moderate and severe interfacial reaction were prepared by flake PM and annealing to study the effect of interfacial reaction on Young's modulus. Both qualitative and quantitative characterizations of CNT/Al interfacial reaction were conducted through TEM observation and electrochemical dissolution. The results showed that the strong reinforcing effect of reaction-formed Al{sub 4}C{sub 3} and the significant volume expansion effect during CNTs-Al{sub 4}C{sub 3} transformation resulted in Young's modulus increase with greater CNT/Al interfacial reaction degree. The significant role of raw CNTs quality in “Young's modulus-interfacial reaction degree” relationship was discussed. Both raw CNT quality and CNT/Al interfacial reaction need to be well controlled and optimized for fabricating CNT/Al nanocomposite with higher Young's modulus.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2018

Interfacial structure and properties of Cu/Al joints brazed with Zn-Al filler metals

Highlights: • The formation mechanism of Cu side interfacial compounds of Cu/Al joints with Zn-Al filler metals are revealed accurately. • The Cu side interfacial structure is uncertain and dependent on brazing parameters, especially cooling rate after brazing. • The close relation among composition, brazing parameters, interfacial structure and mechanical properties is discovered. - Abstract: Seeing that opinions vary, no unanimous conclusion has been drawn on Cu side interfacial structure and its relationship with the mechanical properties of Cu/Al joints brazed with Zn-Al filler metals, XRD, SEM and HAADF-STEM were used to accurately reveal the Cu side interfacial structure and the mechanism concerned. The relationship among the brazing process, interfacial structure and mechanical properties of the joints was systematically studied. The following phenomena and principles were newly found and clarified. The Cu side interfacial structure are uncertain and dependent on brazing parameters, especially cooling rate after brazing, in addition to the composition of Zn-Al filler metal. High cooling rate promotes the formation of CuZn and Al{sub 4.2}Cu{sub 3.2}Zn{sub 0.7} compounds, while slow cooling rate is beneficial for the formation of Cu-Al interfacial compounds at the Cu side interface. Increasing brazing temperature or lengthening holding time enhances the dissolution of base metals, which results in the increase of Al and Cu contents at the Cu side interface, thus promoting the formation of CuAl{sub 2} compound. Besides, increasing Al content in Zn-Al filler metal also promotes the formation of CuAl{sub 2} compound by directly increasing Al content at the Cu side interface. The significant differences in joint strength are caused by the differences of Cu side interfacial compounds essentially. When the thin CuZn and Al{sub 4.2}Cu{sub 3.2}Zn{sub 0.7} layers exist at the Cu side interface, the brazed joint possesses high shear strength. On the contrary, the formation of Cu-Al compound layers at the Cu side interface, especially CuAl{sub 2}, will severely degrade the joint strength.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Microstructure, precipitates and hardness of selectively laser melted AlSi10Mg alloy before and after heat treatment

Highlights: • Microstructural characterization of SLM AlSi10Mg alloy and comparison with cast and powder AlSi10Mg • Effect of solution heat treatment and aging on the hardness change of SLM AlSi10Mg alloy • Evolution of strengthening precipitates and Fe-rich intermetallics in SLM AlSi10Mg during heat treatment - Abstract: The microstructure and precipitates within selectively laser melted (SLM) AlSi10Mg alloys in the as-built state and after T6 heat treatment were examined and correlated to the hardness evolution. The as-built alloy exhibited columnar patterns perpendicular to the build-direction and fish-scale pattern along the build-direction originating from the melt pool. The microstructure consisted of fine Al cells and eutectic structure with up to 4 μm in size. Tiny needle-like Si particles with highly faulted structure were identified within the Al cells and formed semi-coherent interface with the matrix. Nanoscale Si particles and π-Al{sub 8}Si{sub 6}Mg{sub 3}Fe phase were observed to segregate along the cell and grain boundary. Solution heat treatment (SHT) at 520 °C resulted in the dissolution of Al cellular microstructure. Precipitation and coarsening of the Si particles occurred, while the aspect ratio of Si particles remained nearly constant. The π-Al{sub 8}Si{sub 6}Mg{sub 3}Fe phase decomposed into plate-shaped β-Al{sub 5}SiFe. The artificial aging (AA) at 160 °C did not alter the microstructure but led to the formation of metastable Mg{sub 2}Si precipitates. The GP zones and β″ were identified through transmission electron microscopy after AA of 6 h, and β″ existed up to AA of 24 h. The hardness decreased after SHT due to the coarsening of the microstructure and reduced solid solution hardening. Hardness reached maximum magnitude after AA of 6–10 h due to the precipitation hardening, and remained relatively unchanged up to AA of 24 h. Microstructure and/or hardness of gas atomized powders and bulk cast AlSi10Mg alloys were also examined as references.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Coarsening of nanoscale (Ti,Mo)C precipitates in different ferritic matrixes

Coarsening of nanoscale (Ti,Mo)C precipitates within quasi-polygonal ferritic (QPF) matrix and polygonal ferritic (PF) matrix is studied via HRTEM and In-situ heating TEM. Influenced by different nucleation processes, inverse coarsening process showing dissolution of large clustered precipitates and growth of small interphase precipitates is directly observed in the PF matrix. However, due to the evolution of high-density subboundaries, coarsening of precipitates in QPF matrix is mainly characterized by the subboundary migration assisted coarsening process, during which arch-like coarsened precipitates form after the sweeping of subboundaries. Analysis of atomic structure clarify that “imposts” of the arch-like coarsened precipitates are established by the re-precipitation of solute atoms from movable subboundary to the close packed planes {111} of (Ti,Mo)C precipitates, and that the “key stones” are constructed due to the change of re-precipitation planes to {200}. Geometric phase analysis (GPA) illustrates that not only the change of re-precipitation direction during the formation of arch-like precipitates, but also the selective coarsening of clustered precipitates in PF matrix, is caused by the highly anisotropic strain field around (Ti,Mo)C precipitates.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Crystal development during carbonation of lime-based mortars in different environmental conditions

Highlights: • High CO{sub 2} and DiloCarb® treatment favour advanced carbonation and self-healing. • In the lime mortar without ceramics, channel type pores occur in the aggregate border. • In the lime mortars with ceramics, vug type pores are produced in the binder during kneading. • The formation of tabular CaCO{sub 3} polymorphs caused an increase in stress leading to microshrinkage cracks. • The use of a ceramic provoked dissolution and then re-precipitation of more stable polymorphs. - Abstract: This study examines crystal development during the carbonation of lime mortars according to the additives used and curing conditions. Two types of samples were prepared, one with sand and the other one additionally including Roman ceramics. These mortars were cured: 1) by spraying with a carbonation accelerator product under laboratory conditions; 2) in a climate chamber under 20 °C, 60% relative humidity, and 1600 ppm CO{sub 2}; and 3) under laboratory conditions as controls. Polarized light microscopy, SEM-EDS and XRD were used at 28, 90, 120 and 180 days to monitor the carbonation process. Observations indicate the development of different CaCO{sub 3} polymorphs, which appeared as metastable phases. The early nucleation of a well-defined calcite phase as the most stable CaCO{sub 3} polymorph was only identified in the chamber-cured samples. Differences in the pore network were observed depending on the composition and morphology of the mortar components and the environmental curing conditions.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Response relationship between loading condition and corrosion fatigue behavior of nickel-aluminum bronze alloy and its crack tip damage mechanism

Highlights: • The differences of corrosion fatigue behavior of NAB alloy in air and in 3.5% NaCl solution are carefully compared. • The corrosion environment significantly accelerates the crack growth of NAB alloy and decreases the fatigue threshold. • The corrosion fatigue crack growth rate increases with the decrease of loading frequency. • The acidification and the dealumination occur in process of corrosion fatigue, resulting in the deterioration of crack tip. - Abstract: Corrosion fatigue is one of the major forms for nickel‑aluminum bronze alloy used in marine propeller. It is greatly important to understand the corrosion fatigue behavior of nickel‑aluminum bronze alloy in seawater for the purpose of improving the service life of marine equipment. In this study, corrosion fatigue crack growth rate of nickel‑aluminum bronze alloy in 3.5% NaCl solution was tested under various stress intensity factors, stress ratios and loading frequencies to reveal its corrosion fatigue mechanism. The results show that corrosion environment significantly accelerates the crack growth and decreases the corrosion fatigue threshold, which is attributed to the corrosion reactions between the metals of crack tip and corrosive medium. Among the various factors, loading frequency has more predominant influence on the corrosion fatigue crack growth rate of nickel‑aluminum bronze alloy, which can be rationally explained by the hydrogen embrittlement mechanism. Additionally, in the process of corrosion fatigue crack growth, the acidification and the dealumination would occur at the crack tip, resulting in the corrosion dissolution of κ phases and the deterioration in mechanical properties of crack tip.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effects of in-process cryocooling on metallurgical and mechanical properties of friction stir processed Al7075 alloy

Highlights: • For in-process cryocooling (IPC) during FSP, an efficient cooling fixture was designed & fabricated. • FSP of Al7075 alloy with IPC setup suppressed precipitate coarsening as well as grain growth. • Nanosize η′ precipitates (20–30 nm) in IPC condition increased work hardening capacity & strength. • Simultaneous improvement in ductility & strength occurred for sample FSPed with IPC. - Abstract: Friction stir processing (FSP) of heat treatable aluminum alloys is reported to deteriorate strength and hardness properties in spite of huge grain size refinement. The improvement in strength due to the grain size refinement after FSP could not be able to offset the reduction in strength due to coarsening or dissolution of the strengthening precipitate(s). To overcome this, the present work investigates an effective way of heat rejection from the FSP zone to control the precipitate evolution besides the grain size refinement during FSP of Al7075 alloy. The FSP was carried out with standardized process parameters (i.e. 720 rpm, 65 mm/min traverse speed) under two different cooling environments: (i) at normal air cooling and (ii) by rushing a chilled mixture (−30 °C) of liquid nitrogen and methanol through the bottom of the backing plate. Microstructural evolution was examined through optical, scanning and transmission electron microscopy and electron backscatter diffraction to confirm the grain size and morphology of precipitate(s) formed. The in-process cryocooling during the FSP led to 65 and 72% improvement in the Vickers hardness and tensile strength, respectively, in comparison to the solutionized base metal. The results have been analyzed in terms of precipitate interface characteristics and its strengthening effect, Hall–Petch strengthening due to grain size reduction and tradeoff between them.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Preparation and electrochemical performance of sulfur-alumina cathode material for lithium-sulfur batteries

Highlights: ► Micron-sized alumina was synthesized as adsorbent for lithium-sulfur batteries. ► Sulfur-alumina material was synthesized via crystallizing nucleation. ► The Al{sub 2}O{sub 3} can provide surface area for the deposition of Li{sub 2}S and Li{sub 2}S{sub 2}. ► The discharge capacity of the battery is improved during the first several cycles. - Abstract: Nano-sized sulfur particles exhibiting good adhesion with conducting acetylene black and alumina composite materials were synthesized by means of an evaporated solvent and a concentrated crystallization method for use as the cathodes of lithium-sulfur batteries. The composites were characterized and examined by X-ray diffraction, environmental scanning electron microscopy and electrochemical methods, such as cyclic voltammetry, electrical impedance spectroscopy and charge–discharge tests. Micron-sized flaky alumina was employed as an adsorbent for the cathode material. The initial discharge capacity of the cathode with the added alumina was 1171 mAh g{sup −1}, and the remaining capacity was 585 mAh g{sup −1} after 50 cycles at 0.25 mA cm{sup −2}. Compared with bare sulfur electrodes, the electrodes containing alumina showed an obviously superior cycle performance, confirming that alumina can contribute to reducing the dissolution of polysulfides into electrolytes during the sulfur charge–discharge process.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Stability of the solid electrolyte Li{sub 3}OBr to common battery solvents

Graphical abstract: The stability of the anti-perovskite phase Li{sub 3}OBr has been assessed in a variety of battery solvents. - Highlights: • Lithium stable solid electrolyte Li{sub 3}OBr unstable to polar organic solvents. • Solvation with no dissolution destroys long-range structure. • Ion exchange with protons observed. - Abstract: Recently a new class of solid lithium ion conductors was reported based on the anti-perovskite structure, notably Li{sub 3}OCl and Li{sub 3}OBr. For many beyond lithium-ion battery uses, the solid electrolyte is envisioned to be in direct contact with liquid electrolytes and lithium metal. In this study we evaluated the stability of the Li{sub 3}OBr phase against common battery solvents electrolytes, including diethylcarbonate (DEC) and dimethylcarbonate (DMC), as well as a LiPF{sub 6} containing commercial electrolyte. In contact with battery-grade organic solvents, Li{sub 3}OBr was typically found to be insoluble but lost its crystallinity and reacted with available protons and in some cases with the solvent. A low temperature heat treatment was able to restore crystallinity of the samples; however evidence of proton ion exchange was conserved.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Carbonated hydroxyapatite starting from calcite and different orthophosphates under moderate hydrothermal conditions: Synthesis and surface reactivity in simulated body fluid

Highlights: • Carbonated apatite (CAP) could be easily obtained from CaCO{sub 3} and orthophosphates. • Highest CaCO{sub 3} dissolution and apatitic carbonate content were obtained with H{sub 3}PO{sub 4}. • A-B-type CAP was formed. • The synthesized CAP was thermally stable up to 1000 °C. • This CAP showed high biomineralization activity before and after thermal treatment. - Abstract: The one-step synthesis of carbonated hydroxyapatite (CAP) using calcite and different orthophosphates was investigated in a closed batch reactor. Only orthophosphoric acid could lead to the complete decomposition of calcite particles, when the reaction temperature was set at 80 °C. On the other hand, the reaction time and the dilution of the initial calcite suspension had no significant influence on the formation of the solid products. CAP was formed as the main crystalline calcium phosphate with the carbonate content in the range of 4.2–4.6 wt.%. The thermal decarbonation of the synthesized CAP started at 750 °C but it was only significant at 1000 °C under air atmosphere. This thermal decarbonation was total at 1200 °C or above. All CAP samples and products following thermal treatments were found bioactive in the test using simulated body fluid (SBF) solution.

36 MATERIALS SCIENCE↗