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Thickness and microstructure characterization of TGO in thermal barrier coatings by 3D reconstruction
Yttria-stabilized zirconia (YSZ) thermal barrier coatings (TBCs) are prepared by plasma spraying. Thermally grown oxide (TGO) would be formed between YSZ topcoat and bond coat after 50 h thermal service for YSZ TBCs. The electron back scattered diffraction (EBSD) results reveal that the TGO layer is composed of α-Al{sub 2}O{sub 3} and cubic Al{sub 2}NiO{sub 4} layers. Measured values of TGO thickness from the 2D-SEM image are greater than or equal to its real thickness due to the fact that the TGO layer is much rolling so that up and down surfaces of the TGO can't be completely perpendicular to the cross-section direction confirmed by 3D-SEM. Furthermore, 3D-SEM results reveal that the real thickness of TGO layer is 3.10 μm instead of 7.1 μm. In addition, 3D-EBSD confirmed that α-Al{sub 2}O{sub 3} layer in TGO is composed of single layer of grains and Al{sub 2}NiO{sub 4} layer consist of multilayer of grains while α-Al{sub 2}O{sub 3} layer is mixed with single layer and multilayer of α-Al{sub 2}O{sub 3} grains from observation of the 2D-EBSD image. It provides a new method to characterize real thickness and microstructure of TGO, which is also applied to other film materials. - Highlights: •This work provides a new method to measure the real thickness of TGO. •YSZ TBCs were prepared by plasma spraying. •TGO is formed in TBCs by simulating thermal service at 1100 °C for 50 h. •Real thickness and microstructure of TGO were investigated by 3D reconstruction.
Particle stimulated nucleation during dynamic and metadynamic recrystallisation of Ni-30%Fe-Nb-C alloy
For the first time, a combination of scanning transmission electron microscopy and electron back-scattering diffraction is used to elucidate the early stages of particle stimulated recrystallisation at Nb carbides in Ni-30wt.%Fe alloy subjected to high temperature plane strain compression. While particles with sizes even below 1 μm were found to induce dynamic or metadynamic recrystallisation, only a small fraction of coarse particles served as nucleation sites. - Highlights: • The early stages of particle stimulated recrystallisation at Nb carbides are elucidated • A combination of transmission electron microscopy and electron back scattering diffraction used • Particles below 1 μm size could induce dynamic or metadynamic recrystallization.
Microstructure control to improve creep strength of alumina-forming austenitic heat-resistant steel by pre-strain
Highlights: • The effect of pre-strain on creep strength of AFA steel was studied. • The creep test was performed at 700°C and 200Mpa, and the aging test was carried out using box furnace at 700°C to simulate the microstructural evolution during creep. • Microstuctural evolution was observed by using SEM, EBSD, and TEM to investigate the relationship between creep strength and microstructure. - Abstract: At 700 °C and 200 MPa, the creep rupture time of W-containing alumina-forming austenitic heat-resistant (WAFA) steel increases from 1044 to 3119 h by pre-strain. Pre-strain introduces a lot of dislocation into the matrix and most of the dislocations remain stable to the end of creep without recovery and recrystallization. In addition, the dislocations have enabled secondary NbC and Laves phase to be uniformly distributed and refined. However, the dislocations lower grain boundary strength due to the coarsening of precipitates along grain boundaries Therefore, the increase in the creep rupture time in spite of deterioration of grain boundary strength is attributed to the dislocation strengthening and enhanced precipitation hardening within grains.
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.
Effect of filling materials on the microstructure and properties of hybrid laser welded Al-Mg-Si alloys joints
Highlights: • A serious comparison was made on the hybrid laser welded AA6061-T6 joint with different filling materials. • The microstructure of the welded joint was characterized using EBSD and SEM. • A strength model was successfully built to predict the strength of the hybrid laser welded AA6061-t6 joint. • The study shed new insights on how to select appropriate filling materials when using hybrid laser welding. - Abstract: A serious investigation was conducted to examine the influence of filling materials on the microstructure and properties of hybrid laser welded AA6061-T6 joints. The results of the tensile tests showed that the welded joint with ER4043 filling materials had higher tensile strength than that with ER5356 filling material. Based on the results obtained a strength model was built to predict and explain the enhancement of the yield strength of the hybrid laser welded AA6061-T6 joint with different welding wires. In contrast to the tensile strength, the ER4043 joint showed lower fatigue strength than that of the ER5356 joint due to extensive presence of micropores in fusion zone. Further, the corrosion experiment illustrated that the ER4043 joint had poorer resistance to the corrosive attack under 3.5% NaCl solution. A summary was made on the performance of both welded joints to shed new insights on selecting appropriate filling materials when welding AA6061-T6 by hybrid laser welding method.
Advanced processing of EBSD data to distinguish the complex microstructure evolution of a Cu-Ni-Si alloy induced by fatigue
Highlights: • Microstructure investigation of the fatigue behaviour of a Cu-Ni-Si alloy • Use of ECCI and EBSD to investigate the microstructure evolution related to fatigue dislocations structures • Characterisation of local plastic accommodation through EBSD misorientation criteria - Abstract: The present work aims at identifying the evolution of the microstructure of a Cu-Ni-Si (Corson alloy) alloy after low cycle fatigue by means of advanced electron microscopy analysis techniques (SEM-ECCI, Orientation Imaging Microscopy by means of SEM-EBSD and TEM). Deep attention is paid on the material subjected to high cyclic strains where a transient cellular dislocation structure transformed into precipitate free bands. It is shown that the formation of dislocation cells leads to a high GROD and high GOSaera value and its standard deviation. However, the presence of precipitate free bands results in the low GOSarea level and its low standard deviation.
XRD and SEM/EDS characterization of two quaternary fuel alloys (U-2.5Mo-2.5Ti-5.0Zr and U-1.5Mo-1.5Ti-7.0Zr in wt. %) for fast reactors
The current study focuses on characterization of two potential fuel alloys for sodium-cooled fast reactors: U-2.5Mo-2.5Ti-5.0Zr (U-MT5Z) and U-1.5Mo-1.5Ti-7.0Zr (U-MT7Z) in wt. %. As-cast alloys and annealed (600°C, 500h) alloys are studied by X-ray powder diffraction (XRD) for their bulk structures, and scanning electron microscopy / energy dispersive X-Ray spectroscopy (SEM/EDS) for their microstructures and phase constituents. For as-cast alloys, the XRD results show that U-MT5Z mainly contains γ, while U-MT7Z alloy contains a. In both alloys, there are three phases indicated by EDS, a U-rich phase, secondary phase, and Zr-rich phase. Further, the elemental compositions varied in different phases and in different alloys. After annealing, both alloys exhibit the structures of α-U and U 2 Ti according to XRD. The EDS results suggest there are five phases found in both alloys.
Coupling computational thermodynamics with density-function-theory based calculations to design L12 precipitates in Fe Ni based alloys
Achieving a high-volume fraction of thermodynamically stable L12-type precipitates that are resistant to coarsening is of great importance for the development of low-cost FeNi based austenitic steels. With the aid of computational thermodynamics, this work designed two model alloys: Fe-37.4Ni-6.1Al-2.9Ti (FNAT) and Fe-45.2Ni-5.9Al-8.5Si (FNAS). Both alloys were designed to contain a similar amount of L1 2 precipitate in Fe-Ni matrix without forming other precipitates. Density-Function-Theory (DFT) calculation was coupled with computational thermodynamics to predict the critical radius at which the precipitates change shape from spherical to cuboidal. The calculation results suggest that critical radius for the FNAT alloy is about two orders of magnitude larger than that for the FeNiAlSi alloy. Phase stability and morphology of the L1 2 precipitates in these two alloys were experimentally investigated through X-ray diffraction, atom probe tomography, and scanning and transmission electron microscopy. The L1 2 precipitates in the FeNiAlSi system were found to be cuboidal and rod shaped, with much larger size than the spherical ones in the FeNiAlTi system, agreeing with the calculation results. This work suggested that coupling computational thermodynamics with DFT calculations can be reliably used to design L1 2 precipitates in FeNi based alloys.
Silver-functionalized silica aerogel for iodine capture: Adsorbent aging by NO[subscript 2] in spent
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Tunable structural, morphological and optical properties of undoped, Mn, Ni and Ag-doped CuInS 2 thin films prepared by AACVD
The preparation of high-quality copper indium sulphide, CuInS 2 photo-absorber material with tunable properties for efficient, low-cost, thin film solar cells using scalable methods remains a challenge. In order to address this, high quality off-stoichiometric undoped and Mn, Ni and Ag-doped CuInS 2 (CIS) thin films have been deposited onto glass substrates by aerosol-assisted chemical vapour deposition (AACVD) using metal diethyldithiocarbamate precursors at temperatures of 350, 400 and 450 °C. Data from powder X-ray diffraction (p-XRD), Raman spectroscopy and scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS) suggest a correlation of morphology and composition of tetragonal phase (chalcopyrite and copper-gold-type) sulphur-deficient microcrystalline CIS thin films. For undoped thin films, near-infrared optical absorption and emission with tunable band gap between 1.32 and 1.42 eV are likely associated with donor-acceptor pairs involving deep or shallow electronic states such as sulphur vacancies (V S •• ), indium-copper anti-sites (In Cu •• ) and indium interstitials (In i ••• ) as donors and copper vacancies (V Cu ') as acceptors. Whilst Mn-doped thin films exhibit minimal tunable properties, Ni and Ag-doped films exhibit tunable morphology, composition and near-infrared absorption for small dopant content. Here, though further studies are required to explore the defect chemistry, these results show the utility of AACVD in tuning structural, morphological and optical properties of undoped, Mn, Ni and Ag-doped CIS thin films.
Orientation and morphology of Pt nanoparticles in γ-alumina processed via ion implantation and thermal annealing
Structure and chemistry of metal/metal-oxide interfaces are critical for many catalytic processes and sensing. Pristine interfaces of Pt and γ-Al 2 O 3 were fabricated using high-energy ion implantation and thermal processing. Amorphous regions of alumina develop in single crystal α-alumina during Pt+ implantation and an 800 °C thermal treatment crystalizes amorphized alumina to γ-Al 2 O 3 and allows Pt ions to precipitate within the developing γ-alumina, yielding Pt nanoparticle tetrahedra terminated by {111} surfaces. The phase of alumina that developed and the distribution, morphology, and orientation of Pt nanoparticles was determined using x-ray diffraction, Rutherford backscattering spectrometry, transmission electron microscopy and scanning transmission electron microscopy.
py4DSTEM: A Software Package for Four-Dimensional Scanning Transmission Electron Microscopy Data Analysis
Scanning transmission electron microscopy (STEM) allows for imaging, diffraction, and spectroscopy of materials on length scales ranging from microns to atoms. By using a high-speed, direct electron detector, it is now possible to record a full two-dimensional (2D) image of the diffracted electron beam at each probe position, typically a 2D grid of probe positions. These 4D-STEM datasets are rich in information, including signatures of the local structure, orientation, deformation, electromagnetic fields, and other sample-dependent properties. However, extracting this information requires complex analysis pipelines that include data wrangling, calibration, analysis, and visualization, all while maintaining robustness against imaging distortions and artifacts. In this paper, we present py4DSTEM, an analysis toolkit for measuring material properties from 4D-STEM datasets, written in the Python language and released with an open-source license. We describe the algorithmic steps for dataset calibration and various 4D-STEM property measurements in detail and present results from several experimental datasets. We also implement a simple and universal file format appropriate for electron microscopy data in py4DSTEM, which uses the open-source HDF5 standard. We hope this tool will benefit the research community and help improve the standards for data and computational methods in electron microscopy, and we invite the community to contribute to this ongoing project.
Energetics of a uranothorite (Th 1– x U x SiO 4 ) solid solution
High-temperature oxide melt solution calorimetric measurements were completed to determine the enthalpies of formation of the uranothorite, (USiO 4 ) x –(ThSiO 4 ) 1–x , solid solution. Phase-pure samples with x values of 0, 0.11, 0.21, 0.35, 0.71, and 0.84 were prepared, purified, and characterized by powder X-ray diffraction, electron probe microanalysis, thermogravimetric analysis and differential scanning calorimetry coupled with in situ mass spectrometry, and high-temperature oxide melt solution calorimetry. This work confirms the energetic metastability of coffinite, USiO 4 , and U-rich intermediate silicate phases with respect to a mixture of binary oxides. Furthermore, variations in unit cell parameters and negative excess volumes of mixing, coupled with strongly exothermic enthalpies of mixing in the solid solution, suggest short-range cation ordering that can stabilize intermediate compositions, especially near x = 0.5.
Reactive Adsorption of Humid SO 2 on Metal–Organic Framework Nanosheets
We explore the interactions of copper, zinc, and cobalt metal–organic framework (MOF) nanosheets with sulfur dioxide (40 ppm in air of 85% relative humidity at 25 °C), with the aim of understanding chemically induced structural changes of open-metal MOFs when exposed to wet acid gases such as flue gas. The structural evolution of the frameworks and the sulfur dioxide adsorption characteristics were studied by vibrational spectroscopy, powder X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The stabilities of the materials under the experimental conditions were established as a function of the metal center, with zinc benzenedicarboxylate (ZnBDC) being the most stable followed by CuBDC and CoBDC. After 80 ppm-days of exposure to humid SO 2 atmosphere, each MOF was found to contain roughly one sulfur atom per metal site. Adsorbed sulfur was found in the +6 and +2 oxidation states with the distribution across these states varying according to the metal in the material. The implication of this finding is that the aqueous chemistry of adsorbed sulfur dioxide is strongly influenced by the metal center. The ability to direct electron transfer to or from adsorbed sulfur while maintaining comparable particle and crystal structure is a powerful potential tool for desulfurization technologies.
Strain Effects in SrHfO 3 Films Grown by Hybrid Molecular Beam Epitaxy
Perovskite oxide heterostructures host a large number of interesting phenomena such as ferroelectricity, which are often driven by octahedral distortions in the crystal that may induce polarization. SrHfO 3 (SHO) is a perovskite oxide with a pseudocubic lattice parameter of 4.08 Å that previous density functional theory (DFT) calculations suggest can be stabilized in a ferroelectric P4mm phase when stabilized with sufficient compressive strain. Additionally, it is insulating and possesses a large band gap and a high dielectric constant, making it an ideal candidate for oxide electronic devices. Here, to test the viability of epitaxial strain as a driver of ferroic phase transitions, SHO films were grown by hybrid molecular beam epitaxy (hMBE) with a tetrakis(ethylmethylamino)hafnium(IV) source on GdScO 3 and TbScO 3 substrates. Strained SHO phases were characterized using X-ray diffraction, X-ray absorption spectroscopy, and scanning transmission electron microscopy to determine the space group of the strained films, with the results compared to those of DFT-optimized models of phase stability versus strain. Contrary to past reports, we find that compressively strained SrHfO 3 undergoes octahedral tilt distortions without associated ferroelectric polarization and most likely takes on the I4/mcm phase with the a 0 a 0 c – tilt pattern.
Iridium-Doped Nanosized Zn–Al Layered Double Hydroxides as Efficient Water Oxidation Catalysts
Layered double hydroxides (LDHs) are an ideal platform to host catalytic metal centers for water oxidation (WO) owing to the high accessibility of water to the interlayer region, which makes all centers potentially reachable and activated. In this paper, we report the syntheses of three iridium-doped zinc–aluminum LDHs (Ir-LDHs) nanomaterials (1–3, with about 80 nm of planar size and a thickness of 8 nm as derived by field emission scanning electron microscopy and powder X-ray diffraction studies, respectively), carried out in the confined aqueous environment of reverse micelles, through a very simple and versatile procedure. These materials exhibit excellent catalytic performances in WO driven by NaIO 4 at neutral pH and 25 °C, with an iridium content as low as 0.5 mol % (~0.8 wt %), leading to quantitative oxygen yields (based on utilized NaIO 4 , turnover number up to ~10,000). Nanomaterials 1–3 display the highest ever reported turnover frequency values (up to 402 min –1 ) for any heterogeneous and heterogenized catalyst, comparable only to those of the most efficient molecular iridium catalysts, tested under similar reaction conditions. The boost in activity can be traced to the increased surface area and pore volume (>5 times and 1 order of magnitude, respectively, higher than those of micrometric materials of size 0.3–1 μm) estimated for the nanosized particles, which guarantee higher noble metal accessibility. X-ray absorption spectroscopy (XAS) studies suggest that 1–3 nanomaterials, as-prepared and after catalysis, contain a mixture of isolated, single octahedral Ir(III) sites, with no evidence of Ir–Ir scattering from second-nearest neighbors, excluding the presence of IrO 2 nanoparticles. The combination of the results obtained from XAS, elemental analysis, and ionic chromatography strongly suggests that iridium is embedded in the brucite-like structure of LDHs, having four hydroxyls and two chlorides as first neighbors. These results demonstrate that nanometric LDHs can be successfully exploited to engineer efficient WOCs, minimizing the amount of iridium used, consistent with the principle of the noble-metal atom economy.