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1.
Sci Rep ; 14(1): 7104, 2024 Mar 26.
Artigo em Inglês | MEDLINE | ID: mdl-38531954

RESUMO

We present the fabrication of a MoS2-xSex thin film from a co-sputtering process using MoS2 and MoSe2 commercial targets with 99.9% purity. The sputtering of the MoS2 and MoSe2 was carried out using a straight and low-cost magnetron radio frequency sputtering recipe to achieve a MoS2-xSex phase with x = 1 and sharp interface formation as confirmed by Raman spectroscopy, time-of-flight secondary ion mass spectroscopy, and cross-sectional scanning electron microscopy. The sulfur and selenium atoms prefer to distribute randomly at the octahedral geometry of molybdenum inside the MoS2-xSex thin film, indicated by a blue shift in the A1g and E1g vibrational modes at 355 cm-1 and 255 cm-1, respectively. This work is complemented by computing the thermodynamic stability of a MoS2-xSex phase whereby density functional theory up to a maximum selenium concentration of 33.33 at.% in both a Janus-like and random distribution. Although the Janus-like and the random structures are in the same metastable state, the Janus-like structure is hindered by an energy barrier below selenium concentrations of 8 at.%. This research highlights the potential of transition metal dichalcogenides in mixed phases and the need for further exploration employing low-energy, large-scale methods to improve the materials' fabrication and target latent applications of such structures.

2.
Materials (Basel) ; 16(24)2023 Dec 10.
Artigo em Inglês | MEDLINE | ID: mdl-38138728

RESUMO

Platform heating is one of the effective strategies used in laser powder bed fusion (LPBF) to avoid cracking during manufacturing, especially when building relatively large-size components, as it removes significant process-induced residual strains. In this work, we propose a novel and simple method to spare the elaborate post-processing heat treatment typically needed for LPBF Al-Sc alloys without compromising the mechanical properties. We systematically investigated the effects of LPBF platform heating at 200 °C on the residual stress relief, microstructure, and mechanical performance of a high-strength Al-Mn-Sc alloy. The results reveal that LPBF platform heating at 200 °C is sufficient to largely relieve the process-induced residual stresses compared to parts built on an unheated 35 °C platform. Meanwhile, the platform heating triggered the dynamic precipitation of uniformly dispersed (1.5-2 nm) Sc-rich nano-clusters. Their formation in a high number density (1.75 × 1024 m-3) resulted in a ~20% improvement in tensile yield strength (522 MPa) compared to the build on the unheated platform, without sacrificing the ductility (up to 18%). The improved mechanical properties imply that platform heating at 200 °C can strengthen the LPBF-synthesised Sc-containing Al alloys via in situ aging, which is further justified by an in situ measurement study revealing that the developing temperatures in the LPBF part are within the aging temperature range of Al-Sc alloys. Without any post-LPBF treatments, these mechanical properties have proven better than those of most Al-Sc alloys through long-time post-LPBF heat treatment.

3.
ACS Nano ; 17(21): 21531-21538, 2023 Nov 14.
Artigo em Inglês | MEDLINE | ID: mdl-37902648

RESUMO

Lithium-ion batteries (LIBs) are the dominating energy storage technology for electric vehicles and portable electronic devices. Since the resources of raw materials for LIBs are limited and recycling technologies for LIBs are still under development, improvements in the long-term stability of LIBs are of paramount importance and, in addition, would lead to a reduction in the levelized cost of storage (LCOS). A crucial limiting factor is the aging of the solid electrolyte interphase (SEI) on the active material particles in the anode. Here, we demonstrate the potential of atom probe tomography for elucidating the complex mosaic-type structure of the SEI in a graphite composite anode. Our 3D reconstruction shows unseen details and reveals the existence of an apolar organic microphase pervading the SEI over its entire thickness. This finding is in stark contrast to the prevalent two-layer SEI model, in which organic compounds are the dominating species only in the outer SEI layer being in contact with the liquid electrolyte. The observed spatial arrangement of the apolar organic microphase promises a better understanding of the passivation capability of the SEI, which is necessary to expand the battery lifetime.

4.
Materials (Basel) ; 16(4)2023 Feb 07.
Artigo em Inglês | MEDLINE | ID: mdl-36837019

RESUMO

Tungsten trioxide (WO3) is a versatile n-type semiconductor with outstanding chromogenic properties highly used to fabricate sensors and electrochromic devices. We present a comprehensive experimental study related to piezoresponse with piezoelectric coefficient d33 = 35 pmV-1 on WO3 thin films ~200 nm deposited using RF-sputtering onto alumina (Al2O3) substrate with post-deposit annealing treatment of 400 °C in a 3% H2/N2-forming gas environment. X-ray diffraction (XRD) confirms a mixture of orthorhombic and tetragonal phases of WO3 with domains with different polarization orientations and hysteresis behavior as observed by piezoresponse force microscopy (PFM). Furthermore, using atom probe tomography (APT), the microstructure reveals the formation of N2-filled nanovoids that acts as strain centers producing a local deformation of the WO3 lattice into a non-centrosymmetric structure, which is related to piezoresponse observations.

5.
Materials (Basel) ; 13(22)2020 Nov 21.
Artigo em Inglês | MEDLINE | ID: mdl-33233381

RESUMO

The phase transformation to ausferrite during austempered ductile iron (ADI) heat treatment can be significantly influenced by the alloying element Mo. Utilizing neutron diffraction, the phase transformation from austenite to ausferrite was monitored in-situ during the heat treatment. In addition to the phase volume fractions, the carbon enrichment of retained austenite was investigated. The results from neutron diffraction were compared to the macroscopic length change from dilatometer measurements. They show that the dilatometer data are only of limited use for the investigation of ausferrite formation. However, they allow deriving the time of maximum carbon accumulation in the retained austenite. In addition, the transformation of austenite during ausferritization was investigated using metallographic methods. Finally, the distribution of the alloying elements in the vicinity of the austenite/ferrite interface zone was shown by atom probe tomography (APT) measurements. C and Mn were enriched within the interface, while Si concentration was reduced. The Mo concentration in ferrite, interface and austentite stayed at the same level. The delay of austenite decay during Stage II reaction caused by Mo was studied in detail at 400 °C for the initial material as well as for 0.25 mass % and 0.50 mass % Mo additions.

6.
Nanoscale Adv ; 1(8): 3036-3048, 2019 Aug 06.
Artigo em Inglês | MEDLINE | ID: mdl-36133600

RESUMO

Fe-based superconductors present a large variety of compounds whose physical properties strongly depend on the crystal structure and chemical composition. Among them, the so-called 1111 compounds show the highest critical temperature T c in the bulk form. Here we demonstrate the realization of excellent superconducting properties in NdFeAs(O1-x F x ). We systematically investigated the correlation between the microstructure at the nanoscale and superconductivity in an epitaxial 22 nm NdFeAs(O1-x F x ) thin film on a MgO single crystalline substrate (T c = 44.7 K). Atomic resolution analysis of the microstructure by transmission electron microscopy and atom probe tomography identified several defects and other inhomogeneities at the nanoscale that can act as extrinsic pinning centers. X-Ray diffraction and transmission electron microscopy displayed a broad variation of the a-axis lattice parameter either due to a partially strained layer at the interface to the substrate, high local strain at dislocation arrays, mosaicity, or due to composition variation within the film. The electrical transport properties are substantially affected by intrinsic pinning and a matching field corresponding to the film thickness and associated with the Bean-Livingston surface barrier of the surfaces. The thin film showed a self-field critical current density J c(4.2 K) of ∼7.6 MA cm-2 and a record pinning force density of F p ≈ 1 TN m-3 near 35 T for H‖ab at 4.2 K. These investigations highlight the role of the microstructure in fine-tuning and possibly functionalizing the superconductivity of Fe-based superconductors.

7.
Sci Rep ; 7(1): 3254, 2017 06 12.
Artigo em Inglês | MEDLINE | ID: mdl-28607382

RESUMO

The precipitation mechanism of the δ' (Al3Li) phase in Al-Li alloys has been controversially discussed in recent decades, specifically with respect to a conjectured congruent ordering process. However, kinetics in the Al-Li system does not allow to resolve the intermediate stages of precipitation and hence to experimentally clarify this issue. In this paper, we are revisiting the subject in ternary Al-Cu-Li alloys with pronouncedly slower kinetics, employing Transmission Electron Microscopy, High-Angle Annular Dark-Field Scanning Transmission Electron Microscopy, Differential Scanning Calorimetry and Atom Probe Tomography. The results show clear evidence for congruent ordering in a selected compositional range, revealing an already strongly L12 ordered microstructure after natural aging with a chemically homogeneous Li distribution and a decomposition of the alloy upon annealing at elevated temperatures. The presented study of the δ' precipitation evaluates the reaction pathway of this process and compares it to the predictions of the Bragg-Williams-Gorsky model with respect to decomposition and ordering in this alloy system.

8.
Microsc Microanal ; 23(2): 396-403, 2017 04.
Artigo em Inglês | MEDLINE | ID: mdl-28318469

RESUMO

This study applies atom probe tomography (APT) to analyze the oxide scales formed on model NiAlCr alloys doped with Hf, Y, Ti, and B. Due to its ability to measure small amounts of alloying elements in the oxide matrix and its ability to quantify segregation, the technique offers a possibility for detailed studies of the dopant's fate during high-temperature oxidation. Three model NiAlCr alloys with different additions of Hf, Y, Ti, and B were prepared and oxidized in O2 at 1,100°C for 100 h. All specimens showed an outer region consisting of different spinel oxides with relatively small grains and the protective Al2O3-oxide layer below. APT analyses focused mainly on this protective oxide layer. In all the investigated samples segregation of both Hf and Y to the oxide grain boundaries was observed and quantified. Neither B nor Ti were observed in the alumina grains or at the analyzed interfaces. The processes of formation of oxide scales and segregation of the alloying elements are discussed. The experimental challenges of the oxide analyses by APT are also addressed.

9.
Microsc Microanal ; 18(5): 964-70, 2012 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-23095446

RESUMO

In this article the Cu-Au binding energy in Cu3Au is determined by comparing experimental atom probe tomography (APT) results to simulations. The resulting bonding energy is supported by density functional theory calculations. The APT simulations are based on the Müller-Schottky equation, which is modified to include different atomic neighborhoods and their characteristic bonds. The local environment is considered up to the fifth next nearest neighbors. To compare the experimental with simulated APT data, the AtomVicinity algorithm, which provides statistical information about the positions of the neighboring atoms, is applied. The quality of this information is influenced by the field evaporation behavior of the different species, which is connected to the bonding energies.

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