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Jochen M. Schneider

Publications and source records attributed to Jochen M. Schneider.

At least 19 recordsLinked to original sources

Impact of O concentration on the thermal stability and decomposition mechanism of (Cr,Al)N compared to (Ti,Al)N thin films

The composition-dependent thermal stability of (Cr$_{0.47 \mp 0.03}$Al$_{0.53 \mp 0.03}$)$_{z}$(O$_{y}$N$_{1-y}$)$_{1-z}$ thin films with O concentrations of y = 0, 0.15, and 0.40 is investigated up to 1200 °C and then compared to (Ti$_{0.56}$Al$_{0.44}$)$_{z}$(O$_{y}$N$_{1-y}$)$_{1-z}$. X-ray diffraction reveals a thermal stability limit of 1150 °C independent of the O concentration, as witnessed by the formation of decomposition products, namely h-Cr$_{2}$N for (Cr$_{0.50}$Al$_{0.50}$)$_{0.49}$N$_{0.51}$ and c-Cr for both (Cr$_{0.48}$Al$_{0.52}$)$_{0.48}$(O$_{0.15}$N$_{0.85}$)$_{0.52}$ and (Cr$_{0.44}$Al$_{0.56}$)$_{0.46}$(O$_{0.40}$N$_{0.60}$)$_{0.54}$. Based on TEM and ERDA data, the thermal stability limit is extended to 1100 - 1150 °C. DFT calculations indicate that bond breaking limits the thermal stability. In (Cr,Al)N, N has the lowest activation energy for migration. Furthermore, the O vacancy formation energy is highest in (Cr,Al)(O,N). It has to be overcome to enable diffusion on the non-metal sublattice, which is necessary for forming decomposition products like w-AlN or c-Cr. However, once Cr-N bonds break, decomposition into h-Cr$_{2}$N and subsequent c-Cr together with N$_{2}$ is triggered. This results in N evaporation, generating sufficient non-metal vacancies that greatly enhance diffusion and render the extensive vacancy formation energies for non-metals irrelevant. This reduction of the activation energy for mass transport on the non-metal sublattice to the migration barrier causes the similar thermal stability in (Cr$_{0.47 \mp 0.03}$Al$_{0.53 \mp 0.03}$)$_{z}$(O$_{y}$N$_{1-y}$)$_{1-z}$. In contrast, Al bonds break first without creating non-metal vacancies in (Ti,Al)(O,N). Thus, the high O vacancy formation energy in (Ti,Al)(O,N) significantly increases the thermal stability compared to (Ti,Al)N as well as the here investigated films.

cond-mat.mtrl-sci

Morphology dependent decomposition and pore evolution during oxidation of Cr$_2$AlC coatings revealed by correlative tomography

Quantitative 3D characterization of materials degradation in oxidizing environments remains limited. Here, we apply a correlative tomography-based mass balance framework to Cr$_2$AlC, a coating candidate for accident tolerant nuclear fuel claddings and turbine blades, and show that decomposition and pore evolution during oxidation, quantified by integrating volumetric, structural and compositional data, are strongly governed by grain morphology. The oxidation of sputtered Cr$_2$AlC coatings with equiaxed and columnar grain morphologies was analyzed. While Cr$_7$C$_3$ formed in both coating morphologies, pores formed exclusively in columnar coatings. The expected Cr$_7$C$_3$ volume was estimated by mass-balance calculations assuming that Al-deintercalation enables oxide scale and Al-O-C-N precipitate formation, leading to complete transformation of the Al-deintercalated Cr$_2$AlC into Cr$_7$C$_3$. In equiaxed coatings, the predicted carbide volume agreed with tomography within 3 $\pm$ 3 %, confirming Al-deintercalation-driven Cr$_7$C$_3$ formation. Despite the smaller molar volume of Cr$_7$C$_3$ relative to Cr$_2$AlC, absence of pores imply that transformation shrinkage is likely accommodated by coating thickness reduction. In columnar coatings, the predicted Cr$_7$C$_3$ volume exceeds the measured value by 22 $\pm$ 4 %, and the pore volume expected from transformation shrinkage alone is 13-16 % lower than measured, indicating partial Al deintercalation and clustering of pre-existing defects. This combined methodology provides a general route to quantitatively resolve degradation mechanisms.

cond-mat.mtrl-sci

Self-supported bulk MXene electrodes for electrochemical hydrogen applications

MXenes are promising candidates for electrochemical applications due to their high conductivity, tunable surface chemistry, and catalytic potential. However, their use in bulk electrode form remains unexplored despite advantages such as higher current density and improved mechanical integrity. Herein, we present a methodology for the fabrication of self-supported vdW solid Ti3C2Tz MXene electrodes, produced by cold compaction followed by vacuum heat treatment at 600 °C, which effectively removes interlayer confined water and stabilizes the bulk 3D structure. The resulting binder-free electrodes exhibit enhanced mechanical robustness along with structural and chemical stability in various electrolytes. The MXene electrodes demonstrate adequate HER activity while maintaining electrochemical stability over time, with minimal oxidation or changes in termination surface chemistry. This approach is scalable and cost-effective, overcoming limitations of nanoscale MXene architectures in electrochemical environments and offering a practical pathway toward MXene-based materials for sustainable hydrogen energy technologies.

cond-mat.mtrl-sci

Vacancy-concentration-dependent thermal stability of fcc-(Ti,Al)Nx predicted via chemical-environment-sensitive diffusion activation energies

Thermal decomposition of metastable fcc-(Ti,Al)Nx limits the lifetime of coated components. While energetic decomposition aspects can be modelled reliably, the inherent variability of chemical environment-dependent diffusion activation energies remains systematically unexplored. Here, we predict an activation energy range (envelope) for mass transport in varying chemical environments, reflecting the vacancy concentration range fcc-(Ti0.5Al0.5)1-xNx with x = 0.47, 0.5, 0.53. The stoichiometric compound shows maximum thermal stability, consistent with experimental data. Metal vacancies decrease the average migration energy, while metal and nitrogen vacancies reduce barriers via lattice strain relaxation, enhancing mobility. The strong chemical environment dependence challenges conclusions from single-point activation energy data.

cond-mat.mtrl-sci

Effect of crystallographic texture on dealloying kinetics and composition of nanoporous gold surface

Nanoporous metals allow for tailoring composition and surface-to-volume ratio, both aspects critical for applications in catalysis. Here, Ag70Au30 (2 at. %) films with a face-centered cubic structure were deposited at 400°C, either {111}-textured or randomly oriented. Upon chemical dealloying, atom probe tomography of the nanoporous structure reveals that the textured film retains a up to 2.7 times higher Ag concentration within the ligaments compared to the randomly oriented film that exhibits ligament coarsening, indicating faster dealloying kinetics. Our study highlights the potential of microstructure engineering in tailoring the properties of nanoporous metals for possible future catalytic and electrochemical applications.

cond-mat.mtrl-sci

Prediction and identification of point defect fingerprints in X-ray photoelectron spectra of TiN$_x$ with 1.18 $\le x \le$ 1.37

We investigate the effect of selected N and Ti point defects in $B$1 TiN on N 1s and Ti\,2p$_{3/2}$ binding energies (BE) by experiments and ab initio calculations. X-ray photoelectron spectroscopy (XPS) measurements of TiN$_x$ films with 1.18 $\le x \le$ 1.37 reveal additional N 1s spectral components at lower binding energies. Ab initio calculations predict that these components are caused by either Ti vacancies, which induce a N 1s BE shift of -0.54 eV in its first N neighbors, and/or N tetrahedral interstitials, which have their N 1s BE shifted by -1.18 eV and shift the BE of their first N neighbors by -0.53 eV. However, based on {\it ab initio} data the tetrahedral N interstitial is estimated to be unstable at room temperature. We, therefore, unambiguously attribute the N 1s spectral components at lower BE in Ti-deficient TiN$_x$ thin films to the presence of Ti vacancies. Furthermore, it is demonstrated that the vacancy concentration in Al-capped Ti-deficient TiN$_x$ can be quantified with the here proposed correlative method based on measured and predicted BE data. Our work highlights the potential of ab initio-guided XPS measurements for detecting and quantifying point defects in $B$1 TiN$_x$.

cond-mat.mtrl-sci

The effect of elastic-plastic mismatch and interface proximity on the fracture toughness of Ti-TiN thin films

Magnetron sputtered titanium nitride (TiN) thin films are widely used as protective coatings due to their high hardness, but suffer from inherent brittleness and low fracture toughness, limiting their applicability. The multilayering of TiN films with metallic titanium (Ti) interlayers in the form of bi-layer and tri-layer systems have been studied using microcantilever fracture tests. Plastic dissipation in the Ti layer is shown to lead to an increase in crack growth resistance. The effect of the elastic-plastic mismatch between the two materials on the crack driving force, as well as the size of the fully developed plastic zone in Ti have been quantified in this work for the first time. It is shown that incorporating a Ti layer thickness of 250 nm can improve the fracture resistance by nearly ten times compared to the initiation fracture toughness in TiN, preventing catastrophic fracture of these multi-layered films. These results will aid in physics informed design of optimised thickness of metallic interlayers in multi-layered thin films.

cond-mat.mtrl-sci

Designing artificial zinc phosphate tribofilms with tailored mechanical properties by altering the chain length

Zinc dialkyldithiophosphate (ZDDP), as the most prominent lubrication additive, forms tribofilms consisting primarily of zinc phosphate glasses containing sulfides. As sulfur is linked to environmental concerns, sulfur-free zinc phosphate coatings have been sputtered from a Zn3(PO4)2 target and investigated here. Based on the bridging to non-bridging oxygen ratio, determined by X-ray photoelectron spectroscopy (XPS), the as deposited coatings are classified as metaphosphates. As the annealing temperature is increased, the chain lengths are reduced, as witnessed by XPS data indicated by a loss of phosphorus and oxygen of the coating surface, likely due to hydrolysis with water from the atmosphere. Transmission electron microscopy energy-dispersive X-ray spectroscopy line scans show that the XPS-revealed composition change of the coating surface upon annealing occurs over the whole thickness of the coating. This alteration in composition and chain length reductions causes a rise in hardness, reduced Young's modulus, and wear resistance. Therefore, the properties of the artificial zinc phosphate tribofilms can be tailored via a thermally stimulated composition change, causing an alternation in chain length from meta- to orthophosphate and thereby enabling the design of coatings with desired mechanical properties.

cond-mat.mtrl-sci

Microscale deformation of intermetallic-Mg interface under shear loading

While intermetallic (IM)-metal interfaces in metallic alloys are critical for tuning mechanical properties, they can also act as failure sites, underscoring the importance of determining their strength. This study reports on a novel microshear geometry, and demonstrates its applicability for testing the strength and deformation behavior of IM-metal interfaces in Mg-Al-Ca alloys, a key material for light weight automotive applications. The shear tests are applied to a model bi-layered system grown by magnetron sputtering, comprising of a CaMg2 film deposited onto a Mg layer. A parametric study was performed using finite element modeling to optimize the specimen dimensions. Subsequently, in situ microshear tests conducted inside a scanning electron microscope revealed an interface shear strength of ~136 MPa, and provided insights into the stages of deformation progression. Post mortem examination of the sheared interface revealed an irregular surface indicating ductile deformation at room temperature.

cond-mat.mtrl-sci

Dry Transfer Based on PMMA and Thermal Release Tape for Heterogeneous Integration of 2D-TMDC Layers

A reliable and scalable transfer of 2D-TMDCs (two-dimensional transition metal dichalcogenides) from the growth substrate to a target substrate with high reproducibility and yield is a crucial step for device integration. In this work, we have introduced a scalable dry-transfer approach for 2D-TMDCs grown by MOCVD (metal-organic chemical vapor deposition) on sapphire. Transfer to a silicon/silicon dioxide (Si/SiO$_2$) substrate is performed using PMMA (poly(methyl methacrylate)) and TRT (thermal release tape) as sacrificial layer and carrier, respectively. Our proposed method ensures a reproducible peel-off from the growth substrate and better preservation of the 2D-TMDC during PMMA removal in solvent, without compromising its adhesion to the target substrate. A comprehensive comparison between the dry method introduced in this work and a standard wet transfer based on potassium hydroxide (KOH) solution shows improvement in terms of cleanliness and structural integrity for dry-transferred layer, as evidenced by X-ray photoemission and Raman spectroscopy, respectively. Moreover, fabricated field-effect transistors (FETs) demonstrate improvements in subthreshold slope, maximum drain current and device-to-device variability. The dry-transfer method developed in this work enables large-area integration of 2D-TMDC layers into (opto)electronic components with high reproducibility, while better preserving the as-grown properties of the layers.

physics.app-ph

On the role of Grain Boundary Character in the Stress Corrosion Cracking of Nanoporous Gold Thin Films

For its potential as a catalyst, nanoporous gold (NPG) prepared through dealloying of bulk Ag-Au alloys has been extensively investigated. NPG thin films can offer ease of handling, better tunability of the chemistry and microstructure of the nanoporous structure, and represent a more sustainable usage of scarce resources. These films are however prone to intergranular cracking during dealloying, limiting their stability and potential applications. Here, we set out to systematically investigate the grain boundaries in Au28Ag72 thin films. We observe that a sample synthesized at 400 °C is at least 2.5 times less prone to cracking compared to a sample synthesized at room temperature. This correlates with a higher density of coincident site lattice grain boundaries, especially the density of coherent sigma 3, increased, which appear resistant against cracking. Nanoscale compositional analysis of random high-angle grain boundaries reveals prominent Ag enrichment up to 77 at.%, whereas sigma 3 coherent twin boundaries show Au enrichment of up to 30 at.%. The misorientation and the chemistry of grain boundaries hence affect their dealloying behavior, which in turn controls the cracking, and the possible longevity of NPG thin films for application in electrocatalysis.

cond-mat.mtrl-sci

Constructing phase diagrams for defects by correlated atomic-scale characterization

Phase transformations and crystallographic defects are two essential tools to drive innovations in materials. Bulk materials design via tuning chemical compositions has been systematized using phase diagrams. We show here that the same thermodynamic concept can be applied to understand the chemistry at defects. We present a combined experimental and modelling approach to scope and build phase diagrams for defects. The discovery was enabled by triggering phase transformations of individual defects through local alloying, and sequentially imaging the structural and chemical changes using atomic-resolution scanning transmission electron microscopy. By observing atomic-scale phase transformations of a Mg grain boundary through Ga alloying, we exemplified the method to construct a grain boundary phase diagram using ab initio simulations and thermodynamic principles. The methodology enables a systematic development of defect phase diagrams to propel a new paradigm for materials design utilizing chemical complexity and phase transformations at defects.

cond-mat.mtrl-sci

Chemical and structural characterization of the native oxide scale on a Mg-based alloy

In this study, the structure and composition of the native oxide forming on the basal plane (0001) of Mg-2Al-0.1Ca is investigated by a correlative approach, combining scanning transmission electron microscopy (STEM) and atom probe tomography (APT). Atom probe specimens were prepared conventionally in a Ga focused ion beam (FIB) as well as a Xe plasma FIB in a cryogenic setup and subsequently cleaned in the atom probe to remove surface contamination before oxidation. While thermal energy input from the laser and longer atmospheric exposure time increased the measured hydrogen content in the specimen's apex region, cryo preparation revealed, that the hydrogen uptake in magnesium is independent of the employment of conventional or cryogenic FIB preparation. TEM measurements demonstrated the growth of a (111) MgO oxide layer with 3-4 nm thickness on the basal (0001) plane of the Mg atom probe specimen. APT data further revealed the formation of an aluminum-rich region between bulk Mg and the native oxide. The aluminum enrichment of up to ~20 at.% at the interface is consistent with an inward growth of the oxide scale.

cond-mat.mtrl-sci

Bond formation at polycarbonate | X interfaces (X = Al$_2$O$_3$, TiO$_2$, TiAlO$_2$) studied by theory and experiments

Interfacial bond formation during sputter deposition of metal oxide thin films onto polycarbonate (PC) is investigated by ab initio molecular dynamics simulations and X-ray photoelectron spectroscopy (XPS) analysis of PC | X interfaces (X = Al$_2$O$_3$, TiO$_2$, TiAlO$_2$). Generally, the predicted bond formation is consistent with the experimental data. For all three interfaces, the majority of bonds identified by XPS are (C-O)-metal bonds, whereas C-metal bonds are the minority. Compared to the PC | Al$_2$O$_3$ interface, the PC | TiO$_2$ and PC | TiAlO$_2$ interfaces exhibit a reduction in the measured interfacial bond density by ~ 75 and ~ 65%, respectively. Multiplying the predicted bond strength with the corresponding experimentally determined interfacial bond density shows that Al$_2$O$_3$ exhibits the strongest interface with PC, while TiO$_2$ and TiAlO$_2$ exhibit ~ 70 and ~ 60% weaker interfaces, respectively. This can be understood by considering the complex interplay between the metal oxide composition, the bond strength as well as the population of bonds that are formed across the interface.

cond-mat.mtrl-sci

Large-area deposition of protective (Ti,Al)N coatings onto polycarbonate

Polycarbonate (PC) and protective (Ti,Al)N coatings exhibit extremely different material properties, specifically crystal structure, thermal stability, elastic and plastic behavior as well as thermal expansion coefficients. These differences present formidable challenges for the deposition process development as low-temperature synthesis routes have to be explored to avoid a thermal overload of the polymer substrate. Here, a large-area sputtering process is developed to address the challenges by systematically adjusting target peak power density and duty cycle. Adhering (Ti,Al)N coatings with a critical residual tensile stress of 2.2 +/- 0.2 GPa are obtained in the pulsed direct current magnetron sputtering range, whereas depositions at higher target peak power densities, realized by high power pulsed magnetron sputtering, lead to stress-induced adhesive and/or cohesive failure. The stress-optimized (Ti,Al)N coatings deposited onto PC with a target peak power density of 0.036 kW cm-2 and a duty cycle of 5.3% were investigated by cross-cut test confirming adhesion. By investigating the bond formation at the PC | (Ti,Al)N interface, mostly interfacial CNx bonds and a small fraction of (C-O)-(Ti,Al) bonds are identified by X-ray photoelectron spectroscopy, indicating reactions at the hydrocarbon and the carbonate groups during deposition. Nanoindentation reveals an elastic modulus of 296 +/- 18 GPa for the (Ti,Al)N coating, while a Ti-Al-O layer is formed during electrochemical impedance spectroscopy in a borate buffer solution, indicating protective passivation. This work demonstrates that the challenge posed by the extremely different material properties at the interface of soft polymer substrates and hard coatings can be addressed by systematical variation of the pulsing parameters to reduce the residual film stress.

physics.app-ph

Valence electron concentration- and N vacancy-induced elasticity in cubic early transition metal nitrides

Motivated by frequently reported deviations from stoichiometry in cubic transition metal nitride (TMNx) thin films, the effect of N-vacancy concentration on the elastic properties of cubic TiNx, ZrNx, VNx, NbNx, and MoNx (0.72<x<1.00) is systematically studied by density functional theory (DFT) calculations. The predictions are validated experimentally for VNx (0.77<x<0.97). The DFT results indicate that the elastic behavior of the TMNx depends on both the N-vacancy concentration and the valence electron concentration (VEC) of the transition metal: While TiNx and ZrNx exhibit vacancy-induced reductions in elastic modulus, VNx and NbNx show an increase. These trends can be rationalized by considering vacancy-induced changes in elastic anisotropy and bonding. While introduction of N-vacancies in TiNx results in a significant reduction of elastic modulus along all directions and a lower average bond strength of Ti-N, the vacancy-induced reduction in [001] direction of VNx is overcompensated by the higher stiffness along [011] and [111] directions, resulting in a higher average bond strength of V-N. To validate the predicted vacancy-induced changes in elasticity experimentally, close-to-single-crystal VNx (0.77<x<0.97) are grown on MgO(001) substrates. As the N-content is reduced, the relaxed lattice parameter a0, as probed by X-ray diffraction, decreases from 4.128 A to 4.096 A. This reduction in lattice parameter is accompanied by an anomalous 11% increase in elastic modulus, as determined by nanoindentation. As the experimental data agree with the predictions, the elasticity enhancement in VNx upon N-vacancy formation can be understood based on the concomitant changes in elastic anisotropy and bonding.

cond-mat.mtrl-sci

Correlative Theoretical and Experimental Study of the Polycarbonate | X Interfacial Bond Formation (X = AlN, TiN, TiAlN) during Magnetron Sputtering

To understand the interfacial bond formation between polycarbonate (PC) and magnetron-sputtered metal nitride thin films, PC | X interfaces (X = AlN, TiN, TiAlN) are comparatively investigated by ab initio simulations as well as X-ray photoelectron spectroscopy. The simulations predict significant differences at the interface, as N and Ti form bonds with all functional groups of the polymer, while Al reacts selectively only with the carbonate group of pristine PC. In good agreement with simulations, experimental data reveal that the PC | AlN and the PC | TiAlN interfaces are mainly defined by interfacial C-N bonds, whereas for PC | TiN, the interface formation is also characterized by numerous C-Ti and (C-O)-Ti bonds. Bond strength calculations combined with the measured interfacial bond density indicate the strongest interface for PC | TiAlN followed by PC | AlN, whereas the weakest is predicted for PC | TiN due to its lower density of strong interfacial C-N bonds. This study shows that the employed computational strategy enables prediction of the interfacial bond formation between PC and metal nitrides and that it is reasonable to assume that the research strategy proposed herein can be readily adapted to other organic | inorganic interfaces.

cond-mat.mtrl-sci

On the determination of the thermal shock parameter of MAX phases: A combined experimental-computational study

Thermal shock resistance is one of the performance-defining properties for applications where extreme temperature gradients are required. The thermal shock resistance of a material can be described by means of the thermal shock parameter RT. Here, the thermo-mechanical properties required for the calculation of RT are quantum-mechanically predicted, experimentally determined, and compared for Ti3AlC2 and Cr2AlC MAX phases. The coatings are synthesized utilizing direct current magnetron sputtering without additional heating, followed by vacuum annealing. It is shown that the RT of both Ti3AlC2 and Cr2AlC obtained via simulations are in good agreement with the experimentally obtained ones. Comparing the MAX phase coatings, both experiments and simulations indicate superior thermal shock behavior of Ti3AlC2 compared to Cr2AlC, attributed primarily to the larger linear coefficient of thermal expansion of Cr2AlC. The results presented herein underline the potential of ab initio calculations for predicting the thermal shock behavior of ionically-covalently bonded materials.

cond-mat.mtrl-sci