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The oxidation behavior of iron polycrystals and single crystals with (110) surface orientation was studied at 450°C. Energy-dispersive diffraction with synchrotron radiation provided in situ information regarding the evolution of stress gradients and fiber texture in the oxide scales. Within this low-temperature regime, grain boundaries caused the oxidation kinetics of polycrystalline iron to be more rapid than iron single crystals only during the first minutes of oxidation. Epitaxial growth of iron oxides occurred only on single crystal substrates during the initial oxidation. In situ stress analyses suggested that stress relief occurred invariably in the magnetite layer due to the formation of a fine-grained seam near the iron substrates. Above the magnetite and in the hematite layer, the growth stresses depend initially on volumetric strains and later on inner oxide formation and creep of the hematite.

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We performed Synchrotron X‐ray diffraction (XRD) analyses of internal residual stresses in monolithic samples of a newly developed Li2O–Al2O3–SiO2 (LAS) glass–ceramic produced by sintering and in a commercial LAS glass–ceramic, CERAN®, produced by the traditional crystal nucleation and growth treatments. The elastic constants were measured by instrumented indentation and a pulse‐echo technique. The thermal expansion coefficient of virgilite was determined by high temperature XRD and dilatometry. The c‐axis contracts with the increasing temperature whereas the a‐axis does not vary significantly. Microcracking of the microstructure affects the thermal expansion coefficients measured by dilatometry and thermal expansion hysteresis is observed for the sintered glass–ceramic as well as for CERAN®. The measured internal stress is quite low for both glass–ceramics and can be explained by theoretical modeling if the high volume fraction of the crystalline phase (virgilite) is considered. Using a modified Green model, the calculated critical (glass) island diameter for spontaneous cracking agreed with experimental observations. The experimental data collected also allowed the calculation of the critical crystal grain diameters for grain‐boundary microcracking due to the anisotropy of thermal expansion of virgilite and for microcracking in the residual glass phase surrounding the virgilite particles. All these parameters are important for the successful microstructural design of sintered glass–ceramics.

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Due to their applicability for manufacturing dense, hard and stable coatings, Physical Vapor Deposition (PVD) techniques, such as High Power Impulse Magnetron Sputtering (HiPIMS), are currently used to deposit transition metal nitrides for tribological applications. Cr-Al-N is one of the most promising ceramic coating systems owing to its remarkable mechanical and tribological properties along with excellent corrosion resistance and high-temperature stability. This work explores the possibility of further improving Cr-Al-N coatings by modulation of its microstructure. Multilayer-like Cr1−xAlxN single films were manufactured using the angular oscillation of the substrate surface during HiPIMS. The sputtering process was accomplished using pulse frequencies ranging from 200 to 500 Hz and the resulting films were evaluated with respect to their hardness, Young’s modulus, residual stresses, deposition rate, crystallite size, crystallographic texture, coating morphology, chemical composition, and surface roughness. The multilayer-like structure, with periodicities ranging from 250 to 550 nm, were found associated with misorientation gradients and small-angle grain boundaries along the columnar grains, rather than mesoscopic chemical modulation of the microstructure. This minute modification of microstructure along with associated compressive residual stresses are concluded to explain the increased hardness ranging from 25 to 30 GPa, which is at least 20% over that expected for a film of the same chemical composition grown by a conventional PVD processing route.