30 nm X-ray focusing correlates oscillatory stress, texture and structural defect gradients across multilayered TiN-SiOx thin film

Kečkéš, Jozef; Daniel, Rostislav; Todt, Juraj; Zálešák, Jakub; Sartory, Bernhard; Braun, Stefan; Gluch, Jürgen; Rosenthal, Martin; Burghammer, Manfred; Mitterer, Christian; Niese, Sven; Kubec, Adam

doi:10.1016/j.actamat.2017.11.049

Cited by 59 publications

(25 citation statements)

References 33 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Generally, the full width at half maximum (FWHM) of X-ray diffraction peaks correlates with the size of coherently diffracting domains as well as with the density of structural defects such as dislocations and lattice distortions, represented by strains of 2 nd and 3 rd order. Since the AlCrN crystallites of all thin films exhibited columnar grain morphology, which overall did not change during the thermal treatment, it can be assumed that the FWHM changes over the temperature cycle are sensitive primarily to the variation of structural defect density in the nanocrystals 25,27–29 . In order to evaluate FWHM, c-Cr(Al)N 111 and w-Al(Cr)N 100 diffraction peaks were fitted using the Pseudo-Voigt function for the diffraction vector out-of-plane orientation.…”

Section: Resultsmentioning

confidence: 99%

Stress-controlled decomposition routes in cubic AlCrN films assessed by in-situ high-temperature high-energy grazing incidence transmission X-ray diffraction

Meindlhumer

Klima

Jäger

et al. 2019

Sci Rep

Self Cite

View full text Add to dashboard Cite

The dependence of decomposition routes on intrinsic microstructure and stress in nanocrystalline transition metal nitrides is not yet fully understood. In this contribution, three Al0.7Cr0.3N thin films with residual stress magnitudes of −3510, −4660 and −5930 MPa in the as-deposited state were in-situ characterized in the range of 25–1100 °C using in-situ synchrotron high-temperature high-energy grazing-incidence-transmission X-ray diffraction and temperature evolutions of phases, coefficients of thermal expansion, structural defects, texture as well as residual, thermal and intrinsic stresses were evaluated. The multi-parameter experimental data indicate a complex intrinsic stress and phase changes governed by a microstructure recovery and phase transformations taking place above the deposition temperature. Though the decomposition temperatures of metastable cubic Al0.7Cr0.3N phase in the range of 698–914 °C are inversely proportional to the magnitudes of deposition temperatures, the decomposition process itself starts at the same stress level of ~−4300 MPa in all three films. This phenomenon indicates that the particular compressive stress level functions as an energy threshold at which the diffusion driven formation of hexagonal Al(Cr)N phase is initiated, provided sufficient temperature is applied. In summary, the unique synchrotron experimental setup indicated that residual stresses play a decisive role in the decomposition routes of nanocrystalline transition metal nitrides.

show abstract

Section: Resultsmentioning

confidence: 99%

Stress-controlled decomposition routes in cubic AlCrN films assessed by in-situ high-temperature high-energy grazing incidence transmission X-ray diffraction

Meindlhumer

Klima

Jäger

et al. 2019

Sci Rep

Self Cite

View full text Add to dashboard Cite

show abstract

“…While a range of techniques has been developed and validated in the past decades for macroscopic analyses [13][14][15][16][17][18][19][20][21], the determination of RS at the nano-and micro-scale still has limitations [22]. As far as crystalline materials are concerned, recent studies have shown remarkable resolution of less than 25 nm achievable for the characterisation of thin films using nano focused Synchrotron based X-ray Powder Diffraction (SXPD) techniques [23,24]. As well as SXPD, another class of non-destructive techniques employed for RS evaluation at this scale is based on the analysis of Raman scattering [25,26].…”

Section: Introductionmentioning

confidence: 99%

Generalised residual stress depth profiling at the nanoscale using focused ion beam milling

Salvati

Romano-Brandt

Mughal

et al. 2019

Journal of the Mechanics and Physics of Solids

View full text Add to dashboard Cite

The study of Residual Stress is gaining more and more attention due to its importance in design for structural integrity. At present a lot of emphasis is placed on understanding the origins of mechanical failure that lie at the nano-/micron-scale. This leads to the evident need for evaluating residual stress distributions at increasingly smaller scales, and the search for modern tools capable of accomplishing this task. Prior state-of-the-art methodologies mostly required expensive and time-consuming sample preparation and examination processes to evaluate residual stress, e.g. the study of thin TEM lamellae. The recent advent of Focused Ion Beam methods opened up methods suitable for direct application at sample surface, yet allowing the observation and quantification of stress relief phenomena at the nano-scale. In the last decade, technical aspects of FIB-based method(s) have seen significant development. On the other hand, the calculation framework employed to analyse the experimental outcome remained largely conventional, in most inconvenient for high precision analysis of challenging problems. In the present paper, the eigenstrain-based method previously presented by the authors for the depthresolved evaluation of equi-biaxial residual stress, is generalised to non-equi-biaxial distributions of residual stress. This extends the applicability of the method to a much wider class of problems. The use of cylindrical ring-core shape in FIB-DIC analysis allows reconstructing the full in-plane residual stress tensor as a function of milling depth. We report formulae for calibrated influence functions that have very broad applicability, and can be used in the overwhelming majority of cases. Their derivation is based on an extensive set of FEM simulations that allowed reliable identification of the limitations of this approach, and highlight the importance of making appropriate selection of ring-core diameter(s). Finally, experimental validation of the method is presented that involves the reconstruction a known non-equibiaxial residual stress depth profile, confirming the validity and reliability of the present approach.

show abstract

“…These results are associated with the corrugated nature of the nanostructures formed by substrate oscillation since no texture or chemical composition changes are evident. In previous works from this research group and from others the zig-zag architecture of the grains formed by oblique deposition are associated with periodic variations in residual stresses and misorientation gradients (KECKES et al, 2018;. These features act as barriers for plastic deformation, which increase hardness.…”

Section: Mechanical and Wear Performancementioning

confidence: 75%

“…New advances in characterization techniques have allowed understanding of ingrains mechanisms present in sculptured films. For instance, nano diffraction measurements using focused synchrotron radiation indicated that the production of coatings with tilted grains by GLAD is associated with variations in residual stresses, texture and defects (KECKES et al, 2018). Figure 16 exemplifies the deposition of a TiN-SiOx film in GLAD co-sputtering geometry with multilayers formed by variations in the α angle (-50° and 50°) and its impact on residual stresses.…”

Section: Engineering Of Nanostructured Coatingsmentioning

confidence: 99%

“…Recently, studies indicated zig-zag grains produced by GLAD present changes in microstructure such as texture and residual stresses that can also impact its mechanical properties (KECKES et al, 2018;DANIEL et al, 2020). A variation of GLAD in which the substrate is rocked in front of the target during deposition, continuously changing the angle of arrival of the sputtered material has been proposed…”

Section: Mechanical Propertiesmentioning

confidence: 99%

See 1 more Smart Citation

Manufacture and optimization of nanostructured Cr-Al-N coatings produced by reactive magnetron sputtering

Ávila¹,

Pinto²

View full text Add to dashboard Cite

show abstract

30 nm X-ray focusing correlates oscillatory stress, texture and structural defect gradients across multilayered TiN-SiOx thin film

Cited by 59 publications

References 33 publications

Stress-controlled decomposition routes in cubic AlCrN films assessed by in-situ high-temperature high-energy grazing incidence transmission X-ray diffraction

Stress-controlled decomposition routes in cubic AlCrN films assessed by in-situ high-temperature high-energy grazing incidence transmission X-ray diffraction

Generalised residual stress depth profiling at the nanoscale using focused ion beam milling

Manufacture and optimization of nanostructured Cr-Al-N coatings produced by reactive magnetron sputtering

Contact Info

Product

Resources

About