Time-resolved grazing-incidence pair distribution functions during deposition by radio-frequency magnetron sputtering

Roelsgaard, Martin; Dippel, Ann‐Christin; Borup, Kasper A.; Nielsen, Ida; Broge, Nils Lau Nyborg; Röh, Jan; Gutowski, Olof; Iversen, Bo B.

doi:10.1107/s2052252519001192

Cited by 25 publications

(26 citation statements)

References 35 publications

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“…This makes MCR-ALS especially suitable for the analysis of large datasets generated during in situ and/or operando experiments, e.g., IR, 54 Raman, 55 XAS, 56 XRD, 57 or PDF. 58,59 MCR-ALS provides the characteristic profiles of the individual components and the evolution of these components with time (time-concentration profiles). 59 Comprehensive overviews on MCR-ALS analysis can be found in the literature 39,60 and ESI † section.…”

Section: In Situ Pdf and Xrd Analysesmentioning

confidence: 99%

Effect of molten sodium nitrate on the decomposition pathways of hydrated magnesium hydroxycarbonate to magnesium oxide probed byin situtotal scattering

et al. 2020

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Section: In Situ Pdf and Xrd Analysesmentioning

confidence: 99%

Effect of molten sodium nitrate on the decomposition pathways of hydrated magnesium hydroxycarbonate to magnesium oxide probed byin situtotal scattering

et al. 2020

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“…In all cases, fused silica wafers (UniversityWafer, Inc., South Boston, USA) were used as substrates, providing a reproducible and, thus, easily scalable background signal due to its amorphous structure (Jensen et al, 2015). We sputter-deposited platinum ultrathin films in an RF magnetron sputtering chamber specially designed for in situ PDF measurements (Roelsgaard et al, 2019). In the example described below, the Pt was sputtered for 30 s at an RF power of 12 W in pure Ar plasma at a pressure of 5 Â 10 À2 mbar (1 mbar = 100 Pa) and around 30 C substrate temperature.…”

Section: Sample Preparationmentioning

confidence: 99%

“…Fig. 2(a) depicts the PDF and its structural fit of a sputter-deposited platinum layer on fused silica taken from an in situ sputtering data set (Roelsgaard et al, 2019). A sequential refinement was carried out starting from the thickest film of the data set and going backwards in the series towards thinner samples.…”

Section: Surface-enhanced Sensitivitymentioning

confidence: 99%

Local atomic structure of thin and ultrathin films via rapid high-energy X-ray total scattering at grazing incidence

Dippel

Roelsgaard

Boettger

et al. 2019

Int Union Crystallogr J

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Atomic pair distribution function (PDF) analysis is the most powerful technique to study the structure of condensed matter on the length scale from short- to long-range order. Today, the PDF approach is an integral part of research on amorphous, nanocrystalline and disordered materials from bulk to nanoparticle size. Thin films, however, demand specific experimental strategies for enhanced surface sensitivity and sophisticated data treatment to obtain high-quality PDF data. The approach described here is based on the surface high-energy X-ray diffraction technique applying photon energies above 60 keV at grazing incidence. In this way, reliable PDFs were extracted from films of thicknesses down to a few nanometres. Compared with recently published reports on thin-film PDF analysis from both transmission and grazing-incidence geometries, this work brought the minimum detectable film thickness down by about a factor of ten. Depending on the scattering power of the sample, the data acquisition on such ultrathin films can be completed within fractions of a second. Hence, the rapid-acquisition grazing-incidence PDF method is a major advancement in thin-film technology that opens unprecedented possibilities for in situ and operando PDF studies in complex sample environments. By uncovering how the structure of a layered material on a substrate evolves and transforms in terms of local and average ordering, this technique offers new opportunities for understanding processes such as nucleation, growth, morphology evolution, crystallization and the related kinetics on the atomic level and in real time.

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“…Although our experiments were focused on the crystallization of ferroelectric films from CSD probed by diffraction, the above examples clearly show that the in situ setup can be applied to a broader class of samples and processes. The same setup can be used for pair-distribution function (PDF) measurements for structural characterization of partially disordered powder films (Dippel et al, 2019;Roelsgaard et al, 2019), for characterization of the orientation distribution function (ODF) of textured films, for mapping of Bragg and diffuse scattering of epitaxial films, and for specular and offspecular reflectivity measurements. Thus, the results of the present report can be viewed in a wider perspective and have several possible application areas.…”

Section: Discussionmentioning

confidence: 99%

Experimental setup for high-temperature in situ studies of crystallization of thin films with atmosphere control

Blichfeld¹,

Bakken²,

Chernyshov³

et al. 2020

J Synchrotron Radiat

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Understanding the crystallization process for chemical solution deposition (CSD) processed thin films is key in designing the fabrication strategy for obtaining high-quality devices. Here, an in situ sample environment is presented for studying the crystallization of CSD processed thin films under typical processing parameters using near-grazing-incidence synchrotron X-ray diffraction. Typically, the pyrolysis is performed in a rapid thermal processing (RTP) unit, where high heating rates, high temperatures and atmosphere control are the main control parameters. The presented in situ setup can reach heating rates of 20°C s−1 and sample surface temperatures of 1000°C, comparable with commercial RTP units. Three examples for lead-free ferroelectric thin films are presented to show the potential of the new experimental set-up: high temperature, for crystallization of highly textured Sr0.4Ba0.6Nb2O6 on a SrTiO3 (001) substrate, high heating rate, revealing polycrystalline BaTiO3, and atmosphere control with 25% CO2, for crystallization of BaTiO3. The signal is sufficient to study a single deposited layer (≥10 nm for the crystallized film) which then defines the interface between the substrate and thin film for the following layers. A protocol for processing the data is developed to account for a thermal shift of the entire setup, including the sample, to allow extraction of maximum information from the refinement, e.g. texture. The simplicity of the sample environment allows for the future development of even more advanced measurements during thin-film processing under non-ambient conditions.

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Time-resolved grazing-incidence pair distribution functions during deposition by radio-frequency magnetron sputtering

Cited by 25 publications

References 35 publications

Effect of molten sodium nitrate on the decomposition pathways of hydrated magnesium hydroxycarbonate to magnesium oxide probed byin situtotal scattering

Effect of molten sodium nitrate on the decomposition pathways of hydrated magnesium hydroxycarbonate to magnesium oxide probed byin situtotal scattering

Local atomic structure of thin and ultrathin films via rapid high-energy X-ray total scattering at grazing incidence

Experimental setup for high-temperature in situ studies of crystallization of thin films with atmosphere control

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