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@PHDTHESIS{BANG:641899,
author = {BANG, JOOHEE},
othercontributors = {Thomas, Weber and Fiebig, Manfred},
title = {{N}on-invasive three-dimensional probing of atomic order in
single-crystalline thin films},
school = {ETH Zurich},
type = {Dissertation},
address = {Zurich},
publisher = {ETH Zurich},
reportid = {PUBDB-2025-05245},
pages = {108},
year = {2025},
note = {Dissertation, ETH Zurich, 2025},
abstract = {The emergence of powerful synchrotron sources, fast pixel
detectors, and the increasingavailability of
high-performance computing has facilitated the acquisition
and analysisof high-quality, large-volume diffuse
scattering data, providing insights into the realstructures
of disordered crystals that were not previously possible.
However, its ap-plication to studying local structural order
in thin films remains largely unexplored.This limitation
arises from the strong substrate contributions, which
obscures the weakdiffuse scattering signals from the film,
as well as the restricted reciprocal space cov-erage and
resolution inherent in grazing incidence X-ray diffraction.
This doctoralwork pioneers the extension of single-crystal
diffuse X-ray scattering techniques tothin films, enabling
atomic-scale characterization of complex domain structures
andtheir correlations within and across layers.We introduce
and validate a novel methodology for the structural
characteriza-tion of single-crystalline thin films,
overcoming challenges associated with non-invasiveprobing of
nanoscale domain configurations. A key accomplishment is the
implemen-tation of high-energy ultra-small grazing-incidence
X-ray diffraction, which effectivelymitigates substrate
contributions while achieving large reciprocal space
coverage andhigh sensitivity to small atomic displacements.
The large-volume and high-resolutiondiffuse scattering data
is analyzed using three-dimensional difference pair
distributionfunction (3D-ΔPDF), which provides invaluable
insights into the local atomic structureof
single-crystalline thin films.The methodology is first
applied to disordered oxide perovskite thin films, wherewe
establish a framework for interpreting 3D-ΔPDF features
associated with oxygenoctahedral tilts and cation
displacements. The approach is successfully validated onthe
known structure of SrRuO3 on SrTiO3, revealing a+a−c−
tilts and picometer-scalecation shifts with superior spatial
resolution compared to other characterization meth-ods.
Furthermore, correlation lengths and rotational amplitudes
of the oxygen octahe-dral tilts are analyzed as a function
of layer thickness and temperature, demonstratingthe
potential of the methodology in quantitative analysis.
Central to the analysis isthe divide-and-conquer approach
that allows for the selective examination of
diffusescattering features and ΔPDF signals with distinct
structural properties, showcasingthe versatility of the
methodology.ivBuilding on this validated framework, we
extend our approach to studying com-plex polarization domain
correlations in ferroelectric PbTiO3 and dielectric
SrTiO3(PTO|STO) superlattices. Our findings reveal the
presence of domain correlationswithin and across PTO layers,
extending into adjacent STO layers. We also investi-gated
temperature-dependent phase transitions of the domain
correlations and iden-tified two low-temperature phases with
strong anisotropic diffuse scattering and
onehigh-temperature pattern with ring-like appearance. In
general, thermal stability ofthe low-temperature
configurations increases in superlattices with higher
bilayer thick-ness, and the isotropic configuration emerges
at temperatures significantly above roomtemperature. On the
other hand, the only examined superlattice structure,
wherethe PTO layers are thicker than the STO layers,
exhibits ring-like scattering even atroom-temperature,
suggesting that thicker PTO layers experience reduced
anisotropicstrain from the STO layers.Finally, complementary
3D-ΔPDF analysis reveals the presence of Néel-type do-main
walls in the investigated superlattices. A major
breakthrough of this work isthe non-invasive probing of
buried layers within the superlattices, which unveils
aquadratic-shaped flux-closure polarization configuration
induced by tetragonal straineffects — an observation
rarely achieved with conventional characterization
methods.This demonstrates the method’s capability to
identify local structural chirality, a keyfeature in many
complex materials hosting nontrivial topologies.},
keywords = {info:eu-repo/classification/ddc/530 (Other) /
info:eu-repo/classification/ddc/500 (Other) / Physics
(Other) / Natural sciences (Other)},
cin = {FS DOOR-User},
cid = {$I:(DE-H253)FS_DOOR-User-20241023$},
pnm = {6G3 - PETRA III (DESY) (POF4-6G3)},
pid = {G:(DE-HGF)POF4-6G3},
experiment = {EXP:(DE-H253)P-P07-20150101},
typ = {PUB:(DE-HGF)11},
doi = {10.3929/ETHZ-B-000738059},
url = {https://bib-pubdb1.desy.de/record/641899},
}