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@PHDTHESIS{Creutzburg:441043,
author = {Creutzburg, Marcus},
othercontributors = {Stierle, Andreas},
title = {{A}dsorption of {C}arboxylic {A}cids on {M}agnetite
{S}ingle {C}rystal {S}urfaces},
school = {Universität Hamburg},
type = {Dissertation},
address = {Hamburg},
publisher = {Verlag Deutsches Elektronen-Synchrotron},
reportid = {PUBDB-2020-02286, DESY-THESIS-2020-011},
series = {DESY-THESIS},
pages = {160},
year = {2020},
note = {Dissertation, Universität Hamburg, 2020},
abstract = {Magnetite is a versatile transition metal oxide with
applications in catalysis, biomedical imaging and spintronic
devices. Moreover, magnetite nanoparticles covered with
oleic acid are formed into novel nanocomposite, hierarchical
materials with outstanding mechanical properties in terms of
strength and hardness. Despite their strong influence on the
stability and properties of the nanocomposites, little is
known about interactions that take place at the
oxide/organic interface. In order to further tailor and
improve these materials, it is necessary to study the
controlled adsorption of carboxylic acids on well-defined
flat magnetite single crystal surfaces.Following the surface
science approach the clean magnetite (111) surface was
investigated in this thesis using low energy electron
diffraction (LEED), scanning tunneling microscopy (STM) and
surface X-ray diffraction (SXRD). The surface was found to
be Fe-tet1 terminated after several cycles of argon ion
sputtering and annealing in an oxygen atmosphere followed by
annealing in ultra-high vacuum (UHV). The surface was
homogeneously terminated by a Fe-tet1 layer however, the
surface defect concentration, i.e. missing tet1 ironions,
was around $35\%.The$ clean magnetite (111) surface was
subsequently exposed to formic acid. As the simplest
carboxylic acid, formic acid has been used as a probe
molecule for longer carbonchain carboxylic acids in the
past. The molecule was found to dissociate upon adsorption
at room temperature. Fourier transform infrared
reflection-absorption spectroscopy (FT-IRRAS)revealed two
adsorption sites for the formate molecule. For low
coverages, the formate molecule was adsorbed at the surface
in a chelating bidentate geometry with both formate oxygen
atoms bound to a single substrate tetrahedral iron ion and
the remaining atomic hydrogen was bound to the oxygen
terminated iron defect sites. With increasing coverage,
formic acid was adsorbed in a quasi-bidentate configuration
with one formate oxygen bound to a tetrahedral iron ion and
the other bound to an OH group on the surface. The surface
was covered by a (sqrt(3) x sqrt(3)) R30° superstructure at
saturation coverage, which was visible with LEED and STM.
Both adsorption geometries contributed to the formation of
the superstructure.The adsorption of oleic acid on the
magnetite (001) surface at room temperature was observed to
lift $90\%$ of the (sqrt(2) x sqrt(2)) R45° reconstruction
of the clean surface as proven by LEED and SXRD. The lifting
mechanism is expected to follow the same path as for the
adsorption of atomic hydrogen, water vapor and formic acid
on magnetite (001). The adsorption of hydrogen destabilizes
the tetrahedral interstitial iron, which subsequently
diffuses into one of the two octahedral vacancies. The
second vacancy is filled by iron diffusion from deeper
layers. FT-IRRAS results revealed that oleic acid molecules
adsorbed in a bidentate bridging geometry and the long
carbon chain was oriented perpendicular to the surface. With
increasing oleic acid coverage, non-dissociated molecules
started to adsorb parallel to the surface.The adsorption of
oleic acid on the magnetite (111) surface was different from
the (001) surface. Both dissociated and non-dissociated
molecules were adsorbed in an upright geometryresulting in a
higher layer thickness and higher electron density than on
the (001) surface as determined by X-ray reflectivity (XRR).
When annealing the oleic acid layer at 350 °C, the
thickness and electron density of the layer decrease on both
magnetite (111) and on (001) as a result of molecule
desorption and possible tilt. In addition an atomic
roughening of the magnetite substrate occurs.The different
adsorption behavior of formic and oleic acid on the (001)
and (111) magnetite single crystal surfaces and the
subsequent structural changes in the near-surface region of
magnetite are important aspects for oleic acid stabilized
magnetite nanoparticles. The structural properties of such
nanocomposite materials can be tailored by changing the
ratio of (111)-type and (001)-type facets hence changing the
oleic acid molecule density.},
cin = {FS-NL},
cid = {I:(DE-H253)FS-NL-20120731},
pnm = {6214 - Nanoscience and Materials for Information Technology
(POF3-621) / SFB 986 A07 - Adsorption organischer Säuren
auf Oxidoberflächen und Nanostrukturen (A07) (318017425) /
DFG project 192346071 - SFB 986: Maßgeschneiderte
Multiskalige Materialsysteme - M3 (192346071) / PHGS,
VH-GS-500 - PIER Helmholtz Graduate School
$(2015_IFV-VH-GS-500)$},
pid = {G:(DE-HGF)POF3-6214 / G:(GEPRIS)318017425 /
G:(GEPRIS)192346071 / $G:(DE-HGF)2015_IFV-VH-GS-500$},
experiment = {EXP:(DE-H253)Nanolab-02-20150101 /
EXP:(DE-H253)Nanolab-01-20150101 /
EXP:(DE-H253)Nanolab-03-20150101},
typ = {PUB:(DE-HGF)3 / PUB:(DE-HGF)11},
doi = {10.3204/PUBDB-2020-02286},
url = {https://bib-pubdb1.desy.de/record/441043},
}