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@PHDTHESIS{Schupsky:885822,
author = {Schupsky, Jan Peter},
title = {{C}rystallisation of {O}xidic {G}asifier {S}lags},
volume = {514},
school = {RWTH Aachen},
type = {Dissertation},
address = {Jülich},
publisher = {Forschungszentrum Jülich GmbH Zentralbibliothek, Verlag},
reportid = {FZJ-2020-04113},
isbn = {978-3-95806-506-2},
series = {Schriften des Forschungszentrums Jülich. Reihe Energie
$\&$ Umwelt / Energy $\&$ Environment},
pages = {III, 127, XXII S.},
year = {2020},
note = {RWTH Aachen, Diss., 2020},
abstract = {Gasification is a flexible technology that has the
potential to support the transition from a fossil fuelled to
decarbonised energy supply system. During gasification, an
oxidic residue is produced thatis named as slag. Slag flow
needs to be constant in a gasifier, but a high viscosity
impairs the flow behaviour. The phenomenon of
crystallisation has such effect, yet is only barely
understood. Viscosity of slag can be modelled and therefore
predicted. However, no sufficient model exists to calculate
the viscosity of partly crystallised slags. A sufficient
data source of crystal morphology data is required to enable
the application of an improved viscosity model for partly
crystallised slags. In this study, the crystallisation
characteristics of four synthetic gasifier slags (ST-D-2,
HKT, SOM-1,and HKR) have been investigated. Initially, the
synthetic slag systems have been blended from high purity
compounds. Their compositions are mostly based on real coal
slags that have been investigated in previous studies. The
slag systems were analysed on their melting and
solidification behaviour and so, the temperature parameters
for the following experiments were set. Equilibrium
calculations were conducted with FactSage Equilib programme
to predict solidus and liquidus temperatures, as well as the
crystallised phases. As a first experiment, high temperature
viscosimetry was performed on the four slag systems. ST-D-2
and HKT slags were identified as high viscous, HKR as a low
viscous and SOM-1 as an intermediately viscous slag.
Viscosity measurements revealed non-Newtonian behaviour and
the presence of crystals in the slag. The evolution of
crystallisation was analysed by quenching and CLSM (confocal
laser scanning microscopy) experiments. The resulting slag
samples were analysed via microscopy, X-ray diffraction and
SEM (scanning electron microscopy). ST-D-2, HKT, and SOM-1
slag displayed significant growth of anorthite
(CaAl$_{2}$Si$_{2}$O$_{8}$)crystals. Several more phases
crystallised in these slags, such as cristobalite
(SiO$_{2}$), clinopyroxene((Ca,Mg,Fe)(Si,Al)$_{2}$O$_{6}$),
and olivine ((Ca,Mg,Fe)$_{2}$SiO$_{4}$). In the HKR slag,
melilite (Ca$_{2}$(Al,Mg)(Si,Al)$_{2}$O$_{7}$)was the
dominating crystal phase, followed by olivine and spinel
((Mg,Fe)AlO$_{4}$). For the high viscous slags,
time-temperature-transformation (TTT) diagrams indicated an
incubation time of single hours. SOM-1 slags incubation time
varied between double digit minutes to single hours and
lastly HKR slag displayed very rapid, partly instant
crystallisation. The crystal morphologies of anorthite,
spinel, olivine, and melilite could be defined based on the
sample analysis of quenching and CLSM experiments. Anorthite
was defined as a tetragonal prism with variation in the
elongation, spinel formed idiomorphic octahedrons, olivine
crystallised aselongated, equiaxed bipyramids and melilite
formed large rectangular bipyramids. To gather relevant
morphology data, the crystals were measured on their length
and width to quantify their presence with respect to the
applied temperature. In total, 1022 individual crystals were
measured for the quantification. Generally, the crystals
tend to grow larger at higher temperatures, which is in
agreement with the crystallisation theory. The morphology
was compared with crystallisation of real slag samples from
PiTER reactor (TU Munich, HotVeGas project). Anorthite and
spinel were found in PiTER slag with identical morphologies,
as provided for the synthetic slag samples. This accordance
is an application-related proof that the investigations on
crystal morphologies performed in this study are
reproducible and realistically display crystallisation
processes in gasifiers. Therfore, they are highly applicable
in viscosity models for partly cristallised slags.},
cin = {IEK-2},
cid = {I:(DE-Juel1)IEK-2-20101013},
pnm = {899 - ohne Topic (POF3-899)},
pid = {G:(DE-HGF)POF3-899},
typ = {PUB:(DE-HGF)3 / PUB:(DE-HGF)11},
urn = {urn:nbn:de:0001-2020120102},
url = {https://juser.fz-juelich.de/record/885822},
}