| Records |
| Author |
Prabhakara, V. |
Title  |
Strain measurement for semiconductor applications with Raman spectroscopy and Transmission electron microscopy |
Type |
Doctoral thesis |
| Year |
2021 |
Publication |
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Abbreviated Journal |
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Issue |
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Pages |
149 p. |
| Keywords |
Doctoral thesis; Engineering sciences. Technology; Electron microscopy for materials research (EMAT) |
| Abstract |
Scaling down the size of transistors has been a trend for several decades which has led to improved transistor performance, increased transistor density and hence the overall computation power of IC chips. The trend slowed in recent years due to reliability and power consumption issues at the nanoscale. Hence strain is introduced into transistor channels that has beneficial effects on improving the mobility of charge carriers, providing an alternative pathway for enhancing transistor performance. Therefore, monitoring strain is vital for the semiconductor industry. With the recent trend of decreasing device dimensions (FinFETS ~ 10-20nm) and strain modulation being used throughout, industry needs a reliable and fast method as quality control or defect characterisation. Such a universal strain measurement method does not exist, and one relies on a combination of quantitative in-line methods and complex off-line approaches. In this thesis, I investigated TEM and Raman spectroscopy-based methodologies for strain measurement. In terms of TEM methodologies, advancements are made for the STEM moiré imaging, targeting strain spatial resolution enhancement. I introduce advanced quadrature demodulation and phase stepping interferometry applied to STEM moiré that greatly enhances the spatial resolution while providing enhanced field of view and sensitivity for strain measurement. We introduce ways to reduce scan distortions in strain maps using an alternative scan strategy called “Block scanning” and the non-linear regression applied for strain extraction. Prospects for 3D strain analysis using high-resolution tomography is also investigated which gives direct access for the full second order strain tensors calculation. Finally, we compare strain measurements from TEM techniques with inline techniques like Raman spectroscopy. Raman stress measurement involves sensitive identification of the TO and LO phonon peaks. Raman spectrum of strained Ge transistor channel consists of strongly overlapping peaks within the spectral resolution of the spectrometer. Hence, the process of deconvolution of the two peaks is rather challenging. Hence, we explore new polarisation geometries like radially polarised incoming light which was shown to ease the deconvolution problem resulting in improved precision for Raman stress–strain measurements. |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ admin @ c:irua:182261 |
Serial |
6847 |
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| Author |
Van Grieken, R. |
| Title |
Stof : begrippen, bronnen en analysmethoden |
Type |
P3 Proceeding |
| Year |
1985 |
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P3 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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no |
| Call Number |
UA @ admin @ c:irua:117501 |
Serial |
8582 |
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| Author |
Egoavil, R. |
| Title |
STEM investigation of complex oxides at the atomic scale |
Type |
Doctoral thesis |
| Year |
2014 |
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Abbreviated Journal |
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Pages |
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Doctoral thesis; Electron microscopy for materials research (EMAT) |
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Place of Publication |
Antwerpen |
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0000-00-00 |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ lucian @ c:irua:123302 |
Serial |
3160 |
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| Author |
Van Aert, S. |
| Title |
Statistical parameter estimation theory : a tool for quantitative electron microscopy |
Type |
H1 Book chapter |
| Year |
2012 |
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Issue |
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Pages |
281-309 |
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H1 Book chapter; Electron microscopy for materials research (EMAT) |
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Wiley-VCH |
Place of Publication |
Weinheim |
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0000-00-00 |
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ISBN |
978-3-527-31706-6 |
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UA library record |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ lucian @ c:irua:96693 |
Serial |
3159 |
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| Author |
Van Aert, S.; den Dekker, A.J.; van den Bos, A.; van Dyck, D. |
| Title |
Statistical experimental design for quantitative atomic resolution transmission electron microscopy |
Type |
H1 Book chapter |
| Year |
2004 |
Publication |
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Abbreviated Journal |
Adv Imag Elect Phys |
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Issue |
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Pages |
1-164 |
| Keywords |
H1 Book chapter; Electron microscopy for materials research (EMAT); Vision lab |
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Academic Press |
Place of Publication |
San Diego, Calif. |
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Wos |
000223226700001 |
Publication Date |
2011-01-05 |
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Series Issue |
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Edition |
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| ISSN |
1076-5670; |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Times cited |
13 |
Open Access |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ lucian @ c:irua:47513 |
Serial |
3156 |
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| Author |
Playford, K.; Colin, J.L.; Pacyna, J.M.; Pirrone, N.; Schulz, M.; Van Grieken, R.; Wrembel, Z. |
| Title |
State-of-the-art and research needs for trace metals |
Type |
H3 Book chapter |
| Year |
1998 |
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Issue |
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Pages |
7-11
T2 - Sea-air exchange: processes and modellin |
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H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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no |
| Call Number |
UA @ admin @ c:irua:20972 |
Serial |
8580 |
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| Author |
Zhang, Q.; Vlaeminck, S.E.; DeBarbadillo, C.; Suzuki, R.; Kharkar, S.M.; Al-Omari, A.; Wett, B.; Chandran, K.; Murthy, S.; De Clippeleir, H. |
| Title |
Startup strategies of deammonification reactors treating reject water from thermally hydrolyzed solids |
Type |
P3 Proceeding |
| Year |
2017 |
Publication |
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Abbreviated Journal |
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Issue |
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Pages |
5 p.
T2 - WEFTEC.17, 30 September 4 October 2017, |
| Keywords |
P3 Proceeding; Engineering sciences. Technology; Sustainable Energy, Air and Water Technology (DuEL) |
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no |
| Call Number |
UA @ admin @ c:irua:151113 |
Serial |
8579 |
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| Author |
Salbu, B.; Janssens, K.; Lind, O.C.; Simionovici, A.S.; Trekling, T.; Drakopoulos, M.; Snigireva, I.; Snigirev, A. |
| Title |
SR-based X-ray microbeam techniques utilised for solid-state speciation of U in fuel particles |
Type |
P3 Proceeding |
| Year |
2002 |
Publication |
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Abbreviated Journal |
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Issue |
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Pages |
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P3 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ admin @ c:irua:39943 |
Serial |
5844 |
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| Author |
Elmonov, A.A.; Yusupov, M.S.; Dzhurakhalov, A.A.; Bogaerts, A. |
| Title |
Sputtering of Si(001) and SiC(001) by grazing ion bombardment |
Type |
P1 Proceeding |
| Year |
2008 |
Publication |
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Abbreviated Journal |
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Issue |
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Pages |
209-213 |
| Keywords |
P1 Proceeding; Plasma Lab for Applications in Sustainability and Medicine – Antwerp (PLASMANT) |
| Abstract |
The peculiarities of sputtering processes at 0.5-5 keV Ne grazing ion bombardment of Si(001) and SiC(001) surfaces and their possible application for the surface modification have been studied by computer simulation. Sputtering yields in the primary knock-on recoil atoms regime versus the initial energy of incident ions (E(0) = 0.5-5 keV) and angle of incidence (psi = 0-30 degrees) counted from a target surface have been calculated. Comparative studies of layer-by-layer sputtering for Si(001) and SiC(001) surfaces versus the initial energy of incident ions as well as an effective sputtering and sputtering threshold are discussed. |
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0000-00-00 |
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Series Issue |
84 |
Edition |
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978-86-80019-27-7 |
ISBN |
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Additional Links |
UA library record; WoS full record; |
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Open Access |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ lucian @ c:irua:95704 |
Serial |
3112 |
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| Author |
Vanherck, J. |
| Title |
Spontaneous and induced magnetisation in two-dimensional and bulk Heisenberg ferromagnets : a quantum mechanical treatment |
Type |
Doctoral thesis |
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2020 |
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Abbreviated Journal |
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Issue |
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Pages |
160 p. |
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Doctoral thesis; Condensed Matter Theory (CMT) |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ admin @ c:irua:171875 |
Serial |
6612 |
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| Author |
van Espen, P.; Janssens, K. |
| Title |
Spectrum evaluation |
Type |
H3 Book chapter |
| Year |
1992 |
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Abbreviated Journal |
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Issue |
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Pages |
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H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Chemometrics (Mitac 3) |
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chapter 4 |
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Approved |
no |
| Call Number |
UA @ admin @ c:irua:2809 |
Serial |
5842 |
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| Author |
Jannis, D.; Müller-Caspary, K.; Béché, A.; Oelsner, A.; Verbeeck, J. |
| Title |
Spectrocopic coincidence experiment in transmission electron microscopy |
Type |
Dataset |
| Year |
2019 |
Publication |
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Abbreviated Journal |
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Dataset; Electron microscopy for materials research (EMAT) |
| Abstract |
This dataset contains individual EEL and EDX events where for every event (electron or X-ray), their energy and time of arrival is stored. The experiment was performed in a transmission electron microscope (Tecnai Osiris) at 200 keV. The material investigated is an Al-Mg-Si-Cu alloy. The 'full_dataset.mat' contains the full dataset and the 'subset.mat' has the first five frames of the full dataset. The attached 'EELS-EDX.ipynb' is a jupyter notebook file. This file describes the data processing in order to observe the temporal correlation between the electrons and X-rays. |
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Approved |
no |
| Call Number |
UA @ admin @ c:irua:169112 |
Serial |
6888 |
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| Author |
Injuk, J.; Van Grieken, R.; Blank, A.; Eksperiandova, L.; Buhrke, V. |
| Title |
Specimen preparation |
Type |
H3 Book chapter |
| Year |
2006 |
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Abbreviated Journal |
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Issue |
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Pages |
411-432
T2 - Handbook of practical X-ray fluoresce |
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H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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no |
| Call Number |
UA @ admin @ c:irua:58854 |
Serial |
8573 |
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| Author |
Szalóki, I.; Ro, C.-U.; Osán, J.; de Hoog, J.; Van Grieken, R. |
| Title |
Speciation and surface analysis of single particles using electron-excited X-ray emission spectrometry |
Type |
H3 Book chapter |
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2004 |
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Pages |
569-592
T2 - X-ray spectrometry: recent technologi |
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H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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no |
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UA @ admin @ c:irua:43878 |
Serial |
8570 |
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| Author |
Bruynseels, F.; Van Grieken, R. |
| Title |
Speciation and distribution of sulfur and nitrogen in individual aerosol particles measured by LAMMA |
Type |
P3 Proceeding |
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1984 |
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P3 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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no |
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UA @ admin @ c:irua:117494 |
Serial |
8568 |
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Ravindra, K.; Wauters, E.; Van Grieken, R. |
| Title |
Spatial and temporal variations in particulate Polycyclic Aromatic Hydrocarbon (PAH) levels over Menen (Belgium) and their relation with air mass trajectories |
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H3 Book chapter |
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2007 |
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838-841
T2 - Air pollution modeling and its applic |
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H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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no |
| Call Number |
UA @ admin @ c:irua:65571 |
Serial |
8566 |
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Bencs, L.; Ravindra, K.; Van Grieken, R. |
| Title |
Spatial and temporal variation of anthropogenic palladium in the environment |
Type |
H3 Book chapter |
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2006 |
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433-454
T2 - Palladium emissions in the environmen |
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H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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no |
| Call Number |
UA @ admin @ c:irua:54922 |
Serial |
8565 |
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| Author |
Vos, L.; Van Grieken, R. |
| Title |
Spark source mass spectrometry for trace analysis of diverse biological matrices |
Type |
H3 Book chapter |
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1983 |
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Issue |
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Pages |
303-306
T2 - Mass spectrometry advances 1982 / Sch |
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H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Approved |
no |
| Call Number |
UA @ admin @ c:irua:117486 |
Serial |
8564 |
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| Author |
Török, S.; Szandor, S.; Xhoffer, C.; Van Grieken, R. |
| Title |
Source apportionment of individual aerosol particles at Hungarian background stations |
Type |
H3 Book chapter |
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1993 |
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32-331
T2 - Photo-oxidants: precursors and product |
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H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Approved |
no |
| Call Number |
UA @ admin @ c:irua:6265 |
Serial |
8559 |
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| Author |
Van Grieken, R.; Kontozova, V.; Godoi, R.H.M.; Spolnik, Z.; Worobiec, A.; Deutsch, F.; Bencs, L. |
| Title |
Some studies of the effect of indoor and outdoor pollutants on cultural heritage items |
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P3 Proceeding |
| Year |
2005 |
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P3 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Laboratory Experimental Medicine and Pediatrics (LEMP) |
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no |
| Call Number |
UA @ admin @ c:irua:57632 |
Serial |
8556 |
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| Author |
Caratelli, D.; Gielis, J.; Ricci, P.E.; Tavkhelidze, I. |
| Title |
Some properties of “bulky” links, generated by Generalized Möbius Listing's bodies GML4n |
Type |
P3 Proceeding |
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2013 |
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P3 Proceeding; Engineering sciences. Technology; Sustainable Energy, Air and Water Technology (DuEL) |
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no |
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UA @ admin @ c:irua:108672 |
Serial |
8555 |
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| Author |
Kuczumow, A.; Vekemans, B.; Schalm, O.; Vincze, L.; Dorriné, W.; Gysels, K.; Van Grieken, R. |
| Title |
Some new applications of auxiliary signals in X-ray fluorescence and electron microprobe analysis |
Type |
P1 Proceeding |
| Year |
1999 |
Publication |
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Abbreviated Journal |
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Issue |
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Pages |
197-201
T2 - Proceedings of the European Conferenc |
| Keywords |
P1 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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000081658400032 |
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UA library record; WoS full record |
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no |
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UA @ admin @ c:irua:24716 |
Serial |
8553 |
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| Author |
Vlaeminck, S.E.; Courtens, E.N.P.; Vandekerckhove, T.G.L.; Boon, N. |
| Title |
Some like it hot : perspectives for thermophilic nitrogen removal |
Type |
P3 Proceeding |
| Year |
2015 |
Publication |
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Abbreviated Journal |
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| Volume |
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Issue |
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Pages |
4 p.
T2 - IWA Nutrient Removal and Recovery 2015: |
| Keywords |
P3 Proceeding; Engineering sciences. Technology; Sustainable Energy, Air and Water Technology (DuEL) |
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no |
| Call Number |
UA @ admin @ c:irua:151145 |
Serial |
8552 |
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| Author |
Dingenen, F. |
| Title |
Solar-driven H2 production from seawater using stabilized plasmon-enhanced photocatalysts |
Type |
Doctoral thesis |
| Year |
2023 |
Publication |
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Abbreviated Journal |
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Issue |
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Pages |
XXXVIII, 210 p. |
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Doctoral thesis; Engineering sciences. Technology |
| Abstract |
As natural gas prices proved to be very volatile, sustainable alternatives are highly needed. Water-derived H2 was revealed as a promising substitute, allowing to produce a green energy carrier with a minimum of harmful emissions. Direct splitting of earth-abundant seawater provides an eco-friendly route for the production of clean H2, but is hampered by selectivity and stability issues due to the presence of salts.Photocatalytic seawater splitting is particularly promising for this purpose, as it seems less affected by adversary seawater effects and might rely on free and renewable solar power. Unfortunately, the benchmark photocatalyst, TiO2, still suffers from its low solar light activity. It is only actived upon illumination with energetic ultraviolet light (<5% of the sunlight). In order to broaden the activity window to the visible light, the concept of the 'plasmonic rainbow' was explored. Here, TiO2 is modified with various gold-silver composites that possess the unique optical phenomenon of Surface Plasmon Resonance (SPR). This phenomenon enables the absorption of light at very specific wavelengths, depending on the metal type, size, shape and dielectric environment. The light energy might then be converted into hot carriers, strong local electromagnetic fields and/or heat. By combining multiple composites with various sizes and compositions, a broadband absorption could be obtained, resulting in significantly enhanced activity in photocatalytic model reactions under simulated sunlight. The major disadvantage of these plasmonic nanoparticles is their tendency to oxidize and deactivate. To overcome this, polymer shell stabilization strategies were found to be effective to protect the metal cores. Both conductive and non-conductive polymers were studied. For the former, a mix-and-wait strategy generating polyaniline shells of 2-5 nm was used, whille the latter was based on a Layer-by-Layer approach, allowing (sub) nanometer thickness control. For the actual H2 production experiments, the plasmonic loading was optimized in a pure water:methanol scavenger (7:1) mixture and initially the stabilization strategies proofed to be effective for simulated seawater (0.5M NaCl), even after 2 years. However, in real seawater, the activity decreased drastically due to aggregation of the photocatalyst in the presence of multivalent cations. Finally, facile immobilization strategies using 3D printing showed to be able to yield stable, solar active photocatalyst for real seawater splitting. |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ admin @ c:irua:203196 |
Serial |
9094 |
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| Author |
Peeters, H. |
| Title |
Solar active photocatalytic self-cleaning coatings based on plasmon-embedded titania |
Type |
Doctoral thesis |
| Year |
2023 |
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Abbreviated Journal |
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Issue |
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Pages |
XX, 125 p. |
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Doctoral thesis; Engineering sciences. Technology |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ admin @ c:irua:201390 |
Serial |
9093 |
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| Author |
Admasu, W.F. |
| Title |
Socioeconomic and environmental impact of expropriation of agricultural land for urbanisation in Ethiopia |
Type |
Doctoral thesis |
| Year |
2021 |
Publication |
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Abbreviated Journal |
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Pages |
162 p. |
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Doctoral thesis; Engineering Management (ENM) |
| Abstract |
Globally, incorporation of agricultural lands into the urban boundary has been a common phenomenon. Governments use various alternatives to access the required land, including land expropriation procedures, which refers to the compulsorily taking of land from the landholders without their consent by paying compensation. In Ethiopia, the urban population is growing rapidly which resulted into an increase in the demand for urban land for housing construction, public services provision, and infrastructure developments. As the Ethiopian constitution prohibits sale of landholders, governments, at various levels, have been expropriating land from the surrounding farmers to meet the demand for urban land. The general objective of this thesis is to improve the understanding of the impacts of local land deals for urbanization on socioeconomics of farmers and the environment. The findings of this thesis revealed that there are gaps in the current practices of land expropriation for urban expansion that should be improved. The results showed that the compensation paid to the affected farmers is found to be economically inappropriate, i.e., not enough to restore the affected farmers’ livelihoods, in contrast with the land laws that allows a compensation amount that would put previous land users in a better or the same wellbeing as before the land expropriation. In addition, it is indicated that the land expropriation process does not take into account the value of ecosystem services, which are benefits obtain from the land, and important for the wellbeing of the society. We conclude that while land expropriation is an important tool to obtain land from the landholders when it is needed for public purposes, the practices in the study area show it is adversely affecting the socioeconomics of farmers and the environment. |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ admin @ c:irua:177909 |
Serial |
6944 |
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| Author |
Maciel de Menezes, R. |
| Title |
Skyrmionics and magnonics in chiral ferromagnets : from micromagnetic to atomistic control |
Type |
Doctoral thesis |
| Year |
2021 |
Publication |
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Abbreviated Journal |
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Issue |
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Pages |
222 p. |
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Doctoral thesis; Condensed Matter Theory (CMT) |
| Abstract |
The precise control of skyrmionics and magnonics in magnetic materials is key to the development of novel spin-based technology and information transport applications. Essentially, the inherent stability of magnetic skyrmions (provided by their topological charge) together with their extremely small size (down to a few nanometers) and the ultralow threshold current necessary to move them in nanostructures are the main advantages of skyrmionics. Not least, magnonics offers lower power consumption compared to electronics and the excitation of high frequency (sub-100~nm wavelength) magnons makes it possible for the creation of nanometric devices for ultrafast information transport. Even though extensive research has been carried out in recent years, the precise manipulation of skyrmions and spin waves (magnons) in nanostructures is not fully mastered and needs to be addressed before making functional skyrmionic and magnonic devices. In this thesis, we reveal multiple alternatives for the manipulation of skyrmions and spin-waves in different materials, such as bulk chiral magnets, heterochiral structures, magnet-supperconductor hybrids and two-dimentional magnetic materials. We make use of a multiscale model to numerically simulate the magnetic states at each considered material, from micromagnetic to atomistic control. We first explore the different nucleation mechanisms, activation energy, and the time evolution of the skyrmion formation in chiral magnetic films, crucial for the realization of skyrmion-based devices. We show that the skyrmion lattice is formed from the conical phase progressively, most probably by the formation of chiral bobbres, followed by the cylindrical growth of individual skyrmions from the film surface. That reflects a rod-like (one-dimensional) nucleation of the skyrmion phase, with an activation barrier of several electronvolts per skyrmion for the case of MnSi (Manganese monosilicide). In addition, we reveal the interesting blinking (creation-annihilation) behavior of skyrmions close to the phase boundary between the conical and skyrmion phases, where we recall that such switching between topologically distinct states has been proposed as a bit operation for information storage. Next, we discuss the motion of ferromagnetic and antiferromagnetic skyrmions in heterochiral magnets. We report the characteristic deflection of ferromagnetic skyrmions when moving across a heterochiral interface, where the extent of such deflection is tuned by the applied spin-polarized current and the magnitude of Dzyaloshinskii-Moriya interaction. Following, we show that the antiferromagnetic skyrmion achieves much higher velocities than its ferromagnetic counterpart, yet experiences far stronger confinement in nanoengineered heterochiral tracks, which reinforces antiferromagnetic skyrmions as a favorable choice for skyrmion-based devices. After that, we study the interesting coupling of magnetic skyrmions and superconducting vortices in magnet-superconductor heterostructures. We perform numerical simulations, based on experimental observations, to demonstrate that the stray field of magnetic skyrmions can nucleate antivortices in an adjacent superconducting film, giving rise to a hybrid topological object, the skyrmion-vortex pair, which harbor promising features for skyrmionics and quantum computing applications. We then explore the manipulation of a single skyrmion-vortex pair when currents are applied into both superconducting and magnetic parts of the heterostructure, which is of importance for the facilitated skyrmion guidance in racetrack applications. Afterwards, we make use of the high tunability of magnetic parameters in two-dimensional magnetic materials to reveal the rich phase diagram of exotic magnetic configurations in magnetic monolayers with suppressed nearest-neighbour exchange, where we show that several unique cycloidal, checkerboard, row-wise and spin-ice states are stabilized by the competition between the second-nearest-neighbor exchange, Dzyaloshinskii-Moriya, and dipolar interactions. Additionally, we show the coexistence of ferromagnetic and antiferromagnetic spin-cycloids, as well as novel types of skyrmions and chiral domain walls. Finally, in the last part of the thesis, we present the spin wave properties in the two-dimensional magnetic materials CrBr$3$ and CrI$3$. Using spin-dynamics simulations parametrized from first principles, we reveal that the spin wave dispersion in such materials can be tuned in a broad range of frequencies by strain-engineering, and that a designed pattern of strain, as well as structural defects (halide vacancies) can be turned useful in the design of spin-wave guides. Lastly, we discuss the realization of magnonic crystals by moiré-periodic modulation of magnetic parameters in van der Waals heterostructures, where we show that the several nanometer small periodicities in such samples are ideal for the interference of terahertz spin waves. Recalling the wide range of possibilities for manipulating spin waves in such two-dimensional materials, we therefore suggest these systems as a front-runner for prospective terahertz magnonic applications. |
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Approved |
Most recent IF: NA |
| Call Number |
UA @ admin @ c:irua:184244 |
Serial |
7019 |
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| Author |
Neven, L. |
| Title |
Singlet oxygen-based photoelectrochemical detection of phenolic contaminants |
Type |
Doctoral thesis |
| Year |
2022 |
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234 p. |
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Doctoral thesis; Antwerp Electrochemical and Analytical Sciences Lab (A-Sense Lab) |
| Abstract |
Phenolic compounds can be found everywhere in our daily lives but exhibit high toxicity, low (bio)degradability and hormone-disrupting effects when they are released in the environment. It is for this reason imperative to develop detection strategies for these pollutants. A promising approach involves the use of a photoelectrochemical (PEC) sensor. In this sensor, a photosensitiser (PS) type II, which generates 1O2 under illumination, is used to oxidise phenolic compounds present in the sample. The oxidised phenols are reduced at the electrode surface leading to the generation of an electrocatalytic redox cycle. In this thesis, an in-depth understanding, through the identification of the reactive oxygen species (ROS) in the PEC sensing mechanism, is obtained. The detection strategy is optimised by choosing the PS with the highest 1O2 production and by optimising the detection parameters so that the PEC sensor can be successfully applied for the detection of phenols in industrial samples. First, it was determined that the use of highly fluorinated zinc phthalocyanine derivatives, F52PcZn and F64PcZn, as photocatalysts was optimal for the sensing of phenol due to their high 1O2 production and improved single-site isolation. However, next to 1O2, it was shown that the ROS O2•- and H2O2 were also generated in the PEC sensor. Their contribution to the photocurrent response was studied by rotating disk electrode measurements in function of the pH and applied potential. After this, the PEC detection strategy was optimised in terms of pH and applied potential for the detection of doxycycline, cefadroxil, and phenol. It was found that the use of alkaline pH-levels led to nmol L-1-level detection limits. The combination with square wave voltammetry (SWV) was, also, proposed to allow the quantification and identification of phenolic compounds in a specific sample. At last, the developed PEC and SWV sensors were applied for the measurement of phenolic compounds in industrial water samples. The PEC sensor could follow the decrease of the phenolic concentration throughout the wastewater treatment process while the SWV sensor provided the electrochemical fingerprints of these samples. The thesis concluded that the use of the PEC sensor was advantageous in the measurement of lower concentrated phenolic samples due to its high sensitivity and fast measurement time in comparison to commercial test kits. |
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UA @ admin @ c:irua:187029 |
Serial |
8932 |
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| Author |
Thiruvottriyur Shanmugam, S. |
| Title |
Singlet oxygen-based photoelectrochemical detection of nucleic acids |
Type |
Doctoral thesis |
| Year |
2022 |
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217 p. |
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Doctoral thesis; Engineering sciences. Technology; Antwerp Electrochemical and Analytical Sciences Lab (A-Sense Lab) |
| Abstract |
MicroRNAs (miRNAs) are small oligonucleotides (18-25 bases) that play a key role in epigenetic regulation. Since the discovery of miRNAs in 1993, their role in biological processes has been extensively investigated. By now, it has been evidenced that monitoring and detection of miRNAs can improve (early) disease diagnosis. The existing diagnostic approaches have limitations such as the need for complex multistep protocols for sample preparation, analysis, data interpretation, high cost of equipment, the need for highly qualified personnel, and high laboratory standards. As opposed to this, point-of-care biosensors and chips aim to facilitate the procedure and avoid sending samples into centralized laboratories, which saves time, reduces the chance of sample degradation, and enables analysis of patient samples in remote areas, directly at home or primary and secondary care facilities (i.e. general practitioners and specialists). The latter is essential for therapy assessment and follow-up monitoring of patients with chronic diseases and cancer. Nevertheless, the development of such sensors is lagging compared to the projections of 10 – 20 years ago, mainly due to insufficient sensitivity, poor reproducibility, and the complexity of the sensors’ design reported in the research literature. This motivates the development of new detection strategies and technologies such as photoelectrochemical sensors that combine the best features of different sensing approaches. The primary concern when developing detection technologies for miRNA is the need for a highly sensitive and selective platform. This thesis explores a novel photoelectrochemical (PEC) method that is distinctive owing to its sensitive nature and simple and robust design. Firstly, we focused on the usage of recently emerging commercial gold-sputtered electrode systems for the detection of short nucleic acid with enzymatic amplification. Importantly, cleaning such electrodes is a challenge since the standard procedures known for regular disk electrodes such as polishing cannot be employed here, since it will damage the protective layer on the electrode. However, the electrodes can be washed and pretreated chemically and/or electrochemically. Thus, a procedure to effectively clean and modify the gold-sputtered electrode has been developed, resulting in high-performance gold-sputtered nucleic acid sensors. Next, the usage of molecular photosensitizers as an alternative to enzymatic amplification has been evaluated. We took advantage of the singlet oxygen production by photosensitizers upon photoexcitation, leading to a photocurrent response due to the singlet oxygen-induced (electro)chemical conversions. Following the demonstration of the detection strategy, the analytical performance of the sensing system was evaluated using magnetic beads-based nucleic acid assay on disposable electrode platforms, with a focus to enhance the sensitivity and robustness of the technique in detecting complementary nucleic acid targets. Following the fundamental evaluation of the singlet oxygen-based PEC detection of nucleic acids, we further optimized the assay and measurement parameters and employed the sensing strategy for a polymerase chain reaction-free (PCR-free) quantification of miRNAs related to prostate cancer. By successfully detecting and quantifying low-picomolar range concentrations (< 10 pM) in plasma samples from prostate cancer patients, we successfully showed the applicability of the novel sensing strategy. We have also compared and positioned the performance of our developed PEC strategy with an existing state-of-art technique, i.e. electrochemiluminescence (ECL). Our PEC strategy performed on par with ECL, both yielding low-picomolar detection limits in serum matrices, however quicker and cheaper than ECL. Owing to the versatility of this PEC technique, the final study explored its multiplexing capability. As a starting point in this branch of the research, we have investigated two possible ways for multiplexing. To perform multiple measurements at the same time, constructing calibration plots and quantifying unknown miRNA concentrations in patient samples at the same time, we have developed a high-throughput detection with 96X multi-channel electrode systems and in-house designed and constructed 96XLED illumination sources. Secondly, to detect more than one target miRNA in a single measurement, intra-vial multiplexing where the samples were analyzed for different targets in one vial was also explored. Altogether, this thesis presents the fundamentals, development and application of a novel PEC strategy for detecting short (< 25 bases) nucleic acid sequences, in particular, miRNA. With an aim to serve as a distinctive technique to function as a clinical testing platform without any need for PCR, this work adds value to the development of nucleic acid-based sensors for miRNAs and other short-stranded nucleic acid biomarkers, and benefits in the early detection of diseases like cancer. |
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no |
| Call Number |
UA @ admin @ c:irua:191753 |
Serial |
8931 |
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| Author |
Khan, S.U. |
| Title |
Singlet oxygen-based photoelectrocatalysis : from photosensitizer structures to plasmonic enhancement |
Type |
Doctoral thesis |
| Year |
2023 |
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Abbreviated Journal |
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Issue |
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182 p. |
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Doctoral thesis; Antwerp Electrochemical and Analytical Sciences Lab (A-Sense Lab) |
| Abstract |
Singlet molecular oxygen (1O2) has continuously attracted researchers' interest because of its involvement in various processes, such as in photodynamic reactions in biological and chemical systems. 1O2 is an effective electrophile and potent oxidizing agent and can be easily generated by photosensitization via the illumination of organic dyes with visible light. As described in Chapter 1, 1O2 has gained prominence in various applications such as wastewater treatment, photodynamic therapy of cancer, organic synthesis, and recently developed 1O2-based photoelectrochemical (PEC) sensing of phenolic compounds. Phenolic compounds are a potential source of contaminants that originates from industrial effluents and waste products of chemical and pharmaceutical industries. These phenolic compounds pose severe threats to humans and aquatic life after reaching the environment. Therefore, it is imperative to develop photoactive materials that efficiently generate 1O2 and oxidize phenolic compounds and antibiotics. The existing 1O2 generating photosensitizers (PSs) include porphyrins, phthalocyanines (Pcs), subphthalocyanines (SubPcs), and other dyes such as derivatives of xanthene (e.g., Rose Bengal (RB)), and fluorinated boron-dipyrromethene (BODIPYs), and phenothiazinium dyes (e. g. Methylene Blue (MB)) which display long-lived triplet excited state and can be used in 1O2-based applications. This thesis focuses on preparing efficient hybrid materials based on newly synthesized Pcs, different surface area titanium dioxide (TiO2) and plasmonic gold nanoparticles (AuNPs) for their use in the PEC detection of phenolic compounds. The first focus was on developing a fast amperometric method to test the photo-electrocatalytic activity of 1O2 producing PSs dissolved in MeOH based on the redox cycling of an electroactive phenolic compound, hydroquinone (HQ) (Chapter 2). This method of testing PSs does not require the accumulation of a reaction product since the amperometric signal develops near instantly when the light is on, which enables dynamic monitoring of a PSs activity at varying conditions in a single experiment. This method was crucial to measure high 1O2 quantum yield and low yield in the same experimental conditions. Moreover, the obtained results revealed a range of working parameters affecting the PEC activity of PSs. The next goal was to immobilize tert-butyl substituted aluminum Pc (t-BuPcAlCl) on the solid support, which showed a high 1O2 quantum yield. However, before immobilizing Pc on a solid support such as TiO2, it is essential to know the electronic energy level of Pcs for the possible electron transfers from Pcs to TiO2. Therefore, Chapter 3 explored the (spectro)electrochemical properties of t-BuPcAlCl Pc. Next, in Chapter 4, t-BuPcAlCl Pc and other tert-butyl substituted Pcs with Zn central metal, t-BuPcZn, and its metal-free derivative t-BuPcH2 were immobilized on different surface area TiO2. The PEC activity of immobilized Pcs on TiO2 toward different phenols and antibiotics was studied, and the action mechanism was revealed and compared with sterically hindered fluorinated Pc F64PcZn. In the final part of this thesis plasmonic AuNPs were introduced combined with trimethylsilane-protected acetylene functionalized ZnPc (TMSZnPc) to study the synergistic effect that boosts the overall activity toward the detection of phenols under visible light illumination (Chapter 5) . The TMSZnPc was coupled with AuNPs via a click chemistry approach. The 1O2 quantum yield of TMSZnPc improved significantly after conjugating with AuNPs, and, subsequently, the PEC activity for detecting HQ. The theoretical and experimental investigation demonstrated that the plasmonic enhancement of TMSZnPc is driven by the near-field mechanism. This shows the importance of plasmonic AuNPs with other photoactive species for their use in 1O2-based applications. The fundamental knowledge obtained in this doctoral study will ultimately deepen the understanding of developing 1O2-based PEC sensors for detecting phenolic compounds and pharmaceuticals in the wastewater stream, helping to choose efficient materials and, in the last instance, a more sustainable future especially access to clean water for everyone. |
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Most recent IF: NA |
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UA @ admin @ c:irua:193342 |
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7337 |
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