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“DART explained: how to carry out a discrete tomography reconstruction”. Batenburg KJ, Bals S, Sijbers J, Van Tendeloo G, , 295 (2008)
Keywords: P1 Proceeding; Electron microscopy for materials research (EMAT); Vision lab
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“Enhanced stability against oxidation due to 2D self-organisation of hcp cobalt nanocrystals”. Lisiecki I, Turner S, Bals S, Pileni MP, Van Tendeloo G Springer, Berlin, page 273 (2008).
Keywords: H1 Book chapter; Electron microscopy for materials research (EMAT)
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“Klassieke toetsing in de praktijk”. Bals S, Stes A, Celis V LannooCampus, Leuven, page 211 (2009).
Keywords: H2 Book chapter; Educational sciences; EduBROn; Electron microscopy for materials research (EMAT)
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“Reliable pore-size measurements based on a procedure specifically designed for electron tomography measurements of nanoporous samples”. Van Eyndhoven G, Batenburg KJ, van Oers C, Kurttepeli M, Bals S, Cool P, Sijbers J, (2014)
Keywords: P3 Proceeding; Electron microscopy for materials research (EMAT); Vision lab; Laboratory of adsorption and catalysis (LADCA)
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“The benefits of statistical parameter estimation theory for quantitative interpretation of electron microscopy data”. Van Aert S, Bals S, Chang LY, den Dekker AJ, Kirkland AI, Van Dyck D, Van Tendeloo G Springer, Berlin, page 97 (2008).
Keywords: H1 Book chapter; Electron microscopy for materials research (EMAT); Vision lab
DOI: 10.1007/978-3-540-85156-1_49
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“Investigating lattice strain in Au nanodecahedrons”. Goris B, De Beenhouwer J, de Backer A, Zanaga D, Batenburg J, Sanchez-Iglesias A, Liz-Marzan L, Van Aert S, Sijbers J, Van Tendeloo G, Bals S, , 11 (2016). http://doi.org/10.1002/9783527808465.EMC2016.5519
Keywords: P1 Proceeding; Electron microscopy for materials research (EMAT); Vision lab
DOI: 10.1002/9783527808465.EMC2016.5519
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Skorikov A, Heyvaert W, Albrecht W, Pelt DM, Bals S (2021) EMAT Simulated 3D Nanoparticle Structures Dataset
Abstract: This dataset contains 1000 simulated nanoparticle-like 3D structures and noisy EDX-like elemental maps based on them. These data are intended to be used for quantitative analysis of data processing methods in (EDX) tomography of nanoparticles and training the data-driven approaches for these tasks. The dataset is structured as follows: voxel_data/clean 3D voxel grid representation of the simulated nanoparticles. Voxel intensities are adjusted so that the total intensity equals 103. All 3D structures have unique identifiers in 0..999 range. The data derived from a 3D structure preserves this unique identifier. sinograms/clean Tilt series of projection images obtained from the corresponding 3D structures over an angular range of -75..75 degrees with a tilt step of 10 degrees to simulate a typical tilt series used in EDX tomography. Total intensity in each projection image equals 103. sinograms/noisy Tilt series of projection images corrupted with Poisson noise and an additional spatially uniform background noise. projections/clean Projection images extracted from the clean tilt series at 0 degrees tilt angle. projections/noisy Projection images extracted from the noisy tilt series at 0 degrees tilt angle. images/clean Visualizations of the clean projections as PNG images with the intensity range adjusted to 0..255 images/noisy Visualizations of the noisy projections as PNG images with the intensity range adjusted to 0..255
Keywords: Dataset; Electron microscopy for materials research (EMAT)
DOI: 10.5281/zenodo.4580545
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Grü,newald L, Chezganov D, De Meyer R, Orekhov A, Van Aert S, Bogaerts A, Bals S, Verbeeck J (2023) Supplementary Information for “In-situ Plasma Studies using a Direct Current Microplasma in a Scanning Electron Microscope”
Abstract: Supplementary information for the article “In-situ Plasma Studies using a Direct Current Microplasma in a Scanning Electron Microscope” containing the videos of in-situ SEM imaging (mp4 files), raw data/images, and Jupyter notebooks (ipynb files) for data treatment and plots. Link to the preprint: https://doi.org/10.48550/arXiv.2308.15123 Explanation of the data files can be found in the Information.pdf file. The Videos folder contains the in-situ SEM image series mentioned in the paper. If there are any questions/bugs, feel free to contact me at lukas.grunewaldatuantwerpen.be
Keywords: Dataset; Engineering sciences. Technology; Electron microscopy for materials research (EMAT); Plasma Lab for Applications in Sustainability and Medicine – Antwerp (PLASMANT)
DOI: 10.5281/ZENODO.8042030
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“3D-cavity-confined CsPbBr₃, quantum dots for visible-light-driven photocatalytic C(sp³)-H bond activation”. Gao Y-J, Jin H, Esteban DA, Weng B, Saha RA, Yang M-Q, Bals S, Steele JA, Huang H, Roeffaers MBJ, Carbon Energy , e559 (2024). http://doi.org/10.1002/CEY2.559
Abstract: Metal halide perovskite (MHP) quantum dots (QDs) offer immense potential for several areas of photonics research due to their easy and low-cost fabrication and excellent optoelectronic properties. However, practical applications of MHP QDs are limited by their poor stability and, in particular, their tendency to aggregate. Here, we develop a two-step double-solvent strategy to grow and confine CsPbBr3 QDs within the three-dimensional (3D) cavities of a mesoporous SBA-16 silica scaffold (CsPbBr3@SBA-16). Strong confinement and separation of the MHP QDs lead to a relatively uniform size distribution, narrow luminescence, and good ambient stability over 2 months. In addition, the CsPbBr3@SBA-16 presents a high activity and stability for visible-light-driven photocatalytic toluene C(sp(3))-H bond activation to produce benzaldehyde with similar to 730 mu mol g(-1) h(-1) yield rate and near-unity selectivity. Similarly, the structural stability of CsPbBr3@SBA-16 QDs is superior to that of both pure CsPbBr3 QDs and those confined in MCM-41 with 1D channels.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
DOI: 10.1002/CEY2.559
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“AuNP/MIL-88B-NH₂, nanocomposite for the valorization of nitroarene by green catalytic hydrogenation”. Lelouche SNK, Lemir I, Biglione C, Craig T, Bals S, Horcajada P, Chemistry: a European journal , 1 (2024). http://doi.org/10.1002/CHEM.202400442
Abstract: The efficiency of a catalytic process is assessed based on conversion, yield, and time effectiveness. However, these parameters are insufficient for evaluating environmentally sustainable research. As the world is urged to shift towards green catalysis, additional factors such as reaction media, raw material availability, sustainability, waste minimization and catalyst biosafety, need to be considered to accurately determine the efficacy and sustainability of the process. By combining the high porosity and versatility of metal organic frameworks (MOFs) and the activity of gold nanoparticles (AuNPs), efficient, cyclable and biosafe composite catalysts can be achieved. Thus, a composite based on AuNPs and the nanometric flexible porous iron(III) aminoterephthalate MIL-88B-NH2 was successfully synthesized and fully characterized. This nanocomposite was tested as catalyst in the reduction of nitroarenes, which were identified as anthropogenic water pollutants, reaching cyclable high conversion rates at short times for different nitroarenes. Both synthesis and catalytic reactions were performed using green conditions, and even further tested in a time-optimizing one-pot synthesis and catalysis experiment. The sustainability and environmental impact of the catalytic conditions were assessed by green metrics. Thus, this study provides an easily implementable synthesis, and efficient catalysis, while minimizing the environmental and health impact of the process.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 4.3
DOI: 10.1002/CHEM.202400442
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Cioni M, Delle Piane M, Polino D, Rapetti D, Crippa M, Arslan Irmak E, Pavan GM, Van Aert S, Bals S (2024) Data for Sampling Real‐Time Atomic Dynamics in Metal Nanoparticles by Combining Experiments, Simulations, and Machine Learning
Abstract: Even at low temperatures, metal nanoparticles (NPs) possess atomic dynamics that are key for their properties but challenging to elucidate. Recent experimental advances allow obtaining atomic‐resolution snapshots of the NPs in realistic regimes, but data acquisition limitations hinder the experimental reconstruction of the atomic dynamics present within them. Molecular simulations have the advantage that these allow directly tracking the motion of atoms over time. However, these typically start from ideal/perfect NP structures and, suffering from sampling limits, provide results that are often dependent on the initial/putative structure and remain purely indicative. Here, by combining state‐of‐the‐art experimental and computational approaches, how it is possible to tackle the limitations of both approaches and resolve the atomistic dynamics present in metal NPs in realistic conditions is demonstrated. Annular dark‐field scanning transmission electron microscopy enables the acquisition of ten high‐resolution images of an Au NP at intervals of 0.6 s. These are used to reconstruct atomistic 3D models of the real NP used to run ten independent molecular dynamics simulations. Machine learning analyses of the simulation trajectories allows resolving the real‐time atomic dynamics present within the NP. This provides a robust combined experimental/computational approach to characterize the structural dynamics of metal NPs in realistic conditions.
Keywords: Dataset; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
DOI: 10.5281/ZENODO.10997963
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“Designer phospholipid capping ligands for soft metal halide nanocrystals”. Morad V, Stelmakh A, Svyrydenko M, Feld LG, Boehme SC, Aebli M, Affolter J, Kaul CJ, Schrenker NJ, Bals S, Sahin Y, Dirin DN, Cherniukh I, Raino G, Baumketner A, Kovalenko MV, Nature 626, 542 (2024). http://doi.org/10.1038/S41586-023-06932-6
Abstract: The success of colloidal semiconductor nanocrystals (NCs) in science and optoelectronics is inextricable from their surfaces. The functionalization of lead halide perovskite NCs1-5 poses a formidable challenge because of their structural lability, unlike the well-established covalent ligand capping of conventional semiconductor NCs6,7. We posited that the vast and facile molecular engineering of phospholipids as zwitterionic surfactants can deliver highly customized surface chemistries for metal halide NCs. Molecular dynamics simulations implied that ligand-NC surface affinity is primarily governed by the structure of the zwitterionic head group, particularly by the geometric fitness of the anionic and cationic moieties into the surface lattice sites, as corroborated by the nuclear magnetic resonance and Fourier-transform infrared spectroscopy data. Lattice-matched primary-ammonium phospholipids enhance the structural and colloidal integrity of hybrid organic-inorganic lead halide perovskites (FAPbBr3 and MAPbBr3 (FA, formamidinium; MA, methylammonium)) and lead-free metal halide NCs. The molecular structure of the organic ligand tail governs the long-term colloidal stability and compatibility with solvents of diverse polarity, from hydrocarbons to acetone and alcohols. These NCs exhibit photoluminescence quantum yield of more than 96% in solution and solids and minimal photoluminescence intermittency at the single particle level with an average ON fraction as high as 94%, as well as bright and high-purity (about 95%) single-photon emission. Phospholipids enhance the structural and colloidal integrity of hybrid organic-inorganic lead halide perovskites and lead-free metal halide nanocrystals, which then exhibit enhanced robustness and optical properties.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 64.8
DOI: 10.1038/S41586-023-06932-6
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“Accurate segmentation of dense nanoparticles by partially discrete electron tomography”. Roelandts T, Batenburg KJ, Biermans E, Kübel C, Bals S, Sijbers J, Ultramicroscopy 114, 96 (2012). http://doi.org/10.1016/j.ultramic.2011.12.003
Abstract: Accurate segmentation of nanoparticles within various matrix materials is a difficult problem in electron tomography. Due to artifacts related to image series acquisition and reconstruction, global thresholding of reconstructions computed by established algorithms, such as weighted backprojection or SIRT, may result in unreliable and subjective segmentations. In this paper, we introduce the Partially Discrete Algebraic Reconstruction Technique (PDART) for computing accurate segmentations of dense nanoparticles of constant composition. The particles are segmented directly by the reconstruction algorithm, while the surrounding regions are reconstructed using continuously varying gray levels. As no properties are assumed for the other compositions of the sample, the technique can be applied to any sample where dense nanoparticles must be segmented, regardless of the surrounding compositions. For both experimental and simulated data, it is shown that PDART yields significantly more accurate segmentations than those obtained by optimal global thresholding of the SIRT reconstruction.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); Vision lab
Impact Factor: 2.843
Times cited: 34
DOI: 10.1016/j.ultramic.2011.12.003
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“Advanced reconstruction algorithms for electron tomography : from comparison to combination”. Goris B, Roelandts T, Batenburg KJ, Heidari Mezerji H, Bals S, Ultramicroscopy 127, 40 (2013). http://doi.org/10.1016/j.ultramic.2012.07.003
Abstract: In this work, the simultaneous iterative reconstruction technique (SIRT), the total variation minimization (TVM) reconstruction technique and the discrete algebraic reconstruction technique (DART) for electron tomography are compared and the advantages and disadvantages are discussed. Furthermore, we describe how the result of a three dimensional (3D) reconstruction based on TVM can provide objective information that is needed as the input for a DART reconstruction. This approach results in a tomographic reconstruction of which the segmentation is carried out in an objective manner.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); Vision lab
Impact Factor: 2.843
Times cited: 63
DOI: 10.1016/j.ultramic.2012.07.003
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“Correction of non-linear thickness effects in HAADF STEM electron tomography”. van den Broek W, Rosenauer A, Goris B, Martinez GT, Bals S, Van Aert S, van Dyck D, Ultramicroscopy 116, 8 (2012). http://doi.org/10.1016/j.ultramic.2012.03.005
Abstract: In materials science, high angle annular dark field scanning transmission electron microscopy is often used for tomography at the nanometer scale. In this work, it is shown that a thickness dependent, non-linear damping of the recorded intensities occurs. This results in an underestimated intensity in the interior of reconstructions of homogeneous particles, which is known as the cupping artifact. In this paper, this non-linear effect is demonstrated in experimental images taken under common conditions and is reproduced with a numerical simulation. Furthermore, an analytical derivation shows that these non-linearities can be inverted if the imaging is done quantitatively, thus preventing cupping in the reconstruction.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); Vision lab
Impact Factor: 2.843
Times cited: 67
DOI: 10.1016/j.ultramic.2012.03.005
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“Electron tomography based on a total variation minimization reconstruction technique”. Goris B, van den Broek W, Batenburg KJ, Heidari Mezerji H, Bals S, Ultramicroscopy 113, 120 (2012). http://doi.org/10.1016/j.ultramic.2011.11.004
Abstract: The 3D reconstruction of a tilt series for electron tomography is mostly carried out using the weighted backprojection (WBP) algorithm or using one of the iterative algorithms such as the simultaneous iterative reconstruction technique (SIRT). However, it is known that these reconstruction algorithms cannot compensate for the missing wedge. Here, we apply a new reconstruction algorithm for electron tomography, which is based on compressive sensing. This is a field in image processing specialized in finding a sparse solution or a solution with a sparse gradient to a set of ill-posed linear equations. Therefore, it can be applied to electron tomography where the reconstructed objects often have a sparse gradient at the nanoscale. Using a combination of different simulated and experimental datasets, it is shown that missing wedge artefacts are reduced in the final reconstruction. Moreover, it seems that the reconstructed datasets have a higher fidelity and are easier to segment in comparison to reconstructions obtained by more conventional iterative algorithms.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); Vision lab
Impact Factor: 2.843
Times cited: 171
DOI: 10.1016/j.ultramic.2011.11.004
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“Electronically coupled complementary interfaces between perovskite band insulators”. Huijben M, Rijnders G, Blank DHA, Bals S, Van Aert S, Verbeeck J, Van Tendeloo G, Brinkman A, Hilgenkamp H, Nature materials 5, 556 (2006). http://doi.org/10.1038/nmat1675
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 39.737
Times cited: 315
DOI: 10.1038/nmat1675
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“Hydrogen adsorption properties of platinum decorated hierarchically structured templated carbons”. Oh H, Gennett T, Atanassov P, Kurttepeli M, Bals S, Hurst KE, Hirscher M, Microporous and mesoporous materials: zeolites, clays, carbons and related materials 177, 66 (2013). http://doi.org/10.1016/j.micromeso.2013.04.020
Abstract: In this report, the possibility of Pt catalytic activity for the dissociation of hydrogen molecules and subsequent hydrogen adsorption on sucrose templated carbon at ambient temperature has been studied. In order to investigate Pt catalytic effect for hydrogen storage solely, 6.8 wt.% Pt-doped (Pt/TC) and pure templated carbon (TC) possessing almost identical specific surface area (SSA) and pore volume (Vp) have been successfully synthesized. Since both Pt/TC and TC shares for their textural properties (e.g. SSA and Vp), any difference of hydrogen adsorption characteristic and storage capacity can be ascribed to the presence of Pt nanoparticles. Both samples are characterized by various techniques such as powder Xray diffraction, ICP-OES, Raman spectroscopy, transmission electron microscopy, cryogenic thermal desorption spectroscopy, low-pressure high-resolution hydrogen and nitrogen BET and high-pressure hydrogen adsorption isotherms in a Sieverts' apparatus. By applying hydrogen and deuterium isotope mixture, cryogenic thermal desorption spectroscopy point to a Pt catalytic activity for the dissociation of hydrogen molecules. Furthermore, the hydrogen adsorption isotherms at RT indicate an enhancement of the initial hydrogen adsorption kinetics in Pt-doped system. However, the hydrogen storage capacity of Pt/TC exhibits a negligible enhancement with a strong hysteresis, suggesting no connection between the spillover effect and a feasible hydrogen storage enhancement. (C) 2013 Elsevier Inc. All rights reserved.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 3.615
Times cited: 25
DOI: 10.1016/j.micromeso.2013.04.020
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“Low-dose patterning of platinum nanoclusters on carbon nanotubes by focused-electron-beam-induced deposition as studied by TEM”. Ke X, Bittencourt C, Bals S, Van Tendeloo G, Beilstein journal of nanotechnology 4, 77 (2013). http://doi.org/10.3762/bjnano.4.9
Abstract: Focused-electron-beam-induced deposition (FEBID) is used as a direct-write approach to decorate ultrasmall Pt nanoclusters on carbon nanotubes at selected sites in a straightforward maskless manner. The as-deposited nanostructures are studied by transmission electron microscopy (TEM) in 2D and 3D, demonstrating that the Pt nanoclusters are well-dispersed, covering the selected areas of the CNT surface completely. The ability of FEBID to graft nanoclusters on multiple sides, through an electron-transparent target within one step, is unique as a physical deposition method. Using high-resolution TEM we have shown that the CNT structure can be well preserved thanks to the low dose used in FEBID. By tuning the electron-beam parameters, the density and distribution of the nanoclusters can be controlled. The purity of as-deposited nanoclusters can be improved by low-energy electron irradiation at room temperature.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 3.127
Times cited: 12
DOI: 10.3762/bjnano.4.9
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“Molecular shape-selectivity of MFI zeolite nanosheets in n-decane isomerization and hydrocracking”. Verheyen E, Jo C, Kurttepeli M, Vanbutsele G, Gobechiya E, Korányi TI, Bals S, Van Tendeloo G, Ryoo R, Kirschhock CEA, Martens JA;, Journal of catalysis 300, 70 (2013). http://doi.org/10.1016/j.jcat.2012.12.017
Abstract: MFI zeolite nanosheets with thickness of 2 and 8 nm were synthesized, transformed into bifunctional catalysts by loading with platinum and tested in n-decane isomerization and hydrocracking. Detailed analysis of skeletal isomers and hydrocracked products revealed that the MFI nanosheets display transition-state shape-selectivity similar to bulk MFI zeolite crystals. The suppressed formation of bulky skeletal isomers and C5 cracking products are observed both in the nanosheets and the bulk crystals grown in three dimensions. This is typical for restricted transition-state shape-selectivity, characteristic for the MFI type pores. It is a first clear example of transition-state shape-selectivity inside a zeolitic nanosheet. Owing to the short diffusion path across the sheets, expression of diffusion-based discrimination of reaction products in the MFI nanosheets was limited. The 2-methylnonane formation among monobranched C10 isomers and 2,7-dimethyloctane among dibranched C10 isomers, which in MFI zeolite are favored by product diffusion, was much less favored on the nanosheets compared to the reference bulk ZSM-5 material.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 6.844
Times cited: 121
DOI: 10.1016/j.jcat.2012.12.017
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“Phase formation in intermixed NiGe thin films : influence of Ge content and low-temperature nucleation of hexagonal nickel germanides”. De Schutter B, Devulder W, Schrauwen A, van Stiphout K, Perkisas T, Bals S, Vantomme A, Detavernier C, Microelectronic engineering 120, 168 (2014). http://doi.org/10.1016/j.mee.2013.09.004
Abstract: In this study, we focus on phase formation in intermixed NiGe thin films as they represent a simplified model of the small intermixed interface layer that is believed to form upon deposition of Ni on Ge and where initial phase formation happens. A combinatorial sputter deposition technique was used to co-deposit a range of intermixed NiGe thin films with Ge concentrations varying between 0 and 50 at.%Ge in a single deposition on both Ge (100) and inert SiO2 substrates. In situ X-ray diffraction and transmission electron microscopy where used to study phase formation. In almost the entire composition range under investigation, crystalline phases where found to be present in the as-deposited films. Between 36 and 48 at.%Ge, high-temperature hexagonal nickel germanides were found to occur metastabily below 300 °C, both on SiO2 and Ge (100) substrates. For Ge concentrations in the range between 36 and 42 at.%, this hexagonal germanide phase was even found to be present at room temperature in the as-deposited films. The results obtained in this work could provide more insight in the phase sequence of a pure Ni film on Ge.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 1.806
Times cited: 9
DOI: 10.1016/j.mee.2013.09.004
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“Photocatalytic acetaldehyde oxidation in air using spacious TiO2 films prepared by atomic layer deposition on supported carbonaceous sacrificial templates”. Verbruggen SW, Deng S, Kurttepeli M, Cott DJ, Vereecken PM, Bals S, Martens JA, Detavernier C, Lenaerts S, Applied catalysis : B : environmental 160, 204 (2014). http://doi.org/10.1016/j.apcatb.2014.05.029
Abstract: Supported carbon nanosheets and carbon nanotubes served as sacrificial templates for preparing spacious TiO2 photocatalytic thin films. Amorphous TiO2 was deposited conformally on the carbonaceous template material by atomic layer deposition (ALD). Upon calcination at 550 °C, the carbon template was oxidatively removed and the as-deposited continuous amorphous TiO2 layers transformed into interlinked anatase nanoparticles with an overall morphology commensurate to the original template structure. The effect of type of template, number of ALD cycles and gas residence time of pollutant on the photocatalytic activity, as well as the stability of the photocatalytic performance of these thin films was investigated. The TiO2 films exhibited excellent photocatalytic activity toward photocatalytic degradation of acetaldehyde in air as a model reaction for photocatalytic indoor air pollution abatement. Optimized films outperformed a reference film of commercial PC500.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); Sustainable Energy, Air and Water Technology (DuEL)
Impact Factor: 9.446
Times cited: 37
DOI: 10.1016/j.apcatb.2014.05.029
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“The properties of SIRT, TVM, and DART for 3D imaging of tubular domains in nanocomposite thin-films and sections”. Chen D, Goris B, Bleichrodt F, Heidari Mezerji H, Bals S, Batenburg KJ, de With G, Friedrich H, Ultramicroscopy 147, 137 (2014). http://doi.org/10.1016/j.ultramic.2014.08.005
Abstract: In electron tomography, the fidelity of the 3D reconstruction strongly depends on the employed reconstruction algorithm. In this paper, the properties of SIRT, TVM and DART reconstructions are studied with respect to having only a limited number of electrons available for imaging and applying different angular sampling schemes. A well-defined realistic model is generated, which consists of tubular domains within a matrix having slab-geometry. Subsequently, the electron tomography workflow is simulated from calculated tilt-series over experimental effects to reconstruction. In comparison with the model, the fidelity of each reconstruction method is evaluated qualitatively and quantitatively based on global and local edge profiles and resolvable distance between particles. Results show that the performance of all reconstruction methods declines with the total electron dose. Overall, SIRT algorithm is the most stable method and insensitive to changes in angular sampling. TVM algorithm yields significantly sharper edges in the reconstruction, but the edge positions are strongly influenced by the tilt scheme and the tubular objects become thinned. The DART algorithm markedly suppresses the elongation artifacts along the beam direction and moreover segments the reconstruction which can be considered a significant advantage for quantification. Finally, no advantage of TVM and DART to deal better with fewer projections was observed.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 2.843
Times cited: 42
DOI: 10.1016/j.ultramic.2014.08.005
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“Quantitative electron tomography : the effect of the three-dimensional point spread function”. Heidari H, van den Broek W, Bals S, Ultramicroscopy 135, 1 (2013). http://doi.org/10.1016/j.ultramic.2013.06.005
Abstract: The intensity levels in a three-dimensional (3D) reconstruction, obtained by electron tomography, can be influenced by several experimental imperfections. Such artifacts will hamper a quantitative interpretation of the results. In this paper, we will correct for artificial intensity variations by determining the 3D point spread function (PSF) of a tomographic reconstruction based on high angle annular dark field scanning transmission electron microscopy. The large tails of the PSF cause an underestimation of the intensity of smaller particles, which in turn hampers an accurate radius estimate. Here, the error introduced by the PSF is quantified and corrected a posteriori.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 2.843
Times cited: 6
DOI: 10.1016/j.ultramic.2013.06.005
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“Smart heating profiles for the synthesis of benzene bridged periodic mesoporous organosilicas”. Smeulders G, van Oers C, Van Havenbergh K, Houthoofd K, Mertens M, Martens JA, Bals S, Maes BUW, Meynen V, Cool P, Chemical engineering journal 175, 585 (2011). http://doi.org/10.1016/j.cej.2011.09.116
Abstract: In this study the effects of the heating rate and heating time on the formation of crystal-like benzene bridged periodic mesoporous organosilicas (PMOs) are investigated. The time needed to heat up an autoclave during the hydrothermal treatment has shown to be crucial in the synthesis of PMOs, while the total duration of heating gave rise to only minor differences. By choosing a smart heating profile, superior PMO materials can be obtained in a short time. Different heating profiles in a range from one minute to one hour are adopted by microwave equipment and compared with conventional heating methods. The heating rate has a large influence on the porosity characteristics and the uniformity of the obtained particles. Moreover, two new alternative synthetic strategies to adopt the smart heating profile are presented, in order to give some possible solutions for the expensive microwave equipment.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); Laboratory of adsorption and catalysis (LADCA); Organic synthesis (ORSY)
Impact Factor: 6.216
Times cited: 7
DOI: 10.1016/j.cej.2011.09.116
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“Systematic evaluation of thermal and mechanical stability of different commercial and synthetic photocatalysts in relation to their photocatalytic activity”. Ribbens S, Beyers E, Schellens K, Mertens M, Ke X, Bals S, Van Tendeloo G, Meynen V, Cool P, Microporous and mesoporous materials: zeolites, clays, carbons and related materials 156, 62 (2012). http://doi.org/10.1016/j.micromeso.2012.01.036
Abstract: The effect of thermal treatment and mechanical stress on the structural and photocatalytic properties of eight different (synthetic and commercial) photocatalysts has been thoroughly investigated. Different mesoporous Ti-based materials were prepared via surfactant based synthesis routes (e.g. Pluronic 123, CTMABr = Cetyltrimethylammonium bromide) or via template-free synthesis routes (e.g. trititanate nanotubes). Also, the stabilizing effect of the NaOH/NH4OH post-treatment on the templated mesoporous materials and their photocatalytic activity was investigated. Furthermore, the thermal and mechanical properties of commercially available titanium dioxides such as P25 Evonik® and Millenium PC500® were studied. The various photocatalysts were analyzed with N2-sorption, X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) to obtain information concerning the specific surface area, pore volume, crystal structure, morphology, phase transitions, etc. In general, results show that the NaOH post-treatment leads to an increased control of the crystallization process during calcination resulting in a higher thermal stability, but at the same time diminishes the photocatalytic activity. Mesoporous materials in which pre-synthesized nanoparticles are used as titania source have the best mechanical stability whereas the mechanical stability of the nanotubes is the most limited. At increased temperatures and pressures, the tested commercial titanium dioxides lose their superior photocatalytic activity caused by a decreased accessibility of the active sites. The observed changes in adsorption capacities and photocatalytic activities cannot be assigned to one single phenomenon. In this respect, it shows the need to define a general/standard method to compare different photocatalysts. Furthermore, it is shown that the photocatalytic properties do not necessarily deteriorate under thermal stress, but can be improved due to crystallization, even though the initial material is (partially) destroyed. It is shown that the usefulness of a specific type of photocatalyst strongly depends on the application and the temperature/pressure to which it needs to resist.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT); Laboratory of adsorption and catalysis (LADCA)
Impact Factor: 3.615
Times cited: 8
DOI: 10.1016/j.micromeso.2012.01.036
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“The uptake of ZnO and CuO nanoparticles in the water-flea Daphnia magna under acute exposure scenarios”. Adam N, Leroux F, Knapen D, Bals S, Blust R, Environmental pollution 194, 130 (2014). http://doi.org/10.1016/j.envpol.2014.06.037
Abstract: In this study the uptake of ZnO and CuO nanoparticles by Daphnia magna was tested. Daphnids were exposed during 48 h to acute concentrations of the nanoparticles and corresponding metal salts. The Daphnia zinc and copper concentration was measured and the nanoparticles were localized using electron microscopy. The aggregation and dissolution in the medium was characterized. A fast dissolution of ZnO in the medium was observed, while most CuO formed large aggregates and only a small fraction dissolved. The Daphnia zinc concentration was comparable for the nanoparticles and salts. Contrarily, a much higher Daphnia copper concentration was observed in the CuO exposure, compared to the copper salt. CuO nanoparticles adsorbed onto the carapace and occurred in the gut but did not internalize in the tissues. The combined dissolution and uptake results indicate that the toxicity of both nanoparticle types was caused by metal ions dissolved from the particles in the medium.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); Veterinary physiology and biochemistry
Impact Factor: 5.099
Times cited: 45
DOI: 10.1016/j.envpol.2014.06.037
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“Zeolite \beta nanoparticles based bimodal structures : mechanism and tuning of the porosity and zeolitic properties”. van Oers CJ, Kurttepeli M, Mertens M, Bals S, Meynen V, Cool P, Microporous and mesoporous materials: zeolites, clays, carbons and related materials 185, 204 (2014). http://doi.org/10.1016/j.micromeso.2013.11.021
Abstract: Despite great efforts in the research area of zeolite nanoparticles and their use in the synthesis of bimodal materials, still little is known about the impact of the synthesis conditions of the zeolite nanoparticles on its own characteristics, and on the properties and the formation mechanism of the final bimodal materials. A zeolite β nanoparticles solution is applied in a mesotemplate-free synthesis method, and the influence of the hydrothermal ageing temperature of the nanoparticles solution on both the zeolitic and porosity characteristics of the final bimodal material has been studied. Transmission electron microscopy in combination with 3-dimensional reconstructions obtained by electron tomography revealed that the zeolite β nanoparticles are connected by neck-like structures, thus creating a wormhole-like mesoporous material. Considering the zeolitic properties, a clear threshold is observed in the synthesis temperature series at 413 K. Below and at this threshold, the biporous materials show no apparent zeolitic characteristics, although these materials exhibit a more condensed and uniform SiOSi network in comparison to Al-MCF. Synthesis temperatures above the threshold lead to bimodal structures with defined zeolitic properties. Moreover, the dimensions of the nanoparticles are studied by TEM, revealing an increasing particle size with increasing temperature under the threshold of 413 K, which is in agreement with a sol-mechanism. This mechanism is disturbed after the threshold due to the start of the crystallisation process.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT); Laboratory of adsorption and catalysis (LADCA)
Impact Factor: 3.615
Times cited: 10
DOI: 10.1016/j.micromeso.2013.11.021
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“Preparation and study of 2-D semiconductors with Dirac type bands due to the honeycomb nanogeometry”. Kalesaki E, Boneschanscher MP, Geuchies JJ, Delerue C, Morais Smith C, Evers WH, Allan G, Altantzis T, Bals S, Vanmaekelbergh D, Proceedings of the Society of Photo-optical Instrumentation Engineers
T2 –, Proceedings of SPIE 8981, 898107 (2014). http://doi.org/10.1117/12.2042882
Abstract: The interest in 2-dimensional systems with a honeycomb lattice and related Dirac-type electronic bands has exceeded the prototype graphene1. Currently, 2-dimensional atomic2,3 and nanoscale4-8 systems are extensively investigated in the search for materials with novel electronic properties that can be tailored by geometry. The immediate question that arises is how to fabricate 2-D semiconductors that have a honeycomb nanogeometry, and as a consequence of that, display a Dirac-type band structure? Here, we show that atomically coherent honeycomb superlattices of rocksalt (PbSe, PbTe) and zincblende (CdSe, CdTe) semiconductors can be obtained by nanocrystal self-assembly and facet-to-facet atomic bonding, and subsequent cation exchange. We present a extended structural analysis of atomically coherent 2-D honeycomb structures that were recently obtained with self-assembly and facet-to-facet bonding9. We show that this process may in principle lead to three different types of honeycomb structures, one with a graphene type-, and two others with a silicene-type structure. Using TEM, electron diffraction, STM and GISAXS it is convincingly shown that the structures are from the silicene-type. In the second part of this work, we describe the electronic structure of graphene-type and silicene type honeycomb semiconductors. We present the results of advanced electronic structure calculations using the sp3d5s* atomistic tight-binding method10. For simplicity, we focus on semiconductors with a simple and single conduction band for the native bulk semiconductor. When the 3-D geometry is changed into 2-D honeycomb, a conduction band structure transformation to two types of Dirac cones, one for S- and one for P-orbitals, is observed. The width of the bands depends on the honeycomb period and the coupling between the nanocrystals. Furthermore, there is a dispersionless P-orbital band, which also forms a landmark of the honeycomb structure. The effects of considerable intrinsic spin-orbit coupling are briefly considered. For heavy-element compounds such as CdTe, strong intrinsic spin-‐orbit coupling opens a non-trivial gap at the P-orbital Dirac point, leading to a quantum Spin Hall effect10-12. Our work shows that well known semiconductor crystals, known for centuries, can lead to systems with entirely new electronic properties, by the simple action of nanogeometry. It can be foreseen that such structures will play a key role in future opto-electronic applications, provided that they can be fabricated in a straightforward way.
Keywords: P1 Proceeding; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Times cited: 2
DOI: 10.1117/12.2042882
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“An alternative approach for \zeta-factor measurement using pure element nanoparticles”. Zanaga D, Altantzis T, Sanctorum J, Freitag B, Bals S, Ultramicroscopy 164, 11 (2016). http://doi.org/10.1016/J.ULTRAMIC.2016.03.002
Abstract: It is very challenging to measure the chemical composition of hetero nanostructures in a reliable and quantitative manner. Here, we propose a novel and straightforward approach that can be used to quantify energy dispersive X-ray spectra acquired in a transmission electron microscope. Our method is based on a combination of electron tomography and the so-called zeta-factor technique. We will demonstrate the reliability of our approach as well as its applicability by investigating Au-Ag and Au-Pt hetero nanostructures. Given its simplicity, we expect that the method could become a new standard in the field of chemical characterization using electron microscopy. (C) 2016 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 2.843
Times cited: 19
DOI: 10.1016/J.ULTRAMIC.2016.03.002
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