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“Heterogeneous Pt-catalyzed transfer dehydrogenation of long-chain alkanes with ethylene”. de la Croix T, Claes N, Eyley S, Thielemans W, Bals S, De Vos D, Catalysis Science &, Technology (2023). http://doi.org/10.1039/D3CY00370A
Abstract: The dehydrogenation of long-chain alkanes to olefins and alkylaromatics is a challenging endothermic reaction, typically requiring harsh conditions which can lead to low selectivity and coking. More favorable thermodynamics can be achieved by using a hydrogen acceptor, such as ethylene. In this work, the potential of heterogeneous platinum catalysts for the transfer dehydrogenation of long-chain alkanes is investigated, using ethylene as a convenient hydrogen acceptor. Pt/C and Pt–Sn/C catalysts were prepared<italic>via</italic>a simple polyol method and characterized with CO pulse chemisorption, HAADF-STEM, and EDX measurements. Conversion of ethylene was monitored<italic>via</italic>gas-phase FTIR, and distribution of liquid products was analyzed<italic>via</italic>GC-FID, GC-MS, and 1H-NMR. Compared to unpromoted Pt/C, Sn-promoted catalysts show lower initial reaction rates, but better resistance to catalyst deactivation, while increasing selectivity towards alkylaromatics. Both reaction products and ethylene were found to inhibit the reaction significantly. At 250 °C for 22 h, TON up to 28 and 86 mol per mol Pt were obtained for Pt/C and PtSn<sub>2</sub>/C, respectively, with olefin selectivities of 94% and 53%. The remaining products were mainly unbranched alkylaromatics. These findings show the potential of simple heterogeneous catalysts in alkane transfer dehydrogenation, for the preparation of valuable olefins and alkylaromatics, or as an essential step in various tandem reactions.
Keywords: A1 Journal Article; Electron Microscopy for Materials Science (EMAT) ;
Impact Factor: 5
DOI: 10.1039/D3CY00370A
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“Catalyst design by NH4OH treatment of USY zeolite”. Van Aelst J, Verboekend D, Philippaerts A, Nuttens N, Kurttepeli M, Gobechiya E, Haouas M, Sree SP, Denayer JFM, Martens JA, Kirschhock CEA, Taulelle F, Bals S, Baron GV, Jacobs PA, Sels BF, Advanced functional materials 25, 7130 (2015). http://doi.org/10.1002/adfm.201502772
Abstract: Hierarchical zeolites are a class of superior catalysts which couples the intrinsic zeolitic properties to enhanced accessibility and intracrystalline mass transport to and from the active sites. The design of hierarchical USY (Ultra-Stable Y) catalysts is achieved using a sustainable postsynthetic room temperature treatment with mildly alkaline NH4OH ( 0.02(M)) solutions. Starting from a commercial dealuminated USY zeolite (Si/Al = 47), a hierarchical material is obtained by selective and tuneable creation of interconnected and accessible small mesopores (2- 6 nm). In addition, the treatment immediately yields the NH4+ form without the need for additional ion exchange. After NH4OH modification, the crystal morphology is retained, whereas the microporosity and relative crystallinity are decreased. The gradual formation of dense amorphous phases throughout the crystal without significant framework atom leaching rationalizes the very high material yields (>90%). The superior catalytic performance of the developed hierarchical zeolites is demonstrated in the acid-catalyzed isomerization of alpha-pinene and the metal-catalyzed conjugation of safflower oil. Significant improvements in activity and selectivity are attained, as well as a lowered susceptibility to deactivation. The catalytic performance is intimately related to the introduced mesopores, hence enhanced mass transport capacity, and the retained intrinsic zeolitic properties.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 12.124
Times cited: 64
DOI: 10.1002/adfm.201502772
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“Designing diameter-modulated heterostructure nanowires of PbTe/Te by controlled dewetting”. Kumar A, Kundu S, Samantaray D, Kundu P, Zanaga D, Bals S, Ravishankar N, Nano letters 17, 7226 (2017). http://doi.org/10.1021/ACS.NANOLETT.7B02442
Abstract: <script type='text/javascript'>document.write(unpmarked('Heterostructures consisting of semiconductors with controlled morphology and interfaces find applications in many fields. A range of axial, radial, and diameter-modulated nanostructures have been synthesized primarily using vapor phase methods. Here, we present a simple wet chemical routine to synthesize heterostructures of PbTe/Te using Te nanowires as templates. A morphology evolution study for the formation of these heterostructures has been performed. On the basis of these control experiments, a pathway for the formation of these nanostructures is proposed. Reduction of a Pb precursor to Pb on Te nanowire templates followed by interdiffusion of Pb/Te leads to the formation of a thin shell of PbTe on the Te wires. Controlled dewetting of the thin shell leads to the formation of cube-shaped PbTe that is periodically arranged on the Te wires. Using control experiments, we show that different reactions parameters like rate of addition of the reducing agent, concentration of Pb precursor and thickness of initial Te nanowire play a critical role in controlling the spacing between the PbTe cubes on the Te wires. Using simple surface energy arguments, we propose a mechanism for the formation of the hybrid. The principles presented are general and can be exploited for the synthesis of other nanoscale heterostructures.'));
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 12.712
Times cited: 11
DOI: 10.1021/ACS.NANOLETT.7B02442
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“Deciphering the role of water in promoting the optoelectronic performance of surface-engineered lead halide perovskite nanocrystals”. Bhatia H, Martin C, Keshavarz M, Dovgaliuk I, Schrenker NJ, Ottesen M, Qiu W, Fron E, Bremholm M, Van de Vondel J, Bals S, Roeffaers MBJ, Hofkens J, Debroye E, ACS applied materials and interfaces 15, 7294 (2023). http://doi.org/10.1021/ACSAMI.2C20605
Abstract: Lead halide perovskites are promising candidates for applicability is limited by their structural instability toward moisture. Although a deliberate addition of water to the precursor solution has recently been shown to improve the crystallinity and optical properties of perovskites, the corresponding thin films still do not exhibit a near-unity quantum yield. Herein, we report that the direct addition of a minute amount of water to post-treated substantially enhances the stability while achieving a 95% photoluminescence quantum yield in a NC thin film. We unveil the mechanism of how moisture assists in the formation of an additional NH4Br component. Alongside, we demonstrate the crucial role of moisture in assisting localized etching of the perovskite crystal, facilitating the partial incorporation of NH4+, which is key for improved performance under ambient conditions. Finally, as a proof-of-concept, the application of post-treated and watertreated perovskites is tested in LEDs, with the latter exhibiting a superior performance, offering opportunities toward commercial application in moisture-stable optoelectronics.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 9.5
Times cited: 3
DOI: 10.1021/ACSAMI.2C20605
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“PdPb-catalyzed decarboxylation of proline to pyrrolidine : highly selective formation of a biobased amine in water”. Verduyckt J, Van Hoof M, De Schouwer F, Wolberg M, Kurttepeli M, Eloy P, Gaigneaux EM, Bals S, Kirschhock CEA, De Vos DE, ACS catalysis 6, 7303 (2016). http://doi.org/10.1021/ACSCATAL.6B02561
Abstract: Amino acids have huge potential as platform chemicals in the biobased industry. Pd-catalyzed decarboxylation is a very promising route for the valorization of these natural compounds derived from protein waste or fermentation. We report that the highly abundant and nonessential amino acid L-proline is very reactive in the Pd-catalyzed decarboxylation. Full conversions are obtained with Pd/C and different Pd/MeOx catalysts; this allowed the identification of the different side reactions and the mapping of the reaction network. Due to the high reactivity of pyrrolidine, the selectivity for pyrrolidine was initially low. By carefully modifying Pd/ZrO2 with Pb in a controlled manner-via two incipient wetness impregnation steps-the selectivity increased remarkably. Finally, a thorough investigation of the reaction parameters resulted in an increased activity of this modified catalyst and an even further enhanced selectivity under a low H-2 pressure of 4 bar at 235 degrees C in water. This results in a very selective and sustainable production route for the highly interesting pyrrolidine.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 10.614
Times cited: 27
DOI: 10.1021/ACSCATAL.6B02561
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“Direct Observation of Luminescent Silver Clusters Confined in Faujasite Zeolites”. Altantzis T, Coutino-Gonzalez E, Baekelant W, Martinez GT, Abakumov AM, Van Tendeloo G, Roeffaers MBJ, Bals S, Hofkens J, ACS nano 10, 7604 (2016). http://doi.org/10.1021/acsnano.6b02834
Abstract: One of the ultimate goals in the study of metal clusters is the correlation between the atomic-scale organization and their physicochemical properties. However, direct observation of the atomic organization of such minuscule metal clusters is heavily hindered by radiation damage imposed by the different characterization techniques. We present direct evidence of the structural arrangement, at an atomic level, of luminescent silver species stabilized in faujasite (FAU) zeolites using aberration-corrected scanning transmission electron microscopy. Two different silver clusters were identified in Ag-FAU zeolites, a trinuclear silver species associated with green emission and a tetranuclear silver species related to yellow emission. By combining direct imaging with complementary information obtained from X-ray powder diffraction and Rietveld analysis, we were able to elucidate the main differences at an atomic scale between luminescent (heat-treated) and nonluminescent (cation-exchanged) Ag-FAU zeolites. It is expected that such insights will trigger the directed synthesis of functional metal nanocluster-zeolite composites with tailored luminescent properties.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 13.942
Times cited: 57
DOI: 10.1021/acsnano.6b02834
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“Gold and silver-catalyzed reductive amination of aromatic carboxylic acids to benzylic amines”. Coeck R, Meeprasert J, Li G, Altantzis T, Bals S, Pidko EA, De Vos DE, Acs Catalysis 11, 7672 (2021). http://doi.org/10.1021/ACSCATAL.1C01693
Abstract: The reductive amination of benzoic acid and its derivatives would be an effective addition to current synthesis methods for benzylamine. However, with current technology it is very difficult to keep the aromaticity intact when starting from benzoic acid, and salt wastes are often generated in the process. Here, we report a heterogeneous catalytic system for such a reductive amination, requiring solely H-2 and NH3 as the reactants. The Ag/TiO2 or Au/TiO2 catalysts can be used multiple times, and very little noble metal is required, only 0.025 mol % Au. The catalysts are bifunctional: the support catalyzes the dehydration of both the ammonium carboxylate to the amide and of the amide to the nitrile, while the sites at the metal-support interface promote the hydrogenation of the in situ generated nitrile. Yields of up to 92% benzylamine were obtained.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT); Applied Electrochemistry & Catalysis (ELCAT)
Impact Factor: 10.614
Times cited: 16
DOI: 10.1021/ACSCATAL.1C01693
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“Use of nanoscale carbon layers on Ag-based gas diffusion electrodes to promote CO production”. Pacquets L, Van den Hoek J, Arenas Esteban D, Ciocarlan R-G, Cool P, Baert K, Hauffman T, Daems N, Bals S, Breugelmans T, ACS applied nano materials 5, 7723 (2022). http://doi.org/10.1021/ACSANM.2C00473
Abstract: A promising strategy for the inhibition of the hydrogen evolution reaction along with the stabilization of the electrocatalyst in electrochemical CO2 reduction cells involves the application of a nanoscale amorphous carbon layer on top of the active catalyst layer in a gas diffusion electrode. Without modifying the chemical nature of the electrocatalyst itself, these amorphous carbon layers lead to the stabilization of the electrocatalyst, and a significant improvement with respect to the inhibition of the hydrogen evolution reaction was also obtained. The faradaic efficiencies of hydrogen could be reduced from 31.4 to 2.1% after 1 h of electrolysis with a 5 nm thick carbon layer. Furthermore, the impact of the carbon layer thickness (5–30 nm) on this inhibiting effect was investigated. We determined an optimal thickness of 15 nm where the hydrogen evolution reaction was inhibited and a decent stability was obtained. Next, a thickness of 15 nm was selected for durability measurements. Interestingly, these durability measurements revealed the beneficial impact of the carbon layer already after 6 h by suppressing the hydrogen evolution such that an increase of only 37.9% exists compared to 56.9% without the use of an additional carbon layer, which is an improvement of 150%. Since carbon is only applied afterward, it reveals its great potential in terms of electrocatalysis in general.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT); Laboratory of adsorption and catalysis (LADCA); Applied Electrochemistry & Catalysis (ELCAT)
Impact Factor: 5.9
Times cited: 3
DOI: 10.1021/ACSANM.2C00473
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“Tailoring ZnSe-CdSe colloidal quantum dots via cation exchange : from core/shell to alloy nanocrystals”. Groeneveld E, Witteman L, Lefferts M, Ke X, Bals S, Van Tendeloo G, de Mello Donega C, ACS nano 7, 7913 (2013). http://doi.org/10.1021/nn402931y
Abstract: We report a study of Zn2+ by Cd2+ cation exchange (CE) in colloidal ZnSe nanocrystals (NCs). Our results reveal that CE in ZnSe NCs is a thermally activated isotropic process. The CE efficiency (i.e., fraction of Cd2+ ions originally in solution, Cdsol, that is incorporated in the ZnSe NC) increases with temperature and depends also on the Cdsol/ZnSe ratio. Interestingly, the reaction temperature can be used as a sensitive parameter to tailor both the composition and the elemental distribution profile of the product (Zn,Cd)Se NCs. At 150 °C ZnSe/CdSe core/shell hetero-NCs (HNCs) are obtained, while higher temperatures (200 and 220 °C) produce (Zn1xCdx)Se gradient alloy NCs, with increasingly smoother gradients as the temperature increases, until homogeneous alloy NCs are obtained at T ≥ 240 °C. Remarkably, sequential heating (150 °C followed by 220 °C) leads to ZnSe/CdSe core/shell HNCs with thicker shells, rather than (Zn1xCdx)Se gradient alloy NCs. Thermal treatment at 250 °C converts the ZnSe/CdSe core/shell HNCs into (Zn1xCdx)Se homogeneous alloy NCs, while preserving the NC shape. A mechanism for the cation exchange in ZnSe NCs is proposed, in which fast CE takes place at the NC surface, and is followed by relatively slower thermally activated solid-state cation diffusion, which is mediated by Frenkel defects. The findings presented here demonstrate that cation exchange in colloidal ZnSe NCs provides a very sensitive tool to tailor the nature and localization regime of the electron and hole wave functions and the optoelectronic properties of colloidal ZnSeCdSe NCs.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 13.942
Times cited: 153
DOI: 10.1021/nn402931y
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“Engineering Structural Diversity in Gold Nanocrystals by Ligand-Mediated Interface Control”. Wang Y, Sentosun K, Li A, Coronado-Puchau M, Sánchez-Iglesias A, Li S, Su X, Bals S, Liz-Marzán LM, Chemistry of materials 27, 8032 (2015). http://doi.org/10.1021/acs.chemmater.5b03600
Abstract: Surface and interface control is fundamentally important for crystal growth engineering, catalysis, surface enhanced spectroscopies, and self-assembly, among other processes and applications. Understanding the role of ligands in regulating surface properties of plasmonic metal nanocrystals during growth has received considerable attention. However, the underlying mechanisms and the diverse functionalities of ligands are yet to be fully addressed. In this contribution,
we report a systematic study of ligand-mediated interface control in seeded growth of gold nanocrystals, leading to diverse and exotic nanostructures with an improved surface enhanced Raman scattering (SERS) activity. Three dimensional transmission electron microscopy (3D TEM) revealed an intriguing gold shell growth process mediated by the bifunctional ligand 1,4-benzenedithiol (BDT), which leads to a unique crystal growth mechanism as compared to other ligands, and subsequently to the concept of interfacial energy control mechanism. Volmer-Weber growth mode was proposed to be responsible for BDT-mediated seeded growth, favoring the strongest interfacial energy and generating an asymmetric island growth pathway with internal crevices/gaps. This additionally favors incorporation of BDT at the plasmonic nanogaps, thereby generating strong SERS activity with a maximum efficiency for a core-semishell configuration obtained along seeded growth. Numerical modeling was used to explain this observation. Interestingly, the same strategy can be used to engineer the structural diversity of this system, by using gold nanoparticle seeds with various sizes and shapes, and varying the [Au3+]/[Au0] ratio. This rendered a series of diverse and exotic plasmonic nanohybrids such as semishell-coated gold nanorods, with embedded Raman-active tags and Janus surface with distinct surface functionalities.
These would greatly enrich the plasmonic nanostructure toolbox for various studies and applications such as anisotropic nanocrystal engineering, SERS, and high-resolution Raman bioimaging or nanoantenna devices.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 9.466
Times cited: 18
DOI: 10.1021/acs.chemmater.5b03600
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“Heterogeneous TiO2/V2O5/Carbon Nanotube Electrodes for Lithium-Ion Batteries”. Kurttepeli M, Deng S, Mattelaer F, Cott DJ, Vereecken P, Dendooven J, Detavernier C, Bals S, ACS applied materials and interfaces 9, 8055 (2017). http://doi.org/10.1021/acsami.6b12759
Abstract: Vanadium pentoxide (V2O5) is proposed and investigated as a cathode material for lithium-ion (Li-ion) batteries. However, the dissolution of V2O5 during the charge/discharge remains as an issue at the V2O5–electrolyte interface. In this work, we present a heterogeneous nanostructure with carbon nanotubes supported V2O5/titanium dioxide (TiO2) multilayers as electrodes for thin-film Li-ion batteries. Atomic layer deposition of V2O5 on carbon nanotubes provides enhanced Li storage capacity and high rate performance. An additional TiO2 layer leads to increased morphological stability and in return higher electrochemical cycling performance of V2O5/carbon nanotubes. The physical and chemical properties of TiO2/V2O5/carbon nanotubes are characterized by cyclic voltammetry and charge/discharge measurements as well as electron microscopy. The detailed mechanism of the protective TiO2 layer to improve the electrochemical cycling stability of the V2O5 is unveiled.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 7.504
Times cited: 28
DOI: 10.1021/acsami.6b12759
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“Femtosecond Laser-Controlled Tip-to-Tip Assembly and Welding of Gold Nanorods”. Gonzalez-Rubio G, Gonzalez-Izquierdo J, Banares L, Tardajos G, Rivera A, Altantzis T, Bals S, Pena-Rodriguez O, Guerrero-Martinez A, Liz-Marzan LM, Nano letters 15, 8282 (2015). http://doi.org/10.1021/acs.nanolett.5b03844
Abstract: Directed assembly of gold nanorods through the use of dithiolated molecular linkers is one of the most efficient methodologies for the morphologically controlled tip-to-tip assembly of this type of anisotropic nanocrystals. However, in a direct analogy to molecular polymerization synthesis, this process is characterized by difficulties in chain-growth control over nanoparticle oligomers. In particular, it is nearly impossible to favor the formation of one type of oligomer, making the methodology hard to use for actual applications in nanoplasmonics. We propose here a light-controlled synthetic procedure that allows obtaining selected plasmonic oligomers in high yield and with reaction times in the scale of minutes by irradiation with low fluence near-infrared (NIR) femtosecond laser pulses. Selective inhibition of the formation of gold nanorod n-mers (trimers) with a longitudinal localized surface plasmon in resonance with a 800 nm Ti:sapphire laser, allowed efficient trapping of the (n – 1)-mers (dimers) by hot spot mediated photothermal decomposition of the interparticle molecular linkers. Laser irradiation at higher energies produced near-field enhancement at the interparticle gaps, which is large enough to melt gold nanorod tips, offering a new pathway toward tip-to-tip welding of gold nanorod oligomers with a plasmonic response at the NIR. Thorough optical and electron microscopy characterization indicates that plasmonic oligomers can be selectively trapped and welded, which has been analyzed in terms of a model that predicts with reasonable accuracy the relative concentrations of the main plasmonic species.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 12.712
Times cited: 101
DOI: 10.1021/acs.nanolett.5b03844
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“A combined 3D and 2D light scattering study on aqueous colloidal model systems with tunable interactions”. Liu Y, Claes N, Trepka B, Bals S, Lang PR, Soft matter 12, 8485 (2016). http://doi.org/10.1039/c6sm01376g
Abstract: In this article we report on the synthesis and characterization of a system of colloidal spheres suspended in an aqueous solvent which can be refractive index-matched, thus allowing for investigations of the particle near-wall dynamics by evanescent wave dynamic light scattering at concentrations up to the isotropic to ordered transition and beyond. The particles are synthesized by copolymerization of a fluorinated acrylic ester monomer with a polyethylene-glycol (PEG) oligomer by surfactant free emulsion polymerization. Static and dynamic light scattering experiments in combination with cryo transmission electron microscopy reveal that the particles have a core shell structure with a significant enrichment of the PEG chains on the particles surface. In index-matching DMSO/water suspensions the particles arrange in an ordered phase at volume fraction above 7%, if no additional electrolyte is present. The near-wall dynamics at low volume fraction are quantitatively described by the combination of electrostatic repulsion and hydrodynamic interaction between the particles and the wall. At volume fractions close to the isotropic to ordered transition, the near-wall dynamics are more complex and qualitatively reminiscent of the behaviour which was observed in hard sphere suspensions at high concentrations.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 3.889
Times cited: 2
DOI: 10.1039/c6sm01376g
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“Governing the morphology of PtAu heteronanocrystals with improved electrocatalytic performance”. Mourdikoudis S, Chirea M, Zanaga D, Altantzis T, Mitrakas M, Bals S, Marzán LM, Pérez-Juste J, Pastoriza-Santos I, Nanoscale 7, 8739 (2015). http://doi.org/10.1039/C4NR07481E
Abstract: Platinumgold heteronanostructures comprising either dimer (PtAu) or coresatellite (Pt@Au) configurations were synthesized by means of a seeded growth procedure using platinum nanodendrites as seeds. Careful control of the reduction kinetics of the gold precursor can be used to direct the nucleation and growth of gold nanoparticles on either one or multiple surface sites simultaneously, leading to the formation of either dimers or coresatellite nanoparticles, respectively, in high yields. Characterization by electron tomography and high resolution electron microscopy provided a better understanding of the actual three-dimensional particle morphology, as well as the AuPt interface, revealing quasi-epitaxial growth of Au on Pt. The prepared PtAu bimetallic nanostructures are highly efficient catalysts for ethanol oxidation in alkaline solution, showing accurate selectivity, high sensitivity, and improved efficiency by generating higher current densities than their monometallic counterparts.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 7.367
Times cited: 41
DOI: 10.1039/C4NR07481E
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“Three-dimensional atomic models from a single projection using Z-contrast imaging: verification by electron tomography and opportunities”. De Backer A, Jones L, Lobato I, Altantzis T, Goris B, Nellist PD, Bals S, Van Aert S, Nanoscale 9, 8791 (2017). http://doi.org/10.1039/C7NR02656K
Abstract: In order to fully exploit structure–property relations of nanomaterials, three-dimensional (3D) characterization at the atomic scale is often required. In recent years, the resolution of electron tomography has reached the atomic scale. However, such tomography typically requires several projection images demanding substantial electron dose. A newly developed alternative circumvents this by counting the number of atoms across a single projection. These atom counts can be used to create an initial atomic model with which an energy minimization can be applied to obtain a relaxed 3D reconstruction of the nanoparticle. Here, we compare, at the atomic scale, this single projection reconstruction approach with tomography and find an excellent agreement. This new approach allows for the characterization of beam-sensitive materials or where the acquisition of a tilt series is impossible. As an example, the utility is illustrated by the 3D atomic scale characterization of a nanodumbbell on an in situ heating holder of limited tilt range.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 7.367
Times cited: 33
DOI: 10.1039/C7NR02656K
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“Homogeneous Protein Analysis by Magnetic Core-Shell Nanorod Probes”. Schrittwieser S, Pelaz B, Parak WJ, Lentijo-Mozo S, Soulantica K, Dieckhoff J, Ludwig F, Altantzis T, Bals S, Schotter J, ACS applied materials and interfaces 8, 8893 (2016). http://doi.org/10.1021/acsami.5b11925
Abstract: Studying protein interactions is of vital importance both to fundamental biology research and to medical applications. Here, we report on the experimental proof of a universally applicable label-free homogeneous platform for rapid protein analysis. It is based on optically detecting changes in the rotational dynamics of magnetically agitated core-shell nanorods upon their specific interaction with proteins. By adjusting the excitation frequency, we are able to optimize the measurement signal for each analyte protein size. In addition, due to the locking of the optical signal to the magnetic excitation frequency, background signals are suppressed, thus allowing exclusive studies of processes at the nanoprobe surface only. We study target proteins (soluble domain of the human epidermal growth factor receptor 2 – sHER2) specifically binding to antibodies (trastuzumab) immobilized on the surface of our nanoprobes and demonstrate direct deduction of their respective sizes. Additionally, we examine the dependence of our measurement signal on the concentration of the analyte protein, and deduce a minimally detectable sHER2 concentration of 440 pM. For our homogeneous measurement platform, good dispersion stability of the applied nanoprobes under physiological conditions is of vital importance. To that end, we support our measurement data by theoretical modeling of the total particle-particle interaction energies. The successful implementation of our platform offers scope for applications in biomarker-based diagnostics as well as for answering basic biology questions.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 7.504
Times cited: 16
DOI: 10.1021/acsami.5b11925
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“Composite Supraparticles with Tunable Light Emission”. Montanarella F, Altantzis T, Zanaga D, Rabouw FT, Bals S, Baesjou P, Vanmaekelbergh D, van Blaaderen A, ACS nano 11, 9136 (2017). http://doi.org/10.1021/acsnano.7b03975
Abstract: Robust luminophores emitting light with broadly tunable colors are desirable in many applications such as light-emitting diode (LED)-based lighting, displays, integrated optoelectronics and biology. Nanocrystalline quantum dots with multicolor emission, from core- and shell-localized excitons, as well as solid layers of mixed quantum dots that emit different colors have been proposed. Here, we report on colloidal supraparticles that are composed of three types of Cd(Se,ZnS) core/(Cd,Zn)S shell nanocrystals with emission in the red, green, and blue. The emission of the supraparticles can be varied from pure to composite colors over the entire visible region and finetuned into variable shades of white light by mixing the nanocrystals in controlled proportions. Our approach results in supraparticles with sizes spanning the colloidal domain and beyond that combine versatility and processability with a broad, stable, and tunable emission, promising applications in lighting devices and biological research.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 13.942
Times cited: 36
DOI: 10.1021/acsnano.7b03975
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“Shape control beyond the seeds in gold nanoparticles”. Li W, Tong W, Yadav A, Bladt E, Bals S, Funston AM, Etheridge J, Chemistry Of Materials 33, 9152 (2021). http://doi.org/10.1021/ACS.CHEMMATER.1C02459
Abstract: In typical seed-mediated syntheses of metal nanocrystals, the shape of the nanocrystal is determined largely by the seed nucleation environment and subsequent growth environment (where “environment” refers to the chemical environment, including the surfactant and additives). In this approach, crystallinity is typically determined by the seeds, and surfaces are controlled by the environment(s). However, surface energies, and crystallinity, are both influenced by the choice of environment(s). This limits the permutations of crystallinity and surface facets that can be mixed and matched to generate new nanocrystal morphologies. Here, we control post-seed growth to deliberately incorporate twin planes during the growth stage to deliver new final morphologies, including twinned cubes and bipyramids from single-crystal seeds. The nature and number of twin planes, together with surfactant control of facet growth, define the final nanoparticle morphology. Moreover, by breaking symmetry, the twin planes introduce new facet orientations. This additional mechanism opens new routes for the synthesis of different morphologies and facet orientations.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 9.466
Times cited: 3
DOI: 10.1021/ACS.CHEMMATER.1C02459
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“A titanium(IV)-based metal-organic framework featuring defect-rich Ti-O sheets as an oxidative desulfurization catalyst”. Smolders S, Willhammar T, Krajnc A, Şentosun K, Wharmby MT, Lomachenko KA, Bals S, Mali G, Roeffaers MBJ, De Vos DE, Bueken B, Angewandte Chemie: international edition in English 58, 9160 (2019). http://doi.org/10.1002/ANIE.201904347
Abstract: While titanium-based metal-organic frameworks (MOFs) have been widely studied for their (photo) catalytic potential, only a few Ti-IV MOFs have been reported owing to the high reactivity of the employed titanium precursors. The synthesis of COK-47 is now presented, the first Ti carboxylate MOF based on sheets of (TiO6)-O-IV octahedra, which can be synthesized with a range of different linkers. COK-47 can be synthesized as an inherently defective nanoparticulate material, rendering it a highly efficient catalyst for the oxidation of thiophenes. Its structure was determined by continuous rotation electron diffraction and studied in depth by X-ray total scattering, EXAFS, and solid-state NMR. Furthermore, its photoactivity was investigated by electron paramagnetic resonance and demonstrated by catalytic photodegradation of rhodamine 6G.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 11.994
Times cited: 97
DOI: 10.1002/ANIE.201904347
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“Plasmonic Au@Pd Nanorods with Boosted Refractive Index Susceptibility and SERS Efficiency: A Multifunctional Platform for Hydrogen Sensing and Monitoring of Catalytic Reactions”. Rodal-Cedeira S, Montes-García V, Polavarapu L, Solís DM, Heidari H, La Porta A, Angiola M, Martucci A, Taboada JM, Obelleiro F, Bals S, Pérez-Juste J, Pastoriza-Santos I, Chemistry of materials 28, 9169 (2016). http://doi.org/10.1021/acs.chemmater.6b04941
Abstract: Palladium nanoparticles (NPs) have received tremendous attention over the years due to their high catalytic activity for various chemical reactions. However, unlike other noble metal nanoparticles such as Au and Ag NPs, they exhibit poor plasmonic properties with broad extinction spectra and less scattering efficiency, and thus limiting their applications in the field of plasmonics. Therefore, it has been challenging to integrate tunable and strong plasmonic properties into catalytic Pd nanoparticles. Here we show that plasmonic Au@Pd nanorods (NRs) with relatively narrow and remarkably tunable optical responses in the NIR region can be obtained by directional growth of Pd on penta-twinned Au NR seeds. We found the presence of bromide ions facilitates the stabilization of facets for the directional growth of Pd shell to obtain Au@Pd nanorods (NR) with controlled length scales. Interestingly, it turns out the Au NR supported Pd NRs exhibit much narrow extinction compared to pure Pd NRs, which makes them suitable for plasmonic sensing applications. Moreover, these nanostructures display, to the best of our knowledge, one of the highest ensemble refractive index sensitivity values reported to date (1067 nm per refractive index unit, RIU). Additionally, we showed the application of such plasmonic Au@Pd NRs for localized surface plasmon resonance (LSPR)-based sensing of hydrogen both in solution as well as on substrate. Finally, we demonstrate the integration of excellent plasmonic properties in catalytic palladium enables the in situ monitoring of a reaction progress by surface-enhanced Raman scattering. We postulate the proposed approach to boost the plasmonic properties of Pd nanoparticles will ignite the design of complex shaped plasmonic Pd NPs to be used in various plasmonic applications such as sensing and in situ monitoring of various chemical reactions.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 9.466
Times cited: 80
DOI: 10.1021/acs.chemmater.6b04941
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“Characterization of silver-polymer core–shell nanoparticles using electron microscopy”. Claes N, Asapu R, Blommaerts N, Verbruggen SW, Lenaerts S, Bals S, Nanoscale 10, 9186 (2018). http://doi.org/10.1039/C7NR09517A
Abstract: Silver-polymer core–shell nanoparticles show interesting optical properties, making them widely applicable in the field of plasmonics. The uniformity, thickness and homogeneity of the polymer shell will affect the properties of the system which makes a thorough structural characterization of these core–shell silver-polymer nanoparticles of great importance. However, visualizing the shell and the particle simultaneously is far from straightforward due to the sensitivity of the polymer shell towards the electron beam. In this study, we use different 2D and 3D electron microscopy techniques to investigate different structural aspects of the polymer coating.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT); Sustainable Energy, Air and Water Technology (DuEL)
Impact Factor: 7.367
Times cited: 11
DOI: 10.1039/C7NR09517A
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“Atomic-scale detection of individual lead clusters confined in Linde Type A zeolites”. Fatermans J, Romolini G, Altantzis T, Hofkens J, Roeffaers MBJ, Bals S, Van Aert S, Nanoscale (2022). http://doi.org/10.1039/D2NR01819E
Abstract: Structural analysis of metal clusters confined in nanoporous materials is typically performed by X-ray-driven techniques. Although X-ray analysis has proved its strength in the characterization of metal clusters, it provides averaged structural information. Therefore, we here present an alternative workflow for bringing the characterization of confined metal clusters towards the local scale. This workflow is based on the combination of aberration-corrected transmission electron microscopy (TEM), TEM image simulations, and powder X-ray diffraction (XRD) with advanced statistical techniques. In this manner, we were able to characterize the clustering of Pb atoms in Linde Type A (LTA) zeolites with Pb loadings as low as 5 wt%. Moreover, individual Pb clusters could be directly detected. The proposed methodology thus enables a local-scale characterization of confined metal clusters in zeolites. This is important for further elucidation of the connection between the structure and the physicochemical properties of such systems.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT); Applied Electrochemistry & Catalysis (ELCAT)
Impact Factor: 6.7
Times cited: 2
DOI: 10.1039/D2NR01819E
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“A Comprehensive Study of the Electrodeposition of Nickel Nanostructures from Deep Eutectic Solvents: Self-Limiting Growth by Electrolysis of Residual Water”. Mernissi Cherigui EA, Sentosun K, Bouckenooge P, Vanrompay H, Bals S, Terryn H, Ustarroz J, The journal of physical chemistry: C : nanomaterials and interfaces 121, 9337 (2017). http://doi.org/10.1021/acs.jpcc.7b01104
Abstract: The electrodeposition of nickel nanostructures on glassy carbon was investigated in 1:2 choline chloride – urea (1:2 ChCl-U) deep eutectic solvent (DES). By combining electrochemical techniques with ex-situ FE-SEM, XPS, HAADF-STEM and EDX, the electrochemical processes occurring during nickel deposition were better understood. Special attention was given to the interaction between the solvent and the growing nickel nanoparticles. The application of a suffciently negative potential results into the electrocatlytic hydrolisis of residual water in the DES, which leads to the formation of a mixed layer of Ni/Ni(OH)2(ads). In addition, hydrogen bonds between hydroxide species and the DES components could be formed, quenching the growth of the nickel clusters favouring their aggregation. Due to these processes, a highly dense distribution of nickel nanostructures can be obtained within a wide potential range. Understanding the role of residual water and the interactions at the interface during metal electrodeposition from DESs is essential to produce supported nanostructures in a controllable way for a broad range of applications and technologies.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 4.536
Times cited: 66
DOI: 10.1021/acs.jpcc.7b01104
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“Improving the redox response stability of ceria-zirconia nanocatalysts under harsh temperature conditions”. Arias-Duque C, Bladt E, Munoz MA, Hernandez-Garrido JC, Cauqui MA, Rodriguez-Izquierdo JM, Blanco G, Bals S, Calvino JJ, Perez-Omil JA, Yeste MP, Chemistry of materials 29, 9340 (2017). http://doi.org/10.1021/ACS.CHEMMATER.7B03336
Abstract: <script type='text/javascript'>document.write(unpmarked('By depositing ceria on the surface of yttrium stabilized zirconia (YSZ) nanocrystals and further activation under high-temperature reducing conditions, a 13% mol. CeO2/YSZ catalyst structured as subnanometer thick, pyrochlore-type, ceria-zirconia islands has been prepared. This nanostructured catalyst depicts not only high oxygen storage capacity (OSC) values but, more importantly, an outstandingly stable redox response upon oxidation and reduction treatments at very high temperatures, above 1000 degrees C. This behavior largely improves that observed on conventional ceria-zirconia solid solutions, not only of the same composition but also of those with much higher molar cerium contents. Advanced scanning transmission electron microscopy (STEM-XEDS) studies have revealed as key not only to detect the actual state of the lanthanide in this novel nanocatalyst but also to rationalize its unusual resistance to redox deactivation at very high temperatures. In particular, high-resolution X-ray dispersive energy studies have revealed the presence of unique bilayer ceria islands on top of the surface of YSZ nanocrystals, which remain at surface positions upon oxidation and reduction treatments up to 1000 degrees C. Diffusion of ceria into the bulk of these crystallites upon oxidation at 1100 degrees C irreversibly deteriorates both the reducibility and OSC of this nanostructured catalyst.'));
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 9.466
Times cited: 20
DOI: 10.1021/ACS.CHEMMATER.7B03336
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“Nanorattles with tailored electric field enhancement”. Schnepf MJ, Mayer M, Kuttner C, Tebbe M, Wolf D, Dulle M, Altantzis T, Formanek P, Förster S, Bals S, König TAF, Fery A, Nanoscale 9, 9376 (2017). http://doi.org/10.1039/C7NR02952G
Abstract: Nanorattles are metallic core–shell particles with core and shell separated by a dielectric spacer. These
nanorattles have been identified as a promising class of nanoparticles, due to their extraordinary high
electric-field enhancement inside the cavity. Limiting factors are reproducibility and loss of axial symmetry
owing to the movable metal core; movement of the core results in fluctuation of the nanocavity dimensions
and commensurate variations in enhancement factor. We present a novel synthetic approach for
the robust fixation of the central gold rod within a well-defined box, which results in an axisymmetric
nanorattle. We determine the structure of the resulting axisymmetric nanorattles by advanced transmission
electron microscopy (TEM) and small-angle X-ray scattering (SAXS). Optical absorption and scattering
cross-sections obtained from UV-vis-NIR spectroscopy quantitatively agree with finite-difference
time-domain (FDTD) simulations based on the structural model derived from SAXS. The predictions of
high and homogenous field enhancement are evidenced by scanning TEM electron energy loss spectroscopy
(STEM-EELS) measurement on single-particle level. Thus, comprehensive understanding of
structural and optical properties is achieved for this class of nanoparticles, paving the way for photonic
applications where a defined and robust unit cell is crucial.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 7.367
Times cited: 69
DOI: 10.1039/C7NR02952G
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“From multi- to single-hollow trimetallic nanocrystals by ultrafast heating”. Manzaneda-Gonzalez V, Jenkinson K, Pena-Rodriguez O, Borrell-Grueiro O, Trivino-Sanchez S, Banares L, Junquera E, Espinosa A, Gonzalez-Rubio G, Bals S, Guerrero-Martinez A, Chemistry of materials 35, 9603 (2023). http://doi.org/10.1021/ACS.CHEMMATER.3C01698
Abstract: Metal nanocrystals (NCs) display unique physicochemical features that are highly dependent on nanoparticle dimensions, anisotropy, structure, and composition. The development of synthesis methodologies that allow us to tune such parameters finely emerges as crucial for the application of metal NCs in catalysis, optical materials, or biomedicine. Here, we describe a synthetic methodology to fabricate hollow multimetallic heterostructures using a combination of seed-mediated growth routes and femtosecond-pulsed laser irradiation. The envisaged methodology relies on the coreduction of Ag and Pd ions on gold nanorods (Au NRs) to form Au@PdAg core-shell nanostructures containing small cavities at the Au-PdAg interface. The excitation of Au@PdAg NRs with low fluence femtosecond pulses was employed to induce the coalescence and growth of large cavities, forming multihollow anisotropic Au@PdAg nanostructures. Moreover, single-hollow alloy AuPdAg could be achieved in high yield by increasing the irradiation energy. Advanced electron microscopy techniques, energy-dispersive X-ray spectroscopy (EDX) tomography, X-ray absorption near-edge structure (XANES) spectroscopy, and finite differences in the time domain (FDTD) simulations allowed us to characterize the morphology, structure, and elemental distribution of the irradiated NCs in detail. The ability of the reported synthesis route to fabricate multimetallic NCs with unprecedented hollow nanostructures offers attractive prospects for the fabrication of tailored high-entropy alloy nanoparticles.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 8.6
Times cited: 2
DOI: 10.1021/ACS.CHEMMATER.3C01698
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“Thermal Activation of Gold Atom Diffusion in Au@Pt Nanorods”. Pedrazo-Tardajos A, Arslan Irmak E, Kumar V, Sánchez-Iglesias A, Chen Q, Wirix M, Freitag B, Albrecht W, Van Aert S, Liz-Marzán LM, Bals S, ACS nano (2022). http://doi.org/10.1021/acsnano.2c02889
Abstract: Understanding the thermal stability of bimetallic nanoparticles is of vital importance to preserve their functionalities during their use in a variety of applications. In contrast to well-studied bimetallic systems such as Au@Ag, heat-induced morphological and compositional changes in Au@Pt nanoparticles are insufficiently understood, even though Au@Pt is an important material for catalysis. To investigate the thermal instability of Au@Pt nanorods at temperatures below their bulk melting point, we combined in situ heating with two- and three-dimensional electron microscopy techniques, including three-dimensional energy-dispersive X-ray spectroscopy. The experimental results were used as input for molecular dynamics simulations, to unravel the mechanisms behind the morphological transformation of Au@Pt core–shell nanorods. We conclude that thermal stability is influenced not only by the degree of coverage of Pt on Au but also by structural details of the Pt shell.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 17.1
Times cited: 8
DOI: 10.1021/acsnano.2c02889
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“Chemical and Structural Configuration of Pt Doped Metal Oxide Thin Films Prepared by Atomic Layer Deposition”. Ramachandran RK, Filez M, Solano E, Poelman H, Minjauw MM, Van Daele M, Feng J-Y, La Porta A, Altantzis T, Fonda E, Coati A, Garreau Y, Bals S, Marin GB, Detavernier C, Dendooven J, Chemistry of materials 31, 9673 (2019). http://doi.org/10.1021/acs.chemmater.9b03066
Abstract: Pt doped semiconducting metal oxides and Pt metal clusters embedded in an oxide matrix are of interest for applications such as catalysis and gas sensing, energy storage and memory devices. Accurate tuning of the dopant level is crucial for adjusting the properties of these materials. Here, a novel atomic layer deposition (ALD) based method for doping Pt into In2O3 in specific, and metals in metal oxides in general, is demonstrated. This approach combines alternating exposures of Pt and In2O3 ALD processes in a single ‘supercycle’, followed by supercycle repetition leading to multilayered nanocomposites. The atomic level control of ALD and its conformal nature make the method suitable for accurate dopant control even on high surface area supports. Oxidation state, local structural environment and crystalline phase of the embedded Pt dopants were obtained by means of X-ray characterization methods and high angle annular dark-field scanning transmission electron microscopy (HAADF-STEM). In addition, this approach allows characterization of the nucleation stages of metal ALD processes, by stacking those states multiple times in an oxide matrix. Regardless of experimental conditions, a few Pt ALD cycles leads to the formation of oxidized Pt species due to their highly dispersed nature, as proven by X-ray absorption spectroscopy (XAS). Grazing-incidence small-angle X-ray scattering (GISAXS) and highresolution scanning transmission electron microscopy, combined with energy dispersive X-ray spectroscopy (HR-STEM/EDXS) show that Pt is evenly distributed in the In2O3 metal oxide matrix without the formation of clusters. For a larger number of Pt ALD
cycles, typ. > 10, the oxidation state gradually evolves towards fully metallic, and metallic Pt clusters are obtained within the In2O3 metal oxide matrix. This work reveals how tuning of the ALD supercycle approach for Pt doping allows controlled engineering of the Pt compositional and structural configuration within a metal oxide matrix.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT); Applied Electrochemistry & Catalysis (ELCAT)
Impact Factor: 9.466
Times cited: 6
DOI: 10.1021/acs.chemmater.9b03066
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“Quantitative 3D Investigation of Nanoparticle Assemblies by Volumetric Segmentation of Electron Tomography Data Sets”. Kavak S, Kadu AA, Claes N, Sánchez-Iglesias A, Liz-Marzán LM, Batenburg KJ, Bals S, The journal of physical chemistry: C : nanomaterials and interfaces 127, 9725 (2023). http://doi.org/10.1021/acs.jpcc.3c02017
Abstract: Morphological characterization of nanoparticle assemblies and hybrid nanomaterials is critical in determining their structure-property relationships as well as in the development of structures with desired properties. Electron tomography has become a widely utilized technique for the three-dimensional characterization of nanoparticle assemblies. However, the extraction of quantitative morphological parameters from the reconstructed volume can be a complex and labor-intensive task. In this study, we aim to overcome this challenge by automating the volumetric segmentation process applied to three-dimensional reconstructions of nanoparticle assemblies. The key to enabling automated characterization is to assess the performance of different volumetric segmentation methods in accurately extracting predefined quantitative descriptors for morphological characterization. In our methodology, we compare the quantitative descriptors obtained through manual segmentation with those obtained through automated segmentation methods, to evaluate their accuracy and effectiveness. To show generality, our study focuses on the characterization of assemblies of CdSe/CdS quantum dots, gold nanospheres and CdSe/CdS encapsulated in polymeric micelles, and silica-coated gold nanorods decorated with both CdSe/CdS or PbS quantum dots. We use two unsupervised segmentation algorithms: the watershed transform and the spherical Hough transform. Our results demonstrate that the choice of automated segmentation method is crucial for accurately extracting the predefined quantitative descriptors. Specifically, the spherical Hough transform exhibits superior performance in accurately extracting quantitative descriptors, such as particle size and interparticle distance, thereby allowing for an objective, efficient, and reliable volumetric segmentation of complex nanoparticle assemblies.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 3.7
Times cited: 2
DOI: 10.1021/acs.jpcc.3c02017
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“Tuning the Growth of Chiral Gold Nanoparticles Through Rational Design of a Chiral Molecular Inducer”. Van Gordon K, Baúlde S, Mychinko M, Heyvaert W, Obelleiro-Liz M, Criado A, Bals S, Liz-Marzán LM, Mosquera J, Nano Letters (2023). http://doi.org/10.1021/acs.nanolett.3c02800
Abstract: The bottom-up production of chiral gold nanomaterials holds great potential for the advancement of biosensing and nano-optics, among other applications. Reproducible preparations of colloidal nanomaterials with chiral morphology have been reported, using cosurfactants or chiral inducers such as thiolated amino acids. However, the underlying growth mechanisms for these nanomaterials remain insufficiently understood. We introduce herein a purposely devised chiral inducer, a cysteine modified with a hydrophobic chain, as a versatile chiral inducer. The amphiphilic and chiral features of this molecule provide control over the chiral morphology and the chiroptical signature of the obtained nanoparticles by simply varying the concentration of chiral inducer. These results are supported by circular dichroism and electromagnetic modeling as well as electron tomography to analyze structural evolution at the facet scale. Our observations suggest complex roles for the factors involved in chiral synthesis: the chemical nature of the chiral inducers and the influence of cosurfactants.
Keywords: A1 Journal Article; Electron Microscopy for Materials Science (EMAT) ;
Impact Factor: 10.8
DOI: 10.1021/acs.nanolett.3c02800
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