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“Advanced electron microscopy characterisation of important precipitation and ordering phenomena in shape memory systems”. Schryvers D, Shape memory and superelasticity 1, 78 (2015). http://doi.org/10.1007/s40830-015-0006-3
Abstract: The present paper discusses some important aspects of precipitation and ordering in alloy systems that show a martensitic transformation and can or are used as shape memory or superelastic metallic systems. The precipitates are investigated by a variety of conventional and advanced electron microscopy techniques, including atomic resolution, 3D slice-and-view, energy loss spectroscopy etc. Depending on the system, such secondary phases can decrease the probability of a displacive transformation by changing the phase stability in the system, such as in the case of NiAl or NiTiPd, or can mechanically hinder the passage of the transformation interface, as in NiTiNb. On the other hand, properly controlling the nucleation and growth of some precipitates can strongly improve the properties of some types of materials, as is the case for the well-known Ni4Ti3 precipitates.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
DOI: 10.1007/s40830-015-0006-3
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“Measuring lattice strain in three dimensions through electron microscopy”. Goris B, de Beenhouwer J, de Backer A, Zanaga D, Batenburg KJ, Sánchez-Iglesias A, Liz-Marzán LM, Van Aert S, Bals S, Sijbers J, Van Tendeloo G, Nano letters 15, 6996 (2015). http://doi.org/10.1021/acs.nanolett.5b03008
Abstract: The three-dimensional (3D) atomic structure of nanomaterials, including strain, is crucial to understand their properties. Here, we investigate lattice strain in Au nanodecahedra using electron tomography. Although different electron tomography techniques enabled 3D characterizations of nanostructures at the atomic level, a reliable determination of lattice strain is not straightforward. We therefore propose a novel model-based approach from which atomic coordinates are measured. Our findings demonstrate the importance of investigating lattice strain in 3D.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT); Vision lab
Impact Factor: 12.712
Times cited: 87
DOI: 10.1021/acs.nanolett.5b03008
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“2D ZnO mesoporous single-crystal nanosheets with exposed {0001} polar facets for the depollution of cationic dye molecules by highly selective adsorption and photocatalytic decomposition”. Liu J, Hu Z-Y, Peng Y, Huang H-W, Li Y, Wu M, Ke X-X, Van Tendeloo G, Su B-L, Applied catalysis : B : environmental 181, 138 (2016). http://doi.org/10.1016/j.apcatb.2015.07.054
Abstract: Two dimensional (2D) ZnO nanosheets are ideal system for dimensionally confined transport phenomenon investigation owing to specific surface atomic configuration. Therefore, 2D ZnO porous nanosheets with single-crystal nature and {0001} polar facets, likely display some specific physicochemical properties. In this work, for the first time, 2D ZnO mesoporous single-crystal nanosheets (ZnO-MSN) with {0001} polar facets have been designed and prepared via an intriguing colloidal templating approach through controlling the infiltration speed for the suspension of EG-capped ZnO nanoparticles and polymer colloids. The EG-capped ZnO nanoparticles are very helpful for single-crystal nanosheet formation, while the polymer colloids play dual roles on the mesoporosity generation and {0001} polar facets formation within the mesopores. Such special 2D structure not only accelerates the hole-electron separation and the electron transportation owing to the single-crystal nature, but also enhances the selective adsorption of organic molecules owing to the porous structure and the exposed {0001} polar facets with more O-termination (000-1) surfaces: the 2D ZnO-MSN shows highly selective adsorption and significantly higher photodegradation for positively charged rhodamine B than those for negatively charged methyl orange and neutral phenol, comparing with ZnO nanoparticles (ZnO-NP) and ZnO commercial nanoparticles (ZnO-CNP) with high surface areas. This work may shed some light on better understanding the synthesis of 2D porous single-crystal nanosheet with exposed polar surfaces and photocatalytic mechanism of nanostructured semiconductors in a mixed organic molecules system.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 9.446
Times cited: 60
DOI: 10.1016/j.apcatb.2015.07.054
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“Stabilization and encapsulation of gold nanostars mediated by dithiols”. Wang Y, Belén Serrano A, Sentosun K, Bals S, Liz-Marzán LM, Small 11, 4314 (2015). http://doi.org/10.1002/smll.201500703
Abstract: Surface chemistry plays a pivotal role in regulating the morphology of nanoparticles, maintaining colloidal stability, and mediating the interaction with target analytes toward practical applications such as surface-enhanced Raman scattering (SERS)-based sensing and imaging. The use of a binary ligand mixture composed of 1,4-benzenedithiol (BDT) and hexadecyltrimethylammonium chloride (CTAC) to provide gold nanostars with long-term stability is reported. This is despite BDT being a bifunctional ligand, which usually leads to bridging and loss of colloidal stability. It is found however that neither BDT nor CTAC alone are able to provide sufficient colloidal and chemical stability. BDT-coated Au nanostars are additionally used as seeds to direct the encapsulation with a gold outer shell, leading to the formation of unusual nanostructures including semishell-coated gold nanostars, which are characterized by high-resolution electron microscopy and electron tomography. Finally, BDT is exploited as a probe to reveal the enhanced local electric fields in the different nanostructures, showing that the semishell configuration provides significantly high SERS signals as compared to other coreshell configurations obtained during seeded growth, including full shells.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 8.643
Times cited: 36
DOI: 10.1002/smll.201500703
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“Effect of clay modification on structureproperty relationships and thermal degradation kinetics of \beta-polypropylene/clay composite materials”. Papageorgiou DG, Filippousi M, Pavlidou E, Chrissafis K, Van Tendeloo G, Bikiaris D, Journal of thermal analysis and calorimetry 122, 393 (2015). http://doi.org/10.1007/s10973-015-4705-y
Abstract: The influence of neat and organically modified montmorillonite on the structureproperty relationships of a β-nucleated polypropylene matrix has been thoroughly investigated. High-angle annular dark field scanning transmission electron microscopy revealed that the organic modification of clay facilitated the dispersion of the clay, while X-ray diffractograms showed the α-nucleating effect of the clays on the β-nucleated matrix. The results from tensile tests showed that the organic modification of MMT affected profoundly only the tensile strength at yield and at break. The effect of the organic modification of the clay on the thermal stability of the composites was finally evaluated by thermogravimetric analysis, where the samples filled with oMMT decomposed faster than the ones filled with neat MMT, due to the decomposition of the organic salts that were initially used for the modification of MMT. A kinetics study of the thermal degradation of the composites was also performed, in order to export additional conclusions on the activation energy of the samples.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 1.953
Times cited: 7
DOI: 10.1007/s10973-015-4705-y
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“Intrinsic thermal instability of methylammonium lead trihalide perovskite”. Conings B, Drijkoningen J, Gauquelin N, Babayigit A, D'Haen J, D'Olieslaeger L, Ethirajan A, Verbeeck J, Manca J, Mosconi E, Angelis FD, Boyen HG;, Laser physics review 5, 1500477 (2015). http://doi.org/10.1002/aenm.201500477
Abstract: Organolead halide perovskites currently are the new front-runners as light absorbers in hybrid solar cells, as they combine efficiencies passing already 20% with deposition temperatures below 100 °C and cheap solution-based fabrication routes. Long-term stability remains a major obstacle for application on an industrial scale. Here, it is demonstrated that significant decomposition effects already occur during annealing of a methylammonium lead triiode perovskite at 85 °C even in inert atmosphere thus violating international standards. The observed behavior supports the view of currently used perovskite materials as soft matter systems with low formation energies, thus representing a major bottleneck for their application, especially in countries with high average temperatures. This result can trigger a broader search for new perovskite families with improved thermal stability.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 16.721
Times cited: 1691
DOI: 10.1002/aenm.201500477
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“Quantitative STEM normalisation : the importance of the electron flux”. Martinez GT, Jones L, de Backer A, Béché, A, Verbeeck J, Van Aert S, Nellist PD, Ultramicroscopy 159, 46 (2015). http://doi.org/10.1016/j.ultramic.2015.07.010
Abstract: Annular dark-field (ADF) scanning transmission electron microscopy (STEM) has become widely used in quantitative studies based on the opportunity to directly compare experimental and simulated images. This comparison merely requires the experimental data to be normalised and expressed in units of fractional beam-current. However, inhomogeneities in the response of electron detectors can complicate this normalisation. The quantification procedure becomes both experiment and instrument specific, requiring new simulations for the particular response of each instrument's detector, and for every camera-length used. This not only impedes the comparison between different instruments and research groups, but can also be computationally very time consuming. Furthermore, not all image simulation methods allow for the inclusion of an inhomogeneous detector response. In this work, we propose an alternative method for normalising experimental data in order to compare these with simulations that consider a homogeneous detector response. To achieve this, we determine the electron flux distribution reaching the detector by means of a camera-length series or a so-called atomic column cross-section averaged convergent beam electron diffraction (XSACBED) pattern. The result is then used to determine the relative weighting of the detector response. Here we show that the results obtained by this new electron flux weighted (EFW) method are comparable to the currently used method, while considerably simplifying the needed simulation libraries. The proposed method also allows one to obtain a metric that describes the quality of the detector response in comparison with the ideal detector response.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 2.843
Times cited: 27
DOI: 10.1016/j.ultramic.2015.07.010
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“KEu(MoO4)2 : polymorphism, structures, and luminescent properties”. Morozov VA, Arakcheeva AV, Pattison P, Meert KW, Smet PF, Poelman D, Gauquelin N, Verbeeck J, Abakumov AM, Hadermann J, Chemistry of materials 27, 5519 (2015). http://doi.org/10.1021/acs.chemmater.5b01622
Abstract: In this paper, with the example of two different polymorphs of KEu(MoO4)2, the influence of the ordering of the A-cations on the luminescent properties in scheelite related compounds (A′,A″)n[(B′,B″)O4]m is investigated. The polymorphs were synthesized using a solid state method. The study confirmed the existence of only two polymorphic forms at annealing temperature range 9231203 K and ambient pressure: a low temperature anorthic α-phase and a monoclinic high temperature β-phase with an incommensurately modulated structure. The structures of both polymorphs were solved using transmission electron microscopy and refined from synchrotron powder X-ray diffraction data. The monoclinic β-KEu(MoO4)2 has a (3+1)-dimensional incommensurately modulated structure (superspace group I2/b(αβ0)00, a = 5.52645(4) Å, b = 5.28277(4) Å, c = 11.73797(8) Å, γ = 91.2189(4)o, q = 0.56821(2)a*0.12388(3)b*), whereas the anorthic α-phase is (3+1)-dimensional commensurately modulated (superspace group I1̅(αβγ)0, a = 5.58727(22) Å, b = 5.29188(18)Å, c = 11.7120(4) Å, α = 90.485(3)o, β = 88.074(3)o, γ = 91.0270(23)o, q = 1/2a* + 1/2c*). In both cases the modulation arises due to Eu/K cation ordering at the A site: the formation of a 2-dimensional Eu3+ network is characteristic for the α-phase, while a 3-dimensional Eu3+-framework is observed for the β-phase structure. The luminescent properties of KEu(MoO4)2 samples prepared under different annealing conditions were measured, and the relation between their optical properties and their structures is discussed.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 9.466
Times cited: 26
DOI: 10.1021/acs.chemmater.5b01622
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“Fe2O3-TiO2 nanosystems by a hybrid PE-CVD/ALD approach : controllable synthesis, growth mechanism, and photocatalytic properties”. Barreca D, Carraro G, Warwick MEA, Kaunisto K, Gasparotto A, Gombac V, Sada C, Turner S, Van Tendeloo G, Maccato C, Fornasiero P;, CrystEngComm 17, 6219 (2015). http://doi.org/10.1039/c5ce00883b
Abstract: Supported Fe2O3–TiO2 nanocomposites are fabricated by an original vapor phase synthetic strategy, consisting of the initial growth of Fe2O3 nanosystems on fluorine-doped tin oxide substrates by plasma enhanced-chemical vapor deposition, followed by atomic layer deposition of TiO2 overlayers with variable thickness, and final thermal treatment in air. A thorough characterization of the target systems is carried out by X-ray diffraction, atomic force microscopy, field emission-scanning electron microscopy, energy dispersive X-ray spectroscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy. High purity nanomaterials characterized by the co-presence of Fe2O3 (hematite) and TiO2 (anatase), with an intimate Fe2O3–TiO2 contact, are successfully obtained. In addition, photocatalytic tests demonstrate that, whereas both single-phase oxides do not show appreciable activity, the composite systems are able to degrade methyl orange aqueous solutions under simulated solar light, and even visible light, with an efficiency directly dependent on TiO2 overlayer thickness. This finding opens attractive perspectives for eventual applications in wastewater treatment.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 3.474
Times cited: 25
DOI: 10.1039/c5ce00883b
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“Extreme mobility enhancement of two-dimensional electron gases at oxide interfaces by charge-transfer-induced modulation doping”. Chen YZ, Trier F, Wijnands T, Green RJ, Gauquelin N, Egoavil R, Christensen DV, Koster G, Huijben M, Bovet N, Macke S, He F, Sutarto R, Andersen NH, Sulpizio JA, Honig M, Prawiroatmodjo GEDK, Jespersen TS, Linderoth S, Ilani S, Verbeeck J, Van Tendeloo G, Rijnders G, Sawatzky GA, Pryds N, Nature materials 14, 801 (2015). http://doi.org/10.1038/nmat4303
Abstract: Two-dimensional electron gases (2DEGs) formed at the interface of insulating complex oxides promise the development of all-oxide electronic devices. These 2DEGs involve many-body interactions that give rise to a variety of physical phenomena such as superconductivity, magnetism, tunable metalinsulator transitions and phase separation. Increasing the mobility of the 2DEG, however, remains a major challenge. Here, we show that the electron mobility is enhanced by more than two orders of magnitude by inserting a single-unit-cell insulating layer of polar La1−xSrxMnO3 (x = 0, 1/8, and 1/3) at the interface between disordered LaAlO3 and crystalline SrTiO3 produced at room temperature. Resonant X-ray spectroscopy and transmission electron microscopy show that the manganite layer undergoes unambiguous electronic reconstruction, leading to modulation doping of such atomically engineered complex oxide heterointerfaces. At low temperatures, the modulation-doped 2DEG exhibits Shubnikovde Haas oscillations and fingerprints of the quantum Hall effect, demonstrating unprecedented high mobility and low electron density.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 39.737
Times cited: 170
DOI: 10.1038/nmat4303
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“KCN chemical etch for interface engineering in Cu2ZnSnSe4 solar cells”. Buffière M, Brammertz G, Sahayaraj S, Batuk M, Khelifi S, Mangin D, El Mel AA, Arzel L, Hadermann J, Meuris M, Poortmans J;, ACS applied materials and interfaces 7, 14690 (2015). http://doi.org/10.1021/acsami.5b02122
Abstract: The removal of secondary phases from the surface of the kesterite crystals is one of the major challenges to improve the performances of Cu2ZnSn(S,Se)(4) (CZTSSe) thin film solar cells. In this Contribution, the KCN/KOH Chemical etching approach, originally developed for the removal of CuxSe phases in Cu(In,Ga)(S,Se)(2) thin films) is applied to CZTSe absorbers exhibiting various chemical compositions. Two distinct electrical behaviors were observed on CZTSe/CdS solar cells after treatment: (i) the improvement of the fill factor (FF) after 30 s of etching for the CZTSe absorbers showing initially a distortion of the electrical characteristic; (ii) the progressive degradation Of the FF after long treatment time for all Cu-poor CZTSe solar cell samples. The first effect can be attributed to the action of KCN on the absorber, that is found to clean the absorber free surface from most of the secondary phases surrounding the kesterite grains (e.g., Se-0, CuxSe, SnSex, SnO2, Cu2SnSe3 phases, excepting the ZnSe-based phases). The second observation was identified as a consequence of the preferential etching of Se, Sn, and Zn from the CZTSe surface by the KOH solution, combined with the modification of the alkali content of the absorber. The formation of a Cu-rich shell at the absorber/buffer layer interface, leading to the increase of the recombination rate at the interface, and the increase in the doping of the absorber layer after etching are found to be at the origin of the deterioration of the FF of the solar cells.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 7.504
Times cited: 34
DOI: 10.1021/acsami.5b02122
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“Modified chitosan coated mesoporous strontium hydroxyapatite nanorods as drug carriers”. Filippousi M, Siafaka PI, Amanatiadou EP, Nanaki SG, Nerantzaki M, Bikiaris DN, Vizirianakis IS, Van Tendeloo G, Journal of materials chemistry B : materials for biology and medicine 3, 5991 (2015). http://doi.org/10.1039/c5tb00827a
Abstract: Mesoporous strontium hydroxyapatite (SrHAp) nanorods (NRs) have been successfully synthesized using a simple and efficient chemical route, i.e. the hydrothermal method. Structural and morphological characterization of the as-synthesized SrHAp NRs have been performed by transmission electron microscopy (TEM) and high angle annular dark field scanning transmission electron microscopy (HAADF-STEM). TEM and HAADF-STEM measurements of the NRs reveal the coexistence of longer and shorter particles with the length ranging from 50 nm to 400 nm and a diameter of about 20-40 nm. Electron tomography measurements of the NRs allow us to better visualize the mesopores and their facets. Two model drugs, hydrophobic risperidone and hydrophilic pramipexole, were loaded into the SrHAp NRs. These nanorods were coated using a modified chitosan (CS) with poly(2-hydroxyethyl methacrylate) (PHEMA), in order to encapsulate the drug-loaded SrHAp nanoparticles and reduce the cytotoxicity of the loaded materials. The drug release from neat and encapsulated SrHAp NRs mainly depends on the drug hydrophilicity. Importantly, although neat SrHAp nanorods exhibit some cytotoxicity against Caco-2 cells, the Cs-g-PHEMA-SrHAp drug-loaded nanorods show an acceptable cytocompatibility.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 4.543
Times cited: 24
DOI: 10.1039/c5tb00827a
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“Superspace crystallography : a key to the chemistry and properties”. Pinheiro CB, Abakumov AM, IUCrJ 2, 137 (2015). http://doi.org/10.1107/S2052252514023550
Abstract: An overview is given of the recent advances in the field of modulated molecular and inorganic crystals with an emphasis on the links between incommensurability, intermolecular and interatomic interactions and, wherever possible, the properties of the materials. The importance of detailed knowledge on the modulated structure for understanding the crystal chemistry and the functional properties of modulated phases is shown using selected examples of incommensurate modulations in organic molecular compounds and inorganic complex oxides.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 5.793
Times cited: 15
DOI: 10.1107/S2052252514023550
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“Novel poly(butylene succinate) nanocomposites containing strontium hydroxyapatite nanorods with enhanced osteoconductivity for tissue engineering applications”. Nerantzaki M, Filippousi M, Van Tendeloo G, Terzopoulou Z, Bikiaris D, Goudouri OM, Detsch R, Grueenewald A, Boccaccini AR, Express polymer letters 9, 773 (2015). http://doi.org/10.3144/expresspolymlett.2015.73
Abstract: Three series of poly(butylene succinate) (PBSu) nanocomposites containing 0.5, 1 and 2.5 wt% strontium hydroxyapatite [Sr-5(PO4)(3)OH] nanorods (SrHAp nrds) were prepared by in situ polymerisation. The structural effects of Sr-5(PO4)(3)OH nanorods, for the different concentrations, inside the polymeric matrix (PBSu), were studied through high angle annular dark field scanning transmission electron microscopy (HAADF-STEM). HAADF-STEM measurements revealed that the SrHAp nanorods at low concentrations are dispersed inside the polymeric PBSu matrix while in 1 wt% some aggregates are formed. These aggregations affect the mechanical properties giving an enhancement for the concentration of 0.5 wt% SrHAp nrds in tensile strength, while a reduction is recorded for higher loadings of the nanofiller. Studies on enzymatic hydrolysis revealed that all nanocomposites present higher hydrolysis rates than neat PBSu, indicating that nanorods accelerate the hydrolysis degradation process. In vitro bioactivity tests prove that SrHAp nrds promote the formation of hydroxyapatite on the PBSu surface. All nanocomposites were tested also in relevant cell culture using osteoblast-like cells (MG-63) to demonstrate their biocompatibility showing SrHAp nanorods support cell attachment.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 2.983
Times cited: 21
DOI: 10.3144/expresspolymlett.2015.73
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“Determination of the atomic width of an APB in ordered CoPt using quantified HAADF-STEM”. Akamine H, Van den Bos KHW, Gauquelin N, Farjami S, Van Aert S, Schryvers D, Nishida M, Journal of alloys and compounds 644, 570 (2015). http://doi.org/10.1016/j.jallcom.2015.04.205
Abstract: Anti-phase boundaries (APBs) in an ordered CoPt alloy are planar defects which disturb the ordered structure in their vicinity and decrease the magnetic properties. However, it has not yet been clarified to what extend the APBs disturb the ordering. In this study, high-resolution HAADF-STEM images are statistically analysed based on the image intensities estimated by the statistical parameter estimation theory. In the procedure, averaging intensities, fitting the intensity profiles to specific functions, and assessment based on a statistical test are performed. As a result, the APBs in the stable CoPt are found to be characterised by two atomic planes, and a contrast transition range as well as the centre of an inclined APB is determined. These results show that the APBs are quite sharp and therefore may have no notable effect on the net magnetic properties due to their small volume fraction. (C) 2015 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 3.133
Times cited: 12
DOI: 10.1016/j.jallcom.2015.04.205
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“Multifunctional self-assembled composite colloids and their application to SERS detection”. La Porta A, Sanchez-Iglesias A, Altantzis T, Bals S, Grzelczak M, Liz-Marzan LM, Nanoscale 7, 10377 (2015). http://doi.org/10.1039/c5nr01264c
Abstract: We present a simple method for the co-encapsulation of gold nanostars and iron-oxide nanoparticles into hybrid colloidal composites that are highly responsive to both light and external magnetic fields. Self-assembly was driven by hydrophobic interactions between polystyrene capped gold nanostars and iron oxide nanocrystals stabilized with oleic acid, upon addition of water. A block copolymer was then used to encapsulate the resulting spherical colloidal particle clusters, which thereby became hydrophilic. Electron microscopy analysis unequivocally shows that each composite particle comprises a single Au nanostar surrounded by a few hundreds of iron oxide nanocrystals. We demonstrate that this hybrid colloidal system can be used as an efficient substrate for surface enhanced Raman scattering, using common dyes as model molecular probes. The co-encapsulation of iron oxide nanoparticles renders the system magnetically responsive, so that application of an external magnetic field leads to particle accumulation and limits of detection are in the nM range.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 7.367
Times cited: 51
DOI: 10.1039/c5nr01264c
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“{110}-Layered B-cation ordering in the anion-deficient perovskite Pb2.4Ba2.6Fe2Sc2TiO13 with the crystallographic shear structure”. Tyablikov OA, Batuk D, Tsirlin AA, Batuk M, Verchenko VY, Filimonov DS, Pokholok KV, Sheptyakov DV, Rozova MG, Hadermann J, Antipov EV, Abakumov AM;, Journal of the Chemical Society : Dalton transactions 44, 10753 (2015). http://doi.org/10.1039/c4dt03867c
Abstract: A novel anion-deficient perovskite-based compound, Pb2.4Ba2.6Fe2Sc2TiO13, was synthesized via the citrate-based route. This compound is an n = 5 member of the A(n)B(n)O(3n-2) homologous series with unit-cell parameters related to the perovskite subcell a(p) approximate to 4.0 angstrom as a(p)root 2 x a(p) x 5a(p)root 2. The crystal structure of Pb2.4Ba2.6Fe2Sc2TiO13 consists of quasi-2D perovskite blocks with a thickness of three octahedral layers separated by the 1/2[110]((1) over bar 01)(p) crystallographic shear (CS) planes, which are parallel to the {110} plane of the perovskite subcell. The CS planes transform the corner-sharing octahedra into chains of edge-sharing distorted tetragonal pyramids. Using a combination of neutron powder diffraction, Fe-57 Mossbauer spectroscopy and atomic resolution electron energy-loss spectroscopy we demonstrate that the B-cations in Pb2.4Ba2.6Fe2Sc2TiO13 are ordered along the {110} perovskite layers with Fe3+ in distorted tetragonal pyramids along the CS planes, Ti4+ preferentially in the central octahedra of the perovskite blocks and Sc3+ in the outer octahedra of the perovskite blocks. Magnetic susceptibility and Mossbauer spectroscopy indicate a broadened magnetic transition around T-N similar to 45 K and the onset of local magnetic fields at low temperatures. The magnetic order is probably reminiscent of that in other A(n)B(n)O(3n-2) homologues, where G-type AFM order within the perovskite blocks has been observed.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 4.029
Times cited: 1
DOI: 10.1039/c4dt03867c
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“Homogeneity and composition of AlInGaN : a multiprobe nanostructure study”. Krause FF, Ahl JP, Tytko D, Choi PP, Egoavil R, Schowalter M, Mehrtens T, Müller-Caspary K, Verbeeck J, Raabe D, Hertkorn J, Engl K, Rosenauer A, Ultramicroscopy 156, 29 (2015). http://doi.org/10.1016/j.ultramic.2015.04.012
Abstract: The electronic properties of quaternary AlInGaN devices significantly depend on the homogeneity of the alloy. The identification of compositional fluctuations or verification of random-alloy distribution is hence of grave importance. Here, a comprehensive multiprobe study of composition and compositional homogeneity is presented, investigating AlInGaN layers with indium concentrations ranging from 0 to 17 at% and aluminium concentrations between 0 and 39 at% employing high-angle annular dark field scanning electron microscopy (HAADF STEM), energy dispersive X-ray spectroscopy (EDX) and atom probe tomography (APT). EDX mappings reveal distributions of local concentrations which are in good agreement with random alloy atomic distributions. This was hence investigated with HAADF STEM by comparison with theoretical random alloy expectations using statistical tests. To validate the performance of these tests, HAADF STEM image simulations were carried out for the case of a random-alloy distribution of atoms and for the case of In-rich clusters with nanometer dimensions. The investigated samples, which were grown by metal-organic vapor phase epitaxy (MOVPE), were thereby found to be homogeneous on this nanometer scale. Analysis of reconstructions obtained from APT measurements yielded matching results. Though HAADF STEM only allows for the reduction of possible combinations of indium and aluminium concentrations to the proximity of isolines in the two-dimensional composition space. The observed ranges of composition are in good agreement with the EDX and APT results within the respective precisions.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 2.843
Times cited: 11
DOI: 10.1016/j.ultramic.2015.04.012
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“Smart Align : a new tool for robust non-rigid registration of scanning microscope data”. Jones L, Yang H, Pennycook TJ, Marshall MSJ, Van Aert S, Browning ND, Castell MR, Nellist PD, Advanced Structural and Chemical Imaging 1, 8 (2015). http://doi.org/10.1186/s40679-015-0008-4
Abstract: Many microscopic investigations of materials may benefit from the recording of multiple successive images. This can include techniques common to several types of microscopy such as frame averaging to improve signal-to-noise ratios (SNR) or time series to study dynamic processes or more specific applications. In the scanning transmission electron microscope, this might include focal series for optical sectioning or aberration measurement, beam damage studies or camera-length series to study the effects of strain; whilst in the scanning tunnelling microscope, this might include bias-voltage series to probe local electronic structure. Whatever the application, such investigations must begin with the careful alignment of these data stacks, an operation that is not always trivial. In addition, the presence of low-frequency scanning distortions can introduce intra-image shifts to the data. Here, we describe an improved automated method of performing non-rigid registration customised for the challenges unique to scanned microscope data specifically addressing the issues of low-SNR data, images containing a large proportion of crystalline material and/or local features of interest such as dislocations or edges. Careful attention has been paid to artefact testing of the non-rigid registration method used, and the importance of this registration for the quantitative interpretation of feature intensities and positions is evaluated.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Times cited: 131
DOI: 10.1186/s40679-015-0008-4
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“Possibilities and limitations of advanced transmission electron microscopy for carbon-based nanomaterials”. Ke X, Bittencourt C, Van Tendeloo G, Beilstein journal of nanotechnology 6, 1541 (2015). http://doi.org/10.3762/bjnano.6.158
Abstract: A major revolution for electron microscopy in the past decade is the introduction of aberration correction, which enables one to increase both the spatial resolution and the energy resolution to the optical limit. Aberration correction has contributed significantly to the imaging at low operating voltages. This is crucial for carbon-based nanomaterials which are sensitive to electron irradiation. The research of carbon nanomaterials and nanohybrids, in particular the fundamental understanding of defects and interfaces, can now be carried out in unprecedented detail by aberration-corrected transmission electron microscopy (AC-TEM). This review discusses new possibilities and limits of AC-TEM at low voltage, including the structural imaging at atomic resolution, in three dimensions and spectroscopic investigation of chemistry and bonding. In situ TEM of carbon-based nanomaterials is discussed and illustrated through recent reports with particular emphasis on the underlying physics of interactions between electrons and carbon atoms.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 3.127
Times cited: 10
DOI: 10.3762/bjnano.6.158
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“Morphological TEM studies and magnetoresistance analysis of sputtered Al-substituted ZnO films : the role of oxygen”. Van Gompel M, Atalay AY, Gaulke A, Van Bael MK, D'Haen J, Turner S, Van Tendeloo G, Vanacken J, Moshchalkov VV, Wagner P, Physica status solidi : A : applications and materials science 212, 1191 (2015). http://doi.org/10.1002/pssa.201431888
Abstract: In this article, we report on the synthesis of thin, epitaxial films of the transparent conductive oxide Al:ZnO on (0001)-oriented synthetic sapphire substrates by DC sputtering from targets with a nominal 1 at.% Al substitution. The deposition was carried out at an unusually low substrate temperature of only 250 °C in argonoxygen mixtures as well as in pure argon. The impact of the processgas composition on the morphology was analysed by transmission electron microscopy, revealing epitaxial growth in all the cases with a minor impact of the process parameters on the resulting grain sizes. The transport properties resistivity, Hall effect and magnetoresistance were studied in the range from 10 to 300 K in DC and pulsed magnetic fields up to 45 T. While the carrier density and mobility are widely temperature independent, we identified a low fieldlow temperature regime in which the magnetoresistance shows an anomalous, negative behaviour. At higher fields and temperatures, the magnetoresistance exhibits a more conventional, positive curvature with increasing field strength. As a possible explanation, we propose carrier scattering at localised magnetic trace impurities and magnetic correlations.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 1.775
DOI: 10.1002/pssa.201431888
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“Local destruction of superconductivity by non-magnetic impurities in mesoscopic iron-based superconductors”. Li J, Ji M, Schwarz T, Ke X, Van Tendeloo G, Yuan J, Pereira PJ, Huang Y, Zhang G, Feng HL, Yuan YH, Hatano T, Kleiner R, Koelle D, Chibotaru LF, Yamaura K, Wang HB, Wu PH, Takayama-Muromachi E, Vanacken J, Moshchalkov VV;, Nature communications 6, 7614 (2015). http://doi.org/10.1038/ncomms8614
Abstract: The determination of the pairing symmetry is one of the most crucial issues for the iron-based superconductors, for which various scenarios are discussed controversially. Non-magnetic impurity substitution is one of the most promising approaches to address the issue, because the pair-breaking mechanism from the non-magnetic impurities should be different for various models. Previous substitution experiments demonstrated that the non-magnetic zinc can suppress the superconductivity of various iron-based superconductors. Here we demonstrate the local destruction of superconductivity by non-magnetic zinc impurities in Ba0.5K0.5Fe2As2 by exploring phase-slip phenomena in a mesoscopic structure with 119 × 102 nm2 cross-section. The impurities suppress superconductivity in a three-dimensional Swiss cheese-like pattern with in-plane and out-of-plane characteristic lengths slightly below ~1.34 nm. This causes the superconducting order parameter to vary along abundant narrow channels with effective cross-section of a few square nanometres. The local destruction of superconductivity can be related to Cooper pair breaking by non-magnetic impurities.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 12.124
Times cited: 12
DOI: 10.1038/ncomms8614
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“Solidelectrolyte interphase evolution of carbon-coated silicon nanoparticles for lithium-ion batteries monitored by transmission electron microscopy and impedance spectroscopy”. Van Havenbergh K, Turner S, Driesen K, Bridel J-S, Van Tendeloo G, Energy technology 3, 699 (2015). http://doi.org/10.1002/ente.201500034
Abstract: The main drawbacks of silicon as the most promising anode material for lithium-ion batteries (theoretical capacity=3572 mAh g−1) are lithiation-induced volume changes and the continuous formation of a solidelectrolyte interphase (SEI) upon cycling. A recent strategy is to focus on the influence of coatings and composite materials. To this end, the evolution of the SEI, as well as an applied carbon coating, on nanosilicon electrodes during the first electrochemical cycles is monitored. Two specific techniques are combined: Transmission Electron Microscopy (TEM) is used to study the surface evolution of the nanoparticles on a very local scale, whereas electrochemical impedance spectroscopy (EIS) provides information on the electrode level. A TEMEELS fingerprint signal of carbonate structures from the SEI is discovered, which can be used to differentiate between the SEI and a graphitic carbon matrix. Furthermore, the shielding effect of the carbon coating and the thickness evolution of the SEI are described.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 2.789
DOI: 10.1002/ente.201500034
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“Electron tomography based on highly limited data using a neural network reconstruction technique”. Bladt E, Pelt DM, Bals S, Batenburg KJ, Ultramicroscopy 158, 81 (2015). http://doi.org/10.1016/j.ultramic.2015.07.001
Abstract: Gold nanoparticles are studied extensively due to their unique optical and catalytical properties. Their exact shape determines the properties and thereby the possible applications. Electron tomography is therefore often used to examine the three-dimensional (3D) shape of nanoparticles. However, since the acquisition of the experimental tilt series and the 3D reconstructions are very time consuming, it is difficult to obtain statistical results concerning the 3D shape of nanoparticles. Here, we propose a new approach for electron tomography that is based on artificial neural networks. The use of a new reconstruction approach enables us to reduce the number of projection images with a factor of 5 or more. The decrease in acquisition time of the tilt series and use of an efficient reconstruction algorithm allows us to examine a large amount of nanoparticles in order to retrieve statistical results concerning the 3D shape.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); Vision lab
Impact Factor: 2.843
Times cited: 25
DOI: 10.1016/j.ultramic.2015.07.001
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“Reversible Li-intercalation through oxygen reactivity in Li-rich Li-Fe-Te oxide materials”. McCalla E, Prakash AS, Berg E, Saubanere M, Abakumov AM, Foix D, Klobes B, Sougrati MT, Rousse G, Lepoivre F, Mariyappan S, Doublet ML, Gonbeau D, Novak P, Van Tendeloo G, Hermann RP, Tarascon JM;, Journal of the electrochemical society 162, A1341 (2015). http://doi.org/10.1149/2.0991507jes
Abstract: Lithium-rich oxides are a promising class of positive electrode materials for next generation lithium-ion batteries, and oxygen plays a prominent role during electrochemical cycling either by forming peroxo-like species and/or by irreversibly forming oxygen gas during first charge. Here, we present Li-Fe-Te-O materials which show a tremendous amount of oxygen gas release. This oxygen release accounts for nearly all the capacity during the first charge and results in vacancies as seen by transmission electron microscopy. There is no oxidation of either metal during charge but significant changes in their environments. These changes are particularly extreme for tellurium. XRD and neutron powder diffraction both show limited Changes during cycling and no appreciable change in lattice parameters. A density functional theory study of this material is performed and demonstrates that the holes created on some of the oxygen atoms upon oxidation are partially stabilized through the formation of shorter O-O bonds, i.e. (O-2)(n-) species which on further delithiation show a spontaneous O-2 de-coordination from the cationic network and migration to the now empty lithium layer. The rate limiting step during charge is undoubtedly the diffusion of oxygen either out along the lithium layer or via columns of oxygen atoms. (C) 2015 The Electrochemical Society. All rights reserved.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT)
Impact Factor: 3.259
Times cited: 23
DOI: 10.1149/2.0991507jes
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“Quantitative study of particle size distribution in an in-situ grown Al-TiB2 composite by synchrotron X-ray diffraction and electron microscopy”. Tang Y, Chen Z, Borbely A, Ji G, Zhong SY, Schryvers D, Ji V, Wang HW, Materials characterization 102, 131 (2015). http://doi.org/10.1016/j.matchar.2015.03.003
Abstract: Synchrotron X-ray diffraction and transmission electron microscopy (TEM) were applied to quantitatively characterize the average particle size and size distribution of free-standing TiB2 particles and TiB2 particles in an insitu grown Al–TiB2 composite. The detailed evaluations were carried out by X-ray line profile analysis using the restrictedmoment method and multiplewhole profile fitting procedure (MWP). Both numericalmethods indicate that the formed TiB2 particles are well crystallized and free of crystal defects. The average particle size determined from different Bragg reflections by the restricted moment method ranges between 25 and 55 nm, where the smallest particle size is determined using the 110 reflection suggesting the highest lateral-growth velocity of (110) facets. TheMWP method has shown that the in-situ grown TiB2 particles have a very low dislocation density (~1011 m−2) and their size distribution can be described by a log-normal distribution. Good agreement was found between the results obtained from the restricted moment and MWP methods, which was further confirmed by TEM.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 2.714
Times cited: 41
DOI: 10.1016/j.matchar.2015.03.003
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“Heterometal nanoparticles from Ru-based molecular clusters covalently anchored onto functionalized carbon nanotubes and nanofibers”. Vidick D, Ke X, Devillers M, Poleunis C, Delcorte A, Moggi P, Van Tendeloo G, Hermans S, Beilstein journal of nanotechnology 6, 1287 (2015). http://doi.org/10.3762/bjnano.6.133
Abstract: Heterometal clusters containing Ru and Au, Co and/or Pt are anchored onto carbon nanotubes and nanofibers functionalized with chelating phosphine groups. The cluster anchoring yield is related to the amount of phosphine groups available on the nanocarbon surface. The ligands of the anchored molecular species are then removed by gentle thermal treatment in order to form nanoparticles. In the case of Au-containing clusters, removal of gold atoms from the clusters and agglomeration leads to a bimodal distribution of nanoparticles at the nanocarbon surface. In the case of Ru-Pt species, anchoring occurs without reorganization through a ligand exchange mechanism. After thermal treatment, ultrasmall (1-3 nm) bimetal Ru-Pt nanoparticles are formed on the surface of the nanocarbons. Characterization by high resolution transmission electron microscopy (HRTEM) and high angle annular dark field scanning transmission electron microscopy (HAADF-STEM) confirms their bimetal nature on the nanoscale. The obtained bimetal nanoparticles supported on nanocarbon were tested as catalysts in ammonia synthesis and are shown to be active at low temperature and atmospheric pressure with very low Ru loading.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 3.127
Times cited: 7
DOI: 10.3762/bjnano.6.133
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“Mechanical switching of nanoscale multiferroic phase boundaries”. Li YJ, Wang JJ, Ye JC, Ke XX, Gou GY, Wei Y, Xue F, Wang J, Wang CS, Peng RC, Deng XL, Yang Y, Ren XB, Chen LQ, Nan CW, Zhang JX;, Advanced functional materials 25, 3405 (2015). http://doi.org/10.1002/adfm.201500600
Abstract: Tuning the lattice degree of freedom in nanoscale functional crystals is critical to exploit the emerging functionalities such as piezoelectricity, shape-memory effect, or piezomagnetism, which are attributed to the intrinsic lattice-polar or lattice-spin coupling. Here it is reported that a mechanical probe can be a dynamic tool to switch the ferroic orders at the nanoscale multiferroic phase boundaries in BiFeO3 with a phase mixture, where the material can be reversibly transformed between the soft tetragonal-like and the hard rhombohedral-like structures. The microscopic origin of the nonvolatile mechanical switching of the multiferroic phase boundaries, coupled with a reversible 180 degrees rotation of the in-plane ferroelectric polarization, is the nanoscale pressure-induced elastic deformation and reconstruction of the spontaneous strain gradient across the multiferroic phase boundaries. The reversible control of the room-temperature multiple ferroic orders using a pure mechanical stimulus may bring us a new pathway to achieve the potential energy conversion and sensing applications.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 12.124
Times cited: 23
DOI: 10.1002/adfm.201500600
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“Effect of structural defects on the hydriding kinetics of nanocrystalline Pd thin films”. Delmelle R, Amin-Ahmadi B, Sinnaeve M, Idrissi H, Pardoen T, Schryvers D, Proost J, International journal of hydrogen energy 40, 7335 (2015). http://doi.org/10.1016/j.ijhydene.2015.04.017
Abstract: While the microstructure of a metal is well-known to affect its equilibrium hydrogen uptake and therefore the hydriding thermodynamics, microstructural effects on the hydriding kinetics are much less documented. Moreover, for thin film systems, such microstructural effects are difficult to separate from the internal stress effect, since most defects generate internal stresses. Such a decoupling has been achieved in this paper for nanocrystalline Pd thin film model systems through the use of a high-resolution, in-situ curvature measurement set-up during Pd deposition, annealing and hydriding. This set-up allowed producing Pd thin films with similar internal stress levels but significantly different microstructures. This was evidenced from detailed defect statistics obtained by transmission electron microscopy, which showed that the densities of grain boundaries, dislocations and twin boundaries have all been lowered by annealing. The same set-up was then used to study the hydriding equilibrium and kinetic behaviour of the resulting films at room temperature. A full quantitative analysis of their hydriding cycles showed that the rate constants of both the adsorption- and absorption-limited kinetic regimes were strongly affected by microstructure. Defect engineering was thereby shown to increase the rate constants for hydrogen adsorption and absorption in Pd by a factor 40 and 30, respectively. Copyright (C) 2015, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 3.582
Times cited: 13
DOI: 10.1016/j.ijhydene.2015.04.017
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“Phase problem in the B-site ordering of La2CoMnO6 : impact on structure and magnetism”. Egoavil R, Huehn S, Jungbauer M, Gauquelin N, Béché, A, Van Tendeloo G, Verbeeck, Moshnyaga V, Nanoscale 7, 9835 (2015). http://doi.org/10.1039/c5nr01642h
Abstract: Epitaxial double perovskite La2CoMnO6 (LCMO) films were grown by metalorganic aerosol deposition on SrTiO3(111) substrates. A high Curie temperature, T-C = 226 K, and large magnetization close to saturation, M-S(5 K) = 5.8 mu(B)/f.u., indicate a 97% degree of B-site (Co,Mn) ordering within the film. The Co/Mn ordering was directly imaged at the atomic scale by scanning transmission electron microscopy with energy-dispersive X-ray spectroscopy (STEM-EDX). Local electron-energy-loss spectroscopy (EELS) measurements reveal that the B-sites are predominantly occupied by Co2+ and Mn4+ ions in quantitative agreement with magnetic data. Relatively small values of the (1/2 1/2 1/2) superstructure peak intensity, obtained by X-ray diffraction (XRD), point out the existence of ordered domains with an arbitrary phase relationship across the domain boundary. The size of these domains is estimated to be in the range 35-170 nm according to TEM observations and modelling the magnetization data. These observations provide important information towards the complexity of the cation ordering phenomenon and its implications on magnetism in double perovskites, and similar materials.
Keywords: A1 Journal article; Engineering sciences. Technology; Electron microscopy for materials research (EMAT)
Impact Factor: 7.367
Times cited: 37
DOI: 10.1039/c5nr01642h
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