| 1. |
- Ali, Hasan, 1985-, et al.
(författare)
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Quantitative EMCD by use of a double aperture for simultaneous acquisition of EELS
- 2019
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Ingår i: Ultramicroscopy. - : Elsevier BV. - 0304-3991 .- 1879-2723. ; 196, s. 192-196
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Tidskriftsartikel (refereegranskat)abstract
- The weak signal strength in electron magnetic circular dichroism (EMCD) measurements remains one of the main challenges in the quantification of EMCD related EELS spectra. As a consequence, small variations in peak intensity caused by changes of background intervals, choice of method for extraction of signal intensity and equally differences in sample quality can cause strong changes in the EMCD signal. When aiming for high resolution quantitative EMCD, an additional difficulty consists in the fact that the two angular resolved EELS spectra needed to obtain the EMCD signal are taken at two different instances and it cannot be guaranteed that the acquisition conditions for these two spectra are identical. Here, we present an experimental setup where we use a double hole aperture in the transmission electron microscope to obtain the EMCD signal in a single acquisition. This geometry allows for the parallel acquisition of the two electron energy loss spectra (EELS) under exactly the same conditions. We also compare the double aperture acquisition mode with the qE acquisition mode which has been previously used for parallel acquisition of EMCD. We show that the double aperture mode not only offers better signal to noise ratio as compared to qE mode but also allows for much higher acquisition times to significantly improve the signal quality which is crucial for quantitative analysis of the magnetic moments.
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| 2. |
- Ali, Hasan, 1985-, et al.
(författare)
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TEM analysis of multilayered nanostructures formed in the rapid thermal annealed silicon rich silicon oxide film
- 2016
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Ingår i: European Microscopy Congress 2016. - 9783527808465 ; , s. 965-966
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Konferensbidrag (övrigt vetenskapligt/konstnärligt)abstract
- Silicon (Si) nanoparticles (NPs) embedded in an ultrathin silicon rich silicon oxide (SRSO) film through the thermal annealing process has emerged as a highly absorbing layer for third-generation solar cells 1. The concept of using Si NPs is to achieve a band gap tunable absorber layer by controlling the size and structure of Si NPs because of the quantum confinement effect 2. In our study, a multilayer stack of silicon oxide with 35 periods of alternating layers of 1-nm thick near-stoichiometric and 3-nm thick Si-rich hydrogenated silicon oxide were deposited on fused quartz substrate by plasma-enhanced chemical vapor deposition (PECVD) method. Two samples were annealed using a rapid thermal annealing (RTA) furnace in forming gas atmosphere (90% N2 + 10% H2) for 210s and 270s respectively. From the Raman spectroscopy, a reduction in crystallinity of Si has been discovered from 210s annealed sample to 270s annealed sample (shown in Figure 2). The goal of transmission electron microscopy (TEM) analysis is to investigate the nanostructural change of Si in these two annealed samples and try to correlate the TEM observations to the Raman spectroscopy results.As the dimension of the Si nanostructures formed in SRSO films is in nanometer-scale, the energy-filtered TEM (EFTEM) tomography technique using the low-loss signals in electron energy-loss spectroscopy (EELS) has been applied as a powerful technique to correlate the precipitated Si nanostructures to the phase transformation mechanisms in the thermally annealed SRSO films 3. In this case, EFTEM spectrum-imaging (SI) technique was applied to characterize the Si nanostructures formed in SRSO films by different annealing times. The EFTEM SI dataset was acquired from -4eV to 40eV using a 2eV energy slit and the reconstructed zero loss peak (ZLP) was used to calibrate the spectra shift. Si plasmon images were extracted by fitting a Gaussian into the low-loss region with a peak position at 16.7 eV 4 and FWHM of 4.5 eV. In order to analyze the multilayer structures at different annealing durations, the TEM samples were prepared in cross sectional geometry using the conventional polishing and ion milling methods.Figure 1 shows the EFTEM images extracted from the Si plasmon peak, in these images Si appears as bright contrasts. For shorter annealing time, an alternating bright and dark contrast can be observed which indicates that the multilayer structure still remains whereas for longer annealing time, Si shows nanoparticles like contrast. The continuous layer like contrasts shown in Figure 1(a) indicates the overlapping of the contrasts generated by small Si crystallites in a very high density. After longer annealing time (Figure 1(b)), the small Si crystallites grow in size but may take overall less volume fraction due to the Ostwald ripening process. Therefore, it explains the reduction in crystallinity of Si discovered from 210s annealed sample to 270s annealed sample by Raman. However, such a reduction in Si crystallinity was not observed in nitrogen annealed SRSO films, this indicates that samples annealed in the forming gas environment follow a different crystallization mechanism and hydrogen must play a decisive role during the Si crystallization at the initial stage.
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| 3. |
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| 4. |
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| 5. |
- Fu, Le, et al.
(författare)
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Ultrastrong translucent glass ceramic with nanocrystalline, biomimetic structure
- 2018
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Ingår i: Nano letters (Print). - : American Chemical Society (ACS). - 1530-6984 .- 1530-6992. ; 18:11, s. 7146-7154
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Tidskriftsartikel (refereegranskat)abstract
- Transparent/translucent glass ceramics (GCs) have broad applications in biomedicine, armor, energy, and constructions. However, GCs with improved optical properties typically suffer from impaired mechanical properties, compared to traditional sintered full-ceramics. We present a method of obtaining high-strength, translucent GCs by preparing ZrO2-SiO2 nanocrystalline glass ceramics (NCGCs), with a microstructure of monocrystalline ZrO2 nanoparticles (NPs), embedded in an amorphous SiO2 matrix. The ZrO2-SiO2 NCGC with a composition of 65%ZrO2-35%SiO2 (molar ratio, 65Zr) achieved an average flexural strength of 1 GPa. This is one of the highest flexural strength values ever reported for GCs. ZrO2 NPs have a core-shell structure, and the shell is a thin (2–3 nm) amorphous Zr/Si interfacial layer that provides strong bonding between the ZrO2 NPs and SiO2 matrix. The diffusion of Si atoms into the ZrO2 NPs forms a Zr-O-Si superlattice. Electron tomography results show that some of the ZrO2 NPs are connected in one direction, forming in situ ZrO2 nanofibers (with length of ~500 nm), and that the ZrO2 nanofibers are stacked in an ordered way in all three dimensions. The nano-architecture of the ZrO2 nanofibers mimics the architecture of mineralized collagen fibril in cortical bone. Strong interface bonding enables efficient load transfer from the SiO2 matrix to the 3D nano-architecture built by ZrO2 nanofibers and NPs, and the 3D nano-architecture carries the majority of the external load. These two factors synergistically contribute to the high strength of the 65Zr NCGC. This study deepens our fundamental understanding of the microstructure-mechanical strength relationship, which could guide the design and manufacture of other high-strength, translucent GCs.
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| 6. |
- Henning, Dorian F., et al.
(författare)
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Luminescent CeO2:Eu3+ nanocrystals for robust in situ H2O2 real-time detection in bacterial cell cultures
- 2019
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Ingår i: Biosensors & bioelectronics. - : ELSEVIER ADVANCED TECHNOLOGY. - 0956-5663 .- 1873-4235. ; 132, s. 286-293
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Tidskriftsartikel (refereegranskat)abstract
- Hydrogen peroxide (H2O2) quantification in biomedicine is valuable as inflammation biomarker but also in assays employing enzymes that generate or consume H2O2 linked to a specific biomarker. Optical H2O2 detection is typically performed through peroxidase-coupled reactions utilizing organic dyes that suffer, however, from poor stability/reproducibility and also cannot be employed in situ in dynamic complex cell cultures to monitor H2O2 levels in real-time. Here, we utilize enzyme-mimetic CeO2 nanocrystals that are sensitive to H2O2 and study the effect of H2O2 presence on their electronic and luminescent properties. We produce and dope with Eu3+ these particles in a single-step by flame synthesis and directly deposit them on Si and glass substrates to fabricate nanoparticle layers to monitor in real-time and in situ the H2O2 concentrations generated by Streptococcus pneumoniae clinical isolates. Furthermore, the small CeO2:Eu3+ nanocrystals are combined in a single-step with larger, non-responsive Y2O3:Tb3+ nanoparticles during their double-nozzle flame synthesis to engineer hybrid luminescent nanoaggregates as ratiometric robust biosensors. We demonstrate the functionality of these biosensors by monitoring their response in the presence of a broad range of H2O2 concentrations in vitro from S. pneumoniae, highlighting their potential for facile real-time H2O2 detection in vitro in cell cultures.
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| 7. |
- Irkhina, A., et al.
(författare)
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Radiative emission from Cu2ZnSnS4/ZnSn core/shell nanocrystals
- 2019
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Ingår i: Journal of Materials Chemistry C. - : Royal Society of Chemistry. - 2050-7526 .- 2050-7534. ; 7:20, s. 6129-6133
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Tidskriftsartikel (refereegranskat)abstract
- Kesterite Cu2ZnSnS4 (CZTS) nanocrystals so far have been found to luminesce neither at room temperature nor at low temperature. Here a core-shell architecture for kesterite CZTS nanocrystals is demonstrated by applying a ZnSn-alloy shell overcoating approach. These CZTS/ZnSn nanocrystals show luminescence emission at 1.05 eV, which is red-shifted by about 0.4 eV from the absorption onset and is attributed to a radiative transition involving a deep defect. Temperature-dependent photoluminescence measurements within a range of 20-200 K indicate the presence of a competing nonradiative channel with an activation energy of 50-60 meV.
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| 8. |
- Johansson, Malin B., 1972-, et al.
(författare)
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Highly crystalline MAPbI3 perovskite grain formation by irreversible poor-solvent diffusion aggregation, for efficient solar cell fabrication
- 2020
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Ingår i: Nano Energy. - : Elsevier Ltd. - 2211-2855 .- 2211-3282. ; 78
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Tidskriftsartikel (refereegranskat)abstract
- Energy efficient synthesis providing high quality crystalline thin films are highly desired in many applications. Here we devise a non-toxic solvent approach for production of highly crystalline MAPbI3 perovskite by exploiting diffusion aggregation processes. Isopropanol solution based methylammonium lead triiodide (MAPbI3) is used in this context, where the crystal growth initiation starts in an unstable suspension far from equilibrium and the subsequent crystallization is driven by the solubility parameters. The crystal formation is monitored by scanning transmission electron microscope (STEM), observing small crystallization centers growing as time evolves to large grains with high crystal purity. Energy dispersive X-ray spectroscopy (EDS) in STEM mode revealed a Pb rich core-shell structure in newly formed grains. Nano-beam Electron Diffraction (NBED) scan defined PbI2 crystallites in the Pb rich shell with a single crystal MAPbI3 core in newly formed grains. After a week stirring, the same aggregated suspension exhibited grains with only single crystal MAPbI3 structure. The NBED analysis shows a kinetically slow transition from a core shell structure to a single crystal grain. This research presents an impactful insight on the factors that may cause sub-stoichiometric grain boundary effects which can influence the solar cell performance. In addition, the structure, morphology and optical properties of the perovskite grains have been presented. A powder of highly crystalline particles was subsequently prepared by evaporation of the solvent in a low-vacuum oven. Thin film MAPbI3 solar cells were fabricated by dissolving the powder and applying it in a classical fabrication route. The MAPbI3 solar cells gave a champion efficiency of 20% (19.9%) and an average efficiency at approximately 17% with low hysteresis effects. Here a strategy to manufacture the material structure without toxic solvents is highlighted. The single-crystal growth devised here opens both for shelf storage of materials as well as a more flexible manufacturing of devices. The process can likely be extended to other fields, where the intermediate porous framework and large surface area would be beneficial for battery or super capacitor materials.
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| 9. |
- Johansson, Malin B, 1972-, et al.
(författare)
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Porous Fractals of MAPbI3 Perovskite : Characterization of Crystal Grain Formation by Irreversible Diffusion-Limited Aggregation
- 2018
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Konferensbidrag (refereegranskat)abstract
- Isopropanol solution based methylammonium lead triiodide (MAPbI3) is studied during the crystallization process. The crystal growth starts in an unstable suspension far from equilibrium by forming different dendritic patterns and terminates with aggregation of stable cubic crystalline grains into fractal clusters. Using transmission electron microscopy (TEM), the time evolution of a newly mixed suspension was studied over a period of two weeks at room temperature and a sequence of the morphological changes was observed. The crystallization process started with single dendritic growth exhibiting branches at 90 degrees angles to one another. After 4 hours, a multi-dendritic growth pattern and a transformation into small crystalline quantum dots were observed. After a week, clusters of crystal grains were formed into a fractal pattern and these patterns appear to be stable also during the second week. Electron and x-ray diffraction revealed the crystallinity of the quantum dots and the clusters of micrometer-sized crystals. Scanning transmission electron microscope (STEM) together with energy dispersive X-ray spectroscopy (EDS) showed that newly formed large grains, from a one hour old solution, displayed a core-shell structure with higher percentage of Pb atoms as compared to iodine at the surface. In the inner core of the grains the percentage of iodine was slightly higher. The electron diffraction (ED) scan over the newly formed grains revealed a polycrystalline surface whereas the inner part had a single crystal pattern. The same solution, now one-week-old, contained grains with only single crystal patterns in the ED scan and showed no core-shell character or polycrystalline surface. The measured percentage of iodine atoms compared to lead was 2:1 throughout the cross section, which is a quantitative value within the measurement. It can be concluded from these measurements that the suspension approaches higher crystallinity of the perovskite grains in an irreversible process, where the perovskite grains are insoluble in isopropanol. The perovskite material has also been characterized with scanning electron microscopy (SEM) and photoluminescence (PL) mapping where both techniques showed a very porous crystalline material. The PL mapping revealed two peaks at 730 and 760 nm for a thin film spin coated from a newly mixed solution, while a film deposited from a one week old solution showed three peaks, the last one at 830 nm. Because of the high crystallinity, it is suggested that all three peaks are due to band-to-band transitions and not due to localized states. These data will be analyzed further; however, the results contain information of the content of quantum dots versus larger crystals, as well as displaying emission intensity variations at different positions of the grains. The purpose with this project is to understand these phenomena of crystal growth. A new mesoporous perovskite material has been designed for optoelectronic purposes.
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| 10. |
- Xie, Ling, 1982-, et al.
(författare)
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3D analysis of human islet amyloid polypeptide crystalline structures in Drosophila melanogaster
- 2019
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Ingår i: PLOS ONE. - : PUBLIC LIBRARY SCIENCE. - 1932-6203. ; 14:10
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Tidskriftsartikel (refereegranskat)abstract
- Expression of the Alzheimer's disease associated polypeptide A beta 42 and the human polypeptide hormon islet amyloid polypeptide (hIAPP) and the prohormone precursor (hproIAPP) in neurons of Drosophila melanogaster leads to the formation of protein aggregates in the fat body tissue surrounding the brain. We determined the structure of these membrane-encircled protein aggregates using transmission electron microscopy (TEM) and observed the dissolution of protein aggregates after starvation. Electron tomography (ET) as an extension of transmission electron microscopy revealed that these aggregates were comprised of granular subunits having a diameter of 20 nm aligned into highly ordered structures in all three dimensions. The three dimensional (3D) lattice of hIAPP granules were constructed of two unit cells, a body centered tetragonal (BCT) and a triclinic unit cell. A 5-fold twinned structure was observed consisting of the cyclic twinning of the BCT and triclinic unit cells. The interaction between the two nearest hIAPP granules in both unit cells is not only governed by the van der Waals forces and the dipole-dipole interaction but potentially also by filament-like structures that can connect the nearest neighbors. Hence, our 3D structural analysis provides novel insight into the aggregation process of hIAPP in the fat body tissue of Drosophila melanogaster.
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