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Instruments / Technical Area	Publication Details	Published
B21-High Throughput SAXS	Interaction between glyphosate pesticide and amphiphilic peptides for colorimetric analysis Barbara B. Gerbelli , Pedro L. O. Filho , Bruna Cortez , Pedro T. Sodré , Mauricio D. Coutinho-Neto , Ian W. Hamley , Jani Seitsonen , Wendel A. Alves Nanoscale Advances 147 DOI: 10.1039/D2NA00345G Diamond Proposal Number(s): [28659] Open Access Show Abstract ▼ Abstract: The large-scale use of glyphosate pesticides in food production has attracted attention due to environmental damage and toxicity risks. Several regulatory authorities have established safe limits or concentrations of these pesticides in water and various food products consumed daily. The irreversible inhibition of acetylcholinesterase (AChE) activity is one of the strategies used for pesticide detection. Herein, we found that lipopeptide sequences can act as biomimetic microenvironments of AChE, showing higher catalytic activities than natural enzymes in an aqueous solution, based on IC50 values. These biomolecules contain in the hydrophilic part the amino acids L-proline (P), L-arginine (R), L-tryptophan (W), and L-glycine (G), covalently linked to a hydrophobic part formed by one or two long aliphatic chains. The obtained materials are referred to as compounds 1 and 2, respectively. According to fluorescence assays, 2 is more hydrophobic than 1. The circular dichroism (CD) data present a significant difference in the molar ellipticity values, likely related to distinct conformations assumed by the proline residue in the lipopeptide supramolecular structure in solution. The morphological aspect was further characterized using small-angle X-ray scattering (SAXS) and cryogenic transmission electron microscopy (cryo-TEM), which showed that compounds 1 and 2 self-assembly into cylindrical and planar core–shell structures, respectively. The mimetic AchE behaviour of lipopeptides was confirmed by Ellman's hydrolysis reaction, where the proline residue in the peptides act as a nucleophilic scavenger of organophosphate pesticides. Moreover, the isothermal titration calorimetry (ITC) experiments revealed that host–guest interactions in both systems were dominated by enthalpically-driven thermodynamics. UV-vis kinetic experiments were performed to assess the inhibition of the lipopeptide catalytic activity and the IC50 values were obtained, and we found that the detection limit correlated with the increase in hydrophobicity of the lipopeptides, implying the micellization process is more favorable.	Aug 2022
I07-Surface & interface diffraction	Templated electrodeposition as a scalable and surfactant-free approach to the synthesis of Au nanoparticles with tunable aspect ratios Giuseppe Abbondanza , Alfred Larsson , Weronica Linpe , Crispin Hetherington , Francesco Carla , Edvin Lundgren , Gary S. Harlow Nanoscale Advances 2 DOI: 10.1039/D2NA00188H Diamond Proposal Number(s): [21922] Open Access Show Abstract ▼ Abstract: A high-throughput method for the fabrication of ordered arrays of Au nanoparticles is presented. It is based on pulsed electrodeposition into porous anodic alumina templates. In contrast to many synthesis routes, it is cyanide-free, prior separation of the alumina template from the aluminium substrate is not required, and the use of contaminating surfactants/capping agents often found in colloidal synthesis is avoided. The aspect ratio of the nanoparticles can also be tuned by selecting an appropriate electrodeposition time. We show how to fabricate arrays of nanoparticles, both with branched bases and with hemispherical bases. Furthermore, we compare the different morphologies produced with electron microscopies and grazing-incidence synchrotron X-ray diffraction. We find the nanoparticles are polycrystalline in nature and are compressively strained perpendicular to the direction of growth, and expansively strained along the direction of growth. We discuss how this can produce dislocations and twinning defects that could be beneficial for catalysis.	May 2022
I09-Surface and Interface Structural Analysis	Pentacene/perfluoropentacene bilayers on Au(111) and Cu(111): impact of organic–metal coupling strength on molecular structure formation Qi Wang , Jiacheng Yang , Antoni Franco-Canellas , Christoph Buerker , Jens Niederhausen , Pierre Dombrowski , Felix Widdascheck , Tobias Breuer , Gregor Witte , Alexander Gerlach , Steffen Duhm , Frank Schreiber Nanoscale Advances 28 DOI: 10.1039/D1NA00040C Diamond Proposal Number(s): [18860] Open Access Show Abstract ▼ Abstract: As crucial element in organic opto-electronic devices, heterostructures are of pivotal importance. In this context, a comprehensive study of the properties on a simplified model system of a donor–acceptor (D–A) bilayer structure is presented, using ultraviolet photoelectron spectroscopy (UPS), X-ray photoelectron spectroscopy (XPS), low-energy electron diffraction (LEED) and normal-incidence X-ray standing wave (NIXSW) measurements. Pentacene (PEN) as donor and perfluoropentacene (PFP) as acceptor material are chosen to produce bilayer structures on Au(111) and Cu(111) by sequential monolayer deposition of the two materials. By comparing the adsorption behavior of PEN/PFP bilayers on such weakly and strongly interacting substrates, it is found that: (i) the adsorption distance of the first layer (PEN or PFP) indicates physisorption on Au(111), (ii) the characteristics of the bilayer structure on Au(111) are (almost) independent of the deposition sequence, and hence, (iii) in both cases a mixed bilayer is formed on the Au substrate. This is in striking contrast to PFP/PEN bilayers on Cu(111), where strong chemisorption pins PEN molecules to the metal surface and no intermixing is induced by subsequent PFP deposition. The results illustrate the strong tendency of PEN and PFP molecules to mix, which has important implications for the fabrication of PEN/PFP heterojunctions.	Mar 2021
I06-Nanoscience (XPEEM)	Exchange-bias via nanosegregation in novel Fe 2-x Mn 1+x Al ( x = -0.25, 0, 0.25) Heusler films Samer Kurdi , Massimo Ghidini , Giorgio Divitini , Bhaskaran Nair , Ahmed Kursumovic , Paola Tiberto , Sarnjeet Dhesi , Zoe Barber Nanoscale Advances DOI: 10.1039/C9NA00689C Diamond Proposal Number(s): [17563] Open Access Show Abstract ▼ Abstract: Exchange-bias has been reported in bulk nanocrystalline Fe2MnAl, but individual thin films of this Heusler alloy have never been studied so far. Here we study the structural and magnetic properties of nanocrystalline thin films of Fe2–xMn1+xAl (x = –0.25, 0, 0.25) obtained by sputtering and ex-situ post-deposition annealing. We find that Fe2MnAl films display exchange-bias, and that varying Mn concentration determines the magnitude of the effect, which can be either enhanced (in Fe1.75Mn1.25Al) or suppressed (in Fe2.25Mn0.75Al). X-ray diffraction (XRD) shows that our films present a mixed L21-B2 Heusler structure where increasing Mn concentration favors the partial transformation of the L21 phase into the B2 phase. Scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX) reveal that this composition-driven L21→B2 transformation is accompanied by phase segregation at the nanoscale. As a result, the Fe2–xMn1+xAl films that show exchange-bias (x = 0, 0.25) are heterogeneous, with nanograins of an Fe-rich phase embedded in a Mn-rich matrix (a non-negative matrix factorisation algorithm was used to give an indication of the phase composition from EDX data). Our comparative analysis of XRD, magnetometry and X-ray magnetic circular dichroism (XMCD), shows that Fe-rich nanograins and Mn-rich matrix are composed of a ferromagnetic L21 phase and an antiferromagnetic B2 phase, respectively, thus revealing that exchange-coupling between these two phases is the cause of the exchange-bias effect. Our work should inspire the development of single-layer, environmentally-friendly spin valve devices based on nanocomposite Heusler films.	May 2020
I20-Scanning-X-ray spectroscopy (XAS/XES)	Extracting structural information of Au colloids at ultra-dilute concentrations: identification of growth during nanoparticle immobilization George F. Tierney , Donato Decarolis , Norli Abdullah , Scott M. Rogers , Shusaku Hayama , Martha Briceno De Gutierrez , Alberto Villa , C. Richard A. Catlow , Paul Collier , Nikolaos Dimitratos , Peter Wells Nanoscale Advances 4 DOI: 10.1039/C9NA00159J Diamond Proposal Number(s): [17283] Open Access Show Abstract ▼ Abstract: Sol-immobilization is increasingly used to achieve supported metal nanoparticles (NPs) with controllable size and shape; it affords a high degree of control of the metal particle size and yields a narrow particle size distribution. Using state-of-the-art beamlines, we demonstrate how X-ray absorption fine structure (XAFS) techniques are now able to provide accurate structural information on nano-sized colloidal Au solutions at μM concentrations. This study demonstrates: (i) the size of Au colloids can be accurately tuned by adjusting the temperature of reduction, (ii) Au concentration, from 50 μM to 1000 μM, has little influence on the average size of colloidal Au NPs in solution and (iii) the immobilization step is responsible for significant growth in Au particle size, which is further exacerbated at increased Au concentrations. The work presented demonstrates that an increased understanding of the primary steps in sol-immobilization allows improved optimization of materials for catalytic applications.	May 2019

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