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2. Seeds of imperfection rule the mesocrystalline disorder in natural anhydrite single crystals

Author

Stawski, Tomasz M., Smales, Glen J., Scoppola, Ernesto, Jha, Diwaker, Morales, Luiz F. G., Moya, Alicia, Wirth, Richard, Pauw, Brian R., Emmerling, Franziska, and Van Driessche, Alexander E. S.

Subjects
Condensed Matter - Materials Science
Abstract

In recent years, we have come to appreciate the astounding intricacy of the formation process of minerals from ions in aqueous solutions. In this context, a number of studies have revealed that nucleation in the calcium sulfate system is non-classical, involving the aggregation and reorganization of nanosized prenucleation particles. In a recent work we have shown that this particle-mediated nucleation pathway is actually imprinted in the resultant single micron-sized CaSO4 crystals. This property of CaSO4 minerals provides us with an unique opportunity to search for evidence of non-classical nucleation pathways in geological environments. In particular, we focused on the quintessential single crystals of anhydrite extracted from the Naica mine in Mexico. We elucidated the growth history from this mineral sample by mapping growth defects at different length scales. Based on these data we argue that the nano-scale misalignment of the structural sub-units observed in the initial calcium sulfate crystal seed propagate through different length-scales both in morphological, as well as strictly crystallographic aspects, eventually causing the formation of large mesostructured single crystals of anhydrite. Hence, the nanoparticle mediated nucleation mechanism introduces a 'seed of imperfection', which leads to a macroscopic single crystal, in which its fragments do not fit together at different length-scales in a self-similar manner. Consequently, anisotropic voids of various sizes are formed with very well-defined walls/edges. But, at the same time the material retains its essential single crystal nature. These findings shed new light on the longstanding concept of crystal structure., Comment: The dataset and SI files are published here: https://doi.org/10.5281/zenodo.4943234

Published
2021
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4. Enhancing deep visible-light photoelectrocatalysis with a single solid-state synthesis: Carbon nitride/TiO2 heterointerface

Author

Silva, Ingrid F., Pulignani, Carolina, Odutola, Jokotadeola, Galushchinskiy, Alexey, Teixeira, Ivo F., Isaacs, Mark, Mesa, Camilo A., Scoppola, Ernesto, These, Albert, Badamdorj, Bolortuya, Ángel Muñoz-Márquez, Miguel, Zizak, Ivo, Palgrave, Robert, Tarakina, Nadezda V., Gimenez, Sixto, Brabec, Christoph, Bachmann, Julien, Cortes, Emiliano, Tkachenko, Nikolai, Savateev, Oleksandr, and Jiménez-Calvo, Pablo

Published
2025
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5. Evidence for liquid-liquid phase separation during the early stages of Mg-struvite formation.

Author

Karafiludis, Stephanos, Scoppola, Ernesto, Wolf, Stephan E., Kochovski, Zdravko, Matzdorff, David, Van Driessche, Alexander E. S., Hövelmann, Jörn, Emmerling, Franziska, and Stawski, Tomasz M.

Subjects
*PHASE separation, *CRYSTAL growth, *TRANSMISSION electron microscopy, *MAGNESIUM phosphate, *AMMONIUM phosphates, *X-ray scattering
Abstract

The precipitation of struvite, a magnesium ammonium phosphate hexahydrate (MgNH4PO4 · 6H2O) mineral, from wastewater is a promising method for recovering phosphorous. While this process is commonly used in engineered environments, our understanding of the underlying mechanisms responsible for the formation of struvite crystals remains limited. Specifically, indirect evidence suggests the involvement of an amorphous precursor and the occurrence of multi-step processes in struvite formation, which would indicate non-classical paths of nucleation and crystallization. In this study, we use synchrotron-based in situ x-ray scattering complemented by cryogenic transmission electron microscopy to obtain new insights from the earliest stages of struvite formation. The holistic scattering data captured the structure of an entire assembly in a time-resolved manner. The structural features comprise the aqueous medium, the growing struvite crystals, and any potential heterogeneities or complex entities. By analysing the scattering data, we found that the onset of crystallization causes a perturbation in the structure of the surrounding aqueous medium. This perturbation is characterized by the occurrence and evolution of Ornstein-Zernike fluctuations on a scale of about 1 nm, suggesting a non-classical nature of the system. We interpret this phenomenon as a liquid-liquid phase separation, which gives rise to the formation of the amorphous precursor phase preceding actual crystal growth of struvite. Our microscopy results confirm that the formation of Mg-struvite includes a short-lived amorphous phase, lasting >10 s. [ABSTRACT FROM AUTHOR]

Published
2023
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11. Microporous Sulfur–Carbon Materials with Extended Sodium Storage Window

Author

Eren, Enis Oğuzhan, primary, Esen, Cansu, additional, Scoppola, Ernesto, additional, Song, Zihan, additional, Senokos, Evgeny, additional, Zschiesche, Hannes, additional, Cruz, Daniel, additional, Lauermann, Iver, additional, Tarakina, Nadezda V., additional, Kumru, Barış, additional, Antonietti, Markus, additional, and Giusto, Paolo, additional

Published
2024
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14. One-pot Synthesis of a Visible-light Responsive Carbon Nitride/TiO2 Heterointerface Material for Photoelectrocatalytic Applications

Author

F. Silva, Ingrid, primary, Pulignani, Carolina, additional, Odutola, Jokotadeola, additional, Galushchinskiy, Alexey, additional, F. Texeira, Ivo, additional, Isaacs, Mark, additional, Mesa, Camilo A., additional, Scoppola, Ernesto, additional, These, Albert, additional, Badamdorj, Bolortuya, additional, Muñoz-Márquez, Miguel Ángel, additional, Zizak, Ivo, additional, Palgrave, Robert, additional, V. Tarakina, Nadezda, additional, Gimenez, Sixto, additional, Brabec, Christoph, additional, Bachmann, Julien, additional, Cortes, Emiliano, additional, Tkachenko, Nikolai, additional, Savateev, Oleksandr, additional, and Jiménez-Calvo, Pablo, additional

Published
2023
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22. Invasive mussels fashion silk-like byssus via mechanical processing of massive horizontally acquired coiled coils.

Author

Simmons, Miriam, Horbelt, Nils, Sverko, Tara, Scoppola, Ernesto, Jackson, Daniel J., and Harrington, Matthew J.

Subjects
SPIDER silk, PROTEIN precursors, MUSSELS, HORIZONTAL gene transfer, ZEBRA mussel, PROTEIN structure
Abstract

Zebra and quagga mussels (Dreissena spp.) are invasive freshwater biofoulers that perpetrate devastating economic and ecological impact. Their success depends on their ability to anchor onto substrates with protein-based fibers known as byssal threads. Yet, compared to other mussel lineages, little is understood about the proteins comprising their fibers or their evolutionary history. Here, we investigated the hierarchical protein structure of Dreissenid byssal threads and the process by which they are fabricated. Unique among bivalves, we found that threads possess a predominantly β-sheet crystalline structure reminiscent of spider silk. Further analysis revealed unexpectedly that the Dreissenid thread protein precursors are mechanoresponsive a-helical proteins that are mechanically processed into β-crystallites during thread formation. Proteomic analysis of the byssus secretory organ and byssus fibers revealed a family of ultrahigh molecular weight (354 to 467 kDa) asparagine-rich (19 to 20%) protein precursors predicted to form a-helical coiled coils. Moreover, several independent lines of evidence indicate that the ancestral predecessor of these proteins was likely acquired via horizontal gene transfer. This chance evolutionary event that transpired at least 12 Mya has endowed Dreissenids with a distinctive and effective fiber formation mechanism, contributing significantly to their success as invasive species and possibly, inspiring new materials design. [ABSTRACT FROM AUTHOR]

Published
2023
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24. The complex structure of Fomes fomentarius represents an architectural design for high-performance ultralightweight materials

Author

Pylkkänen, Robert, primary, Werner, Daniel, additional, Bishoyi, Ajit, additional, Weil, Dominik, additional, Scoppola, Ernesto, additional, Wagermaier, Wolfgang, additional, Safeer, Adil, additional, Bahri, Salima, additional, Baldus, Marc, additional, Paananen, Arja, additional, Penttilä, Merja, additional, Szilvay, Géza R., additional, and Mohammadi, Pezhman, additional

Published
2023
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30. The complex structure of Fomes fomentarius represents an architectural design for high-performance ultralightweight materials

Author

Pylkkänen, Robert, Werner, Daniel, Bishoyi, Ajit, Weil, Dominik, Scoppola, Ernesto, Wagermaier, Wolfgang, Safeer, Adil, Bahri, Salima, Baldus, Marc, Paananen, Arja, Penttilä, Merja, Szilvay, Géza R., Mohammadi, Pezhman, Department of Bioproducts and Biosystems, Max Planck Institute of Colloids and Interfaces, Utrecht University, KLA-Tencor GmbH, VTT Technical Research Centre of Finland, Aalto-yliopisto, and Aalto University

Subjects
Coriolaceae/chemistry
Abstract

We thank C. Li from the Max Planck Institute of Colloids and Interfaces in Potsdam, Germany, for help during synchrotron measurements at the μSpot beamline at BESSY at the Helmholtz-Zentrum Berlin für Materialien und Energie in Berlin, Germany. We acknowledge the provision of facilities and technical support by Aalto University at the OtaNano Nanomicroscopy Center (Aalto-NMC). This work was supported by the Academy of Finland project 348628, the Jenny and Antti Wihuri Foundation (Centre for Young Synbio Scientists), and the Academy of Finland Center of Excellence Program (2022–2029) in Life-Inspired Hybrid Materials (LIBER) project number 346106, and by internal funding from the VTT Technical Research Center of Finland Ltd. We also acknowledge the Dutch Research Council (NWO, domain Applied and Engineering Sciences: MYCOAT project number 18425) and the Horizon 2020 programs of the European Union (FUNGAR; project 58132 and iNEXT-Discovery, project 871037) for NMR studies. Furthermore, the high-field NMR experiments were supported by uNMR-NL, the National Roadmap Large-Scale NMR Facility of the Netherlands (NWO grant 184.032.207), and the uNMR-NL grid (NWO grant 184.035.002). High strength, hardness, and fracture toughness are mechanical properties that are not commonly associated with the fleshy body of a fungus. Here, we show with detailed structural, chemical, and mechanical characterization that Fomes fomentarius is an exception, and its architectural design is a source of inspiration for an emerging class of ultralightweight high-performance materials. Our findings reveal that F. fomentarius is a functionally graded material with three distinct layers that undergo multiscale hierarchical self-assembly. Mycelium is the primary component in all layers. However, in each layer, mycelium exhibits a very distinct microstructure with unique preferential orientation, aspect ratio, density, and branch length. We also show that an extracellular matrix acts as a reinforcing adhesive that differs in each layer in terms of quantity, polymeric content, and interconnectivity. These findings demonstrate how the synergistic interplay of the aforementioned features results in distinct mechanical properties for each layer.

Published
2023

32. Gradients of Orientation, Composition, and Hydration of Proteins for Efficient Light Collection by the Cornea of the Horseshoe Crab

Author

Spaeker, Oliver, primary, Taylor, Gavin J., additional, Wilts, Bodo D., additional, Slabý, Tomáš, additional, Abdel‐Rahman, Mohamed Ashraf Khalil, additional, Scoppola, Ernesto, additional, Schmitt, Clemens N. Z., additional, Sztucki, Michael, additional, Liu, Jiliang, additional, Bertinetti, Luca, additional, Wagermaier, Wolfgang, additional, Scholtz, Gerhard, additional, Fratzl, Peter, additional, and Politi, Yael, additional

Published
2022
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38. Formation Mechanism of a Nano‐Ring of Bismuth Cations and Mono‐Lacunary Keggin‐Type Phosphomolybdate

Author

Martins, Inês C. B., primary, Al‐Sabbagh, Dominik, additional, Bentrup, Ursula, additional, Marquardt, Julien, additional, Schmid, Thomas, additional, Scoppola, Ernesto, additional, Kraus, Werner, additional, Stawski, Tomasz M., additional, Guilherme Buzanich, Ana, additional, Yusenko, Kirill V., additional, Weidner, Steffen, additional, and Emmerling, Franziska, additional

Published
2022
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39. Characterization of Lipid Bilayers Adsorbed to Functionalized Air/Water Interfaces

Author

Pusterla, Julio, Scoppola, Ernesto, Appel, Christian, Mukhina, Tetiana, Shen, Chen, Brezesinski, Gerald, and Schneck, Emanuel

Abstract

doi:10.26434/chemrxiv-2022-rf7z9, Lipid bilayers immobilized in planar geometries, such as solid-supported or "floating" bilayers, have enabled detailed studies of biological membranes with numerous experimental techniques, notably x-ray and neutron reflectometry. However, the presence of a solid support also has disadvantages as it complicates the use of spectroscopic techniques as well as surface rheological measurements that would require surface deformations. Here, in order to overcome these limitations, we investigate lipid bilayers adsorbed to inherently soft and experimentally well accessible air/water interfaces that are functionalized with Langmuir monolayers of amphiphiles. The bilayers are characterized with ellipsometry, X-ray scattering, and X-ray fluorescence. Grazing-incidence X-ray diffraction reveals that lipid bilayers in a chain-ordered state can have significantly different structural features than regular Langmuir monolayers of the same composition. Our results suggest that bilayers at air/water interfaces may be well suited for fundamental studies in the field of membrane biophysics.

Published
2022
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42. Induced Mineralization of Hydroxyapatite in Escherichia coliBiofilms and the Potential Role of Bacterial Alkaline Phosphatase

Author

Zorzetto, Laura, Scoppola, Ernesto, Raguin, Emeline, Blank, Kerstin G., Fratzl, Peter, and Bidan, Cécile M.

Abstract

Biofilms appear when bacteria colonize a surface and synthesize and assemble extracellular matrix components. In addition to the organic matrix, some biofilms precipitate mineral particles such as calcium phosphate. While calcified biofilms induce diseases like periodontitis in physiological environments, they also inspire the engineering of living composites. Understanding mineralization mechanisms in biofilms will thus provide key knowledge for either inhibiting or promoting mineralization in these research fields. In this work, we study the mineralization of Escherichia colibiofilms using the strain E. coliK-12 W3110, known to produce an amyloid-based fibrous matrix. We first identify the mineralization conditions of biofilms grown on nutritive agar substrates supplemented with calcium ions and β-glycerophosphate. We then localize the mineral phase at different scales using light and scanning electron microscopy in wet conditions as well as X-ray microtomography. Wide-angle X-ray scattering enables us to further identify the mineral as being hydroxyapatite. Considering the major role played by the enzyme alkaline phosphatase (ALP) in calcium phosphate precipitation in mammalian bone tissue, we further test if periplasmic ALP expressed from the phoAgene in E. coliis involved in biofilm mineralization. We show that E. colibiofilms grown on mineralizing medium supplemented with an ALP inhibitor undergo less and delayed mineralization and that purified ALP deposited on mineralizing medium is sufficient to induce mineralization. These results suggest that also bacterial ALP, expressed in E. colibiofilms, can promote mineralization. Overall, knowledge about hydroxyapatite mineralization in E. colibiofilms will benefit the development of strategies against diseases involving calcified biofilms as well as the engineering of biofilm-based living composites.

Published
2023
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48. Not just a fluidifying effect: omega-3 phospholipids induce formation of non-lamellar structures in biomembranes

Author

de Santis, Augusta, primary, Vitiello, Giuseppe, additional, Appavou, Marie-Sousai, additional, Scoppola, Ernesto, additional, Fragneto, Giovanna, additional, Barnsley, Lester C., additional, Clifton, Luke A., additional, Ottaviani, Maria Francesca, additional, Paduano, Luigi, additional, Russo Krauss, Irene, additional, and D’Errico, Gerardino, additional

Published
2020
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