© Xenocs 2022 1 Overview SAXS gives information about © Xenocs 2022 3 Characterization with SAXS Crystalline fraction Phase identification Orientation analysis Lamellar structure Particle or macromolecular shape Temperature Influence on structure Humidity influence on structure Tensile influence on structure Shear influence on structure Specific surface Surface structure and patterns Particle size and size distribution Pore size and size distribution © Xenocs 2022 Molecular weight 4 Length scales © Xenocs 2022 5 Length scales Hierarchical structures example © Xenocs 2022 6 Some advantages of using SAXS SAXS Applications overview Understanding the material structure at the nano-scale is key to the development of new products and services © Xenocs 2022 8 Food Insights SAXS can provide © Xenocs 2022 9 Food Relevant references “Impact of cooling profile on refined palm oil crystallization: Microscopic and small and wide-angle X-Ray scattering investigations” “Size-dependent filling effect of crystalline celluloses in structural engineering of composite oleogels” “Influence of γ-lactones on monolinolein/water bulk and emulsified mesophases” “Stearyl Methacrylate-Based Polymers as Crystal Habit Modifiers for Triacylglycerols” “Lubrication behaviors of core-shell structured particles formed by whey proteins and xanthan gum” “Encapsulation of aspartic protease in nonlamellar lipid liquid crystalline phases” “Characterization of multi-scale structure and thermal properties of Indica rice starch with different amylose contents” “Structural characterization of multilamellar liposomes encapsulating curcumin and vitamin D3” 10.1016/j.foodhyd.2021.107089 “Impact of superheated steam on the moisture transfer, structural characteristics and rheological properties of wheat starch” © Xenocs 2022 10 Food Case study: How do temperature variations influence the structure of chocolate? © Xenocs 2022 11 Food Case study: How do temperature variations influence the structure of chocolate? Measurements and results © Xenocs 2022 12 Food Case study: How do temperature variations influence the structure of chocolate? 1 1▪ 2▪ 3▪ 4▪ 4 3 3 2 © Xenocs 2022 13 Food Case study: How do temperature variations influence the structure of chocolate? Conclusions With these SAXS/WAXS measurements, we have gained insight into the morphological differences generated by 2 thermal routes towards solidification from melt of cocoa butter. • Untempered cocoa butter: Cooling fast in the fridge then bring back to room temperature • Tempered cocoa butter: Cooling to room temperature, then tempering at 35 °C, then bring back to room temperature © Xenocs 2022 14 Cosmetics and consumer care Insights SAXS can provide © Xenocs 2022 15 Cosmetics and consumer care Relevant references “Long-term stability of n-Alkane-in-water Pickering nanoemulsions: Effect of aqueous solubility of droplet phase on Ostwald ripening” “Structural characterization of biocompatible reverse micelles using small-angle X-ray scattering, 31P nuclear magnetic resonance, and fluorescence spectroscopy” “Supramolecular architecture of a multi-component biomimetic lipid barrier formulation” “Double-chain cationic surfactants: Swelling, structure, phase transitions and additive effects” “The rational design of biomimetic skin barrier lipid formulations using biophysical methods” “The cooling process effect on the bilayer phase state of the CTAC/cetearyl alcohol/water surfactant gel” “Liquid crystalline phases of linear alkylbenzene sulphonate in spray-dried detergent powders studied by small-angle X-ray scattering, TEM, and ATR-IR spectroscopy” “Hydrophobization of cellulose nanocrystals for aqueous colloidal suspensions and gels” © Xenocs 2022 16 Cosmetics and consumer care Case study: What is the structure of shampoo and how does it influence its properties? © Xenocs 2022 17 Cosmetics and consumer care Case study: What is the structure of shampoo and how does it influence its properties? Measurement and results 10 10 2 Azimuthal average [a.u.] 8 1▪ 2▪ 3▪ 4▪ 10 3 1 4 6 10 4 10 2 10 -2 10 -1 10 0 10 1 10 q [nm-1] © Xenocs 2022 18 Cosmetics and consumer care Case study: What is the structure of shampoo and how does it influence its properties? Conclusions © Xenocs 2022 19 Polymers Insights SAXS can provide © Xenocs 2022 20 Polymers Relevant references “Strategy for enhancing ultrahigh-molecular-weight block copolymer chain mobility to access large period sizes (>100 nm)” “RAFT aqueous emulsion polymerization of methyl methacrylate: observation of unexpected constraints when employing a non-ionic steric stabilizer block” “Investigation of roughness correlation in polymer brushes via X-ray scattering” “Direct access to polysaccharide-based vesicles with a tunable membrane thickness in a large concentration window via polymerization-induced selfassembly” “Anisotropic nanoparticles as templates for the crystalline structure of an injection-molded isotactic polypropylene/TiO2 nanocomposite” “Investigation of micromechanical behavior and voiding of polyethylene terephthalate/polyethylene-stat-methyl acrylate blends during tensile deformatoni” “Later stage melting of isotactic polypropylene” © Xenocs 2022 21 Polymers Case study: Determination of polymer crystallinity © Xenocs 2022 22 Polymers Case study Determination of polymer crystallinity Total scattering Crystalline fraction Measurements and results Amorphous fraction • • • • © Xenocs 2022 23 Polymers Case study Determination of polymer crystallinity Total scattering Crystalline fraction Conclusions Amorphous fraction © Xenocs 2022 24 Polymers Case study: Characterisation of the polymer crystalline lamellae © Xenocs 2022 25 Polymers Case study: Characterisation of the polymer crystalline lamellae Measurement and results • • • © Xenocs 2022 26 Polymers Case study: Size and periodic organization Measurement and results • ° ° • ° • ° ° ° • © Xenocs 2022 27 Polymers Case study: Size and periodic organization Conclusions ° ° ° © Xenocs 2022 ° 28 Nanoparticles and colloids Insights SAXS can provide © Xenocs 2022 29 Nanoparticles and colloids Relevant references “Influence of an external magnetic field in the two-photon absorption coefficient of magnetite nanoparticles in colloids and thin films” “Key parameters to tailor hollow silica nanospheres for a type I porous liquid synthesis: Optimized structure and accessibility” “Monodisperse hollow silica spheres: An in-depth scattering analysis” “Strain-and field-induced anisotropy in hybrid elastomers with elongated filler nanoparticles” “Scalable synthesis of dispersible iron carbide (Fe3C) nanoparticles by ‘nanocasting’” “An in situ SAXS investigation of the formation of silver nanoparticles and bimetallic silver-gold nanoparticles in controlled wet-chemical reduction synthesis” “Particle size analysis — Small angle X-ray scattering (SAXS)” “Nanoparticle heat-up synthesis: In situ X-ray diffraction and extension from classical to nonclassical nucleation and growth theory” © Xenocs 2022 30 Nanoparticles and colloids Case study: Size distribution of nanoparticles © Xenocs 2022 31 Nanoparticles and colloids Case study: Size distribution of nanoparticles 1 Measurement and results 2 3 1 2 3 © Xenocs 2022 32 Nanoparticles and colloids Case study: Size distribution of nanoparticles Measurement and results • • • © Xenocs 2022 33 Nanoparticles and colloids Case study: Size distribution of nanoparticles Conclusions © Xenocs 2022 34 Renewable energy and storage Insights SAXS can provide © Xenocs 2022 35 Renewable energy and storage Relevant references “Application of experimental design to hydrogen storage: Optimisation of lignin-derived carbons” “Hard–soft carbon composite anodes with synergistic sodium storage performance” “Modulating molecular orientation enables efficient nonfullerene small-molecule organic solar cells” “In operando small-angle X-ray scattering investigation of nanostructured polymer electrolyte for lithium-ion batteries” “Progression of the morphology in random ionomers containing bulky ammonium counterions” “Correlations between precipitation reactions and electrochemical performance of lithium-sulfur batteries probed by operando scattering techniques” “Hierarchical sticker and sticky chain dynamics in self-healing butyl rubber ionomers” “Mesoporous TiO2 microparticles with tailored surfaces, pores, walls, and particle dimensions using persistent micelle templates” © Xenocs 2022 36 Renewable energy and storage Case study: Can time-resolved degradation of catalysts be studied with operando laboratory SAXS? © Xenocs 2022 37 Renewable energy and storage Case study: Can time-resolved degradation of catalysts be studied with operando laboratory SAXS? Measurement and results • • © Xenocs 2022 38 Renewable energy and storage Case study: Can time-resolved degradation of catalysts be studied with operando laboratory SAXS? Conclusions © Xenocs 2022 39 Inorganic Materials Insights SAXS can provide © Xenocs 2022 40 Inorganic Materials Relevant references “Amphiphilic diblock copolymer-mediated structure control in nanoporous germanium-based thin films” “Strengthening mechanisms in Fe-Al based ferritic low-density steels” “Nanocrystalline ODS-iron aluminide by cryo-milling: consolidation, microstructure and mechanical behavior” “Facet Control for Trap-State Suppression in Colloidal Quantum Dot Solids” “Time resolved alkali silicate decondensation by sodium hydroxide solution” “Systematic modification of UiO-66 Metal-Organic Frameworks for Glucose Conversion into 5-Hydroxymethyl Furfural in Water” “Impact of aluminium on the structure of geopolymers from the early stages to consolidated material” “Cysteamine-modified ZIF-8 colloidal building blocks: Direct assembly of nanoparticulate MOF films on gold surfaces via thiol chemistry” © Xenocs 2022 41 Inorganic Materials Case study: In-depth SAXS characterization of fractal structures produced by spray flame synthesis © Xenocs 2022 42 Inorganic Materials Case study: Fractal structures Measurement and results 2 1 1 2 • • © Xenocs 2022 43 Inorganic Materials Case study: Fractal structures Measurement and results • • © Xenocs 2022 44 Inorganic Materials Case study: Fractal structures Measurement and results • • • • © Xenocs 2022 45 Inorganic Materials Case study: Fractal structures Conclusions © Xenocs 2022 46 Biostructural research Insights SAXS can provide © Xenocs 2022 47 Biostructural reseach Relevant references “Effects of artepillin C on model membranes displaying liquid immiscibility” “Effects of oxidation on the physicochemical properties of polyunsaturated lipid membranes” “NMR and crystallographic structural studies of the extremely stable monomeric variant of human cystatin C with single amino acid substitution” “Ionization and structural properties of mRNA lipid nanoparticles influence expression in intramuscular and intravascular administration” “Pre-nucleation cluster formation upon ethyl acetate addition to an aqueous solution of an anionic hydrotrope” “Assessing the efficiency of SBA-15 as a nanocarrier for diphtheria anatoxin” “Mechanistic studies of an automated lipid nanoparticle reveal critical pharmaceutical properties associated with enhanced mRNA functional delivery in vitro and in vivo” “Intrinsically disordered N-terminal domain of the Helicoverpa armigera Ultraspiracle stabilizes the dimeric form via a scorpion-like structure” © Xenocs 2022 48 Biostructural research Case study: Monitoring morphological changes during protein fibrillation © Xenocs 2022 49 Biostructural research Case study: Monitoring morphological changes during protein fibrillation 1 Measurement and results 2 3 1 2 3 © Xenocs 2022 50 Biostructural research Case study: Monitoring morphological changes during protein fibrillation Conclusions © Xenocs 2022 51 Biostructural research Case study: SEC-SAXS for structural investigation of complex samples © Xenocs 2022 52 Biostructural research Case study: SEC-SAXS Measurement and results © Xenocs 2022 53 Biostructural research Case study: SEC-SAXS for structural investigation of complex samples Conclusions © Xenocs 2022 54 Summary Conclusions © Xenocs 2022 55