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Instruments / Technical Area	Publication Details	Published
I07-Surface & interface diffraction	Structural investigation of sulfobetaines and phospholipid monolayers at the air-water interface Naomi Elstone , Thomas Arnold , Maximilian W. A. Skoda , Simon E. Lewis , Peixun Li , Gavin Hazell , Karen J. Edler Physical Chemistry Chemical Physics DOI: 10.1039/D2CP02695C Diamond Proposal Number(s): [11542] Open Access Show Abstract ▼ Abstract: Mixtures of sulfobetaine based lipids with phosphocholine phospholipids are of interest in order to study the interactions between zwitterionic surfactants and the phospholipids present in cell membranes. In this study we have investigated the structure of mixed monolayers of sulfobetaines and phosphocholine phospholipids. The sulfobetaine used has a single 18-carbon tail, and is referred to as SB3-18, and the phospholipid used is DMPC. Surface pressure-area isotherms of the samples were used to determine whether any phase transitions were present during the compression of the monolayers. Neutron and X-Ray reflectometry were then used to investigate the structure of these monolayers perpendicular to the interface. We found that the average headgroup and tail layer thickness was reasonably consistent across all mixtures with a variation of less than 3 Å reported in the total thickness of the monolayers at each surface pressure. However, by selective deuteration of the two components of the monolayers, it was found that the two components have different tail layer thicknesses. For the mixture with equal compositions of DMPC and SB3-18 or with a higher composition of DMPC the tail tilts were found to be constant, resulting in a greater tail layer thickness for SB3-18 due to its longer tail. For the mixture higher in SB3-18 this was not the case, the tail tilt angle for the two components was found to be different and DMPC was found to have a greater tail layer thickness than SB3-18 as a result.	Sep 2022
I07-Surface & interface diffraction	In situ X-ray reflectivity and GISAXS study of mesoporous silica films grown from sodium silicate solution precursors Andi Di , Julien Schmitt , Naomi Elstone , Thomas Arnold , Karen J. Edler Microporous And Mesoporous Materials 153 DOI: 10.1016/j.micromeso.2022.112018 Diamond Proposal Number(s): [52101] Open Access Show Abstract ▼ Abstract: An environmentally friendly and inexpensive silica source, sodium silicate solution, is applied to synthesize a free-standing mesoporous silica film at the air/liquid interface, exploiting the co-assembly of cetyltrimethylammonium bromide and polyethylenimine. The effect of the composition of the solution used for the film formation on the mesostructure of the as-synthesized silica films, characterized by small angle X-ray scattering (SAXS), was investigated. The initial film formation time is estimated by the change in surface pressure with time. Additionally, a possible formation process of the mesostructured silica film is proposed using data from in situ grazing incidence small angle X-ray scattering (GISAXS) and X-ray reflectivity (XRR) measurements. A free-standing film with a wormlike structure formed at the interface and reorganized into a 2D hexagonal ordered structure while drying at room temperature, after removal from the air/solution interface. The ordered 2D hexagonal structure, however, could only be retained to some extent during calcination, in samples where nitrate ions are present in the film formation solution.	May 2022
	Antagonistic mixing in micelles of amphiphilic polyoxometalates and hexaethylene glycol monododecyl ether Andi Di , Julien Schmitt , Kun Ma , Marcelo A. Da Silva , Naomi S. Elstone , Najet Mahmoudi , Peixun Li , Adam Washington , Zi Wang , R. John Errington , Karen J. Edler Journal Of Colloid And Interface Science DOI: 10.1016/j.jcis.2020.06.007 Show Abstract ▼ Abstract: Hypothesis: Polyoxometalates (POMs) are metal oxygen clusters with a range of interesting magnetic and catalytic properties. POMs with attached hydrocarbon chains show amphiphilic behaviour so we hypothesised that mixtures of a non-ionic surfactant and anionic surfactants with a polyoxometalate cluster as headgroup would form mixed micelles, giving control of the POM density in the micelle, but which would differ in size and shape from micelles formed by the individual surfactants. Due to the high charge and large size of the POM, we suggested that these would be nonideal mixtures due to the complex interactions between the two types of surfactants. The nonideality and the micellar composition may be quantified using regular solution theory. With supplementary information provided by small-angle neutron scattering, an understanding of this unusual binary surfactant system can be established. Experiments: A systematic study was performed on mixed surfactant systems containing polyoxometalate-headed amphiphiles (K10[P2W17O61OSi2(CnH2n+1)2], abbreviated as P2W17-2Cn, where n = 12, 14 or 16) and hexaethylene glycol monododecyl ether (C12EO6). Critical micelle concentrations (CMCs) of these mixtures were measured and used to calculate the interaction parameters based on regular solution theory, enabling prediction of micellar composition. Predictions were compared to micelle structures obtained from small angle neutron scattering (SANS). A phase diagram was also established. Findings: The CMCs of these mixtures suggest unusual unfavourable interactions between the two species, despite formation of mixed micelles. Micellar compositions obtained from SANS concurred with those calculated using the averaged interaction parameters for P2W17-2Cn/C12EO6 (n = 12 and 14). We attribute the unfavourable interactions to a combination of different phenomena: counterion-mediated interactions between P2W17 units and the unfolding of the ethylene oxide headgroups of the nonionic surfactant, yet micelles still form in these systems due to the hydrophobic interactions between surfactant tails.	Jun 2020

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