DOI: 10.15125/bath-00954
title: Dataset for "Structural Evolution of Iron Forming Iron Oxide in a Deep Eutectic-Solvothermal Reaction"

description: This dataset contains reduced data from small angle neutron and small angle X-ray scattering experiments, and wide angle scattering S(Q) data as described in the manuscript. These data can be used to model and determine the nanostructure of choline chloride:urea deep eutectic solvents containing iron species, followed during reaction with time as they react and convert into iron oxide nanoparticles. Data are presented as .csv files, and the file names are indexed to samples in the initial file (also .csv) in each folder.
description: Small-angle neutron scattering (SANS) data were collected using the BILBY small angle scattering instrument located at the OPAL reactor neutron source of the Australian Nuclear Science and Technology Organisation, Sydney, Australia. Samples were placed into ‘banjo’ Hellma cells of pathlength 1 mm and sealed with a PTFE plug. The quartz cells were placed into individual metal holders to ensure uniform heat distribution and measured at 90 °C for up to 10h (until the reaction was complete).
SAXS measurements were made using a Xenocs nano-inXider instrument provided by the Materials Characterisation Laboratory of the STFC ISIS Neutron and Muon source. Samples were prepared by sealing 0.5 g of ChCl:urea:iron nitrate:(water) stock solutions into small vials. Samples were placed into an air-circulating temperature-regulated oven at 90 °C and removed after hourly intervals and at 90 min. At the time of removal, samples were placed directly into a freezer until use. Prior to X-ray measurement, the samples were placed into quartz glass X-ray capillaries of 1.5 mm diameter and 10 μm wall thickness and sealed using beeswax. Capillaries were measured at room temperature for several hours.
Neutron S(Q) data were collected using the NIMROD diffraction instrument at TS2 of the STFC ISIS neutron and muon facility. Samples were measured into flat-plate TiZr cells of 1mm pathlength and measured for 2 hours. X-Ray data were collected with a Panalytical X'Pert PRO II instrument, with samples loaded into quartz glass X-Ray capillaries of 2 mm pathlength.
description: SANS data were radially averaged and background subtracted at the point of data collection using an unreacted stock solution of iron nitrate in either pure or hydrated ChCl:urea. The provided files are corrected, background subtracted data files.
SAXS data were radially averaged and background subtracted at the point of data collection using an unreacted stock solution of iron nitrate in either pure or hydrated ChCl:urea. The provided files are corrected, background subtracted data files.
Neutron and X-ray diffraction data data were normalised, reduced and processed using standard procedures in GudrunN (neutron) and GudrunX (X-Rays). The provided files are corrected total scattering files, suitable for use in EPSR modelling of scattering data.
description: SANS data were fitted using the open source SASView software package (www.sasview.org) using a model for particles with an oblate spheroid platelet geometry. 
SAXS data were analysed using the ATSAS software package (https://www.embl-hamburg.de/biosaxs/software.html); seven cycles of a simulated annealing routine in DAMMIF were averaged and filtered, before passing the filtered system through a final refinement in DAMMIN.The neutron and X-ray diffraction data can be modelled using EPSR, more details of which can be found here: https://www.isis.stfc.ac.uk/Pages/Empirical-Potential-Structure-Refinement.aspx

The raw uncorrected neutron diffraction data can also be downloaded from  DOI: 10.5286/ISIS.E.RB1620292 and 10.5286/ISIS.E.RB1620479