Vantec 2000

The small-angle X-ray diffraction
(SAXRD) measurements were performed with a Bruker Nanostar system
(Cu Kα radiation, parallel beam formed by cross-coupled Goebel
mirrors and 3-pinhole collimation system, area detector VANTEC 2000).
The temperature of the sample was controlled with a precision of 0.1
°C. Samples were prepared as a thin film on a Kapton tape substrate.
For all samples temperature-dependent measurements were performed
in the same manner—data were collected every 5 °C for
60 s. A quasi-monodomain sample was prepared by a mechanical shearing
at elevated temperatures (10 °C below the phase transition point)
on a heating table.
Fitting of the experimental diffractograms
and simulation of the patterns were done using Topas 3 software (Bruker).
Each procedure started with choosing the most probable symmetry of
the lattice. Then, the unit cell parameters, intensities of the (Pseudo-Voigt)
signals, and (1/x) background intensity were considered
as independently adjustable parameters.

SAXS and WAXS experiments were performed
at the Multipurpose X-ray Instrument for Nanostructural Characterization
(MINA) at the University of Groningen. The instrument is equipped
with a high-intensity Cu rotating anode X-ray source, providing a
parallel collimated X-ray beam with a photon wavelength of λ
= 0.1543 nm. In order to explore a very broad q-range (0.05–8
nm^–1), the SAXS data were acquired using two different
sample-to-detector distances of 3 and 0.24 m, while the WAXS measurements
were performed using a sample-to-detector distance of 0.08 m (q-range
8–20 nm^–1). The scattering patterns were
collected using a Bruker Vantec2000 detector (pixel size of 68 μm
× 68 μm) and a Bruker Vantec500 detector (pixel size of
136 μm × 136 μm). The samples were prepared by loading
the complex coacervate samples in a sealed glass capillary of 1.5
mm outer diameter with 0.01 mm wall thickness. The SAXS and WAXS patterns
were converted into the 1D scattering intensity profiles by using
Fit2D software. After subtracting the scattering signal from the solvent
background, the three data sets were merged to generate the final
SAXS/WAXS curves, where the scattering intensity profiles are plotted
as a function of the modulus of the scattering vector q = 4πsin
θ/λ. The sample-to-detector distance and the beam center
position were calibrated by using the scattered rings from a standard
silver behenate powder sample.

1H NMR studies were recorded by using either 200 MHz or 500 MHz NMR Varian Unity Plus. Proton chemical shifts are reported in ppm (δ) relative to the internal standard—tetramethylsilane (TMS δ = 0.00 ppm). For assessing ligand stoichiometry, the nanoparticles were oxidized with I₂ and the reaction mixture after the oxidation process was analyzed.
Transmission electron microscopy (TEM) was performed using Zeiss Libra 120 microscope, with LaB6 cathode, fitted up with OMEGA internal columnar filters and CCD camera. For TEM studies, the solutions of functionalized particles were deposited onto carbon-coated copper grids and then thermally annealed at 120 °C for 3 min and slowly cooled down to 30 °C
The small angle X-ray diffraction (SAXRD) and scattering (SAXS) experiments were realized with the Bruker Nanostar system (CuKα radiation, working in parallel beam geometry formed by cross-coupled Goebel mirrors and 3-pinhole collimation system, area detector VANTEC 2000). The temperature of the sample position was maintained with accuracy of 0.1 °C. Specimens were prepared in thin-walled glass capillaries or as thin films on Kapton tape. For all of the samples, temperature dependent measurements were performed in the same manner—the XRD diffractograms were collected every 5 °C for 300 s with 40 °C/min heating rate between consecutive data collection points.