Pilatus 300k

Transmission WAXS
diffractograms were obtained under vacuum using a Mat:Nordic instrument
from SAXLAB equipped with a Rigaku 003+ high brilliance microfocus
Cu-radiation source (wavelength = 1.5406 Å) and a Dectris Pilatus
300K detector. Samples were placed at a distance of 134 mm from the
sample and irradiated for 1800 s. The sample-to-detector distance
was calibrated using silver behenate powder. The SaxsGUI software
was used for data reduction.

The structural characterization was performed
in the 1W2A beamline
of the Beijing Synchrotron radiation Facility (BSRF). Selected samples
were previously fractionated in a Linkam THMS600 hot stage connected
to a liquid nitrogen station. The final heating was performed from
25 to 140 °C at 5 °C/min in a Linkam TST350 hot stage, and
the WAXS patterns were taken simultaneously. An exposure time of 25
s was used, and the patterns were taken every 30 s (i.e., every 2.5
°C). A Pilatus 1M detector collected the scattering patterns
with a resolution of 981 × 1043 pixels (pixel size = 79 ×
79 μm²). The sample-to-detector distance was 121.8
mm, and the wavelength was 1.54 Å.
WAXS experiments, on
selected samples, were performed with transmission geometry at RT.
These experiments were performed on a Xeuss 2.0 system (Xenocs SA),
equipped with a microfocus Cu Kα X-ray source (GeniX3D, 50 kV,
0.6 mA), generating X-ray radiation of a wavelength of 1.54 Å.
The detector used was a Pilatus 300K (DECTRIS, Swiss) with a resolution
of 487 × 619 pixels (pixel size = 172 × 172 μm²). The sample-to-detector distance was 138.61 mm, and exposure
time of 1800 s. The 1D intensity profiles were integrated from background-corrected
2D WAXS patterns with an azimuthal angle range of 0–90°.

For solubilizing conditions
(above the transition
pH, generally above pH 6), samples were measured at three synchrotron
facilities: Beamline B21, Diamond Light Source, UK, beamline 12.3.1,
SIBYLS, Advanced Light Source, Berkeley, USA and beamline SWING, SOLEIL
synchrotron facility, Paris, France.
For phase-separating samples
that display sediment (below the transition pH, generally pH 3–5.5),
measurements were performed using an in-house X-ray scattering system,
with a Genix3D (Xenocs) low divergence Cu Kα radiation source
(wavelength of λ = 1.54 Å) with a Pilatus 300 K (Dectris)
detector and scatterless slits setup^{59 (link)} as
well as beamline I22 at Diamond Light Source. Here, samples were measured
inside 1.5 mm quartz capillaries (Hilgenberg).

DXB measurements were performed using the BL39XU beamline (SPring-8, Japan). The X-ray beam was monochromatized to 15.2 keV using a Si 111 double-crystal monochromator. Monochromatic X-rays were focused to a spot of ∼ 0.52 μm × 0.77 μm using K–B mirrors. The sample-to-detector distance was 85 mm, and 2,000 time-resolved diffraction images from silver halide nanocrystals immobilized on the polyimide film were recorded on a 2D photon-counting detector (Pilatus 300 K, Dectris Switzerland). The exposure time per frame and interval time were set to 50.0 and 53.0 ms, respectively.

GM solution was extruded through a 1 mm tube into DMF and left for 30 s to obtain a filament. Three positions from the edge to the center of this filament were selected for study. Experiments were conducted on Xeuss 2.0 SAXS system (Xenocs, France) with a Pilatus 300K (Dectris) detector using Cu Kα radiation (50 kV, 60 mA) and an exposure time of 10 min. The sample‐detector distance was 294 mm, which was calibrated using silver behenate. 1D scattering profiles were reduced from the 2D data using Foxtrot.