Thms600

Simultaneous in situ small-angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS) experiments were performed at the ALBA Synchrotron facility in Barcelona (Spain), beamline BL11-NCD. A Linkam THMS600 (Linkam, Surrey, UK) hot stage coupled to a liquid nitrogen cooling system was used to cool and heat the samples, which were previously placed into glassy capillaries. The same thermal protocol adopted in the non-isothermal DSC experiments was used to get the SAXS/WAXS patterns, in which crystallization and melting of the samples are followed, thus obtaining comparable results by the two different techniques.
The X-ray energy source was 12.4 keV (λ = 1.03 Å). For the SAXS setup, the distance between the sample and the detector (ADSC Q315r detector, Poway, CA, USA, with a resolution of 3070 × 3070 pixels, pixel size of 102 µm²) was 6463 mm with a tilt angle of 0°. Calibration was performed with silver behenate. Regarding WAXS configuration, a distance of 132.6 mm was used between the sample and the detector, with a tilt angle of 21.2°. Chromium (III) oxide (Rayonix LX255-HS detector, Evanston, IL, USA, with a resolution of 1920 × 5760 pixels, pixel size of 44 µm²) was employed for calibration. Scattering intensity as a function of scattering vector, q = 4πsinθλ⁻¹ data are obtained, where λ is the X-ray wavelength, and 2θ is the scattering angle.

Raman spectroscopy for the electrolyte structure was conducted on Horiba LabRAM HR Evolution microscope. Raman spectroscopy for low temperature and in situ batteries was tested by confocal Thermo-Fisher Scientific DXR microscope. Both of them used a 532 nm excitation laser. DSC was carried out in METTLER TOLEDO DSC3 in the procedure of +25~−150 °C with a cooling rate of 10 K min⁻¹, constant temperature for 2 mins and –150~+25 °C with a heating rate of 5 K min⁻¹. The polarizing microscope was using Olympus BX51TRF. The refrigerating system for low-temperature characterizations is Linkam THMS600. NMR was characterized on Bruker ASCEND400. XPS was conducted on X-ray Photoelectron Spectrometer (Axis Ultra DLD) with an excitation source of Al K_α X-ray.

Optical properties of single crystals were observed using a polarizing microscope (Olympus, BX51-P) with the combination of a temperature controller (Linkam, TMS92) and a hot stage (Linkam, THMS600) (Supplementary Fig. 12). The interference colours were converted into the optical anisotropic parameters of the optical retardations using the Michel Levy birefringence chart (Nikon interference colour chart) and a Berek compensator (Olympus, U-CBE) under observations with white light. The Δn values were obtained from the optical retardation (R) and thickness of the crystal (t). The thicknesses of the crystals were measured using a confocal laser microscope with a × 50 objective lens (Keyence, VK-9500).

Raman spectra were measured by a confocal Raman spectroscope (JY Horiba HR800). The excitation laser is 532 nm (2.33 eV), and was focused on the sample through a 50× objective. The excitation power was kept below 1 mW. The circularly polarized light was generated by a polarizer and a quarter-wave plate. Helicity-resolved Raman spectra were measured by rotating a polarizer in the collection light path (Supplementary Fig. 2). The variation of temperature was realized by a cryogenic chamber (Linkam THMS600), which was refrigerated by liquid nitrogen. After being exfoliated onto the 300 nm SiO₂/Si substrate, the 1T-TaS₂ sample was subsequently (<30 min) put into the cryostat, and the sample was protected by the argon (Ar) atmosphere to avoid oxidation.

The liquid crystalline texture and the alignment of the columns were investigated by POM for bulk HAT6. The measurements were carried out by using a Zeiss Axioskop Scope A1 optical microscope, with crossed polarizers, connected to a Linkam THMS600 heating stage. The stage was equipped with a liquid nitrogen Dewar allowing a precise control of heating and cooling rates.
The ITO-coated liquid crystalline cell used in the DS measurement was also employed for the POM investigations. The temperature program applied for the DS measurements was also used for the POM measurements.

The ice
recrystallization inhibition (IRI) activity of the PEG and PVA polymers
was measured using a modified splat assay.^{59 (link)} A 10 μL sample of each polymer dissolved in SM buffer II was
dropped 1.4 m onto a chilled glass coverslip placed on an aluminum
plate on dry ice. Upon hitting the chilled coverslip, an ice wafer
was formed instantaneously. The glass coverslip was transferred to
a Linkam THMS600 cryostage and left to anneal at −8 °C
under a N₂ atmosphere for 30 min after taking an initial
photograph at t = 0. Photographs (initial and after
30 min of annealing) were collected using an Olympus CX 41 microscope
with a UIS-2 20×/0.45/∞/0-2/FN22 lens and crossed polarizers
(Olympus Ltd., Southend-on-Sea, U.K.), which was equipped with a Canon
DSLR 500D digital camera. Processing of each image was conducted using
the freely available Fiji (ImageJ) software.^{60 (link)} In summary, the number of crystals in the 20× magnified images
of the wafers were counted. Average values obtained were compared
to the values of the SM-II buffer controls.

The downconversion photoluminescence measurements
were performed
on an Edinburgh FLS1000 PL spectrometer equipped with a PMT detector
and a 450 W ozone-free Xenon arc lamp as a light source. The powder
samples were placed into a quartz spectrophotometer cell (Starna Cells,
Inc). The excitation and emission scans were collected with a bandwidth
of 3 nm, a dwell time of 0.5 s, and a step size of 1 nm in the measured
range of 350–500 (excitation) and 525–750 nm (emission).
Judd–Ofelt calculations were performed based on the excitation
measurements in the range of 350–550 nm. For upconversion measurements,
an MDL-III-980 laser centered at 980 nm with a power of 2500 mW was
employed as the excitation source and emission spectra were recorded
from 450–750 nm. The system is not equipped with an integrating
sphere, preventing any UC quantum efficiency measurements. The lifetime
measurements were performed with a microsecond flash lamp (frequency:
25 Hz, 1–2 μs pulse) over the range of 10 ms with a 2
ms delay time, resulting in a 5 μs detector response (2000 channels).
The low-temperature measurements were performed using a LINKAM THMS600
temperature-controlled stage, which was added to the spectrometer
setup. Liquid nitrogen was used as the cooling agent.