Interface 1000

Cyclic voltammetry measurements were conducted with a Gamry Interface 1000 potentiostat using a glassy carbon working electrode (0.071 cm² surface area), a platinum wire counter electrode, and a silver wire pseudo-reference electrode. Prior to use, the working electrode was polished with aqueous alumina slurry, and both the working and counter electrodes were cleaned by washing sequentially with water, ethanol, acetone, and dichloromethane and then sonicating in dichloromethane for 15 min. A three-neck electrochemical cell was washed and oven-dried prior to use. Measurements were taken at a scan rate of 200 mV s⁻¹ under a nitrogen atmosphere using a 25 mL volume of 0.1 M (n-Bu)₄NPF₆ in dichloromethane. Potentials were referenced to ferrocene and adjusted to be presented relative to SCE by adding 0.380 V. In the presence of the supporting electrolyte, MPC-1–2 exhibited limited solubility. Voltammograms were obtained for the solvent blank, and after each sequential addition of MPC-1–2, ferrocene, halide 4b, and Hantzsch ester to the electrochemical cell (Supplementary Fig. 56).

The morphology of the obtained samples was investigated by a LEO 1530 field emission SEM and a JEOL‐2100 TEM (JEOL, GmbH, Eching, Germany) at 200 kV. XRD Patterns were collected using a Bruker D8 diffractometer with Cu_Kα radiation. N₂ adsorption‐desorption isotherms were conducted by using Quantachrome Autosorb‐1 systems at 77 K. Specific surface areas were calculated by using the Brunauer‐Emmett‐Teller (BET) method based on a multipoint analysis. The chemical states of the elements in the samples were characterized using X‐ray photoelectron spectroscopy (XPS) with an ESCA‐Lab‐220i‐XL X‐ray Photoelectron Spectrometer (Thermo Fisher Scientific) with Al_Kα sources (hν=1486.6 eV). The Raman spectra were obtained using a LabRAM HR Evolution Raman spectrometer with a HeNe laser as the excitation line at λ=633 nm. Thermogravimetric analysis was carried out on PerkinElmer (TGA 8000) in the temperature range of 30–900 °C at a heating rate of 10 °C min⁻¹ under argon. The electrochemical impedance spectroscopy (EIS) was recorded on GAMRY Interface 1000 within a frequency range from 100 kHz to 0.01 Hz.

A Gamry Interface
1000 potentiostat (Gamry Instruments, US) was used for electrochemical
impedance spectroscopy (EIS), linear sweep voltammetry (LSV), and
lithium transference number evaluations. The ionic conductivities
of the polymer blends were evaluated via EIS in stainless steel (SS)
symmetric cells (SS|PEO-ppz|SS); spectra were measured in a frequency
range from 1 MHz to 0.01 Hz across a range of temperatures. At each
temperature, the sample was allowed to equilibrate for 30 min before
analysis. LSV was performed in a range from the open circuit voltage
(OCV) to 5.5 V at 0.2 mV s^–1 in an asymmetric cell
(Li|PEO-pTFAP2Li|SS). The lithium transference number was measured
using the Bruce–Vincent method,^{49 (link)} with a combination of DC polarization via chronoamperometry and
EIS (before and after polarization). The Li|PEO-pTFAP2Li|Li symmetric
cell was prepared inside an argon-filled glovebox before measuring
the initial resistance (R₀), then subjecting
it to a DC bias of 10 mV to get the initial (I₀) and steady state (I_SS) currents
and finally measuring the steady state resistance (R_SS). Galvanostatic charge–discharge cycling of
LFP|PEO-pTFAP2Li|Li cells at 0.05 and 0.2 C were measured on an Arbin
testing system (Model No. BT2X43; Arbin Instrument, US) at 100 °C.

In-plane conductivity of all films was measured using a four-point conductivity cell (BekkTech BT-110) employed with a Gamry Interface 1000 potentiostat [30 (link)]. A rectangular section of the film (length: >1.0 cm, width (W): 0.5 cm) was cut and placed in the conductivity cell. The cell was then placed in DI water (500 mL), and electrochemical impedance spectroscopy (EIS) was performed after stabilization of the open circuit potential (frequency: 10 Hz–1 MHz, AC voltage: 10 mV). The EIS data were analyzed in Gamry Echem Analyst software and the resistance, R (Ω), obtained from the Nyquist plot. The ionic conductivity, σ, was measured as follows: $\sigma =\frac{L}{RWT}$
where L, W and T are the distance between two electrodes (0.5 cm), the width and the thickness of the film, respectively.

The specimens were cut to sizes of 15 × 15 × 10 mm. They were connected to an insulated electrical lead wire and mounted using an epoxy. Then, the cross-section of the specimen was prepared through grinding and polishing using #2000 SiC paper and diamond paste (3 μm), respectively. The polished cross-section, except for an area of 0.09 cm², was electrically insulated with a resin. According to ASTM G108, a double loop-electrochemical potentiokinetic reactivation (DL-EPR) test was performed [40 ]. The test solution was 0.5 M H₂SO₄ + 0.01 M KSCN at 30 °C and was deaerated at a rate of 200 mL N₂/min for 30 min. A DL-EPR test was performed using a potentiostat (Interface 1000, Gamry Instruments, Warminster, PA, USA). Pt wire and a saturated calomel electrode were used as the counter and reference electrodes, respectively. Anodic scan to vertex potential (+400 mV(SCE)) and reactivation were swept, and the scan rate was at a rate of 1.677 mV/s. According to the standard [39 ], the ratio of Ir/Ia was determined, indicating the degree of sensitization (DOS).
After the test, the specimen was taken out and ultrasonically cleaned, and the cross-section was observed using an optical microscope (AXIOTECH 100 HD, ZEISS, Oberkochen, Germany).