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Gels 2022, 8, 193 3 of 13 2. Results and Discussion 2.1. Preparation of the B8-BMPTFSI Ionogel and Insights into the Mechanism of Self-Assembly and Thixotropy To prepare a B8-BMPTFSI ionogel, an appropriate amount of B8 was added into a certain volume of BMPTFSI, which was stirred at 60 ◦C. After B8 was completely dissolved, the hot solution was cooled to 25 ◦C for 20 min, affording the B8-BMPTFSI ionogel. The critical gelation concentration (CGC) of the B8-BMPTFSI ionogel was 0.7% (w/v), and the ionogel was thermal-reversible, the sol–gel phase inversion temperature (Tg) of the 0.7% (w/v) B8-BMPTFSI ionogel was 76.4 ◦C. The B8-BMPTFSI ionogel exhibited hysteresis-free thixotropic behavior, and corresponding rheological data (Figure 1a) indicated that the gel Gels 2022, 8, x FOR PEER REVIEW 4 of 14 can recover itself after damage by shear force, and that recovery can be repeated. Figure 1. (a) Step-strain measurements of the B8-BMPTFSI ionogel (2%, w/v) over 2 cycles (with an Figure 1. (a) Staelpte-rsntartainignsmtraeinasouf 0r.e0m5 aenndt1s00o%f twhiethB18H-zBaMt 2P5T°CF)S; (Ibi)oFnTo-IgReslpe(2ct%ra,owf th/evB)8oxvereorge2l acnydclDeMs F(with solution of B8; (c) changes in the 1H NMR shi◦ft of N-H and different O-H groups of B8 in an alternating strain of 0.05 and 100% with 1 Hz at 25 C); (b) FT-IR spectra of the B8 xerogel and BMPTFSI/DMSO-d6 at ratios (v/v) of 40:60 with the increase in the B8 concentration from 5% (w/v) DMF solution of B8; (c) changes in the 1H NMR shift of N-H and different O-H groups of B8 in to 20% (w/v); (d) XRD diffraction pattern of the B8-BMPTFSI ionogel (2%, w/v). The optimized self- BMPTFSI/DMSaOss-edmblaytmraotdioesof(vB/8vo)btoafin4e0d:6b0y wtheitohrethicealicnaclcruelastieonins (tGhaeusBs8ianco0n9cBe3nLtYrPatmioenthfordo)m: (e5)%Th(ew/v) 6 length of the B8 molecule and the distance of a layered structure of B8, the width of the 1D assembly to 20% (w/v); (d) XRD diffraction pattern of the B8-BMPTFSI ionogel (2%, w/v). The optimized of B8, and the C-Cl‧‧‧H-N H-bonding interaction between B8 molecules; (f) the distance between the self-assembly mode of B8 obtained by theoretical calculations (Gaussian 09 B3LYP method): (e) The side chains of A8, the C=O...H-N interaction between A8 molecules. Color code: C = gray; H = white; length of the B8Om=oreledc; Nul=ebalnued; Cthl =egdriesetna.nce of a layered structure of B8, the width of the 1D assembly of B8, and the C-Cl· · · H-N H-bonding interaction between B8 molecules; (f) the distance between X-ray diffraction (XRD) patterns of the B8-BMPTFSI ionogel (Figure 1d) were rec- the side chains of A8, the C=O . . . H-N interaction between A8 molecules. Color code: C = gray; orded to obtain information regarding the self-assembly of B8. Three clear reflection peaks H = white; O = red; N = blue; Cl = green. corresponding to d-spacings of 29.57 Å, 14.51 Å, and 9.87 Å in a ratio of 1: 1/2: 1/3 were observed, respectively, suggesting the presence of a lamellar structure with a periodicity of 29.57 Å in the gel state [35]. The peak corresponding to a d-spacing of 3.56 Å is charac- teristic of the π-π stacking distance, indicative of the presence of π-π interactions betweenPDF Image | Thixotropic Ionogel Electrolyte for Sodium Batteries
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