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Easily accessible linear and hyperbranched polyesters as solid polymer electrolytes
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DOI：10.1016/j.eurpolymj.2024.112965.png)
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Abstract
En 中文
Herein we report synthesis, characterization, thermal properties, ionic conductivity and oxidative stability of novel linear and hyperbranched polyesters. Tri-acrylate ester of commercially available 1,1,1-Tris(hydroxymethyl)propane ( M1 ) was used as the primary building block for the synthesis of linear and hyperbranched polymers. A3 + B2 type polycondensation between M1 and dithiols of two different chain lengths (C3, C6) by 100 % atom efficient thiol-acrylate Michael addition reaction, followed by consumption of the unreacted acrylate esters (in the linear or terminal units) with 1-butane thiol produced two hyperbranched polymer namely HB-P1 and HB-P2 . For synthesis of linear analogues, one of the equivalent acrylate esters was reacted first with 1-butane thiol and the resulting di-acrylate monomer was polymerized with the C3 and C6-dithiols, producing linear polymers L -P1 and L -P2 . All the polymers showed molecular weight ( M n ) in the range of 5000 -6000 gmol - 1 with low dispersity. TGA analysis revealed sufficient thermal stability of the polymers for the application as solid polymer electrolyte. All the polymers are amorphous, showing only a glass transition in the range of - -45 degrees C (C3 spacer) to - 50 degrees C (C6 spacer) and no crystallization peak. In presence of lithium bis(trifluoromethanesulfonyl) imide (LiTFSI) salt the T g increased by - 10 degrees C. Solid polymer electrolytes were prepared by incorporating LiTFSI at a molar ratio of polymer carbonyl units to lithium of C = O/Li of 10 and ionic conductivity ( sigma) was evaluated by electrochemical impedance spectroscopy (EIS). Moderate values in the range of 10 -7 S cm - 1 were obtained at 25 degrees C with slightly higher values for the linear polymers. The ionic conductivity increased up to - 2 orders of magnitude at higher temperatures. The oxidative stability of the polymer electrolytes against lithium-metal electrodes revealed onset potential for the first degradation in the range of 3.8 V, indicating moderate stability that might be suitable for testing applications in all-solid-state lithium-metal batteries using sulfur or lithium iron phosphate cathodes.
Keywords:
Thiol-acrylate Michael addition reaction
Polyester synthesis
Linear and hyperbranched polymer
Solid polymer electrolytes
Lithium-ion conductivity
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