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The process utilizes 1,4,5,8\u2010naphthalenetetracarboxylic anhydride and urea as reactants, replacing traditional toxic organic solvents with water and ethanol. This investigation explores the effects of various reaction conditions, such as the water\u2010to\u2010ethanol volume ratio, reaction time, and temperature, on product morphology, resulting in distinct structures like sheets, columns, and layers. Notably, hollow square\u2010tubular polyimides (HST\u2010PIs) are synthesized under specific conditions: a 2:1 water\u2010to\u2010ethanol volume ratio, 24 h reaction time, and 200 \u00b0C temperature. This study attributes self\u2010assembly to three primary non\u2010covalent interactions: hydrogen bonding, \u03c0\u2013\u03c0 stacking, and hydrophobic interactions. The gel permeation chromatography (GPC) analysis indicates that the PIs molecular weight predominantly ranges from 10 000 to 15 000. As an electrode material, hollow square tubular polyimides (HST\u2010PIs) exhibit an initial discharge capacity of 297.9 mAh\u00b7g\n                    <jats:sup>\u22121<\/jats:sup>\n                    at a current rate of 0.1 C, with a coulombic efficiency of 79%. After ten cycles, the coulombic efficiency improves to 97% and maintains above 98% in the subsequent cycles. This study presents an innovative and environmentally friendly method for the molecular self\u2010assembly of hollow tubular organic polymers.\n                  <\/jats:p>","DOI":"10.1002\/smtd.202500251","type":"journal-article","created":{"date-parts":[[2025,4,30]],"date-time":"2025-04-30T03:29:53Z","timestamp":1745983793000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Solvothermal Self\u2010Assembly of Hollow Square\u2010Tubular Polyimides for Aqueous Batteries"],"prefix":"10.1002","volume":"10","author":[{"given":"Ya","family":"Zhao","sequence":"first","affiliation":[{"name":"College of Environmental and Chemical Engineering Dalian University  Dalian Liaoning 116622 China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Chaoqiao","family":"Yang","sequence":"additional","affiliation":[{"name":"College of Environmental and Chemical Engineering Dalian University  Dalian Liaoning 116622 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