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Herein, we report the aqueous miscible organic solvent treatment (AMOST) of borate-intercalated layered double hydroxides (LDHs), forming highly exfoliated Mg3Al-LDH nanosheets, and evaluate them as high surface area supports for polyethyleneimine (PEI)-based direct air capture (DAC). Compared with carbonate-intercalated Mg3Al-LDH, the borate-intercalated analogue undergoes substantially greater AMOST-induced exfoliation, producing predominantly mono-\/few-layer nanosheets with a very high specific surface area of 762 m2 g\u20131 and a total pore volume of 3.02 cm3 g\u20131. The high surface area and porosity allow incorporation using a nominal PEI loading of 67 wt %, enabling direct comparison of the carbonate- and borate-derived support architectures. Under humid breakthrough conditions at 400 ppm CO2\/N2 and 25 \u00b0C, the borate-derived PEI-Mg3Al-LDH composite can achieve a high CO2 uptake of 2.90 mmol g\u20131, reaching 78% capacity in 20 min, demonstrating fast sorption kinetics. The sorbent also exhibits 96 % capacity retention after 20 adsorption\u2013desorption cycles \u2013 competitive with reported PEI-supported solid amine sorbents measured under comparable dry DAC conditions. These results establish borate-assisted LDH exfoliation as a promising strategy for preparing high surface area supports for solid amine DAC sorbents.<\/jats:p>","DOI":"10.1021\/acsami.6c17102","type":"journal-article","created":{"date-parts":[[2026,10,19]],"date-time":"2026-10-19T11:02:28Z","timestamp":1792407748000},"page":"58210-58225","source":"Crossref","is-referenced-by-count":0,"title":["Polyethyleneimine-Impregnated Exfoliated Layered Double Hydroxide-Based Nanosheets for Direct Air Capture of CO2"],"prefix":"10.1021","volume":"18","author":[{"given":"Matthew R. 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