Effect of the Gel Drying Method on Properties of Semicrystalline Aerogels Prepared with Different Network Morphologies

The purpose of this study was to investigate the effect of different drying methods on the structure and properties of semicrystalline polymer aerogels. Aerogels, consisting of either globular or strut-like morphologies, were prepared from poly(ether ether ketone) (PEEK) or poly(phenylene sulfide) (...

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Main Authors: Glenn A. Spiering, Garrett F. Godshall, Robert B. Moore
Format: Article
Language:English
Published: MDPI AG 2025-06-01
Series:Gels
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Online Access:https://www.mdpi.com/2310-2861/11/6/447
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author Glenn A. Spiering
Garrett F. Godshall
Robert B. Moore
author_facet Glenn A. Spiering
Garrett F. Godshall
Robert B. Moore
author_sort Glenn A. Spiering
collection DOAJ
description The purpose of this study was to investigate the effect of different drying methods on the structure and properties of semicrystalline polymer aerogels. Aerogels, consisting of either globular or strut-like morphologies, were prepared from poly(ether ether ketone) (PEEK) or poly(phenylene sulfide) (PPS) and dried using vacuum drying, freeze-drying, or supercritical CO<sub>2</sub> extraction. Vacuum drying was found to result in aerogels with a higher shrinkage, smaller mesopores (with pore widths of 2–50 nm), and smaller surface areas compared to the use of supercritical extraction as the drying method. Freeze-dried aerogels tended to have properties between those of vacuum-dried aerogels and aerogels prepared with supercritical extraction. High network connectivity was found to lead to improved gel modulus, which increased the ability of aerogels to resist network deformation due to stresses induced during drying. The PEEK and PPS aerogel networks consisting of highly connected strut-like features were considerably stiffer than those composed of globular features, and thus shrank less under the forces induced by vacuum drying or freeze-drying. The aerogels prepared from PPS were found to have larger mesopores and smaller surface areas than the aerogels prepared from PEEK. The larger mesopores of the PPS aerogels induced lower capillary stresses on the aerogel network, and thus shrank less. This work demonstrates that preparing PEEK and PPS gels with strut-like features can allow aerogel processing with simpler evaporative drying methods rather than the more complex supercritical drying method.
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spelling doaj-art-591f51c5b4b8424cbebc8dbb3c1e89952025-08-20T03:27:02ZengMDPI AGGels2310-28612025-06-0111644710.3390/gels11060447Effect of the Gel Drying Method on Properties of Semicrystalline Aerogels Prepared with Different Network MorphologiesGlenn A. Spiering0Garrett F. Godshall1Robert B. Moore2Department of Chemistry, Macromolecules Innovation Institute, Virginia Tech, Blacksburg, VA 24061, USADepartment of Chemistry, Macromolecules Innovation Institute, Virginia Tech, Blacksburg, VA 24061, USADepartment of Chemistry, Macromolecules Innovation Institute, Virginia Tech, Blacksburg, VA 24061, USAThe purpose of this study was to investigate the effect of different drying methods on the structure and properties of semicrystalline polymer aerogels. Aerogels, consisting of either globular or strut-like morphologies, were prepared from poly(ether ether ketone) (PEEK) or poly(phenylene sulfide) (PPS) and dried using vacuum drying, freeze-drying, or supercritical CO<sub>2</sub> extraction. Vacuum drying was found to result in aerogels with a higher shrinkage, smaller mesopores (with pore widths of 2–50 nm), and smaller surface areas compared to the use of supercritical extraction as the drying method. Freeze-dried aerogels tended to have properties between those of vacuum-dried aerogels and aerogels prepared with supercritical extraction. High network connectivity was found to lead to improved gel modulus, which increased the ability of aerogels to resist network deformation due to stresses induced during drying. The PEEK and PPS aerogel networks consisting of highly connected strut-like features were considerably stiffer than those composed of globular features, and thus shrank less under the forces induced by vacuum drying or freeze-drying. The aerogels prepared from PPS were found to have larger mesopores and smaller surface areas than the aerogels prepared from PEEK. The larger mesopores of the PPS aerogels induced lower capillary stresses on the aerogel network, and thus shrank less. This work demonstrates that preparing PEEK and PPS gels with strut-like features can allow aerogel processing with simpler evaporative drying methods rather than the more complex supercritical drying method.https://www.mdpi.com/2310-2861/11/6/447aerogelxerogelcryogelgel drying methodssemicrystalline polymer aerogelaromatic polymers
spellingShingle Glenn A. Spiering
Garrett F. Godshall
Robert B. Moore
Effect of the Gel Drying Method on Properties of Semicrystalline Aerogels Prepared with Different Network Morphologies
Gels
aerogel
xerogel
cryogel
gel drying methods
semicrystalline polymer aerogel
aromatic polymers
title Effect of the Gel Drying Method on Properties of Semicrystalline Aerogels Prepared with Different Network Morphologies
title_full Effect of the Gel Drying Method on Properties of Semicrystalline Aerogels Prepared with Different Network Morphologies
title_fullStr Effect of the Gel Drying Method on Properties of Semicrystalline Aerogels Prepared with Different Network Morphologies
title_full_unstemmed Effect of the Gel Drying Method on Properties of Semicrystalline Aerogels Prepared with Different Network Morphologies
title_short Effect of the Gel Drying Method on Properties of Semicrystalline Aerogels Prepared with Different Network Morphologies
title_sort effect of the gel drying method on properties of semicrystalline aerogels prepared with different network morphologies
topic aerogel
xerogel
cryogel
gel drying methods
semicrystalline polymer aerogel
aromatic polymers
url https://www.mdpi.com/2310-2861/11/6/447
work_keys_str_mv AT glennaspiering effectofthegeldryingmethodonpropertiesofsemicrystallineaerogelspreparedwithdifferentnetworkmorphologies
AT garrettfgodshall effectofthegeldryingmethodonpropertiesofsemicrystallineaerogelspreparedwithdifferentnetworkmorphologies
AT robertbmoore effectofthegeldryingmethodonpropertiesofsemicrystallineaerogelspreparedwithdifferentnetworkmorphologies