时间稳定的超分子聚合物盐实现高性能 3D 全芳香族聚酰亚胺晶格,Small

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时间稳定的超分子聚合物盐实现高性能 3D 全芳香族聚酰亚胺晶格
Small ( IF 13.0 ) Pub Date : 2023-05-10 , DOI: 10.1002/smll.202303188
Cody W Weyhrich ₁ , John W Will _{2,

3} , Garvit Nayyar ₄ , Clarissa C Westover ₅ , Steven Patterson ₆ , Clay B Arrington ₁ , Christopher B Williams _{3,

7} , Timothy E Long _{1,

4}

Affiliation

还原光聚合 (VP) 增材制造 (AM) 是选择性地应用紫外线将光活性聚合物固化成微米级分辨率的复杂几何形状，其脂肪族热固性材料的选择有限，且热性能相对较差。与含丙烯酸酯的亲核试剂进行开环二酐生成二丙烯酸酯-二羧酸，在与溶液中的芳香族二胺中和后，可产生光活性聚酰亚胺（PI）前体（称为聚盐）。原位 FTIR 光谱与溶液和光流变测量相结合，揭示了由于氮杂迈克尔加成而导致的 4,4'-二氨基二苯胺 (ODA) 聚盐的先前未知的时间依赖性不稳定性。用含吸电子砜的单体例如4,4'-二氨基二苯砜(DDS)替换含给电子醚的二胺，阻止了芳香族胺与活化的丙烯酸酯双键的氮杂-迈克尔加成。新型 DDS 聚盐光固化解决方案也经过类似分析和验证的长期稳定性，从而实现了聚酰亚胺有机凝胶中间体的可重复印刷。随后的 VP AM 提供了复杂复杂的 3 维 (3D) 结构和出色的表面光洁度，正如扫描电子显微镜所证明的那样。此外，新颖的 PMDA-HEA/DDS 解决方案能够生产出第一个由全芳香族聚酰亚胺组成的梁网格结构。通过使用交替的聚盐成分打印零件，进一步证明了聚盐平台用于多材料打印的多功能性。

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Temporally Stable Supramolecular Polymeric Salts Enabling High-Performance 3D All-Aromatic Polyimide Lattices

Vat photopolymerization (VP) Additive Manufacturing (AM), in which UV light is selectively applied to cure photo-active polymers into complex geometries with micron-scale resolution, has a limited selection of aliphatic thermoset materials that exhibit relatively poor thermal performance. Ring-opening dianhydrides with acrylate-containing nucleophiles yielded diacrylate ester-dicarboxylic acids that enabled photo-active polyimide (PI) precursors, termed polysalts, upon neutralization with an aromatic diamine in solution. In situ FTIR spectroscopy coupled with a solution and photo-rheological measurements revealed a previously unknown time-dependent instability of 4,4′-oxydianiline (ODA) polysalts due to an aza-Michael addition. Replacement of the electron-donating ether-containing diamine with an electron withdrawing sulfone-containing monomer, e.g., 4,4′-diaminodiphenyl sulfone (DDS), prohibited the aza-Michael addition of the aromatic amine to the activated acrylate double bond. Novel DDS polysalt photocurable solutions are similarly analyzed and validated long-term stability, which enabled reproducible printing of polyimide organogel intermediates. Subsequent VP AM afforded 3-dimensional (3D) structures of intricate complexity and excellent surface finish, as demonstrated with scanning electron microscopy. In addition, the novel PMDA-HEA/DDS solution enabled the production of the first beam latticed architecture comprised of all-aromatic polyimide. The versatility of a polysalt platform for multi-material printing is further demonstrated by printing parts with alternating polysalt compositions.

更新日期：2023-05-10

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