US 11,884,002 B2
Additive manufacturing of hierarchical three- dimensional micro-architected aerogels
Marcus A. Worsley, Livermore, CA (US); Xiaoyu Zheng, Livermore, CA (US); Patrick G. Campbell, Livermore, CA (US); Eric Duoss, Livermore, CA (US); James Oakdale, Livermore, CA (US); Christopher Spadaccini, Livermore, CA (US); and Ryan Hensleigh, Livermore, CA (US)
Assigned to Lawrence Livermore National Security, LLC, Livermore, CA (US); and Virginia Polytechnic Institute and State University, Blacksburg, VA (US)
Appl. No. 17/049,934
Filed by Lawrence Livermore National Security, LLC, Livermore, CA (US); and Virginia Polytechnic Institute and State University, Blacksburg, VA (US)
PCT Filed Apr. 5, 2019, PCT No. PCT/US2019/026142
§ 371(c)(1), (2) Date Oct. 22, 2020,
PCT Pub. No. WO2019/209493, PCT Pub. Date Oct. 31, 2019.
Claims priority of provisional application 62/662,064, filed on Apr. 24, 2018.
Prior Publication US 2021/0237344 A1, Aug. 5, 2021
Int. Cl. B01J 13/00 (2006.01); B29C 64/124 (2017.01); B33Y 10/00 (2015.01); B33Y 70/00 (2020.01); C08K 3/04 (2006.01); C01B 32/194 (2017.01); C01B 32/198 (2017.01); B29C 64/30 (2017.01); B33Y 40/20 (2020.01); C08F 283/06 (2006.01); C08J 9/28 (2006.01); B29K 105/00 (2006.01)
CPC B29C 64/124 (2017.08) [B01J 13/0091 (2013.01); B29C 64/30 (2017.08); B33Y 10/00 (2014.12); B33Y 40/20 (2020.01); B33Y 70/00 (2014.12); C01B 32/194 (2017.08); C01B 32/198 (2017.08); C08F 283/065 (2013.01); C08J 9/286 (2013.01); C08K 3/042 (2017.05); B29K 2105/0061 (2013.01); C01B 2204/22 (2013.01); C01B 2204/26 (2013.01); C01B 2204/32 (2013.01); C01P 2002/82 (2013.01); C01P 2004/03 (2013.01); C01P 2006/10 (2013.01); C08J 2205/026 (2013.01); C08J 2333/08 (2013.01)] 14 Claims
OG exemplary drawing
 
1. A method for making a three-dimensional micro-architected aerogel, comprising:
(a) curing a reaction mixture comprising a co-sol-gel material and at least one catalyst to obtain a crosslinked co-sol-gel, wherein step (a) comprises curing the reaction mixture at a temperature of 100° C. or less;
(b) providing a photoresin comprising a solvent, a photoinitiator, a crosslinkable polymer precursor, and a dispersion of the crosslinked co-sol-gel;
(c) curing the photoresin using projection microstereolithography layer-by-layer to produce a wet gel having a pre-designed three-dimensional structure;
(d) drying the wet gel to produce a dry gel; and
(e) pyrolyzing the dry gel to produce a three-dimensional micro-architected aerogel.