Abstract The 3D freeze printing (3DFP) of nanocellulose aerogels are demonstrated with large‐scale aligned pore orientations as a sustainable alternative to current acoustical materials. In contrast with the unidirectional pore network orientations obtained from current 3DFP techniques, a bidirectional orientation is achieved by using an inhomogeneous printing substrate to alter the thermal gradient within the print volume. The microstructural morphology shows that bidirectional printing results in a 2D pore orientation, with comparatively thinner pore walls and larger pore widths. Acoustic measurements reveal that altering the pore network characteristics significantly affects the acoustical behavior of the printed CNC aerogels; the wider pores allow the bidirectional CNC aerogels to provide higher sound absorption performance at lower frequencies than the unidirectional samples. Notably, both 3D Freeze printed CNC aerogels provide substantially higher sound transmission loss performance as compared to current acoustical materials. The unidirectional pore structure results in CNC aerogels with higher stiffness and improved energy absorption performance, with both 3D freeze printed CNC aerogels outperforming other CNC aerogel materials in their stiffness‐to‐density ratios. The ability to simultaneously control their pore orientation and macrostructural geometry paves the way for printing complex shaped CNC aerogel structures for multifunctional noise control applications.
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Additive Manufacturing of Poly(phenylene Sulfide) Aerogels via Simultaneous Material Extrusion and Thermally Induced Phase Separation
Abstract Additive manufacturing (AM) of aerogels increases the achievable geometric complexity, and affords fabrication of hierarchically porous structures. In this work, a custom heated material extrusion (MEX) device prints aerogels of poly(phenylene sulfide) (PPS), an engineering thermoplastic, via in situ thermally induced phase separation (TIPS). First, pre‐prepared solid gel inks are dissolved at high temperatures in the heated extruder barrel to form a homogeneous polymer solution. Solutions are then extruded onto a room‐temperature substrate, where printed roads maintain their bead shape and rapidly solidify via TIPS, thus enabling layer‐wise MEX AM. Printed gels are converted to aerogels via postprocessing solvent exchange and freeze‐drying. This work explores the effect of ink composition on printed aerogel morphology and thermomechanical properties. Scanning electron microscopy micrographs reveal complex hierarchical microstructures that are compositionally dependent. Printed aerogels demonstrate tailorable porosities (50.0–74.8%) and densities (0.345–0.684 g cm−3), which align well with cast aerogel analogs. Differential scanning calorimetry thermograms indicate printed aerogels are highly crystalline (≈43%), suggesting that printing does not inhibit the solidification process occurring during TIPS (polymer crystallization). Uniaxial compression testing reveals that compositionally dependent microstructure governs aerogel mechanical behavior, with compressive moduli ranging from 33.0 to 106.5 MPa.
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- Award ID(s):
- 2104856
- PAR ID:
- 10478160
- Publisher / Repository:
- Wiley Blackwell (John Wiley & Sons)
- Date Published:
- Journal Name:
- Advanced Materials
- Volume:
- 36
- Issue:
- 34
- ISSN:
- 0935-9648
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
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