Defense Date
2025
Document Type
Thesis
Degree Name
Doctor of Philosophy
Department
Chemistry
First Advisor
Everett Carpenter
Second Advisor
Massimo Bertino
Abstract
This dissertation investigates the synthesis, characterization, and scale-up of aerogels derived from both synthetic resorcinol–formaldehyde (RF) and natural polymer (pectin) systems. The work focuses on developing cost-effective, industrially scalable fabrication routes that maintain high surface area, low thermal conductivity, and structural integrity. Phenolic RF aerogels were synthesized using catalysts including sodium silicate, diethylenetriamine (DETA), and 3-aminopropyltrimethoxysilane (APTMS) under freeze-drying and ambient pressure drying (APD) conditions. APTMS-based systems achieved surface areas above 600 m²/g with 30 to 50 percent lower shrinkage than conventional formulations. Camphene was introduced as a novel APD solvent, producing aerogels with pore architectures comparable to freeze-dried materials and thermal conductivities as low as 23 mW/m·K (R ≈ 4.1 per inch).
Biopolymer-based pectin aerogels were synthesized using sodium silicate as both catalyst and silicate source, enabling drying via tert-butanol or camphene. These gels achieved surface areas up to 80 m²/g, densities of 0.12 g/cm³, and thermal conductivities near 27 mW/m·K. BET and BJH analyses confirmed mesoporosity (10 to 40 nm), while SAXS and SEM verified structural uniformity.
Both aerogel systems were successfully upscaled to 14 cm × 14 cm × 1 cm panels through mold-assisted gelation and controlled solvent exchange. Cost modeling indicates that large-scale pectin aerogel production with greater than 99.9 percent solvent recovery can be economically competitive with commercial thermal insulators. This research bridges laboratory-scale synthesis and industrial feasibility, providing mechanistic and process insights essential for scalable, sustainable aerogel manufacturing.
Rights
© The Author
Is Part Of
VCU University Archives
Is Part Of
VCU Theses and Dissertations
Date of Submission
10-9-2025