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DOE OSTI2026

Selective Sorbent Design: CaS Aerogel for Rapid Remediation of Aqueous Pb (II)

Heavy metals are a persistent environmental problem due to their high toxicity, even at very low concentrations (parts per billion, ppb). The removal of such diluted heavy metals is challenging because of the competition the counterions (Ca 2+ , Na + , Mg 2+ , etc.) present in natural water bodies. The design of sorbents capable of removing ions below the action limit (15 ppb for Pb 2+ ) requires a strong driving force for selective uptake and rapid removal. In this work, we report the synthesis of porous CaS aerogels (surface area = 143.6 m 2 /g) by oxidative assembly of CaS nanoparticles and describe their use in selective Pb 2+ ion remediation from water. Despite the presence of amorphous CaCO 3 (up to 50 wt %) in the gel network, the gels demonstrated a capacity of 17.1 mmol Pb/g aerogel (3543 mg/g), and this could be augmented to 22.5 mmol Pb/g aerogel (4593 mg/g) by modifying the synthesis to reduce CaCO 3 content to ca. 15 wt %. Moreover, the selectivity of CaS aerogels toward Pb 2+ ions is high, as evidenced by little-to-no change in the distribution constant (K d ∼ 10 4 ) in the presence of competing ions (1 M) such as Na + , Mg 2+ , and Ca 2+ . During remediation with low concentrations (100 ppb) of Pb 2+ with CaS aerogels, the level of Pb 2+ dropped to 5.4 ppb (below the 15 ppb EPA limit) within 1 h with a 95.4% removal efficiency. In contrast to the CO 2 supercritically dried aerogels, lower surface area ambient dried gels (xerogels) only remove 40% of the lead ions from a 100 ppb solution, saturating within 1 h. The efficiency and rapidity of selective Pb 2+ uptake using CdS aerogels arise from a combination of a strong thermodynamic driving force for cation exchange (K eq = 2.5 × 10 27 ) and chemisorption along with favorable kinetics associated with the high surface area porous architecture. These results show that formation of high surface area metal chalcogenide aerogels by oxidative assembly to form nanocrystalline architectures, as previously demonstrated for II−VI and IV−VI semiconductors, can be extended to the more highly ionic alkaline earth sulfides.

Aerogels↗

DOE OSTI2021

Bismuth-Functionalized Silica Aerogels for Iodine Capture

The U.S. Department of Energy is looking into alternative sorbents for the removal of radioiodine from off-gas streams in a used nuclear fuel reprocessing plant. One class of sorbents considered are bismuth-functionalized silica aerogels which offer an efficient capture of iodine from off-gas streams and are environmentally friendly and lower cost when compared to silver-functionalized sorbents. Two types of bismuth-functionalized silica aerogels were successfully manufactured using a hierarchical synthesis approach:1) The Bi 3+ -aerogel with bismuth oxide nitrate hydroxide hydrate particles and 2) Bi-aerogel with bismuth metal and bismuth sulfide nanoparticles. Both sorbents exhibited high sorption capacity for iodine. However, presence of particles of different composition, size, and distribution on aerogel support resulted in different iodine loadings. The Bi 3+ -aerogel exhibited sorption capacity of 289 mg/g. In contrast, Bi-aerogel exhibited more that 20% higher sorption capacity. The heat-treatment of Bi 3+ -aerogel at 225? under hydrogen atmosphere increased iodine loading capacity to 351 mg/g.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2023

Optimizing Surfactant Templating of Yttria-Stabilized Zirconia Aerogels for High-Temperature Applications: Effect of Anionic and Nonionic Surfactant

Aerogels, mesoporous materials with extreme material properties including high specific surface area, low density, and low thermal conductivity, can be useful for applications including catalysis, sorption media, and drug delivery. The low thermal conductivity and high surface area of aerogels makes them advantageous as thermal management systems, specifically for aerospace or aeronautics applications. However, the pore collapse and subsequent surface area decrease of aerogels following exposure to high temperatures must be mitigated to allow aerogels to be effectively used in thermal management applications. This work investigates the anionic surfactant sodium dodecyl sulfate (SDS) and the nonionic surfactant Pluronic® P-123 as surfactant templates in yttria-stabilized zirconia (YSZ) aerogels. By utilizing surfactant templates, known to influence pore structure, it is anticipated that sintering and densification of the aerogels following high-temperature exposure will be mitigated. It was determined that the addition of SDS and P-123 increased the surface area and pore volume of as-dried aerogels and suppressed crystallite growth at high temperatures. However, the impact of surfactant templates on the surface area and pore volume of heat-treated aerogels was negligible, potentially due to low concentrations of surfactant and the removal of the surfactant following high-temperature exposure.

Yttria-stabilized zirconia aerogels↗

NASA NTRS2024

Post-Synthetic Modification of Yttria-Stabilized Zirconia Aerogels with Silica Coatings for Enhanced Thermal Stability

Maintaining high surface area and porosity at high temperatures is important when considering aerogels for use in thermal management systems. The mesoporous structure of aerogels results in extremely low thermal conductivity, making them lightweight, high performance insulating materials. Maintaining these properties requires innovative routes to suppress sintering and pore collapse as use temperatures rise. The current work aims to improve the pore structure stability of yttria-stabilized zirconia aerogels by the addition of a SiO 2 coating. The functionalization of surface hydroxyl groups by the addition of SiO 2 is hypothesized to mitigate condensation reactions, which are a driving force for shrinkage and pore structure collapse. Zirconia aerogels with 0, 10 and 30 mol% yttria (YO 1.5 ) additions were coated in a tetraethyl orthosilicate (TEOS) solution and exposed to temperatures up to 1200°C. Crystal structure, pore structure, and aerogel morphology were investigated to understand changes in aerogel thermal stability. The SiO 2 coating exhibited a greater influence on pore stability over yttria concentration, with specific surface area of the coated aerogels being twice that of the uncoated aerogels up to 1000°C. However, the presence of the SiO 2 coating promoted rapid sintering and densification at 1200°C, establishing an upper use temperature for SiO 2 and a need to develop other coating chemistries.

aerogel↗

DOE OSTI2023

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.

Chemistry↗

DOE OSTI2020

Thermal and Electrical Properties of Isocyanate Derived Organic Aerogels for Cryogenic Insulation Applications

The use and storage of cryogens such as liquefied nitrogen, helium, hydrogen among others requires reliable and efficient thermal insulation systems. Passive insulation from high performance materials that are well-known for their inherent low thermal conductivity would reduce the overall costs involved in design, manufacture and maintenance of such systems. One such class of materials are referred to as aerogels. These materials are known for their low density, high mesoporosity, high surface areas, low thermal conductivity and high acoustic impedance. Aerogels were invented by S.S. Kistler in 1931 and the most common type are those made of silica. However, the inherent fragility of silica aerogels makes them hard to mass produce, and therefore applications have been limited. A major breakthrough was introduced by our team almost 20 years ago with the invention of polymer crosslinked silica aerogels. Those materials shifted attention to all-polymer aerogels that have overcome all fragility issues associated with their inorganic counterparts. This study focuses on such polymeric aerogels that can be mass produced as large monoliths while maintaining the low thermal conductivity of traditional silica aerogels over a wide temperature range. Manufacturing flexibility of polymeric aerogels allows fabrication of blocks and sheets that can be applied in various configurations to insulate cryogenic and superconducting devices. The thermal conductivity with 80 K and room temperature boundary are reported as well as other properties (electrical), that need to be considered when designing devices for cryogenic applications.

Churu, Gitogo↗

NASA NTRS2005

Silica Aerogels Doped with Ru(II) Tris 1,l0-Phenanthro1ine)-Electron Acceptor Dyads: Improving the Dynamic Range, Sensitivity and Response Time of Sol-Gel Based Oxygen Sensors

Complexes 1 and 2 were characterized in fluid and frozen solution and as dopants of silica aerogels. The intramolecular quenching efficiency of pendant 4-benzoyl-N-methylpyridinium group (4BzPy) is solvent dependent: emission is quenched completely in acetonitrile but not in alcohols. On the other hand, N-benzyl-N'-methylviologen (BzMeV) quenches the emission in all solvents completely. The differences are traced electrochemically to a stronger solvation effect by the alcohol in the case of 1. In fiozen matrices or absorbed on the surfaces of silica aerogel, both 1 and 2 are photoluminescent. The lack of quenching has been traced to the environmental rigidity. When doped aerogels are cooled to 77K, the emission shifts to the blue and its intensity increases in analogy to what is observed with Ru(II) complexes in media undergoing fluid-to-rigid transition. The photoluminescence of 1 and 2 from the aerogel is quenched by oxygen diffusing through the pores. In the presence of oxygen, aerogels doped with 1 can modulate their emission over a wider dynamic range than aerogels doped with 2, and both are more sensitive than aerogels doped with Ru(II) tris(1,l0- phenanthroline). In contrast to frozen solutions, the luminescent moieties in the bulk of aerogels kept at 77K are still accessible, leading to more sensitive platforms for oxygen sensors than other ambient temperature configurations.

Kevebtusm Bucgikas↗

NASA NTRS2010

Aerogel-Positronium Technology for the Detection of Small Quantities of Organic and/or Toxic Materials

The Ps-aerogel system [Ps is positronium (an electron-positron-hydrogen-like atom)] has been evaluated and optimized as a potential tool for planetary exploration missions. Different configurations of use were assessed, and the results provide a quantitative measure of the expected performance. The aerogel density is first optimized to attain maximum production of Ps that reaches the pores of the aerogel. This has been accomplished, and the optimum aerogel density is .70 mg/cm3. The aerogel is used as a concentrator for target volatile moieties, which accumulate in its open porosity over an extended period of time. For the detection of the accumulated materials, the use of Ps as a probe for the environment at the pore surface, has been proposed. This concept is based on two steps: (1) using aerogel to produce Ps and (2) using the propensity of Ps to interact differently with organic and inorganic matter. The active area of such a detector will comprise aerogel with a certain density, specific surface area, and gas permeability optimized for Ps production and gas diffusion and adsorption. The aerogel is a natural adsorber of organic molecules, which adhere to its internal surface, where their presence is detected by the Ps probe. Initial estimates indicate that, e.g., trace organic molecules in the Martian atmosphere, can be detected at the ppm level, which rivals current methods having significantly higher complexity, volume, mass, and power consumption (e.g. Raman, IR).

Petkov, Mihail P.↗

NASA NTRS2005

Nonflammable, Hydrophobic Aerogel Composites for Insulation

Aerogel composites that are both nonflammable and hydrophobic have been developed for use as lightweight thermal- insulation materials for cryogenic systems. Aerogels are well known in the industry for their effectiveness as thermal insulators under cryogenic conditions, but the treatments used heretofore to render them hydrophobic also make them flammable. Nonflammability would make it safer to use aerogel insulation, especially in oxygen-rich environments and on cryogenic systems that contain liquid oxygen. A composite of this type is a silica aerogel reinforced with fibers. In comparison with unreinforced aerogels, the aerogel composite is about ten times as stiff and strong, better able to withstand handling, and more amenable to machining to required shapes. The composite can be made hydrophobic and nonflammable by appropriate design of a sol-gel process used to synthesize the aerogel component. In addition to very low thermal conductivity needed for insulation, aerogel composites of this type have been found to exhibit high resistance to moisture and nonflammability in oxygen-rich atmospheres: Samples floating on water for months gained no weight and showed no signs of deterioration. Samples were found to be nonflammable, even in pure oxygen at atmospheric pressure [14.7 psia (0.10 MPa)]

Redouane, Begag↗

DOE OSTI2020

Durable polymer-aerogel based superhydrophobic coatings: a composite material

Provided are polymer-aerogel composite coatings, devices and articles including polymer-aerogel composite coatings, and methods for preparing the polymer-aerogel composite. The exemplary article can include a surface, wherein the surface includes at least one region and a polymer-aerogel composite coating disposed over the at least one region, wherein the polymer-aerogel composite coating has a water contact angle of at least about 140° and a contact angle hysteresis of less than about 1°. The polymer-aerogel composite coating can include a polymer and an ultra high water content catalyzed polysilicate aerogel, the polysilicate aerogel including a three dimensional network of silica particles having surface functional groups derivatized with a silylating agent and a plurality of pores.

Kissel, David J.↗

DOE OSTI2022

Electrocatalysis of Oxygen Reduction Reaction in a Polymer Electrolyte Fuel Cell with a Covalent Framework of Iron Phthalocyanine Aerogel

Carbon aerogels have been studied in the context of fuel cell electrodes mainly as catalyst support materials due to their high surface area, porosity, and electrical conductivity. Recently, aerogels composed solely of inorganic molecular complexes have shown to be promising materials for the electrocatalysis of oxygen reduction reaction (ORR). These aerogels consist of atomically dispersed catalytic sites. Herein, we report on the synthesis and characterization of an aerogel-based catalyst: iron phthalocyanine aerogel. It was synthesized by coupling of ethynyl-terminated phthalocyanine monomers and then heat-treated at 800 °C to increase its electrical conductivity and catalytic activity. Further, the aerogels reported here were tested as catalysts for ORR in acidic conditions for the first time and found to have a ultra-high number of atomically dispersed catalytic sites (7.11 × 10 20 sites g –1 ) and very good catalytic activity (E onset = 0.9 V vs RHE and TOF = 9.2 × 10 –3 e – s –1 site –1 at 0.8 V vs RHE). The iron phthalocyanine aerogel was also studied in a proton exchange membrane fuel cell, reaching a peak power density of 292 mW cm –2 and an open circuit voltage of 0.83 V.

25 ENERGY STORAGE↗

DOE OSTI2021

Bioinspired aligned magnetic features in aerogels for humidity sensing

Many natural plant tissues, such as pinecones, utilize structures to transduce changes in humidity into movement or strain. These often employ layered structures with aligned features in order to create differential stress across the material as different portions swell at different rates. Here, by replicating these types of structures in synthetic materials we can create structures that respond to humidity in a similar manner. Taking these aligned features as inspiration, silica aerogels with tailored humidity reactive properties were created. This behavior was achieved by creating aligned features in these aerogels using a Helmholtz coil to produce a uniform magnetic field that aligned ferrofluid droplets into chains and needle like features. These magnetite-based structures were shown to retain their superparamagnetic properties, allowing them to easily be removed from the aerogels, leaving a large number of aligned channels. Aerogels with the removed needles experienced significantly different strains than both unmodified aerogels and aerogels with the aligned features still in place. Aerogels with these tunable aligned features could be used in humidity sensors that can transduce changes in humidity into strain and could be used in applications such as volatile organic compound capture.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

An All-Ceramic, Anisotropic, and Flexible Aerogel Insulation Material

To exploit the high-temperature superinsulation potential of anisotropic thermal management materials, the incorporation of ceramic aerogel into the aligned structural networks is indispensable. Yet, the long-standing obstacle to exploring ultralight superinsulation ceramic aerogels is the inaccessibility of its mechanical elasticity, stability, and anisotropic thermal insulation. Here, we report a recoverable, flexible ceramic fiber-aerogel composite with anisotropic lamellar structure, where the interfacial cross-linking between ceramic fiber and aerogel is important in its superinsulation performance. The resulting ultralight aerogel composite exhibits a density of 0.05 g/cm 3 , large strain recovery (over 50%), and low thermal conductivity (0.0224 W m –1 K –1 ), while its hydrophobicity is achieved by in situ trichlorosilane coating with the water contact angle of 135°. The hygroscopic tests of such aerogel composites demonstrate a reversible thermal insulation. The mechanical elasticity and stability of the anisotropic composites, with its soundproof performance, shed light on the low-cost superelastic aerogel manufacturing with scalability for energy saving building applications.

36 MATERIALS SCIENCE↗

NASA NTRS2014

Synthesis, Processing, and Characterization of Inorganic-Organic Hybrid Cross-Linked Silica, Organic Polyimide, and Inorganic Aluminosilicate Aerogels

As aerospace applications become ever more demanding, novel insulation materials with lower thermal conductivity, lighter weight and higher use temperature are required to fit the aerospace application needs. Having nanopores and high porosity, aerogels are superior thermal insulators, among other things. The use of silica aerogels in general is quite restricted due to their inherent fragility, hygroscopic nature, and poor mechanical properties, especially in extereme aerospace environments. Our research goal is to develop aerogels with better mechanical and environmental stability for a variety of aeronautic and space applications including space suit insulation for planetary surface missions, insulation for inflatable structures for habitats, inflatable aerodynamic decelerators for entry, descent and landing (EDL) operations, and cryotank insulation for advance space propulsion systems. Different type of aerogels including organic-inorganic polymer reinforced (hybrid) silica-based aerogels, polyimide aerogels and inorganic aluminosilicate aerogels have been developed and examined.

Insulation materials↗

DOE OSTI2022

Polyimide aerogels for ballistic impact protection

The ballistic performance of edge-clamped monolithic polyimide aerogel blocks (12 mm thickness) has been studied through a series of impact tests using a helium-filled gas gun connected to a vacuum chamber and a spherical steel projectile (approximately 3 mm diameter) with an impact velocity range of 150–1300 m s -1 . The aerogels had an average bulk density of 0.17 g cm -3 with high porosity of approximately 88%. The ballistic limit velocity of the aerogels was estimated to be in the range of 175–179 m s -1 . Moreover, the aerogels showed a robust ballistic energy absorption performance (e.g., at the impact velocity of 1283 m s -1 at least 18% of the impact energy was absorbed). At low impact velocities, the aerogels failed by ductile hole enlargement followed by a tensile failure. By contrast, at high impact velocities, the aerogels failed through an adiabatic shearing process. Given the substantially robust ballistic performance, the polyimide aerogels have a potential to combat multiple constraints such as cost, weight, and volume restrictions in aeronautical and aerospace applications with high blast resistance and ballistic performance requirements such as in stuffed Whipple shields for orbital debris containment application.

42 ENGINEERING↗

DOE OSTI2024

Improved Manufacturability and Throughput of Ultra- Transparent, Super-Insulating Aerogels

AeroShield Materials produces a novel silica aerogel material with exemplary thermal performance and unprecedented optical clarity, offering the potential for super-insulating fenestration and insulated glass to reduce thermal losses in the built environment by billions of dollars every year. One of the most significant challenges facing AeroShield today is the total amount of time that is required to produce large monolithic aerogel samples. This overall process can require as much as 144 hours total, which can significantly hinder scale-up to an economically viable product. The purpose of this Phase 1 research was to continue development of our novel aerogel manufacturing process to reduce material processing time by up to 10x, greatly improving product throughput and reducing cost. AeroShield’s manufacturing process can be divided into 4 major stages, each with their own distinct set of parameters and time requirements. Under this Phase 1 award, AeroShield was able to identify and optimize a number of these parameters, including molding materials, solvent rinse conditions, critical point drying time, and annealing conditions. AeroShield also performed thorough analyses on how these optimized parameters affected important final characteristics of the gels, including optical clarity, thermal conductivity, and dimensional stability. This campaign culminated in the production of laboratory scale aerogel samples using significantly lower process times of both 36 and 18 total hours, which represent Phase 1 Target and Stretch goals. In order to achieve widespread market adoption, monolithic sheets of the aerogel material must be made to industry-standard sizes (8’ x 12’) at a cost that provides 5-7 year or less breakeven energy savings for consumers (<$2 sq/ft). The work performed under this Phase 1 award shows that time and materials required to make aerogel samples, which make up a significant portion of their overall cost, can be greatly reduced without sacrificing quality. AeroShield plans to use these optimized processes to produce larger, product-relevant sized aerogels in order to achieve target final material costs.

Wilke, Kyle↗

NASA NTRS2006

Thermal Performance Of Space Suit Elements With Aerogel Insulation For Moon And Mars Exploration

Flexible fiber-reinforced aerogel composites were studied for use as insulation materials of a future space suit for Moon and Mars exploration. High flexibility and good thermal insulation properties of fiber-reinforced silica aerogel composites at both high and low vacuum conditions make it a promising insulation candidate for the space suit application. This paper first presents the results of a durability (mechanical cycling) study of these aerogels composites in the context of retaining their thermal performance. The study shows that some of these Aerogels materials retained most of their insulation performance after up to 250,000 cycles of mechanical flex cycling. This paper also examines the problem of integrating these flexible aerogel composites into the current space suit elements. Thermal conductivity evaluations are proposed for different types of aerogels space suit elements to identify the lay-up concept that may have the best overall thermal performance for both Moon and Mars environments. Potential solutions in mitigating the silica dusting issue related to the application of these aerogels materials for the space suit elements are also discussed.

Tang, Henry H.↗

NASA NTRS2009

Improved Aerogel Vacuum Thermal Insulation

An improved design concept for aerogel vacuum thermal-insulation panels calls for multiple layers of aerogel sandwiched between layers of aluminized Mylar (or equivalent) poly(ethylene terephthalate), as depicted in the figure. This concept is applicable to both the rigid (brick) form and the flexible (blanket) form of aerogel vacuum thermal-insulation panels. Heretofore, the fabrication of a typical aerogel vacuum insulating panel has involved encapsulation of a single layer of aerogel in poly(ethylene terephthalate) and pumping of gases out of the aerogel-filled volume. A multilayer panel according to the improved design concept is fabricated in basically the same way: Multiple alternating layers of aerogel and aluminized poly(ethylene terephthalate) are assembled, then encapsulated in an outer layer of poly(ethylene terephthalate), and then the volume containing the multilayer structure is evacuated as in the single-layer case. The multilayer concept makes it possible to reduce effective thermal conductivity of a panel below that of a comparable single-layer panel, without adding weight or incurring other performance penalties. Implementation of the multilayer concept is simple and relatively inexpensive, involving only a few additional fabrication steps to assemble the multiple layers prior to evacuation. For a panel of the blanket type, the multilayer concept, affords the additional advantage of reduced stiffness.

Ruemmele, Warren P.↗