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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)]
Fiber reinforced aerogel composites
Fiber reinforced aerogel composites, including a transparent composite material that contains an aerogel and fibers embedded into the aerogel and/or bonded to one or more surfaces of the aerogel, and composites that contain an aerogel tile and an assemblage of fibers embedded into the aerogel tile or bonded to the aerogel tile that are useful as Cherenkov radiators for the detection and identification of subatomic particles. Also, methods of making and using the composites.
Aerogel Composites for Aerospace Thermal Protection
Aerogel composites formed by infiltrating organic and/or inorganic aerogels into fiber matrix materials enable us to exploit the low thermal conductivity and low density of aerogels while maintaining the strength, structure and other useful properties of a porous fiber matrix. New materials for extreme heating ranges are needed to insulate future spacecraft against the extreme heat of planetary atmospheric entry, but the insulation mass must be minimized in order to maximize the payload. A reusable system passively insulates to survive heating unchanged for relatively low heating. Ablators, which sacrifice mass to control heating, are used to protect vehicles against more extreme heating for a single use thermal protection system (TPS). Aerogel composites were fabricated and tested for spacecraft thermal protection. The high-temperaturey high heat flux tests described in this paper were performed in NASA Ames arc-jet facilities to simulate spacecraft atmospheric entry, and include heating conditions predicted for the forebody and backshell of the Mars Science Lander (MSL) entry probe. The aerogel composites tested showed excellent thermal performance in the arc-jet tests, functioning both as reusuable insulation under lower heat fluxes, and as ablative aerogels under the extreme heating predicted for the MSL forebody.
Ceramic Aerogel Composite Materials and Characterization
Aerogels a.k.a "Solid Smoke" are gels with the liquid phase replaced by gas, leaving behind a highly porous material with a nanoscale framework. Due to the porous, nanoscale structure, aerogels have the lowest known density and conductivity of solids. Aerogels have the potential for being a breakthrough material because of their extremely light weight and unique properties. In this paper, we address overcoming their most profound weaknesses: mechanical fragility and very high surface activity, which leads to a lowered sintering temperature. A matrix of ceramic aerogel composite materials was produced to investigate their properties and functionality. Mechanical property measurements and Scanning Electron Micrographs are used to identify trends and structure of these ceramic composite materials. Thermal cycling was used to identify the sintering points of the materials.
Improved Silica Aerogel Composite Materials
A family of aerogel-matrix composite materials having thermal-stability and mechanical- integrity properties better than those of neat aerogels has been developed. Aerogels are known to be excellent thermal- and acoustic-insulation materials because of their molecular-scale porosity, but heretofore, the use of aerogels has been inhibited by two factors: (1) Their brittleness makes processing and handling difficult. (2) They shrink during production and shrink more when heated to high temperatures during use. The shrinkage and the consequent cracking make it difficult to use them to encapsulate objects in thermal-insulation materials. The underlying concept of aerogel-matrix composites is not new; the novelty of the present family of materials lies in formulations and processes that result in superior properties, which include (1) much less shrinkage during a supercritical-drying process employed in producing a typical aerogel, (2) much less shrinkage during exposure to high temperatures, and (3) as a result of the reduction in shrinkage, much less or even no cracking.
Silica-Aerogel Composites Opacified with La(0.7)Sr(0.3)MnO3
As part of an effort to develop improved lightweight thermal-insulation tiles to withstand temperatures up to 1,000 C, silica aerogel/fused-quartz-fiber composite materials containing La0.7Sr0.3MnO3 particles as opacifiers have been investigated as potentially offering thermal conductivities lower than those of the otherwise equivalent silica-aerogel composite materials not containing La(0.7)Sr(0.3)MnO3 particles. The basic idea of incorporating opacifying particles into silica-aerogels composite to reduce infrared radiative contributions to thermal conductivities at high temperatures is not new: it has been reported in a number of previous NASA Tech Briefs articles. What is new here is the selection of La(0.7)Sr(0.3)MnO3 particles as candidate opacifiers that, in comparison with some prior opacifiers (carbon black and metal nanoparticles), are more thermally stable. The preparation of a composite material of the present type includes synthesis of the silica-aerogel component in a sol-gel process. The La(0.7)Sr(0.3)MnO3 particles, made previously in a separate process, are mixed into the sol, which is then cast onto fused-quartz-fiber batting. Then the aerogel-casting solution is poured into the mold, where it permeates the silica fiber felt. After the sol has gelled, the casting is aged and then subjected to supercritical drying to convert the gel to the final aerogel form. The separate process for making the La(0.7)Sr(0.3)MnO3 particles begins with the slow addition of corresponding proportions of La(CH3COOH)3, Mn(CH3COOH)3, and Sr(NO3)2 to a solution of H2O2 in H2O. The solution is then peptized by drop-wise addition of NH4OH to obtain a sol. Next, the sol is dried in an oven at a temperature of 120 C to obtain a glassy solid. The solid is calcined at 700 C to convert it to La(0.7)Sr(0.3)MnO3. Then La(0.7)Sr(0.3)MnO3 particles are made by ball-milling the calcined solid. The effectiveness of La(0.7)Sr(0.3)MnO3 particles as opacifiers and thermal-conductivity reducers depends on the statistical distribution of particle sizes as well as the relative proportions of La(0.7)Sr(0.3)MnO3 and aerogel. For experiments performed thus far, samples of aerogel/fiber composites were formulated to have, variously, silica target density of 0.07 or 0.14 g/cu cm and to contain 30 percent of La(0.7)Sr(0.3)MnO3 in average particle size of 0.3 or 3 microns. The thermal conductivities of the samples containing the 3 micron La(0.7)Sr(0.3)MnO3 particles were found to be lower than those of the samples containing the 0.3 micron La(0.7)Sr(0.3)MnO3 particles. The optimum particle size is believed to be between 1 and 5 microns.
Influence of Aerogel Morphology and Reinforcement Architecture on Gas Convection in Aerogel Composites
A variety of thermal protection applications require lightweight insulation capable of withstanding temperatures well above 900 C. Aerogels offer extremely low-density thermal insulation due to their mesoporous structure, which inhibits both gas convection and solid conduction. Silica aerogel systems are limited to use temperatures of 600-700 C, above which they sinter. Alumina aerogels maintain a porous structure to higher temperatures than silica, before transforming to -alumina and densifying. We have synthesized aluminosilicate aerogels capable of maintaining higher surface areas at temperatures above 1100 C than an all-alumina aerogel using -Boehmite as the aluminum source and tetraethoxysilane (TEOS) as the silicon source. The pore structure of these aerogels varies with thermal exposure temperature and time, as the aluminosilicate undergoes a variety of phase changes to form transition aluminas. Transformation to -alumina is inhibited by incorporation of silica into the alumina lattice. The aerogels are fragile, but can be reinforced using a large variety of ceramic papers, felts or fabrics. The objective of the current study is to characterize the influence of choice of reinforcement and architecture on gas permeability of the aerogel composites in both the as fabricated condition and following thermal exposure, as well as understand the effects of incorporating hydrophobic treatments in the composites.
Aerogel Composites: Strong and Waterproof
Aerogels are exotic materials having superior thermal and physical properties with great potential for both space and industrial uses. Although aerogels are excellent low-density insulators with unique acoustic and optical properties, their commercialization potential is currently limited by moisture absorption, fragility, and cost. This paper describes useful, easily scaled-up solutions to the first two of these three problems. The waterproofing and water-repellent method described here is a cheaper and simpler improvement over previous permanent methods.
Polyimide Cellulose Nanocrystal Composite Aerogels
Polyimide (PI) aerogels are highly porous solids having low density, high porosity and low thermal conductivity with good mechanical properties. They are ideal for various applications including use in antenna and insulation such as inflatable decelerators used in entry, decent and landing operations. Recently, attention has been focused on stimuli responsive materials such as cellulose nano crystals (CNCs). CNCs are environmentally friendly, bio-renewable, commonly found in plants and the dermis of sea tunicates, and potentially low cost. This study is to examine the effects of CNC on the polyimide aerogels. The CNC used in this project are extracted from mantle of a sea creature called tunicates. A series of polyimide cellulose nanocrystal composite aerogels has been fabricated having 0-13 wt of CNC. Results will be discussed.
Novel Cryogenic Insulation Materials: Aerogel Composites
New insulation materials are being developed to economically and reliably insulate future reusable spacecraft cryogenic tanks over a planned lifecycle of extreme thermal challenges. These insulation materials must prevent heat loss as well as moisture and oxygen condensation on the cryogenic tanks during extended groundhold, must withstand spacecraft launch conditions, and must protect a partly full or empty reusable cryogenic tank from significant reentry heating. To perform over such an extreme temperature range, novel composites were developed from aerogels and high-temperature matrix material such as Space Shuttle tile. These materials were fabricated and tested for use both as cryogenic insulation and as high-temperature insulation. The test results given in this paper were generated during spacecraft re-entry heating simulation tests using cryogenic cooling.
Composite Aerogel Multifoil Protective Shielding
New technologies are needed to survive the temperatures, radiation, and hypervelocity particles that exploration spacecraft encounter. Multilayer insulations (MLIs) have been used on many spacecraft as thermal insulation. Other materials and composites have been used as micrometeorite shielding or radiation shielding. However, no material composite has been developed and employed as a combined thermal insulation, micrometeorite, and radiation shielding. By replacing the scrims that have been used to separate the foil layers in MLIs with various aerogels, and by using a variety of different metal foils, the overall protective performance of MLIs can be greatly expanded to act as thermal insulation, radiation shielding, and hypervelocity particle shielding. Aerogels are highly porous, low-density solids that are produced by the gelation of metal alkoxides and supercritical drying. Aerogels have been flown in NASA missions as a hypervelocity particle capture medium (Stardust) and as thermal insulation (2003 MER). Composite aerogel multifoil protective shielding would be used to provide thermal insulation, while also shielding spacecraft or components from radiation and hypervelocity particle impacts. Multiple layers of foil separated by aerogel would act as a thermal barrier by preventing the transport of heat energy through the composite. The silica aerogel would act as a convective and conductive thermal barrier, while the titania powder and metal foils would absorb and reflect the radiative heat. It would also capture small hypervelocity particles, such as micrometeorites, since it would be a stuffed, multi-shock Whipple shield. The metal foil layers would slow and break up the impacting particles, while the aerogel layers would convert the kinetic energy of the particles to thermal and mechanical energy and stop the particles.
Digitally-Engineered Impact Resistant Aerogel Composites for MMOD Protection (DIRAC-MP)
This project implemented a digital-engineering approach to optimize the impact absorption performance of polymer aerogels and aerogel-based composites for Micrometeoroids and Orbital Debris (MMOD) containment. We developed a curated materials database and a machine-learning framework to derive composition-response relationships, enabling predictive design and targeted material selection. In support of experimental validation, a split Hopkinson pressure bar (SHPB) test rig, specifically adapted for low-density aerogel materials, was designed and built in-house. This project accelerates the development of new aerogel formulations, producing candidate materials tailored for enhanced impact-absorption behavior.
Silica/Polymer and Silica/Polymer/Fiber Composite Aerogels
Aerogels that consist, variously, of neat silica/polymer alloys and silica/polymer alloy matrices reinforced with fibers have been developed as materials for flexible thermal-insulation blankets. In comparison with prior aerogel blankets, these aerogel blankets are more durable and less dusty. These blankets are also better able to resist and recover from compression . an important advantage in that maintenance of thickness is essential to maintenance of high thermal-insulation performance. These blankets are especially suitable as core materials for vacuum- insulated panels and vacuum-insulated boxes of advanced, nearly seamless design. (Inasmuch as heat leakage at seams is much greater than heat leakage elsewhere through such structures, advanced designs for high insulation performance should provide for minimization of the sizes and numbers of seams.) A silica/polymer aerogel of the present type could be characterized, somewhat more precisely, as consisting of multiply bonded, linear polymer reinforcements within a silica aerogel matrix. Thus far, several different polymethacrylates (PMAs) have been incorporated into aerogel networks to increase resistance to crushing and to improve other mechanical properties while minimally affecting thermal conductivity and density. The polymethacrylate phases are strongly linked into the silica aerogel networks in these materials. Unlike in other organic/inorganic blended aerogels, the inorganic and organic phases are chemically bonded to each other, by both covalent and hydrogen bonds. In the process for making a silica/polymer alloy aerogel, the covalent bonds are introduced by prepolymerization of the methacrylate monomer with trimethoxysilylpropylmethacrylate, which serves as a phase cross-linker in that it contains both organic and inorganic monomer functional groups and hence acts as a connector between the organic and inorganic phases. Hydrogen bonds are formed between the silanol groups of the inorganic phase and the carboxyl groups of the organic phase. The polymerization process has been adapted to create interpenetrating PMA and silica-gel networks from monomers and prevent any phase separations that could otherwise be caused by an overgrowth of either phase. Typically, the resulting PMA/silica aerogel, without or with fiber reinforcement, has a density and a thermal conductivity similar to those of pure silica aerogels. However, the PMA enhances mechanical properties. Specifically, flexural strength at rupture is increased to 102 psi (=0.7 MPa), about 50 times the flexural strength of typical pure silica aerogels. Resistance to compression is also increased: Applied pressure of 17.5 psi (=0.12 MPa) was found to reduce the thicknesses of several composite PMA/silica aerogels by only about 10 percent.
Synthesis and characterization of UiO-66-NH 2 incorporated graphene aerogel composites and their utilization for absorption of organic liquids
This work details the synthesis, materials characterization and absorption capacity of graphene aerogel (GA) loaded with UiO-66-NH 2 metal organic framework (MOF). Throughout the study, a series of density-tunable MOF/GA composites were synthesized by adjusting the MOF/graphene oxide (GO) mass ratio of the precursors before hydrothermal reduction and subsequent critical point drying to achieve MOF-x%/GA composites, with x, ranging from 0 to 100, denoting the weight percent ratio of MOF to GO in the starting solution. Scanning electron microscopy (SEM) images and Barrett-Joyner-Halenda (BJH) pore size calculations supported that MOF loading enlarged the macroporous (>50 nm) structure of the GA framework but had no influence on the mesoporous (2–50 nm) structure of GA. The degree of MOF loading first decreased and then increased the density of resulting composites, exhibiting a minimum for the 10–30% samples. Such behavior with respect to MOF loading has not been reported previously. MOF-x%/GA samples were further investigated for absorption capacity using various organic liquids. MOF-30%/GA proved to be the best absorbent sample for all solvents tested, achieving the highest capacity for chloroform at 147.0 ± 10.0 mg/mg. The behavior is attributed to the structural changes induced by the MOF incorporation as well as the interactions between the organic molecules and the MOF.
Polyurea-Based Aerogel Monoliths and Composites
aerogel insulation material was developed that will provide superior thermal insulation and inherent radiation protection for government and commercial applications. The rubbery polyureabased aerogel exhibits little dustiness, good flexibility and toughness, and durability typical of the parent polyurea polymer, yet with the low density and superior insulation properties associated with aerogels. The thermal conductivity values of polyurea-based aerogels at lower temperature under vacuum pressures are very low and better than that of silica aerogels. Flexible, rubbery polyurea-based aerogels are able to overcome the weak and brittle nature of conventional inorganic and organic aerogels, including polyisocyanurate aerogels, which are generally prepared with the one similar component to polyurethane rubber aerogels. Additionally, with higher content of hydrogen in their structures, the polyurea rubber-based aerogels will also provide inherently better radiation protection than those of inorganic and carbon aerogels. The aerogel materials also demonstrate good hydrophobicity due to their hydrocarbon molecular structure. There are several strategies to overcoming the drawbacks associated with the weakness and brittleness of silica aerogels. Development of the flexible fiber-reinforced silica aerogel composite blanket has proven to be one promising approach, providing a conveniently fielded form factor that is relatively robust in industrial environments compared to silica aerogel monoliths. However, the flexible, silica aerogel composites still have a brittle, dusty character that may be undesirable, or even intolerable, in certain application environments. Although the cross - linked organic aerogels, such as resorcinol- formaldehyde (RF), polyisocyanurate, and cellulose aerogels, show very high impact strength, they are also very brittle with little elongation (i.e., less rubbery). Also, silica and carbon aerogels are less efficient radiation shielding materials due to their lower content of hydrogen element. The invention involves mixing at least one isocyanate resin in solvent along with a specific amount of at least one polyamine hardener. The hardener is selected from a group of polyoxyalkyleneamines, amine-based polyols, or a mixture thereof. Mixing is performed in the presence of a catalyst and reinforcing inorganic and/or organic materials, and the system is then subjected to gelation, aging, and supercritical drying. The aerogels will offer exceptional flexibility, excellent thermal and physical properties, and good hydrophobicity. The rubbery polyurea-based aerogels are very flexible with no dust and hydrophobic organics that demonstrated the following ranges of typical properties: densities of 0.08 to 0.293 g/cu cm, shrinkage factor (raerogel/rtarget) = 1.6 to 2.84, and thermal conductivity values of 15.2 to 20.3 mW/m K.
Metal Nanoparticle Aerogel Composites
We have fabricated sol-gels containing gold and silver nanoparticles. Formation of an aerogel produces a blue shift in the surface plasmon resonance as a result of the decrease in the dielectric constant of the matrix upon supercritical extraction of the solvent. However, as a result of chemical interface damping this blue shift does not obey effective medium theories. Annealing the samples in a reducing atmosphere at 400 C eliminates this discrepancy and results in narrowing and further blue shifting of the plasmon resonance. Metal particle aggregation also results in a deviation from the predictions of effective medium theories, but can be controlled through careful handling and by avoiding the use of alcohol. By applying effective medium theories to the heterogeneous interlayer surrounding each metal particle, we extend the technique of immersion spectroscopy to inhomogeneous materials characterized by spatially dependent dielectric constants, such as aerogels. We demonstrate that the shift in the surface plasmon wavelength provides the average fractional composition of each component (air and silica) in this inhomogeneous layer, i.e. the porosity of the aerogel or equivalently, for these materials, the catalytic dispersion. Additionally, the kinetics suggest that collective particle interactions in coagulated metal clusters are perturbed during silica gelation resulting in a change in the aggregate geometry.
Flame-retardant cellulose-aerogel composite from agriculture waste for building insulation
Bio-based thermal insulation materials are in high demand due to their availability, reproducibility, and carbon-sequestration nature. However, high flammability, moisture condensation, and high thermal conductivity of biogenic material are major concerns for sustainable building applications. In this study, we report the fire-retardant cellulose aerogel insulation nanocomposites derived from wheat straw and silica aerogel, in which sodium bicarbonate improves its fire retardancy. We combined blended straw fibers and hammermilled straw fibers to create a structural hierarchy composite. The blended straw, with its longer and thicker size, served as reinforcement, while the hammermilled straw fibers acted as filler. This hierarchical structure was further integrated with aerogel for applications in green buildings. The as-prepared materials show a low thermal conductivity of 24.1 mW/m.K, high flexural modulus of 736 MPa, hydrophobicity with a water contact angle of 110.42°, and excellent fire retardancy. Altogether, this work provides an effective method for the synthesis of fire-retardant biogenic thermal insulation materials and shows a promising way for next-generation bio-based insulation materials.