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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
NASA NTRS2006

The Compressive Behavior of Isocyanate-crosslinked Silica Aerogel at High Strain Rates

Aerogels are low-density, highly nano-porous materials. Their engineering applications are limited due to their brittleness and hydrophilicity. Recently, a strong lightweight crosslinked silica aerogel has been developed by encapsulating the skeletal framework of amine-modified silica aerogels with polyureas derived by isocyanate. The mesoporous structure of the underlying silica framework is preserved through conformal polymer coating, and the thermal conductivity remains low. Characterization has been conducted on the thermal, physical properties and the mechanical properties under quasi-static loading conditions. In this paper, we present results on the dynamic compressive behavior of the crosslinked silica aerogel (CSA) using a split Hopkinson pressure bar (SHPB). A new tubing pulse shaper was employed to help reach the dynamic stress equilibrium and constant strain rate. The stress-strain relationship was determined at high strain rates within 114-4386/s. The effects of strain rate, density, specimen thickness and water absorption on the dynamic behavior of the CSA were investigated through a series of dynamic experiments. The Young's moduli (or 0.2% offset compressive yield strengths) at a strain rate approx.350/s were determined as 10.96/2.08, 159.5/6.75, 192.2/7.68, 304.6/11.46, 407.0/20.91 and 640.5/30.47 MPa for CSA with densities 0.205, 0.454, 0.492, 0.551,0.628 and 0.731 g/cu cm, respectively. The deformation and failure behaviors of a native silica aerogel with density (0.472 g/cu cm ), approximately the same as a typical CSA sample were observed with a high speed digital camera. Digital image correlation technique was used to determine the surface strains through a series of images acquired using high speed photography. The relative uniform axial deformation indicated that localized compaction did not occur at a compressive strain level of approx.17%, suggesting most likely failure mechanism at high strain rate to be different from that under quasi-static loading condition. The Poisson s ratio was determined to be 0.162 in nonlinear regime under high strain rates. CSA samples failed generally by splitting, but were much more ductile than native silica aerogels.

Luo, H.↗
NASA NTRS2008

High Temperature Aerogels for Thermal Protection Systems

High temperature aerogels in the Al2O3-SiO2 system are being investigated as possible constituents for lightweight integrated thermal protection system (TPS) designs for use in supersonic and hypersonic applications. Gels are synthesized from ethoxysilanes and AlCl3.6H2O, using an epoxide catalyst. The influence of Al:Si ratio, solvent, water to metal and water to alcohol ratios on aerogel composition, morphology, surface area, and pore size distribution were examined, and phase transformation on heat treatment characterized. Aerogels have been fabricated which maintain porous, fractal structures after brief exposures to 1000 C. Incorporation of nanofibers, infiltration of aerogels into SiC foams, use of polymers for crosslinking the aerogels, or combinations of these, offer potential for toughening and integration of TPS with composite structure. Woven fabric composites having Al2O3-SiO2 aerogels as a matrix also have been fabricated. Continuing work is focused on reduction in shrinkage and optimization of thermal and physical properties.

Hurwitz, Frances I.↗
NASA NTRS2008

Evaluating Dimethyldiethoxysilane for use in Polyurethane Crosslinked Silica Aerogels

Silica aerogels are highly porous materials which exhibit exceptionally low density and thermal conductivity. Their "pearl necklace" nanostructure, however, is inherently weak; most silica aerogels are brittle and fragile. The strength of aerogels can be improved by employing an additional crosslinking step using isocyanates. In this work, dimethyldiethoxysilane (DMDES) is evaluated for use in the silane backbone of polyurethane crosslinked aerogels. Approximately half of the resulting aerogels exhibited a core/shell morphology of hard crosslinked aerogel surrounding a softer, uncrosslinked center. Solid state NMR and scanning electron microscopy results indicate the DMDES incorporated itself as a conformal coating around the outside of the secondary silica particles, in much the same manner as isocyanate crosslinking. Response surface curves were generated from compression data, indicating levels of reinforcement comparable to that in previous literature, despite the core/shell morphology.

Randall, Jason P.↗
NASA NTRS2008

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.

Paik, Jong-Ah↗
NASA NTRS2007

Structure-Property Relationships in Porous 3-D Nanostructures as a Function of Preparation Conditions: Isocyanate Cross-Linked Silica Aerogels

Sol-gel derived silica aerogels are attractive candidates for many unique thermal, optical, catalytic, and chemical applications because of their low density and high mesoporosity. However, their inherent fragility has restricted use of aerogel monoliths to applications where they are not subject to any load. We have previously reported cross-linking the mesoporous silica structure of aerogels with di-isocyanates, styrenes or epoxies reacting with amine decorated silica surfaces. These approaches have been shown to significantly increase the strength of aerogels with only a small effect on density or porosity. Though density is a prime predictor of properties such as strength and thermal conductivity for aerogels, it is becoming clear from previous studies that varying the silica backbone and size of the polymer cross-link independently can give rise to combinations of properties which cannot be predicted from density alone. Herein, we examine the effects of four processing parameters for producing this type of polymer cross-linked aerogel on properties of the resulting monoliths. We focus on the results of C-13 CP-MAS NMR which gives insight to the size and structure of polymer cross-link present in the monoliths, and relates the size of the cross-links to microstructure, mechanical properties and other characteristics of the materials obtained.

Meador, Mary Ann B.↗
NASA NTRS2009

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.

Rhine, Wendell↗
NASA NTRS2007

Structure-Property Relationships in Porous 3-D Nanostructures as a Function of Preparation Conditions: Isocyanate Cross-Linked Silica Aerogels

Sol-gel derived silica aerogels are attractive candidates for many unique thermal, optical, catalytic, and chemical applications because of their low density and high mesoporosity. However, their inherent fragility has restricted use of aerogel monoliths to applications where they are not subject to any load. We have previously reported cross-linking the mesoporous silica structure of aerogels with di-isocyanates, styrenes or epoxies reacting with amine decorated silica surfaces. These approaches have been shown to significantly increase the strength of aerogels with only a small effect on density or porosity. Though density is a prime predictor of properties such as strength and thermal conductivity for aerogels, it is becoming clear from previous studies that varying the silica backbone and size of the polymer cross-link independently can give rise to combinations of properties which cannot be predicted from density alone. Herein, we examine the effects of four processing parameters for producing this type of polymer cross-linked aerogel on properties of the resulting monoliths. We focus on the results of 13C CP-MAS NMR which gives insight to the size and structure of polymer cross-link present in the monoliths, and relates the size of the cross-links to microstructure, mechanical properties and other characteristics of the materials obtained.

Meador, Mary Ann B.↗
NASA NTRSDate not supplied

Enhanced Thermal Stability of High Yttria Concentration YSZ Aerogels

Aerogels demonstrate extraordinarily low thermal conductivity and low density, presenting a promising form of lightweight insulation for aerospace applications. The primary challenge is stabilization of the highly porous structure at temperatures to 1200 °C. Upon collapse of the pore structure, the favorable thermal properties and low density are diminished. Yttria-stabilized zirconia (YSZ) aerogels are synthesized to investigate the effect of composition on morphology, phase behavior, and thermal stability (specific surface area, pore size distribution). This work demonstrates the improvement in thermal stability of zirconia aerogels with increased yttria content. Furthermore, changes in structure and surface chemistry of YSZ aerogels are studied in both oxidizing and inert atmospheres. With an improved understanding of aerogel structure and performance, metal oxide aerogels can be developed to withstand the extreme environments of space exploration.

Nathaniel Olson↗
NASA NTRS2021

Effect of Urea Links in the Backbone of Polyimide Aerogels

Flexible, conformal polyimide aerogels with low density, good mechanical properties and high surface areas have attracted much attention for many potential applications such as lightweight antenna substrates, insulating materials for launch vehicles, inflatable structures, aircraft or space suits. Development and improvements to fabrication of polyimide aerogel thin films have been reported over the last decade to meet the needs of many of these applications. However, most starting materials are expensive. In this research, we utilized commercially available, low cost monomers including 4,4’-bis(4-aminophenoxy)propane (BAPP) and 3,3’,4,4’-benzophenone tetracarboxylic dianhydride (BTDA), and 4,4-methylene diphenyl di-isocyanate (MDI) in fabricating polyimide (PI) and polyimide-urea (PIU), which were then cross-linked with 1,3,5-tris(4-aminophenoxy)benzene (TAB). It was found that the addition of MDI into the PI chains not only maintained the flexibility of the aerogel films, but also enhanced the film casting, allowing the production on pilot scale. With the capability in producing robust films at affordable cost, application of the PIU aerogel films can be expanded to terrestrial goods such as winter clothing, or pipe wrapping, etc. In addition, the presence of only a small addition of the urea links in the polyimide chains in PIU aerogels led to lower shrinkage when compared to the corresponding PI aerogels, leading to lower density

Baochau N. Nguyen↗
NASA NTRSDate not supplied

Auxetic Thermo-Responsive Shape-Memory Polyurethane Aerogels

Shape memory polymer aerogels are stimuli-responsive aerogel materials that incorporate polymer aerogel characteristics such as flexibility at low density, and high porosity with shape-changing capabilities upon exposure to external stimuli. By designing the structure of these materials at meso- to macroscale, their shape memory response can be efficiently engineered to show an auxetic response such as a negative Poisson’s ratio, leading to an active and tunable metamaterial. We present a material technology based on a shape memory polyurethane aerogel derived from aliphatic triisocyanate and triethylene glycol, which demonstrates and remembers an auxetic shape change through a thermomechanical cycle first below, and then back again above the glass transition temperature of the polyurethane. Our auxetic shape memory polyurethane aerogels exhibit a significant auxetic response with a negative Poisson’s ratio of approximately -0.8 at 15% compressive strain. This technology is expected to impact multiple areas of interest in relation to commercial, aeronautic, and aerospace industries. Potential applications include minimally invasive medical technologies, soft robotics, and self-deployable structures and habitats. Structure-property relationships of the auxetic shape memory polymer aerogels will be discussed.

Sadeq Malakooti↗
NASA NTRS2014

Synthesis and Properties of Cross-Linked Polyamide Aerogels

We report our ongoing research on polyamide aerogels made by step growth polymerization using a combination of terephthaloyl chloride, isophthaloyl chloride and m-phenylenediamine. Crosslinking of the amine capped polymer chains with 1,3,5-benzenetricarbonyl trichloride causes gelation in as little as two to five minutes. Removing the reaction solvent is accomplished through solvent exchange, followed by drying using supercritical CO2 extraction to give colorless aerogels with densities ranging from 0.07 to 0.33 grams per cubic centimeter and surface areas as high as 440 square meters per gram. Statistical experimental design methodology has been utilized to investigate dependence of properties of these aerogels, such as density, compressive modulus, and surface area, on changes in fabrication parameters including formulated number of amide oligomer repeat units (n-value), acid chloride (meta, para or combination), and solids concentration of solution used for gelation. For example, the density of these materials was found to be dependent on the acid chloride type and the solids concentration, but n was not a significant variable. However, surface area was significantly influenced by all three parameters. The polyamide aerogels represent a potential cost savings over previously reported polyimide aerogels, since monomers are all inexpensive and commercially available. Surface area and density were both highest when 100 terephthaloyl chloride was used but a combination of 5 solid concentration, 100 terephthaloyl chloride and n of 20 gave the best combination of properties.

cross-linked↗
NASA NTRS2018

Aerogel-Based Insulation Materials for Cryogenic Applications

Many different aerogel-based materials are now being used in thermal insulation systems for cryogenic applications. These materials include flexible composite blankets, bulk-fill particles, and polymer composites in both evacuated and non-evacuated environments. In ambient environments, aerogels provide superior thermal performance compared to conventional polymeric foam and cellular glass insulations while offering unique advantages in avoiding problems with weathering, moisture, and mechanical damage. Aerogels are also used as spacer materials in multilayer insulation systems. These layered systems provide combined structural-thermal capability for cryogenic systems in either vacuum-jacketed or externally-applied insulation designs. Test data (effective thermal conductivity) include a wide range of both commercial and experimental aerogel materials. Testing was performed using laboratory cryostats and standard methods including full range vacuum (from ambient pressure to high vacuum) and boundary temperatures 293 K and 78 K. Examples of aerogel-based insulation systems are given for both evacuated and non-evacuated applications.

heat transfer↗
NASA NTRS2018

Aerogel-Based Insulation Materials for Cryogenic Applications

Many different aerogel-based materials are now being used in thermal insulation systems for cryogenic applications. These materials include flexible composite blankets, bulk-fill particles, and polymer composites in both evacuated and non-evacuated environments. In ambient environments, aerogels provide superior thermal performance compared to conventional polymeric foam and cellular glass insulations while offering unique advantages in solving problems with weathering, moisture, and mechanical damage. Aerogels are also used as spacer materials in multilayer insulation systems. These layered systems provide combined structural-thermal capability for cryogenic systems in either vacuum-jacketed or externally-applied insulation designs. Test data (effective thermal conductivity) include a wide range of both commercial and experimental aerogel materials. Testing was performed using laboratory cryostats and standard methods including full range vacuum (from ambient pressure to high vacuum) and boundary temperatures 293 K and 78 K. Examples of aerogel-based insulation systems are given for both evacuated and non-evacuated applications.

aerogel layered composites↗
NASA NTRSDate not supplied

Understanding thermal stability in doped zirconia aerogels for high temperature applications

The high porosities and low densities of ceramic aerogels offer outstanding insulative performance in applications where weight is a critical factor. The high surface-to-volume ratios and specific surface areas provide extremely low thermal conductivity, but also contribute to rapid densification of the pore structure at elevated temperatures. This densification diminishes their favorable properties and inhibits use of aerogels in high temperature applications. The purpose of this work is the establishment of a design framework for thermally stable, highly porous materials. Here we will review our recent studies on the effects of synthetic parameters and dopant chemistry on the evolution of zirconia-based aerogels. The structural evolution was studied to 1200 °C using nitrogen physisorption, scanning and transmission electron microscopy, and x-ray diffraction. The role of dopant identity and concentration in thermal stability was elucidated. In context of the design framework, dopant chemistry is an aggregate for many closely related material properties, each of which may contribute to aerogel structural evolution. To develop a truly predictive design framework for ceramic-based aerogels, systematic and comprehensive evaluation of thermodynamic and kinetic properties must be performed in conjunction with studies on structural evolution.

aerogel↗
NASA NTRS2024

Synthesis of Flexible Polyamide Aerogels Cross-Linked with a Tri-Isocyanate

A new series of flexible polyamide (PA) aerogels was synthesized using terephthaloyl chloride (TPC), 2,2′-dimethylbenzidine (DMBZ) and cross-linked with an inexpensive, commercially available tri-isocyanate (Desmodur N3300A) at polymer concentrations of 6–8 wt.% total solids and repeating units, n, from 30 to 60. The cross-linked DMBZ-based polyamide aerogels obtained, after supercritically drying using liquid CO 2 , had shrinkages of 19–27% with densities ranging from 0.12 g/cm 3 to 0.22 g/cm 3 , porosity and surface areas up to 91% and 309 m 2 /g, respectively, and modulus values ranging from 20.6 to 109 MPa. Evidence suggests that a higher flexibility could be achieved using DMBZ in the polyamide backbone with N3300A as a cross-linker, when compared to previously reported TPC-mPDA-BTC PA aerogels, N3300A-polyimide aerogels, and N3300-reinforced silica aerogels.

aerogels↗
NASA NTRS1991

Volatiles in interplanetary dust particles and aerogels

Volatiles measured in 25 interplanetary dust particles (IDPs) are a mixture of both indigenous materials and contaminants associated with the collection and processing of the ODPs prior to analysis. Most IDPs have been collected in the stratosphere using a silicone oil/freon mixture (20:1 ratio) coated on collector plates. Studies have shown that silicone oil, freon and hexane residues remain with the ODPs, despite attempts to clean the IDPs. Analysis of the IDPs with the LMMS-technique produces spectra with a mixture of indigeneous and contaminants components. The contamination signal can be identified and removed; however, the contamination signal may obscure some of the indigeneous component's signal. Employing spectra stripping techniques, the indigenous volatile constituents associated with the IDPs can be identified. Volatiles are similar to those measured in CI or CM carbonaceous chondrites. Collection of IDPs in low-Earth orbit utilizing a Cosmic Dust Collection Facility attached to Space Station Freedom has been proposed. The low-density material aerogel has been proposed as a collection substrate for IDPs. Our studies have concentrated on identifying volatile contaminants that are associated with aerogel. We have found that solvents used for the preparation of aerogel remain in aerogel and methods must be developed for removing the entrapped solvents before aerogels can be used for an IDP collection substrate.

Gibson, E. K., Jr.↗
NASA NTRS1992

Suitability of silica aerogel as a capture medium for interplanetary dust

Impact experiments using silica aerogel as a deceleration and capture medium for interplanetary dust are reported. A rough correlation is noted between increasing particle track lengths and decreasing aerogel density, and there is a poor correlation of track lengths with impact velocity at laboratory attainable velocities of 5-7 km/s. It is concluded that aerogel track lengths should not be used as velocity indicators. Chemical analyses are also reported of aerogel samples used in this study in order to assess the risks concerning contamination of interplanetary dust particles by the silica aerogel capture medium. It is demonstrated that this material is impressively clean.

Barrett, R. A.↗
NASA NTRS1998

Prototype Aerogel Insulation for Melamine-Foam Substitute: Critical Space Station Express Rack Technology

There is a current lack of environmentally acceptable foams to insulate Long-Duration Human Spaceflight Missions, including the experimental Express Rack for the Space Station. A recent 60-day manned test in a sealed chamber at Johnson Space Center (JSC) was nearly aborted, because of persistently high formaldehyde concentrations in the chamber. Subsequent investigation showed that the source was melamine foam (used extensively for acoustic insulation). The thermal and acoustic potential for melamine-foam substitutes is evaluated for scale-up to a silica-based foam and aerogel, which is environmentally benign for long duration space flight. These features will be discussed in reference to an aerogel prototype to: 1) assemble material strength data for various formulated aerogels, both silica and organic carbon aerogels; 2) assemble the aerogel into panels of mylar/vacuum-encapsulated rigid boards which can be molded in various shapes and rigidities; and 3) describe a process for space applications for formaldehyde-free, long duration thermal and acoustic insulators.

Noever, David A.↗