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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

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

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

Energy response characterization of current-mode MeV Cherenkov aerogel detectors

Current-mode Cherenkov aerogel detectors have been used to measure time resolved spectra of MeV radiographic x-ray sources and have been considered to replace gas Cherenkov systems. The simulations of the Cherenkov response of aerogel detectors have uncertainties in how to model the complex structure of aerogels. Data from three sites—the Idaho electron beam, the Los Alamos Site electron beam and microtron sources at Los Alamos—have been used to calibrate the relative energy response of 15 aerogels, varying in density from 10 to 430 mg/cm 3 , from incident electrons with energies from 1 to 12 MeV. Detector simulations need to introduce density variation in the aerogels to match the collected data.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND

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.

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.

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.

Fabrication and Atomic Force Microscopy Characterization of Molecular Composites of Fullerenes in Aerogel Matrix for Optical Limiting

An optical limiter is a device which exhibits a decrease in the transmittance in a material with an increase in intensity of light. Sol-gel techniques offer many advantages in the fabrication of materials. These materials possess many desirable properties for nonlinear optical (NLO) device applications which include transparency, high thermal and chemical stabilities, very low refractive index and dielectric constants. C60 shows a higher excited state absorption cross section than the ground state absorption cross section over the complete visible spectrum, and the spectrum of the excited state absorption of C60 has the same general shape as the ground state absorption. This fact suggests that fullerenes are ideal optical limiting materials. Aerogels are fabricated by sol-gel processing. One of the key issues is the dispersion of fullerenes into small and uniform pores of silica aerogel host matrices. The aerogel network was characterized by Raman spectroscopy. Atomic force microscopy is a technique with many advantages to characterize the aerogel materials. The morphology of the cleaved surface for a C60/aerogel sample shows that there are long paralleled shaped stripes with 20-30 nm in width and about 500 nm in length on the cleaved surface. The cleaved surface also was etched by 5% HF solution for one minutes, and it became smoother after HF etching. The main feature in on the surface is the spherical particles with the size of few nanometers, and no aggregated fullerenes appear. The fullerenes are well dispersed in the aerogel matrices.

Lu, W. J .

Aerogel Beads as Cryogenic Thermal Insulation System

An investigation of the use of aerogel beads as thermal insulation for cryogenic applications was conducted at the Cryogenics Test Laboratory of NASA Kennedy Space Center. Steady-state liquid nitrogen boiloff methods were used to characterize the thermal performance of aerogel beads in comparison with conventional insulation products such as perlite powder and multilayer insulation (MLI). Aerogel beads produced by Cabot Corporation have a bulk density below 100 kilograms per cubic meter (kg/cubic m) and a mean particle diameter of 1 millimeter (mm). The apparent thermal conductivity values of the bulk material have been determined under steady-state conditions at boundary temperatures of approximately 293 and 77 kelvin (K) and at various cold vacuum pressures (CVP). Vacuum levels ranged from 10(exp -5) torr to 760 torr. All test articles were made in a cylindrical configuration with a typical insulation thickness of 25 mm. Temperature profiles through the thickness of the test specimens were also measured. The results showed the performance of the aerogel beads was significantly better than the conventional materials in both soft-vacuum (1 to 10 torr) and no-vacuum (760 torr) ranges. Opacified aerogel beads performed better than perlite powder under high-vacuum conditions. Further studies for material optimization and system application are in progress.

Fesmire, J. E.

A Fluorescent Aerogel for Capture and Identification of Interplanetary and Interstellar Dust

Aerogels are extremely low-density solids whose superiority as capturing media for hypervelocity (v > 0.5 km/s) grains has been well established. A prominent example is the use of silica aerogel as the collecting medium for cometary and interstellar grains on NASA s Stardust mission. Aerogel collectors have been deployed in low-earth orbit, but severe background from anthropogenic orbital debris has so far prevented the identification of more than a handful of interplanetary particles. No interstellar particles have been identified so far. Since they are on hyperbolic orbits, extraterrestrial particles are faster than orbital debris, so could in principle be identified on that basis, but existing aerogels give little information on impact velocity. With this in mind, we have developed a novel calorimetric aerogel which passively records the kinetic energy of captured hypervelocity particles.

Dominguez, Gerardo

Ultrasonic Micro-Blades for the Rapid Extraction of Impact Tracks from Aerogel

The science return of NASA's Stardust Mission with its valuable cargo of cometary debris hinges on the ability to efficiently extract particles from silica aerogel collectors. The current method for extracting cosmic dust impact tracks is a mature procedure involving sequential perforation of the aerogel with glass needles on computer controlled micromanipulators. This method is highly successful at removing well-defined aerogel fragments of reasonable optical clarity while causing minimal damage to the surrounding aerogel collector tile. Such a system will be adopted by the JSC Astromaterials Curation Facility in anticipation of Stardust s arrival in early 2006. In addition to Stardust, aerogel is a possible collector for future sample return missions and is used for capture of hypervelocity ejecta in high power laser experiments of interest to LLNL. Researchers will be eager to obtain Stardust samples for study as quickly as possible, and rapid extraction tools requiring little construction, training, or investment would be an attractive asset. To this end, we have experimented with micro-blades for the Stardust impact track extraction process. Our ultimate goal is a rapid extraction system in a clean electron beam environment, such as an SEM or dual-beam FIB, for in situ sample preparation, mounting and analysis.

Ishii, H. A.

Carbon Nanofiber Incorporated Silica Based Aerogels with Di-Isocyanate Cross-Linking

Lightweight materials with excellent thermal insulating properties are highly sought after for a variety of aerospace and aeronautic applications. (1) Silica based aerogels with their high surface area and low relative densities are ideal for applications in extreme environments such as insulators for the Mars Rover battery. (2) However, the fragile nature of aerogel monoliths prevents their widespread use in more down to earth applications. We have shown that the fragile aerogel network can be cross-linked with a di-isocyanate via amine decorated surfaces to form a conformal coating. (3) This coating reinforces the neck regions between secondary silica particles and significantly strengthens the aerogels with only a small effect on density or porosity. Scheme 1 depicts the cross-linking reaction with the di-isocyanate and exhibits the stages that result in polymer cross-linked aerogel monoliths.

Vivod, Stephanie L.

Di-Isocyanate Crosslinked Aerogels with 1, 6-Bis (Trimethoxysilyl) Hexane Incorporated in Silica Backbone

Silica aerogels are desirable materials for many applications that take advantage of their light weight and low thermal conductivity. Addition of a conformal polymer coating which bonds with the amine decorated surface of the silica network improves the strength of the aerogels by as much as 200 times. Even with vast improvement in strength they still tend to undergo brittle failure due to the rigid silica backbone. We hope to increase the flexibility and elastic recovery of the silica based aerogel by altering the silica back-bone by incorporation of more flexible hexane links. To this end, we investigated the use of 1,6-bis(trimethoxysilyl)hexane (BTMSH), a polysilsesquioxane precursor3, as an additional co-reactant to prepare silica gels which were subsequently cross-linked with di-isocyanate. Previously, this approach of adding flexibility by BTMSH incorporation was demonstrated with styrene cross-linked aerogels. In our study, we varied silane concentration, mol % of silicon from BTMSH and di-isocyanate concentration by weight percent to attempt to optimize both the flexibility and the strength of the aerogels.

Vivod, Stephanie L.

Aerogels Insulate Against Extreme Temperatures

In 1992, NASA started to pursue the development of aerogel for cryogenic insulation. Kennedy Space Center awarded Small Business Innovation Research (SBIR) contracts to Aspen Systems Inc., of Marlborough, Massachusetts, that resulted in a new manufacturing process and a new flexible, durable, easy-to-use form of aerogel. Aspen Systems formed Aspen Aerogels Inc., in Northborough, Massachusetts, to market the product, and by 2009, the company had become the leading provider of aerogel in the United States, producing nearly 20 million square feet per year. With an array of commercial applications, the NASA-derived aerogel has most recently been applied to protect and insulate people s hands and feet.

Source record

Tailoring of Boehmite-Derived Aluminosilicate Aerogel Structure and Properties: Influence of Ti Addition

Aluminosilicate aerogels offer potential for extremely low thermal conductivities at temperatures greater than 900 C, beyond where silica aerogels reach their upper temperature limits. Aerogels have been synthesized at various Al:Si ratios, including mullite compositions, using Boehmite (AlOOH) as the Al source, and tetraethoxy orthosilicate as the Si precursor. The Boehmite-derived aerogels are found to form by a self-assembly process of AlOOH crystallites, with Si-O groups on the surface of an alumina skeleton. Morphology, surface area and pore size varies with the crystallite size of the starting Boehmite powder, as well as with synthesis parameters. Ternary systems, including Al-Si-Ti aerogels incorporating a soluble Ti precursor, are possible with careful control of pH. The addition of Ti influences sol viscosity, gelation time pore structure and pore size distribution, as well as phase formation on heat treatment.

Hurwitz, Frances I.

Low-Density, Aerogel-Filled Thermal-Insulation Tiles

Aerogel fillings have been investigated in a continuing effort to develop low-density thermal-insulation tiles that, relative to prior such tiles, have greater dimensional stability (especially less shrinkage), equal or lower thermal conductivity, and greater strength and durability. In preparation for laboratory tests of dimensional and thermal stability, prototypes of aerogel-filled versions of recently developed low-density tiles have been fabricated by impregnating such tiles to various depths with aerogel formations ranging in density from 1.5 to 5.6 lb/ft3 (about 53 to 200 kg/cu m). Results available at the time of reporting the information for this article showed that the thermal-insulation properties of the partially or fully aerogel- impregnated tiles were equivalent or superior to those of the corresponding non-impregnated tiles and that the partially impregnated tiles exhibited minimal (<1.5 percent) shrinkage after multiple exposures at a temperature of 2,300 F (1,260 C). Latest developments have shown that tiles containing aerogels at the higher end of the density range are stable after multiple exposures at the said temperature.

Santos, Maryann

Thermal Performance Testing of Order Dependancy of Aerogels Multilayered Insulation

Robust multilayer insulation systems have long been a goal of many research projects. Such insulation systems must provide some degree of structural support and also mechanical integrity during loss of vacuum scenarios while continuing to provide insulative value to the vessel. Aerogel composite blankets can be the best insulation materials in ambient pressure environments; in high vacuum, the thermal performance of aerogel improves by about one order of magnitude. Standard multilayer insulation (MU) is typically 50% worse at ambient pressure and at soft vacuum, but as much as two or three orders of magnitude better at high vacuum. Different combinations of aerogel and multilayer insulation systems have been tested at Cryogenics Test Laboratory of NASA Kennedy Space Center. Analysis performed at Oak Ridge National Laboratory showed an importance to the relative location of the MU and aerogel blankets. Apparent thermal conductivity testing under cryogenic-vacuum conditions was performed to verify the analytical conclusion. Tests results are shown to be in agreement with the analysis which indicated that the best performance is obtained with aerogel layers located in the middle of the blanket insulation system.

Johnson, Wesley L.

Benzimidazole Based Aerogel Materials

The present invention provides aerogel materials based on imidazoles and polyimidazoles. The polyimidazole based aerogel materials can be thermally stable up to 500 C or more, and can be carbonized to produce a carbon aerogel having a char yield of 60% or more, specifically 70% or more. The present invention also provides methods of producing polyimidazole based aerogel materials by reacting at least one monomer in a suitable solvent to form a polybenzimidazole gel precursor solution, casting the polybenzimidazole gel precursor solution into a fiber reinforcement phase, allowing the at least one gel precursor in the precursor solution to transition into a gel material, and drying the gel materials to remove at least a portion of the solvent, to obtain an polybenzimidazole-based aerogel material.

Rhine, Wendell E.