Tannin Based Foams Utilizing 10B-Al-N Atomic Layer Deposition

Materials and Coatings
Tannin Based Foams Utilizing 10B-Al-N Atomic Layer Deposition (GSC-TOPS-333)
A composite carbon foam structure derived from “green” sustainable natural resources for radiation shielding
Overview
Atomic layer deposition (ALD) is a cost-effective nanoadditive-manufacturing technique that allows for the conformal coating of substrates with atomic control in a benign temperature and pressure environment. Through the introduction of paired precursor gases, thin films can be deposited on a myriad of substrates regardless of topography. By providing atomic layer control, where single layers of atoms can be deposited, the fabrication of metal transparent films, precise nano-laminates, and coatings of nanochannels and pores is achievable. A characteristic of the surface adsorption and reaction mechanisms in ALD is that they are normally self-limiting, allowing for atomically accurate control of nanometer (nm) thickness. Therefore, high uniformity and precise thickness control make ALD an attractive process for the creation of optical and other nano-scale devices.

The Technology
Commercially available Borric Acid can be deposited along with alumina via a three step ALD process where a boron-10-alumina complex is deposited. The Boron in the alumina complex allows for better gamma ray capture at a significant weight reduction. Boron has one of the largest neutron absorption cross sections of all the elements of the periodic table, and nitrogen has a larger neutron absorption cross section than carbon. Borates play a key role in the operation of nuclear power plants, and they are essential in the safety and control of pressurized water reactors (PWRs) and boiling water reactors. Boron 10 Metal (Boron-10) is a stable (non-radioactive) isotope of Boron. It is both naturally occurring and a produced by fission, can be found via Borric10 acid. By mixing the acid with methanol a precursor has been developed to inject into an ALD reactor system. The super cycle of borric-10 acid along with alumina precursors and water creates the B10-Al-O or N composite. Tannins are nontoxic, renewable, cheap and abundant polyphenolic oligomers extracted from tree barks. They are versatile, natural, phenolic compounds that may be extracted from many tree species. Condensed, flavonoid tannins are considered as an ‘eco-friendly’ base of resin when compared to homologous phenolic materials of petrochemical origin. The polyphenolic structure of condensed tannins explains their reactivity as a base of resin and their high-carbon yield. Tannin extraction from tree bark is an easy and ecological process, using only hot water and a few additives.
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Benefits
  • Cheap and renewable materials
  • High neutron absorption
  • Highly versatile

Applications
  • Radiation shielding
  • Nuclear power plant shielding
Technology Details

Materials and Coatings
GSC-TOPS-333
GSC-18403-1
Patent Pending
Similar Results
Transparent perspective view illustrating an ALD chamber when not processing wafers.
Atomic Layer Deposition Chamber for Automated Semiconductor Processing Equipment
Researchers at JPL have redesigned a typical standalone ALD chamber in a way that is fully compatible with automated semiconductor processing systems, yet maintains the benefits of a conventional ALD chamber—a small-volume reaction chamber, heated sample holders, and laminar gas flow. The unique three-part ALD chamber incorporates the heater, sample transfer mechanism, and laminar gas injectors into a collapsing pancake design, which enables self-assembly within the reaction chamber. The design utilizes a facedown sample arrangement, which reduces particulate contamination compared to standard faceup ALD systems. Integration with the MBE system also ensures that the ALD chamber remains clean and contaminant-free compared with conventional shared-use, standalone ALD systems. Further, the chamber is engineered to use the fewest number of actuators and provide the greatest design flexibility for all types of host systems and ALD processes. Because no automated system currently exists that incorporates both MBE and ALD processes in one unbroken vacuum system, atmosphere exposure is unavoidable when transferring components for processing. Encapsulating ALD and MBE processing chambers offers a significant process improvement and reduces the cost of producing components with precise MBE films. This innovation is anticipated to add great value to advanced image detector processing at JPL, as well as to the semiconductor industry. Originally developed for specific use with a JPL-developed MBE system, this innovation would be useful for any semiconductor industry customer seeking to prevent atmosphere exposure to MBE films prior to ALD processing in an automated system.
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High Atomic Number Coatings for Fabrics
High atomic number materials, such as tantalum, do not bond well to oxygen- and hydroxyl-rich surfaces, such as glass fibers. These metals often form surface oxides when layered on glass fabric, resulting in flaking of the high atomic number material off the fabric during cutting, folding, and/or handling. To improve coating durability, this invention applies a lower atomic number metal as a tie down layer first before applying the high atomic number metal layer. The tie down layer reduces oxide formation between the substrate and the high atomic number material, promoting adhesion. Titanium has shown strong adhesion with different metals and is effective at reducing oxide formation when diffusion bonded to itself or other materials. It has been shown to be effective at improving durability when thermally sprayed onto a glass fiber fabric as a tie down layer for a subsequent tantalum layer (also applied via RF plasma spray). The titanium layer is only approximately 1 mil thick but results in strong adhesion of the tantalum layer by inter-metallic or diffusion bonding. A thermal spray process may be used, as well. This innovation enables the delivery of high atomic metal coating on glass fiber fabrics and other polymeric substrates that are lower cost, lighter weight, and durable to form a flexible cloth material with Z-graded radiation shielding. Coated samples have been produced and the technology is currently at a technology readiness level (TRL) of 4 (prototype).
Credit: NASA
Atomic Layer Deposition-Enhanced Far-to-Mid Infrared Camera Coating
The ALD-Enhanced Far-to-Mid IR Camera Coating is fabricated by first applying a conductively loaded epoxy binder ~500 microns thick onto a conductive metal substrate (e.g., Cu, Al). This serves to provide high absorptance and low reflectance at the longest wavelength of interest, as well as to provide a mechanical buffer layer to reduce coating stress. Borosilicate glass microspheres are coated with a thin film metal via ALD, essentially turning the microspheres into resonators. That film is optically thin in the far infrared and approximates a resistive (~200 ohms per square) coating. Light trapped in the borosilicate glass microspheres is reflected back and forth within the glass–at each contact point, the light is attenuated by 50%. A monolayer of thin metal film-coated borosilicate glass microspheres is applied to the epoxy binder and cured, forming a robust mechanical structure that can be grounded to prevent deep dielectric charging by ionizing radiation in space. Once cured, the far-to-mid IR absorber structure can be coated with a traditional ~20-to-50 microns “black” absorptive paint to enhance the absorption band at short wavelengths, or a “white” diffusive paint to reject optical radiation. At this thickness and broad tolerance, the longwave response of the coating is preserved. Tailoring the electromagnetic properties of the coating layers and geometry enables realization of a broad band absorption response where the mass required per unit area has been minimized. While NASA originally developed the ALD-Enhanced Far-to-Mid IR Camera Coating for the Stratospheric Observatory for Infrared Astronomy mission, its robustness, absorptive qualities, and optical performance make it a significant addition to IR and terahertz imaging systems. The IR camera coating is at Technology Readiness Level (TRL) 3 (experimental proof-of-concept) and is available for patent licensing.
Microscopic nano-texture of MAC
Molecular Adsorber Coating (MAC)
MAC is a zeolite based coating that captures and traps molecules in its microscopically porous structure. This microscopic nano-textured structure, consisting of large open pores or cavities, within a crystal- like structure, provides a large surface area to mass ratio that maximizes available trapping efficiency. MAC is a durable coating that is applied through spray application. These sprayable coatings eliminate the major drawbacks of puck type adsorbers (weight, size, and mounting hardware requirements), resulting in cost savings, mass savings, easier utilization, greater adsorber surface area, more flexibility, and higher efficiency. This coating works in air, as well as vacuum systems, depending on the application. There is potential for ground based spin-off applications of this coating, particularly in areas where contaminants and volatile compounds need to be collected and contained. Example industries include: pharmaceutical production, the food industry, electronics manufacturing (circuit boards and wafers), laser manufacturing, vacuum systems, chemical processing, paint booths, and general gas and water adsorption.
Conductive Oxides
Conductive High-Toughness Oxides
Oxide coatings have been used in thermal and environmental barrier layers for coatings for hot section turbine applications, among other uses. With the PS-PVD method, Glenn researchers observed the formation of a minority phase of a metastable oxide (zirconium oxide) that is usually found only in a vapor state. They found that the high temperatures and fast deposition process of the PS-PVD system incorporated nonequilibrium phases in the coating and retained them at room temperature as well as at high temperature in the absence of oxygen. The material is vaporized and condensed on the surface via a rapid quenching, essentially &#34trapping&#34 this phase in the deposited coating. The coating microstructure and composition can also be manipulated by changing the processing parameters, allowing the thickness of the coating to be tailored to a given application. Since this metastable phase is conductive, this coating can be used as (for example) an extremely sensitive (thermal or temperature) sensor. It also has very good durability and erosion resistance, making it useful as a protective and conductive coating for electronics and microelectronics. This is an early-stage technology requiring additional development, and Glenn welcomes co-development opportunities.
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