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The research work described in the present paper was carried out to develop and evaluate thermal protection materials for application to the Space Shuttle and future programs. The philosophy, methodology of testing, and facilities are discussed which had to be developed in view of the new requirements placed on the thermal protection system, in particular the requirement of multiple flight capability.
Metal–organic frameworks (MOFs) provide a versatile platform for incorporating multiple metal ions within a single crystalline framework, yet achieving spatial and stoichiometric order in heterometallic nodes remains a synthetic challenge. Building on our previously reported, highly thermally stable Ce/Ti bimetallic MOF NU-3000, we identified and isolated two additional crystalline phases, NU-2998 and NU-2999, that arise from the same Ce/Ti nanocluster precursor under modified solvothermal conditions. Systematic variation of reaction temperature, time, solvent ratio, and modulator concentration directs the assembly of these distinct frameworks. Structural analysis and comprehensive characterization studies reveal that these MOFs each feature an unreported nodal geometry with nanocavities of different sizes. NU-2998 even adopts an unreported topology, denoted nui , that features an elongated pore spanning 4 nm. Together, these findings establish a synthesis route that starts with a nanocluster and ends with a set of bimetallic MOFs, offering a glimpse into the pathway-dependent assembly of multimetallic porous materials. Finally, we evaluated the thermal stability of each additional analogue and compared them to NU-3000, providing further insight into material stability. NU-3000 maintained the highest thermal stability and was evaluated as a catalyst for CO oxidation at elevated temperatures.
Researchers at Los Alamos have developed a 3D broadband, noncontact, and nonlinear ultrasonic phased array technology that enables businesses to characterize and identify cracks and defects using laserbased sensing at ultra-high resolution. It can be applied to a wide range of commercial and industrial markets, e.g., aerospace, aeronautical, nuclear energy, oil and gas, and civil and material engineering and more broadly to those interested in the non-destructive evaluation (NDE) of materials and structures. Traditional phased-array technology for subsurface imaging operate over a narrow frequency range, with a limited number of sensors, using one type of ultrasonic waves which may decrease the likelihood of detecting a structural material crack. This technology fills the information gap by utilizing the potential of laser-based sensing to remove all these limitations. We are seeking a commercialization partner to license the technology or fund us through a Cooperative Research and Development Agreement (CRADA) to further develop a usable product for commercial purposes.
The NASA/JSC Atmospheric Reentry Materials and Structures Evaluation Facility (ARMSEF) was intensively and extensively involved in ground testing of spacecraft materials and thermal protection systems (TPS) in simulated reentry conditions. Ground experiments on surface catalytic efficiency of such TPS requires a knowledge of the flow system in the arc jet. In the work described, spectroscopic diagnostic techniques are used to determine the free stream constituents. Specifically, the emission spectrum of the free stream constituents was obtained and the species therein identified. A laser system was added on, which will give the added capacity of studying the arc jet flow using Laser Raman Spectroscopy (LRS). The LRS technique will complement information obtained from the emission spectra. A short list of further work that can be done in the area of spectroscopic investigations on the arc jet is mentioned.
The challenges facing the designers of planetary construction machinery, construction methods, and indigenous construction materials are examined. Machinery and methods are studied from the perspective of mass and power constraints, and indigenous material use is viewed from a technical and mass-benefit vantage point. It is argued that the value of an object on the lunar surface is inexorably linked to its mass due to the high cost of space transportation. Payload capabilities and delivery costs for selected U.S. launch vehicles are given in tabular form. Power vs mass for selected construction vehicles and lunar surface hardware is illustrated. It is concluded that construction materials must be evaluated on their mass-cost of production vs the mass of equal materials delivered direct. Machinery must be designed to be both mass and power efficient, with a premium on performance per unit of mass and power.
Multifunctional hydroxyapatites single crystals have been studied for their applications as the laser host material since past several decades. It is only recently their potential has been evaluated for bioactive materials. In the past researches, Czochralski and flux growth methods have been utilized to achieve single crystals. We have used low temperature processing techniques for synthesis. Organic melt was used to achieve oriented fibers by the directional solidification method. This organic treated material has different characteristics than coarsened oxide materials. Our approach involved low temperature processing using nano engineered powders of the material system Na2O-K2O-CaO- MgO-SrO-SiO2. Also, borates were processed by sintering and grain growth. Effect of -ray was studied by measuring the electrical characteristics of radiated samples. Our experiments to further improve mechanical characteristics indicate that substitution of calcium with some other elements such as gallium have great potential to improve the radiation hardening and mechanical properties of bones.
Reusable holders have been devised for evaluating high-temperature, plasma-resistant re-entry materials, especially fabrics. Typical material samples tested support thermal-protection-system damage repair requiring evaluation prior to re-entry into terrestrial atmosphere. These tests allow evaluation of each material to withstand the most severe predicted re-entry conditions.
Chlorofluorocarbon (CFC) 113 is currently specified as the precision cleaning and verification fluid for orbiter materials. The production ban of CFC 113, an ozone-depleting chlorofluorocarbon, has resulted in a search for a replacement cleaning fluid. Recently, the 3M Company announced the manufacture of a new class of cleaning fluids, hydrofluoroethers. The first in this class of cleaning fluids is HFE 7100, perfluorobutyl methyl ether. This cleaning fluid has been submitted for consideration as a replacement for CFC 113. One of the requirements of the certification process for a replacement cleaning fluid is compatibility testing. The Johnson Space Center (JSC) Materials and Manufacturing Division has requested that NASA JSC White Sands Test Facility perform the compatibility testing with HFE 7100 on selected orbiter materials. Most of the materials selected for testing were previously evaluated for compatibility with CFC 113. Some of the materials are new additions to the orbiter or were not available when the compatibility testing was performed with CFC 113. These materials were evaluated with both cleaning fluids and the results were used to compare the response to the cleaning fluid and to satisfy the certification process requirements. It was found that HFE 7100 is generally compatible with the materials tested.
The Performance of staple rayon fiber and AVTEX continuous rayon fiber was evaluated as precursor materials for heatshields. The materials studied were referenced to the IRC FM5055A heatshield materials flown during the past decade. Three different arc jet facilities were used to simulate portions of the reentry environment. The IRC FM5055A and the AVTEX FM5055G, both continuous rayon fiber woven materials having the phenolic impregnant filled with carbon particles were compared. The AVTEX continuous fiber, unfilled material FM5822A was also examined to a limited extent. Test results show that the AVTEX FM5055G material provided a close substitute for the IRC FM5055A material both in terms of thermal protection and roll torque performance.
Tunable solid-state lasers are of enormous interest for applications including fundamental spectroscopy, remote sensing of the earth atmosphere, medical surgery, and optical communications. Efficient and widely tunable lasers have been developed for the 800-1100 nm region based on transition metal doped insulators like e.g. Ti:Sapphire. The development of transition metal lasers operating at longer wavelength, however, has been limited by the luminescence efficiency of existing materials. We are currently evaluating Mn doped Ca5(PO4)3F as a new solid-state laser material for the 1-2 micro-m region. Preliminary spectroscopic studies revealed that Mn:Ca5(PO4)3F exhibits an intense near infrared luminescence which extends from 1100-1300 nm. Based on lifetime measurements we estimated the luminescence quantum efficiency to be as high as 90 deg./0 at room temperature. The near infrared luminescence properties of Mn doped Ca5(PO4)3F and its potential for solid-state laser applications will be discussed in detail.
Design verification tests were performed on samples representing the aerobrake of the Mars/Pathfinder vehicle. The test specimens consisted of the SLA-561V ablator bonded to the honeycomb structure. The primary objective was to evaluate the ablation materials performance and to measure temperatures within the ablator, at the structural bondline and at the back sheet of the honeycomb structure. Other objectives were to evaluate the effect of ablative repair plug material treatment and voids in the heat shield. A total of 29 models were provided for testing in the Ames 60MW arc-jet facility. Of these, 23 models were flat-faced and six remaining models were curved edge ones, intended to simulate the conditions on the curved rim of the forebody where the maximum shear occurred. Eight sets of test conditions were used. The stagnation point heating rates varied from 47 to 240 W/cm2 and the stagnation pressures from 0.15 to 0.27 atm. (The maximum flight values are 132 W/cm2 and 0.25 atm) The majority of these runs were made at a nominal stagnation pressure of 0.25 atm. Two higher pressure runs were made to check the current (denser) ablation material for spallation, or other forms of thermal stress failure. Over 60% of the flatfaced models yielded good thermocouple data and all produced useful surface recession information. Of the five curved-edge models that were tested, only one gave good data; the remaining ones experienced model-holder failure. The test results can be summarized by noting that no failure of the ablative material was observed on any model. Also, the bondline temperature design limit of 250 C was never reached within an equivalent flight time despite a stagnation point heat load that exceeded the maximum flight value by up to 130%. At heating rates of over 200W/cm2 and stagnation pressures of 0.25 atm, or greater, the average surface recessions exceeded 0.5 cm on some models. The surface roughness increased dramatically at pressures above 0.25 atm and was four times greater at 0.27 atm than at 0.25 atm. Procured repair plug material performed much better than room-temperature cured plugs, as observed in the previous tests. Voids in the ablator did not increase local temperatures and gaps did not grow during testing.
During the Hubble Space Telescope (HST) second servicing mission (SM2), astronauts noticed that the multilayer insulation (MLI) covering the telescope was damaged. Large pieces of the outer layer of MLI (aluminized Teflon fluorinated ethylene propylene (Al-FEP)) were torn in several locations around the telescope. A piece of curled up Al-FEP was retrieved by the astronauts and was found to be severely embrittled, as witnessed by ground testing. Goddard Space Flight Center (GSFC) organized a HST MLI Failure Review Board (FRB) to determine the damage mechanism of FEP in the HST environment, and to recommend replacement insulation material to be installed on HST during the third servicing mission (SM3) in 1999. Candidate thermal control replacement materials were chosen by the FRB and tested for environmental durability under various exposures and durations. This paper describes durability testing of candidate materials which were exposed to charged particle radiation, simulated solar flare x-ray radiation and thermal cycling under load. Samples were evaluated for changes in solar absorptance and tear resistance. Descriptions of environmental exposures and durability evaluations of these materials are presented.
Over recent years, ceramic matrix materials such as SiC–SiC and C–C have been gaining interest for use in fusion reactors, light water reactors (LWRs), and high-temperature reactors (HTRs). These materials are good candidates to operate in very high temperature and moderate to high radiation environments. The evaluation of composite materials, in general, is challenging because of variations in precursor materials, variations in the fabrication process across fabricators, and the wide range of potential fiber architectures, to name a few. However, the need to evaluate neutron-irradiated properties adds another layer of complexity, which includes cost, timeline, and specimen size limitations (often associated with irradiation testing). A qualification methodology for the use of ceramic composites is provided in the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code Section III-5-HHB. The methodology is supported by ASTM International (ASTM) guides, which provide a pathway to accomplish this effort. Part of the qualification strategy is for the designer to collect material property data on environmental conditions representative of its design envelope. These data include irradiation effects. This report presents an experimental study and test campaign developed to partially address this gap by providing initial mechanical and physical property data required for design. A variety of different materials using different manufacturing techniques are considered as part of this campaign. The test plan suggests performing a screening or partial irradiation study to assist the designer during the material selection process. The designer can then perform a more comprehensive qualification study if the material performance is promising. This work focuses on the status of the specimen preparations (machining of samples), the current test methods and failure analysis as well as the preparation of irradiation vehicles for the irradiation campaign. The irradiation will be performed at Oak Ridge National Laboratory (ORNL) in the High Flux Isotope Reactor (HFIR) and at Idaho National Laboratory (INL) in the Advanced Test Reactor (ATR).
Additive manufacturing (AM) is an emerging method for cost-efficient fabrication of complex topology nuclear reactor parts from high-strength corrosion resistance alloys, such as stainless steel and Inconel. AM of metallic structures for nuclear energy applications is currently based on laser powder bed fusion (LPBF) process, which has the capability of melting metallic powder and net shaping the structures with relatively high precision. Some of the challenges with using LPBF method for nuclear manufacturing include the possibility of introducing pores into metallic structures. Integrity of AM structures needs to be evaluated nondestructively because material flaws could lead to premature failures in high temperature nuclear reactor environment. Currently, there exist limited capabilities to evaluate actual AM structures non-destructively. Pulsed Thermography Imaging (PTI) provides a capability for non-destructive evaluation (NDE) of subsurface defects in arbitrary size structures. The PTI method is based on recording material surface temperature transients with infrared (IR) camera following thermal pulse delivered on material surface with flash light. The PTI method has advantages for NDE of actual AM structures because the method involves one-sided non-contact measurements and fast processing of large sample areas captured in one image. Following initial qualification of an AM component for deployment in a nuclear reactor, a PTI system can also be used for in-service nondestructive evaluation (NDE) applications. In this report, we describe recent progress in enhancing PTI capabilities in detecting microscopic defects in metallic specimens. SS316 and IN718 specimens were developed with a pattern of subsurface calibrated flat bottom hole (FBH) defects with diameters from 500µm to 200µm. FBH’s were created with EDM (electron discharge machining) drill. PTI imaging data was processed Spatial Temporal Denoised Thermal Source Separation (STDTSS) unsupervised machine learning (ML) algorithm. We show that defects as small as 200µm in SS316 and IN718 can be detected with STDTSS algorithm. To the best of our knowledge, these are the smallest detected defects which are reported in literature.
Additive manufacturing (AM) is an emerging method for cost-efficient fabrication of complex topology nuclear reactor parts from high-strength corrosion resistance alloys, such as stainless steel and Inconel. AM of metallic structures for nuclear energy applications is currently based on laser powder bed fusion (LPBF) process. Some of the challenges with using LPBF method for nuclear manufacturing include the possibility of introducing pores into metallic structures. Integrity of AM structures needs to be evaluated nondestructively because material flaws could lead to premature failures in high temperature nuclear reactor environment. Currently, there exist limited capabilities to evaluate actual AM structures non-destructively. Pulsed Thermal Tomography Imaging (PTT) provides a capability for non-destructive evaluation (NDE) of subsurface defects in arbitrary size structures. The PTT method is based on recording material surface temperature transients with infrared (IR) camera following thermal pulse delivered on material surface with flash light. The PTT method has advantages for NDE of actual AM structures because the method involves one-sided non-contact measurements and fast processing of large sample areas captured in one image. Following initial qualification of an AM component for deployment in a nuclear reactor, a PTT system can also be used for in-service nondestructive evaluation (NDE) applications. In this report, we describe recent progress in enhancing PTT capabilities in detecting and visualizing microscopic defects in metallic specimens. The thermal tomography (TT) algorithm obtains depth reconstructions of spatial effusivity from the data cube of sequentially recorded surface temperatures. However, interpretation of TT images is non-trivial because of blurring of images with increasing depth. To address this challenge, we have developed a deep learning convolutional neural network (CNN) to classify size and orientation subsurface defects in simulated TT images. CNN is trained on a database of TT images created for a set of simulated metallic structures with elliptical subsurface voids. Test of CNN performance demonstrate the ability to classify radii and angular orientation of subsurface defects in TT images. In addition, we have shown that CNN trained on elliptical defects is capable of classifying irregular-shaped defects obtained from scanning electron microscopy (SEM) of stainless steel sections printed with LPBF.
This paper summarizes a 4-year effort to evaluate and implement a nonflammable substitute coolant for application in the Saturn instrument unit (IU) environmental control system (ECS). Discussed are candidate material evaluations, detailed investigations of the properties of the coolant selected, and a summary of the implementation into a flight vehicle.
The evaluation of potentially useful low cost encapsulation materials is discussed. The goal is to identify, evaluate, test and recommend encapsulant materials and processes for the production of cost effective, long life solar cell modules. Technical investigations concerned the development of advanced cure chemistries for lamination type pottants; the continued evaluation of soil resistant surface treatment, and the results of an accelerated aging test program for the comparison of material stabilities. New compounds were evaluated for efficiency in curing both ethylene/vinyl acetate and ethylene/methyl acrylate pottants intended for vacuum bag lamination of solar cells. Two component aliphatic urethane casting syrups were evaluated for suitability as solar module pottants on the basis of optical, physical and fabrication characteristics.
In a variety of high-energy-density (HED) systems, x-rays of a given energy are used to generate shockwaves, bulk motion, and impulse in materials. As radiation energy is deposited within the material, the material is heated. The number of photons of a certain wavelength absorbed is determined by the spectral intensity of the radiation and the material’s opacity evaluated at that wavelength. This heating results in a pressure increase dictated by the material’s equation of state. Depending on the intensity of the absorbed radiation, it may also cause the material to change phase into a liquid, gas, or plasma. The increased pressure drives the heated surface layer to blow off, imparting impulse and sending a compressive wave into the bulk of the material. Additionally, the compression wave interacts with the solid boundary of the material, resulting in a tensile wave that may cause the material to spall. The impulse generated by the deposition of x-ray energy within the sample can be modeled using purely analytical methods, e.g. the Bethe, Bade, Averell, and Yost (BBAY) model. However, the blow-off process is rather complicated, and proper modeling efforts must account for material ejected by spallation, vaporization, jetting, and plasma ablation. For this reason, analytical models have an unclosed term describing the final energy of the blown-off material Ef(z). Prior modeling efforts have arbitrarily fixed this at some value or modeled it using a limiting set of thermodynamic assumptions. The work we are currently performing uses validated simulations using sophisticated photon transport, equation of state, and strength models/data to provide a fit for Ef(z) that is useful for predictive calculation of impulse. We will apply our methodology and show results for different materials and x-ray sources. This work is particularly useful for the design of experiments studying x-ray impulse generation. The present report is outlined as follows. Section 1.2 describes a series of HED experiments investigating x-ray-generated impulse in materials. Section 1.3 describes the computational approach we employ in this study, and presents validation results against the aforementioned experiments. Section 1.4 introduces analytical models for impulse generation, as well as our method for utilizing impulse from simulations to close the models. We discuss the concept of impulse-spectrum sensitivity, it’s application to uncertainty quantification, and derive a very useful analytical expression for it in 1.5. We then summarize recent progress in this project and discuss future work in section 1.6.