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NASA NTRS2008

Triboluminescent Materials for Smart Optical Damage Sensors for Space Applications

There is a need to develop a new technique of damage detection for composites, which could detect cracking or delamination from any desired location within a material structure in real time. Recently, triboluminescent materials have been proposed as smart sensors of structural damage. To sense the damage, these materials can be epoxy bonded, coated in a polymer matrix, or embedded in a composite host structure. When the damage or fracture takes place in the host structure, the resultant fracture of triboluminescent crystals creates a light emission. This will warn in real time that structural damage has occurred. The triboluminescent emission of the candidate phosphor has to be bright enough that the light reaching from the point of fracture to the detector through a fiber optic cable is detectable. There are a large number of triboluminescent materials, but few satisfy the above criterion. The authors have synthesized an organic material known as Europium tetrakis (dibenzoylmethide) triethylammonium (EuD4TEA), which is a potential candidate for application as a damage sensor and could be made into a wireless sensor with the addition of microchip, antenna, and electronics. Preliminary results on the synthesis and characterization of this material are presented.

Aggarwal, M. D.↗

DOE OSTI2015

Engineering the mechanical properties of ultrabarrier films grown by atomic layer deposition for the encapsulation of printed electronics

Direct deposition of barrier films by atomic layer deposition (ALD) onto printed electronics presents a promising method for packaging devices. Films made by ALD have been shown to possess desired ultrabarrier properties, but face challenges when directly grown onto surfaces with varying composition and topography. Challenges include differing nucleation and growth rates across the surface, stress concentrations from topography and coefficient of thermal expansion mismatch, elastic constant mismatch, and particle contamination that may impact the performance of the ALD barrier. In such cases, a polymer smoothing layer may be needed to coat the surface prior to ALD barrier film deposition. We present the impact of architecture on the performance of aluminum oxide (Al{sub 2}O{sub 3})/hafnium oxide (HfO{sub 2}) ALD nanolaminate barrier films deposited on fluorinated polymer layer using an optical calcium (Ca) test under damp heat. It is found that with increasing polymer thickness, the barrier films with residual tensile stress are prone to cracking resulting in rapid failure of the Ca sensor at 50 °C/85% relative humidity. Inserting a SiN{sub x} layer with residual compressive stress between the polymer and ALD layers is found to prevent cracking over a range of polymer thicknesses with more than 95% of the Ca sensor remaining after 500 h of testing. These results suggest that controlling mechanical properties and film architecture play an important role in the performance of direct deposited ALD barriers.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Upgrading the Performance and Stability of Lithium, Manganese-Rich Layered Oxide Cathodes with Combined-Formic Acid and Spinel Coating Treatment

We report improving sluggish rate performance and cycling stability of Li, Mn-rich cathode materials (LMR) is of great importance for practical implementation. Here, dual surface modification on LMR particles with formic acid washing and spinel coating improves the electrochemical performance. Dilute formic acid can remove the Li2CO3 surface impurities and selectively reduce Ni while significantly increasing specific surface area by ~32 %, unlocking more electrochemically active surfaces. Spinel coating enhances cycle stability by suppressing detrimental side reactions at electrode-electrolyte interfaces at high voltage. Post-annealing temperature was found to significantly affect the cathode performance. Higher temperature favors diffusion of transition metal (TM)/Li ions of the spinel coating from surface to the bulk, removing the coating by possible reconstruction into the layered structure and thus degrading the performance. The spinel coating also appears to increase Co 3+ segregation on the particle surface. Compared to the original material, the optimized sample demonstrates 47 % higher capacity retention at 3C and retains 89 % of initial capacity after 150 cycles at 0.5C. Besides, the specific energy density of 523 Wh kg -1 can be attained after 150 cycles at 0.5C. Moreover, the post-cycling analysis of modified sample verifies a better structural integrity with less particle cracking. Altogether, this study portrays an alternative strategy to overcome the shortcomings of LMR cathode materials.

25 ENERGY STORAGE↗

DOE OSTI2025

Formation of Composite SiC/SiC Joints by Embedded Wire Chemical Vapor Deposition

The joining of ceramic monoliths or composites to date has primarily been limited to the formation of brittle monolithic joints using heterogeneous (dissimilar) materials, similar to brazing in metals. The development of a damage-tolerant joint layer by SiC fiber reinforcements is demonstrated here. Tube workpieces made of SiC fiber-SiC matrix composite are joined using a nonwoven SiC fiber mat densified by embedded wire chemical vapor deposition (EWCVD), creating a fiber-reinforced weld-like joint by homogeneous joining. EWCVD uses a localized heating method to target deposition and growth to the joint region specifically, while minimizing thermal damage to the surrounding composite tube material. X-ray computed tomography (XCT) is used to nondestructively characterize as-made joints for relative density, adhesion, and composition. In situ XCT analysis during mechanical testing revealed crack deflections in the bonding layer, which indicates a toughening mechanism typical of ceramic matrix composite phase. Gas permeation testing of these proof-of-concept composite joints identified relatively high leak rates in comparison to fully coated SiC/SiC composite tube workpieces. In conclusion, the novelty of the composite joining method and current technology challenges, including gas permeability, are discussed in comparison with traditional ceramic joints and materials.

SiC↗

DOE OSTI2024

Effects of catholyte aging on high-nickel NMC cathodes in sulfide all-solid-state batteries

Sulfide solid-state electrolytes (SSEs) in all-solid-state batteries (SSBs) are recognized for their high ionic conductivity and inherent safety. The LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) cathode offers a high thermodynamic potential of approximately 3.8 V vs. Li/Li + and a theoretical specific capacity of 200 mA h g −1 . However, the practical utilization of NMC811 in sulfide SSBs faces significant interfacial challenges. The oxidation instability of sulfide solid electrolytes against NMC811 and the formation of the cathode electrolyte interphase (CEI) during cycling lead to degradation and reduced cell performance. Volumetric changes in NMC during lithiation and de-lithiation can also cause detachment from sulfide electrolytes or internal particle cracking. Despite extensive galvanostatic cycling studies to address the issues, the calendar life of sulfide SSBs remains poorly understood. Here, we systematically studied the effects of four different catholytes on the calendar aging of LiNbO 3 (LNO)-coated NMC811, including Li 6 PS 5 Cl (LPSCl), Li 3 InCl 6 –Li 6 PS 5 Cl (LIC–LPSCl), Li 3 YCl 6 –Li 6 PS 5 Cl (LYC–LPSCl), and Li 10 GeP 2 S 12 (LGPS). Our results indicate that LPSCl provides optimal capacity retention when stored at high state-of-charge (SOC) at room temperature, but the LIC–LPSCl cathode shows significant capacity degradation and chemical incompatibility. We also established an effective electrochemical calendar aging testing protocol to simulate daily usage, enabling quick inference of the calendar life of SSBs. In conclusion, this new testing approach accelerates materials selection strategies for high-nickel NMC composite cathodes in sulfide SSBs.

25 ENERGY STORAGE↗

NASA NTRS1978

Array automated assembly task, phase 2. Low cost silicon solar array project

Several modifications instituted in the wafer surface preparation process served to significantly reduce the process cost to 1.55 cents per peak watt in 1975 cents. Performance verification tests of a laser scanning system showed a limited capability to detect hidden cracks or defects, but with potential equipment modifications this cost effective system could be rendered suitable for applications. Installation of electroless nickel plating system was completed along with an optimization of the wafer plating process. The solder coating and flux removal process verification test was completed. An optimum temperature range of 500-550 C was found to produce uniform solder coating with the restriction that a modified dipping procedure is utilized. Finally, the construction of the spray-on dopant equipment was completed.

Rhee, S. S.↗

NASA NTRS2004

Development of Ceramic Matrix Composites For High Temperature Applications

The microstructure and mechanical properties of carbon fiber reinforced silicon carbide (C/SiC) composites that incorporated molecular-level oxidation inhibitors designed to increase the material s high temperature durability were characterized. The viability of a fiber-level inhibitor incorporated as part of a layered interface system as well as a molecularly-integrated matrix-level oxidation inhibitor that is co-deposited with the SiC matrix during Chemical Vapor Infiltration (CVI) was determined. It was expected that the inhibitor would act as a glass former that will getter the oxygen and form a crack sealant to reduce further ingress of oxygen into the composite. Three composites were examined. Composite A was a baseline C(sub f)/SiC(sub m) composite that incorporated a approx. 0.4 micron pyrolytic carbon (PyC) fiber coating to promote strength and toughness, and a CVI-derived SiC matrix. Composite B was a C(sub f)/SiC(sub m) composite incorporating a approx 0.4 micron pyrolytic carbon (PyC) fiber coating to promote strength and toughness, a approx. 0.6 micron B4C fiber-level oxidation barrier coating, and a CVI-derived SiC matrix. Composite C was a C(sub f) /SiC(sub m) composite that incorporated a approx. 0.4 micron pyrolytic carbon (PyC) fiber coating to promote strength and toughness, a approx. 0.6 micron B4C fiber-level oxidation barrier coating, and a BxC-SiC oxidation-inhibited matrix produced by CVI co-deposition. All composites were reinforced with 10 plies of T-300 balanced plain weave carbon fabric with 3K tows at 12.5 ends per inch.

Heimann, Paula↗

DOE OSTI2017

Determination of He and D permeability of neutron-irradiated SiC tubes to examine the potential for release due to micro-cracking

Driven by the need to enlarge the safety margins of light water reactors in both design-basis and beyond-design-basis accident scenarios, the research and development of accident-tolerant fuel (ATF) has become an importance topic in the nuclear engineering and materials community. Continuous SiC fiber-reinforced SiC matrix ceramic composites are under consideration as a replacement for traditional zirconium alloy cladding owing to their high-temperature stability, chemical inertness, and exceptional irradiation resistance. Among the key technical feasibility issues, potential failure of the fission product containment due to probabilistic penetrating cracking has been identified as one of the two most critical feasibility issues, together with the radiolysisassisted hydrothermal corrosion of SiC. The experimental capability to evaluate the hermeticity of SiC-based claddings is an urgent need. In this report, we present the development of a comprehensive permeation testing station established in the Low Activation Materials Development and Analysis laboratory at Oak Ridge National Laboratory. Preliminary results for the hermeticity evaluation of un-irradiated monolithic SiC tubes, uncoated and coated SiC/SiC composite tubes, and neutron-irradiated monolithic SiC tubes at room temperature are exhibited. The results indicate that this new permeation testing station is capable of evaluating the hermeticity of SiC-based tubes by determining the helium and deuterium permeation flux as a function of gas pressure at a high resolution of 8.07 x 10 -12 atm-cc/s for helium and 2.83 x 10 -12 atm-cc/s for deuterium, respectively. The detection limit of this system is sufficient to evaluate the maximum allowable helium leakage rate of lab-scale tubular samples, which is linearly extrapolated from the evaluation standard used for a commercial as-manufactured light water reactor fuel rod at room temperature. The un-irradiated monolithic SiC tube is hermetic, as is manifested by the un-detectable deuterium permeation flux at various feeding gas pressures. A large helium leakage rate was detected for the uncoated SiC/SiC composite tube exposed to atmosphere, indicating it is inherently not hermetic. The hermeticity of coated SiC/SiC composite tubes is strongly dependent on the coating materials and the preparation of the substrate SiC/SiC composite samples. To simulate the practical application environment, monolithic CVD SiC tubes were exposed to neutron irradiation at the High Flux Isotope Reactor under high heat flux from the internal surface to the external surface. Although finite element analysis and resonant ultrasound spectroscopy measurement indicated that the combined neutron irradiation and high heat flux gave rise to a high probability of cracking within the sample, the hermeticity evaluation of the tested sample still exhibited gas tightness, emphasizing that SiC cracking is inherently a statistical phenomenon. The developed permeation testing station is capable of measuring the gas permeation flux in the range of interest with full confidence based on the presented results. It is considered a critical pre- /post-irradiation examination technique to characterize SiC-based cladding materials in asreceived and irradiated states to aid the research and development of ATF.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2016

Evaluating the Upset Protrusion Joining (UPJ) Method to Join Magnesium Castings to Dissimilar Metals

This presentation discusses advantages and best practices for incorporating magnesium in automotive component applications to achieve substantial mass reduction, as well as some of the key challenges with respect to joining, coating, and galvanic corrosion, before providing an introduction and status update of the U.S. Department of Energy and Department of Defense jointly sponsored Upset Protrusion Joining (UPJ) process development and evaluation project. This update includes sharing performance results of a benchmark evaluation of the self-pierce riveting (SPR) process for joining dissimilar magnesium (Mg) to aluminum (Al) materials in four unique coating configurations before introducing the UPJ concept and comparing performance results of the joints made with the UPJ process to those made with the SPR process. Key results presented include: The benchmark SPR process can produce good joints in the MgAM60B-Al 6013 joint configuration with minimal cracking in the Mg coupons if the rivet is inserted from the Mg side into the Al side; Numerous bare Mg to bare Al joints made with the SPR process separated after only 6-wks of accelerated corrosion testing due to fracture of the rivet as a result of hydrogen embrittlement; For the same joint configurations, UPJ demonstrated substantially higher pre-corrosion joint strengths and post-corrosion joint strengths, primarily because of the larger diameter protrusion compared to smaller SPR rivet diameter and reduced degradation due to accelerated corrosion exposure; As with the SPR process, numerous bare Mg to bare Al joints made with the UPJ process also separated after 6-wks of accelerated corrosion testing, but unlike the SPR experience, the UPJ joints experienced degradation of the boss and head because of galvanic corrosion of the Mg casting, not hydrogen embrittlement of the steel rivet; In the configuration where both the Mg and Al were pretreated with Alodine 5200 prior to joining and the complete assembly was powder-coated afterwards, the UPJ process showed substantial improvement in corrosion performance compared to SPR where many SPR joints had separated after only 6-wks of exposure, but none of the UPJ joints had separated even after 8-wis; and In the cases where the Al panel was coated prior to joining to the pretreated Mg coupons, neither the SPR or UPJ joints showed any joint separation or substantial joint performance degradation even after 12-wks of accelerated corrosion exposure.

36 MATERIALS SCIENCE↗

NASA NTRS1975

Thermal fatigue resistance of NASA WAZ-20 alloy with three commercial coatings

Screening tests using three commercial coatings (Jocoat, HI-15, and RT-1A) on the nickel-base alloy NASA WAZ-20 were performed by cyclic exposure in a Mach 1 burner facility. These tests showed Jocoated WAZ-20 to have the best cracking resistance. The thermal fatigue resistance of Jocoated WAZ-20 in both the random polycrystalline and directionally solidified polycrystalline forms relative to that of other superalloys was then evaluated in a fluidized-bed facility. This investigation showed that Jocoated random polycrystalline WAZ-20 ranked approximately in midrange in thermal fatigue life. The thermal fatigue life of directionally solidified Jocoated WAZ-20 was shorter than that of other directionally solidified alloys but still longer than that of all alloys in the random polycrystalline form.

Bizon, P. T.↗

NASA NTRS1966

Coating permits use of strain gage in water and liquid hydrogen

Strain gage installation covered with a three-layer coating of commercial materials makes measurements in water and liquid hydrogen. It consists of a selected foil strain gage bonded with a modified commercial heat-curring epoxy cement. The outer protective layer of the gage installation may develop cracks when immersed in liquid hydrogen.

Berven, B. B.↗

NASA NTRS1979

Effect of grain orientation and coating on thermal fatigue resistance of a directionally solidified superalloy (MAR-M 247)

The effect of off-axis directionally solidified (DS) grain growth on thermal fatigue life of Mar-M 247 alloy was evaluated. Uncoated conventionally cast as well as DS wedge bars were cycled in a burner rig between 1070 C and room temperature. The longitudinal axis and leading edge of the specimen coincided. As the angle between the specimen longitudinal axis and growth axis increased, the thermal fatigue life decreased for both the uncoated and aluminide-coated bars. Life increases of about 50 cycles for the DS conditions were attributed to coating. The decrease in thermal fatigue life with increasing angle is primarily attributed to the increase in modulus of elasticity with increasing angle and not to the intersection of DS grain boundaries with the specimen leading edge. The thermal fatigue cracks were observed to be transgranular in the DS material. Limited tensile and stress-rupture properties of conventionally cast and off-axis DS Mar-M 247 alloy are also presented.

Bizon, P. T.↗

DOE OSTI2016

Method to produce catalytically active nanocomposite coatings

A nanocomposite coating and method of making and using the coating. The nanocomposite coating is disposed on a base material, such as a metal or ceramic; and the nanocomposite consists essentially of a matrix of an alloy selected from the group of Cu, Ni, Pd, Pt and Re which are catalytically active for cracking of carbon bonds in oils and greases and a grain structure selected from the group of borides, carbides and nitrides.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Method to produce catalytically active nanocomposite coatings

36 MATERIALS SCIENCE↗

DOE OSTI2019

Method to produce catalytically active nanocomposite coatings

36 MATERIALS SCIENCE↗

DOE OSTI2023

Sub-stoichiometric metal nitrides

A non-stoichiometric nanocomposite coating and method of making and using the coating. The non-stoichiometric nanocomposite coating is disposed on a base material, such as a metal or ceramic; and the nanocomposite consists essentially of a matrix of an alloy selected from the group of Cu, Ni, Pd, Pt and Re which are catalytically active for cracking of carbon bonds in oils and greases and a grain structure selected from the group of borides, carbides and nitrides.

Eryilmaz, Osman Levent↗

NASA NTRS1989

Fracture resistance of a TiB2 particle/SiC matrix composite at elevated temperature

The fracture resistance of a commercial TiB2 particle/SiC matrix composite was evaluated at temperatures ranging from 20 to 1400 C. A laser interferometric strain gauge (LiSG) was used to continuously monitor the crack mouth opening displacement (CMOD) of the chevron-notched and straight-notched, three-point bend specimens used. Crack growth resistance curves (R-curves) were determined from the load versus displacement curves and displacement calibrations. Fracture toughness, work-of-fracture, and R-curve levels were found to decrease with increasing temperature. Microstructure, fracture surface, and oxidation coat were examined to explain the fracture behavior.

Jenkins, Michael G.↗

DOE OSTI2014

Surface structure and electrical properties of solution processed lanthanum nickelate films

Conducting oxides with perovskite crystal structure have many advantages over the simple Pt or Au, Pt based metal bottom electrodes (BE), particularly in fabrication of ferroelectric as well as resistive random access memory devices, if they possess smooth surface morphology. LaNiO{sub 3} (LNO) thin films were prepared by modified chemical solution deposition method. Precursor solutions were spin coated onto SiO{sub 2}-substrates. Deposited layers were thermally treated in a pre-heated furnace at 550 °C and oxygenated up to 800 °C. Results of AFM and FESEM showed that films are very smooth (Ra = 1.69 nm), dense, crack-free and with monodispersed nanocrystallites. Growth conditions such as spinning rate, annealing rates and temperatures etc. have been optimized for mono dispersed crystallinity with very smooth surface morphology. Sheet resistivity, carrier concentration and RMS roughness were correlated with growth temperatures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗