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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
NASA NTRS2001

Dynamic Fatigue of ULE Glass

Ultra Low Expansion (ULE) glass is used in a number of applications which require a low thermal expansion coefficient. One such application is telescope mirror elements. An allowable stress can be calculated for this material based upon modulus of rupture data; however, this does not take into account the problem of delayed failure. Delayed failure, due to stress corrosion can significantly shorten the lifetime of a glass article. Knowledge of the factors governing the rate of subcritical flaw growth in a given environment enables the development of relations between lifetime, applied stress and failure probability for the material under study. Dynamic fatigue is one method of obtaining the necessary information to develop these relationships. In this study, the dynamic fatigue method was used to construct time-to-failure diagrams for both 230/270 ground and optically polished samples. The grinding and polishing process reduces the surface flaw size and subsurface damage, and relieves residual stress by removing materials with successively smaller grinding media. This resulted in an increase in the strength of the optic during the grinding and polishing sequence. There was also an increase in the lifetime due to grinding and polishing. It was found that using the fatigue parameters determined from the 230/270 grit surface are not significantly different from the optically polished values. Although the lower bound of the polished samples is more conservative, neither time-to-failure curves lie beyond the upper or lower bound of the confidence limits. Therefore, designers preferring conservative limits could use samples without residual stress present (polished samples) to determine the fatigue parameters and inert Weibull parameters from samples with the service condition surface, to determine time-to-failure of the optical element.

Tucker, Dennis S.↗
DOE OSTI2022

Alternate Methods for Cleaning Zirconium Plate

The United States High Performance Research Reactor Conversion Program identified the need to transition from highly enriched uranium fuel to lowly enriched uranium fuel for high power research and civil reactors. One of the fuel configurations selected for these reactors was a uranium (U) foil alloyed with 10% molybdenum (Mo). The U-10Mo fuel foil was then covered with a zirconium (Zr) interlayer and pressed into an aluminum cladding. Idaho National Laboratory prescribed a need to remove surface oxidation on the Zr prior to bonding it with U-10Mo fuel foil. To determine the best method of oxidation removal, a variety of polishing methods, including hand polishing with a diamond paste or Scotch-Brite™ pads, mechanically wet-polishing with abrasive belts, and chemical etching with hydrofluoric/nitric acid mixtures, were investigated on pre-polished Zircaloy 702 sheets purchased directly from the manufacturer. No change in surface roughness was detected using any of these methods relative to the as-received material. In fact, scanning electron microscopy detected grit from hand polishing with Amplex Grade 30 waste soluble diamond paste and Scotch-Brite™ pads. Visible staining was found, and fluorine detected via X-ray photoelectron spectroscopy on the flash etching samples. These contaminants were not seen on the as-received material. In addition to the need to remove the oxide layer on the Zr prior to co-rolling, there are concerns that the Neolube debonding agent on the co-rolling can may contaminate the Zr surface after co-rolling. The experimental results found that zirconium in contact with Neolube coated steel plates was easily cleaning with ethanol wiping after heat treated and no carbide inclusions remained on the surface. Overall, all cleaning methods tested did not significantly change the surface roughness of the plates or reduce the oxide layer present on the zirconium. Carbon was found on all the samples, before and after cleaning, except for the flash etch samples which detected fluorine instead. The insignificant changes seen in the cleaned plates relative to the as received plates question the need for cleaning prior to rolling. Further investigation in the requirements for cleaning at this step is recommended. Current methods for cleaning the surface after hot rolling with alcohol appear sufficient. After hot rolling, if Neolube does peel off the can and onto the zirconium coated foil surface, a dry abrasive or diamond paste polish is not recommended due to the chance of abrasive being embedded into the surface. However, the ability of an etchant to lift the lubricant off the zirconium surface indicates that a spot etch method could work to clean specific spots where Neolube is present, if the need arises.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Electropolishing of a Full-Sized U-10Mo Plate

Electropolishing is used to remove material from the surface of a metal using electric potential and current. U-10Mo fuel is produced from a low enriched uranium plate alloyed with 10% molybdenum (U-10Mo). Electropolishing is being considered in two steps of the process of fabricating this U-10Mo fuel. First, it could be used as a means initially improving the surface finish of the cast plate while removing smut from the casting process from the surface prior to homogenization. Second, it could be used again after homogenization to remove oxidation and continue to improve the surface finish prior to hot rolling. The purpose of this work is to demonstrate the process on full-size ingots and optimize the process. A depleted uranium U-10Mo plate was electropolished three times: the first two times were prior to homogenization and the third after a homogenization step. The first two polishes decreased the overall roughness, as measured by laser confocal microscopy. After each polish, a smoother and shinier blue-gold surface was left on the plate. Upon homogenization, the surface had a more matte appearance and the surface roughness increased back to the pre-homogenization values obtained prior to the initial polish. After electropolishing the homogenized pieces, the changes in surface roughness increased, as measured by laser confocal microscopy. The final polishing step was not long enough to return the surface roughness to pre-homogenization conditions, implying less polishing is needed before the homogenization versus afterwards. Heat generation during the polish was addressed by circulating the electrolyte solution through an external heat exchanger; however, solubility and anodization challenges require further study.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1995

High efficiency radioisotope thermophotovoltaic prototype generator

A radioisotope thermophotovoltaic generator space power system (RTPV) is lightweight, low-cost alternative to the present radioisotope thermoelectric generator system (RTG). The fabrication of such an RTPV generator has recently become feasible as the result of the invention of the GaSb infrared sensitive photovoltaic cell. Herein, we present the results of a parametric study of emitters and optical filters in conjuction with existing data on gallium antimonide cells. We compare a polished tungsten emitter with an Erbia selective emitter for use in combination with a simple dielectric filter and a gallium antimonide cell array. We find that the polished tungsten emitter is by itself a very selective emitter with low emissivity beyond 4 microns. Given a gallium antimonide cell and a tungsten emitter, a simple dielectric filter can be designed to transmit radiant energy below 1.7 microns and to reflect radiant energy between 1.7 and 4 microns back to the emitter. Because of the low long wavelength emissivity associated with the polished tungsten emitter, this simple dielectric filter then yields very respectable system performance. Also as a result of the longer wavelength fall-off in the tungsten emissivity curve, the radiation energy peak for a polished tungsten emitter operating at 1300 K shifts to shorter wavelengths relative to the blackbody spectrum so that the radiated energy peak falls right at the gallium antimonide cell bandedge. The result is that the response of the gallium antimonide cell is well matched to a polished tungsten emitter. We propose, therefore, to fabricate an operating prototype of a near term radioisotope thermophotovoltaic generator design consisting of a polished tungsten emitter, standard gallium antimonide cells, and a near-term dielectric filter. The Jet Propulsion Laboratory will design and build the thermal cavity, and JX Crystals will fabricate the gallium antimonide cells, dielectric filters, and resultant receiver panels. With 250 Watts of heat input, we expect this prototype to produce over 300 Watts of electrical energy output for a system energy conversion efficiency of over 12%. This low risk, near term design provides advances relative to present radioisotope thermophotovoltaic generators and has the additional advantage of allowing component and system development and testing to begin immediately. Improved cells and filters can easily be incorporated in this baseline system if they should become available in the future.

Avery, James E.↗
NASA NTRS1961

Electron and Light Microscopy Techniques Suitable for Studying Fatigue Damage in a Crystallized Glass Ceramic

The crystals of Pyroceram are randomly oriented and highly reflective so that standard microscopy techniques are not satisfactory for studying this material. Standard replicating procedures proved difficult to use. New microscopy techniques and procedures have therefore been developed. A method for locating, orienting, and identifying specific areas to be viewed with an electron microscope is described. This method not require any special equipment. Plastic replicas were found to be unsatisfactory because of their tendency to adhere to Pryoceram. This caused them to tear when released or resulted in artifacts. Preshadowed silicon monoxide replicas were satisfactory but required a releasing agent. A method of depositing the releasing agent is described. To polish specimens without evidence of fire-polishing, it was found necessary to use a vibratory polishing technique. Chrome oxide was used as the abrasive and either water or kerosene as the lubricant. Vibratory polishing is extremely slow, but surfaces so polished show no evidence of fire polishing, even when examined by electron microscopy. The most satisfactory etching process used for Pyroceram 9608 consisted of a primary etch of 5 milliliters of hydrochloric acid (concentrated), 5 milliliters of hydrogen fluoride (45 percent), and 45 milliliters of water, and a secondary etch with methyl alcohol replacing the water. Best results were obtained with total etching times from 25 to 30 seconds. Staining of the Pyroceram surface with a Sanford's marker was found to be an expedient way to reduce the glare of reflected light.

Harrell, Shelley↗
NASA NTRS2015

Grazing Incidence Optics Technology

This project is to demonstrate the capability to directly fabricate lightweight, high-resolution, grazing-incidence x-ray optics using a commercially available robotic polishing machine. Typical x-ray optics production at NASA Marshall Space Flight Center (MSFC) uses a replication process in which metal mirrors are electroformed on to figured and polished mandrels from which they are later removed. The attraction of this process is that multiple copies can be made from a single master. The drawback is that the replication process limits the angular resolution that can be attained. By directly fabricating each shell, errors inherent in the replication process are removed. The principal challenge now becomes how to support the mirror shell during all aspects of fabrication, including the necessary metrology to converge on the required mirror performance specifications. This program makes use of a Zeeko seven-axis computer-controlled polishing machine (see fig. 1) and supporting fabrication, metrology, and test equipment at MSFC. The overall development plan calls for proof-of-concept demonstration with relatively thick mirror shells (5-6 mm, fig. 2) which are straightforward to support and then a transition to much thinner shells (2-3 mm), which are an order of magnitude thinner than those used for Chandra. Both glass and metal substrates are being investigated. Currently, a thick glass shell is being figured. This has enabled experience to be gained with programming and operating the polishing machine without worrying about shell distortions or breakage. It has also allowed time for more complex support mechanisms for figuring/ polishing and metrology to be designed for the more challenging thinner shells. These are now in fabrication. Figure 1: Zeeko polishing machine.

Ramsey, Brian↗
NASA NTRSDate not supplied

Making Thin Sections from National Treasures: A Little Moon Rock Goes a Long Way

NASA’s Johnson Space Center curates the Apollo sample collection through their facilities in Houston, TX. It is a dual-purpose facility, intended both to store and preserve the precious samples, as well as to make them available for ongoing scientific study and public examination. The facilities consist of multiple vaults and lab spaces, including the Apollo Thin Section Lab. Although it is a part of the Curation facilities, this lab is intended to process specific lunar rock and dust samples into what are called “thin sections”. A thin section is a microscope slide with a very thin, highly polished slice of rock material mounted on it. These are used not only for microscope viewing, but also for a range of other sophisticated scientific instruments to map and measure fine details of the rock’s physical and chemical composition and structure. The process of making a thin section requires great care and patience and is an art in itself; each one is unique, and each sample can behave very differently while going through the same basic procedures. In general, it begins by taking a small chip of rock from a much larger sample. The rock fragment is placed within a small mold and liquid epoxy is poured over it and allowed to harden, producing what is called a “potted butt” (Figure 1). This is to stabilize the rock so that it won’t fragment or crumble during polishing, and to fill any cracks or voids within the rock. Once hardened, the epoxy on the bottom is carefully ground away to expose the rock surface within, which is then polished to a 1-micron finish. A thin new layer of fresh epoxy is then applied to the polished surface and used to mount it to a silica slide. Once the mounting epoxy has hardened, the potted butt is cut off less than one millimeter above the slide using a low-speed circular saw. This thin layer of sample material attached to the slide undergoes further grinding and polishing, typically bringing the sample thickness down to about 35 microns – roughly one third of the thickness of a human hair. The remaining potted butt is saved for future scientific investigations and can be re-polished and used again until all the rock material within it is used up. A single thin section can be reused countless times by numerous different researchers. In addition, thin sections are often exquisitely beautiful (Figure 2) and in some cases, lunar thin sections are used as public display samples, such as at the Smithsonian Air and Space Museum in Washington, DC. The production of thin sections allows an immense variety of research to be conducted on a tiny amount of rock or mineral material, allowing the bulk of the Apollo collection to stay pristine and unaltered, and thus, remain available for next generation of lunar scientists to further our insight into the Moon’s geological diversity, and to bring valuable new insights to our understanding of the origin of the Earth-Moon system.

J J Kent↗
DOE OSTI2024

Validation of the VUV-reflective coating for next-generation liquid xenon detectors

Abstract Coating detector materials with films highly reflective in the vacuum ultraviolet region improves sensitivity of the next-generation rare-event detectors that use liquid xenon. In this work, we investigate the MgF 2 -Al-MgF 2 coating designed to achieve high reflectance at 175 nm, the mean wavelength of liquid xenon (LXe) scintillation. The coating was applied to an unpolished, passivated copper substrate mimicking a realistic detector component of the proposed nEXO experiment, as well as to two unpassivated substrates with “high” and “average” levels of polishing. After confirming the composition and morphology of the thin-film coating using TEM and EDS, the samples underwent reflectance measurements in LXe and gaseous nitrogen (GN2). Measurements in LXe exposed the coated samples to -100°C for several hours. No peeling of the coatings was observed after several thermal cycles. Polishing is found to strongly correlate with the measured specular reflectance (R spec ). In particular, 5.8(5)% specular spike reflectance in LXe was measured for the realistic sample at 20° of incidence, while the values for similar angles of incidence on the high and average polish samples are 62.3(1.3)% and 27.4(7)%, respectively. At large angles (66°–75°), theR spec in LXe for the three samples increases to 23(5)%, 80(8)%, and 84(18)%, respectively. The R spec at around 45° was measured in both GN2 and LXe for average polish sample and shows a reasonable agreement. Importantly, the total reflectance of the samples is comparable and estimated to be 92(8)%, 85(8)%, and 83(8)% in GN2 for the realistic, average, and high polish samples, respectively. This is considered satisfactory for the next-generation LXe experiments that could benefit from using reflective films, such as nEXO and DARWIN, thus validating the design of the coating.

Instruments & Instrumentation↗
DOE OSTI2022

Ion Exchange Processing of AP-105 Hanford Tank Waste through Crystalline Silicotitanate in a Staged 2- then 3-Column System (Rev.1)

The Tank Side Cesium Removal (TSCR) system, under development by Washington River Protection Solutions LLC (WRPS), will send initial low-activity Hanford waste tank supernate feeds to the Hanford Waste Treatment and Immobilization Plant (WTP) Low-Activity Waste (LAW) Facility. In addition to entrained solids removal from the supernate, the primary goal of TSCR is to remove cesium-137 ( 137 Cs) by ion exchange, allowing contact handling of the liquid effluent product at the WTP. Crystalline silicotitanate (CST) ion exchange media, manufactured by Honeywell UOP, LLC (product IONSIVTM R9140-B), was selected as the ion exchange media at TSCR. CST is a non-elutable inorganic material that has demonstrated robust chemical, physical, and radiation tolerance while maintaining functionality. However, exchange kinetics of Cs onto CST is slow, resulting in low utilization of the CST Cs load capacity before unacceptable Cs breakthrough. Two process flow designs have been tested, as follows. 1. Lead-lag column processing: The lead column was removed after the lag column effluent reached the waste acceptance criteria (WAC) limit, the lag column was moved into the lead position, and a new lag column was installed. This format used ~52% Cs load capacity on the lead column. 2. Lead-lag-polish column processing: The processing was stopped when the polish column effluent reached the WAC limit. This format resulted in 81% Cs load capacity on the lead column. Testing with diluted feed from Hanford tank AP-105 (AP-105DF) incorporated a nuanced change to the lead-lag-polish column system where the polish column was inserted when the lag column effluent reached WAC limit. A 10.9-L volume of AP-105DF (diluted to 5.6 M Na) was processed through the Direct Feed Test Platform system, established at Pacific Northwest National Laboratory to support small-scale waste qualification efforts. The columns consisted of 10-mL CST beds (CST Lot 2002009604, sieved to screen out >30-mesh particles) placed in 1.5-cm-inner-diameter columns. Feed was processed at 1.83 bed volumes (BV) per hour; the flowrate, in terms of contact time with the CST bed, matched the expected flowrate at TSCR. The <30-mesh CST sieve cut was expected to provide appropriate performance scaling to a full-height column. The installation of the polish column later in processing (after processing 523 BVs) did not appear to fundamentally change the utilization of the lead column for Cs exchange nor did it extend the total feed processing volume when compared to the previous test with AP-107 feed. Table ES.1 and Figure ES.1 summarize the measured AP-105DF Cs load performance.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Nanoscale Consequences of Irradiation Investigated by RAD-AFM (Final Report)

To assess the feasibility of measuring material property changes induced by ion irradiation one pristine and three legacy HT-9 samples were sectioned and polished. The polish protocol was first optimized using a pristine unirradiated HT-9 sample before polishing the ion irradiated samples as the spot size was small and repeated polishing could remove the ion irradiated region entirely. AFM tapping mode was used to assess the surface quality after each polish. AFM based hardness mapping was optimized for new diamond tips specifically for use with the HT-9 samples to compensate for differences in grain size, precipitates, and heterogeneity of hardness relative to past samples. In addition, a hardness calibration protocol was developed using NIST copper, nickel, and steel reference materials. Co-located SEM-EDS and AFM analysis was used to verify the ion irradiated edge using the silver/tungsten coating as a fiducial mark. Once benchmarked, the hardness across the ion irradiated cross section, a comparison of bulk hardness according to neutron irradiation, and the hardness of the ion irradiated surface edge was measured.

36 MATERIALS SCIENCE↗
NASA NTRS1978

Fatigue behavior of two alloys for Space Shuttle applications

Two superalloys used extensively in the Space Shuttle main engine are Incoloy 903 and Inconel 718. The fatigue behavior of the two alloys under varying conditions is considered. Three heats of Incoloy 903 and two of Inconel 718 were used in the study. Material was tested in several conditions, including mill polish, longitudinal mill polish, transverse mill polish, chemically milled, chemically milled plus shotpeened on one side and on both sides, gas tungsten arc welded, and electron beam welded. Both round and flat tensile specimens were tested in universal test machines. It was found that surface condition influences test results. Transverse scratches resulting from polishing and rougher surfaces lower the stress at runout in relation to that obtained on longitudinally polished and/or smooth-surfaced specimens.

Adsit, N. R.↗
NASA NTRS1993

Readying advanced composites for the microscope

Concerns related to the proper preparation of composite specimens for microstructural analysis are examined. Proper preparation will minimize the amount of surface and subsurface damage at each stage of the procedure so that the microstructural features of the final-polished specimen can be accurately determined as a function of the composite's response to processing, testing, or service conditions. This requires that an optimum combination of abrasive type, size, and bond be applied during each grinding, lapping, and polishing step. Machine settings, such as polishing speed, force, and relative polishing direction, are also important. Guidelines are given for each step of the six-stage specimen preparation process: sectioning, planar grinding, sample integrity, polishing, and etching.

Zipperian, Donald C.↗
NASA NTRS1994

Neutral Ion Figuring of Chemical Vapor Deposited SiC

Ion figuring of optical components is a relatively new technology that can alleviate some of the problems associated with traditional contact polishing. Because the technique is noncontacting, edge distortions and rib structure print through do not occur. This investigation was aimed at determining the effect of ion figuring on surface roughness of previously polished or ductile ground ceramic optical samples. This is the first step in research directed toward the combination of a prefinishing process (ductile grinding or polishing) with ion figuring to produce finished ceramic mirrors. Multiple, chemical vapor deposited silicon carbide (CVD SiC) samples were polished or ductile ground to specular or near-specular roughness. These samples were then characterized to determine topographic surface information. The surface evaluation consisted of stylus profilometry, interferometry, and optical and scanning electron microscopy. The surfaces were then ion machined to depths from 0 to 5 micron. The finished surfaces were characterized to evaluate the effects of the ion-machining process with respect to the previous processing methods and the preexisting subsurface damage. This study provides some of the information required to effectively utilize a combined ductile grinding or polishing with ion machining as a procedure for figuring optical components.

Fawcett, Steven C.↗
NASA NTRS2001

Fabricating High Resolution Mirrors for Hand X-Ray Astronomy

We describe the fabrication process for producing high-resolution conical mirrors for hard x-ray astronomy. When flown aboard stratospheric balloons, these high-resolution reflective mirrors focus hard x-rays (10-70 keV) emitted from cosmic sources such as supernovae, neutron stars, and quasars onto imaging focal plane detectors. Focused hard x-ray images allow scientists to determine the elemental compositions, temperatures, magnetic fields, velocities, and gravitational fields of these celestial bodies. The fabrication process involves generating super-polished mandrels, mandrel metrology, mirror shell nickel electroforming, and mirror testing. Each mandrel is a cylinder consisting of two conical segments; each segment is approximately 305-mm long. Through precision grinding these mandrels before super polishing, we have achieved 30 arc seconds, half power diameter replicated mirrors. During a May 2001 high atmosphere balloon flight, these mirrors focused high energy x-rays from three different celestial sources. However, we seek to improve the angular resolutions of future mirror shells by a factor of two. To achieve this goal, we have begun single point diamond turning the mandrels before super polishing. This has allowed greater precision tolerances on mandrel surface roughness and axial figure errors before super polishing. Surface roughnesses before polishing have been reduced from approximately 60 nm to approximately 15 nm. The peak to valley axial figure profile errors have been reduced from approximately 1.0 micrometers to approximately 0.4 micrometers. We are currently in Phase 2 of the HERO (high energy replicated optics) program which entails the production of sixteen 6-m-focal-length mirror modules, each containing a nested array of 15 mirror shells of diameters ranging from 50-mm to 94-mm. This flight is slated for the fall of 2003.

Speegle, Chet O.↗
NASA NTRS2011

Method of fabricating a whispering gallery mode resonator

A method of fabricating a whispering gallery mode resonator (WGMR) is provided. The WGMR can be fabricated from a particular material, annealed, and then polished. The WGMR can be repeatedly annealed and then polished. The repeated polishing of the WGMR can be carried out using an abrasive slurry. The abrasive slurry can have a predetermined, constant grain size. Each subsequent polishing of the WGMR can use an abrasive slurry having a grain size that is smaller than the grain size of the abrasive slurry of the previous polishing iteration.

Savchenkov, Anatoliy A.↗
NASA NTRS2012

Progress in the Fabrication and Testing of Telescope Mirrors for the James Webb Space Telescope

The telescope of the James Webb Space Telescope (JWST) is an f/20, three mirror anastigmat design, passively cooled (40K) in an L2 orbit. The design provides diffraction limited performance (Strehl > or = 0.8) at .=2 m. To fit within the launch vehicle envelope (Arianne V), the 6.6 meter primary mirror and the secondary mirror support structure are folded for launch, then deployed and aligned in space. The primary mirror is composed of 18 individual, 1.3 meter (flat flat) hexagonal segments, each adjustable in seven degrees of freedom (six rigid body + radius of curvature) provided by a set of high precision actuators. The actuated secondary mirror (approx.0.74m) is similarly positioned in six degrees of rigid body motion. The approx..70x.51m, fixed tertiary and approx. 0.17m, flat fine steering mirror complete the telescope mirror complement. The telescope is supported by a composite structure optimized for performance at cryogenic temperatures. All telescope mirrors are made of Be with substantial light-weighting (21 kg for each 1.3M primary segment). Additional Be mounting and supporting structure for the high precision (approx.10nm steps) actuators are attached to the primary segments and secondary mirror. All mirrors undergo a process of thermal stabilization to reduce stress. An extensive series of interferometric measurements guide each step of the polishing process. Final polishing must account for any deformation between the ambient temperature of polishing and the cryogenic, operational temperature. This is accomplished by producing highly precise, cryo deformation target maps of each surface which are incorporated into the final polishing cycle. All flight mirrors have now completed polishing, coating with protected Au and final cryo testing, and the telescope is on track to meet all system requirements. We here review the measured performance of the component mirrors and the predicted performance of the flight telescope.

Bowers, Charles↗
NASA NTRS1960

Factors Affecting the Ductility and Strength of NaCl Single Crystals Tested in Flexure

An experimental investigation has revealed that the initial deformation of NaCl single crystals is anelastic rather than Hookean. This anelastic deformation is manifested by a low slope foot in the load‐deflection curve. The magnitude of the foot is dictated by the pretreatment given the specimen. Treatments which increase or decrease the fresh dislocation density respectively increase or decrease the length of the initial anelastic foot. The order of increasing ductility and strength with specimen pretreatment was found to be (1) heated at 135 C, (2) as cleaved, (3) coated with silver, (4) heated at 135 C and then water polished, (5) water polished and then coated with silver, (6) water polished, (7) water polished and then heated at 135 C, (8) annealed at 700 C, and (9) annealed at 700 C and then water polished. The experimental results have been discussed in terms of the role played in deformation and fracture by surface cracks, grown‐in dislocations, and fresh dislocations.

Stearns, C. A.↗
DOE OSTI2025

Analysis of Niobium Electropolishing Using a Generalized Distribution of Relaxation Times Method

Using electrochemical impedance spectroscopy, we have devised a method of sensing the microscopic surface conditions on the surface of niobium as it is undergoing an electrochemical polishing (EP) treatment. The method uses electrochemical impedance spectroscopy (EIS) to gather information on the surface state of the electrode without disrupting the polishing reaction. The EIS data is analyzed using a so-called distribution of relaxation times (DRT) method. Using DRT, the EIS data can be deconvolved into discrete relaxation time peaks without any a priori knowledge of the electrode dynamics. By analyzing the relaxation time peaks, we are able to distinguish two distinct modes of the EP reaction. As the polishing voltage is increased, the electrode transitions from the low voltage EP mode, characterized by a single relaxation time peaks, to the high voltage EP mode, characterized by two relaxation time peaks. We theorize that this second peak is caused by the formation of an oxide layer on the electrode. We also find that this oxide induced peak transitions from to a negative relaxation time, which is indicative of a blocking electrode process. By analyzing EPed samples, we show that samples polished in the low voltage mode have significantly higher surface roughness due to grain etching and faceting. We find that the surface roughness of the samples only improves when the oxide film peak is present and in the negative relaxation time region. This shows that EIS combined with DRT analysis can be used to predict etching on EPed Nb. This method can also be performed before or during the EP, which could allow for adjustment of polishing parameters to guarantee a smooth cavity surface finish.

43 PARTICLE ACCELERATORS↗