Results for “specimen holder” — Page 3

NASA NTRS1990

Effects of an unbalanced magnetron in a unique dual-cathode, high rate reactive sputtering system

Simple plasma and magnetic field measurements are presented to illustrate the opportunities afforded by using unbalanced magnetrons in a dual-cathode system. The system employs a pair of opposed cathodes, 38 cm x 13 cm, placed 27.5 cm apart, to coat specimens mounted on a rotational substrate holder. Comparisons are drawn between the original 'balanced' magnetron and several unbalanced configurations in terms of field strengths, deposition rates, etching characteristics, and substrate ion current densities for the growth of TiN films. The effects of 'unbalancing' on the nature of the plasma within the 3D geometry of the deposition chamber are elucidated via plasma probe and magnetic field studies performed under a variety of conditions. All the unbalanced configurations examined provided enhanced ion bombardment at the surface of the growing film. The closed-field or opposed magnet geometry resulted in a threefold or greater increase in current density when compared with that obtained using the corresponding mirrored geometry under the same conditions.

Rohde, S. L.↗

NASA NTRS1988

Gas permeation measurements on small polymer specimens

Mass spectrometry was used to measure oxygen and nitrogen permeabilities while polarography was used to measure oxygen permeabilities for several contact lens materials. Applicable sample holders were designed and fabricated to accommodate curved and flat specimens. A prepared standard was used to calibrate the mass spectrometric analyses. The oxygen permeability values determined by mass spectrometry were significantly greater than those determined by polarography. This was attributed to the phase boundary phenomena and the limiting oxygen permeance of water inherent in the polarographic technique. Polarographic values determined were in good agreement with proprietary values obtained by polarography, with the exception of one material.

Burns, Karen S.↗

NASA NTRS1977

Shuttle Spacelab Core Equipment Freezer

This paper describes the preliminary design of a Shuttle Spacelab Core Equipment Freezer. The unit will provide the capability to freeze and store many experiment specimens. Two models of the unit are planned. One model provides storage at -70 C; the other model will provide -70 C storage, a freeze dry capability, storage at a selectable temperature in the range of 0 C to -70 C, and means of maintaining close temperature tolerances. In addition an exchanger loop will be available at 4 C for cooling of a centrifuge and a remote storage compartment. A test tube holder, a dish holder and thermal capacitors for rapid freezing of large specimens will also be provided. A Stirling Cycle was selected as the active refrigerator for minimum cost and weight.

Copeland, R. J.↗

DOE OSTI2025

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Facile Tensile Testing Platform for In Situ Transmission Electron Microscopy of Nanomaterials

In situ tensile testing using transmission electron microscopy (TEM) is a powerful technique to probe structure-property relationships of materials at the atomic scale. In this work, a facile tensile testing platform for in situ characterization of materials inside a transmission electron microscope is demonstrated. The platform consists of: 1) a commercially available, flexible, electron-transparent substrate (e.g., TEM grid) integrated with a conventional tensile testing holder, and 2) a finite element simulation providing quantification of specimen-applied strain. The flexible substrate (carbon support film of the TEM grid) mitigates strain concentrations usually found in free-standing films and enables in situ straining experiments to be performed on materials that cannot undergo localized thinning or focused ion beam lift-out. The finite element simulation enables direct correlation of holder displacement with sample strain, providing upper and lower bounds of expected strain across the substrate. The tensile testing platform is validated for three disparate material systems: sputtered gold-palladium, few-layer transferred tungsten disulfide, and electrodeposited lithium, by measuring lattice strain from experimentally recorded electron diffraction data. The results show good agreement between experiment and simulation, providing confidence in the ability to transfer strain from holder to sample and relate TEM crystal structural observations with material mechanical properties.

2D materials↗

NASA NTRS1979

Attaching strain transducers to fragile materials

A-shaped clamp prevents damage to thin, brittle specimens and supports displacement transducer away from heated zone. Also it defines reference points for strain measurement on specimen surface thus preventing specimen cracking due to unequal thermal expansion between clamp and holder.

Duggan, M. F.↗

NASA NTRS1991

Spacecraft thermal control coatings (AO 138-6)

The experiment A0 138-6 was located on the trailing edge of LDEF as part of the Experiment FRECOPA. Material specimens 2 x 2 cm, independently mounted in sample-holders with their surface in the same reference plane, were exposed to space. Materials include paints (conductive or not), SSMs, polymeric films, surface coatings, composite materials, and metals. The results show that for some materials the degradation was higher for samples in the canister than for those directly mounted on the tray; contamination problems were ruled out, the higher temperature experienced by the samples inside the canister probably explains this phenomenon.

Paillous, Alain↗

NASA NTRS1992

Spacecraft thermal control coatings

The Experiment AO 138-6 was located on the trailing edge of the Long Duration Exposure Facility as part of the French Cooperative Payload (FRECOPA) Experiment. It was purely passive in nature: material specimens 2 x 2 cm, independently mounted in sample-holders, with their surface in the same reference plane, were exposed to space. Thirty samples were set in a vacuum-tight canister which was opened in space a few days after LDEF deployment and closed while still in orbit ten months later; twenty-four samples were directly exposed to space for the total flight duration (preflight handling, shuttle bay environment, separation from shuttle, shuttle environment, LEO environment, docking, descent, transfer to KSC). Materials included paints (conductive or nonconductive), SSM's, polymeric films, surface coatings, composite materials, and metals. After sample retrieving, inspection and measurements were carried out in atmospheric laboratory conditions on each sample: observation with binocular lenses and scanning electron microscopy, spectral relectance and transmittance using an integrating sphere in the wavelength range 280-2300 nm, emissivity by the means of a Gier & Dunkle portable reflectometer, electron spectroscopy for chemical analysis-x-ray photoelectron spectroscopy (ESCA-XPS), and Rutherford backscattering spectroscopy (RBS) measurements on some selected samples. The results obtained from flight were compared to laboratory data obtained in UV-irradiation tests when these data were available. As a general statement a good spectral concordance is observed for all samples not in the canister so long as air recoveries are taken into account. For one material, the degradation is more important for the sample in the canister than for those of the same material mounted at the surface of the tray; for most samples in the canister the degradation is slightly higher than the one which can be predicted from laboratory standard irradiations. Contamination problems having been ruled out, the higher temperature experience by the samples on the inside of canister probably explains these phenomena.

Guillaumon, Jean-Claude↗

NASA NTRS1979

"Gentle" holder for brittle ceramics

Fixture uses commercially available flexible refractory fabric to gently hold brittle ceramic specimens for alignment during high temperature tests up to 2000 F and above. Assembly is held at both ends by water cooled straps that keep fabric/fixture bond area cold during tests.

Stevens, E. G.↗

NASA NTRS1985

Spring-Loaded Transducer Holder

Portable ultrasonic scanner moves transducer at constant pressure. Spring-loaded holder moves ultrasonic transducer over test sample at constant pressure. Setup used to determine rate of debond taking place in glued materials subjected to fatigue loading. Holder designed as portable field unit adapted to fatigue machine that transmits data while specimen tested.

Gardner, M. R.↗

DOE OSTI2020

High Flux Helium Irradiation of Dispersion-Strengthened Tungsten Alloys and Effects of Heavy Metal Impurity Layer Deposition

Tungsten has been chosen as the plasma-facing material (PFM) for the divertor region in ITER and also a candidate PFM for future plasma-burning nuclear fusion reactors. During fusion device operation, PFMs will be exposed to low-energy He irradiation at high temperatures, resulting in sub-surface bubbles and surface morphology changes such as pores and fuzz. Carbide dispersion-strengthened W materials may enhance the ductility of W, but their behavior under high flux He irradiation remains unclear. In this work, the response of dispersion-strengthened tungsten materials to high flux, low energy He irradiation at high temperature is examined. Tungsten alloyed with 1, 5, or 10 wt. % tantalum carbide or titanium carbide exposed to these conditions result in surface pores, coral-like feature growth and sub-surface helium bubbles. Reactor-relevant helium irradiation (5 x 10 26 m -2 fluence) combined with high powered laser pulses to simulate off-normal reactor events does not significantly alter the surface morphology, as the surface nanostructures appear stable and cracks are only observed on a localized region of one sample. However, specimens show the development of an impurity layer on the surface, likely impurity deposition from the sample holder during irradiation, resulting in a mixed material layer on the surface. Helium bubbles exist in this impurity layer, and obscure conclusions about helium interactions with the carbide dispersoids. Nonetheless, it is clear that the dispersoid microstructure limits He bubble formation and subsequent surface nanostructuring, attributed to the dispersoid composition.

36 MATERIALS SCIENCE↗

NASA NTRS1985

Real-time SEM studies in controlled reactive atmospheres

A unique scanning electron accessory has been developed that allows the observation of specimens under partial pressures of any gas. The sample is placed in a metal support boat inside a special sample holder. The sample in the boat is imaged on a CRT and is simultaneously recorded on a videotape, allowing the reaction between the sample and the gas to be observed in real time. Sample changes can be seen continuously as the sample is being heated or cooled. This process allows the observation of material transformations such as phase changes as they happen. Temperatures as high as 1000 C have been used and are continuously monitored using a thermocouple with a digital display on the CRT and videotape. X-ray analyses can also be run before and after any reactions. In the study described here, thick-film screen-printing inks using molybdenum/tin compositions as a replacement for silver were developed to be used on terrestrial photovoltaic cells. Pieces were placed on the sample stage and heated in both O2 and H2 atmospheres. The results were used to determine the most effective frits to be used in the thick-film inks.

Gallagher, B. D.↗

DOE OSTI2021

Measurement of High-temperature Thermophysical Properties of Bulk and Coatings Using Modulated Photothermal Radiometry

This paper presents the development of instrumentation for the measurement of high-temperature thermal conductivity of bulk and coatings using a modulated photothermal radiometry (MPR) method, where a sample is heated by an intensity-modulated laser to probe into different layers of the sample. While MPR has been previously established, most of the previous studies only focus on the measurement at room temperature. The MPR has not been well studied for measurements of bulk and coating materials at high temperatures, which are increasingly important for a multitude of applications, such as materials used in the concentrating solar power (CSP) plants and the nuclear reactors. MPR is a non-contact technique that utilizes the intrinsic thermal emission from the specimens for thermometry, which is favorable for measurements at high temperatures in harsh environment. The authors designed and utilized a sample holder suitable for high temperature measurement up to 973 K with good temperature uniformity within the sample. The high-temperature MPR setup was validated by measuring bulk materials with known thermal conductivity. The setup and technique were then extended to the measurement of black solar-absorbing coatings of 10 to 50 μm thick on various substrates by modulating the frequency of the laser heating beam and the thermal penetration depth. Here, the studies showed that thermal conductivities of typical solar-absorbing coatings are 0.4 ~ 0.8 W m -1 K -1 , indicating a possibly large temperature drop within the coating under high solar irradiation flux, such as over 1000-sun for central solar towers in CSP plants.

14 SOLAR ENERGY↗

DOE OSTI2024

Calibrating cryogenic temperature of TEM specimens using EELS

Cryogenic Scanning/Transmission Electron Microscopy has been established as a leading method to image sensitive biological samples and is now becoming a powerful tool to understand materials' behavior at low temperatures. However, achieving precise local temperature calibration at low temperatures remains a challenge, which is especially crucial for studying phase transitions and emergent physical properties in quantum materials. In this study, we employ electron energy loss spectroscopy (EELS) to measure local cryogenic specimen temperatures. Here we use the temperature-dependent characteristics of aluminum's bulk plasmon peak in EEL spectra, which shifts due to changes in electron density caused by thermal expansion and contraction. We successfully demonstrate the versatility of this method by calibrating different liquid nitrogen cooling holders in various microscopes, regardless of whether a monochromated or non-monochromated electron beam is used. Temperature discrepancies between the actual temperature and the setpoint temperatures are identified across a range from room temperature to 100 K. This work demonstrates the importance of temperature calibrations at intermediate temperatures and presents a straightforward, robust method for calibrating local temperatures of cryogenically-cooled specimens in electron microscopes.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Ultralow-temperature cryogenic transmission electron microscopy using a new helium flow cryostat stage

Advances in cryogenic electron microscopy have opened new avenues for probing quantum phenomena in correlated materials. This study reports the installation and performance of a new side-entry condenZero cryogenic cooling system for JEOL (Scanning) Transmission Electron Microscopes (S/TEM), utilizing compressed liquid helium (LHe) and designed for imaging and spectroscopy at ultra-low temperatures. The system includes an external dewar mounted on a vibration-damping stage and a pressurized, low-noise helium transfer line with a remotely controllable needle valve, ensuring stable and efficient LHe flow with minimal thermal and mechanical noise. Performance evaluation demonstrates a stable base temperature of 4.37 K measured using a Cernox bare chip sensor on the holder with temperature fluctuations within ±0.004 K. Complementary in-situ electron energy-loss spectroscopy (EELS) via aluminum bulk plasmon analysis was used to measure the local specimen temperature and validate cryogenic operation during experiments. The integration of cryogenic cooling with other microscopy techniques, including electron diffraction and Lorentz TEM, was demonstrated by resolving charge density wave (CDW) transitions in NbSe2 using electron diffraction, and imaging nanometric magnetic skyrmions in MnSi via Lorentz TEM. In conclusion, this platform provides reliable cryogenic operation below 7 K, establishing a low-drift route for direct visualization of electronic and magnetic phase transformations in quantum materials.

Charge density wave↗

DOE OSTI2026

High-Temperature SiC Cladding End Plug Irradiation Design and HFIR Readiness

This report documents the design of a High Flux Isotope Reactor (HFIR) irradiation experiment intended to evaluate irradiation effects on the hermeticity of silicon carbide (SiC) end plug specimens under a radial fast neutron flux gradient at representative light-water reactor (LWR) temperatures of approximately 300 °C. The overarching goal of this work is to statistically evaluate SiC end plug hermeticity and mechanical properties following irradiation using the high-throughput irradiation capability discussed here. Each specimen consists of a short section of SiC fiber–reinforced SiC (SiC/SiC) tube with a single monolithic SiC end plug joined to one end. The experiment allows up to 66 specimens to be irradiated in six different stacks within a dry, sealed irradiation capsule derived from the previously developed high-temperature SiC/SiC cladding bowing experiment. The neutronics basis, thermal analysis, and HFIR readiness of the experiment are discussed in this report for two possible design cases. The first design case is based on existing approval documentation and components that are on hand and approved for use, so the experiment insertion would require only specimen receipt, specimen pre-irradiation characterization, experiment assembly, and final fabrication package approval. The second design case provides improved thermal robustness and the preferred end plug geometry but requires fabrication of a modified holder and revisions to the HFIR approval documentation, in addition to the other activities required for the first design case, before insertion.

Hott, Daniel [Oak Ridge National Laboratory (ORNL)↗

DOE OSTI2025

Development of a Target Rod Rabbit Holder Facility in the Large Removable Beryllium Position

A new facility, the removable beryllium-target rod rabbit holder facility (RB*-TRRH), was designed and fielded in the large removable beryllium (RB*) position in the High Flux Isotope Reactor (HFIR). This facility supports three shortened target rod rabbit holders (sTRRHs), which allow for the irradiation of six axially stacked rabbit capsules per sTRRH. This will allow for the simultaneous irradiation of 18 rabbit capsules in the RB* position and will provide an alternative location for low-cost rabbit capsules to be irradiated in HFIR. The first capsules inserted into this facility are 18 perforated capsules that contain representative steel specimens of interest to the calandria of Canada deuterium uranium (CANDU) reactors as part of a lifetime extension program with Canadian Nuclear Laboratories (CNL).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗