Rapid microcantilever preparation for conditional fracture toughness evaluation
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The measurements are reported of the millimeter wave surface resistance R(sub s) at 58.6 GHz of bulk samples of RBa2Cu3O(7-delta) (R = Y,Eu,Dy,Sm,Er) and of YBa2Cu3O(7-delta) superconducting films, in the temperature range from 20 to 300 K. The bulk samples were prepared by cold pressing the powders of RBa2Cu3O(7-delta) into one in. disks. The powders were prepared by several sinterings in one atmosphere of oxygen at 925 C, with grindings between sinterings, to obtain the superconducting phase. The thin films were deposited on SrTiO3 and LaGaO3 substrates by pulsed laser ablation. Each sample was measured by replacing the end wall of a gold-plated Te sub 013 circular mode copper cavity with the sample and determining the cavity quality factor . From the difference in the Q-factor of the cavity, with and without the sample, the R(sub s) of the sample was determined.
For this study, three Pd/H-CHA samples were prepared containing 53.0%, 10.8% and 6.5% paired Al sites at near fixed Si/Al ratio and similar Pd loading. According to H 2 temperature-programmed reduction, Pd was present almost exclusively as isolated cations in the two samples containing the higher concentrations of paired Al sites, whereas in the other sample PdO was also present. Simulated lean cold start tests on the fresh samples conducted in a microflow reactor showed that the sample containing PdO stored the lowest amount of NOx. When tested with CO/H 2 , the sample containing 53.0% paired Al sites showed significantly better storage capacity than the other samples and deactivated less rapidly upon sequential tests. Experiments using lean gasoline engine exhaust revealed similar trends. This study showed that a high concentration of paired Al sites in Pd/H-CHA is beneficial for NOx storage capacity, thermal durability, and minimizing deactivation in the presence of CO/H 2 .
The figure depicts an apparatus that pulverizes brittle material by means of a combination of ultrasonic and sonic vibration, hammering, and abrasion. The basic design of the apparatus could be specialized to be a portable version for use by a geologist in collecting powdered rock samples for analysis in the field or in a laboratory. Alternatively, a larger benchtop version could be designed for milling and mixing of precursor powders for such purposes as synthesis of ceramic and other polycrystalline materials or preparing powder samples for x-ray diffraction or x-ray fluorescence measurements to determine crystalline structures and compositions. Among the most attractive characteristics of this apparatus are its light weight and the ability to function without need for a large preload or a large power supply: It has been estimated that a portable version could have a mass <0.5 kg, would consume less than 1 W h of energy in milling a 1-cm3 volume of rock, and could operate at a preload <10 N. The basic design and principle of operation of this apparatus are similar to those of other apparatuses described in a series of prior NASA Tech Briefs articles, the two most relevant being Ultrasonic/ Sonic Drill/Corers With Integrated Sensors (NPO-20856), Vol. 25, No. 1 (January 2001), page 38 and Ultrasonic/ Sonic Mechanisms for Deep Drilling and Coring (NPO-30291), Vol. 27, No. 9 (September 2003), page 65. As before, vibrations are excited by means of a piezoelectric actuator, an ultrasonic horn, and a mass that is free to move axially over a limited range. As before, the ultrasonic harmonic motion of the horn drives the free-mass in a combination of ultrasonic harmonic and lower-frequency hammering motion. In this case, the free-mass is confined within a hollow cylinder that serves as a crushing chamber, and the free-mass serves as a crushing or milling tool. The hammering of the free-mass against a material sample at the lower end of the chamber grinds the sample into powder in a relatively short time. The restriction of the free-mass to axial motion only makes the grinding very efficient. The free-mass can be fabricated to have teeth on its lower face to enhance the grinding effect. Optionally, there can be a hole at the bottom of the chamber covered with a sieve to tailor the size distribution of the powder leaving the crushing chamber.
In this paper, the effect of nanoparticles Al2O3 and Al3-X compounds (X = Ti, V, Zr) on the improvement of mechanical properties of aluminum alloys for elevated temperature applications is presented. These nanoparticles were selected based on their low cost, chemical stability and low diffusions rates in aluminum at high temperatures. The strengthening mechanism at high temperature for aluminum alloy is based on the mechanical blocking of dislocation movements by these nanoparticles. For Al2O3 nanoparticles, the test samples were prepared from special Al2O3 preforms, which were produced using ceramic injection molding process and then pressure infiltrated by molten aluminum. In another method, Al2O3 nanoparticles can also be homogeneously mixed with fine aluminum powder and consolidated into test samples through hot pressing and sintering. With the Al3-X nanoparticles, the test samples are produced as precipitates from in-situ reactions with molten aluminum using conventional permanent mold or die casting techniques. It is found that cast aluminum alloy using nanoparticles Al3-X is the most cost effective method to produce high strength aluminum alloys for high temperature applications in comparison to nanoparticles Al2O3. Furthermore, significant mechanical properties retention in high temperature environment could be achieved with Al3-X nanoparticles, resulting in tensile strength of nearly 3 times higher than most 300- series conventional cast aluminum alloys tested at 600 F.
Highlights: • A series TiO{sub 2}-reduced graphene oxide (RG) nanocomposites were prepared by hydrothermal methods at different temperature. • The photocatalytic performance of TiO{sub 2}-RG was illustrated by a TiOC interfacial chemical bond. • The photocatalytic properties were investigated by UV–vis test and degrading Rhodamine B. • The results revealed that the nanocomposites obtained at 120 °C possessed the optimum photocatalytic performance. - Abstract: In this study, a hydrothermal-prepared TiO{sub 2}-RG nanocomposites series exhibited excellent photocatalytic activities, of which the results can be largely influenced by a TiOC interfacial chemical bond between TiO{sub 2} nanoparticles and RG nanosheets. A stirring TiO{sub 2}-RG sample was prepared as contrast analysis using the same wet process except for heating. The characteristics of the composites were tested by X-ray diffraction (XRD), Raman, FT-IR, Differential scanning calorimetry (DSC), Thermogravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS) analysis. The photocatalytic properties were verified by UV–vis diffuse reflectance spectra (DRS) testing as well as degrading Rhodamine B (RhB). Our research results show that the better TiOC interfacial chemical bond was formed, the narrower band gap of the nanocomposite was then obtained. The best hydrothermal synthesizing temperature was found out as 120 °C. The TiO{sub 2}-RG nanocomposite, as inexpensive, nontoxic and highly photo-catalytically active, may let it have a potential use in various photocatalytic applications.
Conducting polyaniline/titanium dioxide (PANI/TiO{sub 2}) composites have been succesfully synthesized by insitu polymerization technique. The PANI/TiO{sub 2} nanocomposites of different compositions were prepared by varying weight percentage of TiO{sub 2} nanoparticles such as 10 wt%, 20 wt%, 30 wt%, 40 wt% and 50 wt% into the fixed amount of the aniline monomer. The prepared powder samples were characterized by X-ray diffractometer (XRD) and Scanning electron microscope (SEM). The intensity of diffraction peaks for PANI/TiO{sub 2} composites is lower than that for TiO{sub 2}. SEM pictures show that the nanocomposite were prepared in the form of long PANi chains decorated with TiO{sub 2} nanoparticles. The dielectric properties and AC conductivity were studied in the frequency range1K Hz–10M Hz. At higher frequencies, the composites exhibit almost zero dielectric loss and maximum value of σ{sub ac} is found for a concentration of 20 wt% TiO{sub 2} in polyaniline. The interface between polyaniline and TiO{sub 2} plays an important role in yielding a large dielectric constant in nanocomposites.
The need for next-generation, accident-tolerant fuels has generated significant interest in the restart of domestic fuels testing at the Transient Reactor Test (TREAT) facility. The TREAT reactor is designed to produce large, transient fluxes that replicate the effects of a wide variety of accident conditions on an irradiated fuel sample. Peak powers generated during short pulses approach 20 GW with a neutron flux of approximately 10{sup 17} n cm{sup -2} s{sup -1}. As part of the restart effort, new vehicle designs are being explored for sample irradiation, including the Static Environment Rodlet Transient Test Apparatus (SERTTA) and variants. As part of the SERTTA designs, micro-pocket fission detectors (MPFDs) are being explored for localized flux measurements before, during, and after transient operations. These detectors are also being considered as part of future, core-wide instrumentation for the TREAT reactor. However, the high fluxes associated with the pulses in the TREAT core present certain thermodynamic concerns given their intensity and the amount of energy they will release within the MPFDs within such a short amount of time. Assuming each fission that occurs in a MPFD results in a fission fragment depositing 85 MeV of energy in the substrate on average and each MPFD has 0.5 μg of natural uranium deposited on it, a 100 ms long pulse in the TREAT reactor at 1017 n cm{sup -2} s{sup -1} flux will produce approximately 4.6 x 10{sup 6} fissions in an MPFD. This pulse deposits 6.3 x 10{sup -5} J in the substrate over a 100 ms duration. That amount of energy is sufficient to melt roughly 33% of the Pt under the UO{sub 2} deposition or a circular spot with a diameter of approximately 860 μm. Of course, the above estimate makes a number of simplifying assumptions and ignores heat transfer, but does serve to illustrate the point that this rapid heating effect could be detrimental to the integrity and life of these in-core MPFDs. To study how these layers are affected by large transient neutron fluxes, five samples were prepared, pre-analyzed, and then subjected to a pulse in the central thimble of the Kansas State University TRIGA Mark II reactor to a peak power of 1.58 GW. After being allowed to decay to safer radiation levels, the sample substrates and coatings were inspected using scanning electron microscopy (SEM) to identify any changes to their surface morphology. Indeed, certain changes were found and are discussed in greater detail in this paper.
Technetium (99Tc) immobilization by doping into iron oxide mineral phases may alleviate the problems with Tc volatility during vitrification of nuclear waste. Reduced Tc, Tc(IV), substitutes for Fe(III) in the crystal structure by a process of Tc reduction from Tc(VII) to Tc(IV) followed by co-precipitation of Fe oxide minerals. Two Tc-incorporated Fe minerals (Tc-goethite and Tc-magnetite/maghemite) were prepared and tested for Tc retention in glass melt samples at temperatures between 600 – 1,000 oC. After being cooled, the solid glass specimens prepared at different temperatures were analyzed for Tc oxidation state using Tc K-edge XANES. In most samples, Tc was partially oxidized from Tc(IV) to Tc(VII) as the melt temperature increased. However, Tc retention in glass melt samples prepared using Tc-incorporated Fe minerals were moderately higher than in glass prepared using KTcO4 because of limited and delayed Tc volatilization.
We report on tubular cladding optical waveguides fabricated in Neodymium doped Wollastonite-Tricalcium Phosphate glass in the eutectic composition. The glass samples were prepared by melting the eutectic powder mixture in a Pt-Rh crucible at 1600 °C and pouring it in a preheated brass mould. Afterwards, the glass was annealed to relieve the inner stresses. Cladding waveguides were fabricated by focusing beneath the sample surface using a pulsed Ti:sapphire laser with a pulsewidth of 120 fs working at 1 kHz. The optical properties of these waveguides have been assessed in terms of near-field intensity distribution and transmitted power, and these results have been compared to previously reported waveguides with double-line configuration. Optical properties have also been studied as function of the temperature. Heat treatments up to 700 °C were carried out to diminish colour centre losses where waveguide's modes and transmitted power were compared in order to establish the annealing temperature at which the optimal optical properties were reached. Laser experiments are in progress to evaluate the ability of the waveguides for 1064 nm laser light generation under 800 nm optical pumping.
Copper (Cu) activated LiF phosphor in nanocrystalline form has been prepared by the chemical co-precipitation method for radiation dosimetry application. The formation of nanocrystalline structure has been confirmed by X-ray diffraction and Scanning electron microscopy. Cubical shaped nanostructure with average particle size of 33nm has been formed. The sample was prepared at different concentration of Cu from 0.01mol% to 3 mol%. TL properties were investigated by studying the glow curve after irradiating the phosphor to gamma ray Co{sup 60} source with dose of 15 Gy. It has been found that nanocrystalline LiF: Cu show simple glow curve structure with a single glow peak at 404 K where as commercially available phosphors exhibits multi peak complex glow curve structure. The effect of different normality on the TL properties of phosphor has been studied. Maximum TL intensity for LiF: Cu (0.1mol %) phosphor is observed at the normality of 0.5N and annealing temperature of 200°C. The phosphor showed good linearity up to 10 KGy.
Task 2 of the IFCMCP was designed to utilize vibrational spectroscopy, microscopy, X-ray diffraction, and calorimetry to explore the spectroscopic, structural, and chemical properties of plutonium compounds relevant to the nuclear fuel cycle. An important precursor to this work is production of fresh, high-quality plutonium samples. Given the health hazards and material accountability associated with plutonium, sample production is not trivial and production experiments require extensive planning and coordination by research and support staff. Further, because alpha-emissions from plutonium produce time- and dose dependent radiolysis resulting in structural defects, particularly in the presence of water, freshly prepared plutonium samples must be carefully packaged and analyzed with urgency following their production. In FY21, SRNL and UND engaged in numerous research studies involving production and subsequent characterization of plutonium dioxide, plutonium fluoride, plutonium oxalate, and plutonium nitrate. Specific efforts involving each of these compounds are described in detail in the body of this report.
Conducting polyaniline/tin oxide (PANI/SnO{sub 2}) nanocomposites have been successfully synthesized by in-situ polymerization technique. The PANI/SnO{sub 2} nanocomposites of different compositions were prepared by varying weight percentage of SnO{sub 2} nanoparticles such as 10 wt%, 20 wt%, 30 wt%, 40 wt% and 50 wt% into the fixed amount of the aniline monomer. The prepared powder samples were characterized by X-ray diffractometer (XRD), Fourier Transform Infrared spectroscopy (FT-IR) and Scanning electron microscope (SEM). The intensity of diffraction peaks for PANI/SnO{sub 2} composites is increases with increasing SnO{sub 2} wt%. SEM observation showed that the prepared SnO{sub 2} nanoparticles were uniformly dispersed and highly stabilized throughout the macromolecular chain that formed a uniform metal-polymer nanocomposite material. AC electrical conductivity and dielectric properties were studied in the frequency range of 1 KHz -1 MHz. At higher frequencies, the composites exhibit almost zero dielectric loss and maximum value of AC electrical conductivity (σ{sub ac}) of 0.21 S/m is found for a concentration of 30 wt% of SnO{sub 2} in polyaniline.
The SRS salt-stone Facility is designed and permitted to immobilize and dispose of low-level radioactive and hazardous liquid waste (salt solution) remaining from the processing of radioactive material at the Savannah River Site. The salt-stone Processing Facility (SPF) is permitted as a wastewater treatment facility per the South Carolina Department of Health and Environmental Control Regulations (SCDHEC) South Carolina Hazardous Waste Management Regulations (SCHWMR) R.61-67. The salt-stone Disposal Facility is permitted as a solid waste landfill site, as defined by SCDHEC Regulations R61-107.19. The salt-stone Sampling and Analysis Plan provides the SCDHEC with the chemical and physical characterization strategy for the salt solution and salt-stone waste form. During operation, samples are collected from Tank 50H on a quarterly basis and are analyzed by the Savannah River National Laboratory (SRNL) for over chemical and radioactive components. The analytical results are compared to the salt-stone waste acceptance criteria in a technical report. SRNL also prepares salt-stone samples from the quarterly sample and premix binder materials provided by the SPF to determine the non-hazardous nature of the grout to meet the requirements of the SCDHEC regulation for the 'Characteristic of Toxicity', R.61-79.261.24(b) and the 'Universal Treatment Standards', R.61-79.268.48.4. salt-stone samples are collected, size reduced, packaged, and shipped to an independent United States EPA certified laboratory, or a laboratory that holds an equivalent certification such as one from the National Environmental Laboratory Accreditation Program to perform the EPA Toxicity Characteristic Leaching Procedure (TCLP) extraction of the salt-stone sample. SRNL reviews the results of the TCLP analysis and prepares a report detailing the sample preparation and analysis that is used by the salt-stone Facility to demonstrate the nonhazardous nature of the salt-stone waste form. (authors)
Light microscopy conducted on samples of Archean sediments reveals phosphate microaggregates which are suggestive of a biotic origin (Arrhenius et al., 1993). These aggregates, typically 15 micrometers wide and 50 micrometers long, are thought to be the mineral remains of colonies of microorganisms that lived during the late Archean Eon (greater than or equal to 2.5 Ga). Confocal microscopy was used to study the structures of these microaggregates in three dimensions. Samples used in this study are from the lowermost section of drill core taken from the Dales Gorge Member of the Brockman Iron-Formation (Hamersley Basin) in Western Australia. These sediments are well-preserved and escaped extensive metamorphism typically experienced by older rocks of this type. Two types of samples were prepared for study under the microscope: thin sections (30 micrometers) for transmitted light microscopy to study the general rock texture and to locate the grains of interest, and thick sections (3mm) for confocal microscopy to determine the 3-D structure of the aggregates in situ. The samples have been carefully polished so that they may be directly placed on the oil-immersion lens without the use of a cover slip. No chemical treatments of the surfaces have been performed. The aggregates often form clusters, although isolated aggregates have also been found. The clusters tend to distribute along microbands in the rocks. Electron microprobe analyses show that the phosphate grains and their inclusions, besides calcium and phosphorus, contain no major elements heavier than sodium. The proportions of calcium to phosphorus, the absence of stoichiometric amounts of other cations such as magnesium and iron, as well as optical properties suggest apatite as the mineral form.
The Adaptive Caching Assembly (ACA) is part of the Sampling and Caching System on the Mars 2020 Perseverance Rover, and consists of multiple stations that process, hermetically seal, and store sample tubes containing collected Martian material, either rock cores or regolith samples, in preparation for caching on the surface of Mars. The ACA stations consist of seven active degrees-of-freedom, as well as a large number of passive mechanisms that must operate in extreme Mars temperature and pressure conditions. A robotic arm within the Rover manipulates the sample tubes between ACA stations as part of an end-to-end sampling sequence, and utilizes a compliant end effector to accommodate misalignments during station interactions. Stringent hardware cleanliness requirements were dictated to ensure collected samples would not be compromised, which significantly impacted the design, assembly, and test operations of the ACA. Three ACAs were assembled to support ground testing and flight operations, which were exposed to environmental testing to validate functionality in Mars-like conditions. A number of challenges existed from design through test, including volume constraints, mechanism controllability and operation, the effects of tight tolerances, and cleanliness requirements.
We describe the phase stability of a cemented tungsten carbide prepared using a high-vanadium tool steel as the cementing/binder phase and confirm suppression of (Fe, W) 6 C η-phase formation, attributed to the preferential formation of a V 0.78 W 0.22 C 1-x phase that exists as islands within the Fe-rich binder matrix. The samples were prepared using spark plasma sintering (SPS), starting from commercially available WC and A11-LVC tool steel powders. The starting powders were ball milled adding 10, 15, and 20 vol.% steel. An A11-LVC tool steel was chosen as a low-cost hard steel (49 HRC) that does not contain Ni or Co but has a high vanadium (~9 wt.%) and carbon (~1.75 wt.%) content. Our results show that sintering by SPS can produce high-density (>98%) WC-steel specimens in which the matrix wets the WC grain surfaces and formation of the brittle η-phase is avoided. The η phase is often regarded as embrittling and undesirable, and its presence can result in degradation of mechanical properties. Microhardness values for the WC-10 and WC-15 vol.% steel samples were 12.3 ± 1.2 and 13.0 ± 0.9 GPa, respectively, whereas the fracture toughness values were 8.83 ± 0.48 and 8.81 ± 0.61 MPa·m 1/2 , respectively.
Iron is one of the abundant elements of Mother Nature and its compound, iron oxide is an interesting material to study since its discovery in the form of magnetite. It can exist in many phases such as hematite and maghemite, this unique nature has put it as a potential candidate in various applications. The aim of this work is to study the influence of different precursor concentrations on the microstructural and magnetic properties of iron oxide thin film. All samples were prepared via the sol-gel method followed by a spin coating technique on quartz substrates. Iron oxide films were confirmed as maghemite phase from X-ray diffraction patterns. The film morphology was examined by a field emission scanning electron microscope and it showed non-systematic value of average grain size and film thickness throughout the study. Hysteresis loop further confirmed that maghemite is a magnetic material when it was characterized by a vibrating sample magnetometer. The coercivity did not show any correlation with molarity. Nevertheless, it increased as the precursor concentration of the film increased due to the domain behaviour. In conclusion, maghemite thin films were successfully synthesized by the sol-gel method with different precursor concentrations in this work.