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At least 667 records · Page 37

All sources NASA NTRS DOE OSTI

DOE OSTI2012

Enhancement of thermoelectric figure-of-merit at low temperatures by titanium substitution for hafnium in n -type half-Heuslers Hf 0.75–x Ti x Zr 0.25 NiSn 0.99 Sb 0.01

We report the effect of titanium (Ti) substitution for hafnium (Hf) on thermoelectric properties of (Hf, Zr)-based n-type half-Heuslers: Hf 0.75–x Ti x Zr 0.25 NiSn 0.99 Sb 0.01 , has been studied. The samples are made by arc melting followed by ball milling and hot pressing via the nanostructuring approach. A peak thermoelectric figure-of-merit (ZT) of ~1.0 is achieved at 500 °C in samples with a composition of Hf 0.5 Zr 0.25 Ti 0.25 NiSn 0.99 Sb 0.01 due to a slight increase in carrier concentration and also a lower thermal conductivity caused by Ti. The ZT values below 500 °C of hot pressed Hf 0.5 Zr 0.25 Ti 0.25 NiSn 0.99 Sb 0.01 samples are significantly higher than those of the same way prepared Hf 0.75 Zr 0.25 NiSn 0.99 Sb 0.01 samples at each temperature, which are very much desired for mid-range temperature applications such as waste heat recovery in automobiles.

nanostructuring↗

DOE OSTI2021

Thermal Evolution of Internal Strain in Doped PbTe

Recent improvements in the efficiency of heat-to-electricity energy conversion in lead chalcogenide thermoelectrics involve reducing the thermal conductivity by incorporating large amounts of internal strain. The extent to which typical lead chalcogenide processing techniques (such as doping, ball milling, and densification) increase internal strain and dislocation density must be quantified to improve materials design. In this study, neutron powder diffraction is leveraged to evaluate the internal strain introduced by ball milling in doped and undoped powders. Doping with Na and/or Eu increases internal strain beyond ball milling alone, with the greatest increase from combining the two dopants. Strain recovery occurs in each powder above 400 K but can be suppressed by co-doping, indicating a strong dopant–dislocation interaction in this system. Therefore, high-temperature processing of PbTe powders should be avoided if high internal strain is desired. Low-temperature densification and/or rapid pressing techniques may be key to maintaining internal strain in the final pressed pellet. The diffraction peak asymmetry and correlated elastic softening measured in pressed PbTe pellets in past studies were not observed in the precursor powders measured here, suggesting that measurements of the Debye temperature on final pressed pellets are required to examine the influence of defect-induced elastic softening on thermal conductivity. This work provides key guidance for defect engineering to maximize internal strain and thermoelectric performance in PbTe thermoelectrics.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Anisotropy analysis of thermoelectric properties of Bi{sub 2}Te{sub 2.9}Se{sub 0.1} prepared by SPS method

The n-type Bi{sub 2}Te{sub 2.9}Se{sub 0.1} materials were synthesized by the direct fusion technique. The polycrystalline samples were fabricated by the uniaxial pressing of powders in spark plasma sintering (SPS) apparatus. The materials were subjected to the heat treatment in H{sub 2}-Ar atmosphere at 470 K for 24 h. The influence of preparation conditions on the anisotropy of electrical and thermal properties was thoroughly studied for the direction perpendicular and parallel to the pressing force. The microstructure and the chemical composition of both types of samples were examined using a scanning microscope (SEM) equipped with an X-ray energy dispersion detector (EDX). The XRD method was applied for the phase analysis of materials, as well as, for determination of preferred orientation of Bi{sub 2}Te{sub 2.9}Se{sub 0.1} grains. The Seebeck coefficient distribution was studied by the scanning thermoelectric microprobe (STM). Temperature dependences of thermoelectric properties (thermal and electrical conductivities, Seebeck coefficient) were measured in the temperature from 300 K to 550 K. The statistical analysis of results has shown strong influence of pressing force direction both on structural and transport properties. The applied heat treatment of materials significantly improves their thermoelectric figure of merit. Particularly, it was found that annealing in H2-Ar atmosphere leads to enhancement of the ZT three times up to {approx}0.7 at 370 K in perpendicular direction to the pressing force.

36 MATERIALS SCIENCE↗

DOE OSTI2014

A study of ferromagnetic signals in SrTiO{sub 3} nanoparticles

It has been suggested that ferromagnetism may be a universal feature of nanoparticles related to particle size. We study this claim for the case of commercially produced SrTiO{sub 3} nanoparticles purchased from Alfa-Aesar. Both loosely-packed nanoparticle samples and pellets formed using uniaxial pressure were studied. Both loose and pressed samples were annealed in either air or in vacuum of 5×10{sup −6} Torr at 600, 800 and 1000°C. Then x-ray diffraction and SQUID measurements were made on the resulting samples. It was found that annealed loose powder samples always had a linear diamagnetic magnetization versus field response, while their pressed pellet counterparts exhibit a ferromagnetic hysteresis component in addition to the linear diamagnetic signal. Williamson-Hall analysis reveals that the particle size in pressed pellet samples increases with annealing temperature but does not change significantly in loose powder samples. The main conclusion is that the act of pressing pellets in a die introduces a spurious ferromagnetic signal into SQUID measurements.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Growth and optical properties of partially transparent Eu doped CaF{sub 2} ceramic

Partially transparent ceramic of 2 at.% Eu doped CaF{sub 2} have been grown preferentially towards [111] direction. For this purpose, Eu doped CaF{sub 2} nanoparticles (size∼12 nm) obtained by a low temperature solution growth method has been pressed at 1000°C under vacuum. The preferentially grown ceramic shows 15% transparency within the visible range of spectrum. As confirmed by the X-ray diffraction result, the hot pressed ceramic exhibits reduced lattice volume than the nanopowder. It indicates Eu{sup 3+} as the dominant substituting ions at the Ca{sup 2+} sites of CaF{sub 2} lattice in the hot pressed ceramic material. It is corroborated by the photoluminescence results of hot pressed ceramic which shows strong red emission corresponding to Eu{sup 3+} sites. However, photoluminescence of nanopowder exhibits intense peak in the blue region of the spectrum which is characteristics of Eu2+ sites.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2023

Effect of PBX prill size on the compressive properties of PBX 9502

Plastic-Bonded Explosive (PBX) prills are agglomerates a few millimeters in diameter composed of High Explosive crystals non-uniformly distributed in and surrounded by a polymer binder. When pressed at elevated temperatures at or above the binder melt temperature the polymer flows to uniformly coat the HE crystals to create a well-consolidated compaction. In reality it does so imperfectly, such that x-ray tomographic scans often look like a collection of prills mashed together. It is speculated that the larger the prill, the more non-uniform the binder distribution, but this has never been proven. Even if that were not so, the larger the prill the farther binder must flow toward the middle to homogenize during pressing. Thus, the degree of homogenization depends in part on prill size. The degree to which binder flows during pressing in turn affects the void distribution within pressed charges, which one suspects will affect shock sensitivity and material strength. In this paper we explore, for ~30 PBX 9502 formulation batches using the same TATB powder lot, how prill size affects the compressive mechanical properties.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Determining Infrared Optical Constants for Dolomite using Single Angle Reflectance and Spectroscopic Ellipsometry

The optical constants, namely the real (n) and imaginary (k) parts of the complex refractive index, are of particular interest to generate the infrared (IR) spectra of liquid and solid materials in different morphologies. To obtain n/k, however, most materials are typically not found in the monolithic forms necessary to easily measure n/k, and thus require the use of other methods such as pressing powders to form planar, specularly-reflective pellets. In this work dolomite crystals are measured using fixed-angle IR reflectance spectroscopy in both 1) a monolithic form with the crystal fixed in epoxy and polished, but data are also recorded from 2) pressed-pellet forms of powders of the same mineral using the same spectroscopic protocols. First results for the two methods are compared. It was found that the measured reflectance can vary by as much as a factor of two between the dolomite crystals and the pressed powder forms. For the two-sample preparation approaches the preliminary spectra are compared and the implications and limitations of each method for determining the optical constants of given materials are discussed. Comparison to literature data suggest that polarization effects likely account for the differing amplitude results for reflectance (and hence the k -vectors): Dolomite is known to be biaxial with significantly differing ordinary and extraordinary rays; the pressed pellet method measures an ensemble of microcrystals in randomly oriented positions, whereas the single crystal maintains just one orientation relative to the optical axis.

ellipsometry, dolomite, complex refractive index, ↗

DOE OSTI2013

An elastography method based on the scanning contact resonance of a piezoelectric cantilever

Purpose: Most tissues may become significantly stiffer than their normal states when there are lesions inside. The tissue's modulus can then act as an identification parameter for clinic diagnosis of tumors or fibrosis, which leads to elastography. This study introduces a novel elastography method that can be used for modulus imaging of superficial organs. Methods: This method is based on the scanning contact-resonance of a unimorph piezoelectric cantilever. The cantilever vibrates in its bending mode with the tip pressed tightly on the sample. The contact resonance frequency of the cantilever-sample system is tracked at each scanning point, from which the sample's modulus can be derived based on a beam dynamic model and a contact mechanics model. Scanning is performed by a three-dimensional motorized stage and the whole system is controlled by a homemade software program based on LabVIEW. Results: Testing onin vitro beef tissues indicates that the fat and the muscle can be easily distinguished using this system, and the accuracy of the modulus measurement can be comparable with that of nanoindentation. Imaging on homemade gelatin phantoms shows that the depth information of the abnormalities can be qualitatively obtained by varying the pressing force. The detection limit of this elastography method is specially examined both experimentally and numerically. Results show that it can detect the typical lesions in superficial organs with the depth of several centimeters. The lateral resolution of this elastography method/system is better than 0.5 mm, and could be further enhanced by using more scanning points. Conclusions: The proposed elastography system can be regarded as a sensitive palpation robot, which may be very promising in early diagnosis of tumors in superficial organs such as breast and thyroid.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2020

Fabrication of lignocellulosic biomass paper containing nanofibrillated biomass

Fibrillated cellulose has been frequently used for making nanopapers and thin films. However, limited work has been carried out in the construction of such materials using native lignocellulosic biomass. Making papers from fibrillated biomass allows complete utilization of whole plant material and may reduce chemical and energy consumption. Ultra-friction grinding was used to directly fibrillate knife-milled poplar into micro- to nano-sized biomass fibers. Papers were made using the fibrillated biomass containing nanofibrillated biomass and their mechanical properties were tested. Biomass papers made via press-drying had higher tensile strength than papers made by air-drying. A higher press-drying temperature of 180 °C produced stronger papers than at 150 °C. Guar gum substantially increased the strength of the press-dried papers in comparison to cationic starch. Press-drying increased the thermogravimetric peak decomposition temperature by 13 °C in comparison to air-drying.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2024

Adhesion in thermomechanically processed seaweed-lignocellulosic composite materials

The increasing concerns associated with petroleum-derived polymers motivate the development of sustainable, renewably sourced alternatives. In ubiquitous applications such as structural materials for infrastructure, the built environment as well as packaging, where natural materials such as wood are used, we rely on nonrenewable and nondegradable polymers to serve as adhesives. In wood panels, such as medium density fiberboards (MDFs), formaldehyde-based resins are predominantly used to bond wood fibers and to provide strength to the materials. To further mitigate the environmental impact of construction materials, more sustainable adhesives need to be investigated. Here, in this article, we introduce Ulva seaweed as an adhesive to enable cohesion and strength in hot-pressed wood panels. Upon hot-pressing, powdered Ulva flows in between the wood particles, generating a matrix, which provides strong binding. We show that the flexural strength of Ulva-bonded wood biocomposites increases with increasing Ulva concentrations. At an Ulva concentration of 40 wt%, our composites reach an average elastic modulus of 6.1 GPa, and flexural strength of 38.2 MPa (compared to 4.7 GPa and 22.6 MPa, respectively, for pure wood compressed at the same pressing conditions). To highlight the bonding mechanisms, we performed infrared and x-ray photoelectron spectroscopy and identified indications of fatty acid mobility during hot-pressing. In addition, we demonstrate that the presence of Ulva improves other properties of the composites such as water resistance and fame retardancy. Ulva is also shown to behave as an excellent adhesive agent between two prepressed beams. Finally, we perform an in-depth analysis of the environmental impact of wood-Ulva biocomposites.

36 MATERIALS SCIENCE↗

DOE OSTI2016

ONE-DIMENSIONAL TIME TO EXPLOSION (THERMAL SENSITIVITY) TESTS ON PETN, PBX-9407, LX-10, AND LX-17

Incidents caused by fire and combat operations can heat energetic materials that may lead to thermal explosion and result in structural damage and casualty. Some explosives may thermally explode at fairly low temperatures (< 100 C) and the violence from thermal explosion may cause a significant damage. Thus it is important to understand the response of energetic materials to thermal insults. The One Dimensional Time to Explosion (ODTX) system at the Lawrence Livermore National Laboratory has been used for decades to measure times to thermal explosion, threshold thermal explosion temperature, and determine the kinetic parameters of thermal decomposition of energetic materials. Samples of different configurations (pressed part, powder, paste, and liquid) can be tested in the system. The ODTX testing can also provide useful data for assessing the thermal explosion violence of energetic materials. This report summarizes the results of our recent ODTX experiments on PETN powder, PBX-9407 pressed part, LX-10 pressed part, LX-17 pressed part and compares the test data that were obtained decades ago with the older version of ODTX system. Test results show the thermal sensitivity of various materials tested in the following order: PETN> PBX-9407 > LX-10 > LX-17.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Effect of PBX Prill Size on the Compressive Properties of PBX 9502

36 MATERIALS SCIENCE↗

DOE OSTI2019

A Paris-Edinburgh Cell for High-Pressure and High-Temperature Structure Studies on Silicate Liquids Using Monochromatic Synchrotron Radiation

A Paris-Edinburgh press combined with a multi-channel collimator assembly has been commissioned at the GeoSoilEnviro Center for Advanced Radiation Sources (GSECARS) beamline for monochromatic X-ray scattering, with an emphasis on studying low-Z liquids, especially silicate liquids at high pressure. The Paris-Edinburgh press is mounted on a general-purpose diffractometer, with a pixel array detector mounted on the detector arm. The incident monochromatic undulator beam with energies up to 60 keV is focused both horizontally and vertically to a beam size about 30 × 30 µm. With this setup, background scattering from the surrounding pressure media is completely removed at 2θ angles above 10° for samples larger than 1.05 mm in diameter. Thirty minutes is typically sufficient to collect robust X-ray scattering signals from a 1.6 mm diameter amorphous silicate sample. Cell assemblies for the standard Paris-Edinburgh anvils have been developed and pressures and temperatures up to 7 GPa and 2300 K, respectively, have been maintained steadily over hours. We have also developed a cupped-toroidal Drickamer anvil to further increase pressure and temperature capabilities. The cupped-toroidal Drickamer anvil combines features of a modified Drickamer anvil and the traditional Paris-Edinburgh anvil. Pressures up to 12 GPa have been generated at temperatures up to 2100 K.

58 GEOSCIENCES↗

NASA NTRS1977

Consolidation of silicon nitride without additives

The feasibility of producing a sound, dense Si3N4 body without additives was explored, using conventional gas hot isostatic pressing techniques and an uncommon hydraulic hot isostatic pressing technique. These two techniques produce much higher pressure 275-413 MN/m sq (40,000 - 60,000 psi) than hot-pressing techniques. Evaluation was based on density measurement, microscopic examination, both optical and electron, and X-ray diffraction analysis. The results are summarized as follows: (1) Si3N4 can be densified to high density, greater than 95% of theoretical, without additions. (2) The higher density Si3N4 specimens appear to be associated with a greater amount of alpha to beta transformation. (3) Under high pressure, the alpha to beta transformation can occur at a temperature as low as 1150 C. (4) Grain deformation and subsequent recrystallization and grain refinement result from hot isostatic pressing of Si3N4.

Sikora, P. F.↗

NASA NTRS1985

Capsulation of moldings made from silicon ceramic material

Ceramic articles are potted for hot isostatic pressing by porous glass and/or ceramic coating which is sintered to a pressure-tight coating in vacuo. Thus, a powdered SiO2 glass mixture with saturated alcohol sterin is sprayed on a SI3N4 ceramic, dried, introduced into the press which is evacuated to less than 0.013 mbar and heated to approximately 1200 C to drive off the organic binder and leave a powdered glass coating on the ceramic. The coating is sintered by heating to approximately 1200 C for 0.5 to 2 hours and forms a tight gass-impermeable layer. The press is heated to approximately 1700 C at 1000-300 bar and isostatic pressing is performed in the conventional manner.

Rossmann, A.↗

NASA NTRS1986

Improved consolidation of silicon carbide

Alpha silicon carbide powder was consolidated by both dry and wet methods. Dry pressing in a double acting steel die yielded sintered test bars with an average flexural strength of 235.6 MPa with a critical flaw size of approximately 100 micro m. An aqueous slurry pressing technique produced sintered test bars with an average flexural strength of 440.8 MPa with a critical flaw size of approximately 25 micro m. Image analysis revealed a reduction in both pore area and pore size distribution in the slurry pressed sintered test bars. The improvements in the slurry pressed material properties are discussed in terms of reduced agglomeration and improved particle packing during consolidation.

Freedman, M. R.↗

NASA NTRS1986

At least some errors are randomly generated (Freud was wrong)

An experiment was carried out to expose something about human error generating mechanisms. In the context of the experiment, an error was made when a subject pressed the wrong key on a computer keyboard or pressed no key at all in the time allotted. These might be considered, respectively, errors of substitution and errors of omission. Each of seven subjects saw a sequence of three digital numbers, made an easily learned binary judgement about each, and was to press the appropriate one of two keys. Each session consisted of 1,000 presentations of randomly permuted, fixed numbers broken into 10 blocks of 100. One of two keys should have been pressed within one second of the onset of each stimulus. These data were subjected to statistical analyses in order to probe the nature of the error generating mechanisms. Goodness of fit tests for a Poisson distribution for the number of errors per 50 trial interval and for an exponential distribution of the length of the intervals between errors were carried out. There is evidence for an endogenous mechanism that may best be described as a random error generator. Furthermore, an item analysis of the number of errors produced per stimulus suggests the existence of a second mechanism operating on task driven factors producing exogenous errors. Some errors, at least, are the result of constant probability generating mechanisms with error rate idiosyncratically determined for each subject.

Sellen, A. J.↗

NASA NTRS1986

Improved consolidation of silicon carbide

Freedman, M. R.↗