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At least 811 records · Page 45

High temperature sensor/microphone development for active noise control

The industrial and scientific communities have shown genuine interest in electronic systems which can operate at high temperatures, among which are sensors to monitor noise, vibration, and acoustic emissions. Acoustic sensing can be accomplished by a wide variety of commercially available devices, including: simple piezoelectric sensors, accelerometers, strain gauges, proximity sensors, and fiber optics. Of the several sensing mechanisms investigated, piezoelectrics were found to be the most prevalent, because of their simplicity of design and application and, because of their high sensitivity over broad ranges of frequencies and temperature. Numerous piezoelectric materials are used in acoustic sensors today; but maximum use temperatures are imposed by their transition temperatures (T(sub c)) and by their resistivity. Lithium niobate, in single crystal form, has the highest operating temperature of any commercially available material, 650 C; but that is not high enough for future requirements. Only two piezoelectric materials show potential for use at 1000 C; AlN thin film reported to be piezoactive at 1150 C, and perovskite layer structure (PLS) materials, which possess among the highest T(sub c) (greater than 1500 C) reported for ferroelectrics. A ceramic PLS composition was chosen. The solid solution composition, 80% strontium niobate (SN) and 20% strontium tantalate (STa), with a T(sub c) approximately 1160 C, was hot forged, a process which concurrently sinters and renders the plate-like grains into a highly oriented configuration to enhance piezo properties. Poled samples of this composition showed coupling (k33) approximately 6 and piezoelectric strain constant (d33) approximately 3. Piezoactivity was seen at 1125 C, the highest temperature measurement reported for a ferroelectric ceramic. The high temperature piezoelectric responses of this, and similar PLS materials, opens the possibility of their use in electronic devices operating at temperatures up to 1000 C. Concurrent with the materials study was an effort to define issues involved in the development of a microphone capable of operation at temperatures up to 1000 C; important since microphones capable of operation above 260 C are not generally available. The distinguishing feature of a microphone is its diaphragm which receives sound from the atmosphere: whereas, most other acoustic sensors receive sound through the solid structure on which they are installed. In order to gain an understanding of the potential problems involved in designing and testing a high temperature microphone, a prototype was constructed using a commercially available lithium niobate piezoelectric element in a stainless steel structure. The prototype showed excellent frequency response at room temperature, and responded to acoustic stimulation at 670 C, above which temperature the voltage output rapidly diminished because of decreased resistivity in the element. Samples of the PLS material were also evaluated in a simulated microphone configuration, but their voltage output was found to be a few mV compared to the 10 output of the prototype.

Shrout, Thomas R.↗

Modules of rupture and oxidation resistance of S12.55Al0.6O0.72N3.52 sialon

A Sialon of formula Si2.55Al0.6O0.72N3.52 was made from ball-milled alpha-Si3N4, AIN, and SiO2 by sintering the powder compacts at 1760 C for 4 hours in stagnant nitrogen. This Sialon had an average modulus of rupture ranging from 404 megapascals (58.6 ksi) at room temperature to 254 megapascals (36.8 ksi) at 1400 C. Oxidation tests at 1400 C in air showed it to have a parabolic oxidation rate constant less than or equal to 2.8x10 to the -10th power sq g/cm4 hr, which is smaller than that of any other Si3N4-base ceramic reported in the literature.

Arias, A.↗

Bend strengths of reaction bonded silicon nitride prepared from dry attrition milled silicon powder

Dry attrition milled silicon powder was compacted, sintered in helium, and reaction bonded in nitrogen-4 volume percent hydrogen. Bend strengths of bars with as-nitrided surfaces averaged as high as 210 MPa at room temperature and 220 MPa at 1400 C. Bars prepared from the milled powder were stronger than those prepared from as-received powder at both room temperature and at 1400 C. Room temperature strength decreased with increased milling time and 1400 C strength increased with increased milling time.

Herbell, T. P.↗

Crystallization of the glassy grain boundary phase in silicon nitride ceramics

The role was studied of the intergranular glassy phase in silicon nitride as-processed with yttria as a sintering aid. The microstructure, crystallization, and viscosity of the glassy phase were areas studied. Crystallization of the intergranular glassy phase to more refractory crystalline phases should improve the high temperature mechanical properties of the silicon nitride. The addition of a nucleating agent will increase the rate of crystallization. The measurement of the viscosity of the glassy phase will permit the estimation of the high temperature deformation of the silicon nitride.

Drummond, Charles H., III↗

Lubricating Properties of Ceramic-Bonded Calcium Fluoride Coatings on Nickel-Base Alloys from 75 to 1900 deg F

The endurance life and the friction coefficient of ceramic-bonded calcium fluoride (CaF2) coatings on nickel-base alloys were determined at temperatures from 75 F to 1900 F. The specimen configuration consisted of a hemispherical rider (3/16-in. rad.) sliding against the flat surface of a rotating disk. Increasing the ambient temperature (up to 1500 F) or the sliding velocity generally reduced the friction coefficient and improved coating life. Base-metal selection was critical above 1500 F. For instance, cast Inconel sliding against coated Inconel X was lubricated effectively to 1500 F, but at 1600 F severe blistering of the coatings occurred. However, good lubrication and adherence were obtained for Rene 41 sliding against coated Rene 41 at temperatures up to 1900 F; no blisters developed, coating wear life was fairly good, and the rider wear rate was significantly lower than for the unlubricated metals. Friction coefficients were 0.12 at 1500 F, 0.15 at 1700 F, and 0.17 at 1800 F and 1900 F. Because of its ready availability, Inconel X appears to be the preferred substrate alloy for applications in which the temperature does not exceed 1500 F. Rene 41 would have to be used in applications involving higher temperatures. Improved coating life was derived by either preoxidizing the substrate metals prior to the coating application or by applying a very thin (less than 0.0002 in.) burnished and sintered overlay to the surface of the coating. Preoxidation did not affect the friction coefficient. The overlay generally resulted in a higher friction coefficient than that obtained without the overlay. The combination of both modifications resulted in longer coating life and in friction coefficients intermediate between those obtained with either modification alone.

Sliney, Harold E.↗

Microstructure development of novel composite heating elements for steel decarbonization

The iron and steel industry is critical for the modern world but is also responsible for 7% of the total energy sector CO2 emissions. It is a difficult industry to decarbonize due to the high temperature heat required for the production of steel, such as reheating steel slabs to ~1250 °C for hot rolling. Electrification of this process using resistive heating is currently not possible due to the poor creep resistance of MoSi2 heating elements, which need to be operated well below their maximum temperatures when mounted horizontally. To solve this problem, novel MoSi2 composite heating elements with SiBCN ceramic reinforcements are being developed using high energy ball milling and electric field assisted sintering (EFAS). The microstructure and density of the composites after sintering depends on the sintering parameters chosen. Herein we present the effects of EFAS sintering parameters on the microstructure and density of the MoSi2-SiBCN composites.

36 - MATERIALS SCIENCE↗

Boride-based Ceramic Super-high Temperature Thermocouples in Harsh Environments (Final Scientific/Technical Report)

An electromotive force (emf) can be generated along a temperature gradient between the cold end and hot end of a thermoelectric material, termed the Seebeck effect. Based on the Seebeck effect, metallic alloys have been extensively employed to detect temperatures for centuries, named thermocouples. However, commercially available thermocouple alloys suffer from limitations, such as oxidation, chemical degradation, and poor long-term stability under high-temperature harsh environments. This DOE-funded project aimed to develop high-temperature, chemically tolerant thermocouples suitable for operation in extreme environments relevant to semiconducting thermoelectric materials. The research focused on boride-based semiconducting thermoelectric compounds as candidates for next-generation thermocouples with enhanced oxidation resistance, chemical stability, and thermal robustness under conditions representative of charcoal-fired electricity facilities. During the funded years, boride materials were synthesized using an arc-plasma technique under ambient air and argon atmospheres, enabling scalable and cost-effective production compared with conventional boride fabrication methods. The synthesized borides were processed into nanostructured powders, followed by consolidation into dense bulk materials using a spark plasma sintering (SPS) bottom-up approach. Comprehensive characterization was performed, including microstructural analysis, electrical transport measurements, and optical and thermal property evaluation. Both p-type and n-type boride electric legs were fabricated and integrated into boride-based thermocouples. The thermal and irradiation stabilities of the boride nanomaterials and bulk thermoelectric materials were systematically evaluated to assess suitability for long-term operation in harsh environments. Additionally, 12 students were broadly hands-on trained spanning the full research workflow, including word processing and technical editing (e.g., LATEX for manuscript and poster preparation), data collection and analysis (using Python and related libraries and hardware interfaces), sample preparation (including arc-plasma synthesis and spark plasma sintering), and advanced characterization techniques (such as X-ray diffraction, UV–vis spectroscopy, electron microscopy, differential thermal analysis (DTA), and Seebeck coefficient measurements, etc). Overall, this project demonstrated the feasibility of boride-based thermoelectric materials as durable high-temperature thermocouples, providing a promising pathway toward robust temperature sensing technologies aligned with DOE energy infrastructure and extreme-environment monitoring needs.

20 FOSSIL-FUELED POWER PLANTS↗

A sinter-free future for solid-state battery designs

The newly developed sequential decomposition synthesis (SDS) method permits the fabrication of ceramic solid electrolytes with thickness close to today's polymer separators and offers opportunities to obtain the desired phase at reduced temperatures.

25 ENERGY STORAGE↗

Modulation of dielectric properties of hexagonal/cubic boron nitride composites

In this work, we synthesized mixed-phase hexagonal-boron nitride (h-BN)/cubic-BN (c-BN) composites with varying ratios and investigated their frequency and temperature-dependent dielectric properties. As the ratio of c-BN increased, we observed a corresponding increase in the dielectric constant of the composites. Furthermore, we used spark-plasma sintering (SPS) to treat the mixed-phase composite, which resulted in a phase transformation from mixed phase to pure h-BN phase. Remarkably, the composite exhibited an increase in dielectric constant after the SPS process, which can be attributed to the densification of the composite and the enhancement in grain size. Our approach presents a promising strategy for effectively modulating the dielectric properties of BN, which is crucial for advanced electronics.

Physics↗

Decoding Early Candidacy of High Entropy Alloys for Nuclear Application using the Advanced Test Reactor through Predictive Methods and Combinatorial Testing

High Entropy Alloys (HEAs) are identified candidates for nuclear applications owing to their superb mechanical and thermal properties. In line with evaluating their candidacy, a challenge remains in their validity as structural replacements for extreme environments. Each compositional graded specimen consists up to four different compositions spanning the fueled zone for non-prototypical neutron irradiation testing in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL). We have fabricated a set of four compositionally graded specimens using spark plasma sintering that include at least five of the following elements: Cr, C, Al, Zr, Mo, Nb, Ta, V, Ti, W, and Fe. In time for this meeting the role of temperature expected to play a role in-pile cladding chemical interactions (FCCI), mechanical interactions (FCMI), irradiation damage, creep, and resistance will be reported. The irradiated portion has a scheduled irradiation date in April 2020 and with post irradiation examination (PIE) to follow.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Reliability of two sintered silicon nitride materials

Two types of sintered silicon nitride were evaluated in terms of reliability: an experimental high pressure nitrogen sintered material and a commercial material. The results show wide variations in strength for both materials. The Weibull moduli were 5.5, 8.9, and 11 for the experimental material at room temperature, 1200, and 1370 C, respectively. The commercial material showed Weibull moduli of 9.0, 8.6, and 8.9 at these respective temperatures. No correlation between strength and flaw size was noted for the experimental material. The applicability of the Weibull and Griffith theories to processing defects on the order of 100 microns or less in size are discussed.

Mieskowski, D. M.↗

High-Performance Ambient-Temperature Heat Pipe

Heat pipe with two channels designed for regulation of temperature in enclosed spaces. Made of aluminum, heat-transfer material is ammonia. Contains two channels: one for vapor phase and one for liquid phase of ammonia. Porous wick of sintered aluminum powder lines vapor channel and fills slot between two channels. Design confers several advantages.

Keddy, Michael D.↗

Coarsening in Solid-Liquid Mixtures Studied on the Space Shuttle

Ostwald ripening, or coarsening, is a process in which large particles in a two-phase mixture grow at the expense of small particles. It is a ubiquitous natural phenomena occurring in the late stages of virtually all phase separation processes. In addition, a large number of commercially important alloys undergo coarsening because they are composed of particles embedded in a matrix. Many of them, such as high-temperature superalloys used for turbine blade materials and low-temperature aluminum alloys, coarsen in the solid state. In addition, many alloys, such as the tungsten-heavy metal systems, coarsen in the solid-liquid state during liquid phase sintering. Numerous theories have been proposed that predict the rate at which the coarsening process occurs and the shape of the particle size distribution. Unfortunately, these theories have never been tested using a system that satisfies all the assumptions of the theory. In an effort to test these theories, NASA studied the coarsening process in a solid-liquid mixture composed of solid tin particles in a liquid lead-tin matrix. On Earth, the solid tin particles float to the surface of the sample, like ice in water. In contrast, in a microgravity environment this does not occur. The microstructures in the ground- and space-processed samples (see the photos) show clearly the effects of gravity on the coarsening process. The STS-83-processed sample (right image) shows nearly spherical uniformly dispersed solid tin particles. In contrast, the identically processed, ground-based sample (left image) shows significant density-driven, nonspherical particles, and because of the higher effective solid volume fraction, a larger particle size after the same coarsening time. The "Coarsening in Solid-Liquid Mixtures" (CSLM) experiment was conducted in the Middeck Glovebox facility (MGBX) flown aboard the shuttle in the Microgravity Science Laboratory (MSL-1/1R) on STS-83/94. The primary objective of CSLM is to measure the temporal evolution of the solid particles during coarsening.

Caruso, John J.↗

Experimental Characterization of Additively Manufactured Nickel-Titanium Shape Memory Alloy Heat Pipes

Shape memory alloys (SMA) have been identified for use in spacecraft components as replacement for conventional deployment mechanisms. They may be used in thermal management components such as radiators to create self-deploying radiators. One SMA, NiTi, has also been developed for additive manufacturing processes. Heat pipes are a common way to create highly effective and lightweight spaceflight radiators, and heat pipes can also be made from NiTi and related alloys. The wick is the critical element of a functioning heat pipe, and recent progress over the past years has led to the development of additively manufactured heat pipe wicks in various materials. The combination of these efforts is the focus of this project: creating an additively manufactured, shape memory alloy self-deploying heat pipe radiator. This paper will focus on the experimental characterization of these additively manufactured NiTi heat pipes. The heat pipe coupons were additively manufactured by direct metal laser sintering (DMLS), with an integral liquid cooled condenser. Heat is input to the heat pipe via a thin film heater. Thermocouples were spot welded to the heat pipes to measure temperature at several axial locations. The heat pipes were tested with two working fluids: water and ethanol. Ethanol is not an ideal working fluid for heat pipes but is useful in characterizing them because it wets well to a wide variety of surfaces. Water is in general a superior working fluid for heat pipes, but its contact angle and therefore wicking performance strongly depends on the surface chemistry of the surface it is in contact with. A particular measurement of interest in this test is the evaporator to condenser thermal conductance, which will be compared in the full paper to recently published correlations for additively manufactured heat pipes. Experimental results for two straight geometry and one bellows geometry heat pipe will be presented. The bellows geometry is of interest for condenser of the self-deploying radiator design.

Additive manufacturing↗

Fast and Scalable Synthesis of LiNi 0.5 Mn 1.5 O 4 Cathode by Sol–Gel-Assisted Microwave Sintering

High-voltage spinel LiNi 0.5 Mn 1.5 O 4 (LNMO) is a promising cathode material for high-energy-density and high-power-density lithium-ion batteries (LIBs). The high cost of the currently available LIBs needs to be addressed urgently for wide application in the transport sector (electric vehicles, buses) and large-scale energy storage systems (ESS). Of significance, herein, novel fast and scalable microwave-assisted synthesis of LNMO is reported, which leads to a production cost cut. X-ray diffraction (XRD) analysis confirms the formation of the desired phase with high crystallinity. Field emission scanning (FE-SEM) and transmission electron microscopy (TEM) analyses indicate that the synthesized phase is of nanometric size (50–150 nm) due to an extremely short sintering time (20 min). The material synthesized at 750 °C shows a higher initial discharge capacity (130 mA h g -1 ) than that synthesized at 650 °C (115 mA h g -1 ). The materials heat treated at higher temperatures show better electrochemical performance in terms of initial capacity, rate capability, and improved cycling. The improved electrochemical performance of LNMO at 750 °C is attributed to the formation of a stable crystal structure, low charge transfer resistance at the electrode/electrolyte interface, high electrical conductivity due to the presence of a disorder structure, and improved ionic diffusivity.

25 ENERGY STORAGE↗

Cast Aluminum Alloys for High Temperature Applications Using Nanoparticles Al2O3 and Al3-X Compounds (X = Ti, V, Zr)

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.

Lee, Jonathan A.↗

Inkless, dry printing nanographene via in-Situ Coordinated laser ablation and sintering processes

Printing carbon, such as graphene and other carbon structures, for flexible and printed electronics currently relies on either ink-based printing, laser-induced forward transfer (LIFT), or laser-induced graphitization (LIG) to convert carbon-rich precursor materials, such as polymers, to graphene-like carbon structures. Liquid inks contain toxic solvents, surfactants, and stabilizing additives that degrade electrical conductivity and require high-temperature post-processing. On the other hand, LIG is limited by the substrate. Here, this study introduces an additive manufacturing method for dry-printing carbon nanomaterials, ranging from amorphous carbon to crystalline graphene-like structures, on various substrates. The system utilizes laser ablation of a solid graphite target to create pure carbon nanoparticles in situ and on demand. An inert gas carries the nanoparticles onto the substrate, where they can be deposited either as amorphous structures or laser-sintered in real time to form various graphitic structures. The study of laser processing parameters, specifically fluence and pulse repetition frequency, revealed three unique regimes of nanostructure evolution that influence the morphological and electrical properties of these printed structures. Raman spectroscopy confirmed graphitization with a resistivity slightly higher than that of the bulk graphite target. The conductivity/resistivity could be tuned as a function of sintering laser power. Scanning transmission electron microscopy (STEM) revealed that turbostratic nanographene formed with an interlayer spacing of 0.40 nm. Despite ink-based printing methods, such as screen printing, inkjet printing (IJP), and aerosol jet printing (AJP), this eco-friendly and green manufacturing technique could eliminate toxic chemicals, reduce environmental impact, and enable single-step fabrication of carbon-based devices for applications in wearable sensors, energy storage, flexible electronics, and Internet of Things (IoT) devices.

Additive nanomanufacturing↗

Effect of Sintering on Mechanical and Physical Properties of Plasma-Sprayed Thermal Barrier Coatings

The effect of sintering on mechanical and physical properties of free-standing plasma-sprayed ZrO2-8 wt% Y2O3 thermal barrier coatings (TBCs) was determined by annealing them at 1316 C in air. Mechanical and physical properties of the TBCs, including strength, modes I and II fracture toughness, elastic modulus, Poisson s response, density, microhardness, fractography, and phase stability, were determined at ambient temperature as a function of annealing time ranging from 0 to 500 h. All mechanical and physical properties, except for the amount of monoclinic phase, increased significantly in 5 to 100 h and then reached a plateau above 100 h. Annealing resulted in healing of microcracks and pores and in grain growth, accompanying densification of the TBC s body due to the sintering effect. However, an inevitable adverse effect also occurred such that the desired lower thermal conductivity and good expansivity, which makes the TBCs unique in thermal barrier applications, were degraded upon annealing. A model was proposed to assess and quantify all the property variables in response to annealing in a normalized scheme. Directionality of as-sprayed TBCs appeared to have an insignificant effect on their properties, as determined via fracture toughness, microhardness, and elastic modulus measurements.

Choi, Sung R.↗