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High temperature mechanical properties of polycrystalline hafnium carbide containing 13- volume-percent hafnium diboride
Production of high strength refractory compounds and microconstituents into refractory metal matrix
Singlet exciton fission has the potential to increase the efficiency of crystalline silicon solar cells beyond the conventional single junction limit. Perhaps the largest obstacle to achieving this enhancement is uncertainty about energy coupling mechanisms at the interfaces between silicon and exciton fission materials such as tetracene. Here, the previously reported silicon‐hafnium oxynitride‐tetracene structure is studied and a combination of magnetic‐field‐dependent silicon photoluminescence measurements and density functional theory calculations is used to probe the influence of the interlayer composition on the triplet transfer process across the hafnium oxynitride interlayer. It is found that hafnium oxide interlayers do not show triplet exciton sensitization of silicon, and that nitrogen content in hafnium oxynitride layers is correlated with enhanced sensitization. Calculation results reveal that defects in hafnium oxynitride interlayers with higher nitrogen content introduce states close to the band‐edge of silicon, which can mediate the triplet exciton transfer process. Some defects introduce additional deleterious mid‐gap states, which may explain observed silicon photoluminescence quenching. These results show that band‐edge states can mediate the triplet exciton transfer process, potentially through a sequential charge transfer mechanism.
A simple analytical procedure is described for accurately and precisely determining the zirconium or hafnium content of molybdenum-base alloys. The procedure is based on the reaction of the reagent Arsenazo III with zirconium or hafnium in strong hydrochloric acid solution. The colored complexes of zirconium or hafnium are formed in the presence of molybdenum. Titanium or rhenium in the alloy have no adverse effect on the zirconium or hafnium complex at the following levels in the selected aliquot: Mo, 10 mg; Re, 10 mg; Ti, 1 mg. The spectrophotometric measurement of the zirconium or hafnium complex is accomplished without prior separation with a relative standard deviation of 1.3 to 2.7 percent.
Silicon nitride and hafnium nitride coatings were deposited by reactive RF sputtering on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. Depositions were at two background pressures, 8 and 20 mtorr, and at two different fractions (f) of nitrogen in argon, 0.25 and 0.60, for hafnium nitride and at f = 0.25 for silicon nitride. The coatings and the interface between the coating and substrates were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. A Knoop microhardness of 1650 + or - 100 kg/sq mm was measured for hafnium nitride and 3900 + or - 500 kg/sq mm for silicon nitride. The friction coefficients between a 440C rider and the coatings were measured under lubricated conditions. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C.
Silicon nitride and hafnium nitride coatings were deposited by reactive RF sputtering on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. Depositions were at two background pressures, 8 and 20 mtorr, and at two different fractions (f) of nitrogen in argon, 0.25 and 0.60, for hafnium nitride and at f = 0.25 for silicon nitride. The coatings and the interface between the coating and substrates were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. A Knoop microhardness of 1650 + or 100 kg/sq mm was measured for hafnium nitride and 3900 + or 500 kg/sq mm for silicon nitride. The friction coefficients between a 440C rider and the coatings were measured under lubricated conditions. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C.
The tensile strain rate sensitivity and the stress-rupture strength of Mo-base and W-base alloy wires, 380 microns in diameter, were determined over the temperature range from 1200 K to 1600 K. Three molybdenum alloy wires; Mo + 1.1w/o hafnium carbide (MoHfC), Mo + 25w/o W + 1.1w/o hafnium carbide (MoHfC+25W) and Mo + 45w/o W + 1.1w/o hafnium carbide (MoHfC+45W), and a W + 0.4w/o hafnium carbide (WHfC) tungsten alloy wire were evaluated. The tensile strength of all wires studied was found to have a positive strain rate sensitivity. The strain rate dependency increased with increasing temperature and is associated with grain broadening of the initial fibrous structures. The hafnium carbide dispersed W-base and Mo-base alloys have superior tensile and stress-rupture properties than those without HfC. On a density compensated basis the MoHfC wires exhibit superior tensile and stress-rupture strengths to the WHfC wires up to approximately 1400 K. Addition of tungsten in the Mo-alloy wires was found to increase the long-term stress rupture strength at temperatures above 1400 K. Theoretical calculations indicate that the strength and ductility advantage of the HfC dispersed alloy wires is due to the resistance to recrystallization imparted by the dispersoid.
Biaxial stress is identified to play an important role in the polar orthorhombic phase stability in hafnium oxide-based ferroelectric thin films. However, the stress state during various stages of wake-up has not yet been quantified. In this work, the stress evolution with field cycling in hafnium zirconium oxide capacitors is evaluated. The remanent polarization of a 20 nm thick hafnium zirconium oxide thin film increases from 9.80 to 15.0 µC cm –2 following 10 6 field cycles. This increase in remanent polarization is accompanied by a decrease in relative permittivity that indicates that a phase transformation has occurred. The presence of a phase transformation is supported by nano-Fourier transform infrared spectroscopy measurements and scanning transmission electron microscopy that show an increase in ferroelectric phase content following wake-up. The stress of individual devices field cycled between pristine and 10 6 cycles is quantified using the sin 2 (ψ) technique, and the biaxial stress is observed to decrease from 4.3 ± 0.2 to 3.2 ± 0.3 GPa. The decrease in stress is attributed, in part, to a phase transformation from the antipolar Pbca phase to the ferroelectric Pca2 1 phase. This work provides new insight into the mechanisms controlling and/or accompanying polarization wake-up in hafnium oxide-based ferroelectrics.
This report documents the integral experiment evaluation and publication for IER-532 (TEX-Hf), Thermal/Epithermal eXperiments (TEX) with highly enriched uranium (HEU) fuel and hafnium (Hf), moderated and reflected by polyethylene. The design of TEX-Hf is a variation of IER-297 (TEX-HEU), with the inclusion of hafnium as a diluent material. The experiment and evaluation include seven configurations, all of which were acceptable as benchmark cases. These benchmark cases provide validation for hafnium in the thermal, intermediate, and fast neutron energy regimes by maximizing the sensitivity in k eff to the hafnium cross sections. The evaluation was reviewed and accepted by the International Criticality Safety Benchmark Evaluation Project (ICSBEP) Technical Review Group on April 17, 2024, and was submitted to the ICSBEP in August 2024 following subgroup approval.
The poster entails the known problems and updated design solutions for the hafnium absorber latching mechanism. The hafnium absorber latching mechanism is a part of the safety rod system located within ATR's core. The latching mechanism's primary function was to attach hafnium absorbers to the safety rod drive system.
Previous work has examined the evidence for a gadolinium bias within SCALE. This work extends the previous work to include benchmark models with hafnium experiments from the ICSBEP Handbook. VALID contains only one experiment with hafnium: MIX-COMP-THERM-008. Newly generated models provide an opportunity to assess the potential presence of a hafnium bias.
The abundances of zirconium and hafnium have been determined in nine stony meteorites by a new, precise neutron-activation technique. The Zr/Hf abundance ratios for the chondrites vary in a rather narrow range, consistent with previously published observations from our group. Replicate analyses of new, carefully selected clean interior samples of the Cl chondrite Orgueil yield mean zirconium and hafnium abundances of 5.2 and 0.10 ppm, respectively. These abundances are lower than we reported earlier for two Cl chondrite samples which we now suspect may have suffered contamination. The new Cl zirconium and hafnium abundances are in closer agreement with predictions based on theories of nucleosynthesis than the earlier data.
Hafnium nitride coatings were deposited by reactive RF sputtering from a hafnium target in nitrogen and argon gas mixtures. The rate of deposition, composition, electrical resistivity and complex index of refraction were investigated as a function of target substrate distance and the fraction nitrogen, (fN2) in the sputtering atmosphere. The relative composition of the coatings is independent on fN2 for values above 0.1. The electric resistivity of the hafnium nitride films changes over 8 orders of magnitude when fN2 changes from 0.10 to 0.85. The index of refraction is almost constant at 2.8(1-0.3i) up to fN2 = 0.40 then decreases to 2.1(1 - 0.01i) for higher values of fN2.
Silicon nitride and hafnium nitride coatings were deposited on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. The coatings and the interface between the coating and substrate were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. Oxide was found at all interfaces with an interface width of at least 600 A for the oxidized substrates and at least 300 A for the unoxidized substrates. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C. Coatings of both nitrides deposited at 8 mtorr were found to have increased adhesion to both oxidized and unoxidized 440C over those deposited at 20 mtorr.
An investigation was undertaken to determine the effects of the hot-pressing variables (temperature, pressure, and time) on the density and grain size of hafnium carbide disks. The purpose was to provide information necessary for the production of high-density test shapes for the determination of physical and mechanical properties. Hot-pressing of -325 mesh hafnium carbide powder was accomplished with a hydraulic press and an inductively heated graphite die assembly. The ranges investigated for each variable were as follows: temperature, 3500 to 4870 F; pressure, 1000 to 6030 pounds per square inch; and time, 5 to 60 minutes. Hafnium carbide bodies of approximately 98 percent theoretical density can be produced under the following minimal conditions: 4230 F, 3500 pounds per square inch, and 15 minutes. Further increases in temperature and time resulted only in greater grain size.
High temperature ablation resistant ceramic composites have been made. These ceramics are composites of zirconium diboride and zirconium carbide with silicon carbide, hafnium diboride and hafnium carbide with silicon carbide and ceramic composites which contain mixed diborides and/or carbides of zirconium and hafnium. along with silicon carbide.
The sintering behavior of a mixture of hafnium carbide and 10 weight percent cobalt powders is presented. Compacts were heated in a vacuum at elevates temperatures for densification and removal of the cobalt. Densities of 99 percent of theoretical for the hafnium carbide were achieved with a maximum sintering temperature of 2200' C. Retained cobalt, grain size, microhardness, and weight loss were determined.
The behavior of refractory hafnium and zirconium based materials are being investigated at NASA Ames as part of ongoing research aimed at developing superior heat resistant materials for aerospace applications. Hafnium and zirconium diboride based materials have shown high temperature capabilities in simulated reentry environments indicating that these materials may successfully operate as reusable oxidation resistant components for leading edge applications. Due to the refractory nature of these materials, processing of fine-grained uniform microstructures poses a number of challenges. To better understand the process-property-microstructure relationship, processing of these materials has been carried out with conventional hot pressing in addition to the novel approach of Spark Plasma Sintering (SPS). The two processing methods are compared and contrasted in an evaluation of the sintering behavior of high temperature diboride based materials and preliminary physical and mechanical properties are presented.