Search NASA⌕ Search

SEARCH · Search NASA

Results for “HIGH TEMPERATURE FURNACE TREATMENT”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 19 records

Cast Alumina-Forming Austenitic Stainless Steels for High Temperature Heat Treatment Furnace Rolls

Alloy developers worldwide have struggled to create creep-resistant alumina-forming, iron-based austenitic stainless steels for use as high-temperature structural alloys, but with limited success in balancing alloy cost, oxidation, and creep resistance. Here, this article describes the research and development of a novel cast alumina-forming austenitic stainless steel. This work won the prestigious Engineering Materials Achievement Award presented at IMAT 2023 in Detroit.

36 MATERIALS SCIENCE↗

Better Particle Accelerators with SRF Technology

The use of superconducting radio frequency (SRF) technology is a driving force in the development of particle accelerators. Scientists from around the globe are working together to develop the newest materials and techniques to improve the quality and efficiency of the SRF cavities that are essential for this technology.

43 PARTICLE ACCELERATORS↗

Continuous Fly-Through High-Temperature Synthesis of Nanocatalysts

Conventional thermal treatment system, such as muffle and tube furnaces, typically feature low ramping and cooling rates, which lead to steep thermal gradients during bulk material synthesis that generate inefficient, non-uniform reaction conditions and result in nanoparticle aggregation. Herein, we demonstrate a continuous fly-through material synthesis approach using a novel high-temperature reactor design based on the emerging thermal-shock technology. By facing two sheets of carbon paper with a small distance apart (1–3 mm), we are able to generate uniform, ultra-high temperatures that can reach up to 3200 K within 50 ms by simply applying a voltage of 15 V. We can control this high-temperature to enable ultrafast chemical reactions by continuously feeding raw materials through the device from one end to the other, allowing the final products to be rapidly collected. As a proof-of-concept demonstration, we synthesized Pt nanocatalysts ~4 nm in size anchored to carbon black via this fly-through high-temperature reactor at ~1400 K. Furthermore, we find these supported Pt nanoparticles feature excellent electrocatalytic activities toward methanol oxidation reaction. Compared to existing heating methods, this continuous fly-through high temperature reactor offers a new and highly efficient platform for the synthesis of nanomaterials at high temperatures.

Qiao, Yun↗

Melting and Crystallization Behavior of CaO-MgO-Al2O3-SiO2 Silicates Relevant to Turbine Engine Applications

The melting and crystallization behavior of four quaternary CaO-MgO-Al2O3-SiO2(CMAS) silicates were investigated. The CaO:SiO2 ratios of these systems were based on various terrestrial sources of ingested particles relevant to gas turbine engine operating environments. Melting behavior was characterized using differential scanning calorimetry, and high temperature intrinsic crystallization products were determined by furnace heat treatments of the glasses at 1200°C, 1300°C, and 1400°C. The silicates exhibited a wide range of melting temperatures from ~1240°C up to ~1500°C, with most of the compositions exhibiting incongruent melting behavior. High temperature crystallization products included CaSiO3,CaAl2Si2O8, Ca2MgSi2O7, and Ca(Mg,Al)Si2O6, although SiO2 was the only crystalline phase observed at 1400°C.

Jamesa L. Stokes↗

Design and performance of a new induction furnace for heat treatment of superconducting radiofrequency niobium cavities

Superconducting radio frequency (SRF) cavities made of high purity niobium (Nb) are the building blocks of many modern particle accelerators. The fabrication process includes several cycles of chemical and heat treatment at low ({approx}120 Degree-Sign C) and high ({approx}800 Degree-Sign C) temperatures. In this contribution, we describe the design and performance of an ultra-high-vacuum furnace which uses an induction heating system to heat treat SRF cavities. Cavities are heated by radiation from the Nb susceptor. By using an all-niobium hot zone, contamination of the Nb cavity by foreign elements during heat treatment is minimized and allows avoiding subsequent chemical etching. The furnace was operated up to 1400 Degree-Sign C with a maximum pressure of {approx}1 Multiplication-Sign 10{sup -5} Torr and the maximum achievable temperature is estimated to be higher than 2000 Degree-Sign C. Initial results on the performance of a single cell 1.5 GHz cavity made of ingot Nb heat treated at 1200 Degree-Sign C using this new induction furnace and without subsequent chemical etching showed a reduction of the RF losses by a factor of {approx}2 compared to cavities made of fine-grain Nb which underwent standard chemical and heat treatments.

43 PARTICLE ACCELERATORS↗

Reproducibility of High-Q SRF Cavities by High Temperature Heat Treatment

Recent work on high-temperature (> 600 °C) heat treatment of ingot Nb cavities in a customized vacuum furnace for several hours showed the possibility of achieving Q0-values of up to ~5×10 10 at 2.0 K, 1.5 GHz and accelerating gradients of ~20 MV/m. This contribution presents results on further studies of the heat treatment process to produce cavities with high Q0 values for continuous-wave accelerator application. Single-cell cavities of different Nb purity have been processed through few cycles of heat-treatments and chemical etching. Measurements of Q0 as a function of temperature at low RF field and of Q0 as a function of the RF field at or below 2.0 K have been made after each treatment. Measurements by TOF-SIMS of the impurities depth profiles were made on samples heat treated with the cavities.

Dhakal, Pashupati↗

Fermilab experience of post-annealing losses in SRF niobium cavities due to furnace contamination and the ways to its mitigation: a pathway to processing simplification and quality factor improvement

We investigate the effect of high temperature treatments followed by only high-pressure water rinse (HPR) of superconducting radio frequency (SRF) niobium cavities. The objective is to provide a cost effective alternative to the typical cavity processing sequence, by eliminating the material removal step post furnace treatment while preserving or improving the RF performance. The studies have been conducted in the temperature range 800-1000C for different conditions of the starting substrate: large grain and fine grain, electro-polished (EP) and centrifugal barrel polished (CBP) to mirror finish. An interesting effect of the grain size on the performances is found. Cavity results and samples characterization show that furnace contaminants cause poor cavity performance, and a practical solution is found to prevent surface contamination. Extraordinary values of residual resistances ~ 1 nOhm and below are then consistently achieved for the contamination-free cavities. These results lead to a more cost-effective processing and improved RF performance, and, in conjunction with CBP, open a potential pathway to acid-free processing.

43 PARTICLE ACCELERATORS↗

Vertically oriented ZrO 2 –TiO 2 –Nb 2 O 5 –Al 2 O 3 mixed nanopatterned bioceramics on Ti6Al7Nb implant assessed by laser spallation technique

Recently, reports on the fabrication of nonstructural configuration have generated scientific interest due to increased awareness of the oxide nanotubes in the biomedical implant field and other industrial approaches. In this paper, highly ordered ZrO 2 –TiO 2 –Nb 2 O 5 –Al 2 O 3 nanotube arrays were grown by physical vapor deposition (PVD) of a zirconium layer on titanium-niobium alloy implant (IMPTi67) and succeeding anodic oxidation at a constant voltage (60 V) with exposure times ranging from 30 to 300 min. To crystallize the resulting mixed oxide nanotubes, heat treatment was also applied. The nanotubes were placed in an atmospheric furnace at temperatures ranging from 450 to 800 °C for 2 h. This treatment provided a morphological evolution was strongly influenced by the anodization time, where highly aligned bamboo-shaped oxide nanotubes (161 ± 44 nm in inside diameter and ~1 μm in length) were formed after 300 min of anodization. After annealing at temperature below 500 °C, the nano-array configuration remained stable and the average inner diameter decreased to around 40 nm. The effects of anodically fabrication time on the adhesion strength of four-phase multilayered mixed oxide nanotubes on anodized Zr/IMPTi67 surfaces assed by microscratch analysis. From the results, increasing the annealing temperature further to 800 °C fully destroyed the nanotubes and consequently the tubular arrangement was converted to a coarse grain structure. It was revealed that annealing at 450 °C for 2 h was the optimum conditions for stable nanotubular array generation, where the highest adhesion strength (shifted from 2595.59 to 2640.12 mN), microhardness (372 HV) and hydrophilicity (15 ± 1°) were recorded. It is notify that the adhesion strength of highly ordered mixed nanotubes was remarkably decreased after thermal treatment at 800 °C (1817.51 mN). Through the laser spallation analysis, the intrinsic adhesion strength of the Zr/IMPTi67 interface was found to be at 63 MPa, while the first stages of failure occurred at a stress state of 35 MPa. The adhesion of the film with the tubular structure proved to have a significantly larger adhesion strength of 246 MPa for the complete failure and 203 MPa for incipient stages of spallation. Finally, the considered surface modification can be an effective step in determining the interface strength between biomedical implants and the nanostructured coatings.

36 MATERIALS SCIENCE↗

The suppression of low-temperature intergranular brittleness in ferritic Fe-Mn alloys

A method for obtaining cryogenic toughness in an Fe-12Mn-0.2Ti alloy by a controlled cooling technique is presented. The intergranular fracture surface of the quenched alloy, using an AES, revealed no significant difference from that obtained by the bulk transgranular fracture surface, indicating the absence of large-scale grain boundary segregation during the austenitizing treatment. Attention is given to the step cooling method, using a furnace at temperatures of 100 to 120 C, followed by fast cooling to ambient temperature, which in turn produces a high-impact toughness without intergranular brittleness. It is concluded that the sources of brittle intergranular fracture in the alloy are both chemical, operating in martensitic structure, and nonchemical, active during quenching from the austenitizing treatment.

Hwang, S. K.↗

The effect of fuel to nitrates ratio on the properties of FeCr{sub 2}O{sub 4} nanopowders

Highlights: • Single phase spinel FeCr{sub 2}O{sub 4} nanopowders were formed without further heat treatment based on powder X-ray diffraction, FTIR and EDS studies. • The probable combustion mechanism with thermodynamic concepts involved in the formation of FeCr{sub 2}O{sub 4} nanopowders were discussed. • The effect of different amount of fuel to metal nitrates ratio (F/N) on the self-combusted FeCr{sub 2}O{sub 4} nanopowders was investigated. • It greatly affects the morphologies, different nanocrystallite sizes, and magnetic properties by using different combinations of F/N ratios. - Abstract: The solution combustion of spinel type FeCr{sub 2}O{sub 4} nanopowders via different ratios of fuel to stating metal nitrates was investigated. The synthesized FeCr{sub 2}O{sub 4} nanopowders were deemed to be single phase spinel type material based on powder X-ray diffraction, FTIR and EDS studies. The properties of synthesized FeCr{sub 2}O{sub 4} nanopowders such as morphology, porosity, elemental composition, crystallite size, strain and lattice deformations, magnetic moment, and coercivity were influenced by the amount of the fuel used in the combustion process. FeCr{sub 2}O{sub 4} nanopowders with different morphologies, porosities, structural, and magnetic properties could be prepared in a single procedure on a hotplate magnetic stirrer without the need for high temperature furnaces.

36 MATERIALS SCIENCE↗

Fundamental R&D for high-Q0 650 MHz SRF cavities for hadron linacs

Upcoming projects requiring high-Q0 ~650 MHz elliptical cavities, such as MSU’s Facility for Rare Isotope Beams’ energy upgrade and Fermilab’s PIP-II, drive a need to better understand RF losses due to magnetic flux. With sample sets from two different Niobium vendors, we explore the efficacy of the fast-cooldown method, and high- temperature annealing in promoting flux expulsion. Additionally, we report the results of vertical tests comparing the effect of electropolishing and furnace baking treatments on the cavity flux sensitivity. We also directly measure the flux pinning force in niobium samples, and correlate it with different heat treatments, and flux expulsion performance.

K.McGee, K.McGee↗

The role of silver in self-lubricating coatings for use at extreme temperatures

The advantages and disadvantages of elemental silver as a tribological material are discussed. It is demonstrated that the relatively high melting point of 961 deg C, softness, marked plasticity, and thermochemical stability of silver combine to make this metal useful in thin film solid lubricant coatings over a wide temperature range. Disadvantages of silver during sliding, except when used as a thin film, are shown to be gross ploughing due to plastic deformation under load with associated high friction and excessive transfer to counterface surfaces. This transfer generates an irregular surface topography with consequent undesirable changes in bearing clearance distribution. Research to overcome these disadvantages of element silver is described. A comparison is made of the tribological behavior of pure silver with that of silver formulated with other metals and high-temperature solid lubricants. The composite materials are prepared by co-depositing the powdered components with an airbrush followed by furnace heat treatment or by plasma-spraying. Composite coatings were formulated which are shown to be self-lubricating over repeated, temperature cycles from low temperature to about 900 deg C.

Sliney, H. E.↗

The use of silver in self-lubricating coatings for extreme temperatures

The advantages and disadvantages of elemental silver as a tribological material are discussed. It is demonstrated that the relatively high melting point of 961 deg C, softness, marked plasticity, and thermochemical stability of silver combine to make this metal useful in thin film solid lubricant coatings over a wide temperature range. Disadvantages of silver during sliding, except when used as a thin film, are shown to be gross ploughing due to plastic deformation under load with associated high friction and excessive transfer to counterface surfaces. This transfer generates an irregular surface topography with consequent undesirable changes in bearing clearance distribution. Research to overcome these disadvantages of element silver is described. A comparison is made of the tribological behavior of pure silver with that of silver formulated with other metals and high-temperature solid lubricants. The composite materials are prepared by co-depositing the powdered components with an airbrush followed by furnace heat treatment or by plasma-spraying. Composite coatings were formulated which are shown to be self-lubricating over repeated, temperature cycles from low temperature to about 900 deg C.

Sliney, H. E.↗

Low-Temperature Plasma Treatment for Enhanced Recovery of Highly Valued Critical REEs from Coal (Final Report)

The principle objective of this project was to develop a novel process flowsheet using low-temperature plasma treatment (LTP) integrated with conventional hydrometallurgical processes to recover rare earth elements (REEs), especially highly valued REEs (i.e. scandium and critical REEs), from coal and coal byproducts. LTP treatment was used to pretreat the solid feed material prior to leaching in an effort to improve the leaching characteristics of the REEs and potentially reduce acid consumption. Initially, a detailed experimental program was performed on a laboratory LTP furnace to identify a set of process parameter values to be used for assessing the enhanced leaching performance achieved on four specific gravity fractions of West Kentucky No. 13 and Fire Clay coarse coal refuse materials. High-temperature oxidation (HTO)) was also evaluated as a means for improving REE leachability on the same fractions of both coal sources. The lixiviants used to assess leachability improvements included: i) untreated water, ii) 0.1 M ammonium sulfate solution and iii) 1.2 M sulfuric acid solution at a temperature of 75°C. The laboratory data was used to develop multiple process flow sheets using HTO only to produce a rare earth oxide mix concentrate or utilizing both LTP and HTO treatment processes to generate a high purity heavy REO mix concentrate and a light REO mix concentrate. A techno-economic analysis was performed on each circuit. Low-temperature plasma oxidation was found to enhance REE leaching characteristics for all specific gravity (SG) fractions of the West Kentucky No. 13 coarse refuse material. The leaching recovery improvement was preferentially achieved for the heavy REEs with higher values obtained when treating the lower density fraction material. For example, the leaching recovery for the heavy REEs in the untreated 1.6 SG Float fraction material was 8% in a 0.1 M ammonium sulfate solution. After LTP treatment for 32 hours, heavy REE recovery increased to 33%. The corresponding recovery value for the light REEs was 10%. These findings indicate a strong affinity of the heavy REEs with the organic material, which is the component being reduced in content during the LTP treatment. Scanning electron micrographs showed the development of a honeycomb structure with increased LTP treatment with higher surface area as confirmed from BET measurements. Higher surface area promotes improved leaching efficiency due to enhance chemical interactions. When using 1.2 M sulfuric acid, the LTP treatment was found to provide a heavy REE recovery increase from 23% to 53% for the 1.6 SG Float fraction which corresponded to an ash content increase from around 20% to 35%. However, LTP treatment provided no improvement in leaching characteristic for the 2.2 SG sink material in the acid solution, which was likely due to the low organic content. The LTP treatment of the Fire Clay SG fractions provided no improvement in REE leaching characteristic, which may be due to the association with REE minerals such as monazite and REE-associated mineral matter such as clays. High temperature oxidation using temperatures in the range of 600-750OC was found to significantly enhance the leaching characteristics of both the light and heavy REEs for all density fractions in both coarse coal refuse materials. Generally, the increase in light REE recovery for the West Kentucky material was from 15% for the untreated material to 90% for the HTO treated material at 600°C. Recovery values dropped significantly when using temperatures below 600°C and above 750°C. The impact of the excessive temperatures was most likely a result of sintering. For the heavy REEs, HTO significantly improved recovery in the lighter SG fractions, which may be due to an affinity with the organic content. Only limited heavy REE recovery improvement was obtained for the denser SG fractions. Another benefit of HTO is the conversion of calcium-based minerals to a very soluble calcium oxide, which is removable using a mild acid solution, and the conversion of Fe minerals to relatively insoluble minerals such as hematite and magnetite. The pregnant leaching solution produced from the leaching of all SG fractions obtained from both coal sources was treated using two stages of solvent extraction procedurally modeling a rougher-cleaner circuit followed by oxalic acid precipitation. Rare earth oxide products having a purity greater than 97% was produced from nearly all of the SG fractions. A novel process flowsheet was developed based on the selective leaching of heavy REEs that was made possible through LTP treatment of West Kentucky No. 13 coarse refuse followed by salt leaching. In the flowsheet, coal refuse material is ground to a top size of 1mm and then treated by LTP. The treated material is mixed into a 0.1 M ammonium sulfate solution and then filtered to produce a heavy REE enriched pregnant leach solution. The heavy REEs are concentrated by two stages of selective precipitation to produce a heavy REE mix oxalate and then roasted to obtain a heavy REO mix concentrate. The solid residues remaining after salt leaching is dried and then subjected to HTO treatment followed by concentration using selective precipitation and roasting to produce a light REO mix concentrate. An alternative circuit was developed using HTO treatment only to treat 100% of the coarse refuse material followed by selective precipitation and roasting to generate a high purity REO mix product. A techno-economic analysis performed for the treatment of West Kentucky No. 13 and Fire Clay coarse refuse based on a hypothetical 500-tph plant revealed that the net present value for all scenarios was significantly negative. Primary reasons include: i) a substantial decrease in the basket value of the final product relative to the feed and ii) high chemical costs relative to the amount of product generated. The basket value reduction was primarily due to little to no scandium recovery due to poor leaching characteristics when using low acid concentrations as necessitated by the low feed grades. Operating costs were primarily influenced by the chemical costs relative to the kilograms of concentrate produced and feed grade. For the Fire Clay coarse refuse material, the total operating cost was estimated to be $354 per kg of REO produced which was higher than the basket value of the REO product ($276/kg). Approximately 37% of the total cost was the sulfuric acid used during the leaching process. A comparative analysis performed to assess the economic viability of using low-temperature plasma furnaces found that market value enhancement for the generation of both heavy REO and light REO concentrates will be needed in addition to significant technology advancements to reduce the cost of plasma furnaces.

01 COAL, LIGNITE, AND PEAT↗

Tribological Performance of PM400 Bushings in Oscillatory Sliding from 25 to 927 °C

Small bore (6.35 millimeter) bushings, made from NASA PM400 solid lubricant composite, were evaluated in oscillatory sliding contact against a nickel-based superalloy shaft. Tests were conducted in air from 25 to 900 degrees Centigrade for extended periods (1 million cycles, plus or minus 15 degrees, 1 hertz) to assess the suitability of PM400 in gas turbine and reciprocating engine exhaust gas path control valve applications. Operating torque and estimated friction was monitored throughout the test duration and wear was measured at the end of test. In general, friction, torque and wear was low. At temperatures above 600 degrees Centigrade, bushing dimensional stability was achieved via short duration pre-test furnace exposure heat treatments. Preliminary test results show that bushings made from NASA PM400 are feasible for aerospace and industrial applications.

high temperature solid lubricants↗

Experimental Investigation of a Novel Membrane-Based Condensing Heat Exchanger for High Efficiency Furnaces

Building space heating consumes approximately one-third of all global natural gas end use. Higher-efficiency (i.e., condensing) furnaces constitute only about 30% of the annual furnace shipments in the United States because the condensing heat exchangers must use highly expensive, corrosion-resistant materials to be protected from acidic components in the furnace flue gas stream. Increasing the market share of high-efficiency furnaces will reduce greenhouse gas emissions. This study developed and tested a benchtop prototype of a novel membrane-based heat exchanger (MHX) for high-efficiency furnaces to achieve nonacidic condensation via nanoporous membranes. Test results show that both sensible and latent heat were recovered by the MHX, and the fraction of latent heat recovery ranged from about 25% to 45% over the range of operating conditions evaluated. The amount of water condensed through the MHX increased with the increase of flue gas flow rate and decreased with increasing coolant temperature. The fraction of latent heat recovery decreased with the increase of flue gas flow rate and coolant temperature. The pH value of condensed water from the MHX was only mildly acidic, varying from 5.3 to 5.6 without any additional treatment, about 2.0 to 2.3 pH points higher (i.e., less acidic) than typical values for the condensate from conventional condensing furnaces. Therefore, feasibility of the MHX was experimentally verified, and the MHX could enable wider market penetration of highly energy-efficient condensing furnaces by reducing costs associated with managing the acid condensation compared with conventional condensing furnaces, possibly enabling the use of existing vent systems when replacing noncondensing furnaces (due to higher flue gas exit temperatures), and possibly reducing furnace first costs.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Utilization of Tabula Rasa to Stabilize Bulk Lifetimes in n-Cz Silicon for High-Performance Solar Cell Processing

We investigate a high temperature, high cooling-rate anneal Tabula Rasa (TR) and report its implications on n-type Czochralski-grown silicon (n-Cz Si) for photovoltaic fabrication. Tabula Rasa aims at dissolving and homogenizing oxygen precipitate nuclei that can grow during the cell process steps and degrade the cell performance due to their high internal gettering and recombination activity. The Tabula Rasa thermal treatment is performed in a clean tube furnace with cooling rates >100 degrees C/s. We characterize the bulk lifetime by Sinton lifetime and photoluminescence mapping just after Tabula Rasa, and after the subsequent cell processing. After TR, the bulk lifetime surprisingly degrades to <; 0.1ms, only to recover to values equal or higher than the initial non-treated wafer (several ms), after typical high temperature cell process steps. Those include boron diffusion and oxidation; phosphorus diffusion/oxidation; ambient annealing at 850 degrees C; and crystallization annealing of tunneling-passivating contacts (doped polycrystalline silicon on 1.5 nm thermal oxide). The drastic lifetime improvement during high temperature cell processing is attributed to improved external gettering of metal impurities and annealing of intrinsic point defects. Time and injection dependent lifetime spectroscopy further reveals the mechanisms of lifetime improvement after Tabula Rasa treatment. Additionally, we report the efficacy of Tabula Rasa on n-type Cz-Si wafers and its dependence on oxygen concentration, correlated to position within the ingot.

14 SOLAR ENERGY↗

In Situ Apparatus to Study Gas–Metal Reactions and Wettability at High Temperatures for Hot-Dip Galvanizing Applications

The understanding of gas–metal reactions and related surface wettability at high temperatures is often limited due to the lack of in situ surface characterization. Ex situ transfers at low temperature between annealing furnace, wettability device, and analytical tools induce noticeable changes of surface composition distinct from the reality of the phenomena.Therefore, a high temperature wettability device was designed in order to allow in situ sample surface characterization by x-rays photoelectron spectroscopy after gas/metal and liquid metal/solid metal surface reactions. Such airless characterization rules out any contamination and oxidation of surfaces and reveals their real composition after heat treatment and chemical reaction. The device consists of two connected reactors, respectively, dedicated to annealing treatments and wettability measurements. Heat treatments are performed in an infrared lamp furnace in a well-controlled atmosphere conditions designed to reproduce gas–metal reactions occurring during the industrial recrystallization annealing of steels. Wetting experiments are carried out in dispensed drop configuration with the precise control of the deposited droplets kinetic energies. The spreading of drops is followed by a high-speed CCD video camera at 500-2000 frames/s in order to reach information at very low contact time. First trials have started to simulate phenomena occurring during recrystallization annealing and hot-dip galvanizing on polished pure Fe and FeAl8 wt.% samples. The results demonstrate real surface chemistry of steel samples after annealing when they are put in contact with liquid zinc alloy bath during hot-dip galvanizing. The wetting results are compared to literature data and coupled with the characterization of interfacial layers by FEG-Auger. It is fair to conclude that the results show the real interest of such in situ experimental setup for interfacial chemistry studies.

36 MATERIALS SCIENCE↗