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At least 19 records

Fractography of the high temperature hydrogen attack of a medium carbon steel

Results are reported for an experimental study of the microscopic fracture processes associated with hydrogen attack of a commercially produced plain carbon steel in a well-controlled high-temperature hydrogen environment of high purity. In the experiments, sheet samples were exposed to laboratory-grade hydrogen at a pressure of 3.5 MN/sq m and a temperature of 575 C. The fractography of gas-filled fissures and failed tension specimens is analyzed in an effort to identify any predominant microstructural defect associated with fissure formation, the prevalent modes of fracture, and the contribution of gas-filled fissures to the overall failure process. It is found that the tensile properties of the examined steel were significantly degraded after as few as 136 hr of exposure to a high-purity hydrogen atmosphere at 575 C; that the yield strength, ultimate strength, and elongation at fracture were all reduced progressively with increasing exposure time; and that the yield and ultimate strengths were reduced more than 40% after 408 hr while elongation was reduced to less than 2%.

Nelson, H. G.↗

Effect of high-temperature hydrogen exposure on sintered alpha-SiC

Sintered alpha-silicon carbide was exposed to pure, dry hydrogen at high temperatures for times up to 500 hr. Weight loss and corrosion were seen after 50 hr at temperatures as low as 1000 C. Corrosion of SiC by hydrogen produced grain boundary deterioration at 1100 C and a mixture of grain and grain boundary deterioration at 1300 C. Statistically significant strength reductions were seen in samples exposed to hydrogen for times greater than 50 hr and temperatures above 1100 C. Critical fracture origins were identified by fractography as either general grain boundary corrosion at 1100 C or as corrosion pits at 1300 C. A maximum strength decrease of approximately 33 percent was seen at 1100 and 1300 C after 500 hr exposure to hydrogen. A computer assisted thermodynamic program was also used to predict possible reaction species of SiC and hydrogen.

Hallum, Gary W.↗

Fractography of the high temperature hydrogen attack of a medium carbon steel

Microscopic fracture processes were studied which are associated with hydrogen attack of a medium carbon steel in a well-controlled, high-temperature, high-purity hydrogen environment. Exposure to a hydrogen pressure and temperature of 3.5 MN/m2 and 575 C was found to degrade room temperature tensile properties with increasing exposure time. After 408 hr, yield and ultimate strengths were reduced by more than 40 percent and elongation was reduced to less than 2 percent. Initial fissure formation was found to be associated with manganese rich particles, most probably manganese oxide, aligned in the microstructure during the rolling operation. Fissure growth was found to be associated with a reduction in carbide content of the microstructure and was inhibited by the depletion of carbon. The interior surfaces of sectioned fissures or bubbles exhibit both primary and secondary cracking by intergranular separation. The grain surfaces were rough and rounded, suggesting a diffusion-associated separation process. Specimens that failed at room temperature after exposure to hydrogen were found to exhibit mixed mode fracture having varying amounts of intergranular separation, dimple formation, and cleavage, depending on exposure time.

Melson, H. G.↗

Ab initio Screening of Refractory Nitrides and Carbides for High Temperature Hydrogen Permeation Barriers

Density functional theory was used to screen eleven refractory materials – two pure metals, six nitrides, and three carbides–as high-temperature hydrogen permeation barriers to prevent hydrogen embrittlement. Activation energies were calculated for atomic hydrogen (H) diffusion into the first subsurface layer from the lowest energy surface of the high-temperature phase of each candidate material. The candidate barrier materials with the highest activation energies are h-BN, c-BN, HfN, and ZrN with predicted barriers of 3.25 eV, 3.23 eV, 3.14 eV, and 2.76 eV, respectively. Strain energies, Bader charges, and density of states were calculated for the diffusing H at the relaxed initial state and the transition state to provide insight into contributing factors to high energy barriers. The diffusing H atom in materials with the highest predicted barriers are protic. In addition, interstitial H atoms induce mid-gap states in the density of states of both BN polymorphs. The nitrogen retention of each nitride material at high temperatures was predicted using nitrogen vacancy formation energies with respect to gaseous nitrogen. Experimental evaluation of nitrogen retention in h-BN, ZrN, and TiN confirmed their resistance to nitrogen loss at 1773 K. However, of these nitrides, TiN is predicted to be the least stable. This work identifies multiple promising materials that are predicted to be effective hydrogen barriers at high temperatures and that are stable at temperatures above 2700 K, with BN predicted to perform best.

Density Functional Theory (DFT)↗

Superalloy for high-temperature hydrogen environmental applications

A nickel-based superalloy is provided which is resistant to deterioration in hydrogen at high operating temperatures and pressures, and which thus can be used in hydrogen-fueled spacecraft such as the Space Shuttle. The superalloy is characterized by a two-phase microstructure and consists of a gamma-prime precipitated phase in a gamma matrix. The gamma matrix phase is a primary solid solution and the gamma precipitated phase will be an intermetallic compound of the type A.sub.3 B, such as nickel aluminide or titanide. Both phases are coherent, ordered, and compatible, and thus will retain most of their strength at elevated temperatures. The alloy consists essentially of (by weight): Ni 50-60%, Cr 10-20%, Al 2-6%, Co 2-5%, Ti 3-8%, W 5-12%, Mo 5-10%, Nb 1-3%, wherein the ratio W/MO is approximately equal to 1, and Ti/Al ranges from about 1 to about 2.

McKannan, Eugene C.↗

The Use of Immersion Rigs for High Temperature Hydrogen Exposure Testing Within the Nuclear Thermal Rocket Element Environmental Simulator (NTREES)

The Nuclear Thermal Rocket Element Environmental Simulator (NTREES) was designed to perform non-nuclear testing of nuclear thermal rocket (NTR) fuel elements and materials. NTREES can simulate the thermal hydraulic environment within an NTR and has been leveraged to provide critical information on component performance and material compatibility. NTREES has the ability to expose test articles to pressurized Hydrogen gas up to 1000 psig and 225 g/s. NTREES tests are operated in a deoxygenated environment of Nitrogen or Argon pressurized up to 1000 psig. NTREES simulates fission heat through induction heating powered by a 1.2 MW AC power supply, and NTREES has recorded temperatures exceeding 3700K. To perform hot Hydrogen exposure tests on materials more rapidly and earlier in the fuel development process, NTREES must be able to test small material samples on the order of 1 square inch in volume, individual fuel assembly subcomponents, and particle materials. To meet these needs, multiple testing rigs have been developed to immerse test specimens in hot Hydrogen, with each "immersion rig" varying in its capability of sample type and performance range in order to meet the broadest range of testing needs. Herein is a discussion of a selection of these “immersion rigs.”

Nuclear Thermal Propulsion↗

The Use of Immersion Rigs for High Temperature Hydrogen Exposure Testing Within the Nuclear Thermal Rocket Element Environmental Simulator (NTREES): NTREES-5 Hydrogen Heat Exchanger (N5HHX-01)

The Nuclear Thermal Rocket Element Environmental Simulator (NTREES) facility at NASA’s Marshall Space Flight Center (MSFC) subjects materials and components typically found on nuclear thermal propulsion (NTP) systems to non-nuclear simulations of prototypic NTP reactor thermohydraulic environments. With 1.2 MW of inductive power available, the currently employed methods to simulate nuclear heating in NTREES consist of 1) inductively heating a test specimen, which typically cannot be performed on ceramic materials, or 2) heating gas that envelops the test specimen. The latter of these has provided a basis for developing so-called “immersion rigs” to be used in NTREES. Furthermore, immersion rigs are especially useful in the case of smaller, technically challenging test specimens. One such device, the “NTREES-5 Hydrogen Heat Exchanger” (N5HHX-01), designed and deployed to test small material coupons to ~0.5 g/s of 2800 K, 500 psi Hydrogen, is discussed herein. To achieve this desired delivery temperature level, the most suitable material for the N5HHX’s construction was pure tungsten, which imposed budgetary and manufacturing challenges. Also discussed in this paper is the design of the N5HHX rig’s sample container, which became the first iteration of improving NTREES small material coupon test operations by permitting rapid changeout of different material samples.

Reactor Testing↗

The Use of Immersion Rigs for High Temperature Hydrogen Exposure Testing within the Nuclear Thermal Rocket Element Environmental Simulator (NTREES): Thermal Soak Rig (TSR)

The Nuclear Thermal Rocket Element Environmental Simulator (NTREES) facility was purpose constructed to perform non-nuclear evaluations of nuclear thermal propulsion (NTP) system fuel materials and structures within prototypic thermochemical environments. This system has been utilized steadily in its ability to subject test specimens to thermochemical and thermohydraulic environments simulating that of an operating nuclear rocket engine. Fission heat is simulated by induction power and experiments are conducted within a ~1000 psi pressure vessel. Hydrogen is conventionally passed through the heated fuel surrogate test specimen while pressure, temperature, and gas species data are collected at various points along the experiment. In order to test fuel and material coupon samples, a class of test apparatus named “immersion rigs” are being developed and employed to more rapidly test these smaller and more technically challenging test specimen. One example of a promising potential fuel structure, Tristructural-isotropic (TRISO) particles, presents unique challenges for testing of this type. TRISO fuel micro-particles are spheroids typically on the order of 500 – 1000 μm in diameter, and exposing a batch sample to hot hydrogen requires purpose-built special test equipment. Thusly, an immersion rig was developed and successfully demonstrated to expose ~1 g of micro-particles to hydrogen gas at temperatures and pressures relevant to NTP systems for the purpose of fuel evaluation. The rig, comprised primarily of graphite and pure tungsten, houses in its core a batch of micro-particles between pucks of porous silicon carbide (SiC). This approach permits gas flow while simultaneously retaining the particles in place. Herein is a discussion of the design, analysis, fabrication, and testing of the NTREES Thermal Soak Rig (TSR).

Space Nuclear Propulsion↗

Effect of high temperature hydrogen exposure on the strength and microstructure of mullite

The corrosion of near stoichiometric mullite (3Al2O3-2SiO2) by pure dry hydrogen gas was studied at 1050 and 1250 C for times up to 500 hr. The hydrogen preferentially attacked the grain boundaries of the mullite where an aluminosilicate glass was present. Corrosion of the mullite grains was observed after 125 hr at 1250 C. The hydrogen reaction removed SiO2 from the glassy grain boundaries and the mullite grains resulting in a porous alumina rich surface. At 1250 C the strength increased after short exposure times (at least up to 125 hr) and decreased by 53 percent after 500 hr. At 1050 C, all exposure times (25 to 500 hr) decreased the strength. At 500 hr room temperature strength of mullite exposed to 1050 C was reduced by 22 percent. The strength reduction after short exposure times at 1050 C is attributed to crystallization of the grain boundary glass phase.

Herbell, Thomas P.↗

High-temperature Hydrogen Chloride Releases from Mixtures of Sodium Chloride with Sulfates: Implications for the Chlorine-Mineralogy as Determined by the Sample Analysis at Mars Instrument on the Curiosity Rover in Gale Crater, Mars

Hydrogen chloride releases above 500 °C occurred in several samples analyzed by the Sample Analysis at Mars (SAM) evolved gas analyzer on the Curiosity rover in Gale crater. These have been attributed to reactions between chlorides (original or from oxychlorine decomposition) and water. Some of these HCl releases that peaked below the melting temperature of common chlorides did not co-evolve with oxygen or water, and were not explained by laboratory analog work (Figure 1). Therefore, these HCl releases were not caused by MgCl2 or soley due to reactions between water and melting chlorides. The goal of this work was to explain the HCl releases that did not co-evolve with oxygen or water and occurred below the melting point of common chlorides, which have not been explained by previous laboratory analog work. This work specifically evaluates the role of evolved SO2 in the production of HCl.

Clark, J.V.↗

Induction Heating Model of Cermet Fuel Element Environmental Test (CFEET)

Deep space missions with large payloads require high specific impulse and relatively high thrust to achieve mission goals in reasonable time frames. Nuclear Thermal Rockets (NTR) are capable of producing a high specific impulse by employing heat produced by a fission reactor to heat and therefore accelerate hydrogen through a rocket nozzle providing thrust. Fuel element temperatures are very high (up to 3000 K) and hydrogen is highly reactive with most materials at high temperatures. Data covering the effects of high‐temperature hydrogen exposure on fuel elements are limited. The primary concern is the mechanical failure of fuel elements due to large thermal gradients; therefore, high‐melting‐point ceramics‐metallic matrix composites (cermets) are one of the fuels under consideration as part of the Nuclear Cryogenic Propulsion Stage (NCPS) Advance Exploration System (AES) technology project at the Marshall Space Flight Center. The purpose of testing and analytical modeling is to determine their ability to survive and maintain thermal performance in a prototypical NTR reactor environment of exposure to hydrogen at very high temperatures and obtain data to assess the properties of the non‐nuclear support materials. The fission process and the resulting heating performance are well known and do not require that active fissile material to be integrated in this testing. A small‐scale test bed; Compact Fuel Element Environmental Tester (CFEET), designed to heat fuel element samples via induction heating and expose samples to hydrogen is being developed at MSFC to assist in optimal material and manufacturing process selection without utilizing fissile material. This paper details the analytical approach to help design and optimize the test bed using COMSOL Multiphysics for predicting thermal gradients induced by electromagnetic heating (Induction heating) and Thermal Desktop for radiation calculations.

Gomez, C. F.↗

Induction Heating Model of Cermet Fuel Element Environmental Test (CFEET)

Deep space missions with large payloads require high specific impulse and relatively high thrust to achieve mission goals in reasonable time frames. Nuclear Thermal Rockets (NTR) are capable of producing a high specific impulse by employing heat produced by a fission reactor to heat and therefore accelerate hydrogen through a rocket nozzle providing thrust. Fuel element temperatures are very high (up to 3000 K) and hydrogen is highly reactive with most materials at high temperatures. Data covering the effects of high‐temperature hydrogen exposure on fuel elements are limited. The primary concern is the mechanical failure of fuel elements due to large thermal gradients; therefore, high‐melting‐point ceramics‐metallic matrix composites (cermets) are one of the fuels under consideration as part of the Nuclear Cryogenic Propulsion Stage (NCPS) Advance Exploration System (AES) technology project at the Marshall Space Flight Center. The purpose of testing and analytical modeling is to determine their ability to survive and maintain thermal performance in a prototypical NTR reactor environment of exposure to hydrogen at very high temperatures and obtain data to assess the properties of the non‐nuclear support materials. The fission process and the resulting heating performance are well known and do not require that active fissile material to be integrated in this testing. A small‐scale test bed; Compact Fuel Element Environmental Tester (CFEET), designed to heat fuel element samples via induction heating and expose samples to hydrogen is being developed at MSFC to assist in optimal material and manufacturing process selection without utilizing fissile material. This paper details the analytical approach to help design and optimize the test bed using COMSOL Multiphysics for predicting thermal gradients induced by electromagnetic heating (Induction heating) and Thermal Desktop for radiation calculations.

Gomez, Carlos F.↗