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A method of hot hydrostatic pressing of ceramics is described. A detailed description of the invention is given. The invention is explained through an example, and a figure illustrates the temperature and pressure during the hot hydrostatic pressing treatment.
A program was conducted to optimize the composition of NASA IIb-11, an alloy originally developed as a wrought material, for thermal stability and to determine the feasibility for producing the alloy using powder metallurgy techniques. Seven compositions were melted and atomized, hot isostatically pressed, cross rolled to disks and heat treated. Tensile and stress rupture properties from room temperature to 870 C (1600 F) were determined in addition to thermal stability characteristics. Processing variables included hot isostatic pressing parameters and handling, cross rolling procedures and heat treatment cycles. NASA IIb-11E displayed the best combination of overall properties for service as a 760 C (1400 F) disk material. Its composition is 0.06 C, 8.5 Cr, 9.0 Co, 2.0 Mo, 7.1 W, 6.6 Ta, 4.5 Al, 0.75 Ti, 0.5 V, 0.7 Hf, 0.01 B, 0.05 Zr and balance Ni. While the alloy exhibits the highest 760 C (1400 F) rupture strength reported for any powder metallurgy disk alloy to date, additional studies to further evaluate the effects of heat treatment may be required. The alloy is not susceptible to topologically close-packed phase formation during thermal exposure at 870 C (1600 F) for 1,500 hours, but its mechanical property levels are lowered due to grain boundary carbide formation.
A single step is relied on in the canning process for hot isostatic pressing (HIP) metallurgy composites. The composites are made from arc sprayed and plasma sprayed monotape. The HIP can is of compatible refractory metal and is sealed at high vacuum and temperature. This eliminates outgassing during hot isostatic pressing.
60-NITINOL (60 wt.% Ni - 40 wt.% Ti) is being studied as a material for advanced aerospace components. Frequent wire breakage during electrical-discharge machining of this material was investigated. The studied material was fabricated from hot isostatically pressed 60-NITINOL powder obtained through a commercial source. Bulk chemical analysis of the material showed that the composition was nominal but had relatively high levels of certain impurities, including Al and O. It was later determined that Al2O3 particles had contaminated the material during the hot isostatic pressing procedure and that these particles were the most likely cause of the wire breakage. The results of this investigation highlight the importance of material cleanliness to its further implementation.
High density ceramic sinters are manufactured by coating premolded or presintered porous ceramics with a sealing material of high SiO2 porous glass or nitride glass and then sintering by hot isostatic pressing. The ceramics have excellent abrasion and corrosion resistances. Thus LC-10 (Si3N2 powder) and Y2O3-Al2O3 type sintering were mixed and molded to give a premolded porous ceramic (porosity 37%, relative bulk density 63%). The ceramic was dipped in a slurry containing high SiO2 porous glass and an alcohol solution of cellulose acetate and dried. The coated ceramic was treated in a nitrogen atmosphere and then sintered by hot isostatic pressing to give a dense ceramic sinter.
The objective of this program was to evaluate the influence of high thermal gradient casting, hot isostatic pressing (HIP) and alternate heat treatments on the microstructure and mechanical properties of a single crystal nickel base superalloy. The alloy chosen for the study was PWA 1480, a well characterized, commercial alloy which had previously been chosen as a candidate for the Space Shuttle Main Engine high pressure turbopump turbine blades. Microstructural characterization evaluated the influence of casting thermal gradient on dendrite arm spacing, casting porosity distribution and alloy homogeneity. Hot isostatic pressing was evaluated as a means of eliminating porosity as a preferred fatigue crack initiation site. The alternate heat treatment was chosen to improve hydrogen environment embrittlement resistance and for potential fatigue life improvement. Mechanical property evaluation was aimed primarily at determining improvements in low cycle and high cycle fatigue life due to the advanced processing methods. Statistically significant numbers of tests were conducted to quantitatively demonstrate life differences. High thermal gradient casting improves as-cast homogeneity, which facilitates solution heat treatment of PWA 1480 and provides a decrease in internal pore size, leading to increases in low cycle and high cycle fatigue lives.
The thermal history developed in laser powder bed fusion (LPBF) processes has been shown to be complex resulting in equally complex microstructures and mechanical properties. Microscopic observations and Vickers micro-hardness mapping measurements were carried out on diff ;erent section planes of LPBF alloy 718 cuboids. Three-dimensional finite element analysis was used to simulate thermal history and to predict the residual stress distribution in the as-built material. Computational thermodynamics was used to predict the micro-segregation and nucleation driving force of various phases in the bulk and in segregated regions. Varied heat-treatments such as simulated hot isostatic pressing, and double aging were applied. Their influence on the microstructure, microsegregation, precipitate formation, and micro-hardness variations of LPBF alloy 718 were investigated. Hardness map results showed heterogeneous micro-hardness on the xy- and xz-planes of the as-built parts where the bottom plane and center regions had larger hardness of ~315 HV 0.5 while the top plane and contours showed hardness of ~300 HV 0.5 . It was found that the aging treatment increased the overall hardness of the as-built condition from ~310 HV 0.5 to 470 HV 0.5 but also increased the hardness gradient throughout the coupon. After simulated hot isostatic pressing process (i.e., without applied pressure) at 1020 °C for 4 h followed by water quench (HIPWQ), the hardness gradient and hardness was minimized (~210 HV 0.5 ) as the microstructure transitioned from heterogeneous columnar grains in the as-built condition to more uniform recrystallized grains. A double aging treatment was applied to enhance hardness from ~210 HV 0.5 to ~440 HV 0.5 . Finally, HIPWQ followed by double aging produced a homogeneous microstructure and more uniform hardness map with enhanced mechanical properties in LPBF alloy 718 coupons.
Several alpha-SiC materials were processed by hot isostatic pressing (HIPing) and by sintering an alpha-SiC powder containing boron and carbon. Several beta-SiC materials were processed by HIPing a beta-SiC powder with boron and carbon additions. The fracture toughnesses K(sub 1c) of these beta- and alpha-SiC materials were estimated from measurements of Vickers indentations. The three formulas used to estimate K(sub 1c) from the indentation fracture patterns resulted in three ranges of K(sub 1c) estimates. Furthermore, each formula measured the effects of processing differently. All three estimates indicated that fine-grained HIPed alpha-SiC has a higher K(sub 1c) than coarsed-grained sintered alpha-SiC. Hot isostatically pressed beta-SiC, which had an ultrafine grain structure, exhibited a K(sub 1c) comparable to that of HIPed alpha-SiC.
Abstract FeCrAl alloys are a leading candidate material for accident tolerant fuel cladding due to their good performance in both normal light-water reactor operating conditions as well as their resilience to high-temperature accident scenarios. For commercial-scale production, new fabrication techniques need to be investigated. In this study, the effects of fabrication methods on the high-temperature steam oxidation performance of C26M (Fe12Cr6Al2Mo in wt.%) were investigated. Three variants of C26M were manufactured: wrought (cast and forged) (WC26M), powder metallurgy hot isostatic pressing (PMC26M), and laser powder bed fusion additive manufacturing (AMC26M). All three variants were exposed to steam at 1200°C for 2 h. Results showed no significant variation in mass change between the variants after steam exposure. All three variants effectively formed stable protective alumina films with ~0.6–1.3 µ m thickness. This study suggests FeCrAl alloys have excellent resilience to high-temperature steam in nuclear reactor accident scenarios regardless of the fabrication method.
High thermal gradient casting of PWA 1480 was evaluated as an avenue for reducing the size of casting porosity. Hot isostatic pressing (HIP) was also employed for the elimination of casting pores. An alternate to the standard PWA 1480 coating plus diffusion bonding aging heat treatment cycle was also evaluated for potential improvements in the properties of interest to the Space Shuttle Main Engine (SSME) application. Microstructural changes associated with the high thermal gradient casting process were quantified by measurement of the size and density of the casting porosity, the amount of retained casting eutectic, and dendrite arm spacings. The results of the advanced processing have shown an improvement in material microstructure due to high thermal gradient casting. Improved homogeneity of PWA 1480 is advantageous in providing an improved solution heat treatment window and, potentially, easier HIP. High thermal gradient casting improves fatigue life by reducing casting pore size. The alternate heat treatment improves the balance of strength and ductility which appears to improve low cycle fatigue life, but with a reduction in short time stress rupture life. Based upon these tests, hot isostatic pressing appears to afford further improvements in cyclic life, though additional evaluation is suggested. Development of the alternate heat treatment is not recommended due to the reduced stress rupture capability and the need to develop a new properties data base. High thermal gradient casting and HIP are recommended for application to single crystal castings.
The Materials and Processing Laboratory at NASA Marshall Space Flight Center is developing Powder Metallurgy (PM) processing techniques for high temperature cermet and carbide material consolidation. These new group of materials would be utilized in the nuclear core for Nuclear Thermal Rockets (NTR). Cermet materials offer several advantages for NTR such as retention of fission products and fuels, better thermal shock resistance, hydrogen compatibility, high thermal conductivity, and high strength. Carbide materials offer the highest operating temperatures but are sensitive to thermal stresses and are difficult to process. To support the effort, a new facility has been setup to process refractory metal, ceramic, carbides and depleted uranium-based powders. The facility inciudes inert atmosphere glove boxes for the handling of reactive powders, a high temperature furnace, and powder processing equipment used for blending, milling, and sieving. The effort is focused on basic research to identify the most promising compositions and processing techniques. Several PM processing methods including Cold and Hot Isostatic Pressing are being evaluated to fabricate samples for characterization and hot hydrogen testing.
NiTi alloys are emerging as an attractive bearing race material for bearings exposed to high static loads and highly corrosive environments. One obstacle yet to be overcome is the intrinsically high relative cost of these materials compared to traditional bearing steels. Traditional net-shape powder metallurgy methods, such as cold-press and sinter, are not applicable to NiTi alloys because they require hot isostatic pressing (HIP) to achieve full density, flaw free microstructures. Recently, innovative powder metallurgy processing has been successful in forming bearing ring blank shapes through the use of geometrically tailored HIP containers. Microstructural evaluations show that ring blanks made from this process are comparable to material made using conventional HIP containers while substantially reducing material usage.
NiAl-AlN + Cr composites were produced by blending cryomilled NiAl powder with approx. 10 vol % Cr flakes. In comparison to the as-consolidated matrices, hot isostatically pressed Cr-modified materials did not demonstrate any significant improvement in toughness. Hot extruded NiAl-AlN+10.5Cr, however, possessed a toughness twice that determine for the base NiAl-AlN alloy. Measurement of the 1200 to 1400 K plastic flow properties revealed that the strength of the composites was completely controlled by the properties of the NiAl-AlN matrices. This behavior could be successfully modeled by the Rule-of-Mixtures, where load is shed from the weak Cr to the strong matrix.
Glass-bonded sodalite composite waste forms have been developed for the immobilization of liquid radioactive wastes resulting from off-gas treatment during aqueous reprocessing of used nuclear fuel, with a particular focus on 129I. The proposed composite waste form is comprised of aluminosilicate ceramic phases containing volatile radionuclides bonded with a glassy matrix. In this work, a suite of ten candidate low-temperature glass binders (ZnO-Bi2O3-based glasses and a Na2O-B2O3-SiO2 glass) were examined. Six glasses were mixed with caustic scrubber waste simulant previously converted into a sodalite-rich material (to provide glass fractions of 10 and 20 wt.%), uniaxially pressed into pellets, and sintered at 350 °C or 550 °C for 8 h in air. Iodine retention after heat treatment was assessed by neutron activation analysis, showing retention of 67-100 % of expected iodine. The aqueous durabilities of the resulting materials were then determined, following the ASTM C1308 standard test, showing iodine releases of 1 to 23 g m-2 after 4 d. The cumulative iodine release for the best performing system (a zinc-bismuth-borate glass binder) was <1 g m-2, and its iodine retention from processing was 67 %. The iodine releases compared favorably with other waste forms. In parallel, this best-performing composition was also consolidated via hot isostatic pressing (HIP) in a stainless-steel canister at 550 °C for 2 h under 100 MPa pressure. The HIPed sample was produced at the ~20 g scale and showed improved densification and minimal reaction with the canister.
Modern engineered ceramics offer high temperature capabilities not found in even the best superalloy metals. The high temperature properties of several selected ceramics including aluminum oxide, silicon carbide, and silicon nitride are reviewed as they apply to hypersonic engine seal design. A ranking procedure is employed to objectively differentiate among four different monolithic ceramic materials considered, including: a cold-pressed and sintered aluminum oxide; a sintered alpha-phase silicon carbide; a hot-isostatically pressed silicon nitride; and a cold-pressed and sintered silicon nitride. This procedure is used to narrow the wide range of potential ceramics considered to an acceptable number for future detailed and costly analyses and tests. The materials are numerically scored according to their high temperature flexural strength; high temperature thermal conductivity; resistance to crack growth; resistance to high heating rates; fracture toughness; Weibull modulus; and finally according to their resistance to leakage flow, where materials having coefficients of thermal expansion closely matching the engine panel material resist leakage flow best. The cold-pressed and sintered material (Kyocera SN-251) ranked the highest in the overall ranking especially when implemented in engine panels made of low expansion rate materials being considered for the engine, including Incoloy and titanium alloys.
The effects of hot isostatic pressing (HIP) processing parameters on microstructure and bond strength of Al6061/Al6061 plate interfaces were systemically investigated at the micro- and nanoscale. The HIP bonding of the two aluminum plates was performed at four temperatures: 350°C, 400°C, 450°C, and 560°C. The results reveal the formation of micron scaled Mg 2 Si precipitate and uniform nano scaled Mg 2 Al 2 O 5 oxide at the interface. The formation of Mg 2 Al 2 O 5 is closely associated with the fast bulk diffusion of Mg from the Al matrix to the amorphous Al 2 O 3 /Al interface and subsequent reaction between Mg and Al 2 O 3 . Finally, the highest and lowest bond strengths were observed in samples HIP bonded at 450°C and 350°C, respectively.
The process of powder metallurgy (PM) hot isostatic pressing (HIP) works by consolidating powdered materials at relatively high temperature and pressure to form near-net-shaped components. Ideally, PM-HIP production methods can reduce component lead time and improve designs for high-temperature reactors and/or microreactors. To introduce PM-HIP into Section III, Division 5 of the American Society of Mechanical Engineers Boiler and Pressure Vessel Code, it is necessary to show adequate material properties regarding creep, high-temperature low-cycle fatigue, and creep fatigue. However, prior work has shown that the creep-fatigue cycles to failure for PM-HIP 316H stainless steel are greatly reduced compared to the conventional, wrought product. This work continued creep-fatigue analysis on a 316H stainless steel with lower oxygen and nitrogen contents and at different HIP parameters than previously analyzed. The objective was to better understand what is causing the reduced PM-HIP 316H performance so improvements can be made PM-HIP 316H creep-fatigue lifetimes.
The present work correlates the quasi-static, tensile mechanical properties of additively manufactured Ti-6Al-4V extra low interstitial (ELI, Grade 23) alloy to the phase constituents, microstructure, and fracture surface characteristics that changed with post-heat treatment of stress relief (670 °C for 5 h) and hot isostatic pressing (HIP with 100 MPa at 920 °C for 2 h under an Ar atmosphere). Ti-6Al-4V ELI alloy tensile specimens in both the horizontal (i.e., X and Y) and vertical (Z) directions were produced by the laser powder bed fusion (LPBF) technique. Higher yield strength (1141 MPa), higher tensile strength (1190 MPa), but lower elongation at fracture (6.9%), along with mechanical anisotropy were observed for as-stress-relieved (ASR) samples. However, after HIP, consistent and isotropic mechanical behaviors were observed with a slight reduction in yield strength (928 MPa) and tensile strength (1003 MPa), but with a significant improvement in elongation at fracture (16.1%). Phase constituents of acicular α' phase in ASR and lamellar α + β phases in HIP samples were observed and quantified to corroborate the reduction in strength and increase in ductility. The anisotropic variation in elongation at fracture observed for the ASR samples, particularly built in the build (Z) direction, was related to the presence of “keyhole” porosity.