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M3FT-17OR0301070211 - Preparation of Hot Isostatically Pressed AgZ Waste Form Samples

The production of radioactive iodine-bearing waste forms that exhibit long-term stability and are suitable for permanent geologic disposal has been the subject of substantial research interest. One potential method of iodine waste form production is hot isostatic pressing (HIP). Recent studies at Oak Ridge National Laboratory (ORNL) have investigated the conversion of iodine-loaded silver mordenite (I-AgZ) directly to a waste form by HIP. ORNL has performed HIP with a variety of sample compositions and pressing conditions. The base mineral has varied among AgZ (in pure and engineered forms), silver-exchanged faujasite, and silverexchanged zeolite A. Two iodine loading methods, occlusion and chemisorption, have been explored. Additionally, the effects of variations in temperature and pressure of the process have been examined, with temperature ranges of 525°C–1,100°C and pressure ranges of 100–300 MPa. All of these samples remain available to collaborators upon request. The sample preparation detailed in this document is an extension of that work. In addition to previously prepared samples, this report documents the preparation of additional samples to support stability testing. These samples include chemisorbed I-AgZ and pure AgI. Following sample preparation, each sample was processed by HIP by American Isostatic Presses Inc. and returned to ORNL for storage. ORNL will store the samples until they are requested by collaborators for durability testing. The sample set reported here will support waste form durability testing across the national laboratories and will provide insight into the effects of varied iodine content on iodine retention by the produced waste form and on potential improvements in waste form durability provided by the zeolite matrix.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Convergent Manufacturing of Large-Scale Components for Nuclear Applications, via Additive Manufacturing and Powder Metallurgy Hot Isostatic Pressing

Powder metallurgy (PM)–hot isostatic pressing (PM-HIP) has long been recognized as a powerful route for producing fully dense, near net shape metallic components. By consolidating powders under high temperature and pressure, HIP provides isotropic properties, uniform microstructures, and scalability to complex geometries that are vital for sectors such as aerospace, energy, and nuclear power. Yet despite these advantages, the technology has remained constrained by costly trial and error canister fabrication, limitations of conventional forging, and incomplete knowledge about how the canister design influences final part properties. Additive manufacturing (AM), by contrast, thrives on design freedom and geometric flexibility but struggles with speed, scalability, and cost when applied to very large structures. The research presented in this report investigated how a convergent manufacturing approach, combining AM with PM-HIP, can merge the strengths of both technologies, leveraging AM’s flexibility for canister design and HIP’s consolidation capability to deliver reliable, large, and complex parts. The work progressed through three case studies that built on one another in scale and complexity. Small cylindrical canisters fabricated by conventional methods, laser powder bed fusion, and directed energy deposition were filled with stainless steel powders and subjected to HIP. The resulting parts demonstrated near-full density and mechanical properties on par with wrought stainless steel, showing for the first time that AM canisters can be a direct substitute for conventional ones without sacrificing quality. The next step involved a medium-scale, noncentrosymmetric T-valve, which is an enclosed, multibranch geometry that tested the limits of AM + PM-HIP integration. The T-valve achieved predictable shrinkage and uniform densification, confirming feasibility for enclosed designs. However, this study also revealed oxide inclusions and interfacial challenges at the AM + HIP boundary, underscoring the critical importance of controlling interface chemistry and employing robust, in situ strategies, such as melt pool monitoring and thermal monitoring, coupled with nondestructive evaluation techniques such as x-ray computed tomography. Finally, the effort culminated in fabricating a large-scale impeller weighing nearly 2000 lb and spanning 5 ft in diameter. Produced via multirobot wire arc AM and hot isostatic pressed to near-full density, the impeller validated industrial-scale feasibility. Predictive models closely matched experimental shrinkage, tensile properties were spatially uniform across the component, and the AM + PM-HIP interface proved mechanically sound despite the presence of oxide-decorated prior particle boundaries. This large-scale demonstration is a major milestone, showing that hybrid AM + PM‑HIP can reliably deliver components at reactor-relevant scales. Collectively, these studies charted a logical pathway: small-scale work built scientific confidence, medium-scale work highlighted opportunities and challenges, and large-scale work proved industrial impact. The overarching conclusion of this report is that AM + PM-HIP should not be seen as a replacement for forging but as a complementary pathway that provides the US with flexibility, resilience, and new options for manufacturing nuclear-grade components. Looking ahead, several directions emerge as critical to sustaining progress. Predictive modeling must become faster, more accessible, and more accurate, with digital twins and machine learning reducing reliance on trial and error. Powders and alloys must be optimized for HIP, with improved cleanliness, reduced oxides, and tailored chemistries that enhance creep, fatigue, and irradiation resistance. Interfaces between AM and HIP regions must be better engineered through coatings, machining strategies, and surface treatments to mitigate oxide formation and ensure reliable bonding to explore opportunities for HIP of targeted compositional parts, as well as multimaterial HIP cladding applications. Monitoring and nondestructive evaluation need to expand, incorporating multimodal sensors, x-ray computed tomography, and real-time data integration through platforms such as Pelican. At the same time, the pathway to industrial adoption requires techno-economic analysis, machinability studies, and qualification frameworks aligned with industry and regulatory standards. Finally, workforce and academic engagement must be strengthened. Programs that train technicians and engineers for US Navy and US Department of Energy manufacturing challenges should be paired with academic partnerships to support fundamental research, with open sharing of non-export-controlled data to accelerate innovation and build the next generation of experts. In conclusion, this report demonstrates that hybrid AM + PM-HIP is scientifically viable and strategically important. By combining the design agility of AM with the consolidation strength of HIP and embedding modeling, monitoring, and workforce development, this approach provided a transformative new capability for US manufacturing. The path forward is clear: hybrid AM + PM-HIP is not just a promising research direction but is also potentially an industrially relevant pathway that can reshape how nuclear-grade components are designed, qualified, and deployed.

36 MATERIALS SCIENCE↗

Influence of Powder Characteristics and Processing Methods on Creep Performance of Powder Metallurgy Hot Isostatic Pressed SS316

The U.S. nuclear energy expansion goals are driving the demand for manufacturing routes that can rapidly produce large, complex, near net shape components. Powder metallurgy hot isostatic pressing (PM HIP) is an advanced manufacturing technique that can be economically scaled-up, while alleviating the supply chain challenges that forging and casting face in terms of cost and lead time constraints. This makes PM-HIP a viable technology to aid and accelerate large-scale part manufacturing for nuclear applications. However, large-scale qualification and deployment of this technology require a thorough understanding of the influence of powder feedstock quality, powder handling history, hot isostatic pressing (HIP) parameters, and subsequent heat treatment on microstructural evolution and elevated temperature mechanical performance. The present work focusses on 316 austenitic stainless steel (SS316) which is most commonly used in high temperature environments for nuclear applications Results from this study show that PM HIPed SS316 meets ASME tensile requirements at room temperature and at elevated temperature. However, creep performance of PM-HIPed SS316 remains inferior to its wrought counterpart, demonstrating that tensile performance alone is not a reliable metric for long duration high temperature integrity. Further, this report delineates powder derived microstructural features that govern creep damage, with key evidences pointing to “microstructural inheritance” from gas atomized powder feedstocks. Commercial SS316 powders of varying chemical compositions and recycling histories were studies, and the results showed large differences in elemental segregation, oxide surface layers and secondary phase distributions. Multi-scale characterization revealed segregation of chromium, molybdenum, manganese and silicon at the boundaries and the precipitation of manganese-, silicon-, and molybdenum-oxides. During HIP consolidation, these surface oxides transform into decorated prior particle boundaries (PPBs) and grain boundary inclusions that persist through conventional post-HIP solution annealing treatment. The retained oxides in post-HIP microstructures were found to influence grain growth, precipitation behavior, and ultimately creep cavitation and fracture. Such post-HIP heat treatments are therefore limited by a complex trade-off between grain growth, and oxide coarsening which aggravate creep damage by acting as nucleation sites for cavities. The objective of this work is to establish an integrated processing–structure–property framework for PM-HIP 316 stainless steel by investigating the influence of powder feedstock characteristics in pre- and post-HIP processing as well as to understand the significance of post-HIP heat treatment on microstructural evolution and creep properties. The results from this report emphasize the significance of powder feedstock integrity in improving creep performance of PM-HIPed SS316, by highlight the effect of rapid solidification, elemental segregation, oxide formation and powder recycling on microstructural defect inheritance following HIP consolidation. Rather than considering HIP processing, solution annealing, and mechanical performance independently, this report treats powder production, HIP consolidation, post-HIP thermal processing, and creep deformation as interconnected stages within a continuous metallurgical process. The resulting framework will provide a scientific basis for developing feedstock engineering strategies capable of improving long-term reliability of PM-HIP stainless steels and accelerating their qualification for advanced nuclear applications.

Ajjarapu, Pavan [Oak Ridge National Laboratory (OR↗

Isostatic compression process converts polyaromatics into structural material

Isostatic compression process compacts certain powdered aromatic polymers into homogeneous materials that can be machined to form useful components, such as bearings. It provides for complete removal of air in the interstitial spaces surrounding the granules of the powdered polymer before the powder is subjected to isostatic compression.

Ingham, J. D.↗

Earth's isostatic gravity anomaly field: Contributions to National Geodetic Satellite Program

On the assumption that the compensation for the topographic load is achieved in the manner of Airy-Heiskenenan hypothesis at a compensation depth of 30 kilometers, the spherical harmonic coefficients of the isostatic reduction potential U are computed. The degree power spectra of these coefficients are compared with the power spectra of the isostatic reduction coefficients given by Uotila. Results are presented in tabular form.

Khan, M. A.↗

On isostatic geoid anomalies

In regions of slowly varying lateral density changes, the gravity and geoid anomalies may be expressed as power series expansions in topography. Geoid anomalies in isostatically compensated regions can be directly related to the local dipole moment of the density-depth distribution. This relationship is used to obtain theoretical geoid anomalies for different models of isostatic compensation. The classical Pratt and Airy models give geoid height-elevation relationships differing in functional form but predicting geoid anomalies of comparable magnitude. The thermal cooling model explaining ocean floor subsidence away from mid-ocean ridges predicts a linear age-geoid height relationship of 0.16 m/m.y. Geos 3 altimetry profiles were examined to test these theoretical relationships. A profile over the mid-Atlantic ridge is closely matched by the geoid curve derived from the thermal cooling model. The observed geoid anomaly over the Atlantic margin of North America can be explained by Airy compensation. The relation between geoid anomaly and bathymetry across the Bermuda Swell is consistent with Pratt compensation with a 100-km depth of compensation.

Haxby, W. F.↗

Topographic domes on Ganymede - Ice vulcanism or isostatic upwarping

Two formation processes are considered for two gently sloping domeshaped features on the surface of Ganymede, lying on grooved terrain and having diameters of roughly 250 km: (1) water vulcanism, triggered by a major impact, and (2) the isostatic upwarping of a crater formed in a thin crust. Numerical simulations show the volume of the domes to be consistent with eruption through fractures created by an impact that excavates partly through a thin crust. Isostatic upwarp rates calculated as a function of effective crustal temperature indicate that upwarping could also create such a dome if the impact excavated to a depth where the crust was sufficiently warm and mobile. Morphologic evidence suggests that both processes may have been important and, if either of the proposed models is correct, it is strongly implied that grooved terrain formation occurred prior to the thickening and stiffening of Ganymede's crust.

Squyres, S. W.↗

Global isostatic geoid anomalies for plate and boundary layer models of the lithosphere

Commonly used one dimensional geoid models predict that the isostatic geoid anomaly over old ocean basins for the boundary layer thermal model of the lithosphere is a factor of two greater than that for the plate model. Calculations presented, using the spherical analogues of the plate and boundary layer thermal models, show that for the actual global distribution of plate ages, one dimensional models are not accurate and a spherical, fully three dimensional treatment is necessary. The maximum difference in geoid heights predicted for the two models is only about two meters. The thermal structure of old lithosphere is unlikely to be resolvable using global geoid anomalies. Stripping the effects of plate aging and a hypothetical uniform, 35 km, isostatically-compensated continental crust from the observed geoid emphasizes that the largest-amplitude geoid anomaly is the geoid low of almost 120 m over West Antarctica, a factor of two greater than the low of 60 m over Ceylon.

Hager, B. H.↗

Hot isostatically pressed manufacture of high strength MERL 76 disk and seal shapes

The feasibility of using MERL 76, an advanced high strength direct hot isostatic pressed powder metallurgy superalloy, as a full scale component in a high technology, long life, commercial turbine engine were demonstrated. The component was a JT9D first stage turbine disk. The JT9D disk rim temperature capability was increased by at least 22 C and the weight of JT9D high pressure turbine rotating components was reduced by at least 35 pounds by replacement of forged Superwaspaloy components with hot isostatic pressed (HIP) MERL 76 components. The process control plan and acceptance criteria for manufacture of MERL 76 HIP consolidated components were generated. Disk components were manufactured for spin/burst rig test, experimental engine tests, and design data generation, which established lower design properties including tensile, stress-rupture, 0.2% creep and notched (Kt = 2.5) low cycle fatigue properties, Sonntag, fatigue crack propagation, and low cycle fatigue crack threshold data. Direct HIP MERL 76, when compared to conventionally forged Superwaspaloy, is demonstrated to be superior in mechanical properties, increased rim temperature capability, reduced component weight, and reduced material cost by at least 30% based on 1980 costs.

Eng, R. D.↗

Degree variances of the earth's potential, topography and its isostatic compensation

A spherical harmonic expansion of the earth's gravitational potential and equivalent rock topography to degree and order 180 is described. The potential implied by the topography considered as uncompensated and with isostatic compensation has been computed. Good agreement with the observed potential field is found when the depth of compensation in the Airy theory is assumed to be 50 km. At the higher degrees the correlation coefficient between the potential expansion and the equivalent rock topography is about 0.5. The Lachapelle equations for the topographic isostatic potential were tested using 1 x 1 deg equivalent rock topography. The degree variances agree at the lower degrees but at degree 36 the Lachapelle results using 5 deg data underestimate the potential degree variances by about one-third.

Rapp, R. H.↗

Consolidation of Si3N4 without additives (by hot isostatic pressing)

The potential of using hot isostatic pressing (HIP'ing) technique to produce dense silicon nitride materials without or with a reduced amount of additives (much less than 5 w/o) was investigated. Hot isostatic pressing technique can provide higher pressure and temperature than hot pressing can, thus has the potential of requiring less densification aids to consolidate Si3N4 materials. It was anticipated that if such dense materials could be fabricated, the high temperature strength of the material should be improved significantly. Observations on the phase transformation, densification behavior, and microstructures of the samples are also documented. Density, microhardness, four point bend strength (room temperature and 1370 C) were measured on selected densified materials.

Yeh, H. C.↗

Effect of hot isostatic pressing on reaction-bonded silicon nitride

Specimens of nearly theoretical density have been obtained through the isostatic hot pressing of reaction-bonded silicon nitride under 138 MPa of pressure for two hours at 1850, 1950, and 2050 C. An amorphous phase that is introduced by the hot isostatic pressing partly accounts for the fact that while room temperature flexural strength more than doubles, the 1200 C flexural strength increases significantly only after pressing at 2050 C.

Watson, G. K.↗

Microstructure of reaction-bonded silicon nitride consolidated by isostatic hot-pressing

A microstructural examination and chemical analysis are conducted for reaction-bonded Si3N4 specimens that were isostatically hot pressed at 1850, 1950, and 2050 C. The present observations indicate that the previously reported increase in the 1200 C bend strength of reaction-bonded Si3N4, after pressing at 2050 C exclusively, is due to the relative oxygen levels of the isostatically hot pressed specimens; calculations show that an SiO2 content of less than about 2.2 vol pct is needed to yield the 1200 C strength increase.

Mieskowski, D. M.↗

Effect of hot isostatic pressing on the properties of sintered alpha silicon carbide

Two lots of alpha silicon carbide were isostatically hot-pressed under 138 MPa for 2 h in Ar at temperatures up to 2200 C. Nearly theoretically dense specimens resulted. Hot isostatic pressing increased both room-temperature strength and 1200 C strength, and resulted in improved reliability. One lot of material which was pressed at 2200 C showed increases of about 20 percent in room-temperature strength and about 50 percent in 1200 C flexural strength; the Weibull modulus improved about 100 percent.

Watson, G. K.↗

Hot isostatic pressing of ceramics

A mixture containing glass 70 to 95 and BN or B4C powder (0.1-10 microns) 5 to 30 vol. % is used as a secondary pressure medium in hot isostatic pressing of ceramics. Thus, Pyrex beads were mixed with 15% vol. BN powder (average diameter 2 microns), fused at 1400 deg for 2 h, cooled, crushed, and put into a graphite crucible. A Si3N4 sintered body was embedded in the powder, heated in vacuum at 1200 deg for 2 h, treated in a hot isostatic press furnace at 1700 deg and 1000 atm. for 1 h, and cooled to give a Si3N4 ceramic. It was easily separated from the crucible.

Honma, K.↗

Removal of glass adhered to sintered ceramics in hot isostatic pressing

In the hot isostatic pressing of ceramic materials in molten glass using an inert gas as a pressing medium, glass adhered to the sintered ceramics is heated to convert it to a porous glass and removed. Thus, Si3N4 powder was compacted at 5000 kg/sq cm, coated with a 0.5 mm thick BN, embedded in Pyrex glass in a graphite crucible, put inside a hot isostatic press containing Argon, hot pressed at 1750 C and 100 kg/sq cm; cooled, taken out from the crucible, heated at 1100 C for 30 minutes, cooled, and then glass adhered to the sintered body was removed.

Source record↗

Mechanical properties of high gradient and hot isostatically pressed PWA 1480

This program has been designed to evaluate the potential benefits to alloy 1480 material properties due to high thermal gradient casting, hot isostatic pressing, and alternative heat treatment. Alloy 1480 castings have been obtained from vendors representing the extremes of commercial casting thermal gradients. Quantitative characterization of the dendrite arm spacing (DAS) and pore distributions has been conducted. A hot isostatic pressing (HIP) schedule, which avoids the many pitfalls of single crystal HIP has been devised for alloy 1480. In addition, an alternate heat treatment for alloy 1480 has been devised which provides benefits in mechanical properties. The standard gradient cast test material is being evaluated in the standard heat treat condition as a baseline and in the HIP plus alternate heat treated condition. The fhigh gradient cast material is being evaluated in alternate heat treat and HIP plus alternate heat treated conditions. Evaluations focus on demonstration of the benefits due to the applied processes, especially in the area of cyclic life.

Fritzemeier, L. G.↗

Strength of hot isostatically pressed and sintered reaction bonded silicon nitrides containing Y2O3

The hot isostatic pressing of reaction bonded Si3N4 containing Y2O3 produced specimens with greater room temperature strengths than those by high pressure nitrogen sintering of the same material. Average room temperature bend strengths for hot isostatically pressed reaction bonded silicon nitride and high pressure nitrogen sintered reaction bonded silicon nitride were 767 and 670 MPa, respectively. Values of 472 and 495 MPa were observed at 1370 C. For specimens of similar but lower Y2O3 content produced from Si3N4 powder using the same high pressure nitrogen sintering conditions, the room temperature strength was 664 MPa and the 1370 C strength was 402 MPa. The greater strengths of the reaction bonded silicon nitride materials in comparison to the sintered silicon nitride powder material are attributed to the combined effect of processing method and higher Y2O3 content.

William A Sanders↗