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Materials for Advanced Ultrasupercritical Steam Turbines Task 4: Cast Superalloy Development

The Steam Turbine critical stationary structural components are high integrity Large Shell and Valve Casing heavy section Castings, containing high temperature steam under high pressures. Hence to support the development of advanced materials technology for use in an AUSC steam turbine capable of operating with steam conditions of 760°C (1400°F) and 35 Mpa (5000 psia), Casting alloy selection and evaluation of mechanical, metallurgical properties and castability with robust manufacturing methods are mandated. Alloy down select from Phase 1 based on producability criteria and creep rupture properties tested by NETL-Albany and ORNL directed the consortium to investigate cast properties of Haynes 282 and Haynes 263. The goals of Task 4 in Phase 2 are to understand a broader range of mechanical properties, the impact of manufacturing variables on those properties. Scale up the size of heats to production levels to facilitate the understanding of the impact of heat and component weight, on metallurgical and mechanical behavior. GE Power & Water Materials and Processes Engineering for the Phase 2, Task 4.0 Castings work, systematically designed and executed casting material property evaluation, multiple test programs. Starting from 15 lbs. cylinder castings to world’s first 17,000 lbs. poured weight, heavy section large steam turbine partial valve Haynes 282 super alloy casting. This has demonstrated scalability of the material for steam Turbine applications. Activities under Task 4.0, Investigated and characterized various mechanical properties of Cast Haynes 282 and Cast Nimonic 263. The development stages involved were: 1) Small Cast Evaluation: 4 inch diam. Haynes 282 and Nimonic 263 Cylinders. This provided effects of liquidus super heat range and first baseline mechanical data on cast versions of conventional vacuum re-melted and forged Ni based super alloys. 2) Step block castings of 300 lbs. and 600 lbs. Haynes 282 from 2 foundry heats were evaluated which demonstrated the importance of proper heat treat cycles for Homogenization, and Solutionizing parameters selection and implementation. 3) Step blocks casting of Nimonic 263: Carried out casting solidification simulation analysis, NDT inspection methods evaluation, detailed test matrix for Chemical, Tensile, LCF, stress rupture, CVN impact, hardness and J1C Fracture toughness section sensitivity data and were reported. 4) Centrifugal Casting of Haynes 282, weighing 1400 lbs. with hybrid mold (half Graphite and half Chromite sand) mold assembly was cast using compressor casing production tooling. This test provided Mold cooling rates influence on centrifugally cast microstructure and mechanical properties. Graphite mold section out performs sand mold across all temperatures for 0.2% YS; %Elongation, %RA, UTS at 1400°F. Both Stress-LMP and conditional Fracture toughness plots data were in the scatter band of the wrought alloy. 5) Fundamental Studies on Cooling rates and SDAS test program. Evaluated the influence of 6 mold materials Silica, Chromite, Alumina, Silica with Indirect Chills, Zircon and Graphite on casting solidification cooling rates. Actual Casting cooling rates through Liquidus to Solidus phase transition were measured with 3 different locations based thermocouples placed in each mold. Compared with solidification simulation cooling rates and measurement of SDAS, microstructure features were reported. The test results provided engineered casting potential methods, applicable for heavy section Haynes 282 castings for optimal properties, with foundry process methods and tools. 6) Large casting of Haynes 282 Drawings and Engineering FEM models and supplemental requirements with applicable specifications were provided to suppliers for the steam turbine proto type feature valve casing casting. Molding, melting and casting pouring completed per approved Manufacturing Process Plan during 2014 Q4. The partial valve casing was successfully cast after casting methods were validated with solidification simulation analysis and the casting met NDT inspection and acceptance criteria. Heat treated and sectioned to extract trepan samples at different locations comparing with cast on coupons test data. Material properties requisite for design, such as tensile, creep/rupture, LCF, Fracture Toughness, Charpy V-notch chemical analysis testing were carried out. The test results will be presented in the final report. The typical Haynes 282 large size Steam Turbine production casting from Order to Delivery foundry schedule with the activity break up is shown in Figures 107 and 108. • From Purchase Order placement to Casting pouring ~ 26 weeks. 1. Sales and commercial review 3 2. Engineering Drawings/models review 4 3. Pattern and core box manufacturing 6 4. Casting process engineering review 4 5. FEM and solidification simulation analysis 4 6. Gating & Feeder Attachments, Ceramic tiling 2 7. Molding and coremaking production scheduling 6 8. Melting planning and schedule 3 9. Pouring, cooling and shake out 2 • From Pouring to casting Delivery ~ 29 weeks 10. Shot blast and riser cutting, gates removal 3 11. Homogenizing , solutionizing HT furnace prep 4 12. Grinding, Fettling 2 13. Aging HT Cycle, cooling 2 14. VT and LPT NDT inspections 2 15. Radiographic inspection 4 16. Mechanical testing, Chemical analysis test certs 4 17. Casting weld repair upgrades and Aging PWHT 4 18. NDT after weld repairs and casting upgrades 3 19. Casting Final Inspection and test certifications 3 20. Package and delivery 2 Hence the Total Lead time from P.O to Casting delivery is approximately 55 weeks. The Task 4.2 and Task 4.3 activities and reporting completed.

Thangirala, Mani↗

Effect of Slag-Steel Reaction on the Initial Solidification of Molten Steel during Continuous Casting

With the mold simulator technique, the effect of slag-steel reaction on the initial shell solidification as well as the heat transfer and lubrication behavior of the infiltrated mold/shell slag film was studied in this article. The results showed that the Al{sub 2}O{sub 3} content, the CaO/SiO{sub 2} ratio, and the viscosity of mold flux were increased with the progress of the slag-steel reaction during casting. The slag-steel reaction has two major effects on the initial shell solidification: one is increasing the mold heat flux and shell thickness by the decrease of slag film thickness. The other is the reduction of mold heat flux by the increase of crystal fraction in slag film. Mold flux with a lower basicity, viscosity, and crystallization temperature would result in a larger liquid slag consumption and the uneven infiltration of slag into the mold and shell gap that eventually leads to the irregular solidification of initial shell with a poor surface quality, such as slag entrapment and depressions as well as glaciation marks. Conversely, mold flux with a higher viscosity, basicity, and crystallization temperature would result in a smaller liquid slag consumption, which would cause the poor mold lubrication, the longitudinal shell surface defects, and drag marks.

36 MATERIALS SCIENCE↗

Influence of Electropulsing Treatment on the Initial Solidification of Molten Steel During Continuous Casting

An electropulsing-assisted mold simulator (EPMS) technique was developed to investigate the effect of pulsed electric current on the initial solidification behavior of molten steel during the process of continuous casting. The results indicated that the variation of mold hot surface temperatures in the meniscus area decreased from 375.8 K to 394 K for the case without electropulsing treatment (EPT) to 363.5 K to 377.3 K for the one with EPT. The mold surface heat fluxes fluctuated around the baseline of 0.83 and 2.42 MW/m{sup 2} in the cases with and without EPT, respectively, which indicated that a higher thermal resistance between the initial shell and copper mold was introduced by employing the EPT. The crystal fraction of slag films increased from 69.8 to 77.9 pct, whereas the grain size of mold flux film decreased, when compared the case of EPT treatment with the benchmark one, which suggested that the pulsed electric current promotes the movement of molten clusters and particles, leading to the enhancement of mold flux crystallization and the improvement of thermal resistance. Moreover, the solidification structure of steel along the direction of solidification (from the mold to melt) includes a fine chilled grain layer close to the mold, a columnar dendrite layer in the middle, and equiaxed grains next to the melt core, in which a compacted microstructure with smaller secondary dendrite arm spacing was observed in the case of the EPT. The results demonstrate that the EPT could refine the as-cast solidification microstructure.

36 MATERIALS SCIENCE↗

Use of DSC and DMA Techniques to Help Investigate a Material Anomaly for PTFE Used in Processing a Piston Cup for the Urine Processor Assembly (UPA) on International Space Station (ISS)

Human urine and flush water are eventually converted into drinking water with the Urine Processor Assembly (UPA) aboard the International Space Station (ISS). This conversion is made possible through the Distillation Assembly (DA) of the UPA. One component of the DA is a molded circular piston cup made of virgin polytetrafluoroethylene (PTFE). The piston cup is assembled to a titanium component using eight fasteners and washers. Molded PTFE produced for spare piston cups in the first quarter of 2010 was different in appearance and texture, and softer than material molded for previous cups. For the suspect newer PTFE material, cup fasteners were tightened to only one-half the required torque value, yet the washers embedded almost halfway into the material. The molded PTFE used in the DA piston cup should be Type II, based on AMS 3667D and ASTM D4894 specifications. The properties of molded PTFE are considerably different between Type I and II materials. Engineers working with the DA thought that if Type I PTFE was molded by mistake instead of Type II material, that could have resulted in the anomalous material properties. Typically, the vendor molds flat sheet PTFE from the same material lot used to mold the piston cups, and tensile testing as part of quality control should verify that the PTFE is Type II material. However, for this discrepant lot of material, such tensile data was not available. Differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) were two of the testing techniques used at the NASA/Marshall Space Flight Center (MSFC) to investigate the anomaly for the PTFE material. Other techniques used on PTFE specimens were: Shore D hardness testing, tensile testing on dog bone specimens and a qualitative estimation of porosity by optical and scanning electron microscopy.

Wingard, Doug↗

3D printing of packaging inserts from biomass-fungi composites: Environmental sustainability analysis

In this study, a comprehensive Life cycle assessment (LCA) is conducted on molded packaging inserts from expanded polystyrene (EPS) foam, molded packaging inserts from biomass-fungi composite, and 3D-printed packaging inserts from biomass-fungi composite under the low mix / high volume (LMHV) scenario and molded and machined packaging inserts from EPS foam, molded and machined packaging inserts from biomass-fungi composite, and 3D-printed packaging inserts from biomass-fungi composite under the high mix / low volume (HMLV) scenario. Six environmental impact categories—climate change, acidification, eutrophication, fossil resource scarcity, land use, and water consumption—are analyzed to evaluate the environmental trade-offs associated with each type of packaging inserts. Under the LMHV scenario, molded packaging inserts from biomass-fungi composite emerge as the best option due to their lower impact on climate change, acidification and water consumption compared to other types of packaging inserts. Conversely, molded packaging inserts from biomass-fungi composite face challenges in land use and eutrophication, primarily due to raw material production. LCA also reveals that 3D-printed packaging inserts from biomass-fungi composite are the most environmentally favorable option under the HMLV scenario, due to significantly lower contributions to climate change, eutrophication, and water consumption compared to other types of packaging inserts. Conversely, 3D-printed packaging inserts from biomass-fungi composite face challenges in acidification and land use, primarily due to raw material production. As part of the LCA, sensitivity analyses show that sourcing energy from 100% renewable sources substantially lowers climate change impacts across all packaging types, while varying transportation distances results in only minor changes, indicating the dominant role of upstream material and manufacturing processes. Additional sensitivity analysis is conducted under the HMLV scenario to assess the impact of material removal during machining on the environment. The amount of material removal is varied from 10 to 70% for the sensitivity analysis and it highlights that the amount of material removed during machining has no significant impact on climate change for packaging inserts from EPS foam. However, molded and machined packaging inserts from biomass-fungi composite show an increasing trend in climate change with higher amount of material removal, while 3D-printed packaging inserts from biomass-fungi composite exhibit a decreasing trend, driven by reduced raw material usage and energy consumption.

09 BIOMASS FUELS↗

Design and Production for Maximum Structural Efficiency With Respect to Fiber Orientation With Increased Understanding of Hybrid Fiber Flow Behavior

Discontinuous fiber-reinforced thermoplastic composites have gained considerable attention in automotive, aerospace, and other industries, due to their high-rate of production combined with their ability to attain complex and intricate shapes. Among other high-rate thermoplastic manufacturing processes, injection-molding is one of the most common manufacturing methods due to fast production and high surface finishing of complex geometries. Fiber orientation in discontinuous fiber composites plays a pivotal role in determining the mechanical, electrical, and thermomechanical properties, underscoring the necessity to comprehend fiber orientation in injection molded parts. Among different fiber types, glass and carbon fibers are most common in the composite industries. The recent trend of hybrid composites comprising both glass fiber (GF) and carbon fiber (CF) is also gaining importance in the automotive industry. Hybrid fiber options allow designers to optimize the balance between glass and carbon fibers by leveraging the high durability and low cost of GF while the strength and lightweight properties of CF. Consequently, comparing the fiber oriented distribution (FOD) of injection molded composites containing GF, CF, and a hybrid of GF/CF is critical to investigating the local mechanical properties of intricate structures for high-end applications. In Phase I of this project, FOD in injection-molded panels with respect to distance from the gate was analyzed using X-ray computed tomography (X-CT) for GF, CF, and hybrid CF/GF (CGF) reinforced nylon 66. To understand the reason behind the FOD with different fiber types, computational fluid dynamics (CFD) and rheology were performed. Samples were extracted at three locations: near the gate, center, and opposite end. Thickness of the layers of typical skin-shell-core type FOD varies with fiber type and location. GF achieved flow direction alignment (in shell) earlier than viscous CF and CGF near the gate, whereas CF showed the highest flow-direction alignment at the center due to shear induced orientation. At the opposite end, GF experienced more backflow than others indicating faster mold filling owing to its lower viscosity. Hybrid CGF exhibited GF-dominated center and CF-dominated end region. The numerical model used to obtain FOD and rheological predictions for the CF and GF composites served to corroborate the trends observed in the experimental trials. The FOD responses across fiber types and location were reflected in their longitudinal and transverse properties. Only GF showed higher longitudinal modulus over transverse modulus near the gate attributed to rapid alignment, whereas CF and CGF exhibited opposite trend. However, fountain flow enhanced the longitudinal modulus over transverse modulus with the distance for all, particularly for CF. This study offers insights into mold filling behavior of different fibers which are critical in optimizing injection molding conditions for tailored final properties.

36 MATERIALS SCIENCE↗

Silicon crystals: Process for manufacturing wafer-like silicon crystals with a columnar structure

Wafer-like crystals suitable for making solar cells are formed by pouring molten Si containing suitable dopants into a mold of the desired shape and allowing it to solidify in a temperature gradient, whereby the large surface of the melt in contact with the mold is kept at less than 200 D and the free surface is kept at a temperature of 200-1000 D higher, but below the melting point of Si. The mold can also be made in the form of a slit, whereby the 2 sides of the mold are kept at different temperatures. A mold was milled in the surface of a cylindrical graphite block 200 mm in diameter. The granite block was induction heated and the bottom of the mold was cooled by means of a water-cooled Cu plate, so that the surface of the mold in contact with one of the largest surfaces of the melt was held at approximately 800 D. The free surface of the melt was subjected to thermal radiation from a graphite plate located 2 mm from the surface and heated to 1500 D. The Si crystal formed after slow cooling to room temperature had a columnar structure and was cut with a diamond saw into wafers approximately 500 mm thick. Solar cells prepared from these wafers had efficiencies of 10 to 11%.

Authier, B.↗

Method of Fabricating Chopped-Fiber Composite Piston

A three-dimensional piston molding is fabricated from a mixture of chopped, carbon tow filaments of variable length, which are prepregged with carbonaceous organic resins and/or pitches and molded by conventional molding processes into a near net shape, to form a carbon-fiber reinforced organic-matrix composite part. Continuous reinforcement in the form of carbon-carbon composite tapes or pieces of fabric can be also laid in the mold before or during the charging of the mold with the chopped-fiber mixture, to enhance the strength in the crown and wrist-pin areas. The molded chopped-fiber reinforced organic-matrix composite parts are then pyrolized in an inert atmosphere, to convert the organic matrix materials to carbon. These pyrolized parts are then densified by reimpregnation with resins or pitches, which are subsequently carbonized. Densification is also accomplished by direct infiltration with carbon by vapor deposition processes. Once the desired density has been achieved, the piston molds are machined to final piston dimensions, and piston ring grooves are added. To prevent oxidation and/or to seal the piston surface or near surface, the chopped-fiber piston is coated with ceramic and/or metallic sealants: and/or coated with a catalyst.

Rivers, H. Kevin↗

Macrosegregation Resulting from Directional Solidification Through an Abrupt Change in Cross-Sections

Simulations of the directional solidification of two hypoeutectic alloys (Al-7Si alloy and Al-19Cu) and resulting macrosegregation patterns are presented. The casting geometries include abrupt changes in cross-section from a larger width of 9.5 mm to a narrower 3.2 mm width then through an expansion back to a width of 9.5 mm. The alloys were chosen as model alloys because they have similar solidification shrinkages, but the effect of Cu on changing the density of the liquid alloy is about an order of magnitude greater than that of Si. The simulations compare well with experimental castings that were directionally solidified in a graphite mold in a Bridgman furnace. In addition to the simulations of the directional solidification in graphite molds, some simulations were effected for solidification in an alumina mold. This study showed that the mold must be included in numerical simulations of directional solidification because of its effect on the temperature field and solidification. For the model alloys used for the study, the simulations clearly show the interaction of the convection field with the solidifying alloys to produce a macrosegregation pattern known as "steepling" in sections with a uniform width. Details of the complex convection- and segregation-patterns at both the contraction and expansion of the cross-sectional area are revealed by the computer simulations. The convection and solidification through the expansions suggest a possible mechanism for the formation of stray grains. The computer simulations and the experimental castings have been part of on-going ground-based research with the goal of providing necessary background for eventual experiments aboard the ISS. For casting practitioners, the results of the simulations demonstrate that computer simulations should be applied to reveal interactions between alloy solidification properties, solidification conditions, and mold geometries on macrosegregation. The simulations also presents the possibility of engineering the mold-material to avoid, or mitigate, the effects of thermosolutal convection and macrosegregation by selecting a mold material with suitable thermal properties, especially its thermal conductivity.

Lauer, M.↗

Mathematical Modeling on the Influence of Casting Parameters on Initial Solidification at the Meniscus of Slab Continuous Casting

In the current study, the two-dimensional mold model was applied to investigate the influence of different casting parameters on the initial solidification at the meniscus of the continuous casting mold. The profile of the meniscus and the slag rim, and the heat flux on the hot face of the copper plate, were compared with different locations of the mold and different casting parameters. The depth of the oscillation marks and solidified meniscus through simulation was measured with different casting parameters. With the mold oscillating downward from the peak to the valley, the maximum heat flux on the hot face of the copper plate near the meniscus increased from 4.3 to 5.5 MW/m{sup 2}, the thickness of the slag rim decreased from 4.7 to 4.2 mm, and the height of the curved meniscus also decreased. With the increase of casting speed from 1.2 to 1.45 m/min, the maximum speed of the upper backflow increased from 0.6 to 0.8 m/s, and the lowest location of the meniscus at approximately 310 mm from the copper plate decreased from 22 to 12 mm below the meniscus near the nozzle, where the slag entrapment easily occurred. With the increase of the casting speed, casting superheat, and oscillation frequency, and the decrease of the water flow rate in the mold and oscillation amplitude, the thickness of the slag rim decreased. With the increase of casting speed and superheat, and the decrease of the water flow rate in the mold, oscillation frequency, and oscillation amplitude, the depth of the solidified meniscus decreased. The regression equation was fitted to estimate the depth of hooks at the subsurface of slabs.

36 MATERIALS SCIENCE↗

FY 2011 Miniature Spherical Retroreflectors (Final Report)

PNNL conducted a systematic optical modeling effort to study and compare retroreflector designs with respect to available optical materials. The optical Strehl ratio (SR) and cross section figures of merit were used to compare the performance of candidate optical designs. Further modeling was conducted to assess the relationships between standoff range and retroreflector diameter and cross section. Analysis showed that small diameter retroreflectors have very high optical link loss, since the net loss scales by retroreflector diameter to the 4th power. Optical retroreflection efficiency is also important, but extracting ideal performance from a complicated design must be tempered by the fact that the effective retroreflector range varies only as the fourth root of the cross section. It's therefore imperative to maintain a reasonable retroreflector diameter, but striving for perfect optical performance may be a costly effort that does not merit the modest performance gain. Several promising designs were developed for visible and mid-infrared applications, which embraced lessons learned in the standoff range study. These designs included a polymer clad glass core approach for visible wavelengths and a concentric shell design using chalcogenide glass for the mid-infrared. Injection molding feasibility studies demonstrated that it was practical to fabricate visible polymer retroreflectors using this approach. Such an approach may be a practical solution for the LLNL project. Our primary focus is to develop mid-infrared designs; therefore compression molding chalcogenide glass was adopted for fabricating mid-infrared retroreflectors. A significant effort was focused on developing practical compression molding methods that provided reasonable device yield. A custom compression molding press was developed in collaboration with a private engineering firm. Many successful molding studies were conducted during this effort, but ultimately the fragile nature of the chalcogenide glass and the unfavorable thermal expansion properties limited the feasibility of fabricating the thin shell structures needed for this design. An alternative Cat's Eye retroreflector design was therefore adopted. This design is constructed using two hemispherical structures that can be fabricated by conventional grinding and polishing methods or by molding with high yield. The cross section of this design is very good (and can be further improved by applying a highly reflective coating to the rear surface), but has reduced field of view as a design trade off as well as the isotropic nature of Luneburg-style retroreflector.

36 MATERIALS SCIENCE↗

Carbon Fiber Reinforced Polyolefin Body Panels

This project addresses an automotive industry desire for a cost-effective, lightweight material for body panels that offers mass reduction compared to steel and aluminum body panels, and a cost savings compared to incumbent polymer body panels. Inexpensive polypropylene (PP) combined with <10 weight % reclaimed/recycled carbon fiber (rCF) have the potential to meet both performance and affordability targets for lightweight, paintable vertical body panels. This project supports DOE and IACMI technical goals of reducing production cost of CF composites >25% in 5 years on a path to >50% in 10 years and demonstrating technologies for >80% recyclability or reuse of fiber reinforced composites in 5 years on a path to >95% in 10 years. Alternative body panel materials must meet all fit and surface finish requirements, and match the appearance of metal body panels adjacent to them. The PP/rCF materials must maintain exterior dimensional requirements with a low co-efficient of thermal expansion, excellent paintability, and mechanical performance. Thermoplastic injection molding offers significant reduction in tooling costs as injection molding dies are typically less than half the cost of stamping dies. This project utilized rCF compounded with special formulations of PPs to produce automotive components that meet requirements for fit, finish, mechanical performance, and paintability while offering significant mass savings over incumbent metal panels. It will also offer a cost savings versus other composite solutions. Fenders were molded at the IACMI – Corktown facility using an existing fender tool. Ford Motor Company was the industry lead for this project and provided project management, testing, painting and adhesion testing, and developed the cost-model/business case. Ford engaged and aggregated cost share with Borealis who provided materials, technical support for process trials, and participated in coordination meetings. Vehicles Technology Area staff in Corktown assisted in project management, process trials, molded fenders, and benchmarked physical characteristics. Over 450 plaques were molded with two different gating systems to look at processing conditions and specimens were excised for mechanical testing. Plaques were also used for paint trials, surface analysis, and dimensional analysis. Subsequently, over 200 fenders were molded at IACMI – Corktown. These fenders were used for paint trials, surface analysis, and dimensional analysis. The PP/rCF systems met all of the requirements except for paint appearance. Additional development of paint primer and top coat is necessary to fulfill automotive OEM paint surface requirements.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Quantitative Evaluations of Surface Cleanliness in IF Steel Slabs at Unsteady Casting

Macro-inclusions in the surface layer of slabs are mainly responsible for the sliver defects in IF steel sheets. In the present work, macro-inclusions in six kinds of unsteady cast IF steel slabs involving four unsteady states (casting start, ladle change, nozzle change and casting end) in one casting sequence were quantitatively characterized using an automatic inclusion analyzer with a total detection area of 238,048 mm{sup 2}. The cleanliness of corresponding normal slabs was also evaluated as the benchmark study, and the number density (ND) of inclusions > 50 µm was used to describe the surface slab cleanliness. Generally, alumina-based and mold powder inclusions were detected, and the former type was further subdivided into alumina clusters, alumina associated with bubbles, refractory-related alumina, Al-Ti complex oxides and CaO-Al{sub 2}O{sub 3}-MgO. Several large-sized alumina-based inclusions were detected in the normal slabs with an average ND of 0.31 N/cm{sup 2}, although they had very low total oxygen (TO) contents (10~13 ppm). No mold powder inclusions were found in normal slabs. For all the unsteady slabs, alumina-based and mold powder inclusions were both observed, and the percentage of the former kind was ≥ 90 pct. The average density of macro-inclusions for the first slab was 1.621 N/cm{sup 2}, whose cleanliness was much worse than any of the other unsteady slabs. The first slab should be downgraded. For the second slab, the ND of macro-inclusions was 0.385 N/cm{sup 2}, which was still larger than the normal slabs because of the lasting effect of the re-oxidation. For the penultimate, cap-off and SEN changed slabs, the density of macro-inclusions fluctuated from 0.25~0.35 N/cm{sup 2}, which was close to the average level of normal slabs. However, mold flux-originated inclusions were frequently observed in these slabs because of flow pattern variations due to the casting speed change. In terms of the slab during the ladle change process, mold powder inclusions were frequently detected even though the casting speed remained constant. A mold powder entrapment mechanism was proposed, which showed the entrapment occurred owing to the flow pattern change induced by forming/dropping of SEN clogs due to re-oxidation by FeO in the ladle slag and tundish steel temperature variations during the ladle change practice. The severity of powder entrapment and re-oxidation was also given for different kinds of unsteady slabs, which provides a direct guide to treating these slabs in the steel plant.

36 MATERIALS SCIENCE↗

Integrated System of Thermal/Dimensional Analysis for Quality Control of Metallic Melt and Ductile Iron Casting Solidification

The main objective of the present work is to introduce a specific experimental instrument and technique for simultaneously evaluating cooling curves and expansion or contraction of cast metals during solidification. Contraction/expansion analysis illustrates the solidification parameters progression, according to the molten cast iron characteristics, which are dependent on the melting procedure and applied metallurgical treatments, mold media rigidity and thermal behavior [heat transfer parameters]. The first part of the paper summarizes the performance of this two-mold device. Its function is illustrated by representative shrinkage tendency results in ductile cast iron as affected by mold rigidity (green sand and furan resin sand molds) and inoculant type (FeSi-based alloys), published in part previously. The second part of the paper illustrates an application of this equipment adapted for commercial foundry use. It conducts thermal analysis and volume change measurements in a single ceramic cup so that mold media as well as solidification conditions are constants, with cast iron quality as the variable. Experiments compared gray and ductile cast iron solidification patterns. Gray iron castings are characterized by higher undercooling at the beginning and at the end of solidification and lower graphitic expansion. Typically, ductile cast iron exhibits higher graphitic, initial expansion, conducive for shrinkage formation in soft molds.

36 MATERIALS SCIENCE↗

Better Actuation Through Chemistry: Using Surface Coatings to Create Uniform Director Fields in Nematic Liquid Crystal Elastomers

Controlling the molecular alignment of liquid crystal monomers (LCMs) within nano- and microstructures is essential in manipulating the actuation behavior of nematic liquid crystal elastomers (NLCEs). In this paper, we study how to induce uniformly vertical alignment of nematic LCMs within a micropillar array to maximize the macroscopic shape change using surface chemistry. Landau–de Gennes numerical modeling suggests that it is difficult to perfectly align LCMs vertically in every pore within a poly(dimethylsiloxane) (PDMS) mold with porous channels during soft lithography. In an untreated PDMS mold that provides homeotropic anchoring of LCMs, a radially escaped configuration of LCMs is observed. Vertically aligned LCMs, a preferred configuration for actuation, are only observed when using a PDMS mold with planar anchoring. Guided by the numerical modeling, we coat the PDMS mold with a thin layer of poly(2-hydroxyethyl methacrylate) (PHEMA), leading to planar anchoring of LCM. Confirmed by polarized optical microscopy, we observe monodomains of vertically aligned LCMs within the mold, in agreement with modeling. Finally, after curing and peeling off the mold, the resulting NLCE micropillars showed a relatively large and reversible radial strain (~30%) when heated above the nematic to isotropic transition temperature.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Advanced Infusion Techniques with 3-D Printed Tooling

The manufacturing of tooling for large, contoured surfaces for fiber-layup applications requires significant effort to understand the geometry and then to subtractively manufacture the tool. Traditional methods for the auto industry use clay that is hand sculpted. In the marine pleasure craft industry, the exterior of the model is formed from a foam lay-up that is either hand cut or machined to create smooth lines. Engineers and researchers at Oak Ridge National Laboratory s Manufacturing Demonstration Facility (ORNL MDF) collaborated with Magnum Venus Products (MVP) in the development of a process for reproducing legacy whitewater adventure craft via digital scanning and large scale 3-D printed layup molds. The process entailed 3D scanning a legacy canoe form, converting that form to a CAD model, additively manufacturing (3-D Print) the mold tool, and subtractively finishing the mold s transfer surfaces. Future work will include applying a gelcoat to the mold transfer surface and infusing using vacuum assisted resin transfer molding, or VARTM principles, to create a watertight vessel. The outlined steps were performed on a specific canoe geometry found by MVP s principal participant. The intent of utilizing this geometry is to develop an energy efficient and marketable process for replicating complex shapes, specifically focusing on this particular watercraft, and provide a finished product for demonstration to the composites industry. The culminating part produced through this agreement has been slated for public presentation and potential demonstration at the 2016 CAMX (Composites and Advanced Materials eXpo) exposition in Anaheim, CA. Phase I of this collaborative research and development agreement (MDF-15-68) was conducted under CRADA NFE-15-05575 and was initiated on May 7, 2015, with an introduction to the MVP product line, and concluded in March of 2016 with the printing of and processing of a canoe mold. The project partner Magnum Venous Products (MVP) is a small business. Phase II as discussed herein is under consideration by MVP as of this writing. Overall, it is anticipated that developing this process for manufacturing tooling for complex contoured surfaces has applicability to naval and other watercraft as well as bathrooms and large trucks.

42 ENGINEERING↗

Process Development and Optimization of a Direct Cast U-6Nb 250 mm Hemispherical Component

Direct Casting is the process of casting a near-net shape part of U-6wt%Nb in a multi-zone VIM furnace for subsequent heat treatment and machining in to a final component. This report describes work to further develop a sound technical basis and best practices for mold design and process parameters for the Direct Casting of U-6Nb components with a hemispherical geometry. Specifically, process parameters and mold design are examined in detail for producing a 250 mm diameter hemisphere component. The goal is to efficiently produce a sound casting with a minimum of microporosity and uniform niobium composition. Prior work had tried unsuccessfully to cast this shape in a large single-coil vacuum induction melting (VIM) furnace. These castings had unacceptable levels microporosity and niobium segregation. In this work, this same part was cast in a multi-zone VIM and a sound casting was obtained. Beyond simply casting a sound part, this work aimed to optimize the hot-top design, metal pouring temperature, and mold pole temperature. Sound castings where produced using both a tapered and step hot-top designs. There were slightly lower porosity levels and about 5% better metal usage with the step hot-top so that design slightly better. With the current mold design, which uses a funnel and filter arrangement, there a large amount of superheat loss in the funnel/filter during mold filling. This temperature loss, and the apparent variability in the filling behavior, lead to casting defects in the pole region of several of the castings. The variability and defects were overcome by moving to a higher mold pole temperature (850°C) and a higher metal pour temperature (1500°C). For future work it is believed that a no-funnel design, with the filter integral to the crucible, will be a better and more robust strategy.

42 ENGINEERING↗

Low pressure process for continuous fiber reinforced polyamic acid resin matrix composite laminates

A low pressure processor was developed for preparing a well-consolidated polyimide composite laminate. Prepreg plies were formed from unidirectional fibers and a polyamic acid resin solution. Molding stops were placed at the sides of a matched metal die mold. The prepreg plies were cut shorter than the length of the mold in the in-plane lateral direction and were stacked between the molding stops to a height which was higher than the molding stops. The plies were then compressed to the height of the stops and heated to allow the volatiles to escape and to start the imidization reaction. After removing the stops from the mold, the heat was increased and 0 - 500 psi was applied to complete the imidization reaction. The heat and pressure were further increased to form a consolidated polyimide composite laminate.

Druyun, Darleen A.↗