Profiling hot isostatically pressed canister–wasteform interaction for Pu-bearing zirconolite-rich wasteforms

Zirconolite-rich full ceramic wasteforms designed to immobilize Pu-bearing wastes were produced via hot isostatic pressing (HIP) using stainless steel (SS) and nickel (Ni) HIP canisters. A detailed profiling of the elemental compositions of the major and minor phases over the canister–wasteform interaction zone was performed using scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM-EDS) characterization. Bulk sample analyses from regions near the center of the HIP canister were also conducted for both samples using X-ray diffraction and SEM-EDS. The sample with the Ni HIP canister showed almost no interaction zone with only minor diffusion of Ni from the inner wall of the canister into the near-surface region of the wasteform. The sample with the SS HIP canister showed ∼100–120 μm of interaction zone dominated by high-temperature Cr diffusion from canister materials to the wasteform with the Cr predominantly incorporated into the durable zirconolite phase. We also examined, for the first time, changes to the HIP canister wall thickness caused by HIPing and demonstrated that no canister wall thinning occurred. Instead, in the areas examined, the canister wall thickness was observed to increase (up to ∼20%) due to the compression occurring during the HIP cycle. Further, only sparse formation of (Cr, Mn)-rich oxide particles were noted within the HIP canister inner wall area immediately adjacent to the ceramic material, with no evidence for reverse diffusion of ceramic materials. Though the HIP canister–wasteform interaction extends to ∼120 μm when using an SS HIP canister for the system investigated, this translates to <<1 vol.% for an industrial scale HIPed wasteform. Importantly, the HIP canister–wasteform interactions did not produce any obviously less durable phases in the wasteform or had any detrimental impact on the HIP canister properties.     

Estimates of daily oxygen consumption,carbon dioxide and methane emissions,and heat production for beef and dairy cattle using spot gas sampling

A simulation study was conducted to examine accuracy of estimating daily O₂ consumption, CO₂ and CH₄ emissions, and heat production (HP) using a spot sampling technique and to determine optimal spot sampling frequency (FQ). Data were obtained from 3 experiments where daily O₂ consumption, emissions of CO₂ and CH₄, and HP were measured using indirect calorimetry (respiration chamber or headbox system). Experiment 1 used 8 beef heifers (ad libitum feeding; gaseous exchanges measured every 30 min over 3 d in respiration chambers); Experiment 2 used 56 lactating Holstein-Friesian cows (restricted feeding; gaseous exchanges measured every 12 min over 3 d in respiration chambers); Experiment 3 used 12 lactating Jersey cows (ad libitum feeding; gaseous exchanges measured every hour for 1 d using headbox style chambers). Within experiment, averages of all measurements (FQALL) and averages of measurements selected at time points with 12, 8, 6, or 4 spot sampling FQ (i.e., sampling every 2, 3, 4, and 6 h in a 24-h cycle, respectively; FQ12, FQ8, FQ6, and FQ4, respectively) were compared. Within study a mixed model was used to compare gaseous exchanges and HP among FQALL, FQ12, FQ8, FQ6, and FQ4, and an interaction of dietary treatment by FQ was examined. A regression model was used to evaluate accuracy of spot sampling within study [i.e., FQALL (observed) vs. FQ12, FQ8, FQ6, or FQ4 (estimated)]. No interaction of diet by FQ was observed for any variables except for CH₄ production in experiment 1. No FQ effect was observed for gaseous exchanges and HP except in experiment 2 where CO₂ production was less (5,411 vs. 5,563 L/d) for FQ4 compared with FQALL, FQ12, and FQ8. A regression analysis between FQALL and each FQ within study showed that slopes and intercepts became farther from 1 and 0, respectively, for almost all variables as FQ decreased. Most variables for FQ12 and FQ8 had root mean square prediction error (RMSPE) less than 10% of the mean and concordance correlation coefficient (CCC) greater than 0.80, and RMSPE increased and CCC decreased as FQ decreased. When a regression analysis was conducted with combined data from the 3 experiments (mixed model with study as a random effect), results agreed with those from the analysis for the individual studies. Prediction errors increased and CCC decreased as FQ decreased. Generally, all the estimates from FQ12, FQ8, FQ6, and FQ4 had RMSPE less than 10% of the means and CCC greater than 0.90 except for FQ6 and FQ4 for O₂ consumption and CH₄ production. In conclusion, the spot sampling simulation with 3 indirect calorimetry experiments indicated that FQ of at least 8 samples (every 3 h in a 24-h cycle) was required to estimate daily O₂ consumption, CO₂ and CH₄ production, and HP and to detect changes in those in response to dietary treatments. This sampling FQ may be considered when using techniques that measure spot gas exchanges such as the GreenFeed and face mask systems.     

Microstructure and coloring mechanism of iron spots on bluish white porcelain from Jingdezhen of the Song Dynasty

Jingdezhen is famous for its bluish white (Qingbai) porcelains of the Song Dynasty, and those decorated with iron spots are distinctive among them. Herein, iron spots on a bluish white porcelain were investigated using a series of microscopic and spectroscopic characterizations. We found the decreasing iron content from more than 8 wt% to about 2 wt% during the glaze color transition from rusty to brown and finally into green, which built a connection on the coloring mechanism of iron-rich crystallized glaze and celadon glaze. We identified the rare ε-Fe₂O₃, a promising magnetic material, in both the dark brown crystals and the triangular crystals in the rusty area, which is its first discovery among bluish white porcelains. Based on these findings, we discussed the coloring mechanism of iron-spot decoration along with the physical form of the iron oxide crystals, indicating the partially reducing atmosphere during firing process.     

Influence of pressure and dwell time on pressure-assisted sintering of calcium cobaltite

Calcium cobaltite Ca₃Co₄O₉, abbreviated Co349, is a promising thermoelectric material for high-temperature applications in air. Its anisotropic properties can be assigned to polycrystalline parts by texturing. Tape casting and pressure-assisted sintering (PAS) are a possible future way for a cost-effective mass-production of thermoelectric generators. This study examines the influence of pressure and dwell time during PAS at 900°C of tape-cast Co349 on texture and thermoelectric properties. Tape casting aligns lentoid Co349. PAS results in a textured Co349 microstructure with the thermoelectrically favorable ab-direction perpendicular to the pressing direction. By pressure variation during sintering, the microstructure of Co349 can be tailored either toward a maximum figure of merit as required for energy harvesting or toward a maximum power factor as required for energy harvesting. Moderate pressure of 2.5 MPa results in 25% porosity and a textured microstructure with a figure of merit of 0.13 at 700°C, two times higher than the dry-pressed, pressureless-sintered reference. A pressure of 7.5 MPa leads to 94% density and a high power factor of 326 µW/mK² at 800°C, which is 11 times higher than the dry-pressed reference (30 MPa) from the same powder.     

Effect of metallurgical evolution during post-weld aging treatment on localised corrosion of resistance spot welding joints of A286 superalloy

The combined effect of resistance spot welding and precipitation hardening on the localised corrosion of A286 superalloy is studied. The specimens tested by double loop electrochemical potentiokinetic reactivation were welded in the solution treated condition, and then subjected to different precipitation hardening treatments. For both base metal and weld nugget, the maximum localised corrosion is reached when η phase is clearly observable. The fact that the localised corrosion resistance of weld nugget is different from that shown by base metal may be explained by the segregation of Ni and Ti towards the interdendritic region of weld nugget (studied by using scanning electron microscope/energy dispersive X-ray analysis).     

低活化马氏体钢热变形行为及机理型本构建模研究

利用Gleeble-3500热模拟试验机研究了低活化马氏体钢在变形温度为850～950 ℃、应变速率为0.001～1 s^-1条件下的热变形行为。建立了流变应力本构方程，并评估了该方程的预测能力。绘制了低活化马氏体钢在不同应变下的热加工图。结果表明：在较高的应变速率条件下，该材料主要发生动态回复，在较高变形温度和较低应变速率下具有明显的动态再结晶特征；本构方程的预测结果与实验结果符合良好；变形温度870～930 ℃、应变速率0.001～0.01 s^-1和变形温度920～950 ℃、应变速率0.3～1 s^-1分别是真应变为0.4和0.6下最优的热加工区域。     

Nonmechanical criteria proposed for prediction of hot tearing sensitivity in 2024 aluminum alloy

Two theoretical criteria represented by Katgerman, and Clyne and Davies for prognosticating hot tearing sensitivity were compared. Both unrefined and grain-refined samples of Al2024 alloy were solidified at various cooling rates ranging from 0.4 to 17.5 °C/s. Thermal analysis was used to detect dendrite coherency point and temperature of eutectic reaction. Curves of solid and liquid fractions were plotted based on Newtonian method to determine hot tearing susceptible areas. The experimental results show that the most susceptible zone in which hot tearing can occur in Al2024 is where Al₂CuMg intermetallic compound forms as a eutectic phase at last stage of mushy-state interval. Also, both criteria are in a good agreement with each other at high cooling rates used in direct-chill casting process while Clyne and Davies' model is more acceptable to determine hot tearing tendency from low to medium cooling rates.     

Hot corrosion studies of a salt-coated Ni-based superalloy under flowing wet air and sulfur vapor ambient

Corrosion of a salt-coated Ni-superalloy has been studied at 900°C under a wet air and sulfur vapor ambient. The corrosion thickness, after an incubation of ~60 hr, linearly increases with the corrosion time t and the onset of surface spallation occurred at t ≈ 60 hr. The corroded layer consists of a corrosion front dominated by Cr₃S₄ scales and linear precipitate structures, an inner corrosion layer dominated by Ni₃S₂ and NiO, and an outer corrosion layer dominated by Al₂O₃ networks surrounding the Ni₃S₂ and/or NiO scale structures. The corrosion mechanism is discussed based on the coexistence of H₂O, sulfur, and oxygen.     

热冲压工艺参数对22MnB5马氏体钢汽车B柱性能影响的有限元模拟

通过有限元仿真软件Autoform分析了热冲压过程中工艺参数的变化对22MnB5马氏体钢B柱起皱、回弹、减薄、马氏体量以及强度的影响。结果表明:22MnB5马氏体钢B柱热冲压最优化工艺参数为加热温度930 ℃,冷却速率80 ℃/s。该工艺参数下,热冲压过程各处均完成马氏体转变,硬度分布均匀,材料减薄率较低,热冲压成形效果好,尺寸精度高,冲压件强度均大于1400 MPa。     

热处理对挤压态Mg-6Gd-5Y-1Zn合金组织与性能的影响

通过对Mg-6Gd-5Y-1Zn(质量分数,%)合金在固溶和时效处理状态下显微组织和力学性能的研究发现,α-Mg基体、沿挤压方向分布的条状18R-LPSO相、少量的Mg₂₄(GdYZn)₅ 相以及细层片状的14H-LPSO相构成了挤压态合金的组成相。挤压态合金经固溶(T4)处理后,一部分18R-LPSO相溶入基体,并且基体中的14H-LPSO相伸长同时粗化。挤压态合金经过固溶加时效(T6)处理后,大量β′相从α-Mg基体中析出。T6态合金的室温力学性能最好,其屈服强度、抗拉强度及伸长率分别为272 MPa、406 MPa和6.1%。β′相沉淀也发生在挤压态合金的直接人工时效(T5)处理过程,但相比于T6处理,14H-LPSO相和β′相在基体中的体积分数均偏低。