A thermal perspective of flash sintering: The effect of AC current ramp rate on microstructure evolution

In flash sintering experiments, the thermal history of the sample is key to understanding the mechanisms underlying densification rate and final properties. By combining robust temperature measurements with current-ramp-rate control, this study examined the effects of the thermal profile on the flash sintering of yttria-stabilized zirconia, with experiments ranging from a few seconds to several hours. The final density was maximized at slower heating rates, although processes slower than a certain threshold led to grain growth. The amount of grain growth observed was comparable to a similar conventional thermal process. The bulk electrical conductivity correlated with the maximum temperature and cooling rate. The only property that exhibited behavior that could not be attributed to solely the thermal profile was the grain boundary conductivity, which was consistently higher than conventional in flash sintered samples. These results suggest that, during flash sintering, athermal electric field effects are relegated to the grain boundary.     

Influence of SiC microstructure on its corrosion behavior in molten FLiNaK salt

The influence of the microstructure on the corrosion rate of three monolithic SiC samples in FLiNaK salt at 900 °C for 250 h was studied. The SiC samples, labeled as SiC-1, SiC-2, and SiC-3, had corrosion rates of 0.137, 0.020, and 0.043 mg/cm²h, respectively. Compared with grain size and the presence of special grain boundaries (i.e., Σ3), the content of high-angle grain boundaries (HAGBs) appeared to have the strongest influence on the corrosion rate of SiC in FLiNaK salt, since the corrosion rate increased six times as the concentration of high-angle grain boundaries increased from 19 to 32% for SiC-2 and SiC-1, respectively. These results stress the importance of controlling the content of HAGBs during the production process of SiC.     

Modeling for the electromagnetic properties and EMI shielding of Cf/mullite composites in the gigahertz range

The electromagnetic properties and EMI shielding effectiveness of C_f/mullite composites via the spark plasma sintering were intensively investigated in the gigahertz range (8.2–12.4 GHz). Experimental results have revealed excellent electromagnetic properties and a high value of EMI shielding effectiveness (nearly 40 dB) for C_f/mullite composites with 1.65 vol% carbon fillers at thickness of 2 mm. We quantitatively characterize the contributions of microstructural features to overall EMI shielding effectiveness using a micromechanics-based homogenization model. The EMI shielding effectiveness enhances with respect to the C_f volume concentration before the threshold. The increasing trend of EMI shielding effectiveness with respect to AC (alternating current) frequency can be attributed to enhanced conductivity at high gigahertz range. It is demonstrated that filler and frequency dependent interface effects are essential to obtain excellent electromagnetic properties of C_f/mullite composite. The present research can provide guidances for the design of ceramic-based composites applied in high-temperature EMI shielding devices.     

Micro-structural study of Yaozhou celadons (Tang to Yuan Dynasty): probing crystalline and glassy phases

The Yaozhou kiln complex is a representative production center of ancient northern China, famous for the celadon production. In this work, bubbles, glassy matrix and residual crystals of celadon glazes produced from the Tang to Yuan Dynasty were analyzed by using optical microscopy, Raman spectroscopy and scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS). The results revealed that the Song, Jin and Yuan productions present bigger bubble and higher area ratios of the Si-O bending over stretching modes than the Tang and Wudai productions. This is consistent with firings at higher temperatures during Song, Jin and Yuan Dynasties. It is also in agreement with the historical studies, which revealed the change from wood-firing to coal-firing during Song Dynasty. The observation of calcium phosphate in Yaozhou productions indicated that the glaze ash had been used. No iron-based particle was identified by Raman spectroscopy in the glazes of all periods. The green color is certainly due to iron ion dispersed in the glassy matrix. Our study also confirmed no significant change in glaze raw materials used for Yaozhou productions from Tang to Yuan Dynasty.     

Irradiation-induced microstructure damage in He-irradiated 3C-SiC at 1000℃

The effect of the high-temperature helium irradiation on microstructural evolution of 3C-SiC was investigated by the combination of Raman spectroscopy, conventional transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). 3C-SiC wafers were irradiated with 130 keV He⁺ ions at fluences of 2 × 10¹⁶ He⁺/cm², 4 × 10¹⁶ He⁺/cm² and 2 × 10¹⁷ He⁺/cm² at 1000℃. Helium bubbles, dislocation loops, and their interaction with the stacking faults were focused on and characterized by TEM. Helium bubbles preferentially nucleate and grow on stacking faults. Bubble links on the (100) plane in 3C-SiC are formed. In addition, stacking faults can effectively trap irradiation-induced lattice defects to enhance their recovery. The type of irradiation-induced lattice defects and elemental distribution are also investigated. The research results are valuable for the 3C-SiC used in the advanced nuclear energy systems.     

Influence of ZrB2 hard ceramic reinforcement on mechanical and wear properties of aluminum

In this work, the effect of ZrB₂ (0, 5, 10 and 20?vol%) ceramic reinforcement on densification, structure, and properties of mechanically alloyed Al was investigated. The milling of Al-ZrB₂ powder compositions resulted in formation of agglomerates with varied size. In particular, the size of agglomerates was reduced considerably with increased addition of ZrB₂ to Al. Interestingly, the densification of hot pressed Al increased from 96.06% to 99.22% with ZrB₂ addition. The reduction of agglomerates size was attributed to the enhanced densification of Al-ZrB₂ composites. Pure Al showed relatively low hardness (0.94?GPa) and it was improved to 1.78?GPa with the addition of 20?vol% ZrB₂. The mechanical properties have significantly been improved for Al-ZrB₂ composites. Especially Al - 20?vol% ZrB₂ possessed a very high yield strength (529?MPa), compressive strength (630?MPa) and compressive strain of 19.25%. Realization of such a good combination of mechanical properties is the highest ever reported for Al composites so far in the literature. The coefficient of friction (COF) of Al-ZrB₂ varied narrowly between 0.33 and 0.40 after dry sliding wear against steel disc. The wear rate of Al-ZrB₂ composites was within mild wear regime and varied between 98.88?×?10^?6 and 34.66?×?10^?6 mm³/Nm. Among all the compositions, Al - 20?vol% ZrB₂ composite exhibited the lowest wear rate and high wear rate was noted for pure Al. Mild abrasion, tribo-oxidation, third body wear (wear debris) and delamination were the major material removal mechanisms for Al-ZrB₂ composites. Overall the hardness, strength and wear resistance of Al - 20?vol% ZrB₂ composite was improved by 84.3%, 84.3% and 64.2%, respectively when compared to pure Al.     

In-situ TEM observation of structural changes in nano-crystalline CoCrCuFeNi multicomponent high-entropy alloy (HEA) under fast electron irradiation by high voltage electron microscopy (HVEM)

The structural changes induced in a CoCrCuFeNi multicomponent nano-crystalline high-entropy alloy (HEA) under fast electron irradiation were investigated by in-situ transmission electron microscopy (TEM) using a high voltage electron microscope (HVEM). A fine-grained face centered cubic (fcc) single phase was obtained in the sputtered specimens. The fcc solid solution showed high phase stability against irradiation over a wide temperature range from 298 to 773 K, and remained as the main constituent phase even when the samples were irradiated up to 40 displacement per atom (dpa). Moreover, the irradiation did not seem to induce grain coarsening. This is the first report on the irradiation damage in 5-component HEA under MeV electron irradiation.     

Effect of Ba nonstoichiometry on the phase composition,microstructure, chemical stability and electrical conductivity of BaxCe0.7Zr0.1Y0.1Yb0.1O3−δ (0.9≤x≤1.1) proton conductors

The perovskite proton conductors Ba_xCe_0.7Zr_0.1Y_0.1Yb_0.1O_3−δ (x=0.9, 0.94, 0.98, 1.0, 1.03, 1.06, and 1.1) have been successfully prepared by the conventional solid state reaction route. X-ray diffraction (XRD) patterns of the samples indicate that Ba_xCe_0.7Zr_0.1Y_0.1Yb_0.1O_3−δ (x≥1.0) samples possess a single phase orthorhombic structure, but a secondary phase (Y,Ce)O_2−δ exists in Ba_xCe_0.7Zr_0.1Y_0.1Yb_0.1O_3−δ (x<1.0) samples. SEM photographs show that the grain size of Ba_xCe_0.7Zr_0.1Y_0.1Yb_0.1O_3−δ increases and the porosity decreases with Ba²⁺ content varying from x=0.9 to 1.1. Because of ZnO addition as sintering aid, the sintering temperature of the samples reduces from 1550 °C to 1250 °C. The chemical stability of the samples against CO₂ decreases with the increase in Ba content from x=0.9 to 1.1. All the samples show a excellent stability against water vapor at 850 °C. The conductivities of the samples increase and the activation energies reduce with the increase in Ba content. The present results suggest that it is very important to control the stoichiometry of cations to obtain desired perovskite type high temperature proton conductors.     

Preparation and characterization of mullite whisker reinforced ceramics made from coal fly ash

Ceramics with mullite whiskers were prepared from coal fly ash and Al₂O₃ raw materials, with AlF₃ used as an additive. The phase structures and microstructures of the ceramics were identified via X-ray diffraction and scanning electron microscopy, respectively. The results show that pickling of coal fly ash is an effective method for enhancing the flexural strength of ceramics. Sintering temperature and AlF₃ addition were also key factors influencing the creation of ideal ceramics. The ceramic made from pickled coal fly ash, 6?wt% AlF₃, and sintered at 1200?°C, exhibited the highest flexural strength of 59.1?MPa, and had a bulk density of 1.32?g/cm³ and porosity of 26.8%. The results show that ceramic materials made under these conditions are ideal candidates for manufacturing ceramic proppants for the exploitation of unconventional oil and gas resources.     

Alloying behavior and novel properties of CoCrFeNiMn high-entropy alloy fabricated by mechanical alloying and spark plasma sintering

An equiatomic CoCrFeNiMn high-entropy alloy was synthesized by mechanical alloying (MA) and spark plasma sintering (SPS). During MA, a solid solution with refined microstructure of 10 nm which consists of a FCC phase and a BCC phase was formed. After SPS consolidation, only one FCC phase can be detected in the HEA bulks. The as-sintered bulks exhibit high compressive strength of 1987 MPa. An interesting magnetic transition associated with the structure coarsening and phase transformation was observed during SPS process.