Densification mechanism and microstructure characteristics of nano- and micro- crystalline alumina by high-pressure and low temperature sintering

Fully dense ceramics with retarded grain growth can be attained effectively at relatively low temperatures using a high-pressure sintering method. However, there is a paucity of in-depth research on the densification mechanism, grain growth process, grain boundary characterization, and residual stress. Using a strong, reliable die made from a carbon-fiber-reinforced carbon (C_f/C) composite for spark plasma sintering, two kinds of commercially pure α-Al₂O₃ powders, with average particle sizes of 220 nm and 3 μm, were sintered at relatively low temperatures and under high pressures of up to 200 MPa. The sintering densification temperature and the starting threshold temperature of grain growth (T_sg) were determined by the applied pressure and the surface energy relative to grain size, as they were both observed to increase with grain size and to decrease with applied pressure. Densification with limited grain coarsening occurred under an applied pressure of 200 MPa at 1050 °C for the 220 nm Al₂O₃ powder and 1400 °C for the 3 μm Al₂O₃ powder. The grain boundary energy, residual stress, and dislocation density of the ceramics sintered under high pressure and low temperature were higher than those of the samples sintered without additional pressure. Plastic deformation occurring at the contact area of the adjacent particles was proved to be the dominant mechanism for sintering under high pressure, and a mathematical model based on the plasticity mechanics and close packing of equal spheres was established. Based on the mathematical model, the predicted relative density of an Al₂O₃ compact can reach ～80 % via the plastic deformation mechanism, which fits well with experimental observations. The densification kinetics were investigated from the sintering parameters, i.e., the holding temperature, dwell time, and applied pressure. Diffusion, grain boundary sliding, and dislocation motion were assistant mechanisms in the final stage of sintering, as indicated by the stress exponent and the microstructural evolution. During the sintering of the 220 nm alumina at 1125 °C and 100 MPa, the deformation tends to increase defects and vacancies generation, both of which accelerate lattice diffusion and thus enhance grain growth.     

Synthesis and slurry spray coating of barium strontium alumino silicate on SiC substrate

Barium strontium alumino silicate (BSAS); (Ba_0.6Sr_0.4Al₂Si₂O₈) was synthesized through solid state reaction between BaCO₃, SrCO₃, Al₂O₃ and SiO₂ subjected to wet milling in isopropanol for about 24 h. The sequence of the solid state reaction was studied by subjecting to DG/DTG from room temperature to 1550 °C. The crystallographic phase evolution was confirmed by X-ray diffraction of the powders calcined in the range 1000 to 1300 °C for 2 h. The monoclinic celsian phase obtained at 1300 °C, pelletized through uniaxial pressing was sinterable to 67 to 78% density in the temperature range of 1300 to 1500 °C. The density improved to 75 to 94% after ball milling for 76 h, while ZrO₂ addition further improved the density by 2%. The celcian phase of BSAS was dispersed in isopropyl alcohol, milled for about 24 h and spray coated on to plain SiC and mullite precoated SiC substrates. Sintering of coated samples and characterization for weight gain/loss, microstructure, scratch test prove that mullite + BSAS coating is more effective than single layer coating of BSAS on SiC substrates.     

Spray pressure variation effect on the properties of CdS thin films for photodetector applications

Herein, we report the photosensing property of CdS thin films. CdS thin films were coated onto glass substrates via a spray pyrolysis method using different spray pressures. Prepared films were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), and optical and photoluminescence spectroscopy. XRD analysis demonstrated the growth of crystalline CdS films with crystallite sizes varying from 26 to 29 nm depending on the pressure. The SEM and EDAX analyses revealed nearly-stoichiometric CdS films with smooth surfaces and slight variation in grain morphology due to pressure changes. Optical measurements showed a direct bandgap varying from 2.37 eV to 2.42 eV due to pressure changes. A photodetector was also fabricated using the grown CdS films; the fabricated photodetector exhibited good performance depending on the spray pressure. A spray pressure of 1.5 GPa resulted in high photoresponsivity and external quantum efficiency.     

A novel approach for bulk micromachining of 4H-SiC by tool-based electrolytic plasma etching in HF-free aqueous solution

Bulk micromachining of single-crystal SiC has been challenging due to its extreme stability both mechanically and chemically. To address this issue, a novel tool-based electrolytic plasma etching method is proposed, with which micropatterns and micro-holes are fabricated in SiC in a hydrofluoric acid-free aqueous solution with no need for masks. The material removal is the result of the combined effects of electrolytic plasma chemistry and physics. The chemistry refers to the reaction of Si with hydroxyl radical to form various SiO_x and with H to form silanes, and the reactions of C to form volatile carbon oxides or hydrocarbons, all of which are accomplished and enhanced under the electrolytic plasma atmosphere. Besides, the local high temperature of plasma thermally promotes the evaporation or dissolution of SiO₂ in NaOH solution. The tool-based electrolytic plasma etching method provides alternative approaches for the fabrication of SiC-based MEMS and devices.     

Effect of in-flight particle behavior on the morphology of flame sprayed Er2O3 splats

The morphology and microstructure of splats impact the comprehensive capability of a new coating methodology called chelate flame spraying (CFS). This study addresses the quantitative characterization of the spread morphologies of flame sprayed Er₂O₃ splats directly deposited under different spray conditions on aluminum alloy substrates with a mirror finish. The influence of the in-flight particle temperature and velocity, carrier gas type, and carrier gas ratio on the solidification mechanism of molten droplets was investigated. Image analysis methods were employed to identify single splats from the morphology observed with field-emission scanning electron microscopy (FE-SEM). In addition, Er₂O₃ films were synthesized on an Al–Mg alloy (A5052) substrate using N₂ or O₂ as the carrier gas. When O₂ was used as the carrier gas, 109-μm-thick films were deposited on the A5052 substrate. The cross-sectional porosity of the films was 3.8%. In contrast, films with 101-μm thickness were synthesized on the A5052 substrate when N₂ was used as the carrier gas. The cross-sectional porosity of these films was 13.8%. The results showed that the carrier gas type (N₂) and carrier gas ratio had a significant effect on the flattening behavior of the molten droplets. A spraying method combined with multidimensional modes is proposed to control the morphology of the splats.     

基于纸喷雾离子化衍生质谱法快速检测PM2.5中的醌污染物

醌类化合物是PM2.5中的一类有害物质。本研究建立了纸喷雾离子化衍生质谱法快速测定PM2.5中的醌类污染物。通过衍生化反应在醌化合物中引入氨基，提高醌在纸喷雾中的离子化效率。随后对衍生化试剂种类、电压、喷雾溶剂种类等反应条件进行优化。在最优实验条件下，采用内标法定量分析1,4-苯醌、甲基对苯醌、1,4-萘醌和1,4-蒽醌，4种化合物均呈现较好的线性关系，其检出限分别为4.49、20.89、0.13、0.17 ng。利用该方法分析PM2.5实际样品中的萘醌和蒽醌，均获得了较好的定性和定量结果。     

Turbulent boundary layer control with a spanwise array of DBD plasma actuators

The turbulent boundary layer control on NACA 0012 airfoil with Mach number ranging from 0.3 to 0.5 by a spanwise array of dielectric barrier discharge(DBD)plasma actuators by hot-film sensor technology is investigated.Due to temperature change mainly caused through heat produced along with plasma will lead to measurement error of shear stress measured by hot-film sensor,the correction method that takes account of the change measured by another sensor is used and works well.In order to achieve the value of shear stress change,we combine computational fluid dynamics computation with experiment to calibrate the hot-film sensor.To test the stability of the hot-film sensor,seven repeated measurements of shear stress at Ma = 0.3 are conducted and show that confidence interval of hot-film sensor measurement is from-0.18 to 0.18 Pa and the root mean square is 0.11 Pa giving a relative error 0.5％over all Mach numbers in this experiment.The research on the turbulent boundary layer control with DBD plasma actuators demonstrates that the control makes shear stress increase by about 6％over the three Mach numbers,which is thought to be reliable through comparing it with the relative error 0.5％,and the value is hardly affected by burst frequency and excitation voltage.     

Effect of suspension characteristics on the performance of thermal barrier coatings deposited by suspension plasma spray

This paper investigates the influence of suspension characteristics on microstructure and performance of suspensions plasma sprayed (SPS) thermal barrier coatings (TBCs). Five suspensions were produced using various suspension characteristics, namely, type of solvent and solid load content, and the resultant suspensions were utilized to deposit five different TBCs under identical processing conditions. The produced TBCs were evaluated for their performance i.e. thermal conductivity, thermal cyclic fatigue (TCF) and thermal shock (TS) lifetime. This experimental study revealed that the differences in the microstructure of SPS TBCs produced using varied suspensions resulted in a wide-ranging overall TBC performance. All TBCs exhibited thermal conductivity lower than 1 W/(m. K) except water-ethanol mixed suspension produced TBC. The TS lifetime was also affected to a large extent where 10 wt % solid loaded ethanol and 25 wt % solid loaded water suspensions produced TBCs exhibited the highest and the lowest lifetime, respectively. On the contrary, TCF lifetime was not as significantly affected as thermal conductivity and TS lifetime, and all ethanol suspensions showed marginally better TCF lifetime than water and ethanol-water mixed suspensions deposited TBCs.     

Effect of environmental pressure on the microstructure of YSZ thermal barrier coating via suspension plasma spraying

Suspension plasma spraying (SPS) as a potential technique to prepare thermal barrier coatings (TBCs) has been attracting more and more attention. However, most reports on SPS were carried out in the atmosphere. Given the unique features of in-flight particles and plasma jets under low pressure, the resulting coatings are expected to be different from those under atmospheric pressure. In this article, yttria-stabilized zirconia (YSZ) thermal barrier coatings were prepared using suspension plasma spraying under different environmental pressures. The results show that as the environmental pressure decreased, the column-like structural coating turned into a vertical crack segmented structure, as well as a dramatic decrease in surface roughness. More nanoparticle agglomerates were formed in the coating under lower environmental pressures. The real porosity of the coating increased with a decrease in environmental pressure.     

Investigation the effect of FeNiCoCrMo HEA addition on properties of B4C ceramic prepared by spark plasma sintering

In this study, monolithic B₄C and B₄C-based ceramics incorporating FeNiCoCrMo dual-phase (FCC and BCC) high entropy alloys (HEAs) were produced by spark plasma sintering (SPS). The effect of additives on the densification behavior, mechanical properties, microstructures, and phase evaluation of the samples were investigated. X-ray analysis confirmed the existence of FCC structured HEA and depletion of BCC structured HEA, after high-temperature reaction between B₄C-HEAs. The addition of HEAs enhanced the densification behavior by liquid phase sintering. Furthermore, hardness and fracture toughness values of the samples increased with increasing HEAs content. Fracture toughness and hardness values for all composites were higher than the monolithic B₄C. A combination of the highest density (∼99.22 %) and the best mechanical properties (32.3 GPa hardness and 4.53 MPa m^1/2 fracture toughness) was achieved with 2.00 vol.% HEA addition.