Selective laser melting of alumina: A single track study

Ceramics-based additive manufacturing is a complex process and the solidification mechanism and microstructural evolution are currently not fully understood. In this work, Al₂O₃ single tracks were formed using a customised selective laser melting (SLM) system equipped with a high power diode laser. The effects of laser energy density (LED) on geometry, microstructure and micro-mechanical properties of Al₂O₃ tracks were investigated. To better understand the solidification mechanism, a transient three-dimensional thermal model was developed for predicting the thermal behaviour of the melt pool. The results indicated the use of high LED gave rise to decreased viscosity and surface tension of the molten alumina and led to localized melting of the substrate. Both, in turn, enabled the formation of a continuous solidified track. The solidified tracks were primarily composed of columnar dendrite. When relatively high LED (≥?25.7?kJ/m) was applied, equiaxed dendrite appeared along the central line near the track surface. The size of dendritic grains decreased with the decreased LED, attributed to the increased cooling rate at solidification interface. The micro-hardness of the solidified track was found to be inversely proportional to the grain size owning to grain boundary strengthening effect.     

Comparative investigation of microstructure,mechanical properties and strengthening mechanisms of Al-12Si/TiB2 fabricated by selective laser melting and hot pressing

Near-fully dense Al-12Si matrix composites reinforced with TiB₂ ceramic particles (2?wt%) were successfully fabricated by selective laser melting (SLM) and hot pressing (HP) of powder mixtures. TiB₂ ceramic particles are homogeneously distributed in the Al-12Si matrix at the micrometer-scale owing to a very good wetting between molten Al-12Si alloy and TiB₂ ceramic. The microstructural analysis of the as-fabricated SLM samples show the formation of a supersaturated α-Al phase and the decrease of free residual Si with respect to the hot-pressed ones. Both composites exhibit a fine microstructure with a grain size of ~?5.1?µm and ~?5.8?µm for SLM- and HP-fabricated samples with addition of TiB₂ ceramic particles. The SLM Al-12Si/TiB₂ composite exhibits significantly improved microhardness (~?142?±?6.0 HV_0.05) and yield strength (~247?±?4.0?MPa) compared to the corresponding HP one. Fine cell morphology and nanostructured dispersion strengthening are responsible for the improved mechanical strength of the Al-12Si/TiB₂ composite processed by SLM.     

Robust SiO2 gate dielectric thin films prepared through plasma-enhanced atomic layer deposition involving di-sopropylamino silane (DIPAS) and oxygen plasma: Application to amorphous oxide thin film transistors

DIPAS (di-isopropylamino silane, H₃Si[N(C₃H₇)₂]) and O₂ plasma were employed, using plasma-enhanced atomic layer deposition (PEALD), to deposit silicon oxide to function as the gate dielectric at low temperature, i.e., below 200 °C. The superior amorphous SiO₂ thin films were deposited through the self-limiting reactions of atomic layer deposition with a deposition rate of 0.135 nm/cycle between 125 and 200 °C. PEALD-based SiO₂ thin layer films were applied to amorphous oxide thin film transistors constructed from amorphous In-Ga-Zn-O (IGZO) oxide layers, which functioned as channel layers in the bottom-gated thin film transistor (TFT) structure, with the aim of fabricating transparent electronics. The SiO₂ gate dielectric exhibited the highest TFT performance through the fabrication of heavily doped n-type Si substrates, with a saturation mobility of 16.42 cm²/V·s, threshold voltage of 2.95 V and large on/off current ratio of 3.69 × 10⁸. Ultimately, the highly doped Si was combined with the ALD-based SiO₂ gate dielectric layers, leading to a saturation mobility of 16.42 cm²/V·s, threshold voltage of 2.95 V, S-slope of 0.1944, and on/off current ratio of 3.69 × 10⁸. Semi-transparent and transparent TFTs were fabricated and provided saturation mobilities of 22.18 and 24.29 cm²/V·s, threshold voltages of 4.18 and 2.17 V, S-slopes of 0.1944 and 0.1945, and on/off current ratios of 9.63 × 10⁸ and 1.03 × 10⁷, respectively.     

An attempt to predict the mechanism of Mo-Ni-O powders electrodeposition from the results of their TEM analysis

The Mo-Ni-O powders were electrodeposited from ammonium sulfate containing electrolytes with different Mo/Ni ion concentration ratios. The phase composition of these powders was investigated using TEM, EDS and XRD analysis. The TEM analysis showed that two types of particles were present in the powders: amorphous and crystalline. For crystalline particles it was found that two phases, MoO₃ and MoNi₄ prevail in all powders, while the NiO phase was detected in the powder electrodeposited at Mo/Ni = 0.3/1. These findings are in good agreement with our previous results where MoO₃, MoNi₄ and NiMoO₄ phases were detected in the recrystallized Mo-Ni-O powders. In this work we discovered that the NiMoO₄ phase was formed by solid state reaction between NiO and MoO₃ at elevated temperature.     

Preform impregnation to optimize the properties and microstructure of RB-SiC prepared with laser sintering and reactive melt infiltration

Indirect selective laser sintering (SLS) was combined with reactive melt infiltration (RMI) to fabricate RB-SiC, and the effects of preform impregnation with different carbon source on the carbonized sample and final RB-SiC were investigated. Results show that the impregnation treatment led to increased bulk density and mechanical strength of samples at all stages. The pore size dwindled and the porosity decreased significantly for the carbonized sample, and the content of Si reduced for the final RB-SiC. The impregnation with PF resin containing 30 % nano carbon black (PFnanoC) seems more promising for the comprehensive properties improvement, the final RB-SiC had a relatively fewer amount of residual pore and carbon and showed superior mechanical properties compared with those of sample impregnated with only PF resin. Kinetics analysis indicates a slower pore-clogging rate under the PFnanoC impregnation condition, which avoided or hindered a too-early infiltration cease during the RMI process.     

Direct laser additive manufacturing of high performance oxide ceramics: A state-of-the-art review

The implementation of additive manufacturing for ceramics is more challenging than for other material classes, since most of the shaping methods require polymer binder. Laser additive manufacturing (LAM) could offer a new binder-free consolidation route, since it is capable of processing ceramics in a direct manner without post-processing. However, laser processing of ceramics, especially high performance oxide ceramics, is limited by low thermal shock resistance, weak densification and low light absorptance at room temperature; particularly in the visible or near-infrared range. An extensive review focusing only on LAM (powder bed fusion – laser beam and directed energy deposition) of high performance oxide ceramics is currently lacking. This state-of-the-art review gives a detailed summary and critical analysis about process technologies, part properties, open challenges and process monitoring in the field of oxide ceramics. Improvements in accuracy and mechanical strength are proposed that could open LAM of oxide ceramics to new fields.     

Fabrication and microstructure development of Yb:YAG transparent ceramics from co-precipitated powders without additives

Sintering additives are generally considered to be important for improving densification in fabrication of transparent ceramics. However, the sintering aids as impurities doped in the laser materials would decrease the laser output power and produce additional heat during laser operation. In this work, Yb:YAG ceramics were vacuum-sintered without additives at different temperatures for various soaking time through using ball-milled powders synthesized by co-precipitation route. The densification behavior and grain growth kinetics of Yb:YAG ceramics were systematically investigated through densification curves and microstructural characterizations. It was determined that the densification in the 1500°C-1600°C temperature range was controlled by a grain-boundary diffusion. It is revealed that the volume diffusion is the main mechanism controlling the grain growth between 1600°C and 1750°C. Although SiO₂ additives can promote densification during low-temperature sintering, the optical transmittance of Yb:YAG ceramic with no additives, sintered at 1800°C for 15 hours, reaches a maximum of 83.4% at 1064 nm, very close to the measured transmittance value of Yb:YAG single crystal. The optical attenuation loss was measured at 1064 nm in Yb:YAG transparent ceramic, to be 0.0035 cm⁻¹, a value close to that observed for single crystals.     

Hot-pressing and post-HIP treatment of Fe2+:ZnS transparent ceramics from co-precipitated powders

Transparent Fe²⁺:ZnS polycrystals are 3–5 μm mid-IR laser gain materials with great importance. In this paper, a novel route combining wet-chemical co-precipitation, hot-pressed sintering and post hot isostatic pressing (HIP) treatment was proposed for Fe²⁺:ZnS transparent ceramics. Fe²⁺:ZnS powders were synthesized successfully by the wet-chemical co-precipitation method, which was suitable for particle size and morphology controlling and then ceramics consolidation. Transparent Fe²⁺:ZnS ceramics with comparatively high optical quality were successfully fabricated by two step sintering method combining hot pressing and post-HIP treatment. This approach is a promising candidate for fabricating Fe²⁺:ZnS ceramics with large size, low cost, short cycle, and flexible concentration distribution design.     

Evaluation of bonding effectiveness of a self-etch and an etch-and-rinse adhesive resin to un-treated and Er:Yag laser treated dentin using mini-interfacial fracture toughness test

The aim of current study was to assess interfacial bonding effectiveness of self-etch and etch-and-rinse dental adhesives to untreated and Er:YAG laser-treated dentine using mini-interfacial fracture toughness (mini-iFT) test. 32 selected non-carious third molars were divided into two groups: untreated and Er:YAG laser treated. The laser-treated specimens were subjected to Er:YAG laser with energy density of 25.82?J/cm². Both groups were further assigned to two groups based on adhesive systems: self-etch and etch-and-rinse. The teeth were sectioned perpendicular to the adhesive/dentine interface to obtain 1.5?×?2?mm wide longitudinal rectangular sections. A single notch then was prepared at the adhesive-dentine interface. The mini-iFT test was done via a 4-point bend testing until failure and the KIC was calculated. All specimens were observed using a, scanning electron microscope (SEM). The data were analysed using two-way analysis of variance (ANOVA) at a significant level of 0.05. Weibull parameters including Weibull modulus and characteristic strength also were calculated for each experimental group. Two-way ANOVA showed both variables (the type of adhesive system and laser treatment) significantly influenced the mini-iFT values of specimens (p?≤?0.001). The self-etch and laser-treated group showed lower mini-iFT than the etch-and-rinse and untreated samples. SEM observations revealed that the fracture region was located at the adhesive-dentine interface in most of the specimens. The Er:YAG laser treatment may adversely affects the bonding effectiveness of the dentine/adhesive interface. The mini-iFT method can be used as a discriminative and valid method for the evaluation of bonding effectiveness at the adhesive-dentine interface.     

生物柴油副产物粗甘油催化氧化脱水制备丙烯酸

用生物柴油副产物粗甘油催化氧化脱水制丙烯酸,该过程耦合了甘油脱水制丙烯醛和丙烯醛选择性氧化制备丙烯酸两步反应。结果表明,在甘油脱水反应中,使用Cs3PW12O40, P-ZSM-5和Co0.5H2PO4/SiO2等固体酸催化剂,可得到较高的丙烯醛收率(最高86.9%)。利用上述催化剂和MoVW基氧化催化剂,在脱水/氧化双催化剂床层构型反应器中,以甘油为原料合成丙烯酸的收率达50%~80%,直接加入粗甘油可获得相似的丙烯酸收率。     

From Metal‐Metal Bonding to Supra‐Metal‐Metal Bonding Directed Self‐Assembly: Supramolecular Architectures of Group 10 and 11 Metals with Ligands from Mono‐ to Poly‐Pyrazoles

The supramolecular architectures of pyrazole ligands with polynuclear metal centers have established a wide variety of constructing motifs. This review focuses on the metal‐metal bonding and Supra‐Metal‐Metal Bonding directed self‐assembly of supramolecular architectures of pyrazole ligands ranging from simple mono‐pyrazoles and derivatives to bipyrazoles and polypyrazoles with group 10 and 11 elements. The utility of the constructing motifs (μ‐pyrazolato‐N,N′)₂ doubly‐bridged dimetal corners in the metal‐metal‐bonding directed self‐assembly approaches with spontaneous deprotonation from bipyrazole to tripyrazole and tetrapyrazolyl calix[4]arene ligands, metallomacrocyclic and cage‐like complexes have been synthesized. The proton switching programmable self‐assembly strategy using pyrazole‐based bifunctional ligands has been developed by Yu. They have obtained organic homo‐ or hetero‐metallic supramolecular complexes from macrocycles, cages, to one dimensional polymers.     

An investigation of atomic force microscopy,surface topography and adhesion of luting cements to zirconia: effect of silica coating,zirconia primer and laser

This study evaluated the effect various surface conditioning methods on the surface topography and adhesion of luting cements to zirconia. Zirconia blocks (N?=?25) were randomly assigned to five groups according to the surface conditioning methods: (a) No conditioning, control (CON), (b) tribochemical silica coating (TSC), (c) MDP-based zirconia primer (ZRP), (d) coating with nano aluminum nitride (ALN) (e) etching with Er: YAG laser (LAS). The conditioned zirconia blocks were further divided into five subgroups to receive the luting cements: (a) MDP-based resin cement (Panavia F2.0) (PAN), (b) 4-META-based cement (Super Bond) (SUB), (c) UDMA-based (GCem) (GCE), (d) bis-GMA based (Bifix QM) (BIF) and (e) polycarboxylate cement (Poly-F) (POL). Cements were applied in polyethylene moulds (diameter: 3?mm; height: 2?mm). The bonded specimens were first thermocycled for 5500 cycles (5–55?°C) and then adhesive interface was loaded under shear (0.5?mm/min). The data (MPa) were analyzed using 2-way ANOVA, Tukey’s and Bonneferroni tests (alpha?=?0.05). Regardless of the cement type, TSC resulted in significantly higher bond strength (p???0.05) (13.3?±?4.35–25.3?±?6.3) compared to other conditioning methods (2.96?±?1.5–5.4?±?5.47). Regardless of the surface conditioning method, no significant difference was found between MDP, 4-META and UDMA based cements (p?>?0.05) being significantly higher than those of bis-GMA and polycarboxylate cements (p???0.05). Failure types were frequently adhesive in all groups. Tribochemical silica coating provided superior bond results compared to other conditioning methods tested on zirconia especially in conjunction with UDMA- and 4-META-based resin cements.     

Alkali deactivation of high-dust SCR catalysts used for NOx reduction exposed to flue gas from 100 MW-scale biofuel and peat fired boilers: Influence of flue gas composition

Deactivation of vanadium–titanium deNO_x SCR (selective catalytic reduction) catalysts in high-dust position have been investigated in three 100 MW-scale boilers during biofuel and peat combustion. The deactivation of the catalyst samples has been correlated to the corresponding flue gas composition in the boilers. Too investigate the effect on catalyst deactivation a sulphate-containing additive was sprayed into one of the furnaces. Increased alkali content on the SCR catalyst samples decreased the catalytic deNO_x activity. The study has shown a linear correlation between exposure time in the boilers and alkali concentration (mainly potassium) on the samples. The results imply that mainly alkali in ultra fine particles (<100 nm) in the flue gas increased the alkali accumulation on the catalyst samples. Low correlation was found between particles larger than 100 nm and the catalyst deactivation. It was not possible to decrease the deactivation of the catalyst samples by the sulphate-containing additive. Although the additive had an effect in sulphating potassium chloride to potassium sulphate, it did not decrease the amount of potassium in ultra fine particles or the deactivation of the catalyst samples.