Multicomponent bulk metal nitride (Nb1/3Ta1/3Ti1/3)N1−δ synthesis via reaction flash sintering and characterizations

In this research, near fully dense single phase bulk multicomponent transition metal nitride (Nb_1/3Ta_1/3Ti_1/3)N_1−δ has been successfully synthesized from mixed commercial powders of NbN, TaN and TiN via reaction flash sintering technique. This was performed with an applied pressure of ~ 35 MPa at 25°C under a constant DC electric field (~24-32 V/cm). The flash event, which is the abrupt increase in current (up to ~ 25.2 A/mm²) and temperature, occurred without preheating. The threshold power dissipation on the sample right before the flash is ~ 0.7 W/mm³. The formation of single phase (Nb_1/3Ta_1/3Ti_1/3)N_1−δ random solid solution and its compositional uniformity were confirmed by XRD and EDS, respectively. The effects of ball milling duration and limiting current density on phase formation were studied. Simulation based on Joule heating provides an estimate of the ultimate sample temperature of ~ 1850°C. Vickers hardness of the obtained (Nb_1/3Ta_1/3Ti_1/3)N_1−δ is 17.6 ± 0.6 GPa, which is comparable to similarly flash sintered ingredient binary nitrides of TaN and NbN. TGA in air shows that the oxidation resistance of (Nb_1/3Ta_1/3Ti_1/3)N_1−δ is better than that of TaN and NbN but inferior to TiN. The study demonstrates that reaction flash sintering can be a highly efficient technique for synthesizing bulk multicomponent ceramics for both material fundamental investigations and application development.     

Bulk modulus and thermal expansion coefficient of mechano-chemically synthesized Mg2FeH6 from high temperature and high pressure studies

Mg₂FeH₆ was synthesized by ball milling MgH₂ and Fe (2:1 molar ratio) mixture for 72 h followed by heating at 400 °C under H₂ pressure. The hydride formation, its structure and homogeneity were investigated by scanning electron microscopy, X-ray diffraction, transmission electron microscopy and Raman spectroscopy. High pressure in situ synchrotron X-ray diffraction and Vienna ab initio simulation were used to determine bulk modulus of the sample. The bulk modulus of Mg₂FeH₆ was found to be 75.4(4) GPa by optimized experiment and 76.3 GPa by theoretical simulation. From high temperature in situ X-ray diffraction study the volumetric thermal expansion coefficient of Mg₂FeH₆ was found to be α_v = 5.85(3) × 10⁻⁵ + 7.47(7) × 10⁻⁸ (T − T_o)/°C. Decomposition of Mg₂FeH₆ was observed at 425 °C and the decomposition products were Mg, Fe and H₂.     

A Discontinuous Galerkin Method for Three-Dimensional Shallow Water Equations

We describe the application of a local discontinuous Galerkin method to the numerical solution of the three-dimensional shallow water equations. The shallow water equations are used to model surface water flows where the hydrostatic pressure assumption is valid. The authors recently developed a DG\linebreak method for the depth-integrated shallow water equations. The method described here is an extension of these ideas to non-depth-integrated models. The method and its implementation are discussed, followed by numerical examples on several test problems.This revised version was published online in July 2005 with corrected volume and issue numbers.     

Synthesis and compressive behavior of Cr2GeC up to 48 GPa

M_n+1AX_n compounds have gathered huge momentum because of its exciting properties. In this paper we report the synthesis of ternary layered ceramic Cr₂GeC, a 211 M_n+1AX_n compound by hot-pressing. Scanning electron microscopy and X-ray diffraction have been employed to characterize the new synthesized phase. High-pressure compressibility of Cr₂GeC were measured using diamond anvil cell and synchrotron radiation at room temperature up to 48 GPa. No phase transformation was observed in the experimental pressure range. The bulk modulus of Cr₂GeC calculated using the Birch–Murnaghan equation of state is 169 ± 3 GPa, with K′ = 3.05 ± 0.15.     

Multifrequency imaging in the intermittent contact mode of atomic force microscopy: beyond phase imaging

The cantilever dynamics in single-frequency scanning probe microscopy (SPM) are undefined due to having only two output variables, which leads to poorly understood image contrast. To address this shortcoming, generalized phase imaging scanning probe microscopy (GP-SPM), based on broad band detection and multi-eigenmode operation, is developed and demonstrated on diamond nanoparticles with different functionalization layers. It is shown that rich information on tip-surface interactions can be acquired by separating the response amplitude, instant resonance frequency, and quality factor. The obtained data allow high-resolution imaging even in the ambient environment. By tuning the strength of tip-surface interaction, different surface functionalizations can be discerned.     

Influence of Chemical Precleaning on the Plasma Treatment Efficiency of Aluminum by RF Plasma Pencil

This paper is aimed to show the influence of initial chemical pretreatment prior to subsequent plasma activation of aluminum surfaces.The results of our study showed that the state of the topmost surface layer（i.e.the surface morphology and chemical groups）of plasma modified aluminum significantly depends on the chemical precleaning.Commonly used chemicals（isopropanol,trichlorethane,solution of Na OH in deionized water）were used as precleaning agents.The plasma treatments were done using a radio frequency driven atmospheric pressure plasma pencil developed at Masaryk University,which operates in Ar,Ar/O₂ gas mixtures.The effectiveness of the plasma treatment was estimated by the wettability measurements,showing high wettability improvement already after 0.3 s treatment.The effects of surface cleaning（hydrocarbon removal）,surface oxidation and activation（generation of OH groups）were estimated using infrared spectroscopy.The changes in the surface morphology were measured using scanning electron microscopy.Optical emission spectroscopy measurements in the near-to-surface region with temperature calculations showed that plasma itself depends on the sample precleaning procedure.     

Plasma Treatment of Aluminum Using a Surface Barrier Discharge Operated in Air and Nitrogen: Parameter Optimization and Related Effects

This paper presents the results of aluminum surface treatment by diffuse coplanar surface barrier discharge. The goals are to study the effectiveness of the plasma treatment and the dependence of its efficiency on operation parameters, such as sample-to-electrode distance, treatment time or gas atmosphere. Three types of aluminum materials (bricks, sheets and thin films) were tested to ensure the reliability of the treatment. The changes in the surface properties were characterized by the surface free energy, atomic force microscopy, attenuated total reflectance Fourier transform infrared spectroscopy (ATR FTIR) and X-ray photoelectron spec- troscopy (XPS). The influence of aging effect on the treatment was also measured and discussed.     

Evaluation of a Novel Thiol–Norbornene-Functionalized Gelatin Hydrogel for Bioprinting of Mesenchymal Stem Cells

Introduction: Three-dimensional bioprinting can be considered as an advancement of the classical tissue engineering concept. For bioprinting, cells have to be dispersed in hydrogels. Recently, a novel semi-synthetic thiolene hydrogel system based on norbornene-functionalized gelatin (GelNB) and thiolated gelatin (GelS) was described that resulted in the photoclick hydrogel GelNB/GelS. In this study, we evaluated the printability and biocompatibility of this hydrogel system towards adipose-tissue-derived mesenchymal stem cells (ASCs). Methods: GelNB/GelS was synthesized with three different crosslinking densities (low, medium and high), resulting in different mechanical properties with moduli of elasticity between 206 Pa and 1383 Pa. These hydrogels were tested for their biocompatibility towards ASCs in terms of their viability, proliferation and differentiation. The extrusion-based bioprinting of ASCs in GelNB/GelS-high was performed to manufacture three-dimensional cubic constructs. Results: All three hydrogels supported the viability, proliferation and chondrogenic differentiation of ASCs to a similar extent. The adipogenic differentiation of ASCs was better supported by the softer hydrogel (GelNB/GelS-low), whereas the osteogenic differentiation was more pronounced in the harder hydrogel (GelNB/GelS-high), indicating that the differentiation fate of ASCs can be influenced via the adaption of the mechanical properties of the GelNB/GelS system. After the ex vivo chondrogenic differentiation and subcutaneous implantation of the bioprinted construct into immunocompromised mice, the production of negatively charged sulfated proteoglycans could be observed with only minimal inflammatory signs in the implanted material. Conclusions: Our results indicate that the GelNB/GelS hydrogels are very well suited for the bioprinting of ASCs and may represent attractive hydrogels for subsequent in vivo tissue engineering applications.     

A modified method for production of hydrogen from methane

The steam–methane‐reformation (SMR) reaction has been modified by including sodium hydroxide in the reaction. It is found that the reaction: 2NaOH+CH₄+H₂O = Na₂CO₃+4H₂ takes place at much lower temperatures (300–600°C) than the SMR reaction (800–1200°C). The reaction rate is enhanced with a nickel catalyst. We have studied the effect of variously ball‐milled nickel on the reaction rate and determined the optimum particle size of the catalyst. Best results were achieved by grinding the catalyst for 2 h. Prolonged ball milling caused the nickel platelets to coalesce and grow in size decreasing the reaction rate. Copyright © 2011 John Wiley & Sons, Ltd.