New horizon in mechanochemistry—high-temperature,high-pressure mechanical synthesis in a planetary ball mill—with magnesium hydride synthesis as an example

A new route of materials synthesis, namely, high-temperature, high-pressure reactive planetary ball milling (HTPRM), is presented. HTPRM allows for the mechanosynthesis of materials at fully controlled temperatures of up to 450 °C and pressures of up to 100 bar of hydrogen. As an example of this application, a successful synthesis of magnesium hydride is presented. The synthesis was performed at controlled temperatures (room temperature (RT), 100, 150, 200, 250, 300, and 325 °C) while milling in a planetary ball mill under hydrogen pressure ($>$50 bar). Very mild milling conditions (250 rpm) were applied for a total milling time of 2 h, and a milling vial with a relatively small diameter (φ = 53 mm, V = ～0.06 dm³) was used. The effect of different temperatures on the synthesis kinetics and outcome were examined. The particle morphology, phase composition, reaction yield, and particle size were measured and analysed by scanning electron microscopy, X-ray diffraction, differential scanning calorimetry (DSC) techniques. The obtained results showed that increasing the temperature of the process significantly improved the reaction rate, which suggested the great potential of this technique for the mechanochemical synthesis of materials.     

High-resolution FIB-TEM-STEM structural characterization of grain boundaries in the high dielectric constant perovskite CaCu3Ti4O12

In this work, the grain boundaries composition of the polycrystalline CaCu₃Ti₄O₁₂ (CCTO) was investigated. A Focused Ion Beam (FIB)/lift-out technique was used to prepare site-specific thin samples of the grain boundaries interface of CCTO ceramics. Scanning transmission electron microscopy (STEM) coupled with energy dispersive X-ray spectrometry (EDXS) and Electron Energy Loss Spectroscopy (EELS) systems were used to characterize the composition and nanostructure of the grain and grain boundaries region. It is known that during conventional sintering, discontinuous grain growth occurs and a Cu-rich phase appears at grain boundaries. This Cu-rich phase may affect the final dielectric properties of CCTO but its structure and chemical composition remained unknown. For the first time, this high-resolution FIB-TEM-STEM study of CCTO interfacial region highlights the composition of the phases segregated at grain boundaries namely CuO, Cu₂O and the metastable phase Cu₃TiO_4.     

Characteristics of tiger nut milk: effects of milling

A standard method for the extraction of tiger nut milk has been introduced. It has been shown that, although milling duration improves the yield of tiger nut milk solids and its nutrient composition, there is a quantifiable loss of nutrient in the pressing residue during milk extraction. Milling duration improved the colloidal stability of the milk against creaming during 16 h of storage. A higher milling intensity resulted in the aggregation of biological polymers which resulted in colloidal destabilisation. Milling improved the lightness and stability and reduced browning rate of the tiger nut milk during storage. This report is important for the production of tiger nut milk of consistent and comparable characteristics. Milling has been introduced as a processing method for the qualitative and quantitative modulation of the properties of tiger nut milk. It is recommended to develop further strategies to improve the colloidal stability of tiger nut milk as a beverage.     

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.     

Surface modification of poly(tetrafluoroethylene) and poly(ethylene terephthalate) films via environmental crazing

This work addresses the phenomenon of the development of a patterned surface relief on polymer films via different modes of environmental crazing. Commercial films of semicrystalline poly(tetrafluoroethylene) (PTFE) and amorphous glassy poly(ethylene terephthalate) (PET) were subjected to tensile drawing in the presence of physically active liquid environments (carbon tetrachloride or aliphatic alcohols). The structure parameters and wettability of the modified films were studied by AFM, SEM, profilometer measurements and contact angle measurements. Environmental intercrystallite crazing of PTFE is accompanied by the development of an unstable structure with a high free surface, which experiences marked strain recovery upon unloading. As a result of the relief formation, PTFE hydrophobicity is enhanced (the water contact angle increases by 25°). Classical environmental crazing of PET films is accompanied by the formation of an anisotropic surface relief which is an assembly of crazes oriented perpendicular to the direction of tensile drawing, thus leading to the phenomenon of anisotropic wetting. The proposed approach for structural surface modification makes it possible to use the advantages of surface instability and spontaneous self‐organization of the polymer towards the development of a unique surface microrelief. © 2020 Society of Chemical Industry     

Investigating the effect of silver nanorods embedded in polydimethylsiloxane matrix using nanoindentation and its use for flexible electronics

The stretchable electrodes with excellent flexibility, electrical conductivity, and mechanical durability are the most fundamental components in the emerging and exciting field of flexible electronics. This article proposes a method for fabrication of such a stretchable electrode by embedding silver nanorods (AgNRs) into a polydimethylsiloxane (PDMS) matrix that is grown by a unique glancing angle deposition technique. The surface, mechanical, and electrical properties of PDMS are significantly changed after embedding the AgNRs in it. The results show that surface roughness and polarity increase after AgNRs are embedded in the PDMS matrix. Elastic modulus (E) and hardness (H) decrease with an increase in the indentation load as a result of the indentation depth effect. Due to strong interfacial adhesion of AgNRs embedded in the PDMS matrix, the E and H of nanocomposite are increased by 167.6 and 93.3% compared with PDMS film, respectively. Furthermore, the AgNRs-PDMS film has an electrical resistivity value in the order of 10⁻⁷ Ωm. It remains conductive during various mechanical strains such as bending, twisting, and stretching, which is demonstrated using a light-emitting diode circuit. Simultaneously, the antimicrobial activity of silver could make it a promising candidate for wearable electronics.     

Design and performance study of phase‐locked loop using fractional‐order loop filter

The present work reports the realization of an analog fractional‐order phase‐locked loop (FPLL) using a fractional capacitor. The expressions for bandwidth, capture range, and lock range of the FPLL have been derived analytically and then compared with the experimental observations using LM565 IC. It has been observed that bandwidth and capture range can be extended by using FPLL. It has also been found that FPLL can provide faster response and lower phase error at the time of switching compared to its integer‐order counterpart. Copyright © 2014 John Wiley & Sons, Ltd.     

Investigation on external stimuli engendered magnetic ordering in polycrystalline CaCu3Ti4O12 quadruple perovskite

The consequences of high energy mechanical milling, microwave-assisted heating and rapid thermal cooling on magnetic ordering in polycrystalline CaCu₃Ti₄O₁₂ cubic perovskite have been investigated by means of X-ray powder diffractometry (300?K), dc magnetization in field – cooled and zero – field cooled modes (H = 100?Oe and 1000?Oe, T?=?5–300?K) (M – T curves) and M – H loop characteristics (T?=?5?K and 300?K, H_max = 70?kOe). The M – T curves of unmilled and 16?h milled samples show pure antiferromagnetic and weak ferromagnetic ordering, respectively, 1?h and 6?h milled samples demonstrate the coexistence of both the phases while microwave-assisted and quenched samples exhibit classic antiferromagnetic transition and a low temperature paramagnetic–like contribution with different weights, well supported by the M – H loop characteristics. The observed transformations in the magnetic ordering are attributed to the ball-milling induced stress which curtails hybridization of empty Ti-3d orbitals with Cu-3d and O-2p orbitals and secondary phase formation. Oxygen vacancies associated with bound magnetic polarons originate ferromagnetism in the milled samples while unpaired electrons inhabited at the empty sites are the cause of paramagnetic centers. The low-temperature Curie – tail in M – T curve for quenched and microwave assisted samples is attributed to Ti³⁺ cations.     

Electromagnetism-like algorithms for optimized tool path planning in 5-axis flank machining

Optimization of tool path planning using metaheuristic algorithms such as ant colony systems (ACS) and particle swarm optimization (PSO) provides a feasible approach to reduce geometrical machining errors in 5-axis flank machining of ruled surfaces. The optimal solutions of these algorithms exhibit an unsatisfactory quality in a high-dimensional search space. In this study, various algorithms derived from the electromagnetism-like mechanism (EM) were applied. The test results of representative surfaces showed that all EM-based methods yield more effective optimal solutions than does PSO, despite a longer search time. A new EM-MSS (electromagnetism-like mechanism with move solution screening) algorithm produces the most favorable results by ensuring the continuous improvement of new searches. Incorporating an SPSA (simultaneous perturbation stochastic approximation) technique further improves the search results with effective initial solutions. This work enhances the practical values of tool path planning by providing a satisfactory machining quality.