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Materials, Volume 12, Issue 3 (February-1 2019)

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Open AccessReview Copper/Epoxy Joints in Printed Circuit Boards: Manufacturing and Interfacial Failure Mechanisms
Materials 2019, 12(3), 550; https://doi.org/10.3390/ma12030550
Received: 23 January 2019 / Revised: 31 January 2019 / Accepted: 5 February 2019 / Published: 12 February 2019
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Abstract
Printed circuit boards (PCBs) have a wide range of applications in electronics where they are used for electric signal transfer. For a multilayer build-up, thin copper foils are alternated with epoxy-based prepregs and laminated to each other. Adhesion between copper and epoxy composites [...] Read more.
Printed circuit boards (PCBs) have a wide range of applications in electronics where they are used for electric signal transfer. For a multilayer build-up, thin copper foils are alternated with epoxy-based prepregs and laminated to each other. Adhesion between copper and epoxy composites is achieved by technologies based on mechanical interlocking or chemical bonding, however for future development, the understanding of failure mechanisms between these materials is of high importance. In literature, various interfacial failures are reported which lead to adhesion loss between copper and epoxy resins. This review aims to give an overview on common coupling technologies and possible failure mechanisms. The information reviewed can in turn lead to the development of new strategies, enhancing the adhesion strength of copper/epoxy joints and, therefore, establishing a basis for future PCB manufacturing. Full article
(This article belongs to the Section Corrosion and Materials Degradation)
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Open AccessArticle Effect of YAl2 Particles on the Corrosion Behavior of Mg–Li Matrix Composite in NaCl Solution
Materials 2019, 12(3), 549; https://doi.org/10.3390/ma12030549
Received: 4 January 2019 / Revised: 8 February 2019 / Accepted: 10 February 2019 / Published: 12 February 2019
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Abstract
The strength of Mg–Li alloy is greatly improved by the composite strengthening of intermetallic compound YAl2 particles, but the low corrosion resistance of Mg–Li alloy is still the main factor that restricts the application of the alloy and its composites. In this [...] Read more.
The strength of Mg–Li alloy is greatly improved by the composite strengthening of intermetallic compound YAl2 particles, but the low corrosion resistance of Mg–Li alloy is still the main factor that restricts the application of the alloy and its composites. In this paper, the effect of YAl2 particles on the corrosion behavior of Mg–Li alloy was systematically investigated. The results showed that the corrosion resistance of YAl2p/LA143 composite could be significantly improved, accounting for the formation of a transitional interface layer by adding YAl2 particles. The diffusion of yttrium and aluminum atoms from YAl2 particulates improved the stability of the surface film and enhanced the adhesion between the corrosion products and the substrate, which hindered further expansion of pitting. Full article
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Open AccessArticle A New Way of Toughening of Thermoset by Dual-Cured Thermoplastic/Thermosetting Blend
Materials 2019, 12(3), 548; https://doi.org/10.3390/ma12030548
Received: 21 December 2018 / Revised: 31 January 2019 / Accepted: 5 February 2019 / Published: 12 February 2019
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Abstract
The work aims at establishing the optimum conditions for dual thermal and electron beam curing of thermosetting systems modified by styrene/butadiene (SB)-based triblock copolymers in order to develop transparent and toughened materials. The work also investigates the effects of curing procedures on the [...] Read more.
The work aims at establishing the optimum conditions for dual thermal and electron beam curing of thermosetting systems modified by styrene/butadiene (SB)-based triblock copolymers in order to develop transparent and toughened materials. The work also investigates the effects of curing procedures on the ultimate phase morphology and mechanical properties of these thermoset–SB copolymer blends. It was found that at least 46 mol% of the epoxidation degree of the SB copolymer was needed to enable the miscibility of the modified block copolymer into the epoxy resin. Hence, an electron beam curing dose of ~50 kGy was needed to ensure the formation of micro- and nanostructured transparent blends. The micro- and nanophase-separated thermosets obtained were analyzed by optical as well as scanning and transmission electron microscopy. The mechanical properties of the blends were enhanced as shown by their impact strengths, indentation, hardness, and fracture toughness analyses, whereby the toughness values were found to mainly depend on the dose. Thus, we have developed a new route for designing dual-cured toughened micro- and nanostructured transparent epoxy thermosets with enhanced fracture toughness. Full article
(This article belongs to the Special Issue Carbon Fibers and Their Composite Materials)
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Open AccessArticle Tailoring Electro/Optical Properties of Transparent Boron-Doped Carbon Nanowalls Grown on Quartz
Materials 2019, 12(3), 547; https://doi.org/10.3390/ma12030547
Received: 29 January 2019 / Revised: 8 February 2019 / Accepted: 10 February 2019 / Published: 12 February 2019
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Abstract
Carbon nanowalls (CNWs) have attracted much attention for numerous applications in electrical devices because of their peculiar structural characteristics. However, it is possible to set synthesis parameters to vary the electrical and optical properties of such CNWs. In this paper, we demonstrate the [...] Read more.
Carbon nanowalls (CNWs) have attracted much attention for numerous applications in electrical devices because of their peculiar structural characteristics. However, it is possible to set synthesis parameters to vary the electrical and optical properties of such CNWs. In this paper, we demonstrate the direct growth of highly transparent boron-doped nanowalls (B-CNWs) on optical grade fused quartz. The effect of growth temperature and boron doping on the behavior of boron-doped carbon nanowalls grown on quartz was studied in particular. Temperature and boron inclusion doping level allow for direct tuning of CNW morphology. It is possible to operate with both parameters to obtain a transparent and conductive film; however, boron doping is a preferred factor to maintain the transparency in the visible region, while a higher growth temperature is more effective to improve conductance. Light transmittance and electrical conductivity are mainly influenced by growth temperature and then by boron doping. Tailoring B-CNWs has important implications for potential applications of such electrically conductive transparent electrodes designed for energy conversion and storage devices. Full article
(This article belongs to the Special Issue Transparent Conductive Films and Their Applications)
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Open AccessArticle Systematic Investigation of the Synergistic and Antagonistic Effects on the Removal of Pyrene and Copper onto Mesoporous Silica from Aqueous Solutions
Materials 2019, 12(3), 546; https://doi.org/10.3390/ma12030546
Received: 4 January 2019 / Revised: 1 February 2019 / Accepted: 9 February 2019 / Published: 12 February 2019
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Abstract
Polycyclic aromatic hydrocarbons (PAHs) and heavy metals have attracted greater attention due to their single or complex risks. It is urgent to find useful methods to remove these two pollutants together. In this study, SBA15 and MCM-41 were selected and used for the [...] Read more.
Polycyclic aromatic hydrocarbons (PAHs) and heavy metals have attracted greater attention due to their single or complex risks. It is urgent to find useful methods to remove these two pollutants together. In this study, SBA15 and MCM-41 were selected and used for the simultaneous removal of pyrene and copper from aqueous solution. Batch experiments were conducted systematically by investigating the adsorption behavior and effects including kinetics, isotherms, ionic strength and pH effects. Experimental results showed that the Langmuir and pseudo-second-order model fitted the adsorption behavior better. The solution pH values and ionic strength affected the adsorption behavior greatly. Furthermore, the synergistic or antagonistic effects could be observed on the adsorption of pyrene and copper onto MCM-41 and SBA15, respectively. The synergistic and antagonistic effects of pyrene and copper onto mesoporous silica may be attributed to the size of pyrene–copper complex and the average pore size of adsorbents. With the higher pore size, the complex would be adsorbed onto the inner surface of MCM-41 which showed synergistic effect on the adsorption of pyrene and copper. This study shows new guidelines and insight into the study of adsorption behavior of PAHs and heavy metals from aquatic environments. Full article
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Open AccessArticle Enhanced Thermal Stability of Thermoplastic Polymer Nanostructures for Nanoimprint Lithography
Materials 2019, 12(3), 545; https://doi.org/10.3390/ma12030545
Received: 7 January 2019 / Revised: 6 February 2019 / Accepted: 7 February 2019 / Published: 12 February 2019
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Abstract
Thermoplastic polymer micro- and nanostructures suffer pattern decay when heated to a temperature close to or above the polymer’s glass transition temperature. In this work, we report enhanced thermal stability of polycarbonate nanostructures at temperatures well above their glass transition temperatures. Based on [...] Read more.
Thermoplastic polymer micro- and nanostructures suffer pattern decay when heated to a temperature close to or above the polymer’s glass transition temperature. In this work, we report enhanced thermal stability of polycarbonate nanostructures at temperatures well above their glass transition temperatures. Based on this observation, we develop a unique technique for high-resolution polymer patterning by polymer reflows. This technique is characterized as the precise control of polymer reflows regardless of the annealing time, which avoids the time-domain nonlinear reflow of the polymer melt. We also implement thermal nanoimprinting in a step-and-repeat fashion, which dramatically increases the throughput of the thermal nanoimprint. The enhanced pattern stability against thermal reflow also allows for multiple imprinting at the same location to generate complex resist patterns from a simple mold structure. Since modern lithography often uses thin resist films (sub-100 nm) due to the restraint from the pattern aspect ratio, the unusual annealing behavior of thin polymer films is highly relevant in sub-100 nm lithographic processing. Full article
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Open AccessArticle Microstructural Tuning of a Laser-Cladding Layer by Means of a Mix of Commercial Inconel 625 and AISI H13 Powders
Materials 2019, 12(3), 544; https://doi.org/10.3390/ma12030544
Received: 10 January 2019 / Revised: 5 February 2019 / Accepted: 8 February 2019 / Published: 12 February 2019
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Abstract
The aim of this work is to evaluate the microstructural evolutions developed by mixing a corrosion-resistant and high-performance material with a high-hardness material in a coating obtained by laser-cladding technology. In this paper, five different mixtures of Inconel 625 alloy and AISI H13 [...] Read more.
The aim of this work is to evaluate the microstructural evolutions developed by mixing a corrosion-resistant and high-performance material with a high-hardness material in a coating obtained by laser-cladding technology. In this paper, five different mixtures of Inconel 625 alloy and AISI H13 steel powders have been deposited on a plate of 42CrMo4 steel using a 2.2 kW diode pumped Nd:YAG laser. The effect of adding tool steel to a Ni-based superalloy has been analyzed by the characterization of each cladded sample using optical microscopy and scanning electron microscopy (SEM). The precipitates observed in the samples have been analyzed by energy dispersive X-ray spectroscopy (EDS X-ray). SEM micrographs and EDS analysis indicate the existence of Laves phase. It has been observed that the presence of these precipitates is stabilized in a certain range of AISI H13 addition. Full article
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Open AccessArticle The Anisotropic Distortional Yield Surface Constitutive Model Based on the Chaboche Cyclic Plastic Model
Materials 2019, 12(3), 543; https://doi.org/10.3390/ma12030543
Received: 7 January 2019 / Revised: 3 February 2019 / Accepted: 9 February 2019 / Published: 12 February 2019
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Abstract
Considering the cross effect in the evolution of subsequent yield surfaces for metals, an anisotropic distortional yield surface constitutive model is developed. By introducing an anisotropic distortional hardening function into the isotropic hardening part of the classical Chaboche rate-dependent constitutive model, the plastic-deformation-induced [...] Read more.
Considering the cross effect in the evolution of subsequent yield surfaces for metals, an anisotropic distortional yield surface constitutive model is developed. By introducing an anisotropic distortional hardening function into the isotropic hardening part of the classical Chaboche rate-dependent constitutive model, the plastic-deformation-induced distortional and anisotropic hardening behaviors of subsequent yield surfaces are characterized. The experimental data of distortional yield surfaces for T2 pure copper under three different loading paths, including pre-tension, pre-torsion, and pre-tension-torsion proportional loading of 45-degree, are simulated by implementing the models into a numerical user defined material (UMAT) procedure based on the ABAQUS finite element package. To validate the anisotropic plastic model, the simulated yield surfaces are compared with experimental observations and predicted results for a crystal plasticity model and good agreement are noted. The simulations demonstrate that the proposed model can accurately capture the characteristics of the distortional yield surface and the anisotropic hardening process of the yield surface. Moreover, the distortional shapes of experimental subsequent yield surfaces in loading direction and opposite direction can be better revealed by the anisotropic plastic constitutive model than the crystal plastic constitutive model. Full article
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Open AccessArticle Novel Porous Brain Electrodes for Augmented Local Field Potential Signal Detection
Materials 2019, 12(3), 542; https://doi.org/10.3390/ma12030542
Received: 20 December 2018 / Revised: 28 January 2019 / Accepted: 9 February 2019 / Published: 12 February 2019
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Abstract
Intracerebral local field potential (LFP) measurements are commonly used to monitor brain activity, providing insight into the flow of information across neural networks. Herein we describe synthesis and application of a neural electrode possessing a nano/micro-scale porous surface topology for improved LFP measurement. [...] Read more.
Intracerebral local field potential (LFP) measurements are commonly used to monitor brain activity, providing insight into the flow of information across neural networks. Herein we describe synthesis and application of a neural electrode possessing a nano/micro-scale porous surface topology for improved LFP measurement. Compared with conventional brain electrodes, the porous electrodes demonstrate higher measured amplitudes with lower noise levels. Full article
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Open AccessFeature PaperReview Fabrication of Porous Materials by Spark Plasma Sintering: A Review
Materials 2019, 12(3), 541; https://doi.org/10.3390/ma12030541
Received: 28 January 2019 / Revised: 9 February 2019 / Accepted: 11 February 2019 / Published: 12 February 2019
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Abstract
Spark plasma sintering (SPS), a sintering method that uses the action of pulsed direct current and pressure, has received a lot of attention due to its capability of exerting control over the microstructure of the sintered material and flexibility in terms of the [...] Read more.
Spark plasma sintering (SPS), a sintering method that uses the action of pulsed direct current and pressure, has received a lot of attention due to its capability of exerting control over the microstructure of the sintered material and flexibility in terms of the heating rate and heating mode. Historically, SPS was developed in search of ways to preserve a fine-grained structure of the sintered material while eliminating porosity and reaching a high relative density. These goals have, therefore, been pursued in the majority of studies on the behavior of materials during SPS. Recently, the potential of SPS for the fabrication of porous materials has been recognized. This article is the first review to focus on the achievements in this area. The major approaches to the formation of porous materials by SPS are described: partial densification of powders (under low pressures, in pressureless sintering processes or at low temperatures), sintering of hollow particles/spheres, sintering of porous particles, and sintering with removable space holders or pore formers. In the case of conductive materials processed by SPS using the first approach, the formation of inter-particle contacts may be associated with local melting and non-conventional mechanisms of mass transfer. Studies of the morphology and microstructure of the inter-particle contacts as well as modeling of the processes occurring at the inter-particle contacts help gain insights into the physics of the initial stage of SPS. For pre-consolidated specimens, an SPS device can be used as a furnace to heat the materials at a high rate, which can also be beneficial for controlling the formation of porous structures. In sintering with space holders, SPS processing allows controlling the structure of the pore walls. In this article, using the literature data and our own research results, we have discussed the formation and structure of porous metals, intermetallics, ceramics, and carbon materials obtained by SPS. Full article
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Open AccessFeature PaperArticle One-Pot Method for Preparation of Magnetic Multi-Core Nanocarriers for Drug Delivery
Materials 2019, 12(3), 540; https://doi.org/10.3390/ma12030540
Received: 19 January 2019 / Revised: 7 February 2019 / Accepted: 9 February 2019 / Published: 12 February 2019
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Abstract
The development of various magnetically-responsive nanostructures is of great importance in biomedicine. The controlled assembly of many small superparamagnetic nanocrystals into large multi-core clusters is needed for effective magnetic drug delivery. Here, we present a novel one-pot method for the preparation of multi-core [...] Read more.
The development of various magnetically-responsive nanostructures is of great importance in biomedicine. The controlled assembly of many small superparamagnetic nanocrystals into large multi-core clusters is needed for effective magnetic drug delivery. Here, we present a novel one-pot method for the preparation of multi-core clusters for drug delivery (i.e., magnetic nanocarriers). The method is based on hot homogenization of a hydrophobic phase containing a nonpolar surfactant into an aqueous phase, using ultrasonication. The solvent-free hydrophobic phase that contained tetradecan-1-ol, γ-Fe2O3 nanocrystals, orlistat, and surfactant was dispersed into a warm aqueous surfactant solution, with the formation of small droplets. Then, a pre-cooled aqueous phase was added for rapid cooling and the formation of solid magnetic nanocarriers. Two different nonpolar surfactants, polyethylene glycol dodecyl ether (B4) and our own N1,N1-dimethyl-N2-(tricosan-12-yl)ethane-1,2-diamine (SP11), were investigated for the preparation of MC-B4 and MC-SP11 magnetic nanocarriers, respectively. The nanocarriers formed were of spherical shape, with mean hydrodynamic sizes <160 nm, good colloidal stability, and high drug loading (7.65 wt.%). The MC-B4 nanocarriers showed prolonged drug release, while no drug release was seen for the MC-SP11 nanocarriers over the same time frame. Thus, the selection of a nonpolar surfactant for preparation of magnetic nanocarriers is crucial to enable drug release from nanocarrier. Full article
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Open AccessArticle Optical Properties of Oxidized Plasma-Polymerized Organosilicones and Their Correlation with Mechanical and Chemical Parameters
Materials 2019, 12(3), 539; https://doi.org/10.3390/ma12030539
Received: 16 January 2019 / Revised: 31 January 2019 / Accepted: 6 February 2019 / Published: 12 February 2019
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Abstract
Pure tetravinylsilane and its oxygen mixture were used to deposit oxidized plasma polymer films at various effective power (0.1–10 W) and various oxygen fractions (0–0.71) using RF pulsed plasma. The optical properties (refractive index, extinction coefficient, band gap) of the deposited films were [...] Read more.
Pure tetravinylsilane and its oxygen mixture were used to deposit oxidized plasma polymer films at various effective power (0.1–10 W) and various oxygen fractions (0–0.71) using RF pulsed plasma. The optical properties (refractive index, extinction coefficient, band gap) of the deposited films were investigated by spectroscopic ellipsometry (230–830 nm) using an optical model and Tauc‒Lorentz parametrization. Analyses of chemical and mechanical properties of films allowed for the interpretation of changes in optical properties with deposition conditions. The refractive index was revealed to increase with enhanced effective power due to the increased crosslinking of the plasma polymer network but decreased when increasing the oxygen fraction due to the decrease of polymer crosslinking as the number of carbon bonds in the plasma polymer network was eliminated. A very strong positive correlation was found between the Young’s modulus and the refractive index for oxidized plasma polymer films. The optical properties of films correlated with their chemical properties for the specific deposition conditions used in this study. The band gap (1.9–2.9 eV) was assumed to be widened due to the increased concentration of vinyl groups in oxidized plasma polymer films. Full article
(This article belongs to the Special Issue Plasma Polymerized Materials)
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Open AccessArticle Influence of Prior Martensite on Bainite Transformation, Microstructures, and Mechanical Properties in Ultra-Fine Bainitic Steel
Materials 2019, 12(3), 527; https://doi.org/10.3390/ma12030527
Received: 18 January 2019 / Revised: 8 February 2019 / Accepted: 8 February 2019 / Published: 12 February 2019
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Abstract
A multiphase microstructure comprising of different volume fractions of prior martensite and ultra-fine bainite (bainitic ferrite and retained austenite) was obtained by quenching to certain temperatures, followed by isothermal bainitic transformation. The effect of the prior martensite transformation on the bainitic transformation behavior, [...] Read more.
A multiphase microstructure comprising of different volume fractions of prior martensite and ultra-fine bainite (bainitic ferrite and retained austenite) was obtained by quenching to certain temperatures, followed by isothermal bainitic transformation. The effect of the prior martensite transformation on the bainitic transformation behavior, microstructures, and mechanical properties were discussed. The results showed that the prior martensite accelerated the subsequent low-temperature bainite transformation, and the incubation period and completion time of the bainite reaction were significantly shortened. This phenomenon was attributed to the enhanced nucleation ratio caused by the introduced strain in austenite, due to the formation of prior martensite and a carbon partitioning between the prior martensite and retained austenite. Moreover, the prior martensite could influence the crystal growth direction of bainite ferrite, refine bainitic ferrite plates, and reduce the dimension of blocky retained austenite, all of which were responsible for improving the mechanical properties of the ultra-fine bainitic steel. When the content of the prior martensite reached 15%, the investigated steels had the best performance, which were 1800 MPa and 21% for the tensile strength and elongation, respectively. Unfortunately, the increased content of the prior martensite could lead to a worsening of the impact toughness. Full article
(This article belongs to the Special Issue Microstructure and Mechanical Properties of Steels)
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Open AccessArticle Stochastic Constitutive Model of Isotropic Thin Fiber Networks Based on Stochastic Volume Elements
Materials 2019, 12(3), 538; https://doi.org/10.3390/ma12030538
Received: 15 November 2018 / Revised: 20 January 2019 / Accepted: 24 January 2019 / Published: 11 February 2019
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Abstract
Thin fiber networks are widely represented in nature and can be found in man-made materials such as paper and packaging. The strength of such materials is an intricate subject due to inherited randomness and size-dependencies. Direct fiber-level numerical simulations can provide insights into [...] Read more.
Thin fiber networks are widely represented in nature and can be found in man-made materials such as paper and packaging. The strength of such materials is an intricate subject due to inherited randomness and size-dependencies. Direct fiber-level numerical simulations can provide insights into the role of the constitutive components of such networks, their morphology, and arrangements on the strength of the products made of them. However, direct mechanical simulation of randomly generated large and thin fiber networks is characterized by overwhelming computational costs. Herein, a stochastic constitutive model for predicting the random mechanical response of isotropic thin fiber networks of arbitrary size is presented. The model is based on stochastic volume elements (SVEs) with SVE size-specific deterministic and stochastic constitutive law parameters. The randomness in the network is described by the spatial fields of the uniaxial strain and strength to failure, formulated using multivariate kernel functions and approximate univariate probability density functions. The proposed stochastic continuum approach shows good agreement when compared to direct numerical simulation with respect to mechanical response. Furthermore, strain localization patterns matched the one observed in direct simulations, which suggests an accurate prediction of the failure location. This work demonstrates that the proposed stochastic constitutive model can be used to predict the response of random isotropic fiber networks of arbitrary size. Full article
(This article belongs to the Special Issue Randomness and Uncertainty)
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Open AccessArticle Preparation and Characterization of Nanostructured Hollow MgO Spheres
Materials 2019, 12(3), 537; https://doi.org/10.3390/ma12030537
Received: 17 January 2019 / Revised: 5 February 2019 / Accepted: 8 February 2019 / Published: 11 February 2019
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Abstract
Nanostructured hollow MgO microspheres were prepared by the template method. First, D-Anhydrous glucose was polymerized by the hydrothermal method to form a template. Second, a colorless solution was obtained by mixing magnesite with hydrochloric acid in a 1:2 proportion and heating in an [...] Read more.
Nanostructured hollow MgO microspheres were prepared by the template method. First, D-Anhydrous glucose was polymerized by the hydrothermal method to form a template. Second, a colorless solution was obtained by mixing magnesite with hydrochloric acid in a 1:2 proportion and heating in an 80 °C water bath for 2 h. Finally, the template from the first step was placed in the colorless solution, and the resulting precipitate was calcined at 550 °C for 2 h. The phase composition and microstructure of the calcined samples were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The XRD results indicated that the main crystal is periclase. The SEM results indicates that the template carbon microsphere surface is smooth, and the its size is uniform and concentrated in the range of 100–200 nm. The diameters of the samples range from 60 to 90 nm, which is smaller than the size of the carbon microsphere. The TEM results indicates that the sample is hollow with a shell thickness of about 6–10 nm. The specific surface area of the calcined hollow sphere is 59.5 m²·g−1. Full article
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Open AccessArticle First-Principles Study of the Electronic, Vibrational Properties and Anharmonic Effects of Some Si-Based Type-II Binary Clathrates
Materials 2019, 12(3), 536; https://doi.org/10.3390/ma12030536
Received: 21 January 2019 / Revised: 5 February 2019 / Accepted: 6 February 2019 / Published: 11 February 2019
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Electronic, vibrational, and anharmonic studies on some binary clathrate AxSi136 (A = Na, K, Rb, Cs; 0 < x ≤ 24) are theoretically presented. The Fermi energy lies in the range of 1.1 eV to 1.4 eV for Nax [...] Read more.
Electronic, vibrational, and anharmonic studies on some binary clathrate AxSi136 (A = Na, K, Rb, Cs; 0 < x ≤ 24) are theoretically presented. The Fermi energy lies in the range of 1.1 eV to 1.4 eV for NaxSi136 and increases as stoichiometry (x) is tuned from 8 to 12 to 16. The determined isotropic “Mexican-hat” shape of the guest-host potential describing Na motion in the Si28 cage indicates the “off-center” position when the temperature is elevated beyond zero. Accordingly, the calculated Na “off-center” displacements correlate well with the X-Ray Diffraction (XRD) data (0.4 Å–0.5 Å) for a similar composition range (0 < x < 24). The lack of first-principles analysis on quartic anharmonicity motivates us to initiate a self-consistent model to examine the temperature-dependent rattling frequency Ω(T) of the guest (Na, Rb). The predicted values of Ω(T) for Na24Si136 at 300 K are significantly higher (approximately six times larger) than the value at absolute zero, which contrasts with the case of Rb8Si136. Moreover, underestimation of the isotropic atomic displacement parameter Uiso is caused by the temperature-dependent quartic anharmonicity of Na, and this discrepancy might be offset by the square of the “off-center” displacement. Full article
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Open AccessArticle ZnO Synthesized Using Bipolar Electrochemistry: Structure and Activity
Materials 2019, 12(3), 535; https://doi.org/10.3390/ma12030535
Received: 31 December 2018 / Revised: 29 January 2019 / Accepted: 6 February 2019 / Published: 11 February 2019
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Abstract
The photoactive materials broadly applied in catalysis and energy conversion are generally composed of metal oxides. Among these oxides, ZnO showed a promising photocatalytic activity; however, traditional synthetic routes generated by-products and large amounts of secondary waste. Herein, we report the use of [...] Read more.
The photoactive materials broadly applied in catalysis and energy conversion are generally composed of metal oxides. Among these oxides, ZnO showed a promising photocatalytic activity; however, traditional synthetic routes generated by-products and large amounts of secondary waste. Herein, we report the use of bipolar electrochemistry to generate ZnO nanoparticles using deionized water and a zinc metal to conform to green chemistry practices. TEM imaging demonstrated that the sizes of the bipolar-made ZnO particles were smaller than the commercial sample. The presence of structural defects in ZnO was correlated with the chemical shifts analyzed by X-ray photoelectron spectroscopy (XPS) and by different concentrations of O2− ions in stoichiometric and defected lattice. Further, the diffuse reflectance UV–Vis studies demonstrated a blue-shift in the reflectance spectrum for the bipolar-made oxide. This was also an indication of defects in the ZnO lattice, which related to the formation of shallow levels in the bandgap of the material. The structural and morphological differences influenced the photocatalytic characteristics, revealing a higher photocurrent for the bipolar-made ZnO when compared to the reference sample. This was further manifested in lower total resistivity for all anodes made from the non-stoichiometric ZnO, and also in their shorter diffusion length for charge exchange and electron lifetimes. Full article
(This article belongs to the Section Energy Materials)
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Open AccessArticle Temperature Field Numerical Analysis Mode and Verification of Quenching Heat Treatment Using Carbon Steel in Rotating Laser Scanning
Materials 2019, 12(3), 534; https://doi.org/10.3390/ma12030534
Received: 20 December 2018 / Revised: 23 January 2019 / Accepted: 2 February 2019 / Published: 11 February 2019
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Abstract
Temperature history and hardening depth are experimentally characterized in the rotational laser hardening process for an AISI 1045 medium carbon steel specimen. A three-dimensional finite element model is proposed to predict the temperature field distribution and hardening zone area. The laser temperature field [...] Read more.
Temperature history and hardening depth are experimentally characterized in the rotational laser hardening process for an AISI 1045 medium carbon steel specimen. A three-dimensional finite element model is proposed to predict the temperature field distribution and hardening zone area. The laser temperature field is set up for an average distribution and scanned along a circular path. Linear motion also takes place alongside rotation. The prediction of hardening area can be increased by increasing the rotational radius, which in turn raises the processing efficiency. A good agreement is found between the experimental characterized hardness value and metallographic composition. The uniformity of the hardening area decreases with increasing laser scanning speed. The increased laser power input could help to expand the hardening depth. Full article
(This article belongs to the Special Issue Selected Papers from TIKI ICICE 2018)
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Open AccessArticle WxNbMoTa Refractory High-Entropy Alloys Fabricated by Laser Cladding Deposition
Materials 2019, 12(3), 533; https://doi.org/10.3390/ma12030533
Received: 20 January 2019 / Revised: 6 February 2019 / Accepted: 8 February 2019 / Published: 11 February 2019
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Abstract
WxNbMoTa refractory high-entropy alloys with four different tungsten concentrations (x = 0, 0.16, 0.33, 0.53) were fabricated by laser cladding deposition. The crystal structures of WxNbMoTa alloys are all a single-phase solid solution of the body-centered cubic (BCC) [...] Read more.
WxNbMoTa refractory high-entropy alloys with four different tungsten concentrations (x = 0, 0.16, 0.33, 0.53) were fabricated by laser cladding deposition. The crystal structures of WxNbMoTa alloys are all a single-phase solid solution of the body-centered cubic (BCC) structure. The size of the grains and dendrites are 20 μm and 4 μm on average, due to the rapid solidification characteristics of the laser cladding deposition. These are much smaller sizes than refractory high-entropy alloys fabricated by vacuum arc melting. In terms of integrated mechanical properties, the increase of the tungsten concentration of WxNbMoTa has led to four results of the Vickers microhardness, i.e., Hv = 459.2 ± 9.7, 476.0 ± 12.9, 485.3 ± 8.7, and 497.6 ± 5.6. As a result, NbMoTa alloy shows a yield strength (σb) and compressive strain (εp) of 530 Mpa and 8.5% at 1000 °C, leading to better results than traditional refractory alloys such as T-111, C103, and Nb-1Zr, which are commonly used in the aerospace industry. Full article
(This article belongs to the Special Issue Additive Manufacturing: Alloy Design and Process Innovations)
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Open AccessArticle Influence of Torsion on Matteucci Effect Signal Parameters in Co-Based Bistable Amorphous Wire
Materials 2019, 12(3), 532; https://doi.org/10.3390/ma12030532
Received: 13 December 2018 / Revised: 1 February 2019 / Accepted: 8 February 2019 / Published: 11 February 2019
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Abstract
The Matteucci effect (ME) is one of the lesser-known magnetomechanical effects and is most prominent in bistable amorphous wires. It has some experimental applications—Matteucci effect-based magnetic field sensors are very easy to produce and have inherently linear, hybrid analog/digital output signal. The effect [...] Read more.
The Matteucci effect (ME) is one of the lesser-known magnetomechanical effects and is most prominent in bistable amorphous wires. It has some experimental applications—Matteucci effect-based magnetic field sensors are very easy to produce and have inherently linear, hybrid analog/digital output signal. The effect is still poorly understood, however, and although it relies on torsion of the wire to manifest, there is no available model, or much experimental data, which would quantitatively connect the ME with the sample twist. In this paper, experimental characteristics of ME signal parameters dependence on torsion in Co-based amorphous bistable wire are presented. The results hint at possible applications, such as rotation or critical current sensors, as well as the necessity of torsion control in the development of ME magnetic field sensors. Full article
(This article belongs to the Special Issue Magnetoelastic Materials)
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Open AccessArticle The Penetration Ability of Calcium Silicate Root Canal Sealers into Dentinal Tubules Compared to Conventional Resin-Based Sealer: A Confocal Laser Scanning Microscopy Study
Materials 2019, 12(3), 531; https://doi.org/10.3390/ma12030531
Received: 10 January 2019 / Revised: 3 February 2019 / Accepted: 5 February 2019 / Published: 11 February 2019
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Abstract
The purpose of this study was to compare the penetration ability of calcium silicate root canal sealers and conventional resin-based sealer using confocal laser scanning microscopy (CLSM). A total of 60 recently extracted single-rooted human premolars were used in this study. The root [...] Read more.
The purpose of this study was to compare the penetration ability of calcium silicate root canal sealers and conventional resin-based sealer using confocal laser scanning microscopy (CLSM). A total of 60 recently extracted single-rooted human premolars were used in this study. The root canals were prepared to a size 40/0.06 taper with ProFile rotary instruments and irrigated with NaOCl and EDTA. After drying all canals, the specimens were randomly divided into three experimental groups (n = 20): Group 1, gutta-percha (GP)/AH Plus with continuous wave compaction; group 2, GP/BioRoot RCS with a single-cone technique; and group 3, GP/Endoseal MTA with a single-cone technique. All experimental samples were sectioned perpendicular to their long axis using a low-speed diamond wheel at the apical, middle, and coronal third levels. The penetration abilities of all samples were evaluated using CLSM. A Kruskal–Wallis analysis and a series of Mann–Whitney U post hoc tests were performed. A higher intensity level was found in the coronal area and a lower intensity level in the apical area in all the experimental groups. The AH Plus group showed higher sum fluorescence intensity in the apical and coronal thirds compared with the BioRoot RCS and Endoseal MTA groups, whereas the BioRoot RCS group showed a higher intensity level in the middle third, similar to the AH Plus group. The maximum sealer penetration depth was low in the apical area and high in the coronal area in the AH Plus and Endoseal MTA groups. In the BioRoot RCS group, maximum sealer penetration was observed in the middle third. In conclusion, there were significant differences in sealer penetration pattern and distance according to the root level and sealer type. Full article
(This article belongs to the Special Issue Contemporary Endodontic Materials)
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Open AccessArticle Aging Characteristics of Bitumen from Different Bituminous Pavement Structures in Service
Materials 2019, 12(3), 530; https://doi.org/10.3390/ma12030530
Received: 20 January 2019 / Revised: 30 January 2019 / Accepted: 31 January 2019 / Published: 10 February 2019
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Abstract
The aging of bitumen seriously affects the service life of bituminous pavements. At present, there are many related researches on bitumen aging, but most of them focus on aging endured in indoor surroundings and conditions. Therefore, the conclusions obtained cannot reflect the actual [...] Read more.
The aging of bitumen seriously affects the service life of bituminous pavements. At present, there are many related researches on bitumen aging, but most of them focus on aging endured in indoor surroundings and conditions. Therefore, the conclusions obtained cannot reflect the actual aging changes of bitumen in bituminous pavements in service. In order to study the comprehensive aging process and mechanism of bitumen under the influence of service, we studied bridge deck, traffic lane, and ramp with bituminous pavement structures in service. The bitumen samples obtained from the core samples in different bituminous pavement structures were characterized by gel permeation chromatography (GPC), Fourier transform infrared spectroscopy (FTIR), dynamic shear rheometer (DSR), and fluorescence microscope (FM). The aging degree of different bitumen was analyzed, and conclusions were drawn on changes to bitumen aging from different pavement structures. The results showed that the aging degree of bitumen from the upper layer was the most serious, the aging degree of bitumen at the middle layer was weaker than that of bitumen from the upper layer, and the aging degree of bitumen from the bottom layer was the weakest for the different bituminous pavement structures. The aging of bitumen mainly occurred due to oxygen absorption. After aging, viscoelastic components of bitumen changed, and bitumen became harder. The macromolecule of bitumen could be divided into small molecules, and the small molecular weight of bitumen became large. The styrene-butadiene-styrene (SBS) modifier in the modified bitumen became granular after aging, and it appeared as a single phase in bitumen. The aging changes characterized by different analytical methods showed that the aging degree of bitumen from different layers of bituminous pavement structures in service was different. Effective measures should therefore be taken in time to decrease further aging of bitumen from the upper layer of bituminous pavements due to its inevitable early aging in service. Full article
(This article belongs to the Special Issue Sustainable Designed Pavement Materials)
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Open AccessArticle Application of Crumb Rubber in Cement-Matrix Composite
Materials 2019, 12(3), 529; https://doi.org/10.3390/ma12030529
Received: 17 December 2018 / Revised: 6 February 2019 / Accepted: 8 February 2019 / Published: 10 February 2019
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Abstract
Many studies have used rubber as an additive to form a cement-matrix composite (rubcrete). However, rubcrete has a lower mechanical strength than standard concrete. To improve the properties of rubcrete, this study performed surface modifications on crumb rubber through a partial oxidization reaction. [...] Read more.
Many studies have used rubber as an additive to form a cement-matrix composite (rubcrete). However, rubcrete has a lower mechanical strength than standard concrete. To improve the properties of rubcrete, this study performed surface modifications on crumb rubber through a partial oxidization reaction. The optimal ratio of air to nitrogen was determined by experiments to be 1:4. Fourier transform infrared spectroscopy (FT-IR) was used to identify the functional groups on the surface of the crumb rubber. A colloidal probe of calcium silicate hydrate (C–S–H) was prepared, and the intermolecular interactions between the rubber and the C–S–H were measured using an atomic force microscope (AFM). The experimental results showed that the partially oxidized crumb rubber contained more hydrophilic S–O bonds. The intermolecular force between C–S–H and treated rubber increased by 23% compared to the force between the original rubber and C–S–H. The compressive strength of the hardened cement paste (56 days) with the treated crumb rubber increased 50% in comparison with that of the hardened cement paste with the as-received crumb rubber. Full article
(This article belongs to the Special Issue Recent Advances in Rubber Recycling)
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Open AccessArticle Preparation and Characterization of Poly(δ-Valerolactone)/TiO2 Nanohybrid Material with Pores Interconnected for Potential Use in Tissue Engineering
Materials 2019, 12(3), 528; https://doi.org/10.3390/ma12030528
Received: 27 December 2018 / Revised: 24 January 2019 / Accepted: 6 February 2019 / Published: 10 February 2019
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Abstract
Titanium dioxide/poly(δ-valerolactone) (TiO2/Pδ-VL) nanohybrid material containing interconnected pores with sizes in the range 80–150 μm were prepared by the solvent casting and polymer melting routes, and the dispersion of the TiO2 nanofiller in the Pδ-VL matrix and its adhesion were [...] Read more.
Titanium dioxide/poly(δ-valerolactone) (TiO2/Pδ-VL) nanohybrid material containing interconnected pores with sizes in the range 80–150 μm were prepared by the solvent casting and polymer melting routes, and the dispersion of the TiO2 nanofiller in the Pδ-VL matrix and its adhesion were characterized by X-ray diffraction, differential scanning calorimetry, and scanning electron microscopy. A significant depression in the glass transition temperature (Tg) and melting temperature (Tm) values were revealed for the polymer nanocomposites prepared by the solvent casting technique. For the potential application of the prepared materials in the biomedical domain, complementary analyses were performed to examine the dynamic mechanical properties, and cell adhesion (using the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay), and the results obtained for the samples prepared by the two methods were compared. Interconnected pores were successively produced in the new material by employing naphthalene microparticles as a porogen for the first time, and the results obtained were very promising. Full article
(This article belongs to the Special Issue Advances in Hybrid Biomaterials)
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Open AccessArticle Effects of Reactive MgO on the Reaction Process of Geopolymer
Materials 2019, 12(3), 526; https://doi.org/10.3390/ma12030526
Received: 30 December 2018 / Revised: 20 January 2019 / Accepted: 1 February 2019 / Published: 10 February 2019
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Abstract
In order to compensate for the shrinkage of geopolymer pastes uniformly, reactive MgO powders are evenly dispersed in the geopolymer. The deformation performance, mechanical properties, microstructure and components of geopolymer pastes with reactive MgO are characterized. The effects of the content and the [...] Read more.
In order to compensate for the shrinkage of geopolymer pastes uniformly, reactive MgO powders are evenly dispersed in the geopolymer. The deformation performance, mechanical properties, microstructure and components of geopolymer pastes with reactive MgO are characterized. The effects of the content and the activity of MgO are discussed. The results indicate that the chemical shrinkage, autogenous shrinkage and drying shrinkage decrease with the addition of reactive MgO. MgO reacted with water, and fine Mg(OH)2 crystals forms as a geopolymer paste. Mg(OH)2 produces uniform expansion, which refines the pore size of pastes and the compressive strength increases. The shrinkage of the geopolymer pastes is thus effectively compensated. Full article
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Open AccessArticle Melt-Processed Poly(Ether Ether Ketone)/Carbon Nanotubes/Montmorillonite Nanocomposites with Enhanced Mechanical and Thermomechanical Properties
Materials 2019, 12(3), 525; https://doi.org/10.3390/ma12030525
Received: 10 January 2019 / Revised: 28 January 2019 / Accepted: 8 February 2019 / Published: 10 February 2019
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Abstract
The agglomeration problem of nanofillers, for instance, carbon nanotubes (CNTs) in a poly(ether ether ketone) (PEEK) matrix, is still a challenging assignment due to the intrinsic inert nature of PEEK to organic solvents. In this work, organically modified montmorillonite (MMT) was introduced as [...] Read more.
The agglomeration problem of nanofillers, for instance, carbon nanotubes (CNTs) in a poly(ether ether ketone) (PEEK) matrix, is still a challenging assignment due to the intrinsic inert nature of PEEK to organic solvents. In this work, organically modified montmorillonite (MMT) was introduced as a second filler for improving the dispersion of CNTs in the PEEK matrix and enhancing the mechanical properties, as well as reducing the cost of the materials. The nanocomposites were fabricated through melt-mixing PEEK with CNTs/MMT hybrids, which were prepared in advance by mixing CNTs with MMT in water. The introduction of MMT improved the dispersion stability of CNTs, as characterized by sedimentation and zeta potential. The CNTs/MMT hybrids were maintained in PEEK nanocomposites as demonstrated by the transmission electron microscope. The mechanical and thermomechanical measurements revealed that CNTs together with MMT had a strong reinforcement effect on the PEEK matrix, especially at high temperature, although it had a negative effect on the toughness. A maximum increase of 48.1% was achieved in storage modulus of PEEK nanocomposites with 0.5 wt% CNTs and 2 wt% MMT at 240 °C, compared to that of neat PEEK. The differential scanning calorimetry results revealed that CNTs accelerated the crystallization of the PEEK matrix while a further addition of MMT played an opposite role. The nucleation activity of the fillers was also evaluated by the Dobreva method. Full article
(This article belongs to the Section Advanced Nanomaterials)
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Open AccessArticle Electron Transport in Carbon Nanotubes with Adsorbed Chromium Impurities
Materials 2019, 12(3), 524; https://doi.org/10.3390/ma12030524
Received: 8 January 2019 / Revised: 26 January 2019 / Accepted: 30 January 2019 / Published: 10 February 2019
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Abstract
We employ Green’s function method for describing multiband models with magnetic impurities and apply the formalism to the problem of chromium impurities adsorbed onto a carbon nanotube. Density functional theory is used to determine the bandstructure, which is then fit to a tight-binding [...] Read more.
We employ Green’s function method for describing multiband models with magnetic impurities and apply the formalism to the problem of chromium impurities adsorbed onto a carbon nanotube. Density functional theory is used to determine the bandstructure, which is then fit to a tight-binding model to allow for the subsequent Green’s function description. Electron–electron interactions, electron–phonon coupling, and disorder scattering are all taken into account (perturbatively) with a theory that involves a cluster extension of the coherent potential approximation. We show how increasing the cluster size produces more accurate results and how the final calculations converge as a function of the cluster size. We examine the spin-polarized electrical current on the nanotube generated by the magnetic impurities adsorbed onto the nanotube surface. The spin polarization increases with both increasing concentration of chromium impurities and with increasing magnetic field. Its origin arises from the strong electron correlations generated by the Cr impurities. Full article
(This article belongs to the Special Issue Nanocarbon Based Composites)
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Open AccessArticle Temporary Inhibition of the Corrosion of AZ31B Magnesium Alloy by Formation of Bacillus subtilis Biofilm in Artificial Seawater
Materials 2019, 12(3), 523; https://doi.org/10.3390/ma12030523
Received: 10 December 2018 / Revised: 8 January 2019 / Accepted: 26 January 2019 / Published: 10 February 2019
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Abstract
It is well known that microorganisms tend to form biofilms on metal surfaces to accelerate/decelerate corrosion and affect their service life. Bacillus subtilis was used to produce a dense biofilm on an AZ31B magnesium alloy surface. Corrosion behavior of the alloy with the [...] Read more.
It is well known that microorganisms tend to form biofilms on metal surfaces to accelerate/decelerate corrosion and affect their service life. Bacillus subtilis was used to produce a dense biofilm on an AZ31B magnesium alloy surface. Corrosion behavior of the alloy with the B. subtilis biofilm was evaluated in artificial seawater. The results revealed that the biofilm hampered extracellular electron transfer significantly, which resulted in a decrease of icorr and increase of Rt clearly compared to the control group. Moreover, an ennoblement of Ecorr was detected under the condition of B. subtilis biofilm covering. Significant reduction of the corrosion was observed by using the cyclic polarization method. All of these prove that the existence of the B. subtilis biofilm effectively enhances the anti-corrosion performance of the AZ31B magnesium alloy. This result may enhance the usage of bio-interfaces for temporary corrosion control. In addition, a possible corrosion inhibition mechanism of B. subtilis on AZ31B magnesium alloy was proposed. Full article
(This article belongs to the Section Corrosion and Materials Degradation)
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Open AccessReview Ultrasonic Vibration Assisted Electro-Discharge Machining (EDM)—An Overview
Materials 2019, 12(3), 522; https://doi.org/10.3390/ma12030522
Received: 4 December 2018 / Revised: 23 December 2018 / Accepted: 8 January 2019 / Published: 10 February 2019
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Abstract
Many of the industrial processes, including material removal operation for shape generation on the surface of material, exploit the assistance of ultrasonic vibrations. This trend of using ultrasonic vibration in order to improve the process performance is becoming more and more prominent recently. [...] Read more.
Many of the industrial processes, including material removal operation for shape generation on the surface of material, exploit the assistance of ultrasonic vibrations. This trend of using ultrasonic vibration in order to improve the process performance is becoming more and more prominent recently. One of the significant applications of this ultrasonic vibration is in the industrial processes such as Electro-discharge machining (EDM), where ultrasonic vibration (UV) is inserted as a medium for enhancing the process performance. Mostly ultrasonic vibration is applied along with the EDM process to increase the efficiency of the process through debris cleansing from the sparking gap. There have been significant changes in ultrasonic assisted technology during the past years. Due to its inherent advantages, ultrasonic assistance infiltrated in different areas of EDM, such as wire cut EDM, micro EDM and die sinking EDM. This article presents an overview of ultrasonic vibration applications in electric discharge machining. This review provides information about modes of UV application, impacts on parameters of performance, optimization and process designing on difficult-to-cut materials. On the bases of available research works on ultrasonic vibration assisted EDM, current challenges and future research direction to improve the process capabilities are identified. Literature suggested improved material removal rate (MRR), increased surface roughness (SR) and tool wear ratio (TWR) due to the application of ultrasonic vibration assisted EDM. However, tool wear and surface roughness can be lessened with the addition of carbon nanofiber along with ultrasonic vibration. Moreover, the application of ultrasonic vibration to both tool and workpiece results in higher MRR compared to its application to single electrode. Full article
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Open AccessArticle Efficiency of Novel Photocatalytic Coating and Consolidants for Protection of Valuable Mineral Substrates
Materials 2019, 12(3), 521; https://doi.org/10.3390/ma12030521
Received: 5 December 2018 / Revised: 14 January 2019 / Accepted: 29 January 2019 / Published: 9 February 2019
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Abstract
In the process of protection and consolidation of valuable materials, the efficiency is the crucial property that needs to be considered. TiO2/ZnAl layered double hydroxide (LDH) coating and silicate- and carbonate-based consolidants were synthesized and proposed to be used for protection [...] Read more.
In the process of protection and consolidation of valuable materials, the efficiency is the crucial property that needs to be considered. TiO2/ZnAl layered double hydroxide (LDH) coating and silicate- and carbonate-based consolidants were synthesized and proposed to be used for protection and consolidation of four porous mineral substrates: brick, stone, render and mortar. The photocatalytic efficiency of TiO2/ZnAl LDH coating, as well as consolidation efficiency of two consolidants, both applied on model substrates, were studied. The photocatalytic coating showed significant activity and performed well after the durability tests involving rinsing and freezing/thawing procedures. After treatment with both consolidants, a serious enhancement of consolidation of the used substrates was found. On the other hand, the application of TiO2/ZnAl LDH, as well as consolidants, caused negligible changes in the water vapour permeability values and in appearance of the porous mineral substrates, indicating a high level of compatibility. Full article
(This article belongs to the Special Issue Self-Cleaning Surfaces)
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