Low-phosporous nickel-coated carbon microcoils: Controlling microstructure through an electroless plating process

Carbon microcoils (CMCs) have been coated with a nickel-phosphorus (Ni-P) film using an electroless plating process, with sodium hypophosphite as a reducing agent in an alkaline bath. CMC composites have potential applications as microwave absorption materials. The morphology, elemental composition and phases in the coating layer of the CMCs and Ni-coated CMCs were investigated by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD), respectively. The effects of process parameters such as pH, temperature and coating time of the plating bath on the phosphorus content and deposition rate of the electroless Ni-P coating were studied. The results revealed that a continuous, uniform and low-phosphorous nickel coating was deposited on the surface of the CMCs for 20 min at pH 9.0, plating bath temperature 70 °C. The as-deposited coatings with approximately 4.5 wt.% phosphorus were found to consist of a mix of nano- and microcrystalline phases. The mean particle size of Ni-P nanoparticles on the outer surface of the CMCs was around 11.9 nm. The deposition rate was found to moderately increase with increasing pH, whereas, the phosphorous content of the deposit exhibited a significant decrease. Moreover, the material of the coating underwent a phase transition between an amorphous and a crystalline structure. The thickness of the deposit and the deposition rate may be controlled through careful variation of the coating time and plating bath temperature.     

Synthesis and elevated temperature performance of a polypyrrole-sulfur-multi-walled carbon nanotube composite cathode for lithium sulfur batteries

A sulfur-multi-walled carbon nanotube composite (S/MWCNT) was prepared using a two-step procedure of liquid-phase infiltration and melt diffusion. Polypyrrole (PPy) conductive polymer was coated on the surface of the as-prepared S/MWCNT composite by in situ polymerization of pyrrole monomer to obtain PPy/S/MWCNT composite. The composite materials were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). The electrochemical performance of the as-prepared cathode material was investigated at 25, 40, and 70 °C at various rates. It was found that temperature has dual effects on the performance of Li/S cells. Increasing the temperature, on one hand, facilitates the lithium ion transport through the cathode and, on the other hand, leads to faster dissolution of active material into the electrolyte. The PPy coating can effectively trap polysulfides in its porous structure, even at elevated temperatures, leading to the improvement of the discharge capacity, the cycle stability, and the coulombic efficiency. The electrochemical impedance spectroscopy (EIS) results reveal that the PPy coating reduces the formation of passive layer on the cathode surface, even at high temperatures, resulting in a better elevated temperature performance. A high reversible capacity of 945 mAh g^?1 was maintained after 50 cycles for the PPy/S/MWCNT composite at 70 °C at a rate of 0.5 C.     

Preparation of Gelatin coated hydroxyapatite nanorods and the stability of its aqueous colloidal

This paper describes a novel process for preparing Gelatin coated hydroxyapatite (HAp) nanorods to improve the stability of its aqueous colloid. As Gelatin is a typical protein with abundant hydroxyls, carboxys and imines, it is a very effective functional group to attach onto the surfaces of the HAp particles. Our data show that the Gelatin layer firmly coated on the hydroxyapatite nanorods, and their structure and interfacial chemical bonding have been studied using various techniques, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), high-resolution transmission electron microscopy (HRTEM), differential thermal analysis (DTA) and thermal gravimetric analysis (TGA). The reaction temperature, pH, amount of Gelatin, and Ca/P molar ratio in the material determine the quality of Gelatin coating and the stability of the HAp in aqueous solution. Moreover, an interesting phenomenon was found that the Gelatin coated HAp sediment separated by centrifugal was easily dispersed in water and forms HAp aqueous suspension. The suspension was stable for more than 24 h.     

Polymer-Nanoparticle Composites Composed of Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) and Coated Silver Nanoparticles

The effects of addition of synthesized organic-suspension silver nanoparticles on the crystallization and thermal stability of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) were studied by transmission electron microscopy (TEM), differential scanning calorimetry (DSC), wide-angle X-ray diffraction (XRD), UV-Vis absorption spectroscopy, polarized optical microscopy (POM), and thermal gravimetric analysis (TGA). The TEM images showed the average primary size of the as-synthesized silver nanoparticles, coated with a monolayer of the surfactants consisting of oleic acid and an alkylamine, was about 5 nm with narrow distribution, and that they were uniformly dispersed in n-heptane. PHBV/silver nanocomposites were prepared by melt mixing in an internal mixer and then injection molded into rectangle-shaped specimens by a labscale injection molding device. The coated silver nanoparticles showed a homogenuous dispersion in the PHBV matrix when the content of coated silver nanoparticles was about 1%. Both the DSC and POM data showed the efficient heterogeneous nucleation by the coated silver nanoparticles for facilitating PHBV crystallization. The thermal stability of the PHBV/silver nanocomposites improved with the increase in the content of the coated silver nanoparticles.     

Influence of heat treatment on structure and some physical properties of lithium boro-niobate glass

The glass composition (90?mol% Li₂B₄O₇–10?mol% Nb₂O₅) was prepared by the melt quenching technique. The quenched sample was heat treated at 480°C, 545°C and 630°C for 5?h and heat treated at 780°C with different time. The times were 5, 10, 15, 20, 28, and 36?h. The glass and glass ceramics were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and dc conductivity as a function of temperature. Lithium niobate (LiNbO₃) and lithium diborate (Li₂B₄O₇) were the main phases in glass ceramic addition to traces from LiNb₃O₈. Crystallite size of the main phases determined from the X-ray diffraction peaks are in the range <100?nm. The fraction of crystalline (LiNbO₃) phase increases with increase the heat treatment temperature and time. The relation between physical properties and structure were studied.     

Preparation of graphene-glass fiber-resin composites and its electromagnetic shielding performance

The surface of the glass fiber (GF) was modified by silane coupling agent (KH550) and bovine serum albumin (BSA), and then the graphene oxide (GO) was coated onto the modified surface of the glass fiber. Followed by a reduction reaction, the reduced graphene oxide (RGO) coated on glass fiber was obtained. Finally, the reduced graphene oxide-glass fibers (RGO-GF) were combined with unsaturated resins. The interfacial morphology of reduced graphene oxide-glass fibers was investigated by scanning electron microscopy (SEM). The structure of the materials was analyzed by Fourier transform infrared spectroscopy (FT-IR). The crystal phases of the material were identified by X - ray diffraction (XRD). The mechanical properties and electromagnetic shielding effectiveness of the sample were tested. The results showed that the interface between glass fibers and graphene binds more closely after the glass fibers was treated by KH550. The tensile strength of the RGO-GF composites reached 85.05 MPa. Compared with the GF composites, it increased by 51.4% when the glass fibers content was 30%. The shielding effectiveness of the composites reached 21.3 dB at the frequency range of 8.2–12.4 GHz (x-band). Therefore, by coating the surface with reduced graphene oxide, the glass fibers can make a great shielding effect on the electromagnetic wave.     

Synthesis and Properties of Polyphenylsilsesquioxane Modified Phenolic Resin by in-situ Polymerization from Phenyltriethoxysilane Precursor

A series of phenolic resin-polyphenylsilsesquioxane (PR-PPSQ) composites were prepared by in situ formation from phenyltriethoxysilane (PTES) precursor during polymerization of the PR. The precursor was firstly hydrolyzed in a solution, and then the sol was added to the PR polymerization system. The structures of the composites were investigated by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and solid-state ²⁹Si nuclear magnetic resonance (Si-NMR). The PPSQs were spherical particles with a diameter of about 3 µm and nearly uniformly dispersed in the matrix, as revealed by scanning electron microscopy (SEM). The influence of PTES content on the thermal behavior of the PR was characterized by thermogravimetric analysis (TGA) in nitrogen and air atmospheres. The results showed that the onset temperature and residual weight of the composite containing 20 wt% PTES content were improved by 47°C and 8.4%, respectively, compared to the pure PR. The thermal oxidative stability was also greatly increased; the 50 wt% weight loss temperature rose from 567°C for PR to 601°C. The flexural strength of the composites was improved; in particular, the value of the composite containing 15 wt% PTES content was elevated by 32% (from 41.66 to 55.33 MPa).     

Electrochemical characterization of ionic liquid based gel polymer electrolyte for lithium battery application

High molecular weight polymer poly(vinylidenefluoride-co-hexafluoropropylene) (PVdF-HFP), ionic liquid 1-ethyl-3-methylimidazolium bis(fluorosulfonyl)imide (EMIMFSI), and salt lithium bis(trifluoromethanesulfonyl)imide (LiTFSI)-based free-standing and conducting ionic liquid-based gel polymer electrolytes (ILGPE) have been prepared by solution cast method. Thermal, electrical, and electrochemical properties of 80 wt% IL containing gel polymer electrolyte (GPE) are investigated by thermogravimetric (TGA), impedance spectroscopy, linear sweep voltammetry (LSV), and cyclic voltammetry (CV). The 80 wt% IL containing GPE shows good thermal stability (~?200 °C), ionic conductivity (6.42?×?10^?4 S cm^?1), lithium ion conductivity (1.40?×?10^?4 S cm^?1 at 30 °C), and wide electrochemical stability window (~?4.10 V versus Li/Li⁺ at 30 °C). Furthermore, the surface of LiFePO₄ cathode material was modified by graphene oxide, with smooth and uniform coating layer, as confirmed by scanning electron microscopy (SEM), and with element content, as confirmed by energy dispersive X-ray (EDX) spectrum. The graphene oxide-coated LiFePO₄ cathode shows improved electrochemical performance with a good charge-discharge capacity and cyclic stability up to 50 cycles at 1C rate, as compared with the without coated LiFePO₄. At 30 °C, the discharge capacity reaches a maximum value of 104.50 and 95.0 mAh g^?1 for graphene oxide-coated LiFePO₄ and without coated LiFePO₄ at 1C rate respectively. These results indicated improved electrochemical performance of pristine LiFePO₄ cathode after coating with graphene oxide.     

The kinetics of Cr layer coated on TiNi films for hydrogen absorption

The effect of hydrogen absorption on electrical resistance with temperature for TiNi and TiNi-Cr thin films was investigated. The TiNi thin films of thickness 800 Å were deposited at different angles (? = 0°, 30°, 45°, 60° and 75°) under 10^?5 Torr pressure by thermal evaporation on the glass substrate at room temperature. A layer of Cr of thickness 100 Å was coated on the TiNi thin films. The changing rate of hydrogen absorption increases after Cr layer coating because Cr enhances the catalytic properties of hydrogen absorption in thin films. The rate of hydrogen absorption increases with temperature at lower range but at higher range of temperature it was found to decrease and also it was found that the hydrogen absorption increases with angle of deposition.     

The optimized preparation and electrochemical properties of LiMn1.95Co0.05O4 and Al2O3-coated LiMn1.95Co0.05O4

Cathode material LiMn_1.95Co_0.05O₄ for lithium ion battery was synthesized via solid state reaction, and calcination temperature and time were investigated, respectively. Thermogravimetry (TG) and differential thermal analysis (DTA) measurements were utilized to determine the calcination temperature of precursor sample. The optimized calcination temperature and time are 850 °C and 15 h. The surface of LiMn_1.95Co_0.05O₄ cathode is coated using Al₂O₃ coating materials. The phase structures, surface morphologies, and element types of the prepared LiMn_1.95Co_0.05O₄ and Al₂O₃-coated LiMn_1.95 Co_0.05O₄ were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and energy spectrum analysis (EDS). The 0.5 wt% Al₂O₃-coated compound exhibited better specific capacity and capacity retention than bare sample. The initial discharge capacity was 140.9 mAh/g and capacity retention was 96.7 % after 10 cycles at 0.1 C. Such enhancements are attributed to the presence of a stable Al₂O₃ layer which acts as the interfacial stabilizer on the surface of LiMn_1.95Co_0.05O₄.     

Thermal and magnetic behavior of Angustifolia Kunth bamboo fibers covered with Fe3O4 particles

Several Angustifolia Kunth bamboo fibers, which have been previously treated with an alkaline solution, were coated with magnetite particles. The coating of the fibers was achieved by an in-situ co-precipitation method with Fe²⁺ and Fe³⁺in NaOH or NH₄OH. The fibers were evaluated by chemical analysis using atomic absorption (A.A.) technique, structural characterization by X-ray diffraction (XRD), thermal stability with thermo-gravimetric analysis (TGA) in nitrogen at temperature range between 23 °C and 800 °C and magnetic behavior using vibrating sample magnetometry (VSM) applying a magnetic field between −27 KOe and 27 KOe at room temperature. We found that the thermal stability and magnetization depend of the synthesis method used to cover the Angustifolia Kunth bamboo fibers. In addition, an improved magnetic response was observed when NaOH solution is used to generate the magnetite coating on the fiber surface.     

Annealing Effects on the Structural and Optical Properties of Thermally Deposited Tin Antimony Sulfide Thin Films

We report the deposition and characterization of tin antimony sulfide thin films on a soda glass substrate by a thermal evaporation technique. The thin films were annealed in argon gas at 150, 175, and 300 °C inside glass ampoules. The structural and optical properties of the deposited and annealed films are investigated. X-ray diffraction (XRD) patterns show that the films are polycrystalline in structure. Photoconductivity plot revealed good response in the NIR and visible regions, while the films show no transmittance below 700 nm. The absorption coefficient was of the order of 10⁶ cm^?1. Optical band gaps were also evaluated and a decrease in band gap was observed due to annealing. Hot point probe technique was employed for type of conductivity.     

Protective silicon coating for nanodiamonds using atomic layer deposition

Ultrathin silicon coating was deposited on nanodiamonds using atomic layer deposition (ALD) from gaseous monosilane (SiH₄). The coating was performed by sequential reaction of SiH₄ saturated adsorption and in situ decomposition. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were utilized to investigate the structural and morphological properties of the coating. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were used to compare the thermal stability of nanodiamonds before and after silicon coating. The results confirmed that the deposited cubic phase silicon coating was even and continuous. The protective silicon coating could effectively improve the oxidation resistance of nanodiamonds in air flow, which facilitates the applications of nanodiamonds that are commonly hampered by their poor thermal stability.     

Induced Electronic and Thermal Effects of 86 MeV Nickel Ions in Bisphenol-A Polycarbonate

Bisphenol-A polycarbonate films were irradiated with 86 MeV swift heavy nickel ions at varying fluences, ranging from 1 × 10¹¹ to 1 × 10¹³ ions cm^?2, under vacuum at room temperature, to analyze the induced electrical and thermal modifications. AC conductivity measurements and UV-visible spectroscopy, Fourier transform infra-red (FTIR) spectroscopy, thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) techniques were applied to analyze the changes. A significant, exponential increase in conductivity at higher frequency was observed with the increase of nickel ion fluence. UV-visible analysis corroborated the results of the AC conductivity measurement, revealing the increase in size of the carbon clusters embedded in the polymer network, with the increase of heavy ion fluence. FTIR analysis revealed the formation of alkene and alkyne end groups at higher doses, which further supported the suggestion that the variation in electrical properties induced by the ion irradiation of the polymer was due to development of a carbonaceous phase inside the polymer due to the irradiation. Thermal analysis, i.e., TGA and DSC patterns, showed that chain-scission was the leading phenomena in the heavy ion-irradiated polycarbonate samples, resulting in degradation of their thermal stability.     

A new hyperbranched star polyether electrolyte with high ionic conductivity

Hyperbranched poly(glycidol) containing hydroxyl groups was firstly synthesized via anionic polymerization and then reacted with 2-bromoisobutyl bromide to form macroinitiator HPG-Br. Finally, a hyperbranched star polymer (HPG-PPEGMA) was successfully prepared by atom transfer radical polymerization (ATRP) of poly(ethylene glycol) methyl ether methacrylate using HPG-Br as macroinitiator. The structures and properties of the obtained polymers were characterized by ¹H NMR, attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), differential scanning calorimetry (DSC), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). The ionic conductivity of the polymer electrolytes composed of HPG-PPEGMA and lithium bis(trifluoromethanesulfonimide) (LiTFSI) was investigated via electrochemical impedance spectroscopy. The results showed that the room temperature ionic conductivity of the prepared hyperbranched star polymer electrolytes had a higher ionic conductivity. When [EO]/[Li] was 20, the ionic conductivity of the hyperbranched star polymer electrolyte was up to 1?×?10^?4 Scm^?1 at 30 °C. The onset decomposition temperature of the hyperbranched star polyether could reach 374 °C, indicating that the hyperbranched star polymer had a good thermal stability. The XRD results showed that the structure of the hyperbranched star polymer was beneficial to improve the ionic conductivity due to possessing a low degree of crystallinity.     

Improving the thermal properties of fluoroelastomer (Viton GF-600S) using carbon nanotube

Nanocomposites were prepared using carbon nanotubes (CNTs) in the formulations of fluoroelastomer (FE). Thermogravimetric analysis (TGA) results revealed that CNT improved the thermal properties of FE, resulting in higher amount of FE and char remaining within the temperature range of 520–900 °C, relative to unfilled FE and carbon black (CB)-filled FE. The same results also revealed that more percentage of FE was undegraded or less degraded especially near CNT. Energy dispersive X-ray (EDX) results indicated that the percentage of carbon and fluorine in the residue of TGA scans up to 560 °C of CNT-filled FE (CNT/FE) were higher compared to the CB-filled FE (CB/FE), and CB/FE was higher than FE. EDX results of TGA residue (run up to 900 °C) showed that most of the undegraded FE which was not degraded at temperatures below 560 °C was degraded from 560 °C to 900 °C in both CNT/FE and CB/FE, with the char in CNT/FE being more than that in CB/FE. Residue of samples after TGA scans up to 900 °C indicated that, Zn did not undergo any reaction with CNT in the CNT/FE. In CB/FE, some percentage of ZnO reacted with carbon. EDX analysis of thermal aged specimens under air showed that with increasing aging time, more percentage of C, O, and F were lost from the surface of filler/FE and FE. The order of element loss is: CNT/FE < FE < CB/FE.     

Poly(ethylene oxide)-lithium difluoro(oxalato)borate new solid polymer electrolytes: ion–polymer interaction,structural, thermal,and ionic conductivity studies

Solid polymer electrolytes based on high molecular weight poly(ethylene oxide) (PEO) complexed with lithium difluoro(oxalato)borate (LiDFOB) salt in various EO:Li molar ratios from 30:1 to 8:1 were prepared by using solution casting technique. Ion–polymer interaction, structural, thermal, and ionic conductivity studies have been reported by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), polarized optical microscopy (POM), differential scanning calorimeter (DSC), and impedance analysis. FTIR spectral studies suggested that the interaction of Li⁺ cations with the ether oxygen of PEO, where a triple peak broad band centered at 1105 cm^?1, corresponds to C–O–C stretching and extreme deformation occurs. XRD, POM, and DSC indicated that the inclusion of LiDFOB salt could reduce the crystallinity of PEO. The melting temperature of PEO shifted to lower temperature side by the addition of LiDFOB. The glass transition temperature obtained for the system 10:1 was ?38.2 °C. An increase in the ionic conductivity from 3.95?×?10^?9 to 3.18?×?10^?5 S/cm at room temperature (23 °C) was obtained through the addition of LiDFOB to a high molecular weight PEO. In addition, the ionic conductivity of the polymer electrolyte films followed an Arrhenius relation, and the activation energy decreased with increasing LiDFOB concentration.     

Preparation and Characterization of Para-Aramid Fibers with the Main Chain Containing Heterocyclic Units

Abstract

A para-aramid fiber whose main chain contained heterocyclic units was prepared by low temperature copolycondensation, wet-spinning, and high temperature thermal treatment. The prepared fibers (named F-368) and two commercial aramid fibers, K49 (Kevlar 49, Dupont de Nemours Co., USA) and APMOC (Kamenskvolokno and Tver’khimvolokno, Russia), were characterized and analyzed in detail. Infrared spectroscopy (IR) and wide-angle X-ray diffraction (WAXD) were employed to characterize their chemical and aggregation structures, respectively. The results showed the introduction of heterocyclic units into the wholly para-aromatic polyamide backbone of K49 in the F-368 and APMOC reduced the crystallinity significantly. The tenacity of F-368 and APMOC were 32.2 and 30.5cN/dtex, which were about 68% and 59% higher than that of K49, respectively. Thermogravimetric analysis (TGA) and dynamic mechanical analysis (DMA) were used to investigate their thermal properties; the results indicated that these aramid fibers showed exceptional thermal properties with glass transition temperatures of 240–260?°C, and decomposition temperatures at 510–560?°C, both in nitrogen and air. The TGA results also showed the decomposition mechanism of K49 and the heterocyclic aramid fibers in nitrogen and air were different. The decomposition temperature of K49 was higher than that of the heterocyclic copolyaramid fibers both in nitrogen and air. On the contrary, the char yields of the heterocyclic copolyaramid fibers at 800?°C were higher than that of K49 in both nitrogen and air.     

Interfacial p-n heterojunction of polyaniline-nickel ferrite nanocomposite as room temperature liquefied petroleum gas sensor

In this work, we introduce polyaniline–nickel ferrite (PANI-NF) nanostructured composite to detect liquefied petroleum gas (LPG) at room temperature. The composite synthesized by relatively simple method of in-situ chemical polymerization was structurally characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. The presence of characteristic absorption bands of both PANI and NF in the FTIR spectrum of the composite with small shifts confirmed interfacial interaction of PANI with NF. The XRD studies also confirmed interfacial interaction between PANI and NF in the composite and its crystalline nature with an average crystallite size of 20 nm. Highly agglomerated granular porous morphology favourable for LPG adsorption was revealed by SEM image of the composite. The TEM image of the composite clearly showed nanosized NF particles embedded in PANI matrix. The LPG sensing performance of the composite at room temperature was tested using a film prepared by depositing the composite on an ordinary glass substrate by cost-effective spin coating technique. The maximum sensing response of the composite was found to be 57% at 700 ppm of LPG, with a response time of 50 s and a recovery time of 200 s. The composite was found to be stable for a period of one month. The sensing mechanism has been discussed on the basis of formation of interfacial p–n heterojunction barrier.     

Electrical, structural, and optical properties of ITO thin films prepared at room temperature by pulsed laser deposition

Indium tin oxide (ITO) thin films were prepared by pulsed laser deposition (PLD) on glass substrate at room temperature. Structural, optical, and electrical properties of these films were analyzed in order to investigate its dependence on oxygen pressure, and rapid thermal annealing (RTA) temperature. High quality ITO films with a low resistivity of 3.3 × 10⁻⁴ Ω cm and a transparency above 90% were able to be formed at an oxygen pressure of 2.0 Pa and an RTA temperature of 400 °C. A four-point probe method, X-ray diffraction (XRD), atomic force microscopy (AFM), and UV-NIR grating spectrometer are used to investigate the properties of ITO films.