Synthesis of high performance organic–inorganic composite via click coupling of block polymer and polyhedral oligomeric silsesquioxane

Novel hybrid systems based on poly(styrene-b-(ethylene-co-butylene)-b-styrene) (SEBS) and a polyhedral oligomeric silsesquioxane (POSS) have been synthesized via click chemistry. Different compositions of SEBS-functionalized POSS were obtained from the reaction of azide-functionalized styrene units of SEBS with alkyne-functionalized POSS molecules. Characterization of SEBS-functionalized POSS by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and nuclear magnetic resonance spectroscopy revealed that the POSS molecules were successfully attached to the phenyl group of the SEBS polymer chain following the click reaction. Homogeneous dispersion of POSS molecules in the polymer matrix was demonstrated by scanning electron microscopy. The POSS molecule showed excellent compatibility with polymer matrix, and as a consequence the remarkable enhancement of mechanical properties (breaking stress = 44%, modulus = 285%) and thermal stability for the resulting composite films was achieved. The reinforcing effect is ascribed to both the compatible homogeneous dispersion of POSS in the matrix and the covalent bond between SEBS and POSS molecules arising from the click coupling.     

Preparation and performance of PANI–PVA composite film doped with HCl

The polyaniline (PANI)–poly (vinyl alcohol) (PVA) composite film doped with HCl was prepared by adopting PVA as matrix. Effects of PVA content and film drying temperature on properties of HCl–PANI–PVA composite film were studied. A comparison was made for tensile strength, elasticity, conductivity and thermal stability of PVA, HCl–PANI or HCl–PANI–PVA. PVA film presented the highest tensile strength and elasticity (150.8?MPa and 300.0%), but its conductivity was the lowest. The conductivity of HCl–PANI–PVA was the highest (1500?S?m^?1), and tensile strength and elasticity of HCl–PANI–PVA were higher than those of HCl–PANI. The order of their thermal stability is PVA?>?HCl–PANI?>?HCl–PANI–PVA before 260°C, and the order of their thermal stability is HCl–PANI?>?HCl–PANI–PVA?>?PVA after 260°C. At the same time, the structure and conductive mechanism of composite materials were characterised and analysed through infrared and scanning electron microscopy (SEM).     

Synthesis and performance of TiB2–B4C composites by high pressure of TiC–B mixture

TiB₂–B₄C composites were in situ synthesized and consolidated by high pressure synthesis method from a mixture of TiC and B powders at the pressure and temperature of 5.0 GPa and 1500℃-1900℃. The phase composition, microstructure, density, hardness, thermal conductivity, and electrical resistivity of TiB₂–B₄C composites were analyzed. As the increase in the synthesis temperature, the products were TiB₂ and B₄C phases and that crystallinity improved. TiB₂–B₄C composites were dense without obvious pores. TiB₂–B₄C composites synthesized at 1800℃ obtained the optimized performance, including the relative density of 98.2%, the Vickers hardness of 31.7 ± 1.2 GPa with the load of 9.8 N, the thermal conductivity of 30.3 ± 0.7 W/(m K), and the electrical resistivity of 3.3 × 10⁻³ Ω cm, respectively. The grain size of the TiB₂–B₄C composites changed with the increase in synthesis temperature, leading to the changes in hardness, thermal conductivity, and electrical resistivity.     

Achieving ultrabroad temperature stability range with high dielectric constant and superior energy storage density in KNN–based ceramic capacitors

Multilayer ceramic capacitors (MLCCs) had become an important component of many electronic devices on account of its miniaturization, high capacitance and reliability. To satisfy the requirements of MLCCs, the temperature–insensitivity and dielectric properties of the dielectric ceramics were urgent to be enhanced. In our work, (1–x)K_0.5Na_0.5NbO₃–xBi(Li_0.5Nb_0.5)O₃ (abbreviated to KNN–xBLN) were successfully synthesized by traditional solid state reaction method. On the one hand, the doping BLN induced the diffused phase transition and broadened the dielectric anomaly peaks, which improved the temperature insensitivity of KNN-based ceramics. On the other hand, the nanosized grains and dense microscopy boosted the breakdown electric field. Ultimately, the KNN–0.175BLN samples presented the excellent dielectric properties with high dielectric constant (1735) and low dielectric loss (1.9%) at room temperature with a wide temperature stability range (–62 – 300 °C), which exhibited the wider temperature stability range than X9R specification. Meanwhile, the x = 0.175 samples also achieved a high recoverable energy storage density of 3.71 J/cm³ under the breakdown electric field of 360 kV/cm. The designed KNN–based dielectric materials were expected to be applicable to the energy storage capacitor with standed high operating temperature.     

Preparation of the novel B4C–SiC composite aerogel with high compressive strength and low thermal conductivity

Journal of Porous Materials - A novel B4C–SiC composite aerogel is synthesized using nano boron carbide suspension, 3-aminopropyltriethoxysilane (APTES), and resorcinol–formaldehyde...     

Synthesis and evaluation of water-reducible acrylic–alkyd resins with high hydrolytic stability

Relatively poor hydrolytic stability is one of the major drawbacks of waterborne alkyd resins. Therefore, the shelf life of the paints containing these kinds of resins is usually short. In this research, the hydrolytic stability of water-reducible alkyd resins has been improved by employing polyacid acrylic copolymers in alkyd resins structure. In addition, the effect of other raw materials (such as neutralizing agent) and synthesis conditions on the resins properties was investigated. The results showed that the optimum synthesized water-reducible acrylic–alkyd resins had a high hydrolytic stability and their acid values increased only 23.5% after 4 months storage at ambient temperature. The synthesized resin was also used in an air-drying water-reducible lacquer formulation and its physical and mechanical properties were evaluated.     

Synthesis and characterization of diopside glass–ceramic matrix composite reinforced with aluminum titanate

Glass–ceramic composites in the SiO₂–CaO–MgO–(Na₂O) system, reinforced with 5, 10 and 20 wt.% aluminum titanate were synthesized by pressureless sintering. Optimum sintering temperatures with maximum relative density were determined for each composition. The composites were fired above the crystallization peak temperature of glass–ceramic. Mechanical properties of glass–ceramic and sintered composites, such as fracture toughness, flexural strength and Vickers microhardness, were investigated. The sintered composites were characterized by scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS) and X-ray diffraction (XRD). The results showed that the composite containing 10 wt.% aluminum titanate has desirable behavior in comparison to the base glass–ceramic and the other compositions. It seems that crack deflection by aluminum titanate particles is the prevalent mechanism for improving mechanical characteristics.     

Dual phase nano-particulate AlN composite — A kind of ceramics with high strength and ductility

Ceramics are widely used in many fields due to their excellent properties. However, the brittle fracture is a short board restricting their applications. To understand their deformation mechanism and explore a way to enhance both the strength and ductility, we investigated the mechanical behaviour of dual-phase AlNs composed of amorphous AlN matrix and crystalline nanoparticles under compression via molecular dynamics simulations. The stress concentration exists at the interface of nanocomposite AlN, where the particles and matrix are in the tensile and compressive states of stress, respectively. Strain hardening occurs when crystalline nanoparticle fraction f_v ≥ 40.9%, attributed to the intersection between shear bands. The phase transformation from wurtzite structure (B4) to graphene-like structure (GL) is observed in the crystalline phase, as a result of high hydrostatic stress. After phase transformation, the particle might be cut into half during further compression along with the recovery of the GL structure to the wurtzite structure that could still bear load. The investigation of the effects of the volume fraction, surface-to-volume ratio, distribution pattern of the crystalline nanoparticles indicates that the dual-phase AlN nanocomposite with f_v ≥ 40.9% and triangle distribution of particles would possess both higher strength and ductility.     

The superlattice structure and self-adaptive performance of C–Ti/MoS2 composite coatings

To improve the self-adaptability of MoS₂ coating in different environments, the coatings were doped with functional C and Ti by unbalanced magnetron sputtering system. The clear superlattice structure with minimal modulation period was investigated by High Resolution Transmission Electron Microscope (HRTEM). The co-doped coatings have better mechanical properties due to the special structure and the formation of C–Mo, Ti–S and Ti–O bonds, and better lubrication performance in both high humidity and vacuum than those of the single-doped ones. The doped Ti not only facilitates the formation of the MoS₂ (002) basal plane, but also improves the oxidation resistance of the composite film. The degree of friction-induced graphitization on the wear tracks and the quality of transfer films on the wear scars are key factors affecting the lubrication performance of the composite film. In the high-humidity environment, the reasonable doping elements can promote the formation the high-quality transfer film by interacting with H₂O water molecules, which will benefit the lubrication of the coating better. Our findings deepen the understanding of MoS₂ composite coating and provide a new solution for improving the self-adaptability of the coating.     

Role of Mg–O on phase stabilization in solution combustion processed rocksalt structured high entropy oxide (CoCuMgZnNi)O with high dielectric performance

High entropy oxide (CoCuMgZnNi)O with a phase pure rocksalt was synthesized using low-temperature solution combustion. The precursors were found to combust at 270 °C and 400 °C was considered to be the formation temperature. The high entropy rocksalt oxide (HERO) fully stabilized at 1000 °C shows a single-phase, fcc rocksalt structure with an Fm-3m space group. HERO displays one of its parent oxide Mg–O structural properties as both belong to the cubic family and had lattice parameters very close to each other. The lower cation systems exhibited a transition from spinel to rocksalt structure with the addition of Mg–O. Raman of HERO affirmed a completely disordered occupancy of various metal cations, the formation of HERO at 400 °C, and phase stabilization at 1000 °C. Dielectric measurements at room temperature showed high permittivity (κ) with magnitudes ∼1.9 × 10³, 4.7× 10¹, and 0.9 × 10¹ at 100, 1k, and 100k Hz.     

In-situ synthesis of Al2O3-reinforced high Nb–TiAl laminated composite with an enhanced strength-toughness performance

In this work, the Al₂O₃-reinforced high Nb–TiAl laminated composite is successfully fabricated by an innovative way of direct-current magnetron sputtering combined with the foil-foil metallurgy, with assistance of vacuum hot-pressed sintering. Here, the Nb-coated aluminum foil and titanium foil, microstructure evolution, the lamellar plane distribution and the mechanical performances are carefully studied. Specifically, the composite is composed of the α₂-Ti₃Al, γ-TiAl and α-Al₂O₃ phase, in which the high Nb–TiAl matrix has a fully lamellar microstructure and a high content (～6.5%) of Nb. Taken the textured titanium foil as raw material, the multi-stage annealing process is proved to be an effective way to control the lamellar plane distribution in the high Nb–TiAl matrix, showing that 82.3% of the lamellar planes forms an angle less than 30° from the RD-ND plane of the composite. Moreover, the bending strength and fracture toughness of the composite reach 817 MPa and 12.41 MPa m^1/2, respectively. Further, the toughening and strengthening mechanisms are also detailly discussed. We believe that the major findings in this work can provide a new idea to design the high strength-toughness intermetallic-ceramic composites.     

Synthesis and anticorrosion performance of poly(2,3-dimethylaniline)–TiO2 composite

Poly(2,3-dimethylaniline)–TiO₂ composite (PTC) was prepared by oxidative polymerization of 2,3-dimethylaniline in phosphoric acid medium with ammonium persulphate as oxidant. The composite was characterized by Fourier transformation infrared (FTIR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). TiO₂ particles, rather being simply blended or mixed up, are encapsulated or entrapped into the polymer core, resulting in some significant improvement in its anticorrosion properties. Suitable coating with PTC was formed on steel using epoxy resin, and its corrosion resistance behavior was studied by open circuit potential (OCP) and electrochemical impendence spectroscopy (EIS) in 3.5% NaCl solution and also compared with that of PANI and poly(2,3-dimethylaniline) (P(2,3-DMA)). It has been found out that the coating containing PTC has got higher corrosion resistance than that of PANI and P(2,3-DMA).     

Microstructure and performance of brazed diamond segments with NiCr–x(CuCe) composite alloys

Novel multi-layer brazed diamond segments were fabricated using NiCr–x(CuCe) composite alloys. Differential scanning calorimetry curves of the composite alloys were measured and analysed. The microstructures of the alloy segments and surface topographies of the brazed diamond segments were characterised. Performance tests of the alloy segments and brazed diamond segments were performed. The undercooling degree of the Ni–Cr alloy in the composite alloy increased with the Cu–Ce alloy addition, which led to coarse NiCu-rich regions and Ni₃Si phases. A brazed diamond segment with a 5% Cu–Ce alloy addition exhibited the highest wear resistance and machining performance and the best surface morphology after a wear test. An excessive Cu–Ce alloy addition led to a rapid decrease in wear resistance of the brazed diamond segment owing to the large number of coarse NiCu-rich phases falling off from the composite alloy. The mechanism of the reduction in thermal damage to diamonds by the Cu–Ce alloy is elucidated. Initially the Cu–Ce particles melted and mainly Ni atoms diffused into the Cu–Ce liquid, thereby leading to the formation of NiCu-rich regions and Ce₂Ni₇ and CeNi₂ phases, which in turn promoted the diffusion. The melting temperature of the Ni–Cr composite alloy was significantly reduced by the addition of the Cu–Ce alloy.     

The high temperature reaction of ammonia with carbon and SiC–C ceramics

This contribution aimed at developing a treatment under ammonia in order to eliminate free carbon from the surface of SiC-based fine ceramics like fibers or coatings. The reaction of NH₃ with graphitic and non-graphitic carbon was first investigated through kinetic measurements, in situ gas phase analysis and physicochemical investigations of the solid. The carbon etching rate is controlled by heterogeneous reactions involving active sites arising from bulk structural defects and the formation of HCN. A selection of SiC-based fibers and coatings with various carbon contents and (micro)structures was treated in ammonia in favorable conditions. The analyses of the tested SiC–C specimens revealed a reduction of the free carbon content and, simultaneously, a nitridation of the initial Si–C–(O) continuum over a reaction layer. The growth rate, composition and the volume change of this layer vary with the initial microstructure. The ammonia treatment is able to restore the adhesion of carbon-contaminated surfaces.     

Dodecenyl succinic-β-cyclodextrin with high degree of substitution: Synthesis,characterization and evaluation

β-cyclodextrin (β-CD) has the characteristics of safety, non-toxicity, and a wide range of sources. It can be used in improving surface activity. However, due to the limitation of molecular polarity and solubility, its surface activity and emulsification ability are weak. Therefore, it is necessary to improve adsorption capacity on phase interface by hydrophobic modification. In this article, dodecenyl succinic-β-cyclodextrin (DDS-β-CD) with different substitution degree was prepared by esterification of β-CD with dodecenyl succinic anhydride (DDSA) as the esterifying agent. The product was characterized by FT-IR, ¹H NMR, SEM, and TGA, respectively. Results showed that DDS was successfully introduced into β-CD. Both the degree of substitution (DS) and productivity (P) increased with the addition of DDSA and can reach 0.283 and 85.8%, respectively, when the molar ratio of DDSA to β-CD was 3:1. The modified cyclodextrin showed lower surface tension and higher foaming ability. Compared with octenyl succinic-β-cyclodextrin (OS-β-CD), it was found that the length of hydrophobic segment had a significant effect on the surface tension. Due to its unique properties, it can be used as a good emulsifier for oil-in-water emulsions and a host material for lavender flavor.     

Optimization of SiC–ZrC high emissivity composite flexible coating for thermal protection with high interfacial bond strength and temperature resistance

Aluminum silicate fiber fabric (ASFF) has been widely used in the outer surface of flexible insulation felt on the leeward side of aerospace vehicle. In order to improve the temperature resistance of ASFF, a kind of SiC–ZrC composite coating was prepared on the surface of fiber fabric via spraying method with SiC as emittance agent and ZrC as additive. The surface morphology and mechanical properties of the coating were studied. Compared with the single-component SiC coating, the composite coating could effectively avoid coating spalling and improve the surface integrity at high temperature. After thermal treatment at 1100 °C for 2 h, the interface bond strength of the composite coating/substrate was 52.41% higher than that of SiC coating/substrate. The tensile strength of fiber fabric with SiC–ZrC composite coating could reach 91.75 MPa, which was 101.76% higher than that of raw ASFF. Therefore, the SiC–ZrC coating could greatly improve the temperature resistance of ASFF, and has an attractive application prospect in the field of thermal protection system.     

Bifunctional Ti3C2Tx–CNT/PANI composite with excellent electromagnetic shielding and supercapacitive performance

Ti₃C₂T_x exhibits excellent electromagnetic (EM) shielding and electrochemical properties. However, the inherent re-stacking tendency and easy oxidation of Ti₃C₂T_x limit its further application. In this study, a multi-walled carbon nanotube/polyaniline composite (CNT/PANI, denoted as C–P) was introduced into Ti₃C₂T_x nanosheets to obtain a Ti₃C₂T_x–CNT/PANI composite (T@CP). Owing to the integrated effects of Ti₃C₂T_x and C–P, the contribution of absorption was significantly improved, which finally enhanced the EM shielding performance of T@CP. The highest total EM shielding effectiveness (SE_T) was close to 50 dB (49.8 dB), which was substantially higher than that of pure Ti₃C₂T_x (45.3 dB). Moreover, T@CP demonstrated outstanding supercapacitive performance. The specific capacitance of T@CP (2134.5 mF/cm² at 2 mV/s) was considerably higher than that of pure Ti₃C₂T_x (414.3 mF/cm² at 2 mV/s). These findings provide a new route for the development of high-efficiency Ti₃C₂T_x-based bifunctional EM shielding and electrochemical materials.     

Synthesis and characterization of novel PbS–graphene/TiO2 composite with enhanced photocatalytic activity

In this study novel material PbS–graphene/TiO₂ composites were prepared by sol–gel method. The “as-prepared” composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) with an energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM), UV–vis diffuse reflectance spectra (DRS) and Raman spectroscopic analysis. The photocatalytic activities were investigated by the degradation of methylene blue (MB) as a standard dye. We observed that coupling of PbS with TiO₂ extends the photoresponse to visible region. This revealed that the excellent photoinduced charge separation abilities and transport properties of graphene make these hybrids as potential candidates for developing high-performance next-generation devices.     

Synthesis and characterisation of dental composite materials reinforced with fluoroapatite–mullite glass–ceramic particles

Abstract

Glass–ceramic filler particles containing various amounts of fluoroapatite–mullite crystalline phases were synthesised using SiO₂–Al₂O₃–P₂O₅–CaF₂–CaO system as the base glass formulation. Different additives were used to promote crystallisation in this system. Composite samples were prepared by incorporating the silane treated glass–ceramic particles into the Bis-GMA/TEGDMA (60∶40 mass ratio) epoxy matrix. Structural and microstructural characterisations were conducted using Fourier transform infrared spectroscopy, X-ray diffractometry and scanning electron microscopy (SEM). The mechanical properties of the light cured samples were examined by measuring flexural and diametral tensile strength, as well as conducting Vickers microhardness test. Results obtained in this study showed strong dependence of the flexural strength on the composition of the filler particles. Diametral tensile strength and microhardness values demonstrated lesser sensitivity to the filler composition. Microstructural examination of the samples by SEM revealed particle pull-out, debonding and crack deflection as the major energy consuming mechanisms in the fracture process.     

Synthesis of poly(α-thiophenediyl)benzylidene with high molecular weight and its thermal stability

Summary The synthesis of poly(-thiophenediyl)benzylidene (PTB) with high molecular weight is described. Number-average degrees of polymerization reached about 74. The characterizations of the polymer was investigated by ¹H-NMR, ¹³C-NMR, IR, and UV-VIS spectra. The polymer with well-defined structure and high molecular weight was obtained by polymerization at low temperature and in polar solvent. This polymer was thermally stable and a thermal decomposition took place at 391°C under nitrogen and at 370°C under air. The glass transformation temperature was 117°C and this PTB was nonfusible.