Diamond-like carbon (DLC) films with different thickness (11.26~230.93 nm) were prepared on polyether ether ketone (PEEK) via direct current magnetron sputtering in the time ranging from 2 to 40 min. The effect of deposition time on the structure and composition of surface and interface, as well as the surface hydrophobic, the mechanical and optical transmittance properties of composite films PEEK/DLC were systematically studied. Results show that with the increase of deposition time the film thickness will be enhanced linearly with an average deposition rate of 5.71 nm/min. The density of C atoms and the interface interlocking structure gradually increase, while the interface adhesion decreases with time. By fitting peaks of Raman and XPS spectra, it is found that when the time ≤15 min, the ID/IGvalue by data fitting remains at 0.23~0.25 and the ratio of sp2/sp3 is low (0.58~0.74) due to the influence of substrate. When the time >15 min, as the substrate effect becomes weak the ID/IG value has a great increase (to 0.81), and the sp2/sp3 value turns to be high (0.96~1.12). Prolonging the time will lead to the rise of substrate temperature inducing the ascending of sp2/sp3 ratio. While O content at the surface presents a low-flat trend and part of C=O bonds transformed into C-O bonds. The hardness, elastic modulus, the anti-ultraviolet and infrared barrier properties of PEEK/DLC composite films will rise over time, while the surface roughness and hydrophobicity both have a trend from high to low, reaching a maximum surface roughness and water contact angle of 495 nm and 108.29° at 32 min, respectively.
Electroslag remelting (ESR) has been widely applied as an important technology to produce ingots for special steels and alloys because of its remarkably advantages, such as the process can purify the prepared ingots by effectively eliminating the impurity sulfur and the large inclusions. However, as one of the most important parameters of ESR, the effect of melting rate on the purity of ingot is still controversial. For this purpose, the macro- and micro-structure and nonmetallic inclusion characteristics at different positions of GH4169G ingots produced by industrial-scale argon protected electroslag remelting (PESR) technology with 2 remelting rates were comparatively investigated by means of OM, SEM, EDS and EPMA. The results indicate that a proper high melting rate is beneficial to shorten the local solidification time of ingot, reduce the secondary dendrite arm spacing and refine dendrite structure, but has little effect on the distribution of Nb, Ti and other elements along the radial direction in macro-scale. Besides, the melting rate has little effect on the inclusion types of GH4169G ingot, which are mainly oxides, fluorides and nitrides. The inclusions in the ingot are usually double or three layers with oxide as the core, nitride as the secondary outer layer and carbide as the outermost layer. The influence of the melting rate on the movement of inclusions in the remelting process was simulated via the so called MeltFlow-ESR software. It was found that the increase of melting rate was conducive to the movement of inclusions to the ingot surface, thereby the thickness of the inclusion enriched area on the surface of the ingot and the number of inclusions in the ingot could be reduced. In addition, the increase of melting rate can shorten the time of inclusion precipitation and reduce the size of inclusions.
TiH1.924 nanometer powder was prepared by DC arc method, and then taking TiH1.924 as precursor,TiS3 nanometer flakes with laminar structure was prepared by solid-gas reaction. The structure and performance of TiS3 nanoflakes as anode material for lithium-ion batteries were characterized by X-ray diffractometer (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), Raman spectroscopy and performance testing. The performance of TiS3 nanoflakes as anode for lithium-ion battery was also investigated. The results show that the TiS3 nanoflake has a special nano-laminar structure, and its thickness is about 35 nm. The lithium-ion battery using TiS3 nanoflakes as anode material has good electrochemical performance with the remained capacity of 430 mAh/g after 300 cycles at a current density of 500 mA/g. When the current density is 5 A/g the discharge capacity is 240 mAh/g and when the current density is restored to 100 mA/g, the discharge capacity is stable at 500 mAh/g. The good magnification properties of TiS3 are due to its special nano-flake structure. The mono-laminar structure can better adapt to the volume change caused by the strain in the process of multiple discharge/charging at high current density, so as to prevent the electrode from crushing.
Nano-copper-carbon composites (NCCC) was prepared by one-step pyrolysis in nitrogen atmosphere using natural cotton fiber with adsorbate copper sulfate as template. The carbon coated nano-Cu or micro-Cu was in situ prepared by taking cotton fiber with adsorbate copper sulfate as pyrolytic carbon source and commercial nano-copper or micro-copper as Cu source. The stability of the prepared material was characterized by TEM, XRD and Raman spectroscopy. The results show that NCCC is a typical material with carbon coated nano-Cu core-shell structure, and the carbon coated nano- or micron-Cu materials can be prepared by in-situ pyrolysis, which further confirmed that the pyrolysis atmosphere of cotton fiber could act as carbon source and in-situ reducing agent at the same time. And the oxidation resistance of carbon coated material was verified:the formation of carbon shells allows NCCC to maintain the phase composition of copper and cuprous oxide after exposure to air for 180 days or water for 35 days, and the commercial Cu nanoparticles covered with carbon shells have not been oxidized after 120 days of exposure to air.
Polymethyl methacrylate (PMMA) with different carbon black (CB) contents were prepared by melt blending. Based on the solid-state reaction kinetics, the thermal degradation behavior of PMMA with different CB contents was explored. Through non-isothermal thermogravimetric analysis (TGA) experiments under the conditions of different heating rates, the thermal degradation kinetic models of PMMA with different CB contents were built by four methods, including Friedman, FWO, KAS and Freeman-Carroll. The accuracy of models was verified by comparing with TGA experiments. The results show that PMMA with CB has higher thermal decomposition temperature and activation energy compared with pure PMMA. The PMMA with 0.1% CB presents the highest thermal stability. The activation energy of PMMA first rises and then falls down with increasing CB content, and the maximum increment is 17.76 kJ·mol-1, which proves that adding CB improves the thermal stability of PMMA to a certain extent.
Low cycle fatigue experiments for 316L stainless steel were carried out under circular loading and different strain ranges at 600℃. The microstructures near the fatigue fracture were observed by transmission electron microscope (TEM). The path correlation and amplitude correlation of dislocation structure and the path correlation of dynamic strain aging (DSA) were investigated based on the experimental results. The results show that at room temperature and 600℃, the planar slip is significant under uniaxial loading and the choroid dislocation structure formed. However, the equiaxed cellular dislocation structures are exhibited under circular loading, which reduces the deformation resistance of the material significantly. For equivalent strain range 1.0%, the fatigue life under circular loading is 81% lower than that of the uniaxial loading at 600℃. At the same time, the minimum equivalent strain range required to form a cellular dislocation structure under the circular loading is lower than that of the uniaxial loading. At 600℃, the DSA effect is more complete under circular loading, and the maximum stress drop for equivalent strain range 1.0% increases by 680% compared with that under uniaxial loading. The DSA phenomenon is more evident in the compression stage, and the sawtooth type gradually transitions from type A, type B to type C.
Nanoscale tungsten whiskers grown on the surface of polycrystalline W-plate was subjected intermittently to irradiation of He ions with energy of 150 eV at 400 K. The effect of He ion irradiation on the evolution of nanoscale W-whiskers were investigated by means of scanning electron microscope, transmission electron microscope and mass loss method. The results show that nanoscale W-whiskers were extremely unstable in the course of high-energy He ion irradiation, and the degree of crosslinking between W-whiskers decreases gradually with the increase of irradiation fluence. Due to high-energy He ion sputtering, He bubbles existed in the whiskers will break and lead to collapse and coalesce of the W-whiskers. Meanwhile, certain amount of the yielded W atoms by He ion sputtering may re-deposited on the outer wall or the root of the nanoscale whiskers nearby, and finally, the relevant nanoscale whiskers may evolve into a cone-shaped structure with a thin top and a thick root.
The microstructure and macroscopic mechanical property of polyurethane/sodium silicate grouting materials during curing process were studied by means of scanning electron microscopy, energy dispersive spectroscopy, transmission/diffuse reflectance infrared spectroscopy and mechanical testing. The results show that: within the first 7 days, the compressive strength, fracture toughness and bending strength of the polyurethane/sodium silicate grouting material increased rapidly up to 55.4 MPa, 1025.3 MPa·m1/2 and 29.4 MPa, afterwards, they slowly increased to 58 MPa, 1220.4 MPa·m1/2 and 37.4 MPa respectively; the macroscopic mechanical properties of grouting materials mainly depend on the degree of crosslinking-curing of organic phases; the curing process of the grouting material involves the continuous exchange of water, carbon dioxide and heat between the organic phase and sodium silicate, and finally forms the polyurethane/sodium silicate composite composed of polyurea/polyurethane, which was resulted from the reaction of polyisocyanate with water and polyether polyol and silicate particles cured by sodium silicate gel.
Iron-doped titanium dioxide (Fe-TiO2) nanomaterials were prepared with the stable fibrous nanostructure of self-assembled bola-type amphiphilic short peptide KI3E as organic templateand aminopropyl triethoxysilane as structure-directing agent via sol-gel process to ensure the simultaneous deposition of the titanium dioxide precursor and iron ions on the surface of the peptide templates. The Fe doped-TiO2 nanomaterials were fully characterized by Transmission electron microscope, UV-vis diffuse reflection spectroscopy, X-ray photoelectron spectroscopy, X-ray diffractometer. The results show that iron ions instead of partial titanium ions in the crystal lattice of titanium dioxide, which narrows the band gap of TiO2 and results in enhanced visible light responses. The test results of photocatalytic degradation of rhodamine B and methylene blue indicated that the Fe doped-TiO2 possessed significantly enhanced photocatalytic performance, compared to the commercial TiO2 (P25), while reached a maximum when the doping content of iron ions was 0.5%.
The high-entropy alloys (FeNiCoCr)100-x Al x (x=0, 5) were prepared via a two-step process i.e., low-energy ball milling and then vacuum hot-pressing sintering, while the alloys were post-aged, afterwards, their microstructure and mechanical properties were assessed. The results show that the microstructure of both the as-sintered and the aged alloys composed of fcc-phase and a small amount of bcc phase, but twins presented in the fcc phase, and the proportion of twins for the alloy without Al was relatively high. The alloy with Al had relatively high bcc phase, and many small-angle grain boundaries appeared after aging treatment. The aged FeNiCoCr alloy has the best comprehensive performance, with a compressive true yield strength of 545 MPa. Moreover, the bending strength and the fracture toughness of the aged FeNiCoCr alloy reached 1342 MPa and 32.5 MPa·m1/2. The excellent mechanical properties were attributed to the generation of annealing twins in the fcc-phase and the precipitation of the bcc-phase.