Quantitative evaluation of the oxidation behavior of ZrB2-15 vol.%SiC at a low oxygen partial pressure

Oxidation tests of ZrB₂–SiC composite were carried out at 1373–1923 K under a low oxygen partial pressure of 57 Pa. By making composite with SiC, ZrB₂ shows good oxidation resistance. The ZrB₂-15 vol.%SiC composite shows better oxidation resistance at higher temperatures than ZrB₂-30 vol.%SiC with respect to mass decrease. The SiC depleting is the main cause of this mass decrease and is quite significant under the low oxygen partial pressure. The SiC depleting seems to start to occur at around 1673 K or higher. The mass changes of ZrB₂-15 vol.%SiC are quantitatively discussed by introducing an empirical equation. A first attempt of the evaluation of passive/active transition has been conducted using the obtained values.     

Preparation and thermal performance analysis of novel multilayer cladding structure composites

With regard to the adiabatic principle of insulation, a novel multilayer cladding structure composites (MCSC) with vacuum inside was put forward, which could be used in high temperature insulation field. In the composites, SiO₂ was used to fill the microcracks and protect the carbon matrix from oxidizing. This novel material was composed of two parts, one was the core material consisted of SiC foam ceramic, the other was the flawless outer shell consisted of carbon fiber reinforced composites with vacuum inside that produced by Chemical Vapor Infiltration (CVI) Pyrolytic Carbon (PyC) and silicasol-infiltration–sintering methods. Material density was 0.81 g/cm³. The effective thermal conductivity of MCSC ranged from 0.193 W/m · K to 0.721 W/m · K within the temperature from 303 K to 703 K, which was 13.5–23.3% lower than the value of SiC ceramic foam core materials. However, at 1473 K, the measured data of MCSC and SiC foam were 1.815 W/m · K and 1.911 W/m · K, respectively. It was only 5.02% lower than that of SiC foam.     

Enhanced apatite formation on Ti metal heated in PO2-controlled nitrogen atmosphere

The oxynitridation of biomedical titanium metal under a precisely regulated oxygen partial pressure (P_O2) of 10^? 14 Pa in nitrogen atmosphere at 973 K for 1 h strongly enhanced apatite formation compared with that on Ti heated in air. The factors governing the high apatite-forming ability are discussed from the viewpoint of the surface properties of Ti heated under a P_O2 of 10^? 14 Pa in nitrogen atmosphere determined from X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and zeta potential measurements. Nitrogen (N)-doped TiO₂ (interstitial N) was formed on pure Ti heated under a P_O2 of 10^? 14 Pa in nitrogen atmosphere at 973 K. The XPS O1s main peak shifted toward a lower binding energy upon heating under a P_O2 of 10^? 14 Pa. This shift may be due to the formation of oxygen vacancies. This Ti surface had a positive zeta potential of approximately 20 mV. According to time-of-flight secondary ion mass spectroscopy results, PO₄^3 ? ions were predominantly adsorbed on Ti soaked in simulated body fluid (SBF) after heat treatment, followed by calcium ions. It was concluded that the apatite formation kinetics can be described using the Avrami–Erofeev equation with an Avrami index of n = 2, which implies the instantaneous nucleation of apatite on the surface of Ti soaked in SBF after heat treatment at 973 K under a P_O2 of 10^? 14 Pa.     

Behavior analysis of silica in aluminum production by alumina carbothermic reduction-chlorination process in vacuum

In present work, the behavior of silica was investigated experimentally in the alumina carbothermic reduction process and chlorination process in the temperature range of 1173 K-1763 K. The phase of slags, surface morphology and composition of condensate were examined by means of XRD, SEM and EDS. The results showed that SiC was produced by SiO₂ and C in the temperature range of 1573 K-1673 K, while alumina transformed into corundum completely, then Al₄SiC₄ was produced by SiC and intermediates (Al₄C₃ and Al₄O₄C) obtained during carbothermic reduction of alumina at about 1763 K. In the chlorination process, the silicon-containing materials in the condensate were not found. Because SiO₂ consumed Al₃C₄ and Al₄O₄C, then the recovery rate of aluminum decreased. It was inferred that silica may be unfavourable for aluminum extracted from alumina by carbothermic reduction-chlorination process in vacuum.     

Multi-layer CVD-SiC/MoSi2–CrSi2–Si/B-modified SiC oxidation protective coating for carbon/carbon composites

To further improve the oxidation resistance of coating for carbon/carbon (C/C) composites, a multi-layer CVD-SiC/MoSi₂–CrSi₂–Si/B-modified SiC coating was prepared on the surface of C/C composites by pack cementation and chemical vapour deposition method, respectively. The microstructures, oxidation and thermal shock resistance of the coating were studied. The influence of B content in pack powder on the microstructure and oxidation resistance of B-modified SiC coating was also investigated. The results show that the B-modified SiC coating prepared with 10 wt.% B exhibited the best oxidation protection ability for C/C composites at 1173 K. The multi-layer coatings could protect the C/C composites at 1173 K for 30 h and 1873 K for 200 h, and endure 30 thermal cycles between 1873 K and room temperatures. The oxidation resistance and thermal shock resistance is mainly attributed to their dense structure and self-sealing property.     

Oxidation resistance of hafnium diboride—silicon carbide from 1400 to 2000?°C

Oxidation resistance tests were carried out on HfB₂-20 vol.% SiC prepared by spark plasma sintering. The dense samples were exposed from 1400 to 2000 °C in an ambient atmosphere for 1 h. For comparison, the same material was tested using an arc jet to simulate an atmospheric reentry environment. The oxidation properties of the samples were determined by measuring the weight gain per unit surface area and the thicknesses of the oxide scale. The oxide scale consists of a SiO₂ outer layer, porous HfO₂ layers, and an HfB₂ layer depleted in SiC. A transition in HfO₂ morphology from equixed to columnar and a decrease in SiO₂ viscosity between 1800 and 1900 °C accompanied a rapid increase in weight gain and scale thickness.     

Effect of environment atmosphere on thermal shock resistance of the ZrB2–SiC–graphite composite

The thermal shock resistance of the ZrB₂–SiC–graphite composite was evaluated by measuring the retention of the flexural strength after the electrical resistance heating to the temperature ranging from 1000 °C up to 2500 °C. The experiment was operated in two different environment atmospheres (pure oxygen and low oxygen partial pressure which mixed O₂ and Ar with 1:9) at total pressure 2000 Pa. The residual strength for the specimen decreased gradually as the temperature increased up to 2200 °C, and it was slightly higher when heated in low oxygen partial pressure environment than in pure oxygen. In contrast to the specimen heated in low oxygen partial pressure environment, the residual strength for the specimen in pure oxygen increased steeply as the temperature increased from 1600 °C up to 1800 °C. The analysis of the SEM observations combined with EDS confirmed that the surface oxidation played a positive role in the thermal shock resistance of the ZrB₂–SiC–graphite composite with different environment atmospheres. The results here pointed out a potential method for charactering the effect of environment atmosphere on thermal shock resistance of the ZrB₂–SiC–graphite composite.     

Study on dual binders for fabricating SiC particulate preforms using selective laser sintering

The SiC preforms were successfully produced by selective laser sintering and thermal treatment for fabricating the near-net-shape composites with high SiC volume fraction. The effects of dual binders on the forming accuracy, microstructure and mechanical properties of SiC preforms were investigated. Results show that the SiC preforms with forming accuracy of 98.89% were fabricated by using the dual binders of nylon 6 + NH₄H₂PO₄, which fits the requirement of subsequent near-net-shape manufacturing compared with using single binder of nylon 6 after thermal treatment, the tensile and bend strength were significantly improved by using the dual binders of nylon 6 + NH₄H₂PO₄, which are strong enough to support the external load during infiltration. The bonding among SiC particulates primarily depends on nylon 6 after laser sintering, but after the decomposing of nylon 6, the reaction product of SiP₂O₇ phases can provide effective bonding for maintaining the forming accuracy and supporting mechanical properties of SiC preforms.     

Manufacture of fibrous β-Si3N4-reinforced biomorphic SiC matrix composites for bioceramic scaffold applications

The manufacturing of the Si₃N₄ reinforced biomorphic microcellular SiC composites for potential medical implants for bone substitutions with good biocompatibility and physicochemical properties was performed in a two step process. First, wood-derived porous Si/SiC ceramics with various porosities were produced by liquid silicon infiltration (LSI) at 1550 °C with static nitrogen atmosphere protection (0.1 MPa), followed by subsequent partial removing of the Si in vacuo at 1700 °C for different periods of time. Secondly, the final porous Si₃N₄ fiber/SiC composite was obtained by further chemical reaction of nitrogen with the infiltrated residual silicon at 1400 °C for 4 h under high concentration flowing nitrogen atmospheres (0.5 MPa). The bending strengths of the porous Si₃N₄ fiber/SiC composite at axial and radial direction were measured as 180.03 MPa and 90 MPa respectively. The improvement in bending strength was primarily attributed to grain pull-out and bridging enhanced by the elongated β-Si₃N₄ grains cross-linked in the depth of the pore channels. The TG analysis showed an obvious improvement in oxidation resistance of the nitride specimens.     

Adsorption of NO on potassium-modified Cu (100) vicinal surfaces

The interaction of nitric oxide, NO, with clean and potassium-modified copper surfaces: Cu (001), Cu (119) and Cu (115), in the temperature range of 125–800 K, was investigated using photoelectron spectroscopy based on synchrotron radiation (SR-PS). At 125 K nitric oxide, on the non-modified surface, dissociates and molecules of N₂O obtained by a reaction dominates on the substrate. The sticking coefficient increases with the presence of steps on the surface. Successive annealing of the surface leads to desorption and dissociation of the adsorbed species, at 500 K to chemisorption of remaining oxygen and nitrogen indicating formation of copper oxide and copper nitride. Pre-adsorbed potassium observably increases the sticking coefficient and the alkali metal reacts with the incoming nitric oxide molecules. Apart from the mentioned species, the presence of a nitrate salt (K-NO_x) is deduced from the spectra. Heat treatment of the potassium modified copper causes surface reactions with the appearance of potassium compounds as well. Among the three Cu surfaces, changes concerning the sticking coefficient and different possibility of nitrogen capture after adsorbate dissociation were found. Surface reactions follow the same pattern on the three surfaces.     

Synthesis of SiC ceramic fibers from nuclear reactor irradiated polycarbosilane ceramic precursor fibers

Polycarbosilane (PCS) ceramic precursor fibers are irradiated in a nuclear reactor and pyrolyzed under inert atmosphere. Bridge structure of Si–CH₂–Si is formed in the irradiated products by the rupture of Si–H bonds and succeeding cross-linking. When irradiated at the neutron fluence of 2.2 × 10¹⁷ cm⁻² under N₂ atmosphere, the gel content and ceramic yield at 1,273 K of PCS fibers are up to 80% and 94.3%, respectively, and their pyrolysis products are still fibrous, which illuminates that the infusibility of PCS fibers has been achieved. FT-IR spectra indicate that the chemical structure of pyrolysis products is very similar to that of pure SiC, while X-ray diffraction curves suggest that β-SiC microcrystals are formed in the fibers, and their mean grain size is about 7.5 nm. The oxygen content (1.69–3.77 wt%) is much lower than that of conventional SiC fibers by oxidation curing method (about 15 wt%). Tensile strength of the SiC fibers is up to 2.72 GPa, which demonstrates that their mechanical properties are excellent. After heat-treated at 1,673 K in air for an hour or at 1,873 K under Ar gas atmosphere for 0.5 h, their external appearance is still undamaged and dense, and their tensile strength decreases to a small extent, which verifies that heat resistance of the SiC fibers is eximious.     

Insights into the mechanism of co-adsorption between tetracycline and nano-TiO2 on coconut shell porous biochar in binary system

The coexistence of nanoparticles (NPs) and environmental pollutants has become a new type of pollution, and the co-adsorption behaviors of coexisting NPs and pollutants on the coconut shell porous biochar is important to explore the environmental fate of both pollutants and NPs in complex environments. In this study, the interaction between nano-titanium dioxide (n-TiO₂) and tetracycline (TC) during the adsorption process on the coconut shell biochar (CBC) was explored by adsorption experiment, the co-adsorption mechanisms of TC and n-TiO₂ onto CBC were discussed by morphology and characteristics of Scanning electron microscopy, Brunauer-Emmett-Teller specific surface area, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy analyses. The results showed that the n-TiO₂ in the TC + TiO₂ binary system leads to the TC adsorption decrease by 54.60% averagely. The TC in the TC + TiO₂ binary system increased the n-TiO₂ adsorption by 31.97% averagely but weakened the adsorption affinity of n-TiO₂. Characterization analysis confirmed that, the hydrogen bonding, π-π/n-π interaction and pore filling between TC and CBC were suppressed in the TC + TiO₂ binary system. The TC in the binary system enhances the n-TiO₂ adsorption on the outer surface and the inner surface of CBC by surface bridging and reducing the agglomeration of n-TiO₂.     

Ultra-thin zinc oxide film on Mo(100)

Zinc oxide films on a single crystal Mo(100) substrate were fabricated by annealing the pre-deposited metal Zn films in 10^− 5-10^− 4 Pa O₂ ambience at 300-525 K, and were characterized by in situ Auger electron spectroscopy, electron energy loss spectroscopy, low energy electron diffraction and high-resolution electron energy loss spectroscopy. The results show that the atomic ratio of oxygen to zinc in zinc oxide film is significantly dependent on sample annealing temperature and O₂ pressure. A stoichiometric zinc oxide film has been obtained under ∼10^− 4 Pa O₂ at about 400 K. A redshift of Fuchs-Kliewer phonon energy correlated with surface oxygen deficiency is observed.     

Preparation of La0.8Sr0.2Cr0.97V0.03O3 − δ films for solid oxide fuel cell application

La_0.8Sr_0.2Cr_0.97V_0.03O_3 − δ (LSC) is commonly studied as a ceramic interconnect material as well as a coating material for metallic interconnects for solid oxide fuel cell applications. However, it is difficult to sinter this type of material to high density. In order to overcome this problem and to study the material in form of a thin film we have used Pulsed Laser Deposition to obtain a dense, uniform film with the right stochiometry. Investigation of preparation-parameter dependence of the LSC films deposited on a stainless steel substrate during pulsed-laser deposition was carried out. The LSC films were deposited with KrF excimer laser (248 nm) on a stainless steel substrate at different oxygen pressure and substrate temperatures. The substrate temperature (873-1073 K) and the oxygen background pressure (5-20 Pa) were varied in order to obtain optimal growth conditions. The surface morphology and structural information of the films were obtained using scanning electron microscope (SEM) and X-ray diffraction, respectively. Under the optimal preparation-parameter conditions: substrate temperature of 1023 K and an oxygen pressure of 10 Pa the structure of the film agreed with the target structure and the SEM micrographs show that the surfaces are homogeneous, smooth, crack-free and dense.     

Effect of surface condition on the kinetics of scandium-deuteride formation

We studied the effects of surface oxidation on the kinetics of deuterium (D₂) absorption by Sc. A Sieverts apparatus was used to measure the D₂ absorption kinetics and X-ray photoelectron spectroscopy (XPS) was used to determine the surface oxidation state during heat treatments in ultra-high vacuum. In the as-received condition, the bulk Sc sample was covered by an Sc₂O₃ film. However, the Sc₂O₃ phase decomposed dramatically at 573 K due to the fast diffusion of oxygen from the surface to the bulk. The initial surface of Sc was cleaned of most oxygen by heating up to 873 K whereas the obtained fresh surface at temperatures over 873 K was contaminated by oxygen again when cooled down to room temperature. Due to fresh surfaces available for D₂ absorption, the sample at temperatures over 873 K started to absorb D₂ as soon as it was introduced. The absorption rate at these temperatures appears to be governed by D diffusion in the Sc bulk. However, the sample deuterated at room temperature presented an incubation time before the absorption was observed. And this stage was followed by a surface controlled process that changed gradually to a stage related to deuterium diffusion into the bulk.     

Study of the growth,and effects of filament to substrate distance on the structural and optical properties of Si/SiC core–shell nanowires synthesized by hot-wire chemical vapor deposition

Silicon/silicon carbide (Si/SiC) core–shell nanowires grown on quartz substrates by hot-wire chemical vapor deposition were studied. Nickel was used as a catalyst to induce the growth of these core–shell nanowires followed by the vapor–solid–solid growth mechanism. The nanowires were grown by varying substrate-to-filament distance; d_s-f from 1.9 to 3.1 cm with an interval of 0.4 cm. Lower d_s-f produced a high density of straight core–shell nanowires. A highly crystalline single crystal Si core of the nanowires was produced at lower d_s-f as well. Presence of Si and SiC nano-crystallites embedded within an amorphous matrix in the shell of the nanowires exhibited a high intensity of photoluminescence emission spectra from 600 to 1000 nm. The effects of the d_s-f on the structural and optical properties of the nanowires are discussed.     

SiC Particles Coated by Chromium Silicides

The interaction of chromium vapors with powderlike silicon carbide (SiC) was investigated by X-ray phase analysis, X-ray microanalysis, the EPR method, electron microscopy, and the BET method. It has been established that in the temperature range of 147 K to 2023 K under a pressure of 1.3 Pa, the main interaction product is chromium silicide (Cr₅Si₃), which forms a surface layer on SiC particles in zones with a mean temperature (T _mean) of 1773 K to 1473 K. Moreover, Cr₅Si₃ vapors passing through the disperse SiC system condense in cold-temperature zones on SiC particles and aggregates.     

Effects of water vapor on corrosion behaviors of C/SiC in oxidizing atmosphere containing Na2SO4 vapor

Corrosion of a C/SiC composite has been investigated in the atmosphere containing oxygen, water vapor and sodium sulfate vapor at the temperatures range from 1000 to 1500 °C. The effect of water vapor on the corrosion mechanism of C/SiC were discussed based on the weight change, the residual strength change, the microstructure and calculated results from FactSage. The corrosion of C/SiC is attributed to (i) the permeation of gas through the SiO₂ film below 1300 °C, (ii) the diffusion of oxidant through pores caused by bubbles broken in the SiO₂ film above 1300 °C. The water vapor does not change the corrosion mechanism of C/SiC composite but the temperature range in which the corrosion mechanism works by accelerating the oxidation of SiC and the corrosion of SiO₂.     

Surface nano-structured silicon carbide thin film produced using hot filament decomposition of ethylene at low temperature on silicon wafer

The structure and spectroscopic properties of nano-structured silicon carbide (SiC) thin films were studied for films obtained through deposition of decomposed ethylene (C₂H₄) on silicon wafers via hot filament chemical vapor deposition method at low temperature followed by annealing at various temperatures in the range 300-700 °C. The prepared films were analyzed with focus on the early deposition stage and the initial growth layers. The analysis of the film's physics and structural characteristics was performed with Fourier transform infrared spectroscopy and Raman spectroscopy, scanning electron microscopy with energy dispersive X-ray spectroscopy, and X-ray diffraction. The conditions for forming thin layer of cubic SiC phase (3C-SiC) are found. X-ray diffraction and Raman spectroscopy confirmed the presence of 3C-SiC phase in the sample. The formation conditions and structure of intermediate SiC layer, which reduces the crystal lattice mismatch between Si and diamond, are essential for the alignment of diamond growth. This finding provides an easy way of forming SiC intermediate layer using the Si from the substrate.     

Effects of water vapor on corrosion behaviors of C/SiC in oxidizing atmosphere containing Na2SO4 vapor

Corrosion of a C/SiC composite has been investigated in the atmosphere containing oxygen, water vapor and sodium sulfate vapor at the temperatures range from 1000 to 1500 °C. The effect of water vapor on the corrosion mechanism of C/SiC were discussed based on the weight change, the residual strength change, the microstructure and calculated results from FactSage. The corrosion of C/SiC is attributed to (i) the permeation of gas through the SiO₂ film below 1300 °C, (ii) the diffusion of oxidant through pores caused by bubbles broken in the SiO₂ film above 1300 °C. The water vapor does not change the corrosion mechanism of C/SiC composite but the temperature range in which the corrosion mechanism works by accelerating the oxidation of SiC and the corrosion of SiO₂.