Carbon nanotubes coated with diamond nanocrystals and silicon carbide by hot-filament chemical vapor deposition below 200 °C substrate temperature

Multi-walled carbon nanotubes (MWCNTs) dispersed onto a silicon substrate have been coated with diamond nanocrystals (DNC) and silicon carbide (SiC) from solid carbon and silicon sources exposed to H₂ activated by hot filament chemical vapor deposition (HFCVD) at around 190 °C substrate temperature. MWCNT coating by DNC initiates during filament carburization process at 80 °C substrate temperature under conventional HFCVD conditions. The hybrid nanocarbon material was analyzed by scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, electron energy loss spectroscopy, selected area electron diffraction, X-ray diffraction and Raman spectroscopy. The structure of the MWCNTs is preserved during coating and the smooth DNC/SiC coating is highly conformal. The average grain size is below 10 nm. The growth mechanism of DNC and SiC onto MWCNT surface is discussed.     

Preparation of alumina/carbon nanotubes composites by chemical precipitation

Continuous alumina coating on multi-walled carbon nanotubes (MWCNTs) was successfully prepared by a new method of chemical precipitation using aluminum nitrate and ammonia as starting materials. Structure and morphology of the alumina/multi-walled carbon nanotubes (Al₂O₃/MWCNTs) composites were characterized by transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), infrared spectra (IR), thermo gravimetric analysis (TG), differential thermal analysis (DTA) and N₂ adsorption–desorption. The results show that polyvinyl alcohol (PVA) modification on the surface of MWCNTs contributes to form continuous alumina coating, γ-Al₂O₃ layers with thickness of 1–3 nm cover the surface of MWCNTs and the original structure of MWCNTs is retained during the coating process.     

Synthesis of Fe–SiC Nanowires via Precursor Route

Magnetic SiC nanowires were obtained by the pyrolysis of iron containing polycarbosilane (PCS) which in turn was synthesized by the reaction of polycarbosilane and iron (III) acetylacetonate [Fe(acac)₃] in solvent. Characterization of synthesized polycarbosilane and Fe–SiC were performed with Fourier transformation infrared spectroscopy, energy dispersive X-ray spectrometry, powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, electron spin resonance and vibrating sample magnetometer.     

Dispersion of SiC coated MWCNTs in PEI/silicone rubber blend and its effect on the thermal and mechanical properties

Multi‐walled carbon nanotubes (MWCNTs) are modified by polycarbosilane derived SiC to improve the dispersion of MWCNTs in the polymer matrix. Unmodified and modified MWCNTs are dispersed in PEI/hydroxyl terminated PDMS(HTSR) blend by melt mixing. TEM and FESEM images shows better dispersion of SiC coated MWCNTs in the blend matrix when compared with pure MWCNTs. Thermal stability of the SiC coated MWCNTs added nanocomposite improved drastically than that of the pure MWCNTs. Compared with pure PEI/HTSR binary blend and unmodified MWCNTs/PEI/HTSR ternary blend, the storage modulus, tensile modulus, and tensile strength of SiC coated MWCNTs/PEI/HTSR blend increased, due to the better dispersion of the modified MWCNTs in polymer matrix. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Morphology and Microstructure of Three-Dimensional Orthogonal C/SiC Composites Ablated by an Oxyacetylene Flame at 2900°C

C/SiC composites were prepared by polycarbosilane infiltration pyrolysis and ablated by oxy-acetylene flame at 2900°C for 180 s. The morphology and microstructure of C/SiC were observed by scanning electron microscopy. The phase transition and the composition were confirmed by energy-dispersive spectroscopy and X-ray diffraction. The ablation rates of the center region and the outer region were 2.5 and 1.1 μm/s, respectively. The ablated C/SiC was covered by a turbostratic carbon coating resulting from the pyrolysis of acetylene. White dross attached on the surface was composed of SiO₂ resulting from the sublimation and decomposition of SiC during ablation and oxidization of Si and SiC during cooling. The results indicated that the ablation was due to a combination of carbon coating deposition, decomposition of SiC, oxidation, and mechanical erosion.     

Microstructural and compositional characterisation of the pyrocarbon interlayer in SiC coated low density carbon/carbon composites

SiC coated carbon bonded carbon fibre (CBCF) composites, a special class of carbon/carbon composites for thermal insulation, were investigated. Successful deposition of SiC requires the CBCF material to be first given a pyrocarbon coating. SiC coating on pyrocarbon coated CBCF was assessed using several analytical techniques. X-ray diffraction identified the coating as β SiC. The fibre orientation in two perpendicular planes was determined using X-ray microtomography, and it was found to be random in one plane whereas there was a preferred orientation in the other plane. A comparison was made between the uncoated and pyrocarbon coated substrates in terms of surface roughness, purity and crystallinity, using white light interferometry, neutron activation analysis/secondary ion mass spectrometry and transmission electron microscopy, respectively. The higher roughness, greater purity and increased levels of crystallinity of pyrocarbon coated CBCF are considered to be responsible for the successful deposition of a SiC coating on this material.     

A hot-pressing reaction technique for SiC coating of carbon/carbon composites

A hot-pressing reactive sintering (HPRS) technique was explored to prepare SiC coating for protecting carbon/carbon (C/C) composites against oxidation. The microstructures of the coatings were analyzed by X-ray diffraction and scanning electron microscopy. The results show that, SiC coating obtained by HPRS has a dense and crack-free structure, and the coated C/C lost mass by only 1.84 wt.% after thermal cycles between 1773 K and room temperature for 15 times. The flexural strength of the HPRS-SiC coated C/C is up to 140 MPa, higher than those of the bare C/C and the C/C with a SiC coating by pressure-less reactive sintering. The fracture mode of the C/C composites changes from a pseudo-plastic behavior to a brittle one after being coated with a HPRS-SiC coating.     

A Si–SiC oxidation protective coating for carbon/carbon composites prepared by a two-step pack cementation

To prevent carbon/carbon (C/C) composites from oxidation, a Si–SiC coating has been prepared by a two-step pack cementation technique. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis show that the coating obtained by the first step pack cementation is a porous β-SiC structure, and a dense structure consisting α-SiC, β-SiC and Si is obtained after heat-treatment by the second step pack cementation. By energy dispersive spectroscopy (EDS) analysis, a gradient C–SiC transition layer can be formed at the C/C-coating interface. The as-received coating has excellent oxidation protection ability and can protect C/C composites from oxidation for 166 h at 1773 K in air. The weigh loss of the coated C/C is due to the formation of bubble holes on the coating surface and through-coating cracks in the coating.     

SiC coating toughened by SiC nanowires to protect C/C composites against oxidation

A dense SiC coating toughened by SiC nanowires was prepared on carbon/carbon (C/C) composites using a two-step technique of chemical vapor deposition (CVD) to protect them against oxidation. The morphologies and crystalline structures of the coatings were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. SiC nanowires played a role in decreasing the size of the cracks and improving the thermal shock resistance of the coating. The result of thermal shock between 1773 K and room temperature for 21 times indicates that, compared with the SiC coating without SiC nanowires, the average size of the cracks in the SiC coating toughened with SiC nanowires reduced from 5 ± 0.5 to 3 ± 0.5 μm. The weight loss of the SiC coated C/C composites decreased from 9.32 to 4.45% by the introduction of SiC nanowires.     

Synthesis of Silica Decorated MWCNTs for Field Emission Property

A novel route to nanocomposites containing surface modified multiwalled carbon nanotubes (MWCNTs) by silica thin film is reported. The effect of chemical oxidation on the surface of MWCNTs by using different acid-treatments is studied.The acidic processes are characterized by Raman spectroscopy, thermogravimetry analysis, scanning electron microscopy, and transmission electron microscopy. MWCNTs can be coated homogeneously with silica film by using tetraethoxysilane (TEOS)as a precursor in a sol-gel process. Varying the shell thickness of amorphous silica coating layers on MWCNTs exhibits excellent thermal stability, reliability, and lifetime of field emission properties, especially down to less than 10 nm.     

Corrosion behaviour and biocompatibility of nanoporous niobium incorporated titanium oxide coating for orthopaedic applications

This study investigates the surface characteristics, in vitro biocompatibility and electrochemical behaviour of nanoporous niobium incorporated titanium dioxide (Nb-incorporated TiO₂) coated 316L stainless steel (SS) for orthopaedic applications. The coating material was synthesized by sol-gel methodology and was deposited on 316L SS by using spin coating technique and heat treatment. The experimental conditions were optimized to obtain a coating with nanoporous morphology. The coating was characterized using attenuated total reflectance-Infrared spectroscopy (ATR-IR), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX), atomic force microscopy (AFM) and transmission electron microscopy (TEM). The analysis confirmed the formation of a crystalline nanoporous Nb-incorporated TiO₂ coating with hydrophilic nature. Mechanical studies validated that the coating has excellent adhesion to the specimen and appreciable hardness value. In vitro bioactivity test confirmed that the nanoporous morphology of the coating facilitated enhanced hydroxyapatite (HAp) growth. Electrochemical studies established that the insulative nature of the coating provides excellent corrosion resistance to 316L SS.     

Acceleration and quantitative evaluation of degradation for corrosion protective coatings on buried pipeline: Part II. Application to the evaluation of polyethylene and coal-tar enamel coatings

The pulsed potentiostatic polarization technique proposed previously has been applied to evaluate the electrochemical degradation of polyethylene and coal-tar enamel coated SS400 for buried pipeline. The degradation of coated systems was accelerated and evaluated using electrochemical techniques (pulsed potentiostatic polarization test, electrochemical impedance spectroscopy) and surface analyses (scanning electron microscopy and energy dispersive X-ray spectroscopy). It was found that polyethylene coating had better protective performance than coal-tar enamel coating due to its low porosity. It was confirmed that the electrochemically accelerated test is an effective technique in the evaluation of coating performance.     

Thermal shock resistance of tri‐layer Yb2SiO5/Yb2Si2O7/Si coating for SiC and SiC‐matrix composites

A new tri‐layer Yb₂SiO₅/Yb₂Si₂O₇/Si coating was fabricated on SiC, C/SiC, and SiC/SiC substrates, respectively, using atmospheric plasma spray (APS) technique. All coated samples were subjected to thermal shock test at 1350°C. The evolution of phase composition and microstructure and thermo‐mechanical properties of those samples before and after thermal shock test were characterized. Results showed that adhesion between all the 3 layers and substrates appeared good. After thermal shock tests, through microcracks which penetrated the Yb₂SiO₅ top layer were mostly halted at the Yb₂SiO₅‐Yb₂Si₂O₇ interface and no thermal growth oxide (TGO) was formed after 40‐50 quenching cycles, implying the excellent crack propagation resistance of the environmental barrier coating (EBC) system. Transmission electron microscopy analysis confirmed that twinnings and dislocations were the main mechanisms of plastic deformation of the Yb₂Si₂O₇ coating, which might have positive effects on crack propagation resistance. The thermal shock behaviors were clarified based on thermal stresses combined with thermal expansion behaviors and elastic modulus analysis. This study provides a strategy for designing EBC systems with excellent crack propagation resistance.     

Oxidation Resistance of Multiwalled Carbon Nanotubes Coated with Silicon Carbide

Multiwalled carbon nanotubes (MWCNTs) were coated with a SiC layer using SiO vapor. The growth mechanism of SiC and the oxidation resistance of the SiC-coated MWCNTs were studied. The growth of the SiC layer was controlled by adjusting the partial pressure of CO₂ using carbon felt placed in a crucible. The nanometer-sized SiC particles were deposited onto the tubes by the reaction between SiO( g ) and CO( g ). On the other hand, the thin surface of the MWCNTs was converted to the SiC layer when the carbon felt was not used. The oxidation durability of MWCNTs was improved by the SiC coating. MWCNTs were oxidized completely in air at 650°C for 60 min. However, about 90 mass% of the SiC-coated MWCNTs remained after the same oxidation test.     

In situ growth of copper nanoparticles on multiwalled carbon nanotubes and their application as non-enzymatic glucose sensor materials

Cu-nanoparticles were coated on the sidewall of multiwalled carbon nanotubes (MWCNTs) by a facile and effective in situ approach via the template of a polyelectrolyte (polyethylenimine or poly(sodium 4-styrene sulfonate)) noncovalently functionalized on MWCNTs. Extensive characterizations of the fabricated nanocomposites have been studied using X-ray diffraction, transmission electron microscopy, selected area electron diffraction, X-ray photoelectron spectroscopy, thermal gravimetric analysis and inductively coupled plasma. The results demonstrate that Cu-nanoparticles were well distributed on the surface of MWCNTs. The nanocomposites can be easily modified on the glassy carbon electrodes due to the presence of polyelectrolyte. The electrocatalytic activity of the modified electrodes towards glucose oxidation was investigated by cyclic voltammetry and chronoamperometry. The nanocomposites showed good non-enzymatic electrocatalytic responses to glucose in alkaline media, and can be used for the development of enzyme-free glucose sensors.     

Formation of thin boron nitride coating on multiwall carbon nanotube surfaces

Thin boron nitride films were deposited onto outer surfaces of multiwall carbon nanotubes (MWCNTs) by dip coating, which involves infiltration by boric acid solutions and subsequent nitridation of the boron oxide in ammonia flow at 1050 °C. The overall composition of the samples was determined by electron energy loss (EELS) and X-ray photoelectron spectroscopy (XPS), the surface composition and chemical structure of the BN coatings by XPS, the morphology of the BN/MWCNT composites by scanning and transmission electron microscopy (SEM, TEM), and the resistance against oxidation at elevated temperatures by thermal analysis (TGA). It was proved that single and multilayer BN coverage were achieved at the applied experimental conditions, and the coated samples showed significantly increased oxidation resistance compared to the uncoated MWCNTs.     

A study of the microstructure and mechanical properties of SiC coatings on spherical particles

We have investigated the effect of the microstructure on the mechanical properties of three nearly stoichiometric SiC coatings (SiC, SiC + C and SiC + Si coating), which were coated onto spherical particles as simulated nuclear fuel particles by fluidized-bed chemical vapour deposition (FBCVD). The mechanical properties of the SiC coatings were studied using micro- and nano-indentation. The microstructure was characterised using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). TEM was also used to elucidate the deformation behaviour under the indentation. The FBCVD SiC coatings studied exhibited a higher hardness than conventional CVD SiC coatings, and SiC coating gave the highest hardness among the three coatings. TEM confirmed that the presence of pores affect the Young's modulus of SiC coatings. The high hardness was attributed to the high density of dislocations and their interactions. The initiation and propagation of micro cracks under the confined shear stress was found to be responsible for the mechanism of plastic deformation. Based on this hardness-related plastic deformation mechanism, the variation of hardness in the three types of SiC coating was due to different grain morphologies.     

Field emission from carbon nanotubes on a graphitized carbon fabric

Multi-walled carbon nanotubes (MWCNTs) have been directly grown over a flexible graphitized carbon fabric by water assisted chemical vapor deposition. Field emission properties are compared with randomly oriented multi-walled and single walled carbon nanotube field emitters obtained by spin coating on to carbon fabric. The MWCNTs and single walled carbon nanotubes (SWCNTs) used in spin coating were characterized by X-ray diffraction (XRD) and Raman spectroscopy. High resolution transmission electron microscopy (HRTEM) and scanning electron microscopy (SEM) were used to characterize the field emitters. The use of graphitized carbon fabric as substrate has brought in flexibility in the fabrication of carbon nanotube field emitters. The samples show good field emission properties with a fairly stable emission current. Analysis of field emission based on the Fowler-Nordheim theory reveals current saturation effects at high applied fields for all the samples.     

Oxidation behavior of oxidation protective coatings for PIP-C/SiC composites at 1500 °C

Three-dimensional carbon fiber reinforced silicon carbide (C/SiC) composites were fabricated by precursor infiltration and pyrolysis (PIP) with polycarbosilane as the matrix precursor, SiC coating prepared by chemical vapor deposition (CVD) and ZrB₂-SiC/SiC coating prepared by CVD with slurry painting were applied on C/SiC composites, respectively. The oxidation of three samples at 1500 °C was compared and their microstructures and mechanical properties were investigated. The results show that the C/SiC without coating is distorted quickly. The mass loss of SiC coating coated sample is 4.6% after 2 h oxidation and the sample with ZrB₂-SiC/SiC multilayer coating only has 0.4% mass loss even after oxidation. ZrB₂-SiC/SiC multilayer coating can provide longtime protection for C/SiC composites. The mode of the fracture behavior of C/SiC composites was also changed. When with coating, the fracture mode of C/SiC composites became brittle. When after oxidation, the fracture mode of C/SiC composites without and with coating also became brittle.     

Formation of Nanocrystalline Silicon Carbide Powder from Chlorine-Containing Polycarbosilane Precursors

Nanocrystalline ß-SiC particulates with a grain-size range of 5-20 nm were prepared by heating a prepyrolyzed, chlorine-containing polysilane/polycarbosilane (PS/PCS) to 1600°C. The transformation from the prepyrolyzed PS/PCS to nanocrystalline SiC was investigated by differential thermal analysis, thermogravimetric analysis, X-ray diffractometry, mass spectrometry, and infrared spectroscopy. The results indicated that the nanocrystalline ß-SiC was formed by the crystallization of the PS/PCS random network and the crosslinking of Si-Si, Si-Cl, and Si-CH₂-Si bonds. Transmission electron microscopy observation showed that SiC particulates consisted of equiaxed, randomly oriented, ultrafine grains.