Study on silicon carbide nanowires produced from carbon blacks and structure of carbon blacks

Silicon carbide nanowires were produced from carbon blacks at 1473 K and their microstructure was characterized by TEM, X-ray diffraction, FTIR and Raman spectroscopy. Nanowires of uniform diameters, the smallest averaging 10 nm, and narrow size distribution were obtained from graphitized carbon blacks, and their morphology depends on the properties of carbon black pecursors. High concentration of stacking faults and twins was detected. In addition to silicon carbide nanowires, a silicon carbide layer, about 20 nm thick, was formed on the surface of carbon black aggregates. The interior of the aggregates did not react and analysis of the data showed that it is composed of a mixture of amorphous carbon and small graphitic crystallites. The small lateral sizes of these crystallites remain unchanged during the graphitization process which is limited to the outer layer of the aggregates.     

Surface transformations of carbon (graphene, graphite, diamond, carbide), deposited on polycrystalline nickel by hot filaments chemical vapour deposition

The deposition of carbon has been studied at high temperature on polycrystalline nickel by hot filaments activated chemical vapor deposition (HFCVD). The sequences of carbon deposition are studied by surface analyses: Auger electron spectroscopy (AES), electron loss spectroscopy (ELS), X-ray photoelectron spectroscopy (XPS) in a chamber directly connected to the growth chamber. A general scale law of the (C/Ni) intensity lines is obtained with a reduced time. Both, shape analysis of the AES C KVV line and the C1s relative intensity suggest a three-step process: first formation of graphene and a highly graphitic layer, then multiphase formation with graphitic, carbidic and diamond-like carbon and finally at a critical temperature that strongly depends on the pretreatment of the polycrystalline nickel surface, a rapid transition to diamond island formation. Whatever the substrate diamond is always the final product and some graphene layers the initial product. Moreover it is possible to stabilize a few graphene layers at the initial sequences of carbon deposition. The duration of this stabilization step is strongly depending however on the pre-treatment of the Ni surface.     

石墨表层对四面体非晶炭膜中受激电子的石墨建序化作用

对渗气阴极真空电弧法制备的四而体非晶炭(ta-c)膜实施氧等离子体刻蚀,消除其表面石墨层后,发现:原沉积膜中ta-C石墨表层的消除会影响其受激电子的石墨建序化.应用发射电子能耗谱,表面增强拉曼光谱和表面敏化X光吸收光谱等测量方法,测定了其表层的淌除(程度).样品的氧等离子体刻蚀阻迟了受激电子的石墨化作用,可能归因于多相成核过程中石墨晶核的缺失之故.     

Synthesis of graphitic carbon nitride by reaction of melamine and uric acid

Graphitic carbon nitrides were synthesized starting from melamine and uric acid. Uric acid was chosen because it thermally decomposes, and reacts with melamine by condensation at temperatures in the range of 400–600 °C. The reagents were mixed with alumina and subsequently the samples were treated in an oven under nitrogen flux. Alumina favored the deposition of the graphitic carbon nitrides layers on the exposed surface. This method can be assimilated to an in situ chemical vapor deposition (CVD). Infrared (IR) spectra, as well as X-ray diffraction (XRD) patterns, are in accordance with the formation of a graphitic carbon nitride with a structure based on heptazine blocks. These carbon nitrides exhibit poor crystallinity and a nanometric texture, as shown by transmission electron microscopy (TEM) analysis. The thermal degradation of the graphitic carbon nitride occurs through cyano group formation, and involves the bridging tertiary nitrogen and the bonded carbon, which belongs to the heptazine ring, causing the ring opening and the consequent network destruction as inferred by connecting the IR and X-ray photoelectron spectroscopy (XPS) results. This seems to be an easy and promising route to synthesize graphitic carbon nitrides. Our final material is a composite made of an alumina core covered by carbon nitride layers.     

Effect of substrate and catalyst on the transformation of carbon black into nanotubes

Structural transformation of carbon black (CB) into nanotubes and nano-onion like structures in the presence of bimetallic catalysts (Fe and Ni) is reported and the influence of the substrate (alumina and stainless steel) in the structural transformation is studied. In addition, the importance of a specific weight ratio of CB to catalyst in the transformation of amorphous CB into graphitic nanostructures is verified. The experiments were carried out at 1,000 °C in a horizontal tube furnace under N₂ atmosphere. The samples were characterized by transmission electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, Raman spectroscopy and also thermomagnetic analysis (Curie-temperature determinations) were done to assess thermally induced magnetic phase changes. All the characterization techniques showed the resulting structures were influenced by the substrate and weight ratio for CB to catalysts. However, there was no significant difference in the magnetic performance of the resulting structures obtained on different substrates.     

A Novel Duplex Low-temperature Chromizing Process at 500℃

An optimized low-temperature chromizing process at 500℃ was realized on a plain medium-carbon steel with 0.45 wt pct carbon via a duplex chromizing process which consists of a precursor plasma nitriding, and a followed salt bath thermoreactive deposition and diffusion （TRD） chromizing process. CrN layer with a thin diffusion layer underneath was formed. The duplex chromizing process was studied by optical microscopy （OM）, scanning electron microscopy （SEM）, energy dispersive X-ray spectroscopy （EDS）, X-ray diffraction （XRD）, and transmission electron microscopy （TEM）. It was found that the chromizing speed at 500℃ was successfully enhanced by adding more Cr-Fe powders into the salt bath, and the CrN layer formed at the cost of the prior nitride compound layer. A CrN layer with average 8.1/~m in thickness and 1382 HV0.01 in microhardness was formed on the substrate by duplex chromizing at 500℃ for 24 h. Further more, the CrN layer consisted of nanocrystalline CrN grains.     

A Novel Duplex Low-temperature Chromizing Process at 500℃

An optimized low-temperature chromizing process at 500℃ was realized on a plain medium-carbon steel with 0.45 wt pct carbon via a duplex chromizing process which consists of a precursor plasma nitriding, and a followed salt bath thermoreactive deposition and diffusion (TRD) chromizing process. CrN layer with a thin diffusion layer underneath was formed. The duplex chromizing process was studied by optical microscopy(OM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction(XRD), and transmission electron microscopy (TEM). It was found that the chromizing speed at 500℃ was successfully enhanced by adding more Cr-Fe powders into the salt bath, and the CrN layer formed at the cost of the prior nitride compound layer. A CrN layer with average 8.1μm in thickness and 1382 HV0.01 in microhardness was formed on the substrate by duplex chromizing at 500℃ for 24 h. Further more, the CrN layer consisted of nanocrystalline CrN grains.     

Microscope studies of the morphology and structure of carbon nanotubes

We have studied the morphologies and structures of carbon nanotubes (bucky-tubes) and carbon nanoparticles (buckyonions) using scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM) and scanning tunnelling microscopy (STM). By SEM the carbon nanotubes are observed with features similar to those of some fibrous whiskers grown from pyrolytic graphite. This growth feature is supported by transmission electron microscopy (TEM) observations. The TEM results show also that the graphitic sheets can be bent into curved shapes to cap the nanotubes or form the onions. In the curved graphitic sheets elastic strains induced by layer mismatches and dislocations are revealed. The STM observations on the nanotubes show a bundle-like morphology of the carbon nanotubes, and by atomic resolution images the zigzag and armchair atomic configurations may be identified. The results also show structural distortions which may be produced by folding the graphite sheets to create the nanotubes and are responsible for the lattice mismatch.     

In situ nucleation of carbon nanotubes by the injection of carbon atoms into metal particles

The synthesis of carbon nanotubes (CNTs) of desired chiralities and diameters is one of the most important challenges in nanotube science and achieving such selectivity may require a detailed understanding of their growth mechanism. We report the formation of CNTs in an entirely condensed phase process that allows us, for the first time, to monitor the nucleation of a nanotube on the spherical surface of a metal particle. When multiwalled CNTs containing metal particle cores are irradiated with an electron beam, carbon from graphitic shells surrounding the metal particles is ingested into the body of the particle and subsequently emerges as single-walled nanotubes (SWNTs) or multiwalled nanotubes (MWNTs) inside the host nanotubes. These observations, at atomic resolution in an electron microscope, show that there is direct bonding between the tubes and the metal surface from which the tubes sprout and can be readily explained by bulk diffusion of carbon through the body of catalytic particles, with no evidence of surface diffusion.     

Effect of nano carbon additives on the microstructure of polyvinyl chloride heated up to 2000°C

Polyvinyl chloride (PVC) is one of the most commonly used thermoplastic materials among worldwide polymer consumption. The PVC exhibits particular inherent properties such as low cost and high performance, it can be obtained from different techniques. PVC products will finally become waste. As a result, the quantity of waste PVC is gradually increasing. The waste product PVC can be converted to graphite. Graphitic structure was obtained by carbonization of polymers to 1000°C, and subsequent heating to 2000°C. In this study the effect of carbon nanotube (CNT) and carbon black additives on the graphitic microstructure of PVC polymer was investigated. The solution of PVC in tetrahydrofuran (THF) was prepared then additives were dispersed in solution by ultrasonic. The additives were applied in the concentration between 1 and 3wt%. Changes in graphitic microstructure were studied via Raman spectroscopy, X-ray diffraction, and Transmission electron microscopy (TEM). Morphology of microstructures studies with scanning electron microscopy (SEM). The results show that the additives do not develop the graphitic microstructure and do not improve the formation of flaky graphite crystals.     

Silicide-induced multi-wall carbon nanotube growth on silicon nanowires

A novel multi-walled carbon nanotube (MWNT) growth process is reported based on carbon incorporation in a nickel catalyst layer deposited via plasma-enhanced atomic layer deposition (PEALD) on silicon nanowires and silicon wafer substrates. As-deposited PEALD Ni films containing relatively high amounts of carbon (>18?at.%) were observed to promote the growth of MWNTs upon post-deposition rapid thermal annealing. For these films the carbon originated from the ALD precursor ligand and MWNT growth occurred in the absence of a vapor-phase carbon feedstock. MWNT growth relied on the formation of nickel silicide at the PEALD Ni/Si interface which increased the local carbon concentration in the Ni film sufficiently to promote carbon saturation/precipitation at Ni catalyst grains and nucleate MWNT growth. Similar MWNT growth from annealed PEALD Ni films was not observed on SiO(2)-coated Si wafer substrates, consistent with the role of silicidation in the observed Ni-catalyzed MWNT growth on Si. This MWNT growth mode requires neither the catalytic decomposition of a gaseous hydrocarbon source nor the high-temperature pyrolysis of metallocene materials and purposely avoids a catalyst diffusion barrier at the Si substrate, commonly used in MWNT growth processes on Si.     

Preparation of carbon spheres by low-temperature pyrolysis of cyclic hydrocarbons

Low-temperature pyrolytic decomposition of xylene, benzene, toluene, and naphthalene was investigated as a low-cost method for synthesis of a large quantity of perfectly shaped pure carbon spheres. The reaction occurred in a closed iron container at temperatures in the range of 500–700 °C and under pressure of 20 MPa. Some of the experiments were carried out in the presence of distilled water in vapor state near to its critical point, under which conditions it reacted as a very strong oxidant. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and X-ray diffraction (XRD) analysis were used to investigate the properties of the material obtained. The results demonstrated that synthesis had proceeded in the following sequence: vaporization of hydrocarbon, hydrocarbon transformation to condensing drops of heavy hydrocarbons, then drop growth accompanied by continuous alteration of the heavy carbon compounds until their final carbonization. Synthesis in a closed space stimulated particle growth, and particle diameters reached 1 to 12 μm. Continuous condensation of vapor onto the resulting drops caused agglomeration of some of the spheres to form pearl-necklace-like chains when the spheres docked to one another in the course of growth. Carbon atoms in the spheres were arranged in concentric, incompletely closed graphitic shells, which made them stable up to 600 °C in air. Above this temperature, rapid sphere degeneration occurred. Oxygen reacted with carbon atoms situated at the shell edges during heating in air, with some remaining in the spheres; oxygen penetration increased with treatment temperature.     

Effects of carbon content of carbon steel on its dissolution into a molten aluminum alloy

Hot dip aluminizing of carbon steels with different carbon concentration ranging 0.2–1.1 wt.% was carried out in a molten Al–9.08 wt.% Si–0.98 wt.% Fe alloy at 660 °C. The steel specimens lost weight as a result of dissolution into the melt, and an intermetallic layer was formed on the surface of them. The specimens showed varied dissolution rates depending on carbon concentration. The specimen with the highest carbon content exhibited the slowest dissolution rate. The thickness of the intermetallic layer increased with dipping time following a parabolic relationship. The growth rate of the layer decreased with increase of the carbon content. A diffusion mechanism to control the dissolution of the carbon steel into the molten aluminum alloy was suggested, and the effect of carbon content on the dissolution of the steel substrate into the melt was discussed in connection with the proposed diffusion mechanism and microstructural observations.     

Fabrication of flat capped carbon nanotubes using an arc-discharge method assisted with a Sm-Co catalyst

In this study, carbon nanotubes (CNTs) were fabricated using an arc-discharge method assisted with samarium-cobalt (Sm-Co) chloride as a catalyst. The optimal fabrication condition was determined through a series of experiments on various ambient conditions. Observations were completed using scanning electron microscopy (SEM), Raman spectroscopy, and tunneling electron microscopy (TEM); the main products we observed are well-structured multi-walled carbon nanotubes. By identifying the radial breathing modes (RBMs) of the Raman spectra with a TEM micrograph, we also observed a small number of single-walled carbon nanotubes. With the assistance of the Sm-Co chloride catalyst, the RBMs of the Raman spectra were measured in the ambient pressure of 760 torr. The TEM observations revealed that our nanotubes have good graphitic structures and almost no bamboo defects, which agrees with their Raman measurements with a high I_G/I_D ratio (~88). A perfect graphitic flat cap was found to be attached at the end of the nanotube. Simulation shows that by incorporating 5 carbon pentagons, it is possible to construct a flat capped carbon nanotube. The results of our experiment offer a unique approach to growing high quality CNTs. Such a flat capped structure may useful for further advanced application in nano-electronics and nano-optics.     

烧蚀过程中C/C复合材料的结构演变

利用SEM和TEM考察了3D C／C复合材料在电弧加热器上烧蚀后的材料表层显微组织结构变化。发现炭纤维和基体炭中的石墨微晶经过烧蚀后都得到了明显的发展。在距烧蚀表面几个纳米的深度范围内形成了高度取向的带状石墨织构，同时，在带状织构中间也形成了许多孔洞和缝隙。在距烧蚀表面几个微米的深度形成了卷曲柱状结构，在这些柱状结构周围有许多缺陷。在纤维和基体炭的界面区域，靠近纤维一侧形成了带状织构，且织构间的缝隙变大。     

Thermal stability of Cr-doped diamond-like carbon films synthesized by cathodic arc evaporation

Cr-doped diamond-like carbon (DLC) films were synthesized using a cathodic arc evaporation (CAE) process. The thermal oxidation behavior of Cr-doped DLC films was investigated using thermal gravimetric analysis (TGA) and differential thermal analysis (DTA). The phase identification and microstructural examinations were conducted by X-ray diffraction, scanning electron spectroscopy (SEM), transmission electron spectroscopy (TEM), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS) in order to understand the characteristics of Cr-doped DLC films. The as-deposited Cr-doped DLC film exhibits a lamellar structure observed by TEM. A significant weight loss of film results from the thermal oxidation of carbon occurred at 290 to 342 °C. At the temperature higher than 342 °C, slight weight gain of specimen was observed due to the thermal oxidation of the underlying CrC_xN_y and CrN interlayer. By heat-treated specimens from 200 to 400 °C, Raman spectra reveal the increase of I_D/I_G value conforming to the graphitiation process of the Cr-doped DLC films. Finally, surface reactions of the annealed films using XPS analysis were discussed.     

Preparation, microstructure and hydrogen sorption properties of nanoporous carbon aerogels under ambient drying

Organic aerogels are prepared by the sol-gel method from polymerization of resorcinol with furfural. These aerogels are further carbonized in nitrogen in order to obtain their corresponding carbon aerogels (CA); a sample which was carbonized at 900?°C was also activated in a carbon dioxide atmosphere at 900?°C. The chemical reaction mechanism and optimum synthesis conditions are investigated by means of Fourier transform infrared spectroscopy and thermoanalyses (thermogravimetric/differential thermal analyses) with a focus on the sol-gel process. The carbon aerogels were investigated with respect to their microstructures, using small angle x-ray scattering (SAXS), transmission electron microscopy (TEM) and nitrogen adsorption measurements at 77?K. SAXS studies showed that micropores with a radius of gyration of <0.35 ± 0.07 to 0.55 ± 0.05?nm were present, and TEM measurements and nitrogen adsorption showed that larger mesopores were also present. Hydrogen storage properties of the CA were also investigated. An activated sample with a Brunauer-Emmett-Teller surface area of 1539 ± 20?m(2)?g(-1) displayed a reasonably high hydrogen uptake at 77?K with a maximum hydrogen sorption of 3.6?wt% at 2.5?MPa. These results suggest that CA are promising candidate hydrogen storage materials.     

On selective laser melting of ultra high carbon steel: Effect of scan speed and post heat treatment

Selective laser melting is a laser‐based additive manufacturing process applying layer manufacturing technology and is used to produce dense parts from metallic powders. The application of selective laser melting on carbon steels is still limited due to difficulties arising from carbon content. This experimental investigation aims at gaining an understanding of the application of the process on ultra high carbon steel, which is a special alloy with remarkable structural properties suitable for different industrial applications. The feedstock ultra high carbon steel (2.1% C) powder, 20 μm to 106 μm was prepared by water atomizing technique. This powder was used for the selective laser melting to build specimens 10×10×40 mm in dimensions. To decrease the thermal stresses during layer by layer building, laser scanning was done through 5×5 mm random island patterns while layer thickness was 30 μm. Laser beam diameter, maximum power output, layer thickness and scan speed range were 0.2 mm, 100 W, 30 μm and 50–200 mm/s respectively. The process was done inside high purity nitrogen environment, with less than 0.5% oxygen content. The results illustrate the influence of scan speed from 50 to 200 mm/s on product geometry and dimensions, surface roughness, internal porosity and cracks, microstructure and surface hardness. The effect of post heat treatment by heating and holding for one hour (annealing) at different temperatures of 700°C, 750°C, 950°C is studied. The results indicate that selective laser melting is able to produce near to 95% density of ultra high carbon steel parts with acceptable geometry and surface quality. Porosity cracks, and microstructure formed during the process could be controlled through proper selection of process parameters and post heat treatment. Industrial ultra high carbon steel products can be rapidly fabricated by selective laser melting.     

碳纳米管/羟基磷灰石复合材料的制备及表征

以含钴介孔分子筛为催化剂、乙醇为碳源, 采用CVD法制备碳纳米管(CNTs)。通过原位合成法制备一系列不同碳纳米管含量的碳纳米管/羟基磷灰石(CNTs/HA)复合材料。分别采用XRD、FTIR、TEM、N₂吸附-脱附和Raman光谱等分析手段, 对所合成CNTs/HA复合材料的晶相、结构、形貌和比表面积等进行了表征。同时研究了碳纳米管的添加量对所合成CNTs/HA复合材料形貌的影响。XRD与Raman结果表明, 所得CNTs/HA复合粉体中仅有CNTs与HA两种物相, 纯度较高, 结晶度较好; TEM结果显示, CNTs/HA复合材料中CNTs表面均匀包裹着一层纳米级的针状HA晶粒, 两者形成了较强的界面结合, 且当CNTs与HA的质量比为3:17时, CNTs与HA形成最佳结合状态; N₂吸附-脱附表征结果表明, 与HA的比表面积相比, CNTs/HA复合材料具有较高比表面积。     

Blue luminescence from carbon modified ZnO nanoparticles

In this work, a novel method was used to prepare carbon modified ZnO nanoparticles. The nanoparticles were coated with a layer of poly(methyl methacrylate) by γ radiation firstly, and then the coated nanoparticles were annealed in air. The polymer was burned and carbon was left on the surface of ZnO nanoparticles. A stable blue luminescence peak (~420 nm) can be observed for the carbon modified ZnO nanoparticles. The carbon modified ZnO nanoparticles were also investigated by X-ray photoelectron spectroscopy. The origin of the blue emission was discussed. The blue PL is related to the left carbon. This novel method also can be used to prepare other carbon modified nanoparticles.