Preparation of vapor grown carbon fibers by microwave pyrolysis chemical vapor deposition

Vapor grown carbon fibers have been prepared without any catalyst by microwave pyrolysis chemical vapor deposition using CH₄ as source gas and N₂ as carrier gas at 1050-1150 °C. Scanning electron microscopy images reveal that vapor grown carbon fibers are made up of sub-fibers which are hexagonal and layer-like carbon. Polarized light images indicate that sub-fibers are formed by high-texture carbon and surrounded by a thick layer of medium-textured carbon. Raman spectroscopy indicates that the as-prepared vapor grown carbon fibers exhibit relatively high degree of graphitization. Also, the broadening of the “graphite” peaks observed in the X-ray diffraction pattern, as well as the intensity ratio value of ID/IG of the D- and G-band obtained from Raman spectroscopy, indicate the existence of a large quantity of defects in the vapor grown carbon fibers. Moreover, no impurity is observed by the X-ray diffraction pattern.     

化学气相沉积工艺制备绳状纳米碳管的研究

用硝酸铁作催化剂,乙炔作碳源气体,高纯氮气作稀释气体,在750℃下化学气相沉积生长了绳状纳米碳管,用高分辨扫描电镜观察了所得绳状纳米碳管的形貌.纳米碳管的直径为100～200nm,长度为10～20 μm.文中还提出了绳状纳米碳管的生长机理.     

The chemical vapor deposition of carbon on carbon fibers

The relations between chemical vapor deposition (CVD) parameters and the resultant pyrolytic carbon microstructures have been examined for matrix deposition in fibrous carbon substrates. The parameters considered are temperature (1200–1450°C), pressure (20–630 Torr), C/H ratio ($\text{1}\text{4}\text{–}\text{1}\text{14}$), total flow rate (2–16) 1/min), and carbon felt density (0·12–0·23 g/cm³). Most of the data obtained are in agreement with a CVD model for carbon; where agreement is not obtained, it is surmised that the assumptions of the model may not be satisfied.     

Micromechanical testing of carbon fibers deposited by low-pressure laser-assisted chemical vapor deposition

Carbon fibers were deposited directly from ethylene by laser-assisted chemical vapor deposition. The precursor gas pressures and the incident laser powers were varied. Micro-mechanical testing was carried out using a high-precision micro-manipulator. During three-point bend testing the fibers showed an elastic response, with no residual strain upon unloading, until fracture. The fibers’ strength and Young’s modulus are reported. A model for fiber fracture is proposed based on fiber cross-section analysis. Scanning electron microscopy was used to study the fiber cross-sections and the fiber surface morphology. The mechanical properties are related to the characteristic fiber microstructure investigated by Raman spectroscopy.     

流化床化学气相沉积法制备近化学计量比的Ti N粉体

传统气-固反应工艺制备Ti N粉体存在难以逾越的内扩散控制过程,导致制备高纯、正化学计量比的Ti N粉体至今存在巨大困难。提出了流态化化学气相沉积工艺(FBCVD)制备高质量TiN粉体,即基于TiCl₄-N₂-H₂体系,在往复运动的TiN种子粉体上沉积新生高质量TiN粉体的新方法。实验发现,当TiN种子粉体粒径大于52.95μm时,即使在1000℃沉积2 h也不会失流,同时在TiN种子粉体上获得了亚微米级的结节状新生TiN颗粒。通过氧氮分析仪和XRD分析发现,新方法显著提升了粉体的氮含量,获得了近化学计量比的TiN0.96,且氧含量下降了约40%。此外,流化床中气相沉积TiN的生长模式为岛状生长模式,为工业中制备高质量TiN粉体提供了一种新的方法。     

化学气相催化热解法制备螺旋纳米碳纤维

采用酒石酸铜前驱体热分解得到纳米铜粒子作为催化剂,分别对250℃、280℃、310℃分解产生的纳米铜粒子进行测试分析,在3个温度下用化学气相沉积法生长螺旋纳米碳纤维并进行综合热分析。采用X-射线衍射(XRD)分析其物相组成,晶粒大小;用扫描电子显微镜(SEM)观察螺旋纳米纤维的外观形貌。结果表明,310℃生长出的螺旋纳米碳纤维纯度高、外观形貌清晰,热分析质量损失少。     

Adsorption of nitrate onto nitrogen-doped activated carbon fibers prepared by chemical vapor deposition

Nitrogen-doped activated carbon fibers (ACFs) were prepared by chemical vapor deposition using melamine powder and acetonitrile for introducing quaternary nitrogen on the commercial ACFs, subsequently heated at 950 °C and activated by steam. Adsorption experiments of nitrate in aqueous solution were also conducted to evaluate adsorption capacity of the prepared ACFs using ion chromatography. The amount of introduced nitrogen content and nitrogen species on activated carbon fibers was examined by CHN elemental analyzer and X-ray photoelectron spectroscopy, respectively. As a result, adsorption capacity of quaternary nitrogen-doped ACF (ST-ML-AN-ST) was 0.75 mmol/g, indicating ca. two-times higher than that of untreated ACF (0.38 mmol/g). According to the adsorption data, the Langmuir isotherm model was the best fit. The prepared samples were also regenerated using hydrochloric acid. After regeneration, the adsorption capacity of the nitrogen-doped ACF (ST-ML-AN-ST) showed ca. 80% on average, implying that a portion of nitrates was adsorbed on the prepared ACFs irreversibly.     

Preparation of (110)-oriented SrTiO3 film on quartz glass by laser chemical vapor deposition

SrTiO₃ (STO) film was prepared on quartz glass by laser chemical vapor deposition at a deposition temperature (T_dep) ranged from 760 to 1104 K. Effect of the T_dep on the orientation, crystallinity, texture, and microstructure of the STO film was investigated. As the T_dep was increased, the preferred orientation of the STO film tended to be (110)-orientated with corresponding texture coefficient (TC) on the (110) reflection enhanced from 2.3 to 6; meanwhile, the full width at half maximum of the ω-scan on the (110) reflection decreased from 0.85° to 0.59°. The (110)-oriented grains were in wedge shape about 60 × 150 nm in size, which tended to be flat at an elevated T_dep of 1104 K.     

Preparation of silica glass doped with nitrogen by modified chemical vapor deposition

A thermodynamic analysis of the doping of silica glass with nitrogen by the chemical vapor deposition methods has been carried out. The fundamental differences are revealed between the plasma chemical vapor deposition and modified chemical vapor deposition methods. The basic parameters of nitrogen introduction into silica glass are determined by thermodynamic calculations. It is found that the main factor that ensures doping of silica glass with nitrogen by the modified chemical vapor deposition is an extremely low partial oxygen pressure in the reaction zone. The results of theoretical analysis are used in practice for nitrogenizing silica glass by modified chemical vapor deposition. The increment in the refractive index is equal to 0.0015.     

Preparation of silica glass doped with nitrogen by modified chemical vapor deposition

A thermodynamic analysis of the doping of silica glass with nitrogen by the chemical vapor deposition methods has been carried out. The fundamental differences are revealed between the plasma chemical vapor deposition and modified chemical vapor deposition methods. The basic parameters of nitrogen introduction into silica glass are determined by thermodynamic calculations. It is found that the main factor that ensures doping of silica glass with nitrogen by the modified chemical vapor deposition is an extremely low partial oxygen pressure in the reaction zone. The results of theoretical analysis are used in practice for nitrogenizing silica glass by modified chemical vapor deposition. The increment in the refractive index is equal to 0.0015.     

Preparation of molecular sieving carbon from waste resin by chemical vapor deposition

Molecular sieving carbons (MSCs) were prepared from carbonized phenol-formaldehyde resin wastes by the chemical vapor deposition (CVD) of the pyrolyzed carbon from hydrocarbon species. The pore size of the MSCs could be controlled in the range 0.37-0.42 nm by changing the hydrocarbon species pyrolyzed, the pyrolyzing temperature, and the processing time. It is shown that some of the MSCs have an excellent selectivity for separating CO₂ and CH₄, and others for separating C₃H₈ and C₃H₆. As the mechanism for controlling the pore size during CVD processing, we elucidated that the adsorption of hydrocarbon molecules first takes place on the pore surface and then the adsorbed hydrocarbons pyrolyze into carbon. Therefore, the pore size of the MSC can be adjusted by controlling the amount hydrocarbon adsorbed on the phenol-formaldehyde resin char.     

CFD simulation of laser enhanced modified chemical vapor deposition process

The modified chemical vapor deposition (MCVD) process is one of the most widely used processes to manufacture the optical fiber preforms. There have been several experimental and numerical studies to establish that thermophoresis is the dominant mechanism for the transport of silica particles to the preform wall. There also exists several modification of this process to increase the deposition efficiency in the MCVD process. In this work we have carried out computational fluid dynamics simulation of the coupled equations of mass, momentum, energy and species transport in the laser enhanced thermophoretic deposition process using the conservative finite volume scheme. The effect of laser heating on different parameters such as thermophoresis, conversion rate and deposition efficiency is examined in this study. The presence of laser heating alters the velocity and temperature profile that leads to increase in the conversion and deposition efficiency due to high thermophoresis. The results of numerical simulations are in support of experimental and analytical studies. Our numerical simulations using the conservative finite volume scheme show that deposition efficiency increases with increasing power of the laser.     

Functional copolymer coatings on electrospun fibers via photo-initiated chemical vapor deposition

With the increasing use of implantable patches in biomedical applications, the significance of surface modification techniques in improving biocompatibility, enhancing adhesion, and regulating drug release has grown. A significant challenge that these methods must address is ensuring that the process does not harm the delicate fibers or therapeutic agents they contain. Here, we report surface functionalization of implantable, curcumin loaded Polycaprolactone (PCL) patches with pH-responsive poly(2-hydroxyethyl methacrylate-co-4-vinylpyridine), p(HEMA-co-4VP) polymer thin film. The polymer was coated on the patch surface via photo-initiated chemical vapor deposition (piCVD) where the polymerization was initiated by the UV degradation of the initiator tert-butyl peroxide (TBPO) and the monomer HEMA. Additionally, the piCVD method was utilized to crosslink the HEMA without the use of additional crosslinkers. The pH-responsiveness of the coating was achieved by incorporating 4VP into the copolymer structure. The effect of the coating was demonstrated through degradation and drug release studies. The presence of the polymer coating decelerated the fiber degradation and the pH-dependent swelling of the coating allowed for the control of drug release rates from the patches. The innovative use of piCVD as a coating method provides a platform for advancing tailored surface modifications in various biomedical applications.     

High-speed deposition of silicon nitride thick films via halide laser chemical vapor deposition

Silicon nitride shows significant potential in the field of surface protection for electronic devices owing to its excellent insulation performance and mechanical properties. In this study, silicon nitride films were fabricated via halide laser chemical vapor deposition (LCVD). The effects of deposition parameters on the crystallinity, microstructure, deposition rate (R_dep), Vickers microhardness, nano-hardness and electrical resistivity were investigated. The maximum R_dep of the silicon nitride thick films was 972 µm/h at T_dep of 1573 K and P_tot of 10 kPa, which is the highest value compared with those obtained via conventional CVD. As T_dep increased, the Vickers microhardness and nano-hardness of the films increased to the highest value of 25.1 GPa and 34.8 GPa at 1573 K, respectively. The electrical resistivity of the films decreased with increasing T_dep and showed a maximum value of 1.49 × 10¹⁴ Ω·cm at T_dep of 1273 K.     

High-speed epitaxial growth of SrTiO3 films on MgO substrates by laser chemical vapor deposition

Epitaxial (100) and (111) SrTiO₃ films were prepared on (100) and (111) MgO single-crystal substrates, respectively, using laser chemical vapor deposition. The effect of deposition temperature (T_dep) on the orientation and microstructure of the SrTiO₃ films was investigated. On the (100) MgO substrates, SrTiO₃ films showed a (111) orientation at a low T_dep of 1023 K. (100) SrTiO₃ films, which were epitaxially grown at T_dep=1123–1203 K, had dense cross sections and flat surfaces with rectangular-shaped terraces. On the (111) MgO substrates, (111) SrTiO₃ films were epitaxially grown at T_dep=983–1063 K; however, these films' orientations became random at high T_dep of 1063–1113 K. The (111) SrTiO₃ films consisted of columnar grains with triangular pyramidal caps. The deposition rates of the epitaxial (100) and (111) SrTiO₃ films were 13–25 and 18–32 μm h⁻¹, respectively, which is 5–530 times higher than those obtained by MOCVD.     

Fine-grained 3C-SiC thick films prepared via hybrid laser chemical vapor deposition

An ultraviolet laser (λ = 266 nm) operated in pulsed mode and a diode laser (λ = 1060 nm) operated in continuous mode were simultaneously applied to create a hybrid laser chemical vapor deposition (CVD) approach. Fine-grained 3C-SiC thick films were prepared via hybrid laser CVD by using SiCl₄, CH₄ and H₂ as precursors. The effects of the ultraviolet laser on the preferred orientations, microstructures, microhardness values and deposition rates of 3C-SiC thick films were investigated. The 3C-SiC thick films that were prepared at 4 kPa via diode laser CVD exhibited <110>-orientations and 5-100 µm grain sizes, whereas those prepared via hybrid laser CVD were randomly oriented with 0.5-5 µm grain sizes. Compared to diode laser CVD, the additional irradiation of the ultraviolet laser in the hybrid laser CVD improved the Vickers microhardness values of the 3C-SiC thick films from 30 to 35 GPa, and the maximum deposition rate was also increased from 935 to 1230 µm/h.     

Synthesis of oriented nanotube films by chemical vapor deposition

Oriented nanotube films (20-35 μm thick) were synthesised on flat silicon substrates by chemical vapor deposition (CVD) of a gas mixture of acetylene and nitrogen. For the CVD we used metal oxide clusters formed by spin coating an iron(III) nitrate ethanol solution onto a silicon substrate and subsequent heating. The cluster density and its effects on the nanotube density were investigated as a function of the iron(III) nitrate concentration and the synthesis temperature. A high nanotube density was achieved with a high density of iron oxide clusters as nucleation centres for the growth of nanotubes. The cluster density was controlled by the iron(III) concentration of the ethanolic coating solution and by the synthesis temperature. The perpendicular orientation of the nanotubes with respect to the substrate surface is attributed to a high density of nanotubes.