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This article shows the results of experiments to grow Nitrogen incorporated ultrananocrystalline diamond (N-UNCD) films on commercial natural graphite (NG)/Cu anodes by hot chemical vapor deposition (HFCVD) using a gas mixture of Ar/CH4/N2/H2. The experiments focused on studying the effect of the pressure in the HFCVD chamber, filament-substrate distance, and temperature of the substrate. It was found that a substrate distance of 3.0 cm and a substrate temperature of 575 C were optimal to grow N-UNCD film on the graphite surface as determined by Raman spectroscopy, SEM, and TEM imaging. XPS analysis shows N incorporation through the film. Subsequently, the substrate surface temperature was increased using a heater, while keeping the substrate-filament distance constant at 3.0 cm. In this case, Raman spectra and SEM images of the substrate surface showed a major composition of graphite in the film as the substrate-surface temperature increased. Finally, the process pressure was increased to 10 Torr where it was seen that the growth of N-UNCD film occurred at 2.0 cm at a substrate temperature of 675 C. These results suggest that as the process pressure increases a smaller substrate-filament distance and consequently a higher substrate surface temperature can still enable the N-UNCD film growth by HFCVD. This effect is explained by a mean free path analysis of the main precursors H2 and CH3 molecules traveling from the filament to the surface of the substrate The potential impact of the process developed to grow electrically conductive N-UNCD films using the relatively low-cost HFCVD process is that this process can be used to grow N-UNCD films on commercial NG/Cu anodes for Li-ion batteries (LIBs), to enable longer stable capacity energy vs. charge/discharge cycles.
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The electrical properties of graphene on dielectric substrates, such as silicon carbide (SiC), have received much attention due to their interesting applications. This work presents a method to grow graphene on a 6H-SiC substrate at a pressure of 35 Torr by using the hot filament chemical vapor deposition (HFCVD) technique. The graphene deposition was conducted in an atmosphere of methane and hydrogen at a temperature of 950 °C. The graphene films were analyzed using Raman spectroscopy, scanning electron microscopy, atomic force microscopy, energy dispersive X-ray, and X-ray photoelectron spectroscopy. Raman mapping and AFM measurements indicated that few-layer and multilayer graphene were deposited from the external carbon source depending on the growth parameter conditions. The compositional analysis confirmed the presence of graphene deposition on SiC substrates and the absence of any metal involved in the growth process.
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Vertical graphene nanowalls (VGNs) with excellent heat-transfer properties are promising to be applied in the thermal management of electronic devices. However, high growth temperature makes VGNs unable to be directly prepared on semiconductors and polymers, which limits the practical application of VGNs. In this work, the near room-temperature growth of VGNs was realized by utilizing the hot filament chemical vapor deposition method. Catalytic tantalum (Ta) filaments promote the decomposition of acetylene at â¼1600 °C. Density functional theory calculations proved that C2H* was the main active carbon cluster during VGN growth. The restricted diffusion of C2H* clusters induced the vertical growth of graphene nanoflakes on various substrates below 150 °C. The direct growth of VGNs successfully realized the excellent interfacial contact, and the thermal contact resistance could reach 3.39 × 10-9 m2·K·W-1. The temperature of electronic chips had a 6.7 °C reduction by utilizing directly prepared VGNs instead of thermal conductive tape as thermal-interface materials, indicating the great potential of VGNs to be directly prepared on electronic devices for thermal management.
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By using a methane and hydrogen process gas mixture in an appropriate hot-filament CVD process without further dopant, high electrical conductivity of over 100 S/cm has been achieved in nanocrystalline diamond films deposited on silicon single-crystalline substrates. Furthermore, it was found that an oxygen reactive-ion etching process (O-RIE) can improve the diamond film surface's electron affinity, thus reducing the specific contact resistance. The reduction of the specific contact resistance by a factor of up to 16 was realized by the oxygen ion etching process, down to 6×10-6 Ωcm2. We provide a qualitative explanation for the mechanism behind the contact resistance reduction in terms of the electron affinity of the diamond surface. With the aid of XPS, AFM, and surface wetting measurements, we confirmed that a higher surface electron affinity is responsible for the lower specific contact resistance of the oxygen-terminated nanocrystalline diamond films.
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Single-crystal diamonds in the form of micrometer-scale pyramids were produced using a combination of hot-filament (HF) chemical vapor deposition (CVD) and thermal oxidation processes. The diamond pyramids were compared here with similar ones that were manufactured using plasma-enhanced (PE) CVD. The similarities revealed in the morphology, Raman, and photoluminescent characteristics of the needles obtained using the hot-filament and plasma-enhanced CVD are discussed in connection with the diamond film growth mechanism. This work demonstrated that the HF CVD method has convincing potential for the fabrication of single-crystal diamond needles in the form of regularly shaped pyramids on a large surface area, even on non-conducting substrates. The experimental results demonstrated the ability for the mass production of the single-crystal needle-like diamonds, which is important for their practical application.
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W atoms/clusters are employed to in situ assist the development of layered vertically aligned carbon nanotube arrays (VACNTs) through hot-filament-assisted chemical vapor deposition (HFCVD) with liquid binary Fe3O4/AlOx catalysts. The hot W filament was utilized to in situ evaporate atomic W and form W clusters on Fe catalysts, which have a strong impact on the growth of layered VACNT arrays. The migration and Ostwald ripening of Fe catalysts are found to be suppressed immediately with more W clusters deposition during CNT growth. Through controlling the deposition of W clusters, the electrochemical energy storage performance of as-prepared layered VACNT arrays is also tunable as electrodes of ion-based supercapacitors. The layered VACNT arrays can achieve a high capacity of 83.1 mF cm-2 and possess desirable rate performance due to the suitable hot filament condition (55 W for 90 s). This work provides a new perspective to in-depth understand the behavior of W filament during HFCVD and the significant role of the in situ generated W clusters on the growth of CNTs by maintaining the catalytic activity and structure of catalysts.
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Although the growth rate of diamond increased with increasing methane concentration at the filament temperature of 2100 °C during a hot filament chemical vapor deposition (HFCVD), it decreased with increasing methane concentration from 1% CH4 -99% H2 to 3% CH4 -97% H2 at 1900 °C. We investigated this unusual dependence of the growth rate on the methane concentration, which might give insight into the growth mechanism of a diamond. One possibility would be that the high methane concentration increases the non-diamond phase, which is then etched faster by atomic hydrogen, resulting in a decrease in the growth rate with increasing methane concentration. At 3% CH4 -97% H2, the graphite was coated on the hot filament both at 1900 °C and 2100 °C. The graphite coating on the filament decreased the number of electrons emitted from the hot filament. The electron emission at 3% CH4 -97% H2 was 13 times less than that at 1% CH4 -99% H2 at the filament temperature of 1900 °C. The lower number of electrons at 3% CH4 -97% H2 was attributed to the formation of the non-diamond phase, which etched faster than diamond, resulting in a lower growth rate.
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Diamond is a very interesting material with a wide range of properties, making it highly applicable, for example, in power electronics, chemo- and biosensors, tools' coatings, and heaters. Due to the high demand for this innovative material based on the properties it is already expected to have, it is important to obtain homogeneous diamond layers for specific applications. Doping is often chosen to modify the properties of layers. However, there is an alternative way to achieve this goal and it is shown in this publication. The presented research results reveal that the change in methanol content during the Hot Filament Chemical Vapour Deposition (HF CVD) process is a sufficient factor to tune the properties of deposited layers. This was confirmed by analysing the properties of the obtained layers, which were determined using Raman spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD), and an atomic force microscope (AFM), and the results were correlated with those of X-ray photoelectron spectroscopy (XPS). The results showed that the increasing of the concentration of methanol resulted in a slight decrease in the sp3 phase content. At the same time, the concentration of the -H, -OH, and =O groups increased with the increasing of the methanol concentration. This affirmed that by changing the content of methanol, it is possible to obtain layers with different properties.
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We report the first direct synthesis of graphene on SiO2/Si by hot-filament chemical vapor deposition. Graphene deposition was conducted at low pressures (35 Torr) with a mixture of methane/hydrogen and a substrate temperature of 970 °C followed by spontaneous cooling to room temperature. A thin copper-strip was deposited in the middle of the SiO2/Si substrate as catalytic material. Raman spectroscopy mapping and atomic force microscopy measurements indicate the growth of few-layers of graphene over the entire SiO2/Si substrate, far beyond the thin copper-strip, while X-ray photoelectron spectroscopy and energy-dispersive X-ray spectroscopy showed negligible amounts of copper next to the initially deposited strip. The scale of the graphene nanocrystal was estimated by Raman spectroscopy and scanning electron microscopy.
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We herein present an alternative geometry of nanostructured carbon cathode capable of obtaining a low turn-on field, and both stable and high current densities. This cathode geometry consisted of a micro-hollow array on planar carbon nanostructures engineered by femtosecond laser. The micro-hollow geometry provides a larger edge area for achieving a lower turn-on field of 0.70 V/µm, a sustainable current of approximately 2 mA (about 112 mA/cm2) at an applied field of less than 2 V/µm. The electric field in the vicinity of the hollow array (rim edge) is enhanced due to the edge effect, that is key to improving field emission performance. The edge effect of the micro-hollow cathode is confirmed by numerical calculation. This new type of nanostructured carbon cathode geometry can be promisingly applied for high intensity and compact electron sources.
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We report on the different surface structures of tungsten oxides which have been synthesized using a simple post-annealing-free hot-filament CVD technique, including 0D nanoparticles (NPs), 1D nanorods (NRs), and 2D nanosheet assemblies of 3D hierarchical nanoflowers (NFs). The surface morphologies, crystalline structures, and material compositions have been characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), and Raman spectroscopy, respectively. The sensor performances based on the synthesized samples of various surface morphologies have been investigated, as well as the influences of operating temperature and applied bias. The sensing property depends closely on the surface morphology, and the 3D hierarchical nanoflowers-based gas sensor offers the best sensitivity and fastest response time to NH3 and CH3 gases when operated at room temperature.
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Property modulation of graphene glass by heteroatom doping such as boron (B) and nitrogen (N) is important to extend its practical applications. However, unlike N doping, research studies about the metal-free synthesis of B-doped graphene on glass through the chemical vapor deposition (CVD) method are rarely reported. Herein, we report a hot-filament CVD approach to prepare B-doped graphene glass using diborane (B2H6) as the B dopant. The synthesized B-doped graphene was uniform on a large-scale and composed of nanocrystalline graphene grains. By raising the B2H6 flow from 0 to 15 sccm, the B content of graphene was facilely modulated from 0 to 5.3 at. %, accompanied with the improvement of both transparency and conductivity. The B-doped graphene prepared on glass at 15 sccm B2H6 flow presented the optimal transparent conductive performance superior to those of most reported graphene glass fabricated by other state-of-the-art approaches. Furthermore, for the first time, the performance of graphene glass for wave energy harvesting has been elaborated. It was found that the output power produced by inserting graphene glass into 0.6 M sodium chloride (NaCl) solution could be improved by more than 6 times through B doping. The significant enhancement resulted from the higher waving voltage and smaller resistance of B-doped graphene on glass than the pristine ones. In addition, the waving voltage inversed the polarity after B doping, which was due to the opposite variation of surface potential of pristine and B-doped graphene after NaCl immersion. This work would pave ways for the metal-free preparation and expand the energy-harvesting applications of B-doped graphene materials.
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In this work, we fabricated three carbon nanoplume structured samples under different temperatures using a simple hot filament physical vapor deposition (HFPVD) process, and investigated the role of surface morphology, defects, and graphitic content on relative humidity (RH) sensing performances. The Van der Drift growth model and oblique angle deposition (OAD) technique of growing a large area of uniformly aligned and inclined oblique arrays of carbon nanoplumes (CNPs) on a catalyst-free silicon substrate was demonstrated. The optimal growing temperature of 800 °C was suitable for the formation of nanoplumes with larger surface area, more defect sites, and less graphitic content, compared to the other samples that were prepared. As expected, a low detection limit, high response, capability of reversible behavior, and rapid response/recovery speed with respect to RH variation, was achieved without additional surface modification or chemical functionalization. The holes' depletion has been described as a RH sensing mechanism that leads to the increase of the conduction of the CNPs with increasing RH levels.
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Direct growth of graphene films on glass is of great importance but has so far met with limited success. The noncatalytic property of glass results in the low decomposition ability of hydrocarbon precursors, especially at reduced temperatures (<1000 °C), and therefore amorphous carbon (a-C) films are more likely to be obtained. Here, we report the hydrogen influence on the structural and electrical properties of carbon films deposited on quartz glass at 850 °C by hot-filament chemical vapor deposition (HFCVD). The results revealed that the obtained a-C films were all graphitelike carbon films. Structural transition of the deposited films from a-C to nanocrystalline graphene was achieved by raising the hydrogen dilution ratios from 10 to over 80%. On the basis of systematic structural and chemical characterizations, a schematic process with three steps including sp2 chain aggregation, aromatic ring formation, and sp3 bond etching was proposed to interpret the structural evolution. The nanocrystalline graphene films grown on glass by HFCVD exhibited good electrical performance with a carrier mobility of 36.76 cm2/(V s) and a resistivity of 5.24 × 10-3 Ω cm over an area of 1 cm2. Temperature-dependent electrical characterizations revealed that the electronic transport in carbon films was dominated by defect, localized, and extended states, respectively, when increasing the temperature from 75 to 292 K. The nanocrystalline graphene films presented higher carrier mobility and lower carrier concentration than those of a-C films, which was mainly attributed to their smaller conductive activation energy. The present investigation provides an effective way for direct growth of graphene films on glass at reduced temperatures and also offers useful insights into the understanding of structural and electrical relationship between a-C and graphene.
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This paper analyses the three-dimensional (3-D) surface texture of growing diamond nanocrystals on Au thin films as catalyst on p-type Si substrate using hot filament chemical vapour deposition (HFCVD). Rutherford backscattering spectrometry (RBS), atomic force microscopy (AFM), Raman, X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses were applied also to characterize the 3-D surface texture data in connection with the statistical, and fractal analyses. This type of 3-D morphology allows a deeper understanding of structure/property relationships and surface defects in prepared samples. Our results indicate a promising way for preparing high-quality diamond nanocrystals on Au thin films as catalyst on p-type Si substrate via HFCVD method.
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Single nanocrystalline tungsten carbide (WC) was first synthesized on the tips of vertically aligned carbon nanotubes (VA-CNTs) with a hot filament chemical vapor deposition (HF-CVD) method through the directly reaction of tungsten metal with carbon source. The VA-CNTs with preservation of vertical structure integrity and alignment play an important role to support the nanocrystalline WC growth. With the high crystallinity, small size, and uniform distribution of WC particles on the carbon support, the formed WC-CNTs material exhibited an excellent catalytic activity for hydrogen evolution reaction (HER), giving a η10 (the overpotential for driving a current of 10 mA cm(-2)) of 145 mV, onset potential of 15 mV, exchange current density@ 300 mV of 117.6 mV and Tafel slope values of 72 mV dec(-1) in acid solution, and η10 of 137 mV, onset potential of 16 mV, exchange current density@ 300 mV of 33.1 mV and Tafel slope values of 106 mV dec(-1) in alkaline media, respectively. Electrochemical stability test further confirms the long-term operation of the catalyst in both acidic and alkaline media.
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Diamond coating of suitable template materials and subsequent delamination allows for the manufacturing of free-standing diamond foil. The evolution of the microstructure can be influenced by secondary nucleation via control of process conditions in the hot-filament chemical vapour deposition process. Bending tests show extraordinarily high strength (more than 8 GPa), especially for diamond foils with nanocrystalline structure. A detailed fractographic analysis is conducted in order to correlate measured strength values with crack-initiating defects. The size of the failure causing flaw can vary from tens of micrometres to tens of nanometres, depending on the diamond foil microstructure as well as the loading conditions.