Nanocrystalline SiC films prepared by direct deposition of carbon and silicon ions

The method of direct deposition of carbon and silicon ions was used for preparation of nanocrystalline silicon carbide films. The deposition energy of carbon and silicon ions was 90 eV. The effect of substrate temperature in the range of 500-1150 °C on the structure of SiC films was studied by means of X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD). According to XPS data, the films contained heterobonded Si-C atoms and homobonded Si-Si and C-C atoms, the relation between which varied as the function of substrate temperature. The data of XRD showed a noticeable growth of a nanocrystalline phase of cubic silicon carbide in the films at a temperature of about 700 °C. The content of 3C-SiC nanocrystalline phase reached 80 at.% at 950 °C. There was an established change from cubic polytype to rhombohedral polytype of silicon carbide α-SiC-21R at a substrate temperature higher than 1000 °C. The size of SiC crystal grains depended on the substrate temperature and changed from 4-5 up to 8-10 nm over the range of 700-950 °C. Besides, silicon unbonded with carbon also crystallized in nanocrystalline form with similar sizes of crystal grains. A possible model of the change of the polytypic composition of SiC film under the conditions of direct ion deposition was discussed.     

Electrical properties/Doping efficiency of doped microcrystalline silicon layers prepared by hot-wire chemical vapor deposition

Microcrystalline silicon (μc-Si) doped films were prepared by hot-wire chemical vapor deposition (HWCVD) to investigate the doping efficiency. The incorporation probability of different dopant atoms into the solid-phase is always increasing with the doping gas concentrations, but very different for the doping gases used: trimethylboron (TMB), boron trifluoride (BF₃) and phosphine (PH₃). At the same doping gas concentration in the process gas the incorporation of phosphorus atoms into the solid μc-Si phase is much larger than that of boron atoms with respect to the dissociation probability of the doping gases. The electron and hole concentrations, estimated from Hall measurements, are directly related to the solid phase concentration of the doping atoms and independent of the type of dopant and the doping gas used. This results in an equal doping efficiency of about 20 % for the incorporated B and P atoms in doped HWCVD μc-Si films. For the dopant atom concentration regime investigated the doping efficiency of B atoms is in good agreement with corresponding PECVD doping efficiencies however, the doping efficiency of P atoms is considerably lower for our n-doped films.     

Characteristics of a well-adherent nanocrystalline diamond thin film grown on titanium in Ar/CH4 microwave CVD plasma

The fabrication of a well-adherent diamond film on titanium and its alloys is always problematical due to the different thermal expansion coefficients of the two materials, the complex nature of the interlayer formed during diamond deposition, and the difficulty in achieving very high nucleation density. In this work, well-adherent and smooth nanocrystalline diamond (NCD) thin film is successfully deposited on pure titanium substrate by microwave plasma-assisted chemical vapor deposition (MWPCVD) method in Ar/CH₄ environment. It is found that the average grain size is less than 20 nm with a surface roughness value as low as 12 nm. Morphology, surface roughness, diamond crystal orientation and quality are obtained by characterizing the sample with field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), X-ray diffraction (XRD) and Raman spectroscopy, respectively. Detailed experimental results and mechanisms for NCD film deposition are discussed.     

Simultaneous fabrication of nanocrystalline and {100} textured large-grained diamond films

In this work, we report the simultaneous synthesis of both nanocrystalline and {100} textured large-grained diamond films in one deposition run performed in a 5-kW microwave plasma chemical vapor deposition (MPCVD) reactor. This was achieved by employing the coupled effect of nitrogen addition in the gas phase and substrate temperature on the growth of diamond films. In one deposition run, different substrate surface temperatures were obtained by a novel substrate arrangement, nanocrystalline diamond of high growth rate around 3 μm/h was formed at low temperature, while {100} textured large-grained diamond of much higher growth rate about 11 μm/h was grown at high temperature. This new method opens way for mechanical and tribological applications of both nano-diamond and {100} textured diamond in industrial level. This result indicates that distinct growth modes or growth mechanisms were involved at different substrate temperatures with a certain amount of nitrogen addition. The coupled effect of nitrogen addition and temperature on the growth of CVD diamond films and the involved growth mechanism is briefly discussed from the point of view of gas phase chemistry and surface reactions.     

Solid-state synthesis of tungsten carbide from tungsten oxide and carbon, and its catalysis by nickel

Tungsten carbide has been produced by heating a mixture of tungsten oxide and carbon powder at 1300 °C for 2 h. Further batches were made with additional KCl, KCl + Ni, or KCl + Fe. The products were compared by XRD and SEM. A mixture of WC and W₂C was produced from the plain WO₃/carbon reaction, but adding 1 wt.% nickel assisted the formation of a pure WC phase. Both Ni and Fe assisted the growth of larger WC crystals.     

Synthesis and Characterization of Fine Grained High Density La_2Mo_2O_9-based Oxide-ion Conductors

A cost-efFective technique, including nanocrystalline powder preparation using a modified Pechini method and a two-step low-temperature sintering route, was developed for the synthesis of high performance La2Mo2O9- based oxide-ion conductors. The optimum parameters of the compaction pressure, the first step and ＇the second step sintering temperatures for the synthesis of fine grained, high density and uniform La2Mo2O9- based oxide-ion conductors were determined by a series of sintering experiments. High density and uniform sintered La2Mo2O9 samples with average grain size from 0.8 to 5 μm and La1.96K0.04Mo2O8.96 sample with average grain size as small as 500 nm were synthesized by using this cost-efFective method. The impedance measurement results show that the as-fabricated La2Mo2O9-based ceramics possess much higher ionic conductivity than that obtained by solid state reaction method. It is found that in the range of 0.8-5μm the grain size of dense La2Mo2O9 samples prepared from the nanocrystalline powders has little influence on their conductivities.     

Synthesis, Characterization and Electromagnetic Studies on Nanocrystalline Nickel Zinc Ferrite by Polyacrylamide Gel

Nanocrystalline nickel zinc ferrite powders （Ni=Zn1-xFe2O4, A for x=0, B for x=0.2, C for x=0.5, D for x= 0.8 and E for x= 1） were synthesized by polyacrylamide gel method. X-ray diffraction （XRD）, transmission electron microscopy （TEM） and wave-guide were used to characterize the composition. The XRD results show that the dried gel powders are amorphous, and the characteristic peaks of the spinel Ni0.5Zn0.5Fe2O4 appear after the gel is calcined at 400℃ for 1 h. When the calcining temperatures are 600 and 800℃, the average grain sizes are identified by TEM to be 10 and 30 nm, respectively. The NixZn1-xFe2O4 powders have both dielectric loss and magnetic loss in the frequency range of 8.2-11.0GHz. With the increase of Ni^2＋ ions content, the dielectric parameters （ε′） and permeability （u′） of the NixZn1-xFe2O4 powders decrease while the dielectric loss （ε″）, magnetic loss （u″） and the reflection loss increase.     

Fretting wear behavior of nanocrystalline surface layer of copper under dry condition

Unlubricated fretting tests were performed with a nanocrystalline surface layer of a 99.99 wt.% copper fabricated by means of surface mechanical attrition treatment (SMAT), in comparison with a coarse-grained (CG) copper. The measured friction and wear data show that the fretting wear resistance is markedly enhanced with the nanocrystalline surface layer relative to the CG counterpart. The friction coefficient and wear volume of the SMAT Cu are lower than that of the CG Cu. For both samples, the friction coefficients and wear volumes increase with an increasing applied load and fretting frequency. A rapid increase of the friction coefficient and wear volume under an applied load above a critical value (30 N for the SMAT Cu and 20 N for the CG Cu) is noticed, corresponding to the formation of a continuous oxide layer between two contact surfaces. Also two sharp increases of the friction coefficient and wear volume at fretting frequencies of 50 Hz and 175 Hz were observed for the SMAT and the CG Cu. The former is correlated with the formation of a continuous oxide layer, while the latter corresponds to wearing away of the oxide layer.     

Controlling the growth of nanocrystalline silicon by tuning negative substrate bias

Application of appropriate dc bias to the substrate has been identified as one of the efficient parameters, beyond the mostly used classical ones, in controlling the growth of nanocrystalline silicon (nC-Si:H) network by plasma CVD of SiH₄. The present communication demonstrates that applying negative dc substrate bias at the moderate level the overall nanocrystallinity in the material be enhanced significantly. The nC-Si:H film of ∼70% crystalline volume fraction along with a high σ_D∼3.1×10^-4 S cm^-1 and E_σ∼191 meV has been obtained at a low substrate temperature of 200 °C and with a growth rate of ∼8 nm/min from only 1 sccm of the feed gas SiH₄, using −75 V dc substrate bias and He as the diluent to the plasma. Besides the extent of crystallinity, the average grain size (ρ) has been demonstrated to be controllable within nano-dimensions, 1< ρ<10 nm, by tuning negative dc substrate bias during plasma processing. The present report comprehensively elaborates the effect of applied negative dc substrate bias on the growth morphology of the nC-Si:H thin films from He-diluted SiH₄ plasma, in view of controlling nanocrystallization at low substrate temperature by RF-PCVD, while controlled transmission of energy to the growing surface obtained from metastable and ionic helium (He* and He⁺) bombardment has been deemed instrumental.     

Electrochemical synthesis of nanocrystalline SrNb2O6 powders and characterization of their photocatalytic property

Nanocrystalline SrNb₂O₆ powders were successfully prepared by a simple electrochemical method for the first time, and the influences of electrolytic solution ingredients, electrolyte concentration, and applied electric current intensity on electrochemical process and products were systemically studied. It was found that the formation of strontium niobates strongly relied on the basic or acidic condition of electrolytic solution. When Sr(OH)₂·8H₂O or mixed Sr(OH)₂·8H₂O with SrCl₂·6H₂O was used as electrolyte, Sr₅Nb₄O₁₅ and SrNb₂O₆ phases could simultaneously form, and the relative ratio of Sr₅Nb₄O₁₅ phase to SrNb₂O₆ declined with the increase of SrCl₂·6H₂O content in electrolytic solution. The higher the basicity of electrolytic solution, the more favored the crystallization and development of Sr₅Nb₄O₁₅ phase. Only monoclinic phase SrNb₂O₆ was obtained in neutral SrCl₂·6H₂O solution or acidic solution of SrCl₂·6H₂O with adding hydrochloric acid solution, and a lower concentration of SrCl₂·6H₂O (≤0.50 M) was beneficial to the formation of SrNb₂O₆ phase and stable anodic sparks could be observed. Moreover, the crystallization and development of the nanocrystalline SrNb₂O₆ powders seem to be not sensitive to the applied electric current intensity, their similar particle size and morphology ultimately result in the resemblance in UV-vis absorption and photodegradation. They show a slight red shift of light absorption onset and better photocatalytic performance compared with that prepared by the solid-state reaction.