Effect of process parameters on induction plasma reactive deposition of tungsten carbide from tungsten metal powder

Tungsten carbide deposit was made directly from tungsten metal powder through the reaction with methane in radio frequency induction plasma. Effect of major process parameters on the induction plasma reactive deposition of tungsten carbide was studied by optical microscopy, scanning electron microscopy, X ray diffraction analysis, water displacement method, and microhardness test. The results show that methane flow rate, powder feed rate, particle size, reaction chamber pressure and deposition distance have significant influences on the phase composition, density, and microhardness of the deposit. Extra carbon is necessary to ensure the complete conversion of tungsten metal into the carbide.

Development of Nanopowder Synthesis Using Induction Plasma

The application of induction plasma technology developed for the synthesis of nano- metric powders is summarized. A brief description of the scientific basis for the induction plasma processes is given, followed by the presentation of an induction plasma system developed by Tekna, together with various examples of the nanopowders synthesized using its facilities. The advantages of the induction plasma process over alternative techniques and its adaptability into industrial- scale operation is particularly illustrated. Some specific issues related to the nanopowder synthesis process are also discussed.

Radio Frequency Induction Plasma Spraying of Molybdenum

Radio frequency (RF) induction plasma was used to make free-standing deposition of molybdenum (Mo). The phenomena of particle melting, flattening, and stacking were investigated. The effect of process parameters such as plasma power, chamber pressure, and spray distance on the phenomena mentioned above was studied. Scanning electron microscopy (SEM) was used to analyze the plasma-processed powder, splats formed, and deposits obtained. Experimental results show that less Mo particles are spheroidized when compared to the number of spheroidized tungsten (W) particles at the same powder feed rate under the same plasma spray condition. Molten Mo particles can be sufficiently flattened on substrate. The influence of the process parameters on the flattening behavior is not significant. Mo deposit is not as dense as W deposit, due to the splash and low impact of molten Mo particles. Oxidation of the Mo powder with a large particle size is not evident under the low pressure plasma spray.

Preparation of novel Ni-Ir/γ-Al_2O_3 catalyst via high-frequency cold plasma direct reduction process

The novel Ni-Ir/γ-Al2O3 catalyst, denoted as NIA-P, was prepared by high-frequency cold plasma direct reduction method under ambient conditions without thermal treatment, and the conventional sample, denoted as NIA-CR, was prepared by impregnation, thermal calcination, and then by H2 reduction method. The effects of reduction methods on the catalysts for ammonia decomposition were studied, and they were characterized by XRD, N2 adsorption, XPS, and H2-TPD. It was found that the plasma-reduced NIA-P sample showed a better catalytic performance, over which ammonia conversion was 68.9%, at T = 450℃, P = 1 atm, and GHSV = 30, 000 h^-1. It was 31.7% higher than that of the conventional NIA-CR sample. XRD results showed that the crystallite size decreased for the sample with plasma reduction, and the dispersion of active components was improved. There were more active components on the surface of the NIA-P sample from the XPS results. This effect resulted in the higher activity for decomposition of ammonia. Meanwhile, the plasma process significantly decreased the time of preparing catalyst.

Ni/MgO catalyst prepared using atmospheric high-frequency discharge plasma for CO_2 reforming of methane

A new type of Ni/MgO catalyst was prepared using atmospheric high-frequency discharge cold plasma. The influences of conventional method, plasma method, and plasma plus calcination method on the catalytic activity were studied and the CO2 reforming of methane was chosen as the probe reaction. The catalysts were characterized by X-ray diffraction （XRD）, transmission electron microscope （TEM）, X-ray photoelectron spectroscopy, and CO2 temperature-programmed surface reaction techniques. The results suggested that the nickel-based catalyst prepared by plasma plus calcination method possessed a smaller particle size and a higher dispersion of active component, better low-temperature activity and enhanced anti-coking ability. The conversion of CO2 and CH4 was 90.70% and 89.37%, respectively, and the reaction lasted for 36 h without obvious deactivation under 101.325 kPa and 750°C with CO2/CH4 = 1/1.

Fluid simulation of the effect of a dielectric window with high temperature on plasma parameters in inductively coupled plasma

To maintain the high-density plasma source in inductively coupled plasma(ICP),very high radiofrequency power is often delivered to the antenna,which can heat the dielectric windows near the antenna to high temperature.This high temperature can modulate the plasma characteristics to a large degree.We thus study the effect of dielectric window temperature on plasma parameters in two different ICP structures based on COMSOL software.The distributions of various plasma species are examined at different dielectric window temperatures.The concentration of neutral gas is found to be largely modulated at high dielectric window temperature,which further affects the electron collision probability with neutrals and the electron temperature.However,the electron density profiles are barely affected by the dielectric window temperature,which is mainly concentrated at the center of the reactor due to the fixed power input and pressure.

A fast hybrid simulation approach of ion energy and angular distributions in biased inductively coupled Ar plasmas

In this work,a two-dimensional hybrid model,which consists of a bulk fluid module,a sheath module and an ion Monte-Carlo module,is developed to investigate the modulation of ion energy and angular distributions at different radial positions in a biased argon inductively coupled plasma.The results indicate that when the bias voltage amplitude increases or the bias frequency decreases,the ion energy peak separation width becomes wider.Besides,the widths of the ion energy peaks at the edge of the substrate are smaller than those at the center due to the lower plasma density there,indicating the nonuniformity of the ion energy distribution function(IEDF)along the radial direction.As the pressure increases from 1 to 10 Pa,the discrepancy of the IEDFs at different radial positions becomes more obvious,i.e.the IEDF at the radial edge is characterized by multiple low energy peaks.When a dual frequency bias source is applied,the IEDF exhibits three or four peaks,and it could be modulated efficiently by the relative phase between the two bias frequencies.The results obtained in this work could help to improve the radial uniformity of the IEDF and thus the etching process.

Induction plasma spheroidization of tungsten and molybdenum powders

The melting, evaporation and oxidation behaviors as well as the solidification phenomena of tungsten and molybdenum in induction plasma were studied. Scanning electron microscopy was used to examine the morphology and the cross section of plasma-processed powders. X-ray diffraction was used to analyze the oxides formed on the particle surface of these two metals. The influence of spray chamber pressure on the spheroidization and oxidation phenomena was discussed. The results show that fewer Mo particles than W particles are spheroidized at the same powder feed rate under the same plasma spray condition although molybdenum has a lower melting point. A small fraction of tungsten is evaporized and condensed either on the surface of tungsten particles nearby or on the wall of spray chamber. Tungsten oxides were found in tungsten powder processed under soft vacuum condition. Extremely large grains form inside some spheroidized particles of tungsten powder.

Synthesis of titanium carbide by induction plasma reactive spray

A novel method capable of sufficient mixing of titanium powder and methane of carbon source was developed in the synthesis of titanium carbide by induction plasma reactive spray. X ray diffraction analysis, optical microscopy, scanning electron microscopy, and microhardness test were used to characterize the spray formed deposit. The experimental results show that both primary carburization of the titanium particles inside the plasma flame and secondary carburization of the growing deposit on high temperature substrate contribute to the forming of titanium carbide. The transitional phase of TiC 1- x has the same crystal structure as TiC, but has a slightly low lattice constant. The deposit consists of fine grain structure and large grain structure. The fine grain structure, harder than large grain structure, shows grain boundary fracture.

Numerical and Experimental Investigation on the In-Flight Melting Behaviour of Granulated Powders in Induction Thermal Plasmas

An innovative in-flight glass melting technology with thermal plasmas was developed for the purpose of energy conservation and environment protection. In this study, modelling and experiments of argon-oxygen induction thermal plasmas were conducted to investigate the melting behaviour of granulated soda-lime glass powders injected into the plasma. A two-dimensional local thermodynamic equilibrium （LTE） model was performed to simulate the heat and momentum transfer between plasma and particle. Results showed that the particle temperature was strongly affected by the flow rate of carrier gas and the particle size of raw material. A higher flow rate of carrier gas led to lower particle temperature and less energy transferred to particles which resulted in lower vitrification. The incomplete melting of large particles was attributed to the lower central temperature of the particle caused by a larger heat capacity. The numerical analysis explained well the experimental results, which can provide valuable practical guidelines for the process control in the melting process for the glass industry.

Quantification of trace amounts of impurities in high purity cobalt by high resolution inductively coupled plasma mass spectrometry

A An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of 24 elements （Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb） in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.

Experimental Study of the Influence of Process Pressure and Gas Composition on GaAs Etching Characteristics in Cl_2/BCl_3-Based Inductively Coupled Plasma

A study of Cl2/BCl3-based inductively coupled plasma （ICP） was conducted using thick photoresist mask for anisotropic etching of 50μm diameter holes in a GaAs wafer at a relatively high average etching rate for etching depths of more than 150μm. Plasma etch characteristics with ICP process pressure and the percentage of BCI3 were studied in greater detail at a constant ICP coil/bias power. The measured peak-to-peak voltage as a function of pressure was used to estimate the minimum energy of the ions bombarding the substrate. The process pressure was found to have a substantial influence on the energy of heavy ions. Various ion species in plasma showed minimum energy variation from 1.85 eV to 7.5 eV in the pressure range of 20 mTorr to 50 mTorr. The effect of pressure and the percentage of BCl3 on the etching rate and surface smoothness of the bottom surface of the etched hole were studied for a fixed total flow rate. The etching rate was found to decrease with the percentage of BCl3, whereas the addition of BCl3 resulted in anisotropic holes with a smooth veil free bottom surface at a pressure of 30 mTorr and 42% BC13. In addition, variation of the etching yield with pressure and etching depth were also investigated.

Microstructure, Hardness and Corrosion Resistance of ZrN Films Prepared by Inductively Coupled Plasma Enhanced RF Magnetron Sputtering

ZrN fihns were deposited on Si（111） and M2 steel by inductively coupled plasma （ICP）-enhanced RF magnetron sputtering. The effect of ICP power on the microstructure, mechanical properties and corrosion resistance of ZrN films was investigated. When the ICP power is below 300 W, the ZrN films show a columnar structure. With the increase of ICP power, the texture coefficient （To） of the （111） plane, the nanohardness and elastic modulus of the films increase and reach the maximum at a power of 300 W. As the ICP Power exceeds 300 W, the films exhibit a ZrN and ZrNx mixed crystal structure without columnar grain while the nanohardness and elastic modulus of the films decrease. All the ZrN coated samples show a higher corrosion resistance than that of the bare M2 steel substrate in 3.5% NaCl electrolyte. The nanohardness and elastic modulus mostly depend on the crystalline structure and Tc of ZrN（111）.

Ion Density Distribution in an Inductively Coupled Plasma Chamber

The ion density distribution in the reaction chamber was diagnosed by a Langmuir probe. The rules of the ion density distribution were obtained under the pressures of 9 Pa, 13 Pa, 27 Pa and 53 Pa in the reaction chamber, different radio-frequency powers and different positions. The result indicates that the ion density decreases as the pressure increases, and increases as the power decreases. The ion density of axial position z =0 achieves 5.8×1010 on the center of coil under the power of 200 w and pressure of 9 Pa in the reaction chamber.

Modeling Approach and Analysis of the Structural Parameters of an Inductively Coupled Plasma Etcher Based on a Regression Orthogonal Design

The geometry of an inductively coupled plasma （ICP） etcher is usually considered to be an important factor for determining both plasma and process uniformity over a large wafer. During the past few decades, these parameters were determined by the ＂trial and error＂ method, resulting in wastes of time and funds. In this paper, a new approach of regression orthogonal design with plasma simulation experiments is proposed to investigate the sensitivity of the structural parameters on the uniformity of plasma characteristics. The tool for simulating plasma is CFD-ACE＋, which is commercial multi-physical modeling software that has been proven to be accurate for plasma simulation. The simulated experimental results are analyzed to get a regression equation on three structural parameters. Through this equation, engineers can compute the uniformity of the electron number density rapidly without modeling by CFD-ACE＋. An optimization performed at the end produces good results.

Surface Modification of Nanometre Silicon Carbide Powder with Polystyrene by Inductively Coupled Plasma

An investigation was made into polystyrene （PS） grafted onto nanometre silicon carbide （SIC） particles. In our experiment, the grafting polymerization reaction was induced by a radio frequency （RF） inductively coupled plasma （ICP） treatment of the nanometre powder. FTIR （Fourier transform infrared spectrum） and XPS （X-ray photoelectron spectroscopy） results reveal that PS is grafted onto the surface of silicon carbide powder. An analysis is presented on the effectiveness of this approach as a function of plasma operating variables including the plasma treating power, treating time, and grafting reaction temperature and time.

The determination of 52 elements in marine geological samples by an inductively coupled plasma optical emission spectrometry and an inductively coupled plasma mass spectrometry with a high-pressure closed digestion method

An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is studied by an inductively coupled plasma optical emission spectrometry（ICP-OES） and an inductively coupled plasma mass spectrometry（ICP-MS）. The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error（RE） for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials（GBW07309, GBW07311, GBW07313）, rock reference materials（GBW07103, GBW07104,GBW07105）, and cobalt-rich crust reference materials（GBW07337, GBW07338, GBW07339）, the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation（RSD） and the relative error（RE） are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.

Frequency dependence of plasma characteristics at different pressures in cylindrical inductively coupled plasma source

The effects of driving frequency on plasma parameters and electron heating efficiency are studied in cylindrical inductively coupled plasma(ICP) source. Measurements are made in an Ar discharge for driving frequency at 13.56/2 MHz, and pressures of 0.4-1.2 Pa. In 13.56 MHz discharge, higher electron density(n_e) and higher electron temperature(T_e) are observed in comparison with 2 MHz discharge at 0.6-1.2 Pa. However, slightly higher n_e and T_e are observed in 2 MHz discharge at 0.4 Pa. This observation is explained by enhanced electron heating efficiency due to the resonance between the oscillation of 2 MHz electromagnetic field and electron-neutral collision process at 0.4 Pa. It is also found that the variation of T_edistribution is different in 13.56 and 2 MHz discharge.For ICP at 13.56 MHz, T_eshows an edge-high profile at 0.4-1.2 Pa. For 2 MHz discharge, T_e remains an edge-high distribution at 0.4-0.8 Pa. However, the distribution pattern involves into a center-high profile at 0.9-1.2 Pa. The spatial profiles of n_e remain a center-high shape in both 13.56 and 2 MHz discharges, which indicates the nonlocal kinetics at low pressures. Better uniformity could be achieved by using 2 MHz discharge. The effects of gas pressure on plasma parameters are also examined. An increase in gas pressure necessitates the rise of n_e in both 13.56 and 2 MHz discharges. Meanwhile, T_e drops when gas pressure increases and shows a flatter distribution at higher pressure.