Process monitoring and control methods during direct metal deposition (DMD) are used to ensure a consistent manufacturing quality of the process. In the optical regime, naturally occurring process emission provides therefore selective and specific element lines, which can be obtained by optical spectrometers. However, DMD processes are in the heat conduction regime and superimposed broad spectral emissions dominate the wavelength specific signals. The aim of this work is to investigate the occurrence of different elemental lines in DMD processes as well as deposition track cross-sectional dimensions. Therefore, experiments were simultaneously conducted by using a high-resolution spectrometer (resolution = approx. 47 pm FWHM at 522 nm and 55 pm FWHM at 407.5 nm) and a medium resolution spectrometer (resolution = 0.73 nm FWHM), which were coupled by a bifurcated optical fibre. A parameter study of 27 single track DMD experiments using Co-Cr-based (MetcoClad21) powder on low-alloyed tool steel C45W (1.1730) substrate material, varying laser power, scan velocity and powder feed rate was conducted. Series of spectra were obtained for all sets of parameters with a scan rate of 100 Hz. The individual wavelength spectrum was analysed and classified by an algorithm into two types. Type-A spectra, with specific element emission lines and Type-B spectra, without significant emission lines with mostly predominant thermal emission radiation. Each deposition track was coupled to cross-sectional dimensions, including height, welding depth and melted areas. In addition, certain elemental lines contained in Type-A spectra were verified by using data from the NIST atomic spectra database. The investigation indicates that the relative number of Type-A spectra with respect to the total quantity of spectra, correlates significant to the process parameters. All detected and identified element lines occurred to be non-ionised elements, especially Cr I, Fe I and Mn I lines were frequently observed.

In plasma spraying, hydrogen is widely used as a secondary working gas. Under low-pressure conditions, even small amounts of hydrogen can have a significant effect on the plasma jet as mechanisms such as diffusion and recombination come into play. This study investigates the influence of Ar-H 2 mixtures on electron densities, temperature distributions, and local composition in the plasma jet using optical emission spectroscopy. Several mechanisms reported in the literature are consulted to explain the observed phenomena.

In this study, pure rutile TiO 2 coatings are deposited on stainless steel substrates by very low-pressure plasma spraying (VLPPS). The spraying system was used in the reactive mode, injecting both titanium powder and oxygen gas to achieve nanosize particles. Optical emission spectroscopy showed that the interaction between Ti particles and O 2 occurred in flight. Coating microstructure and phase composition were characterized at the surface and in the bulk with respect to operating parameters. Coating surfaces show typical cauliflower microstructure with many nanoparticles, while the microstructure below was found to change from binary to columnar as spraying distance increases.

In this work, optical emission spectroscopy is used to study plasma-liquid precursor interactions in a plasma spray process. A mapping of the plasma jet is performed with a bundle of seven optical fibers while injecting various liquid precursors. Two suspensions containing a titania (TiO 2 ) powder in different solvents and one solution containing titanium butoxide are analyzed. For each precursor, the evolution of both temperature and spectral line intensities along the plasma jet are observed. Comparing these results brings a new understanding of the precursor decomposition inside the plasma, while the noted contrasts between water and ethanol as solvent, and between the use of a powder and that of an alkoxide as a source of titanium, help to assess the effect of these parameters on the plasma spray process.

In the Plasma Spray-Physical Vapor Deposition (PS-PVD) process, the vapor atom of feedstock material is one deposition unit of the columnar structure coating. It is reported that the gas phase may be transformed into cluster when the powder feeding rate increases from small to large or the sedimentation distance increases from a certain distance to another distance. In order to understanding the variation of vaporized coating material in free plasma jet, the gaseous material capacity of plasma jet must be fundamentally understood. In this work, the thermal characteristics of plasma were firstly measured by optical emission spectrometry (OES). The results show that the free plasma jet is in the local thermal equilibrium due to a typical electron number density from 2.1×1015 to 3.1×1015 cm -3 . In this condition, the temperature of gaseous zirconia can be equal to the plasma temperature. A model was developed to obtain the vapor pressure of gaseous ZrO 2 molecules as a two dimensional map of jet axis and radial position corresponding to different average plasma temperatures. The overall gaseous material capacity of free plasma jet was further established. At a position of plasma jet, clusters may form when the gaseous material exceeds local maximum gaseous material capacity.

The measurement of the spatial distribution of coating thickness of thin coatings applied by thermal spraying can be challenging. For non-magnetic metallic substrates and coatings, X-Ray Fluorescence (XRF) was employed for measuring coating thicknesses in the range of 15 to 60 μm. XRF is used to measure the ratio of atomic fluorescence peaks for an element in the substrate to an element in the coating. With appropriate calibration, the ratio of peak intensities gives the coating thickness for the spot sampled. Mass gain and cross sectional metallography are compared to XRF to determine accuracies and sensitivities of the techniques for plasma sprayed coatings.

Very low pressure plasma spraying (VLPPS) is an emerging process allowing manufacturing oxide and metallic coatings by condensation of vapors generated by feedstock powder vaporization. This process operates at unusually low pressures, typically between 100 and 1000 Pa. This paper aims at presenting recent developments for manufacturing TixAlyN coatings via a reactive mode. At first, nitrogen was used as the primary plasma forming gas to enrich spraying surrounding with nitriding species. Plasma jet mass enthalpy and substrate surface temperature were varied to evidence nitride phase formation during spraying. Then, a secondary nitrogen injection was implemented and located close to the surface to be covered in view of creating a continuous nitrogen supply to promote the nitriding mechanisms on the surface. SEM, XRD, GDOES and NHT were implemented to characterize coatings structure. This study highlights the nitrides formation versus spray operating conditions. The microstructural and mechanical features as well as the chemical composition are presented.

In this paper, the development of surface oxide scale and the evolvement of spallation mechanism of Fe-21Cr-5.6Al super alloy were investigated at 1200°C and 1300°C. The oxidation kinetic curves were obtained by isothermally measuring the weight gain of alloy oxidized with various time durations. The morphologies of oxide scale and grain structures were observed by SEM/EDX, and the phase structure was analyzed by XRD. The results show that the oxidation processes follow the parabolic law and the oxidation rate is higher at 1300°C than 1200°C. Though the FeCrAl alloy shows capabilities against oxidation even at a high temperature of 1300°C, the oxidation behavior and mechanism are distinct from those at moderate temperatures (<1000°C). Different morphologies and phase structure were found in oxide scales generated at different temperatures within the same time duration. Typical buckling was observed in the super alloy when it was subjected to 1200°C. Equiaixed grains with multiple voids were found near the alloy surface. At 1300°C, a flat and thicker oxide layer was formed. The grains were stretched vertically against the alloy and presented as coarse and compact near the interface. The vertically stretching of grain was triggered by fast element transportation inside the alloy. The differences in grain morphologies among the different test temperatures demonstrated that although the super alloy followed parabolic law at both test temperatures, the oxidation processes were different due to the evolvement of grain morphologies and oxide scale structures caused by exposure to high temperature.

Plasma spraying at very low pressure (50-200 Pa) is significantly different from atmospheric plasma conditions (APS). Applying powder feedstock it is possible to defragment the particles into very small clusters or even to evaporate the material. As a consequence, the deposition mechanisms and the resulting coating microstructures could be quite different compared to conventional APS liquid splat deposition. Thin and dense ceramic coatings as well as columnar-structured strain-tolerant coatings with low thermal conductivity can be achieved offering new possibilities for application in energy systems. To exploit the potential of such a gas phase deposition from plasma spray-based processes, the deposition mechanisms and their dependency on process conditions must be better understood. Thus, plasma conditions were investigated by optical emission spectroscopy. Coating experiments were performed, partially at extreme conditions. Based on the observed microstructures, a phenomenological model is developed to identify basic growth mechanisms.

This paper discusses the development of Fe-Cr-C-B powder feedstocks for the production of wear-resistant coatings by HVOF spraying. Chromium content in the powder is in the range of 30 wt% and carbon content is about 5 wt%, yielding a unique powder structure that results in coatings with high and well distributed carbide content. Powder and coating microstructure are examined and the results of wear tests are presented. The extent to which the powders can substitute for conventional carbide coatings is discussed as well.

A consistent thermal and chemical non-equilibrium model for inductive supersonic plasma flow, developed recently, is applied to the modelling of pure argon supersonic plasma flow, which impinges on a substrate below the Mach 1 nozzle. The model considers the ionization of argon atom and the corresponding recombination but the second order ionization is ignored and plasma charge neutrality is assumed. The transport and mass diffusion coefficients are computed using the collision cross-section data, published by Devoto and Murphy and the computations of transport properties are fully coupled with the calculation of the plasma flow fields. The model treats the subsonic discharge region above the supersonic nozzle and the supersonic region below the nozzle together. Two different turbulent models are incorporated into the model to describe the supersonic plasma flow. The modeled radial and axial profiles of electron and heavy species temperatures and electron number densities near the substrate are then compared to those measured by the method of optical emission spectroscopy and finally the most realistic model is identified.

Low pressure plasma spraying (LPPS) and LPPS-Thin Film (LPPS-TF) processes cover a broad operational pressure range from typically 200 mbar down to a few millibars, filling the gap between conventional thermal spray processes, where coatings are made from the liquid phase, and conventional thin film technologies such as PVD or CVD, where coatings are produced from precursors species in the vapor phase. Using some specific parameters of the LPPS-TF process, the injected material can be partially or even completely in gaseous phase, disqualifying diagnostics based on the detection of solid or liquid particles such as the DPV-2000 (Tecnar, St-Bruno, QC, CA). In this case, other optical diagnostic tools have to be used, such as optical emission spectroscopy (OES) to characterize the LPPS-TF process. In this paper, a qualitative study of the properties of the injected material in the plasma jet using DPV-2000 and optical emission spectroscopy is presented by varying specific plasma parameters. Moreover, in some particular cases, it is shown that the combination of DPV measurements and OES can help to monitor the coating process and to improve the basic understanding of the LPPSTF technology.

Characteristics of in flight particles before they impact on the substrate influence strongly the quality of coating obtained by plasma spraying. Various optical techniques can be used to measure the in-flight particle characteristics; some of these techniques require the use of high- speed two-color pyrometers to collect the light emitted by the particle during the in-flight period when they pass through the measurement volume. However, the intense radiation coming from the plasma can affect the particle thermal radiation and lead to erroneous measurements. This work was dedicated to the study of reflected light coming from the plasma and scattered by the injected particles. To achieve this goal, sprayed particles were analyzed by optical emission spectrometry. The light scattered by the particles was found to influence significantly the measured temperature. This work allows thus the estimation of the accuracy of temperature measurements on particle surface for the thermal spraying process. Abstract only; no full-text paper available.

In the thermal spraying of powder materials, it has been observed in practice that the splat shape changes to a disk type from a splash type with increases in the substrate temperature. However, the details of the substrate surface change due to the heating has not been fully characterized. In this study, an AISI 304 stainless steel substrate surface heated to 673K was analyzed precisely by atomic force microscope (AFM), X-ray photoelectron spectroscopy (XPS), and Auger electron spectroscopy. The results obtained revealed that the change of the substrate surface occurred not in the chemical composition but mainly in the surface roughness, especially surface morphology in nano-meter scale. Hence, substrate heating may bring about the change in substrate surface and this change induces the transition phenomenon.

The aim of the present study concerns the effect of the chamber pressure on the structure of a plasma jet. Conventional vacuum plasma spray equipments are currently designed to operate at chamber pressures higher than 10 mbar. Nevertheless, recently, the exploration of lower pressure level conditions seems to have become a new challenge. In the present study, pressure levels as low as 0.5 mbar have been achieved and tested. It is shown that a decrease in the chamber pressure provides a longer and enlarged plasma jet whose length may be longer than one meter for the lowest pressure levels considered. CFD modeling results and photographs performed under vacuum conditions are proposed for the case a standard conical nozzle. Some additional characterizations (using thermocouples and emission spectroscopy) were also conducted but the results are currently being analyzed.

An experimental study is conducted to determine the property fields of 40 MHz argon radio frequency inductively coupled plasma using optical emission spectroscopy. The pure argon plasma was operated at the input power of 0.3 kW and under atmospheric pressure. 29 atomic argon lines with upper level energies ranging from 12.9 to 15.5 eV, continuum emission and line width are used to evaluate plasma parameters such as temperature and electron number density. Since 40 MHz plasma is in almost complete nonequilibrium, the validaty and accuracy of most usual spectroscopic methods are questioned. Analysis based on the Boltzmann diagram, line-to-continuum intensity ratio, population of continuum extrapolated level, and continuum intensity reveals the departure from thermodynamic equilibrium in the plasma. Among these methods, the Boltzmann diagram method is shown to provide reliable plasma excitation temperature as long as the Boltzmann plot is drawn based on enough spectra lines covering from infrared to ultraviolet regions. The continuum emission at wavelengths within visible region can give good estimation of the electron density by using excitation temperature in the continuum relation. The line-to-continuum is not a reliable method for the temperature measurement of nonequilibrim plasma. The electron density obtained from the Saha plot can provide rough estimation of the electron density. It is shown that the electron-atom interaction contribution to the continuum radiation is more important than being expected before for the argon plasma in our study. The non-axisymmetric distribution of the emission was found to exist within the coil zone of the plasma, which may affect the estimation of the local emission coefficient, and consequently the measured plasma fields.

This paper describes a powerful new approach, based on optical emission spectroscopy, for monitoring thermal spraying processes and coating quality. Through online analysis of the emitted process spectra, users can track variations in the running process as well as in the coatings produced. As proven in numerous studies, all relevant process parameters can be separated and detected using OES techniques, and recent work indicates that the method is applicable to all thermal spray processes. Paper text in German.

This study evaluates the through-porosity of HVOF-sprayed Hastelloy C coatings on carbon steel with respect to coating thickness and combustion pressure. The amount of through-porosity in the NiCrMo alloy layer is determined by chemical analysis, using ICP emission spectroscopy, and compared with electrochemical measurements. Paper includes a German-language abstract.

In this paper, spectroscopic and electrostatic probe measurements are made to examine the characteristics of a supersonic dc plasma jet near the surface of titanium plate during a nitriding treatment. The low-pressure nitriding process is done using a mixture of ammonia, nitrogen, and hydrogen gasses. Heating effects from the plasma are evaluated with nickel slug and thermocouple attached to the plate. The authors present the results of their study along with observations, insights, and suggestions on how to improve plasma nitriding processes. Paper includes a German-language abstract.

This paper demonstrates the use of emission spectroscopy for monitoring trace impurities in plasma and flame sprayed layers during deposition. It describes the working principles of the method and presents and analyzes different spraying scenarios where small amounts of certain impurities can have a major consequence if not detected. Paper includes a German-language abstract.