The chemical analysis of TiN films: A round robin experiment

High‐Temperature Oxidation—Testing and Evaluation

“…Round-robin tests of characterization by including a range of analyses such as XPS, EPMA, XRS, AES, Atom Probe Microanalysis (APMA), and XRD are not uncommon. Among these, XRD was felt to be unreliable [40].…”

An interlaboratory comparison of energy dispersive X-ray microanalysis (EDX) of titanium and zirkonium nitrides

“…Secondly, the analysis of these compounds represents a problem for most methods (see e.g. the large scattering of data for the density determined by X-ray diffraction [1] and the dozen papers devoted to the analysis of TiNx by Auger electron spectroscopy [2], [3], and references therein). Numerous publications outline the problems associated with the analysis of these compounds by different methods 1-2, 4].…”

Determination of the Composition of TiNx and TiBxNy Films by AES

“…The N/Ti ratio must be extracted from the overlapping T i-L 3M23M 23 and N -K L 23L23 peaks. In a report of a "round robin" study, Perry et al have summarised 4 different meth ods which have been used by authors in an attempt to correctly determine the N/Ti ratio from spectra ac quired in the derivative mode [2], Some of these meth ods make the assumption that peak shape changes arising from differing TiN ratios do not affect the positive or negative excursions used for quantifica tion. Palmer has suggested that smoothing of high energy resolution data is a useful method to reduce the errors induced by lineshape distortions [4], This tech nique will be considered for the determination of the N/Ti ratio of T i-B -N samples.…”

“…Much work has of been undertaken to establish a simple and accurate method for the determination of the composition of TiNx Films. Many techniques, principally Auger Elec tron Spectroscopy (AES), X-ray Photoelectron Spec troscopy (XPS), Rutherford Backscattering Spectros copy (RBS) and Energy Dispersive X-ray Analysis (EDX) have been considered [1][2][3][4][5][6][7][8]. None of the techReprint requests to Dr. J. Haupt.…”

“…EDX also has a large escape depth and this, combined with the overlap of the Ti LI and N Ka lines and the low probability of the N Ka emission causes difficulties with quantification. The more surface sensitive electron spectroscopic techniques are normally prefered for thin film analysis, but for TiNx problems of peak overlap and peak fit ting in AES and XPS, respectively, have resulted in many different approaches [1,2,5,6,8]. For XPS, the unusual structure in the Ti 2p region between the Ti 2p1/2 and Ti 2p3/2 lines has been ascribed to satel lite structure or the presence of oxygen which varies as a function of N concentration, causing uncertainties in the peak area measurements [1,[6][7][8].…”