Improved quantitative analysis of hard coatings by radiofrequency glow discharge optical emission spectrometry (rf?GD?OES)

Payling, Richard; Aeberhard, M.; Delfosse, Daniel

doi:10.1039/b007543o

Cited by 52 publications

(36 citation statements)

References 19 publications

(22 reference statements)

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“…In low discharge optical emission spectrometry (GD-OES) measurements, a dc bias voltage correction as well as a hydrogen correction were applied for most elements present. 46,47 Before performing quantitative depth profiling on the oxide films, anodized TiAlV and TiAlNb reference oxides with known thickness and composition were remeasured for compensation of possible small daily variations in the sputter rate. Best crater shape and plasma starting conditions were found at 700 Pa, 25 W (modulus ¼ 680, phase ¼ 440).…”

Section: Glow Discharge Optical Emission Spectrometrymentioning

confidence: 99%

Purified titanium oxide with novel morphologies upon spark anodization of Ti alloys in mixed H₂So₄/H₃PO₄ electrolytes

Kern

Zinger²

2006

J Biomedical Materials Res

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The spark anodization behavior of alpha/beta Ti6Al4V and Ti6Al7Nb alloys and of alpha c.p. Ti in H2SO4, H3PO4, and mixtures of these acids was studied. Chemical depth profiling revealed oxides purified with respect to the substrate alloying elements. This was particularly pronounced on Ti alloys spark anodized in H2SO4/H3PO4 mixtures, the Al content decreasing continuously towards the surface, and V and Nb hardly detectable in the outermost 200 nm. The incorporation of S was significantly reduced in mixed electrolytes, while about 8 at-% P was present. A novel oxide morphology with "worm-like" features in the micrometer range, very different from well-known nano/microporous oxides, was found in mixed electrolytes under suitable conditions. Similar but more porous-like morphologies were formed on Ti. Simple alpha/beta substrate microstructural considerations cannot explain the morphological and chemical observations. Raman spectroscopy indicated the presence of mixed anatase, rutile, and brookite phase on anodized Ti alloys. Bond strengths of 34 MPa for worm-like and 40-50 MPa for nano/microporous morphologies as well as excellent abrasion behavior were found. The compatibility of grit-blasting with the spark anodization process for creating multitopography surfaces was demonstrated. Neither the observed chemical effects, nor the observed particular morphology or the presence of brookite have been reported before.

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Section: Glow Discharge Optical Emission Spectrometrymentioning

confidence: 99%

Purified titanium oxide with novel morphologies upon spark anodization of Ti alloys in mixed H₂So₄/H₃PO₄ electrolytes

Kern

Zinger²

2006

J Biomedical Materials Res

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“…This refers to very quick and stable signals, particularly for H and O. Therefore, no hydrogen [16,17] or any other correction is necessary after the measurement. The hydrogen correction is used by other authors because small amounts of hydrogen in the plasma, either from contamination or by sputtering from the sample, can affect the measured intensities due to a change in the emission yield.…”

Section: Resultsmentioning

confidence: 99%

Analysis of interface impurities in electroplated Cu layers by using GD‐OES and TOF‐SIMS

Klemm

Stangl

Peeva³

et al. 2008

Surface & Interface Analysis

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Electrochemically deposited (ECD) copper layers used as interconnect metallizations exhibit incorporated impurities in the form of H, S, C, O, N, and Cl originating from additives in the electrolyte solution. These impurities were observed in the whole layer and especially at the interface to the underlying Cu seed layer due to an increased adsorption at the beginning of the electroplating process. Time-of-flight (TOF)-SIMS and glow discharge optical emission spectroscopy (GD-OES) were carried out for interface analysis of 100-nmECD thin Cu films plated on a 50-nm Cu seed layer deposited by physical vapor deposition (PVD). This reveals the respective advantages and disadvantages of both techniques for thin film analysis. Also the effect of a modification of the electroplating procedure is shown. This so-called Hot Start Plating inhibits the additive adsorption and decreases the undesirable incorporation of impurities.

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“…1,2) The merit of the r.f. plasma extended the application of GD-OES to a variety of samples; for instance, surface coating on a non-conductive substrate can be analyzed by using a similar handling for conductive samples, 3,4) which can attract more concern on surface analysis by using GD-OES. This paper suggests an advanced detection method in r.f.…”

Section: Introductionmentioning

confidence: 99%

Determination of Minor Alloyed Elements in Steel Samples in Radio-frequency Glow Discharge Plasma Optical Emission Spectrometry Associated with Pulsed Bias-Current Modulation Technique

Urushibata

Wagatsuma

2012

ISIJ Int.

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An advanced detection method based on a modulation technique is described in radio-frequency-powered glow discharge plasma optical emission spectrometry (r.f. GD-OES). A frequency-sensitive separation using a fast Fourier transform (FFT) analyser, where a pulsated bias-current was introduced into an r.f. GD plasma, was available for improving the limit of determination for the atomic emission analysis. The FFT analyser has an ability to disperse signal components by frequency, and it is thus employed to select the component of a particular frequency. A dc bias current introduced into the GD plasma can enhance the emission intensities of analyte species greatly, and furthermore, it can be easily pulsated to modulate the emission intensities from the plasma. The modulated emission signal was selectively detected with the FFT analyser, with removing any noise components from the overall signal. The duty ratio of the pulsed bias current largely affected the amplitude of the FFT frequency components, because the pulse waveform comprised sine-function components having frequencies integral-times as much as the fundamental frequency, whose contribution coefficients depended on the duty ratio. This detection method was applied to the determination of vanadium and molybdenum in low-alloyed steel samples. The detection limits were obtained to be 6.2 × 10 -3 mass% V and 2.0 × 10 -3 mass% Mo in low-alloyed steel samples.

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Improved quantitative analysis of hard coatings by radiofrequency glow discharge optical emission spectrometry (rf?GD?OES)

Cited by 52 publications

References 19 publications

Purified titanium oxide with novel morphologies upon spark anodization of Ti alloys in mixed H₂So₄/H₃PO₄ electrolytes

Purified titanium oxide with novel morphologies upon spark anodization of Ti alloys in mixed H₂So₄/H₃PO₄ electrolytes

Analysis of interface impurities in electroplated Cu layers by using GD‐OES and TOF‐SIMS

Determination of Minor Alloyed Elements in Steel Samples in Radio-frequency Glow Discharge Plasma Optical Emission Spectrometry Associated with Pulsed Bias-Current Modulation Technique

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Improved quantitative analysis of hard coatings by radiofrequency glow discharge optical emission spectrometry (rf?GD?OES)

Cited by 52 publications

References 19 publications

Purified titanium oxide with novel morphologies upon spark anodization of Ti alloys in mixed H2So4/H3PO4 electrolytes

Purified titanium oxide with novel morphologies upon spark anodization of Ti alloys in mixed H2So4/H3PO4 electrolytes

Analysis of interface impurities in electroplated Cu layers by using GD‐OES and TOF‐SIMS

Determination of Minor Alloyed Elements in Steel Samples in Radio-frequency Glow Discharge Plasma Optical Emission Spectrometry Associated with Pulsed Bias-Current Modulation Technique

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Purified titanium oxide with novel morphologies upon spark anodization of Ti alloys in mixed H₂So₄/H₃PO₄ electrolytes

Purified titanium oxide with novel morphologies upon spark anodization of Ti alloys in mixed H₂So₄/H₃PO₄ electrolytes