Quantitative trace analysis of technical materials with solid state mass spectrometry: An analytical strategy for SIMS

Distinct improvement in adhesion of diamond coatings on hard metal substrates was achieved by following substrate surface pretreatment [I]: First WC was removed from the substrate surface by etching with Murakami solution (K3[Fe(CN)6] in KOH), after which the Co binder network was etched with H2S04/H202 solution. Then diamond coatings were deposited on the substrates by hot-filament CVD. Apparently during the H2S04/H202 treatment of the Co binder a thin COO / CoS04 film forms, which prior to the diamond deposition would be reduced to CoS by the hydrogen and carbon species involved in the diamond synthesis. Since CoS is a stable compound at the diamond deposition temperatures, its Co vapor pressure and the Co surface mobility should be substantially lower than that for metallic Co. Thus the diamondhard metal interface is no longer influenced detrimentally by the metallic Co binder. This explanation has however not yet been confirmed by analytical methods such as SIMS and XPS. An alternative explanation would be the increassd roughness of the hard metal surface resulting from the removal of the Co binder and the formation of deep grooves on the interface which could lead to the improved adhesion. This however docs not explain why Co migration and other detrimental effects are not observed.

show abstract

“…SIMS measurements were performed using a CAMECA ims 3f ion microscope [25,26]. An 02+ or a CS+ primary beam was applied to sputter the samples.…”

Section: Sims Analysismentioning

confidence: 99%

Murakami and H₂SO₄/H₂O₂ Pretreatment of WC-Co Hard Metal Substrates to Increase the Adhesion of CVD Diamond Coatings

et al. 1995

Self Cite

View full text Add to dashboard Cite

show abstract

“…1 A number of authors have reported measurement techniques to minimize the contribution of uncertainties to the analytical results. [2][3][4][5][6][7][8][9][10] One of the error factors is related to the specimen holder, itself. It has been reported that the obtained secondary ion intensities are different from those among the windows of the specimen holder, 8,11 or from the tilted holder to the electric field of the extraction space.…”

Section: Introductionmentioning

confidence: 99%

Evaluation of the Electric Field above a Specimen Surface during SIMS Analysis

Yamazaki

Enda

2000

ANAL. SCI.

View full text Add to dashboard Cite

Secondary ion mass spectrometry (SIMS) has been a central analytical technique for the microelectronics industry. More precise analysis has become important along with the development and process monitoring of integrated circuits (ICs) production. The level of quantitative analysis is influenced by random and systematic uncertainties. The origin of these uncertainties in SIMS have been well documented by Werner. 1 A number of authors have reported measurement techniques to minimize the contribution of uncertainties to the analytical results. [2][3][4][5][6][7][8][9][10] One of the error factors is related to the specimen holder, itself. It has been reported that the obtained secondary ion intensities are different from those among the windows of the specimen holder, 8,11 or from the tilted holder to the electric field of the extraction space. 6,8 Also, the ion intensities fall off as the analysis location approaches the edge of the holder window. 6,13,14 These detrimental phenomena are attributed to the deviation of secondary ion trajectories by a distortion of the electric field, which is commonly applied above the sample surface in order to effectively collect the emitted secondary ions. It has been accepted that the distortion is caused by warping of the holder faceplate due to pressure from the mounting springs. 9 Besides, it has been demonstrated by a computer simulation that a non-uniform electric field exists near to the window edge of the holder. 14 In the Cameca IMS-type SIMS instrument, a high extraction field, typically 1.0 kV/mm, is used between the sample and a grounded extraction plate (immersion lens cover); therefore, the effect of the specimen holder is more sensitive than for other types of instruments. There are no investigations mentioned in the literature concerning a distorted electric field above various types of specimen holders.In this work, we investigated the distortion area of the electric field near to the edge of the specimen holder window as a function of the faceplate thickness of the specimen holder by a computer simulation after confirming that the computed results was in good agreement with the SIMS experimental results. We also demonstrated the advantage of a specimen holder with a tapered-edge faceplate. ExperimentalThe experiments were conducted using a Cameca IMS-4f ion microscope. A Cs + primary ion beam with an impact energy of 14.5 keV was used. The primary ion current was 100 nA and the raster size was 250 × 250 µm 2 . In the IMS-4f, the specimen holder was biased to -4.5 kV for the detection of negative secondary ions. The distance between the surface of the specimen holder and the grounded extraction plate (immersion lens cover) was 4.5 mm. Thus, an electric field of 1.0 kV/mm was applied above the surface of the specimen holder. 28 Sisecondary ions were detected using a Faraday-cup detector. The diameter of the analyzed area in the center of the crater bottom was 60 µm. The types of specimen holders used in this experiment are summarized in Table 1. The type-B holde...

show abstract

References

2014

Secondary Ion Mass Spectrometry

View full text Add to dashboard Cite

Quantitative trace analysis of technical materials with solid state mass spectrometry: An analytical strategy for SIMS

Cited by 13 publications

References 26 publications

Murakami and H₂SO₄/H₂O₂ Pretreatment of WC-Co Hard Metal Substrates to Increase the Adhesion of CVD Diamond Coatings

Murakami and H₂SO₄/H₂O₂ Pretreatment of WC-Co Hard Metal Substrates to Increase the Adhesion of CVD Diamond Coatings

Evaluation of the Electric Field above a Specimen Surface during SIMS Analysis

References

Contact Info

Product

Resources

About

Quantitative trace analysis of technical materials with solid state mass spectrometry: An analytical strategy for SIMS

Cited by 13 publications

References 26 publications

Murakami and H2SO4/H2O2 Pretreatment of WC-Co Hard Metal Substrates to Increase the Adhesion of CVD Diamond Coatings

Murakami and H2SO4/H2O2 Pretreatment of WC-Co Hard Metal Substrates to Increase the Adhesion of CVD Diamond Coatings

Evaluation of the Electric Field above a Specimen Surface during SIMS Analysis

References

Contact Info

Product

Resources

About

Murakami and H₂SO₄/H₂O₂ Pretreatment of WC-Co Hard Metal Substrates to Increase the Adhesion of CVD Diamond Coatings

Murakami and H₂SO₄/H₂O₂ Pretreatment of WC-Co Hard Metal Substrates to Increase the Adhesion of CVD Diamond Coatings