Highly sensitive detection of net hydrogen charged into austenitic stainless steel with secondary ion mass spectrometry

Tohru Awane; Yoshihiro Fukushima; Takashi Matsuo; Saburo Matsuoka; Yukitaka Murakami; Shiro Miwa

doi:10.1021/ac103100b

Highly sensitive detection of net hydrogen charged into austenitic stainless steel with secondary ion mass spectrometry

Anal Chem. 2011 Apr 1;83(7):2667-76. doi: 10.1021/ac103100b. Epub 2011 Mar 14.

Authors

Tohru Awane¹, Yoshihiro Fukushima, Takashi Matsuo, Saburo Matsuoka, Yukitaka Murakami, Shiro Miwa

Affiliation

¹ Research Center for Hydrogen Industrial Use and Storage, National Institute of Advanced Industrial Science and Technology (HYDROGENIUS), 744 Moto-oka, Nishi-ku, Fukuoka 819-0395, Japan.

PMID: 21401058
DOI: 10.1021/ac103100b

Abstract

Secondary ion mass spectrometry (SIMS) is used to detect local distributions of hydrogen in various materials. However, it has been well-known that it is extremely difficult to analyze net hydrogen (H(N)) in metals with SIMS. This was because hydrogen, which is originated from moisture (H(2)O), hydrocarbon (C(x)H(y)) or other organic materials (C(x)H(y)O(z)) existing on a sample surface or in the SIMS chamber, is simultaneously detected in the SIMS measurement of the H(N), and the H(N) and the background-originated hydrogen (H(BG)) cannot be distinguished in a SIMS profile. The effective method for reductions and determinations of the H(BG) in hydrogen measurements of metallic materials with the SIMS method has not been established. The present paper shows an effective method for reduction and estimation of H(BG) in SIMS analyses of hydrogen charged into type 316 L austenitic stainless steel, and an accurate estimation method of the net charged hydrogen. In this research, a silicon wafer is sputtered by a primary ion beam of a SIMS near an analyzed area (silicon sputtering method) to reduce H(BG). An uncharged type 316 L sample was prepared for estimation of H(BG) in SIMS measurements of the hydrogen-charged sample. The gross intensities of hydrogen between the hydrogen-charged sample and the uncharged sample were compared. The gross intensities of hydrogen of the uncharged sample (26.8-74.5 cps) were much lower than the minimal gross intensities of hydrogen of the hydrogen-charged sample (462-1140 cps). Thus, we could reduce the H(BG) enough to estimate the hydrogen charged into the type 316 L sample. Moreover, we developed a method to determine intensities of H(BG) in the measurement of the hydrogen-charged sample by estimating the time-variation of hydrogen intensities in the measurements of the uncharged sample. The intensities of the charged hydrogen can be obtained by subtracting the estimated intensities of the H(BG) from the gross intensities of hydrogen of the hydrogen-charged sample. The silicon sputtering method used to reduce H(BG) and the determination method for H(BG) in this research can be applied to the accurate hydrogen analysis for other various metallic materials.