Highly hydrogen-sensitive thermal desorption spectroscopy system for quantitative analysis of low hydrogen concentration (∼1 × 1016 atoms/cm3) in thin-film samples

This paper presents experimental results of study of hydrogen accumulation in technically pure titanium alloy at saturation from gas atmosphere. Automated complex Gas Reaction Controller has been used for hydrogen saturation from gas atmosphere. Temperatures increasing from 350 °C to 500 °C allow increase hydrogen sorption process and as a result significantly increase hydrogen concentration in technically pure titanium alloy. At hydrogen saturation from gas atmosphere at temperature 500 °C increasing of saturation time from 10 minutes to 120 minutes leads to hydrogen concentration increasing from 0.1 wt.% to 1 wt.% and increasing of hydrides volume content throughout the samples. The activation energy for hydrogen evolution has been estimated by thermal desorption spectroscopy method by equal 102 kJ/mol.

Download Full-text

Thermal desorption spectroscopy study on a TiN thin film. (II).

Shinku ◽

10.3131/jvsj.31.525 ◽

1988 ◽

Vol 31 (5) ◽

pp. 525-528

Author(s):

Daisuke FUJITA ◽

Teiichi HOMMA ◽

Makoto TANAKA ◽

Toshihiko SATO

Keyword(s):

Thin Film ◽

Thermal Desorption ◽

Thermal Desorption Spectroscopy ◽

Spectroscopy Study

Download Full-text

Improved Accuracy of Thermal Desorption Spectroscopy by Specimen Cooling during Measurement of Hydrogen Concentration in a High-Strength Steel

Materials ◽

10.3390/ma13051252 ◽

2020 ◽

Vol 13 (5) ◽

pp. 1252 ◽

Cited By ~ 2

Author(s):

Eric Fangnon ◽

Evgenii Malitckii ◽

Yuriy Yagodzinskyy ◽

Pedro Vilaça

Keyword(s):

Thermal Desorption ◽

Hydrogen Concentration ◽

High Strength Steel ◽

Vacuum Chamber ◽

Thermal Desorption Spectroscopy ◽

High Strength ◽

Steel Sample ◽

Martensitic Steels ◽

Hydrogen Flux ◽

Redistribution Of Hydrogen

Thermal desorption spectroscopy (TDS) is a powerful method for the measurement of hydrogen concentration in metallic materials. However, hydrogen loss from metallic samples during the preparation of the measurement poses a challenge to the accuracy of the results, especially in materials with high diffusivity of hydrogen, like ferritic and ferritic-martensitic steels. In the present paper, the effect of specimen cooling during the experimental procedure, as a tentative to reduce the loss of hydrogen during air-lock vacuum pumping for one high-strength steel of 1400 MPa, is evaluated. The results show, at room temperature, the presence of a continuous outward hydrogen flux accompanied with the redistribution of hydrogen within the measured steel during its exposure to the air-lock vacuum chamber under continuous pumping. Cooling of the steel samples to 213 K during pumping in the air-lock vacuum chamber before TDS measurement results in an increase in the measured total hydrogen concentration at about 14%. A significant reduction in hydrogen loss and redistribution within the steel sample improves the accuracy of hydrogen concentration measurement and trapping analysis in ferritic and martensitic steels.

Download Full-text

Characterization of Cu/CeO2/γ-Al2O3 Thin Film Catalysts by Thermal Desorption Spectroscopy

Catalysis Letters ◽

10.1007/s10562-005-8002-4 ◽

2005 ◽

Vol 105 (1-2) ◽

pp. 35-40 ◽

Cited By ~ 17

Author(s):

Yong Men ◽

Hubert Gnaser ◽

Christiane Ziegler ◽

Ralf Zapf ◽

Volker Hessel ◽

...

Keyword(s):

Thin Film ◽

Thermal Desorption ◽

Thermal Desorption Spectroscopy ◽

Thin Film Catalysts ◽

Al2o3 Thin Film

Download Full-text

Quantitative Analysis of Hydrogen by Thermal Desorption Spectroscopy(TDS).

Shinku ◽

10.3131/jvsj.42.879 ◽

1999 ◽

Vol 42 (10) ◽

pp. 879-885 ◽

Cited By ~ 2

Author(s):

Yuko HIROHATA

Keyword(s):

Quantitative Analysis ◽

Thermal Desorption ◽

Thermal Desorption Spectroscopy

Download Full-text

Application of EDS Technique for OSP Film Thickness Measurement

ISTFA 2006: Conference Proceedings from the 32nd International Symposium for Testing and Failure Analysis ◽

10.31399/asm.cp.istfa2006p0193 ◽

2006 ◽

Author(s):

Prong Kongsubto ◽

Sirarat Kongwudthiti

Keyword(s):

Thin Film ◽

Quantitative Analysis ◽

Joint Strength ◽

Critical Factor ◽

Thickness Measurement ◽

Ic Manufacturing ◽

And Control ◽

Film Thickness Measurement ◽

Non Destructive

Abstract Organic solderability preservatives (OSPs) pad is one of the pad finishing technologies where Cu pad is coated with a thin film of an organic material to protect Cu from oxidation during storage and many processes in IC manufacturing. Thickness of OSP film is a critical factor that we have to consider and control in order to achieve desirable joint strength. Until now, no non-destructive technique has been proposed to measure OSP thickness on substrate. This paper reports about the development of EDS technique for estimating OSP thickness, starting with determination of the EDS parameter followed by establishing the correlation between C/Cu ratio and OSP thickness and, finally, evaluating the accuracy of the EDS technique for OSP thickness measurement. EDS quantitative analysis was proved that it can be utilized for OSP thickness estimation.

Download Full-text

Investigation of the Pressure Dependent Hydrogen Solubility in a Martensitic Stainless Steel Using a Thermal Agile Tubular Autoclave and Thermal Desorption Spectroscopy

Metals ◽

10.3390/met11020231 ◽

2021 ◽

Vol 11 (2) ◽

pp. 231

Author(s):

Patrick Fayek ◽

Sebastian Esser ◽

Vanessa Quiroz ◽

Chong Dae Kim

Keyword(s):

Stainless Steel ◽

Thermal Desorption ◽

Hydrogen Diffusion ◽

Martensitic Stainless Steel ◽

Thermal Desorption Spectroscopy ◽

Hydrogen Uptake ◽

Hydrogen Solubility ◽

Automotive Components ◽

Set Up ◽

Service Application

Hydrogen is nowadays in focus as an energy carrier that is locally emission free. Especially in combination with fuel-cells, hydrogen offers the possibility of a CO2 neutral mobility, provided that the hydrogen is produced with renewable energy. Structural parts of automotive components are often made of steel, but unfortunately they may show degradation of the mechanical properties when in contact with hydrogen. Under certain service conditions, hydrogen uptake into the applied material can occur. To ensure a safe operation of automotive components, it is therefore necessary to investigate the time, temperature and pressure dependent hydrogen uptake of certain steels, e.g., to deduct suitable testing concepts that also consider a long term service application. To investigate the material dependent hydrogen uptake, a tubular autoclave was set-up. The underlying paper describes the set-up of this autoclave that can be pressurised up to 20 MPa at room temperature and can be heated up to a temperature of 250 °C, due to an externally applied heating sleeve. The second focus of the paper is the investigation of the pressure dependent hydrogen solubility of the martensitic stainless steel 1.4418. The autoclave offers a very fast insertion and exertion of samples and therefore has significant advantages compared to commonly larger autoclaves. Results of hydrogen charging experiments are presented, that were conducted on the Nickel-martensitic stainless steel 1.4418. Cylindrical samples 3 mm in diameter and 10 mm in length were hydrogen charged within the autoclave and subsequently measured using thermal desorption spectroscopy (TDS). The results show how hydrogen sorption curves can be effectively collected to investigate its dependence on time, temperature and hydrogen pressure, thus enabling, e.g., the deduction of hydrogen diffusion coefficients and hydrogen pre-charging concepts for material testing.

Download Full-text