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Thermo Analytic Investigation of Hydrogen Effusion Behavior - Sensor Evaluation and Calibration
(2011)
The well established carrier gas analysis (CGA) method was used to test different hydrogen detectors comprising a thermal conductivity detector (TCD) and a metal oxide semiconducting (MOx) sensor. The MOx sensor provides high hydrogen sensitivity and selectivity, whereas the TCD exhibits a much shorter response time and a linear hydrogen concentration dependency. Therefore, the TCD was used for quantitative hydrogen concentration measurements above 50?µmol/mol. The respective calibration was made using N2/H2 gas mixtures. Furthermore, the hydrogen content and degassing behaviour of titanium hydride (TiH2-x) was studied. This material turned out to be a potential candidate for a solid sample calibration. Vacuum hot extraction (VHE) coupled with a mass spectrometer (MS) was then calibrated with TiH2-x as transfer standard. The calibration was applied for the evaluation of the hydrogen content of austenitic steel samples (1.4301) and the comparison of CGA-TCD and VHE-MS.
Modern methods like carrier gas hot extraction enable the quantification of dissolved hydrogen as well as the determination of the hydrogen trapping and diffusion behavior. This method was applied in order to compare for the first time the hydrogen diffusion and trapping behavior in electrochemically charged and welded duplex stainless steel (1.4462). Characteristic extraction temperatures (400, 650, and 900 °C) were used to quantify the amounts of diffusible hydrogen and trapped hydrogen for the base material and the weld metal, and in order to calculate the effective diffusion coefficients corresponding to the specific temperature. The comparison of the charging methods showed that electrochemically charged samples have a higher content of diffusible hydrogen than the welded samples. In addition, the effusion times increase in welded samples, which indicate a higher amount of trapped hydrogen. In electrochemically charged weld samples, a significant lower concentration of hydrogen was determined than in the base material. In addition, the effective diffusion coefficients were calculated for every microstructure and charging method. It was found that the base material has a higher effective hydrogen diffusion coefficient than that of the weld metal. This effect is due to the tortuous path of hydrogen diffusion in the weld metal.
Offshore wind turbines are an important goal in national energy strategies worldwide. Foundation structures are manufactured from submerged arc welded (SAW) plates with thicknesses up to 200 mm. In that connection, high-strength steels like the S420G2+M are more and more applied offering the possibility for increased stability and load-bearing capacity of the foundations. These offshore steel grades can show a susceptibility for delayed hydrogen assisted cold cracking of the weld joints. For that purpose, a minimum waiting time (MWT) of up to 48 h (dependent on applied standards) is recommended before non-destructive testing is allowed and conducted. But this concept is based on older steel grades that have been used for three or more decades. Nowadays, the metallurgical improvements (clean steels, proper rolling, and heat treatment) of base materials and well as welding consumables must be anticipated. Hence, the MWT concept should be critically discussed as it is assumed to be very conservative. For that reason, the focus of this study was to investigate the diffusion behavior in S420G2+M steel and its multi-layer SAW joint. Electrochemical permeation experiments were carried at room temperature. Boundary conditions were anticipated in terms of using different sample thicknesses. From the experimental data, hydrogen diffusion coefficients and absorbed diffusible hydrogen concentrations had been calculated. It was shown that hydrogen diffusion in the base material is increased compared to the weld metal. In addition, the sample thickness had a significant on the calculated diffusion coefficients. The minimum and maximum diffusion coefficients had been used for numerical modelling of the hydrogen diffusion in the welding joint. It became clear that a MWT must be always regarded together with a critical initial diffusible hydrogen concentration for the evaluation of a possible delayed cracking as diffusion times were mostly > 48 h due to the thick plates.
The steel grade 20MnMoNi5-5 (according to German DIN standard or 16MND5 according to French AFNOR standard) is widely applied in (weld) fabrication of reactor pressure vessel components. Thus, a wide range of welding technologies (like submerged arc welding (SAW) or tungsten inert gas (TIG)) is used resulting in different heat affected zone (HAZ) microstructures. During weld fabrication, the weld joints may take up hydrogen. Especially, the HAZ shows an increased susceptibility for a degradation of the mechanical properties in presence of hydrogen. In addition, the hydrogen-assisted degradation of mechanical properties is influenced by three main local factors: hydrogen concentration, microstructure, and load condition. Hence, the base material (BM) and two different simulated non-tempered as-quenched HAZ microstructures were examined using hydrogen-free and hydrogen-charged tensile specimens. The results indicate that the effect of hydrogen on the degradation is significantly increased in case of the HAZ compared to the BM. In addition, hydrogen has remarkable effect in terms of reduction of ductility. It was ascertained that the degradation of the mechanical properties increases in the order of BM, bainitic HAZ, and the martensitic HAZ. Scanning electron microscope (SEM) investigation showed a distinct change of the fracture topography depended on the microstructure with increasing hydrogen concentration in case of the as-quenched HAZ microstructures.
Der verstärkte Einsatz höherfester Stähle und Zusatzwerkstoffe erfordert ein vertieftes Verständnis der Zusammenhänge zwischen Schweißverfahren, Wärmeeinbringung, Abkühlbedingungen sowie den daraus resultierenden metallurgischen Vorgängen in der Schweißnaht und deren Umgebung. Nur aus dem Zusammenwirken aller Einflussfaktoren lassen sich Strategien ableiten, mit deren Hilfe die Festigkeitseigenschaften bzw. die Lebensdauer von Schweißkonstruktionen in einem Maße verbessert werden können, die den Einsatz höherfester Werkstoffe rechtfertigen und somit deren Leichtbaupotenzial voll ausgenutzt werden kann. Vorgestellt werden einige beispielhafte Untersuchungen an Schweißverbindungen aus höherfesten Feinkornbaustählen zu Interaktionen der Haupteinflussgrößen auf die Kaltrissbildung.----------------------------------------------------------------------------------------------------------------------------
The increased utilisation of higher-strength steels and filler materials necessitates more profound understanding of the connections between the welding process, the heat input, the cooling conditions and the resulting metallurgical processes in the weld and its surroundings. Strategies which help to improve the strength properties and service lives of welded structures to such an extent that the utilisation of higher-strength materials can be justified and their lightweight construction potential can thus be exploited to the full can only be derived from the interaction between all the influencing factors. Examples of a few investigations on welded joints between higher- strength fine-grained structural steels with regard to the interactions between the main variables influencing the cold cracking are presented in this article.
Comparative study between hot extraction methods and mercury method - a national round robin test
(2010)
Comparative study between hot extraction methods and mercury method - a national round robin test
(2010)
A round robin test is presented comprising comparative measurements using hot extraction at different degassing temperatures as well as the mercury method. A major focus of the investigation was verification of the maximum degassing temperature for analysing the diffusible hydrogen in weld metals with bcc-lattice structure. The analyses were executed using a basic stick electrode with high weld metal cracking, a high-alloyed supermartensitic filler wire with different hydrogen contents in the shielding gas and a high-strength solid wire. The results show that degassing temperatures of 150 degrees C and 400 degrees C do not lead to an increase in the measured contents of diffusible hydrogen as compared to measurements at room temperature. The measuring techniques and procedures specified in ISO/DIS 3690:2009 for determining the diffusible hydrogen content in weld metals with bcc-lattice structure yield approximately the same results. This is to say that the mercury method and the hot extraction methods with thermal conductivity detector (TCD) can be regarded as equivalent reference methods.
In this study, hydrogen absorption and diffusion were investigated for various high-alloyed ferritic-austenitic duplex steels. On account of the specific transformation and solidification behaviour, respectively, of duplex steels as compared to single-phase ferritic and austenitic steels, special conditions have to be considered concerning hydrogen absorption which may ultimately lead to microstructure-dependent hydrogen-assisted weld metal cracking. Hydrogen absorption during welding may occur via the shielding gas, moisture from the surroundings or via the welding filler material. As a contribution to the interpretation and prediction of hydrogen-induced cracking in welded duplex steels, the actual hydrogen absorption via the arc as well as the weld metal hydrogen diffusion was investigated for the first time in a duplex steel DS (1.4462), a super duplex steel SDS (1.4501) and in a lean duplex steel LDS (1.4162). Isothermal heat treatment using carrier gas hot extraction enabled quantification of the amounts of hydrogen trapped in the respective microstructure areas. The hydrogen diffusion coefficients were determined by analytical and numerical calculation. The total hydrogen concentrations and the diffusion coefficients were found to be nearly identical. Trapped hydrogen was however observed to be dependent on the material and on the microstructure condition. The influence of hydrogen on the mechano-technological properties of the weld metal was characterized with the help of tensile tests. In addition, the hydrogen embrittlement effect was detected in scanning electron microscopic analyses.
Neutron radiography and tomography have been used for a time resolved in situ analysis and a 3D mapping of hydrogen diffusion in iron and steel. Samples were electrochemically charged with hydrogen and afterwards neutron transmission images were taken. Hydrogen diffusion coefficients in duplex stainless steel were determined at 623 K by measuring and comparing the sample's mean intensity with a hydrogen-free reference sample and subsequent normalisation to standards with known hydrogen content. In technical iron and in supermartensitic stainless steel the hydrogen distributions have been investigated. The radiographic images in iron show blisters, cracks and the distribution of molecular hydrogen inside cracks. The analysis of the diffusion behaviour of hydrogen out of a blister illustrates the capabilities of the method with respect to time and spatial resolution. The neutron tomography of supermartensitic tensile stressed samples illustrates the capability to visualise hydrogen distributions three-dimensionally. -------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
On a utilisé la radiographie neutronique et la tomographie pour une analyse in situ à résolution temporelle et une cartographie 3D de la diffusion de l'hydrogène dans le fer et l'acier. On a chargé des échantillons par électrochimie avec de l'hydrogène et ensuite on a pris des images par émission de neutrons. On a déterminé les coefficients de diffusion de lhydrogène dans l'acier inoxydable duplex à 623 K en mesurant et en comparant l'intensité moyenne de l'échantillon avec un échantillon de référence sans hydrogène et une normalisation subséquente à des échantillons références à teneur connue en hydrogène. On a examiné la distribution d'hydrogène dans le fer technique et dans l'acier inoxydable supermartensitique. Les images radiographiques du fer montrent des soufflures, des fissures, et la distribution de l'hydrogène moléculaire à l'intérieur des fissures. L'analyse du comportement de diffusion de l'hydrogène hors d'une soufflure illustre les possibilités de la méthode par rapport à la résolution temporelle et spatiale. La tomographie neutronique des échantillons supermartensitiques chargés en traction illustre la capacité de visualiser les distributions d'hydrogène en trois dimensions.