This master´s thesis deals with hot dip galvanizing of steel constructions and their protection from corrosion. This work describes the origin of corrosion of steel and its corrosion in different areas and presents degreasing and pickling before hot dip galvanization. It describes possibilities of making zinc layer by the wet and draw method of hot dip galvanization. Furthermore, it puts forward reactions between zinc and iron, possible defects of the zinc layer and influence of the hot dip galvanizing on the steel constructions. The experimental part examines the influence of the hydrogen charging on the material and the time of the flux operation on the quality of layer. The work further analyses the changing of mechanical properties of steels Hardox 500 and Weldox 700 as a result of the hydrogen embrittlement during pickling by the hydrochloric acid.

The present paper studied the influence of hydrogen on the mechanical properties and microstructure of the materials. This study is done by doing hydrogen charging of steel bar specimens. The two types of steel are used for study, structural steel S235 and stainless steel 316L. The tensile test has been performed to get the data of the charged and uncharged specimens. Different strain rates were used to study the effect of the material after charging. The charging time ranged from 24 hours to 144 hours. The specimens are cylindrical shape. Digital image analysis is performed for the uncharged specimens to correctly analyse the strain field and compare it with the results from tensile test. For DIC analysis a GOM correlate software was used to study the 2D strain analysis of the specimen. The results show that hydrogen influences the mechanical properties of the material and microstructure.

En raison d’une combinaison de propriétés physiques, chimiques et mécaniques remarquables, les alliages de titane et de titane sont devenus des candidats prometteurs dans le domaine de l'industrie chimique, de l’aéronautique, de l'aérospatiale et des matériaux biomédicaux. Durant les procédures de fabrication ainsi qu’en service, les composants sont exposés à des environnements tels que la surface de ces composant seront exposées à l’hydrogène. Par conséquent, la compréhension de l’interaction de ces matériaux avec l'hydrogène lors de divers procédés de d’élaboration et de mise en forme est importante afin que leurs propriétés et leurs performances puissent être contrôlées et prédites de manière fiable. Dans le but d'améliorer les propriétés et les performances du titane et de réduire le coût de fabrication des produits en titane, le présent travail se concentre principalement sur les effets de l'hydrogène sur le laminage à froid et le phénomène de recristallisation de deux titanes caractérisés par une structure cristalline différente, c'est-à-dire une structure hexagonale et cubique cubique pour respectivement le titane de pureté commerciale Ti50A et l'alliage de titane β-métastable β-21S. Étant donné que la microstructure du titane et de ses alliages est le facteur contrôlant leurs propriétés et leurs performances, l'évolution microstructurale en présence d'hydrogène introduit par deux méthodes distinctes a été analysée par une combinaison de techniques expérimentales incluant DRX, SEM-EBSD et TEM. L'introduction de l'hydrogène dans le Ti50A par une méthode électrolytique a conduit à la précipitation de deux types d'hydrures (δ-TiHx, ε-TiH2) dans la matrice de phase , et il a été constaté que la fraction volumique de ces hydrures augmentait avec la durée du temps de chargement électrolytique. En raison du mode de formation par précipitation à partir des joints de grains, cinq relations d'orientation (OR) entre la -phase et l'hydrure δ-TiHx ont été déterminées par analyses des projections stéréographiques, et parmi celles-ci trois nouvelles relations d'orientation ont pu être mise en évidence. En outre, la corrélation entre la texture de laminage et la précipitation à l'hydrure a pu être établie. On a constaté que l'existence de la texture de de laminage facilitait la précipitation d'hydrure δ suivant l'orientation d’orientation de type OR2. Les analyses de rayons X révélaient un élargissement des pics de diffraction de la phase , ce qui indiquait une augmentation de la densité de dislocation, ces dislocations étant nécessaires pour tenir compte de l'inadéquation du réseau entre les hydrures et la matrice. Sur la surface d’échantillons déformés en compression, l'observation des traces de glissement et de macle de tension de type TT1 {10 2} < 011> dans les -grains contenant des hydrures a suggéré que les hydrures avaient une certaine capacité à supporter une déformation de cisaillement, en fonction des relations d'orientation entre la matrice et les hydrures mais aussi de leur épaisseur. Bien qu'aucune corrélation directe entre la nucléation des macles et la présence des hydrures n’ait été établie dans cette étude, l'effet des hydrures sur le développement des macles a été constaté. En étudiant l’effet de l'hydrogène sur le comportement au laminage à froid dans Ti50A, il a été possible de montrer que la formation de macle de type TT1 peut être facilitée par l'augmentation du rapport c/a de la maille hexagonale résultant de l’addition de l'hydrogène et de l'existence de contraintes locales générées par la précipitation des hydrures. Un raffinement de la microstructure a également été observé dans le Ti50A hydrogéné, ce qui suggère que la présence d'hydrures a tendance à générer de nouveaux grains de fortes désorientations (HAB). En outre, de nombreuses dislocations géométriquement nécessaires (GND) permettant de tenir compte de l'incompatibilité de contrainte entre l'hydrure et [...] / Due to an attractive combination of physical, chemical and mechanical properties, titanium and titanium alloys have become promising candidates in the field of chemical industry, aerospace and biomedical materials. During manufacturing procedures and applications, components are exposed to environments that can act as sources of hydrogen. Therefore, understanding their interaction with hydrogen upon various mechanical/thermal processing is important so that their properties and performance can be controlled and reliably predicted. With the aim of enhancing the properties and performance of titanium and reducing the cost of manufacturing products, the present work is primarily focusing on the effect of hydrogen on the cold rolling behavior and the subsequent annealing of titanium and titanium alloy characterized by different crystalline structure, i.e. hexagonal and body cubic centered (bcc) structure for the commercial pure titanium Ti50A and metastable β-titanium alloy β-21S, respectively. Since the microstructure of titanium and its alloys is the governing factor that determines their properties and performance, the microstructural evolution in the presence of hydrogen upon various procedures was analyzed by combination of XRD, SEM-EBSD and TEM. The introduction of hydrogen in Ti50A by electrolytic method induced the precipitation of two types of hydrides (δ-TiHx, ε-TiH2) in the  phase matrix, and it was found that the volume fraction of these hydrides increased as the charging time increased. Five orientation relationships (ORs), three of them being new orientation relationships ever reported, between the -phase and the hydride δ-TiHx were determined. Moreover, the correlation between the rolling texture and the hydride precipitation was also established. It was found that the existence of the rolling texture facilitated the precipitation of δ-hydride following the OR2-type orientation relationship. X-ray analyses revealed a broadening of the diffraction peaks corresponding to the  phase, indicating a increase of the dislocation density, these dislocations being necessary to accommodate the lattice misfit between hydrides and the matrix. Under compression loading, the observation of slip traces and tension twin {10 2}< 011> TT1 in the -grains containing hydrides, suggested that the hydrides had a certain ability to accommodate the imposed shear strain, depending on the orientation relationships between the matrix and the hydrides as well as on their thickness. Although no correlation between the nucleation of twinning and the hydride could be established in this study, the hydrides seemed to play an important role on the development of twinning deformation. The effects of hydrogen on the cold rolling behavior in Ti50A showed that, the formation of TT1tension twins can be facilitated due to the increase of the c/a ratio owing to the hydrogen addition and the existence of local stresses generated by the precipitation of hydrides. The refinement of the microstructure was also observed in the hydrogenated Ti50A-H suggesting that the presence of hydrides can enhance the generation of high angle boundaries (HABs). In addition, the formation of numerous geometrically necessary dislocations (GND) allowing the accommodation of the strain incompatibility between the hydride and matrix could be worked out by SEM-EBSD, which also confirmed analyses of the X-ray traces. In the case of β-21S alloy, with bcc structure that can accommodate a larger concentration of interstitial atoms, hydrogen was introduced by gas method. The effect of hydrogen on the microstructure was found to be closely related to the hydrogen concentration. In the range of hydrogen/metal ratio 0.052 < H/M < 0.300, the microstructure consisting of the single β-phase showed that the dissolved hydrogen atoms expanded the bcc β-lattice and suppressed the decomposition of the β phase upon cooling [...]

Zirconium alloys are widely used in the nuclear industry because of their high strength, good corrosion resistance and low neutron absorption cross-section. However, zirconium has strong affinity for hydrogen, which may lead to hydrogen concentration build-up over time during a corrosion reaction when exposed to water. Hydrogen stays in solution at higher temperature but precipitates as zirconium hydrides at ambient temperatures. The formation of zirconium hydrides is considered to be a major cause of embrittlement, in particular as a key step in the mechanism of delayed hydride cracking. Despite the fact that zirconium hydrides have been studied for several decades, the basic nature and mechanisms of hydride formation, transformation and exact structure are not yet fully understood. In order to find the answer to some of these problems, the precipitation and dissolution of hydrides in commercial grade Zr powder were monitored in real time with high resolution synchrotron and neutron radiations, and the whole pattern crystal structure analysis, using Rietveld and Pawley refinements, were performed. For the first time all commonly reported zirconium hydride phases and complete reversible transformation between two different Zr-hydride phases were recorded with a single setup and their phase transformation type have been analyzed. In addition, the preparation route of controversial γ-zirconium hydride (ZrH), its crystal structure and formation mechanisms are also discussed. / <p>Note: The papers are not included in the fulltext online.</p><p>Paper II and III in thesis as manuscript, paper II with title "The phase transformation between the δ and ε Zr hydrides"</p>

Many industries including the medical, aerospace, and automobile industries have increasingly adopted the use of shape memory alloys (SMAs) for a plethora of applications due to their unique thermomechanical properties. From the commercially available SMAs in the market, binary NiTi SMAs have shown the most desirable properties. However, SMA properties can be significantly affected by the fabrication process. One of the most familiar applications of NiTi SMAs is in the design of actuating devices where the shape memory effect properties are highly advantageous. Spring NiTi SMA actuators are among the most commonly used and are generally made by torsion loading a straight wire. Consequently, stress concentrations are formed causing a reduction in recovery force. Other methods for producing springs and other NiTi SMA components is the fast emerging manufacturing method of additive manufacturing (AM). AM often uses metal powders to produce the near-net shape components. A major challenge for SMAs, in particular, is their well-known composition sensitivity. Therefore, it is critical to control composition in NiTi SMAs. In this thesis, a novel method for processing NiTi SMAs for pre-alloyed NiTi SMA powders and springs is presented. A low pressure and low temperature hydriding-pulverization-dehydriding method is used for preparing the pre-alloyed NiTi SMA powders with well-controlled compositions, size, and size distributions from wires. By hydrogen charging as-drawn martensitic NiTi SMA wires in a heated H3PO4 solution, pulverizing, and dehydriding, pre-alloyed NiTi powders of various well-controlled sizes are produced. In addition, a low pressure and low temperature hydriding-dehydriding method is used for producing NiTi SMA helixes from wires. The helix pattern in the pre-alloyed NiTi SMA wires was obtained by hydrogen charging NiTi SMA 500 μm diameter wires at different time intervals, followed by dehydriding to remove the hydrogen. The wires, powders, and resulting helixes were characterized using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and x-ray diffraction (XRD). The relationship between the wire diameter, powder particle size, and helix geometry as a function of hydrogen charging time is investigated. Lastly, the recovery behavior due to the shape memory effect is also investigated after dehydriding.

In this work, Slow Strain Rate Test (SSRT) testing, Light Optical Microscopy (LOM) and Scanning Electron Microscopy (SEM) were used to study the effect of micro-structure, corrosive environments and cathodic polarisation on stress corrosion cracking (SCC) of two grades of high strength steels, Type A and Type B. Type A is manufactured by quench and tempered (Q&amp;T) method. Type B, a normalize steel was used as reference. This study also supports electrochemical polarisation resistance method as an effective testing technique for measuring the uniform corrosion rate. SSRT samples were chosen from base metal, weld metal and Heat Affected Zone (HAZ). SSRT tests were performed at room temperature under free corrosion potential and cathodic polarisation using 4 mA/cm2 in 1 wt% and 3.5 wt% NaCl solutions. From the obtained corrosion rate measurements performed in 1 wt% and 3.5 wt% NaCl solutions it was observed that increased chloride concentration and dissolved oxygen content enhanced the uniform corrosion for all tested materials. Moreover, the obtained results from SSRT tests demonstrate that both Q&amp;T and normalized steels were not susceptible to SCC in certain strain rate(1×10-6s-1) in 1 wt% and 3.5 wt% NaCl solutions under free corrosion potential. It was con-firmed by a ductile fracture mode and high reduction in area. The weld metal of Type A with acicular ferrite (AF), pro-eutectoid (PF) and bainite microstructure showed higher susceptibility to hydrogen assisted stress corrosion cracking compared to base metal and HAZ. In addition, typical brittle intergranular cracking with small reduction in area was observed on the fracture surface of the Type A due to hydrogen charging.

Since hydrogen is an alternative energy source and has both economic and environmental benefits, it has received more attention. To use hydrogen a certain condition must be met, safe pressurized containers which are often made of metal. The metal isrequired due to the high mechanical strength and reasonable cost. The problematic part is that hydrogen affects the mechanical properties of the material. Using metal in an environment with hydrogen will break down and lead to Hydrogen Environmental Embrittlement (HEE). If hydrogen will be used safely, understanding its effect on high-strength steel is necessary. Many studies have been done on hydrogen embrittlement, but it is not sufficient and therefore studies are still ongoing. The goal is to create further understanding of when components exposed to hydrogen in their service environment, in terms of mechanical, fracture surface and microstructural aspects. There are two types of stainless steel that was examined, 304 stainless steel (304 SS) and 316L stainless steel (316L SS), all specimens are cylindrical. The study mainly focused on mainly experimental aspects with some simulations. To charge the samples with hydrogen, a cathodic charging method was chosen. For fast strain rate, samples were loaded from 12 to 48 hours while slow strain rate was not preloaded. Measurement and Digital image correlation (DIC) were used due to slippage during tensile testing, it would also provide the actual engineering stress-strain curve. To see the microstructure, it was sanded, polished and etched. A special container was created to test the slow strain rate. This was done through several different tests. Both types of steel were affected by hydrogen, the yield strength and ductility were reduced. Charging at the slow strain rate leads to extreme embrittlement compared to the high strain rate. The grain boundaries had decreased in size after being charged with hydrogen. The 304 SS grains were more difficult to detect compared to the 316L SS. Different types of factors can affect the result, for the slow strain rate, hydrogen was present all the way until it reached its breaking point and after it started diffusion. Meanwhile, the hydrogen diffusion started at a high strain rate when it was taken out from charging in the container. During the time it takes to place the sample in the tensile testing machine and do the tensile test, the hydrogen diffuses, and it results in less brittleness. Keywords: Hydrogen embrittlement, tensile test, DIC, metallographic. / Eftersom väte är en alternativ energikälla och har både ekonomiska och miljömässiga fördelar har det fått mer uppmärksamhet. För att använda väte måste vissa villkor uppfyllas, det krävs säkra trycksatta behållare som ofta är gjorda av metall. Metall används på grund av kravet på hög mekanisk hållfasthet och rimliga kostnader. Den problematiska delen är att väte påverkar de mekaniska egenskaperna hos materialet. Genom att använda metall i en miljö med vätgas kommer att brytas ned och leda till vätmiljöförsprödning. Om väte kommer att användas på ett säkert sätt är förståelsen för dess effekt på höghållfast stål nödvändig. Det har gjorts många studier om väteförsprödning men det är inte tillräcklig och därför pågår undersökningar fortfarande. Målet är att skapa ytterligare förståelse för när komponenter som utsätts för väte i deras servicemiljö, när det gäller mekaniska, sprick ytan och mikrostrukturella aspekter. Det finns två typer av rostfritt stål som undersöktes, 304 rostfritt stål (304 SS) och 316L rostfritt stål (316L SS), alla prov är cylindriska. Studien fokuserade huvudsakligen på huvudsakligen experimentella aspekter med vissa simuleringar. För att ladda proverna med väte valdes en katodisk laddningsmetod. För snabb töjnings hastighetladdades proverna från 12 till 48 timmar medan långsam töjnings hastighet förladdades inte. Mätning och Digital bildkorrelat (DIC) användes på grund av glidning under dragprovning, dettaskulle ge den korrekta ingenjörs spänning-töjningskurvan. För att se mikrostrukturen så slipades, polerades och etsning utfördes. En speciell behållare skapades för att testa den långsamma töjnings hastighet. Detta gjordes genom flera olika tester. Båda typerna av stål påverkades av väte, avkastningsstyrkan och duktiliteten minskades. Laddning med den långsamma töjnings hastighet leder till extrem försprödhet jämfört med den höga töjnings hastighet. Korngränserna hade minskat sin storlek efter att de laddats med väte. 304 SS-kornen var svårare att upptäcka i jämförelse med 316L SS. Olika typer av faktorer kan påverka resultatet, för långsam töjnings hastighet var väte närvarande hela vägen tills det har nått sin brytpunkt och efter det började diffusion. Under tiden startade vätediffusionen med högt töjnings hastighet när den kom ut laddar behållaren. Under den tid det tar att placera provet i dragprovningsmaskinen och göra dragprovningen så diffuserar vätet och det leder till mindre sprödhet. Nyckelord: Väteförsprödning, dragprovning, DIC, metallografisk.

This research focused on a comprehensive microstructural and mechanical property characterisation study of the Ni-Fe-Cr alloys 718 and 945X. The aim of the project was to better understand the relationship between performance and microstructure of existing (Alloy 718) and newly developed (Alloy 945X) high strength nickel alloys focusing on downhole applications. The main difference between the two alloys is that alloy 945X has lower Nb content than alloy 718, which may minimise the tendency to form delta when combined with correct processing. Previous studies have related the hydrogen embrittlement in alloy 718 with the collection of hydrogen by delta phase. Microstructural characterisation of the new alloy 945X after long term isothermal exposure up to 120 hours in the temperature range 650◦C to 900◦C was conducted with scanning electron microscopy (SEM), to generate a time-temperature-transformation (TTT) diagram. The TTT diagram was used as a road map for designing two isothermal heat treatments of alloy 945X on tensile specimens. Then, the effect of hydrogen charging on the tensile properties and microstructure of the 'as-received' and these two variant heat treatments was investigated. Fractographic analysis showed that, in the presence of hydrogen, intergranular fracture occurred for all the heat treatments, regardless the presence of delta phase at grain boundaries. There was no simple correlation between the volume fraction of delta-phase and susceptibility to hydrogen assisted embrittlement. Rather, it was demonstrated that the morphology and distribution of delta-phase along grain boundaries plays a key role and the other precipitate phases also have an influence through their effect on the ease of strain localisation. This study also examined the hydrogen embrittlement sensitivity of nickel alloy 718 given four different heat treatments to obtain various microstructural states. Each heat treatment leads to differences in the precipitate morphologies of γ', γ'' and delta phases. Material characterisation and fractography of the examined heat treatments were performed using a high resolution FEG-SEM. Three specimens of each condition were pre- charged with hydrogen and tensile properties were compared with those of non-charged specimens. It was observed that hydrogen embrittlement was associated with intergranular and transgranular microcrack formation, leading to an intergranular brittle fracture. delta phase may assist the intergranular crack propagation, and this was shown to be particularly true when this phase is coarse enough to produce crack initia- tion, but this is not the only factor determining embrittlement. Other microstructural features play a role, as does the strength of the material. Finally, the evolution of delta-(Ni3Nb) phase in alloy 718 from the early stages of precipitation, with a particular focus on identifying the grain boundary characteristics that favour precipitation of grain boundary delta phase was investigated. Results showed that delta phase was firstly formed on Σ3 boundaries after 5 hours at the examined temperature (800◦C). Increasing ageing time at 800◦C was observed to lead to an increase in size and precipitation of phases γ'-γ''-delta, an increase in fraction of the special CSL boundaries and an evolution in the morphology of twins and the growth of grains.