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Proceedings of the 2012 9th International Pipeline Conference IPC2012 September 24-28, 2012, Calgary, Alberta, Canada

IPC2012-90390
Application of FIB/SEM/EBSD for Evaluation of Residual Strains and their relationship to Weld Metal Hydrogen Assisted Cold Cracking
1

W.L. Costin , I.H. Brown , L. Green and R. Ghomashchi School of Mechanical Engineering, The University of Adelaide Adelaide, SA 5005, Australia 2 Adelaide Microscopy, The University of Adelaide Adelaide, SA 5005, Australia

ABSTRACT Hydrogen assisted cold cracking (HACC) is a welding defect which may occur in the heat affected zone (HAZ) of the base metal or in the weld metal (WM). Initially the appearance of HACC was associated more closely with the HAZ of the base metal. However, recent developments in advanced steel processing have considerably improved the base material quality, thereby causing a shift of HACC to the WM itself. This represents a very serious problem for industry, because most of the predictive methods are intended for prevention of HACC in the HAZ of the base metal, not in the weld metal [1]. HACC in welded components is affected by three main interrelated factors, i.e. a microstructure, hydrogen concentration and stress level [2-4]. In general, residual stresses resulting from the welding process are unavoidable and their presence significantly influences the susceptibility of weld microstructures to cracking, particularly if hydrogen is introduced during welding [5]. Therefore various weldability tests have been developed over the years which are specifically designed to promote HACC by generating critical stress levels in the weld metal region due to special restraint conditions [4, 6-8]. These tests were used to develop predictive methods based on empirical criteria in order to estimate the cracking susceptibility of both the heat-affected zone and weld metal [4]. However, although the relationship between residual stress, hydrogen and HACC has received considerable attention, the interaction of residual stresses and microstructure in particular at microscopic scales is still not well understood [5, 9-21]. Therefore the current paper focuses on the development and assessment of techniques using Focused Ion Beam (FIB), Scanning Electron Microscopy (SEM) and Electron Backscatter Diffraction for the determination of local residual strains at (sub) micron scales in E8010 weld metal, used for the root pass of X70 pipeline girth welds, and their relationship to the WM

microstructure. The measurement of these strains could be used to evaluate the pre-existing stress magnitudes at certain microstructural features [22]. INTRODUCTION In Australia, shielded metal arc (SMA) welding with cellulosic welding consumables is traditionally used for stovepipe welding of pipelines. This manual metal arc welding technique offers unique productivity advantages and is therefore part of a well established process for pipeline girth weld production. This process involves the use of E6010 electrodes without preheat for the root pass, and E8010 electrodes for subsequent passes [23]. The high moisture content in the cellulosic flux of the electrode decomposes during welding and produces a gaseous shield rich in hydrogen. This hydrogen gas provides a high arc force which results in high welding speeds and improved penetration of the arc [24]. However, hydrogen also dissolves in the molten weld metal and as a result of its reduced solubility after solidification it can diffuse to various regions of the microstructure and promote HACC [4]. The redistribution of hydrogen during and after cooling of the weld depends on thermal, stress related and microstructural factors. The greatest risk of HACC occurs when the weld cools down to temperatures below about 200C. Above this temperature, cracking is unlikely to initiate in High Strength Low Alloy (HSLA) steels, HAZ, or weldmetal [4, 25]. Prior to the utilization of high quality pipeline steels such as X70 and X80, HACC formation was usually associated with the heat affected zone of the base metal (Figure 1). However, recent developments in advanced steel processing have considerably improved the base material quality, thereby enhancing the resistance of the HAZ to HACC. This gradual development of pipeline steels caused a shift of HACC formation from the HAZ of the base metal to the WM itself (Figure 2) [26].

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HAZ
1040 steel

WM

Figure 1:

HACC in the HAZ of the base metal (1040 steel) [27].

HAZ
API 5L X70

WM

generating critical stress levels in the weld metal region through special restraint conditions [4, 6-8]. In the absence of suitable criteria, these tests are used to predict conditions under which weld metal HACC cracking was likely to occur [4]. The susceptibility of the weld metal microstructure to HACC was thereby predicted by calculating the carbon equivalent, an indicator for the hardenability, which is an empirical value, based on the nominal composition of the weld metal [1]. Generally, it was considered that the cracking susceptibility increases with increasing hardness or strength [2, 4]. However, a number of workers [2, 7] have indicated that it is the particular microstructure used to achieve the strength which will have a greater influence on HACC than its strength level per se and that neither hardness, nor strength are reliable indicators for HACC susceptibility. Although the relationship between residual stress, hydrogen and HACC has received considerable attention, the interaction of residual stresses with particular microstructural features still remains unclear [5, 9-21].

Figure 2:

HACC in the weld metal (WMHACC) (API 5L X70 grade base metal).

This represents a very serious problem for industry, because none of the current avoidance strategies are capable of considering the weld metal behavior. For example, the procedures for HACC avoidance embodied in the Australian Pipeline Code AS2885 involve the use of Welding Technology Institute of Australia, WTIA, Technical Note 1, which does not treat the subject of weld metal cracking at all [26]. Overall, there is very little information on the risk of weld metal hydrogen cracking which can provide a basis for the derivation of safe welding conditions. [28]. The following causal factors, presented schematically in Figure 3, must be present simultaneously for the occurrence of HACC in HSLA steel welds [2-4]; i. a stress of sufficient magnitude due to either residual stresses or applied stresses, ii. a critical concentration of diffusible hydrogen, iii. a susceptible microstructure Residual stresses resulting from the welding process are unavoidable and their presence significantly influences the susceptibility of weld microstructures to cracking, particularly if hydrogen is introduced during welding [5, 19]. Therefore various weldability tests have been developed over the years which are specifically designed to promote HACC by

Figure 3:

Stress, hydrogen and weld metal microstructure, all affected by thermal parameters, are the pre-requisites for HACC formation.

For applications in mechanical and materials engineering, a number of semi-destructive analysis methods have been developed based on material removal and the measurement of the associated strain relief [22]. All of these methods rely on the same principle, namely, that the introduction of new tractionfree surfaces causes measurable redistribution (relief) of the elastic strain which can be measured and related to the preexisting stress magnitude e.g. by numerical deformation modelling [22]. However, currently most of these residual strain measurements and calculations are carried out on a macroscopic scale, without consideration of the microstructure which has a significant influence on the local stress/strain levels [29]. Recent developments using electron optical techniques provide opportunities to examine residual stress/strain at microscopic scales. Focused Ion Beam (FIB) milling has been used as a micro-machining tool for material removal [22, 30,

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31] of thin films and sputter coatings. The displacements at the sample surface were measured by using scanning electron microscopy or focused ion beam microscopy in combination with digital image correlation [22, 30, 31]. However there is little information available in the published literature on the application of FIB/SEM for residual stress measurements on the surface of bulk materials and the relationship of these residual strains to the microstructure. Furthermore, none of the proposed methods which are based on displacement measurements by correlation of images before and after material removal are suitable to determine plastic strain that occurred prior to the capture of the first image. Therefore the aims of the current report are: i. to assess the feasibility of using the FIB/SEM for material removal and displacement measurements on the surface of pipeline weld metal specimens, ii. to evaluate the application of FIB channelling contrast and Electron Backscatter Diffraction (EBSD) for revealing the effect of the residual strain release on the adjacent microstructure, HYDROGEN ASSISTED MECHANISMS COLD CRACKING

resulting in an increase in the mean separation between the atoms of the host metal and a decrease in their force of attraction [14]. Thermodynamic evaluations [35] showed that a (tensile) positive hydrostatic component of stress decreases the chemical potential of an interstitial solute, whereas a (compressive) negative hydrostatic component of stress increases the chemical potential of the solute [5]. Under equilibrium conditions, when the chemical potential is uniform, dissolved hydrogen will tend to concentrate in tensile stressed regions, for example, ahead of a crack tip, to lower its chemical potential. As the local hydrogen concentration increases in these regions, the cohesive energy, and consequently the critical stress to break iron-iron atomic bonds decreases [36]. When this critical stress falls below the local stress level, fracture occurs spontaneously. Hydrogen then evolves in the crack volume and the process is repeated [11, 37]. STRAIN ANALYSIS USING FOCUSED ION BEAM MICRO HOLE DRILLING As reported by Withers and Bhadeshia [29] residual stress fields can be categorised according to characteristic length scales. Macroscopic residual stresses are designated type I and they vary continuously over large distances (Figure 4). Hole drilling and other material removal techniques have been widely used for measurements of residual stress on a macroscopic scale [22, 29, 38, 39]. These techniques rely on monitoring of elastic strain or displacements that are induced in components due to the relaxation of residual stresses at newly exposed free surfaces. A brief summary of these established measurement techniques and their attributes are listed in Table 1 of Annex A. In contrast to macroscopic type-I residual stresses, residual stresses which vary over distances comparable to the grain size of the material are designated type-II or intergranular stresses. Residual stresses on a scale smaller than the grain size are designated type-III or atomic scale stresses. In the latter cases, the resulting displacements induced at newly exposed surfaces due to the relaxation of residual stresses have microscopic or submicroscopic dimensions. Low level type-II stresses nearly always exist in polycrystalline materials because of the variation in the elastic and thermal properties of differently oriented neighboring grains. More significant grain scale stresses occur when the microstructure contains several phases or phase transformations have taken place. The type-III category typically includes stresses due to coherency at interfaces and dislocation stress fields [29]. The significance of type-II and type-III residual stresses is driving the development of techniques capable of measuring elastic strains on the micro and nano scales.

The most common mechanisms proposed for HACC are: i. internal pressure due to formation of hydrogen bubbles within the structure ii. formation of brittle hydrides iii. de-cohesion of the matrix at inclusions or precipitates as a result of reduction in interfacial energy due to the presence of hydrogen (hydrogen-enhanced decohesion HEDE model) iv. reduction or enhancement of dislocation mobility (embrittlement or plastic deformation) due to the presence of hydrogen (e.g. hydrogen-enhanced localized plasticity HELP model) The first of these mechanisms has been largely discounted by the fact that crack propagation can occur at sub-atmospheric pressures [15, 32]. The formation of brittle hydrides is not generally applicable to HSLA steels [5, 32] and the hydrogen enhanced local plasticity (HELP) mechanism is discussed elsewhere by the authors [34]. The hydrogen enhanced decohesion theory (HEDE) is a widely accepted model, which involves the degradation of cohesive bonds between iron atoms due to interstitial monatomic hydrogen. Troiano was the first to propose that hydrogen atoms were attracted to regions of high tri-axial tensile stresses where they fill interstitial sites and weaken the cohesive strength of the metal which leads to brittle failure [17]. Oriani reported that, the cohesive force (the force needed to increase the interatomic distance) between metal atoms is affected by hydrogen because it changes the local and the global electronic structure of the metal in which it resides,

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Figure 5:

Approximate length scales and strain sensitivities offered by a range of strain analysis techniques. Those towards the bottom left combine superior spatial resolution with high strain sensitivity [30].

Figure 4:

Residual stress fields categorised according to characteristic length scales [29].

Recently Dual Beam electron microscopes which incorporate both Focused Ion Beam (FIB) and Scanning Electron Microscope (SEM) capabilities have been used for the measurement of type-II and type-III residual stresses in thin films at the micro- and nano scales. The FIB is used for the material removal and lower resolution imaging of the resulting displacements and the SEM, because of its higher resolution, provides the opportunity for comparing the images before and after material removal (image correlation) at higher spatial resolution [22, 30, 31]. Figure 5 shows the approximate length scales and strain sensitivities achieved by several strain measurement techniques. As highlighted, the Dual Beam FIB/SEM enables material removal and image correlation with high spatial resolution and high strain sensitivity. This technique is suitable for measuring displacements down to a few nanometers. Moreover, the large range of magnifications available on the Dual Beam instruments allows the observation of residual stress fields at both the microscopic and the macroscopic scales. Several techniques using various shapes of material removal combined with sputtered or deposited patterns for the digital image correlation and displacement measurements have been reported for thin films and coatings [22, 31, 40]. Kang [31] used a rectangular reference pattern to measure the displacements after the introduction of a milled slot (Figure 6).

Figure 6:

SEM images of a region of a DLC film before (a) and after (b) the introduction of the FIB slot. The rectangles were introduced as reference marks by using a low intensity ion beam. [31]

Korsunsky [22] deposited a thin layer of platinum and created a reference pattern on the surface of this layer by drilling a regular array of small depth holes. Afterwards he milled a ring and determined the strain relief on the surface of the resulting island by measuring the displacement of the holes in the reference pattern (Figure 7).

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milled hole. The distortion is more obvious at high magnifications as highlighted in Figure 11.
Cracktip

Figure 7:

SEM image of a region in a TiN PVD coating after introduction of a FIB milled ring. Prior to ring drilling, a thin layer of Pt was deposited and patterned by drilling a regular array of small depth holes [22].

Figure 8:

Transverse cross section of the selected sample after polishing.

EXPERIMENTAL PROCEDURE AND RESULTS The transverse cross section of a weld metal specimen used in this analysis is shown in Figure 8. A description of the cellulosic SMA welding consumable (E5-1) and the composition of the parent plate are given in Tables 2, 3 and 4 in Annex A. Abrasive wet cutting was used to extract the weld metal and to achieve a suitable specimen size for the sample preparation and subsequent electron optical investigations. In order to minimize surface defects and preparation artifacts, automated sample preparation was used for grinding and polishing, which additionally enables the reproducibility of sample surface conditions. The region selected for analysis was ahead of a crack tip where high residual stresses were expected, as illustrated in Figure 8. A pattern of seven 1.5 m diameter rings were milled using the FIB ahead of the crack tip. FIB and SEM images of the ring pattern were taken for later use, as a reference for the measurement of displacements. The SEM image of the milled rings is shown in Figure 9. A 1.5m diameter micro-hole was then milled in ring 4, at the position of the crack tip, to enable relaxation of residual stresses. After hole drilling SEM and FIB images were captured to allow a qualitative observation of possible displacements. The arrangement of the FIB and SEM column in the Dual Beam results in a large tilt angle between the sample surface and the incident electron beam and therefore the resulting secondary electron images of the sample surface are distorted and require digital tilt correction. This has to be considered when analyzing the deformation of the rings in the SEM images. The qualitative comparison of the images in Figure 9 and Figure 10 indicate slight distortion of ring 5 adjacent to the

Figure 9:

SEM image of ring pattern milled ahead a crack tip.

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nearly aligned) with the incident ion beam direction due to a decrease in the number of emitted secondary electrons, Figure 13.

Figure 10:

SEM image of ring pattern milled ahead a crack tip after material removal.

Figure 12:

Ring pattern milled ahead a crack tip [41].

1,5m

1,5m

Figure 11:

SEM image of ring pattern 5. (a) prior to material removal from ring 5, (b) after material removal form ring 4 prior and after material removal.

However, because the distortion is adjacent to the milled hole, the profile of the ion beam has to be considered. As shown in Figure 12, depending on the ion beam intensity a rounding of the edge will occur during milling which could be interpreted as distortion in the SEM image shown in Figure 11. The next step was to compare the FIB images. For the standard milling configuration there is no tilt of the sample relative to the incident ion beam which has to be considered. The resolution of a conventional ion beam is usually lower than that of an SEM with a field emission filament. In addition, the sample surface will be sputtered during imaging using the ion beam, even at low beam intensities, and this can result in topographic contrast due to selective sputtering as shown in Figures 10 and 15. However, ion beam imaging can reveal the crystallographic orientation of the surface due to ion channeling. Channeling contrast is a result of the varying secondary electron yield due to different crystallographic orientations of the grains within the sample. Thus a grain will appear darker when it is aligned (or

Figure 13:

Schematic illustrating the formation of the channelling contrast [41].

The qualitative comparison of the FIB images in Figures 14 and 15 show even more evidence for deformation of ring 5, and in addition, a displacement of the microstructure within the ring can be observed in Figure 16. Based on the rounding of the edges of the milled hole as shown in Figure 15, the observed deformation of ring 5 seems unlikely to be an artifact resulting from the ion beam profile. The effect of selective sputtering is not considered in this case because the deformation of the ring in Figure 16(a) is located within a region which has the same crystallographic orientation, as revealed by the channeling contrast in Figure 15. Therefore the qualitatively observed deformation of ring 5 adjacent to the milled hole is believed to be displacement caused by relaxation of residual stresses generated at newly exposed free surfaces.

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However the displacements of the microstructure appearing in Figure 16 could be an artifact caused by the exposure of subsurface features due to material removal at the sample surface during imaging.

for analyzing and quantifying the crystallographic aspects of microstructures have been well documented for a wide variety of materials and applications [30, 34]. The Image Quality (IQ) map shown in Figure 17 reveals the microstructure with much more detail and accuracy compared with the channeling contrast technique (Figure 15).

(a) prior material removal


Figure 16:

(b) after material removal


1,5m

FIB image of ring pattern 5 prior and after material removal.

Figure 14:

FIB image of ring pattern milled ahead a crack tip.

Figure 17:

IQ map of ring pattern milled ahead a crack tip.

7 Therefore, the utilization of EBSD and application of image correlation between the FIB and the IQ images, would make it possible to identify the region or the phases most affected by the release of elastic strain energy as a result of micro-hole drilling and material removal. This provides a significant advantage compared with previous methods based on image correlation of ion beam images because of the better resolution and the reduced likelihood of surface damage. CONCLUSIONS AND FUTURE WORK

Figure 15:

FIB image after hole drilling with resulting deformations and displacements.

FIB imaging has poor resolution and may damage the sample surface during observation. Therefore Electron Backscatter Diffraction (EBSD) was employed to obtain more detailed information about the microstructure without damaging the sample surface. The capabilities of this technique

The application of FIB hole drilling for residual strain measurements at microscopic dimensions has been demonstrated in the vicinity of a hydrogen assisted cold crack in the weld metal used for joining X70 line pipe steel. The influence of the ion beam profile on the measurement of displacements has been discussed. However, further investigation is required to determine the relationship between ion beam intensity, sputtering time, hole depth and hole profile. Another important task is to examine the range of hole

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dimensions that can be achieved with this technique so that the limitations for the resolution of the residual strain measurements can be determined. The limitations of FIB imaging for revealing the microstructure related to displacements at microscopic dimensions have been discussed. Due to these limitations, EBSD was employed to reveal the microstructure at higher resolution and with reduced tendency for the introduction of artifacts due to sputtering by the ion beam. The results of this study provide strong evidence for the development of a method to measure residual strain at microscopic dimensions, with respect to the microstructure. Future work will utilise this technique through in-situ observations of slow strain rate tensile tests on hydrogen charged and uncharged weld metal samples. This will provide an opportunity for a better understanding of the relationship between hydrogen, residual stress and microstructure, which will in turn enable the initiation and propagation process for hydrogen assisted cold cracking to be better understood. ACKNOWLEDGMENTS This work is funded by the Energy Pipelines CRC, supported through the Australian Government Cooperative Research Centres Program. The cash and in-kind support from the APIA through its Research and Standards Committee is also gratefully acknowledged. We are grateful to Prof. V. Linton, Dr. F. Barbaro and Mr. L. Fletcher for useful discussion and constructive comments. Special thanks are also due to Adelaide Microscopy and its director, Mr. John Terlet. REFERENCES [1] Yurioka, N., 1999, "Predictive Methods for Prevention and Control of Hydrogen Assisted Cold Cracking," Proc. Weld Metal Hydrogen Cracking in Girth Welds Wollongong. [2] Davidson, J. L., and Olson, D. L. R., 1997, Hydrogen Management in Steel Weldments: Joint Seminar, Melbourne, Australia, 23rd October 1996 : Proceedings of the Seminar, Published by the Organising Committee of the Joint Seminar on behalf of Defence Science and Technology Association and Welding Technology Institute of Australia. [3] Olson, D. L. R., 1998, High Strength Steel Weldment Reliability: Weld Metal Hydrogen Trapping : Final Progress Report, Center for Welding, Joining, and Coatings Research, Colorado School of Mines. [4] Yurioka, N., 1990, "Hydrogen Assisted Cracking in C-Mn and Low Alloy Steel Weldments," International Material Reviews, 35(4). [5] Boellinghaus, T., 2001, "Numerical Modelling of Hydrogen Assisted Cracking," NACE International. [6] Glover A., and Rothwell B., 1999, "Specifications and Practices for Hydrogen Crack Avoidance in Pipeline Girth Welds," Wollongong, Australia. [7] Graville B., 1986, "A Survey Review of Weld Metal Hydrogen Cracking," Welding in the World, 24), pp. 190-198.

[8] Graville B., 1995, "Interpretive Report on Weldability Tests for Hydrogen Cracking of Higher Strength Steels and Their Potential for Standardization," Welding Research Council Bulletin. [9] Boellinghaus, and Hoffmeister, T., 1996, "Scatterbands for Hydrogen Diffusion Coefficients in Steels Having a Ferritic or Martensitic Microstructure and Steels Having an Austenitic Microstructure at Room Temperature," Welding in the World London-, 37(1), pp. 16-23. [10] Oriani, 1994, "A Brief Survey of Useful Information About Hydrogen in Metals," Department of Chemical Engineering and Materials Science University of Minnesota, Salt Lake City. [11] Oriani, R. A., 1972, "Testing of the Decohesion Theory of Hydrogen Induced Crack Propagation," Scripta METALLURGICA, 6(pp. 681-688. [12] Oriani, R. A., 1978, "Hydrogen Embrittlement of Steels," Annual Review Material Science, pp. 327-357. [13] Oriani, R. A., 1970, "The Diffusion and Trapping of Hydrogen in Steel," Acta Metallurgica, 18(1), pp. 147-157. [14] Oriani, R. A., 1993, "The Physical and Metallurgical Aspects of Hydrogen in Metals," Department of Chemical Engineering and Materials Science The University of Minnesota, Palo Alto, CA 94304. [15] Oriani, R. A., and Josephic, P. H., 1974, "Equilibrium Aspects of Hydrogen-Induced Cracking of Steels," Acta Metallurgica, 22(9), pp. 1065-1074. [16] Satoh K., 1972, "Recent Trend of Researches on Restraint Stresses and Strains for Weld Cracking," Welding in the World, 11(pp. 133-155. [17] Troiano, A. R., 1960, "The Role of Hydrogen and Other Interstitials in the Mechanical Behaviour of Metals," Trans. ASM., 52(pp. 54-80. [18] Wongpanya, and Boellinghaus, 2009, "Residual Stress Distribution in Competing S 1100 Ql Butt-Welds Dependent on Plate Thickness and Restraint Length," Takasaki. [19] Wongpanya P., Boellinghaus Th., Lothongkum G., and Hoffmeister H., 2009, "Numerical Modelling of Cold Cracking Initiation and Propagation in S 1100 Ql Steel Root Welds," Welding in the World, 53(3). [20] Yurioka N., 1989, "A Review of Numerical Analyses on the Hydrogen Diffusion in Weldingof Steel," The International Institute of Welding, Japan. [21] Yurioka N., Ohshita S., Nakamura H., and Asano K., 1980, "An Analysis of Microstructure, Strain and Stress on the Hydrogen Accumulation in the Weld Heat-Affected Zone," The International Institute of Welding, Japan. [22] Korsunsky, A. M., Sebastiani, M., and Bemporad, E., 2010, "Residual Stress Evaluation at the Micrometer Scale: Analysis of Thin Coatings by Fib Milling and Digital Image Correlation," Surface and Coatings Technology, 205(7), pp. 2393-2403. [23] Fletcher, L., 2000, "A Holistic Model of Hydrogen Cracking in Pipeline Girth Welding," Welding in the World London, 44(2), pp. 7.

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[24] Weaver, R. J., 2005, "Cellulosic-Covered Electrode Storage," Rio de Janeiro. [25] Coe, F. R., 1973, Welding Steels without Hydrogen Cracking / by F. R. Coe, Welding Institute, Cambridge :. [26] Fletcher, L., 1999, "Weld Metal Cracking in Pipeline Girth Welds," Wollongong. [27] Kou, S., 2003, Welding Metalurgy, John Wiley & Sons, Inc., Hoboken, New Jersey, Chap. 17. [28] Pargeter R.J., 1992, "Effects of Arc Energy, Plate Thickness and Preheat on C-Mn Steel Weld Metal Hydrogen Cracking," Technical Report No. No. 461/1992, TWI Research Report (CRP), U.K. [29] Withers, P. J., and Bhadeshia, H. K. D. H., 2001, "Residual Stress Part 1 - Measurement Techniques," Materials Science and Technology, 17(4), pp. 355-365. [30] Adam J. Schwartz, M. K., Brent L. Adams, David P. Field, 2009, Electron Backscatter Diffraction in Material Science, Springer Science+Business Media, New York. [31] Kang, K. J., Yao, N., He, M. Y., and Evans, A. G., 2003, "A Method for in Situ Measurement of the Residual Stress in Thin Films by Using the Focused Ion Beam," Thin Solid Films, 443(12), pp. 71-77. [32] Hirth, J. P., 1980, "Effects of Hydrogen on the Properties of Iron and Steel," Metallurgical Transactions A, 11 [33] Lynch, S. P., 1979, "Mechanisms of Hydrogen-Assisted Cracking," Met. Forum, 2(pp. 189-200. [34] Brown I. H., Costin W.L. , Barbaro, F. and Ghomashchi, R, 2012, "Application of SEM-EBSD for Measurement of Plastic Strain Fields Associated with Weld Metal Hydrogen Assisted Cold Cracking " Calgary, Alberta, Canada. [35] Li, J. C. M., Oriani, R. A., and Darken, L. S., 1966, "The Thermodynamics of Stressed Solids," Zeitschrift fr Physikalische Chemie, 49(3_5), pp. 271-290. [36] Lee, J. A., 1996, Hydrogen Effect in Materials, The Minerals, Metals & Materials Society. [37] Johnson, H. H., and Troiano, A. R., 1957, "Crack Initiation in Hydrogenated Steel," Nature, 179(4563), pp. 777-777. [38] Niku-Lari, A., Lu, J., and Flavenot, J., 1985, "Measurement of Residual-Stress Distribution by the Incremental Hole-Drilling Method," Experimental Mechanics, 25(2), pp. 175-185. [39] Schajer, G. S., 1988, "Measurement of Non-Uniform Residual Stresses Using the Hole-Drilling Method. Part I--Stress Calculation Procedures," Journal of Engineering Materials and Technology, 110(4), pp. 338-343. [40] Gerdes, H., and Gatzen, H., 2009, "Focused Ion Beam Core Hole Drilling for Stress Detection in Thin-Films," Microsystem Technologies, 15(1), pp. 151-153. [41] Costin, W., 2008, "3D Tomography for Material Science Applications Using Focused Ion Beam Microscopy," Bachelor FH Wr. Neustadt, Wiener Neustadt. [42] N.Coniglio, V. L., E.Gamboa, 2010, "Mechanised WIC Tesing of Boron Containing Smaw Consumables," Technical Report No. APIA09-06.

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ANNEX A MACROSCOPIC RESIDUAL STRESS MEASUREMENT TECHNIQUES

Table 1:

Summary of various measurement techniques and their attributes [29].

MATERIALS
C .08
Table 2:

P .012

Mn .20

Si .27

S .001

Ni .025

Cr .020

Mo .10

Cu .018

Al .035

Nb .054

Ti .018

V .004

B < 0.0003

N .0044

Composition of Grade Steel API 5L X70 Base Plate in wt% (optical emission spectroscopy analysis) [42].

Designation E5-1

Commercial Name Bohler Thyssen Phoenix Cel 80

Grade E8 010-P1

Consumable Diameter (mm) 5

Batch Number (Year) 2113765 (2006)

Table 3:

Consumables Description [42].

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E5-1 Coating E5-1 Rod E5-1 Coating E5-1 Rod


Table 4:

C 13.7 0.065 Mo 0.063 0.007

P 0.015 0.010 Cu 0.007 0.014

Mn 9.2 0.710 Al 0.350 <0.001

Si 6.9 0.019 Nb 0.020 <0.001

S 0.007 Ti 9.400 <0.001

Ni 1.2 0.026 V 0.043 <0.001

Cr 0.049 0.043 B 0.170 <0.0005 N

0.0041

Composition of SMA Welding Consumables in wt% (optical emission spectroscopy analysis) [42].

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