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

IPC2012-90388
Application of SEM-EBSD for Measurement of Plastic Strain Fields associated with Weld Metal Hydrogen Assisted Cold Cracking I.H. Brown , W.L. Costin , F. Barbaro and R. Ghomashchi
1 1 2 1

1- School of Mechanical Engineering The University of Adelaide Adelaide, South Australia, Australia 5005 2- Barbaro and Associates, CBMM Consultant, Wollongong, Australia

ABSTRACT The requirement for more efficient use of materials for pipelines has lead to the application of high strength low alloy steels such as X70 and X80 in pipelines. As the strength of these alloys has increased so has the risk of hydrogen assisted cold cracking (HACC). In Australia to minimize construction time, the root runs of girth welds are produced by shielded metal arc welding using cellulosic electrodes without either pre or post heating. Well defined welding criteria have been developed and are incorporated into the weld procedures for the elimination of HACC in the heat affected zone but the risk of cracking to the weld metal is still of concern. It has been reported that plastic deformation occurs prior to the formation of hydrogen cracks in weld metal. Therefore the evaluation of plastic strains at the micro- and nano-scale and their relationship to the weld metal microstructure could be of great significance in assessing the susceptibility of welds to weld metal hydrogen assisted cold cracking (WMHACC). A method for analysing plastic strains on the micro- and nano-scales using electron backscattered diffraction (EBSD) has been developed. This technique is based on the degradation and rotation of diffraction patterns as a result of crystallographic lattice distortion resulting from plastic deformation. The analysis can be automated to produce an Image Quality (IQ) map in order to relate the spatial distribution of plastic deformation to microstructural features e.g. grains or cracks. The development and assessment of techniques using Scanning Electron Microscopy (SEM) and EBSD for the determination of local plastic strain distribution in E8010 weld metal used for the root pass of X70 pipeline girth welds is discussed. INTRODUCTION Hydrogen Assisted Cold Cracking (HACC) also referred to as delayed cracking or cold cracking is a welding defect shown

by the appearance of cracks which may occur in the heat affected zone (HAZ) of the base metal or the weld metal (WM) [1, 2]. The greatest risk of HACC occurs when the weld cools down to temperatures below about 200C. Above this temperature range, cracking is unlikely to initiate in ferritic structural steels [1, 3]. Of all the imperfections which may occur in welds HACC is reported to be by far the most dangerous. It is known to be the defect with the most serious consequences and the least chance of detection [4]. 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. 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 [4] as illustrated in Figure 1. HAZ
API 5L X70

WM

Figure 1:

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

This represents a very serious problem for industry, because most of the predictive methods are intended for

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prevention of HACC in the HAZ of the base metal, not in the weld metal [5]. There is a general agreement that HACC in HSLA steel welds only occurs if all of the following conditions are present simultaneously [1, 6, 7]; i. a susceptible microstructure. ii. a stress intensity of sufficient magnitude. iii. a critical concentration of diffusible hydrogen. These interrelated conditions are the basic factors for various mechanisms which have been proposed to explain the phenomenon of HACC in metals. 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 iv. reduction or enhancement of dislocation mobility due to the presence of hydrogen However, whilst comprehensive literature has been devoted to the general effects of hydrogen on plastic deformation and crack propagation, the influence of the microstructure still remains unclear [8-14]. Electron backscattered diffraction (EBSD) provides an opportunity to relate the spatial distribution of plastic deformation to microstructural features in a wide variety of materials [15-18]. In the case of WMHACC the application of this technique seems particularly useful for investigating the relationship between microstructure, plastic deformation, crack initiation and the crack propagation path. The current work has shown that this technique is suitable for determining the spatial distribution of plastic strain in relation to the microstructure. Future work will utilise this technique through in-situ SEM/EBSD observations of slow strain rate tensile tests on hydrogen charged and uncharged weld metal samples. This should provide an insight into effect of hydrogen on the relationship between plastic strain, microstructure, crack initiation and propagation. HYDROGEN ENHANCED LOCALIZED PLASTICITY Models based on the reduction or enhancement of dislocation motion assume that hydrogen affects the mobility of dislocations which in turn affects the fracture behavior of materials by changing the extent and character of plasticity. On one hand it has been suggested that hydrogen diffuses into the dilation zone of dislocations producing Cottrell atmospheres which reduce the mobility of dislocations [19] . This process reduces the plasticity of the material ahead of the crack tip and makes deformation at the crack tip more difficult. The crack then propagates in a brittle manner at low levels of applied load. [20]. On the other hand the Hydrogen Enhanced Localized Plasticity (HELP) model [9] proposes that hydrogen increases

dislocation mobility. This model is based on experimental studies undertaken by Beachem [8], and suggests that hydrogen decreases the barrier to dislocation movement resulting in a smaller flow stress and easier local plastic deformation. The increased mobility of dislocations is due to a reduction in the elastic strain fields in the dilation region of dislocations as a result of the diffusion of hydrogen to these regions. Providing the strain rate is low enough and the temperature high enough to enable the hydrogen to move with the dislocation, the reduction in the elastic strain fields reduces the interaction of dislocations with other dislocations or obstacles enabling dislocations to move at lower stress levels. Although there is a characteristic loss of ductility associated with hydrogen embrittlement on the macroscopic scale, this does not preclude significant localized plasticity on a microscopic scale as described. On a microscopic scale localized plastic deformation has been confirmed by transmission electron microscope (TEM) observations (Figure 2) [21]. The sample was imaged in a TEM and showed enhanced movement of the dislocations after the sample was exposed in an atmosphere of hydrogen.

Figure 2:

Image formed by superimposing an image from a pile-up of dislocations against a grain boundary in vacuum (black numbers and dislocation lines),and an image taken from the same pileup at constant stress, after introduction of 95 torr of hydrogen gas in an environmental cell (white numbers and dislocation lines) [21].

Several authors have made direct observations of WMHACC. Savage [14] was the first to employ a direct observation technique of weld metal cold cracking with an optical microscope, and noted the importance of plastic deformation on a macroscopic scale prior to cracking. However, magnification and depth of focus with optical microscopy were inadequate for a detailed analysis. Later, Scanning Electron Microscope (SEM) observations [11] confirmed the relationship between regions of intense plastic deformation and the crack site by the detection of slip bands during in-situ mechanical bending. Figure 3 is a schematic depiction of the process of crack initiation and propagation in a weld as observed by Matsuda [11]. The broken lines highlight regions of intense plastic strain which were detected by SEM observations. Initially, at the root of the weld which acts like a

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notch, a region of intense plastic strain forms in two directions (stage I). A microcrack then forms within the highly strained region (stage II). As the crack propagates a new crack is initiated ahead of the initial crack but still within the highly strained region (stage III). The process is repeated as the crack continues to grow (stages IV and V), until the cracks finally join up to form one macrocrack (stage VI).

into low angle dislocation boundaries separating almost dislocation-free regions with near perfect lattices into subgrains or subcells [22]. If the subgrain size is within the spatial resolution of the SEM and EBSD system, the resultant small changes in orientation may be revealed. Typical values for misorientation resolution using standard EBSD platforms are of the order of 0.5 [15]. One approach for revealing plastic strain is based on the change in the diffraction pattern due to local misorientation between subgrains caused by plastic deformation of the material [18]. The rotation of the diffraction pattern from one subgrain to another within the diffraction volume, results in a degradation of the diffraction pattern as shown in Figure 4. Because of rotations associated with these subgrains, the material within the diffraction volume will no longer meet a specific Bragg condition, but rather a range of near Bragg conditions in three dimensions. This results in a diffraction pattern with degraded contrast (Figure 5). The degree of degradation is dependent on the amount of deformation within the interaction volume.

Figure 3:

Macroscopic mode of crack initiation and propagation. Broken lines outline regions of intense plastic strain [11].

MAPPING PLASTIC DEFORMATION USING EBSD The capabilities of automated Electron Backscatter Diffraction (EBSD) for analysing and quantifying the crystallographic aspects of microstructures have been well documented for a wide variety of materials and applications [15]. EBSD has been used for revealing the spatial distribution of regions of plastic strain related to HACC crack paths in X46 line pipe [16]. The results of that work suggested the feasibility of improving the HACC resistance of pipeline steels through crystallography, texture control, and grain boundary engineering. By utilising a similar method to relate the spatial distribution of plastic deformation to the weld metal microstructural features and their effect on HACC crack initiation and propagation, it is anticipated that improvements to the resistance of weld metal to HACC can be achieved. Intragranular lattice rotation is a common response of many polycrystalline materials to plastic deformation. During plastic deformation line defects (dislocations) are introduced into the lattice of each grain. These defects organize themselves

Figure 4:

Local misorientation in the lattice caused by the formation of subgrains and grain boundaries results in a rotation of the EBSD pattern [18].

Pattern quality degredation

Figure 5:

The pattern rotation as shown in Figure 4 will result in a degradation of the pattern quality. [18].

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The current article is to report on the initial findings of employing EBSD technique to determine the local plastic strain distribution in E8010 weld metal used for the root pass of X70 pipeline girth weld. EXPERIMENTAL PROCEDURE AND RESULTS A transverse cross section of a sample of a shielded metal arc (SMA) weld was examined (Figure 6). The composition of the parent plate and the composition and description of the cellulosic SMA welding consumable (E5-1) are given in Tables 1, 2 and 3 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. After sectioning, the sample was mounted in Bakelite. Because of the sensitivity of the EBSD technique to specimen preparation artifacts and surface defects, automated sample preparation was used for grinding and polishing. To avoid contamination or oxidation, the samples were placed in the specimen chamber of a dual beam focused ion beam scanning electron microscope immediately after polishing,

FSE detector

Figure 7:

Fore-scatter electron (FSE) detector mounted on a planar, rectangular scintillator EBSD detector [15].

Figure 8 is a fore scatter electron image (FSE) of the selected area of Figure 6. The region outlined in Figure 8 shows the formation of two disconnected cracks. Each crack is growing by micro-void coalescence which requires high degree of plastic deformation as suggested by Beachem [8]. The second shorter crack is forming below and to the left of the larger crack as predicted by Matsudas crack growth model previously mentioned. Matsudas model also predicts that the region between the two cracks will be a region of higher plastic strain.
Micro-voids

Figure 6:

Cross section of the selected sample after polishing Solid bridge between cracks

As EBSD measurements require a large tilt angle between the sample and the primary beam, the resulting secondary electron images of the sample surface are distorted and require digital tilt correction. However, the fore scatter electron detector is mounted directly on the EBSD detector (Figure 7) and can therefore produce high quality images that rival those obtained from a secondary electron detector, but without distortion.

Figure 8:

Fore-scatter electron image of two cracks observed in the weld metal.

An EBSD scan of the region outlined in (Figure 8) was collected and the data processed to create an Image Quality (IQ) map from the diffraction patterns. As noted in Figure 4, the

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rotation of the EBSD pattern due to subgrain formation (plastic strain) results in the degradation of the diffraction pattern (Figure 5). The greater the density of these subgrains, the greater the degradation and the darker these regions appear in an IQ map. The IQ map shows the high angle grain boundaries and the subgrain boundaries within these grains. Therefore it reveals the spatial plastic strain distribution within the grains. Such conclusion is arrived at Figure 9 if the highlighted region in Figure 8 is compared with the same region in the IQ image (Figure 9). The darker area in Figure 9 is an indication of high plastic strain in this region resulted from EBSD pattern quality degradation due to plastic strain.

hydrogen charged and uncharged weld metal samples. This should provide an insight into the effect of hydrogen on the relationship between plastic strain, microstructure, crack initiation and crack propagation. 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 and Mr. L. Fletcher for useful discussion and constructive comments. Special thanks are also due to Adelaide Microscopy, its director Mr. John Terlet and technical advice from Mr. Leonard Green. REFERENCES [1] Yurioka, N., 1990, "Hydrogen Assisted Cracking in C-Mn and Low Alloy Steel Weldments," International Material Reviews, 35(4). [2] Fletcher, L., 2000, "A Holistic Model of Hydrogen Cracking in Pipeline Girth Welding," Welding in the World, London, 44(2), pp. 7. [3] Coe, F. R., 1973, Welding Steels without Hydrogen Cracking / by F. R. Coe, Welding Institute, Cambridge :. [4] Fletcher, L., 1999, "Weld Metal Cracking in Pipeline Girth Welds," International Conference on Weld Metal Hydrogen Cracking in Pipeline Girth Welds, Wollongong, Australia. [5] Yurioka, N., 1999, "Predictive Methods for Prevention and Control of Hydrogen Assisted Cold Cracking," Proc. Weld Metal Hydrogen Cracking in Girth Welds Wollongong. [6] 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. [7] 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. [8] Beachem, 1972, "A New Model for Hydrogen Assisted Cracking," Metallurgical Transactions 3( [9] Birnbaum, H. K., and Sofronis, P., 1994, "HydrogenEnhanced Localized Plasticity--a Mechanism for HydrogenRelated Fracture," Materials Science and Engineering: A, 176(1-2), pp. 191-202. [10] Lynch, 1989, "Metallographic Contributions to Understanding Mechanisms of Environmentally Assisted Cracking," Metallography, 23(2), pp. 147-171. [11] Matsuda, 1981, "Sem Dynamic Observation of HydrogenInduced Cold Cracking in Weld Metal of 80kg/Mm2 Class Steel," Transactions of JWRI.

Darker regions indicate areas of high plastic strain between the cracks and voids.

Figure 9:

IQ map of the region shown in Figure 8 reveals the microstructure and the enhanced strain intensity connecting between the cracks.

Several points should be noted from the IQ map of Figure 9. The microstructure is predominantly acicular ferrite and the grain boundaries of the acicular ferrite are clearly defined. In addition the highly strained bridges between the voids evident in Figure 8, now appear dark because of the pattern degradation in these highly plastically deformed regions. CONCLUSIONS AND FUTURE WORK The feasibility of employing an EBSD technique for mapping local plastic strain distribution in the vicinity of weldmetal HACC has been demonstrated in an X70 line pipe girth weld. The application of this technique enabled further confirmation of the model proposed by Savage and later by Matsuda. Future work will utilise this technique through in-situ SEM/EBSD observations of slow strain rate tensile tests on

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[12] Robertson I.M, 2001, "The Effect of Hydrogen on Dislocation Dynamics," Engineering Fracture Mechanics, 68(6), pp. 671-692. [13] Robertson, I. M., and Birnbaum, H. K., 1986, "An HVEM Study of Hydrogen Effects on the Deformation and Fracture of Nickel," Acta Metallurgica, 34(3), pp. 353-366. [14] Savage, 1978, "Hydrogen Induced Cracking in Hy-130 Steel Weldments " Welding Journal, 57(pp. 118-126. [15] Adam J. Schwartz, M. K., Brent L. Adams, David P. Field, 2009, Electron Backscatter Diffraction in Material Science, Springer Science+Business Media, New York. [16] Venegas, V., Caleyo, F., Gonzlez, J. L., Baudin, T., Hallen, J. M., and Penelle, R., 2005, "EBSD Study of Hydrogen-Induced Cracking in Api-5L-X46 Pipeline Steel," Scripta Materialia, 52(2), pp. 147-152. [17] Venegas, V., Herrera, O., Caleyo, F., Hallen, J. M., and Baudin, T., 2010, "Crystallographic Texture Control Helps Improve Pipeline Steel Resistance to Hydrogen-Induced Cracking," 2, pp. 555-561. [18] Wright, S. I., Nowell, M. M., and Field, D. P., 2011, "A Review of Strain Analysis Using Electron Backscatter Diffraction," Microscopy and Microanalysis, 17(03), pp. 316329. [19] Smialowski, M., 1962, Hydrogen in Steel, Pergamon Press. [20] Boellinghaus, T., 2001, "Numerical Modelling of Hydrogen Assisted Cracking," NACE International. [21] Ferreira, P. J., Robertson, I. M., and Birnbaum, H. K., 1998, "Hydrogen Effects on the Interaction between Dislocations," Acta Materialia, 46(5), pp. 1749-1757. [22] Jakobsen, B., Poulsen, H. F., Lienert, U., Almer, J., Shastri, S. D., Srensen, H. O., Gundlach, C., and Pantleon, W., 2006, "Formation and Subdivision of Deformation Structures During Plastic Deformation," Science, 312(5775), pp. 889-892. [23] 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 MATERIALS
C 0.08 P 0.012 Mn 1.20 Si 0.27 S 0.001 Ni 0.025 Cr 0.020 Mo 0.10 Cu 0.018 Al 0.035 Nb 0.054 Ti 0.018 V 0.004 B <0.0003 N 0.0044

Table 1:

Composition of Grade Steel API 5L X70 Base Plate in wt% (optical emission spectroscopy analysis) [23].

Designation

Commercial Name

Grade

Consumable Diameter (mm) 5

Batch Number (Year)

E5-1

Bohler Thyssen Phoenix Cel 80

E8010-P1

2113765 (2006)

Table 2:

Consumables Description [23].

C E5-1 Coating E5-1 Rod Mo E5-1 Coating E5-1 Rod 0.007 0.063 0.065 13.7

P 0.015

Mn 9.2

Si 6.9

S -

Ni 1.2

Cr 0.049

0.010

0.710

0.019

0.007

0.026

0.043

Cu 0.007

Al 0.350

Nb 0.020

Ti 9.400

V 0.043

B 0.170

0.014

<0.001

<0.001

<0.001

<0.001

<0.0005

0.0041

Table 3:

Composition of SMA Welding Consumables in wt% (optical emission spectroscopy analysis) [23].

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