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

Jennifer M. Reichert, Thomas Garcin, Matthias Militzer, Warren J. Poole The Centre for Metallurgical Process Engineering The University of British Columbia Vancouver, BC, Canada

ABSTRACT Linepipe steels are usually microalloyed with Nb to promote the formation of complex microstructures that lead to the required mechanical properties. In particular, Nb in solution affects significantly the austenite decomposition kinetics and the resulting microstructure. A systematic study has been carried out to quantify the influence of Nb on the austenite decomposition kinetics in X80 linepipe steel. Continuous cooling transformation tests were conducted with a Gleeble 3500. The transformation products include ferrite, granular and upper bainite and M/A (martensite/ retained austenite) constituents. For this study optical microscopy was used to investigate the formation of M/A constituents that critically determine the fracture toughness. A relation between M/A and the surrounding microstructure is observed. In combination with an existent model for the prediction of the microstructure evolution during weld thermal cycles, the area fraction, size and morphology of M/A can be predicted for the simulated HAZ, based on the prior austenite grain size, cooling rate and amount of Nb in solution.

INTRODUCTION Advanced high strength low alloy (HSLA) steels are designed to combine superior mechanical properties in terms of strength and fracture toughness with good weldability [1] [2] [3]. When pipe sections are girth welded in the field the heat affected zone (HAZ) experiences a rapid heat treatment cycle such that the resulting microstructure in the HAZ can deviate substantially from that of the base metal. Depending on peak temperatures reached and dwelling times austenite grain growth and dissolution of carbonitrides may occur [4]. Austenite grain size and the content of microalloying elements such as Nb in solution vary significantly across the HAZ and determine the austenite decomposition upon cooling and the resulting mechanical properties.

As the carbon content is low to have good weldability, microalloying elements such as Nb are used to create complex microstructures and to contribute to the strength of the material by transformation and precipitation hardening. In particular, Nb in solid solution shifts the austenite decomposition to lower transformation temperatures, promoting acicular ferrite and bainitic microstructures. Carbon enrichment results in areas of retained austenite at room temperature. The retained austenite partially transforms to martensite forming martensite/ austenite (M/A) particles [5] [6]. For steels containing overall carbon contents greater than 0.06 wt %, the carbon content in the M/A particles has been found experimentally to be about 1.1 1.3 wt % [7]. Arising from the brittle nature of martensite, M/A particles can significantly affect fracture toughness. Many attempts have been made to quantify the degradation of fracture toughness caused by M/A particles. It has been observed that not only the phase fraction is of importance, but also the M/A morphology [8]. Li and Baker [7] reported four different morphologies of M/A particles including blocky like particles, also described as islands [3] [9] [10], connected or nearly connected particles along prior austenite grain boundaries, elongated stringer particles along bainitic ferrite laths and M/A-C particles consisting of M/A and a second phase, i.e. carbide and ferrite. M/A islands were reported with sizes between 0.5 and 5 m and elongated particles were found with a length of up to 10 m and a width between 0.2 to 2 m [7] [9]. Considering the small size of the M/A particles the influence of other microstructure constituents can overlap or outweigh the influence of the M/A constituents [11]. In addition to cracks initiated by M/A constituents it is also reported that M/A particles can delay the growth of cracks, as shown by Li and Baker [7]. This observation indicates a very complex behavior of the influences of M/A particles on fracture toughness, which has not yet been entirely clarified. To describe the specific effect of M/A particles on mechanical properties in the HAZ, it is essential to carefully identify and

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characterize their appearance. A model has been established based on continuous cooling transformation (CCT) tests to predict the microstructure evolution in the HAZ as a function of Nb in solution, austenite grain size and cooling rate [12] [13]. In this study experimental results are presented showing a connection between the thermal cycle, the role of Nb in or out of solution and the resultant microstructure containing different amounts of M/A. These results can be used in combination with the existing microstructure evolution model to predict the fraction and size of M/A along the HAZ.

MATERIAL & EXPERIMENTAL PROCEDURE The material investigated in this study is a hot-rolled X80 linepipe steel supplied by Evraz Inc. NA (Regina, SK). The chemical composition is reported in Table 1 in terms of key alloying elements.
Table 1: Chemical composition of X80 (key alloying elements)

wt% at%

C 0.06 0.28

Mn 1.65 1.7

Nb 0.034 0.020

Ti 0.012 0.014

Mo 0.24 0.14

N 0.005 0.020

The as-received material mainly consists of irregular ferrite, including randomly distributed M/A islands and complex precipitates. The precipitates range in size from 3 to 100 nm and can be grouped into 4 categories: coarse TiN particles, small and large Nb(CN) precipitates and coarse Mo2C particles [4] [14]. A Gleeble 3500 thermo-mechanical simulator (Dynamic System Inc., Poestenkill, NY) was used to conduct CCT tests to produce various microstructures that are typical for the HAZ of welded pipelines. Austenite decomposition, i.e. transformation start temperature and transformation kinetics, was monitored by means of a mechanical contact dilatometer to measure the dimensional changes of tubular CCT specimens (8 mm outer diameter, 1 mm wall thickness, 20 mm length). Tests were conducted under high vacuum (1.3x10-3 Pa) and the temperature was measured and controlled by NiCr-Ni (type K) thermocouples at temperatures up to 1250 C and PtRh-Pt (type S) thermocouples at higher temperatures, spot welded to the sample center. The CCT tests were carried out for three different austenite grain sizes, i.e. 5 m, 26 m and 80 m (equivalent volume diameter) [15]. For the two smaller grain sizes, each test consisted of two thermal treatments. The first one being a solutionizing treatment to dissolve all Nb(CN) at 1300 C followed by a gas quench to room temperature. The second reheating was executed with a heating rate of 100 C/s, to maintain Nb in solution, to 950 C and 1250 C, respectively. The samples were then cooled rapidly at approximately 180 C/s to 900 C and CCT tests at cooling rates of 10, 30, 60 and 100 C/s were carried out either immediately or after a 20 min holding time to re-precipitate Nb. For the largest austenite grain size the samples were heated to 1350 C and

held for 35 s before they were cooled rapidly to 900 C. CCT tests were then, as in the other cases, carried out immediately or after a 20 min holding time at 900 C. Nine of the above mentioned thermal profiles were then selected for the current study to represent various regions of the HAZ from coarse grained to fine grained regions. The identification and quantification of different transformation products has been accomplished using samples etched with 2 % Nital solution. Manual point counting method according to ASTM E562-89 has been applied using a square grid superimposed on micrographs. The ratio of the grid points falling within a given phase to the total number of junctions provides the phase fraction. Le Pera etchant [16] containing equal volumes of 4 % picral and 10 % aqueous Na2S2O5 was applied to prepare samples for the analysis of M/A particles. This etchant reveals M/A particles white in a brown bainitic or ferritic matrix. Images were taken with an optical microscope applying a magnification of 500 times. Image analysis software was used to determine the area fraction, size and shape of M/A constituents. In a first step, the numerical images were transformed into a binary image and a threshold was applied to highlight the M/A constituents from the background. An ellipse was fitted to each particle, providing a major and minor axis. Particles touching the edge of the picture were not taken into account.

RESULTS & DISCUSSION Metallographic analysis of the microstructure resulted in the following phases being identified: ferrite, granular bainite, upper bainite and M/A. Optical micrographs of the simulated HAZ microstructures are shown in Figure 1. Samples are etched with 2 % Nital (a, c, e) and Le Pera (b, d, f), respectively. Figure 1 a and b show a ferritic microstructure formed from a prior austenite grain size of 5 m at a cooling rate of 10 C/s with Nb mainly precipitated. Figure 1 c and d show granular bainite formed at 10 C/s from an intermediate austenite grain size of 26 m with Nb in solution. Upper bainite is presented in Figure 1 e and f, resulting from continuous cooling at 30 C/s from large austenite grains, i.e. 80 m and Nb in solution.

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Figure 1: Optical microstructures obtained during CCT tests etched with 2 % Nital (a, c, e) & Le Pera (b, d, f)

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Table 2: Investigated cases representing the microstructure in the HAZ

GS [m] CR [C/s] Nb

a) 5 10 ppt

b) 5 30 ppt

C) 5 60 ppt

d) 26 10 sol

e) 26 30 ppt

f) 26 60 ppt

g) 26 30 sol

h) 80 30 sol

i) 80 60 sol

Based on the resulting transformation products nine thermal cycles were selected for this study. Table 2 displays the cases that were chosen to represent the HAZ, where ppt stands for Nb precipitated after 20 min. holding at 900 C and sol stands for Nb being entirely dissolved. The selected cases can be grouped into three categories based on the prevailing microstructure. The first category is a mostly ferritic structure formed from small prior austenite grains, i.e. 5 m with Nb mainly precipitated representing the fine grained HAZ (FGHAZ) far away from the fusion line. The second group consists of granular bainite, typical for a wide range along the HAZ where Nb can be in solution or partially precipitated. The third category is an upper bainitic structure typical for but not limited to the coarse grained HAZ (CGHAZ) close to the fusion line where Nb is entirely dissolved. Figure 2 shows the phase fraction of the transformation products resulting from continuous cooling in these selected cases.

Figure 3: Transformation start temperature as a function of the 3 microstructure categories defined above, representing typical HAZ microstructures

The area fraction of M/A particles with respect to the transformation start temperature is shown in Figure 4. Ferritic structures formed at temperatures between 670 and 620 C yield M/A fractions of 3 to 7 % whereas granular bainite accommodates 11 to 13 % of M/A. Upper bainite formed at temperatures lower than 550 C only allows for M/A fractions of approximately 3 %. The M/A fraction can be related to the transformation start temperature Ts (in C) by:
M/A 2 10.7 * exp (Ts 586 ) 2 648 3 (1) 1 exp( 0.14 Ts 85.82)

Figure 2: Area fraction of transformation products resulting from continuous cooling

Figure 3 shows the transformation start temperature resulting from each thermal cycle. As expected, a certain range of transformation start temperature can be attributed to each microstructure category. In the FGHAZ, the austenite decomposition starts with ferrite transformation at temperatures above 620 C. Granular bainite starts to form in the temperature range of 585 to 600 C. Close to the fusion line extensive austenite grain growth and Nb being dissolved shift the transformation start to a temperature range below 550 C.

as shown in Figure 4. Applying this relation to the HAZ of girth welded pipelines, a prediction of the M/A fraction can be made for any position along the HAZ. Close to the fusion line, a low fraction of M/A is expected in the upper bainitic structure. In an extended area between CGHAZ and FGHAZ the amount of M/A is found to be maximal (higher than 10 % area fraction). Far from the fusion line a reduced area fraction of M/A is found in the predominately ferritic microstructure.

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Figure 4: Influence of transformation start temperature Ts on M/A area fraction

When analyzing the appearance of M/A constituents it is of great importance to consider their size and morphology. Carbon enrichment plays an important role in the formation of M/A particles. As a limiting carbon concentration is reached the transformation ceases and the austenite is stabilized and remains untransformed. In the investigated steel grade, at cooling rates higher than 10 C/s ferrite only forms from a small austenite grain size, e.g. 5 m, representative of the FGHAZ. Regions of retained austenite result from the rejection of carbon through the / interface. As ferrite preferably nucleates from austenite grain boundaries and subsequently grows into the austenite grain the maximum carbon enrichment occurs within prior austenite grains resulting in blocky M/A islands. Prior austenite grain boundaries (PAGBs) are not visible in these ferritic structures. The maximum size and aspect ratio of M/A particles is smaller in the ferritic microstructure than in granular bainite or upper bainite. The M/A constituents are randomly distributed as illustrated in Figure 1 b. The number density of M/A particles is constant throughout each sample, while the average particle size is bigger for ferrite formed at a cooling rate of 10 C/s than for ferritic structures formed at higher cooling rates. In previous studies [7] [9] M/A islands were reported with sizes up to 5 m, which is in agreement with the current observations. During the formation of granular bainite carbon is partitioned from the bainitic ferrite and stabilizes the residual austenite resulting in a microstructure containing M/A particles dispersed in bainitic ferrite [17]. In addition PAGBs are decorated with M/A particles building a necklace structure, Figure 1 d. These particles form elongated chains which consist of long particles with lengths of up to 15 m or a combination of smaller particles. In this microstructure the majority of long particles are located along PAGBs while the remaining particles inside prior austenite grains can be grouped into small spherical particles randomly distributed and less frequent elongated particles.

Upper bainite forms at lower temperatures than granular bainite resulting in finer microstructural constituents and in an overall lower M/A fraction. The distribution of M/A constituents is less homogeneous in upper bainite and some areas appear to be clear of M/A under the optical microscope. PAGBs are partially decorated with M/A particles, Figure 1 f, where particles with a maximum length of 10 m are observed. Figure 5 shows the distribution of M/A particles located at PAGBs and inside prior austenite grains, respectively. There is no evidence of M/A constituents aligned at grain boundaries in ferritic microstructures. In granular bainitic structures PAGBs are mostly preserved and a certain amount of grain boundaries seems to be decorated with M/A constituents. While the overall M/A area fraction of the investigated granular bainitic cases varies between 11 and 13.3 % the amount of particles located at PAGBs is constantly determined to be 2.9 0.2 %. The finer scaled microstructure of upper bainite accommodates overall lower fractions of M/A constituents and varying amounts are found along PAGBs and inside PAGs depending on the thermal cycle.

Figure 5: Fraction of M/A particles inside PAGs and along PAGBs

The average particle size is obtained from the area of the ellipse fitted to each particle. The size of M/A particles along PAGBs can be related to the transformation start temperature during continuous cooling as illustrated in Figure 6. An increase in the transformation start temperature results in larger M/A particles along PAGBs. For the investigated cases the maximum average size of particles along PAGBs is 3.25 m2. The size increases by a factor of 4 from upper bainite formed at 508 C to granular bainite formed at 600 C.

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Figure 6: Particle size along PAGBs and inside PAGs

The dependence of the M/A particle size A (in m2) on the transformation start temperature Ts (in C) can be expressed as:

A 2 10 4 * exp(1.61 10 2 Ts )

also be found within grains. M/A at PAGBs is particularly prominent in granular bainite where the area fraction of these M/A particles is approximately 3 %. Further investigations are required to establish quantitative relationships to predict the fraction of M/A at PAGBs as a function of thermal cycles in the HAZ. Preliminary work suggests that it may be possible to relate the fraction of this component to the austenite grain size, at least in a first approximation. The proposed relation between the M/A area fraction and the transformation start temperature is designed to be incorporated into the phenomenological microstructure evolution model [12]. Similarly, the transformation start temperature can be used to distinguish between granular and upper bainite. Thus, Equation 1 for the MA fraction can be used as a pragmatic tool to also describe the transition from granular to upper bainite. The current results provide a first data set to quantitatively predict fraction, type, size, and morphology of M/A constituents as part of the microstructure evolution model along the HAZ. This microstructure prediction will be critical to describe the mechanical properties as a function of the distance from the fusion line.

(2) ACKNOWLEDGMENTS We acknowledge the financial support received from the Natural Sciences and Engineering Research Council of Canada, Evraz Inc. NA and TransCanada Pipelines Ltd. and Qatar National Research Found (QNFR) with gratitude.

The majority of M/A particles located inside PAGs are small spherical particles, resulting in an average size between 0.5 and 1.2 m2 and an average aspect ratio of 2.1 0.2 for all investigated cases. The elongated shape of particles forming a necklace structure results in an average aspect ratio of 3.0 0.1 for particles along PAGBs. The combination of the elongated shape and the formation of a network along the grain boundaries is assumed to be most detrimental to fracture properties of linepipe steels which is confirmed for a steel with similar chemical composition by Davis and King [6] [9].

REFERENCES [1] M. Zhao, K. Yang, and Y. Shan (2002), The effects of thermo-mechanical control process on microstructures and mechanical properties of a commercial pipeline steel, Materials Science and Engineering A, 335 (1-2), pp. 14-20 [2] W. Zhao, W. Wang, S. Chen, and J. Qu (2011), Effect of simulated welding thermal cycle on microstructure and mechanical properties of X90 pipeline steel, Materials Science and Engineering: A, 528 (24), pp. 7417-7422 [3] A. Lambert-Perlade, A. F. Gourgues, and A. Pineau (2004), Austenite to bainite phase transformation in the heataffected zone of a high strength low alloy steel, Acta Materialia, 52 (8), pp. 2337-2348 [4] M. Maalekian, R. Radis, M. Militzer, a. Moreau, and W. J. Poole (2012), In situ measurement and modelling of austenite grain growth in a Ti/Nb microalloyed steel, Acta Materialia, 60 (3), pp. 1015-1026 [5] S. Wang and J. R. Yang (1992), Effects of chemical composition, rolling and cooling conditions on the amount of martensite/ austenite (M /A) constituents formation in low carbon bainitic steels, Materials Science & Engineering A, 154, pp. 43-49

CONCLUSIONS Several observations have been made that characterize the fraction and shape of M/A particles in X80 linepipe steel samples that were obtained in CCT tests simulating typical conditions in the HAZ. The area fraction of M/A constituents can be related to the transformation start temperature of the austenite decomposition. In combination with an existent phenomenological model for the prediction of austenite grain growth, dissolution of precipitates and austenite decomposition into ferrite and bainite, the area fraction of M/A can be predicted as a function of the transformation start temperature. Granular bainite contains the highest area fraction of M/A particles, i.e. up to 12 %. Two types of M/A particles can be distinguished: M/A particles within prior austenite grains and M/A particles at prior austenite grain boundaries. The latter is observed in bainitic microstructures but not in ferrite. M/A particles located inside prior austenite grains are predominantly spherical whereas the particles along grain boundaries are mainly elongated with an aspect ratio of 3.0 0.1. Further, M/A particles along grain boundaries form a necklace structure and similar necklace-type arrangements can

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[6] Davis and J. E. King (1993), Effect of cooling rate on intercritically reheated microstructure and toughness in high strength low alloy steel, Materials Science and Technology, 9, pp. 8-15 [7] Y. Li and T. N. Baker (2010), Effect of morphology of martensiteaustenite phase on fracture of weld heat affected zone in vanadium and niobium microalloyed steels, Materials Science and Technology, vol. 26 (9), pp. 1029-1040 [8] Y. Li, D. N. Crowther, M. J. W. Green, P. S. Mitchell, and T. N. Baker (2001), The Effect of Vanadium and Niobium on the Properties and Microstructure of the Intercritically Reheated Coarse Grained Heat Affected Zone in Low Carbon Microalloyed Steels., ISIJ International, 41 (1), pp. 46-55 [9] C. L. Davis and J. E. King (1994), Cleavage Initiation in the Intercritically Reheated Coarse-Grained HeatAffected Zone: Part I. Fractographic Evidence, Metallurgical and Materials Transactions, 25, pp. 563-5673 [10] I. A. Yakubtsov and J. D. Boyd (2001), Bainite transformation during continuous cooling of low carbon microalloyed steel, Materials Science and Technology, 17 (3), pp. 296-301 [11] H. J. Chen, Y. Kituta, T. Araki, M. Yoneda, and Y. Matsuda (1984), Micro-fracture Behavior Induced by M-A constituents (Island Martensite) in Simulated Welding Heat Affected Zone of HT 80 High Strength Low Alloyed Steel, Acta Metallurgica, 32 (10), pp. 1779-1788 [12] In press: M. Militzer, M. Maalekian, T. Garcin, W. J. Poole (2011), Microstructure evolution model for the HAZ of girth welds in X80 linepipe steel, Rio Pipeline Conference 2011 [13] F. Fazeli, R. Tafteh, M. Militzer, and W. J. Poole (2011), Modeling the Effect of Nb on Austenite Decomposition in Advanced Steels, The international symposium on the recent developments in plate steels. Warrendale (PA): AIST [14] K. Banerjee, M. Militzer, M. Perez, and X. Wang (2010), Nonisothermal Austenite Grain Growth Kinetics in a Microalloyed X80 Linepipe Steel, Metallurgical and Materials Transactions A, 41 (12), pp. 3161-3172 [15] A. K. Giumelli, M. Militzer, E. B. Hawbolt (1999), Analysis of the Austenite Grain Size Distribution in Plain Carbon Steels, ISIJ International, 39 (3), pp. 271-280 [16] F. S. Lepera (1979), Improved Etching Technique for the Determination of Percent Martensite in High-Strength DualPhase Steels, Metallography, 12 (3), pp. 263-268

[17] H. K. D. H. Bhadeshia (2001), Bainite in Steels. H, 2nd Ed., Institute of Materials, London, p. 278

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