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

IPC2012-90485

TENSILE AND FRACTURE PROPERTIES OF X80 STEEL MICROSTRUCTURES RELEVANT TO THE HAZ
Michael J. Gaudet University of British Columbia Vancouver, B.C., Canada ABSTRACT The girth welding of steel pipelines creates a substantial heat affected zone (HAZ) within the base pipeline steel. The HAZ can be considered to be a complex graded microstructure. While there is significant concern as to the fracture and mechanical properties of the HAZ as whole, detailed knowledge about the mechanical properties of the individual microstructures is lacking. For this study, X80 is heat treated in a Gleeble simulator to create samples of bulk microstructures with differing amounts and morphologies of bainite, ferrite and martensite-retained austenite (MA) with a total of 8 microstructures being investigated. The heat treatments were selected specifically to control the level of niobium in solid solution; that is to control whether niobium was fully in solution or contained mainly in niobium carbonitride precipitates. From the heat treated samples a matching tensile and fracture specimens were made. The strongest microstructure proved to be the finest bainitic microstructure, while the lowest strength microstructure was the coarsest bainite sample containing a significant amount of martensite-retained austenite connected along grain boundaries. The fracture behaviour at ambient temperature was studied using the Kahn tear test. The Kahn tear test is a machine notched, thin-sheet, slow strain rate fracture test which has the advantage of being a simple test to conduct. All Kahn tests failed in a ductile manner and it showed that the sample with the coarse bainite, with a connected martensiteretained austenite phase had the lowest unit propagation energy and tear strength while the fine, fully bainitic sample had the highest unit propagation energy and tear strength. Further investigation using SEM measurements of the final fracture surface from the tensile test to determine the tensile toughness. A comparison of the tensile toughness and unit propagation energies showed that there was a complex relationship between the two measurements. However, the samples which had the highest content of MA gave the in lowest unit propagation energy. Warren J. Poole University of British Columbia Vancouver, B.C., Canada

INTRODUCTION It is well established that there are economic advantages of operating natural gas pipelines with high strength steels (e.g. X80 and X100) which allow for higher operating pressures and/or larger diameters when compared to lower strength grades [1]. In the construction of pipelines, multipass metal arc welding is used to join sections of the pipe together. A consequence of the welding process is a region of the linepipe steel in which the microstructure changes significantly; this is the so-called heat affected zone (HAZ). In this region, the timetemperature profile (thermal cycle) that a given position experiences varies with the position relative to the weld fusion line [2]. Consequently a graded microstructure from the fusion line to the unaffected base material is seen. For a single pass of a weld torch, the microstructure can be classified according to the size of microstructural features seen. Close to the weld line is the coarse grain HAZ (CGHAZ) while the next closest is the fine grain HAZ (FGHAZ). In these regions the linepipe steel reaches fully austenitic temperatures, however only the CGHAZ sees significant austenite grain growth. This is important as the size of austenite grains influences both the coarseness of the final microstructure and the phase transformation upon cooling [2]. A very important factor in controlling austenite grain grow is the presence of precipitates which can pin grain boundaries. Many high strength linepipe steels contain niobium in the form of niobium carbonitride (Nb(C,N)) precipitates which may dissolve depending on the temperature and time that a given location in the HAZ experiences. [3-5]. It is worth noting that Nb solid solution level has recently been shown to strongly effect the decomposition of austenite upon cooling. Thus the stability of the Nb(C,N) precipitates, that is if they are in solid solution, will effect both austenite grain size and the final phase transformations in the CGHAZ and FGHAZ.

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For investigation of the mechanical property of real welds hardness profiles across the HAZ are typically used [2]. However hardness measurements provide limited information on yielding and work hardening behaviour. Fracture properties of real welds are typically studied using the Charpy V-notch impact test or the crack tip opening displacement (CTOD) test. It has been noted that placing a fatigue crack or notch into a specific subregion (such as the CGHAZ or FGHAZ) is difficult [2, 6-9]. In this study, mechanical and fracture testing is performed on a range of X80 microstructures produced using thermal simulation. Thermal simulation provides an effective means to isolate and produce bulk specimens suitable for tensile and fracture testing and is commonly used to produce HAZ microstructures [2, 10-18]. Typically, most studies attempt to simulate thermal cycles as experienced in the HAZ of an actual weld [10-18]. For this study, thermal cycles are applied to produce a range of microstructures that are relevant to the HAZ while also being designed to control the prior austenite grain size and the level of niobium in solid solution prior to austenite decomposition. EXPERIMENTAL PROCEDURE Microalloyed X80 linepipe steel supplied by Evraz Inc. NA. for this study. The chemistry is reported in Table 1. Table 1 Steel Chemistry (wt %) C 0.06 Mn 1.65 Nb 0.034 Mo 0.24 Ti 0.012 N 0.005

Samples were machined from the pipe to a size of 200mm X 50mm X 1.20mm. This thin strip design ensures a uniform microstructure is created through the cross section even during thermal cycles with significant heating and cooling rates. Thermal simulations were performed on a Gleeble 3500 thermo-mechanical simulator with cooling controlled by a helium gas quench. There are a total of eight thermal cycles used in this study. The thermal cycles produce a grain size of either 5 m or 42 m [19], with the Nb in Nb(C,N) precipitates or in solid solution upon final cooling, with continuous cooling rates of either 10 C/s or 50 C/s. These thermal cycles are shown schematically in Fig. 1. After the thermal simulation, electrical discharge machining (EDM) was used to produce a tensile and Kahn specimen from the original sample (see Fig. 2). The specimens length was aligned with the length of the strip samples. Samples for metallography were taken from the material between the edge of the fracture specimens notch and the tensile specimen. These were then polished and etched using a 2% Nital solution, and subsequently LePeras etchant and then examined using optical microscopy. Quantification of the microstructures was

Fig. 1 - Thermal cycles for (a) Nb in precipitates, 5m austenite grain size, (b) Nb in precipitates, 42 m austenite grain size, (c) Nb in solution, 5 m austenite grain size, (d)

Nb in solution, 42 m austenite grain size

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(a)

(b)

Fig. 2 Schematics of (a) subsized tensile and (b) Kahn specimens

accomplished using Nital etched images to determine the amounts of ferrite, granular bainite and upper bainite and LePera etched images to determine the amount of M/A (see reference [20] for details). Tensile tests specimens using subsized tensile specimens as shown in Fig. 2a. These tests were performed using an Instron 8872 testing machine with an applied strain rate of 2 x 10 -3 s-1. After testing, the final fracture area was measured using secondary electron imaging on a Hitachi S-2300 scanning electron microscope. This was used with the final load at fracture from tensile tests to calculate the true fracture strain and true fracture stress. Kahn tear testing, [21], was used to assess the fracture properties of the as-received material and the heat treated samples. The Kahn specimen (see Figure 2b) was pulled in tension at a continuous rate which results in the initiation and propagation of a crack. The Kahn test was used here as it is a simple test to perform, and its geometry is compatible with the material which can heat treated in a controlled manner in the Gleeble. The Kahn tests were performed with a crosshead displacement rate of 0.4 mm/min on a MTS 312.21 servohydraulic testing machine. Measurement of load line displacement was accomplished by attaching an extensometer to the pins passing through the specimens. In the processing of data, the pauses have been removed by fitting a high order polynomial to provide an accurate, continuous curve that is comparable to tests done without the interruptions. RESULTS The as-received microstructure is primarily acicular ferrite [19]. Optical images of the nital etched samples for thermal simulations where the prior austenite grain size was 5 m are

shown in Fig. 3. These microstructures are mainly ferritic with a small amount of granular bainite. The structure ofthe granular bainite for both Nb conditions is refined with increased cooling rate. The conditions with Nb in solid solution show more granular bainite and are slightly coarser than the cases with Nb precipited at the same cooling rate. Fig. 4 shows the optical images of the nital etched samples for the conditions with a prior austenite grain size of 42 m. For these samples, the cases with Nb in solid solution are seen to be fully upper bainitic, with the 50 C/s showing a more refined structure. Granular bainite is most significant for Nb precipitated cooled at 10 C/s while Nb precipitated cooled at 50 C/s has similar amounts of granular bainite and upper bainite. Fig. 5 shows the quantification of microstructural components. The engineering stress-strain curves of the heat treated samples are presented in Fig. 5. The use of subsized tensile specimens only affects the post necking results. The gauge length of 12.5 mm will result in a larger total elongation then would be reported in a standard ASTM tensile test with a 50 mm gauge length. Load-displacement curves from the Kahn test are shown in Fig. 6. To assist comparison between samples, the load in these plots have been normalized by the initial thickness of the sample while the displacement has been adjusted to have the peak load aligned to a displacement of zero. Tear strength of the Kahn test is calculated according to Eq. 1[21].

tear

4 Pmax bt

(1)

Where Pmax is the maximum load, t is thickness and b is the length of the initial uncracked ligament. The unit propagation energy (UPE) is a measure of the energy to propagate the crack across the entire ligament normalized by the initial cross-section area. The UPE reported here is taken from the loaddisplacement energy from peak load to one millimeter of displacement past the peak load and is termed UPEd0-1. Limiting the calculation of UPE to 1 mm past peak load minimizes the effect of sample buckling on the back side of the sample on this value. Fig. 8 is a plot of the UPEd0-1 versus tensile toughness. The tensile toughness is calculated by taking the area under the true stress / true strain curve up until the point of final fracture. To do so, the final true fracture strain and true fracture stress were determined using the fracture area measured from the SEM.Table 2 reports values from the tensile and Kahn tear tests.

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Fig. 3 - Nital etched microstructures of conditions of Nb in precipitates, austenite grain size of 5 m with cooling rates of (a) 10 C/s and (b) 50 C/s and of Nb in solution, austenite grain size of 5 m with cooling rates of (c) 10 C/s and (d) 50 C/s

Fig. 4 - Nital etched microstructures of conditions of Nb in precipitates, austenite grain size of 42 m with cooling rates of (a) 10 C/s and (b) 50 C/s and of Nb in solution, austenite grain size of 42 m with cooling rates of (c) 10 C/s and (d) 50 C/s

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Fig. 5 Microstructural constituents of the thermally treated samples

Fig. 6 - Engineering stress-strain curves for samples for (a) Nb in precipitates, 5 m austenite grain size, (b) Nb in precipitates, 42 m austenite grain size, (c) Nb in solution, 5 m austenite grain size, (d) Nb in solution, 42 m austenite grain size

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Fig. 7 Kahn normalized load versus adjusted displacement curves for samples for (a) Nb in precipitates, 5 m austenite grain size, (b) Nb in precipitates, 42 m austenite grain size, (c) Nb in solution, 5 m austenite grain size, (d) Nb in solution, 42 m austenite grain size

Fig. 8 - Kahn UPEd0-1 plotted versus tensile toughness taken from true stress-strain curve extended up to final failure

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Table 2 Mechanical and Fracture Test Results Test As-received 0.2% YS (MPa) 606 UTS (MPa) 692 Total 0.26 True, fracture 0.92 True, fracture (MPa) 1127 Tear (MPa) 1202 Tear / 0.2% YS 2.0 UPEd|0-1 (J/mm2) 0.26 0.26 0.28 0.24 0.25 0.25 0.27 0.26 0.30

Nb precipitated, 441 659 0.23 1.0 1266 1136 2.6 10 C/s, 5um Nb precipitated, 484 708 0.21 1.2 1619 1260 2.6 50 C/s, 5um Nb precipitated, 452 628 0.19 1.1 1405 1105 2.4 10 C/s, 42um Nb precipitated, 513 697 0.23 1.1 1389 1268 2.5 50 C/s, 42um Nb in solid solution, 455 669 0.27 1.4 1626 1177 2.6 10 C/s, 5um Nb in solid solution, 494 715 0.23 1.4 1852 1244 2.5 50 C/s, 5um Nb in solid solution, 546 693 0.17 1.3 1610 1241 2.3 10 C/s, 42um Nb in solid solution, 622 821 0.14 1.5 2310 1422 2.3 50 C/s, 42um Note that Total is larger here compared to regular tests due to the subsize gauge length, i.e. 12.5 mm vs. 50 mm DISCUSSION The temperature history at a given point in the HAZ of a multipass GMAW procedure is a complex function of the heat input conditions for the torch and the welding sequence. For example, a point in the HAZ may, on different passes, reach peak temperatures in the fully austenitic region. The multiple passes may lead to a different austenite grain size due to the cumulative effect of the passes on dissolving Nb(C,N) precipitates and thereby increasing grain growth in austenite due to a lowering of the pinning force from the precipitates and increasing the level of Nb solid solution level. The combination of these two factors (austenite grain size and Nb solid solution level) combine to lower the transformation start temperature which results in microstructures which have a higher amount of low temperature decomposition products. On the other hand, some regions of the HAZ may only have a single pass that reaches a peak temperature (900 oC) which just allows for full austenite formation. In this case, Nb primarily remains in the form of Nb(C,N) and the austenite grain size is small (typically 5 m or less). In order to fully understand the mechanical response of the material for all the cases, it is of value to examine the effect of microstructure on mechanical behaviour for material that has undergone idealized thermal paths, i.e. such as described in this work. As expected, there is a strong relationship between microstructure and mechanical properties. It can be seen that as the microstructure shifts from ferrite to granular bainite and then upper bainite, the yield and tensile strength increase. The formation of higher strength, lower temperature transformation products is favoured by niobium being in solid solution and a large austenite grain size. This type of scenario relates to the

CGHAZ in actual welds. For relatively high cooling rates (1050 C/s for this steel chemistry) which would be typical of the conditions one would expect for a single weld pass, the current work shows that the austenite decomposition products consist of predominately upper bainite and a relatively low fraction of MA i.e for a cooling rate of 10 C/s (see the nital etch in Figure 4c and the LePera etch in Figure 9b). A similar but somewhat finer microstructure is produced for a cooling rate of 50 C/s (Figure 4d). For both of these scenarios, a very good combination of mechanical properties is produced at ambient temperature, i.e. particularly for cooling rates of 50 C/s, a very high yield stress and UPEd0-1 were observed. This is consistent with the refinement of the microstructure and a low fraction of MA phase produced. On the other hand, when austenite decomposition occurs for scenarios where Nb is primarily in solid solution and a fine austenite grain size is observed, one obtains a large fraction of granular bainite or ferrite with the largest fractions of MA phase (for example, see Figure 9a). This type of scenario might apply when a given point was very close to the fusion line during a first weld pass (i.e. Nb precipitates are dissolved) and after decomposition of austenite, a subsequent pass where the peak temperature is just above the temperature necessary to fully form austenite. This appears to deleterious to ambient temperature properties, the yield stress is relatively low and the UPEd0-1 is also low. The case of Nb in solution, with a grain size of 42 m and cooling 10 C/s gives a comparable total elongation to the same condition with cooling at 50 C/s, both of which are significantly less than all other conditions.

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(a)

(b)

Fig. 9 LePera etched microstructures of cases with 42 m austenite grain and 10 C/s for (a) Nb in precipitates and (b) Nb in solid solution

in precipitates and an austenite grain size of 42 m produce microstructures that are susceptible to failure in the presence of the stress concentration, i.e. their tensile toughness values are high, but UPEd0-1 values are low. This attributed to the negative contribution of MA to void nucleation, growth and coalescence. According to Chen et. al., during ductile failure the stress concentrates on the boundary of MA causing it to crack or debond [22]. As these will form voids, higher amounts of MA in the matrix allow void coalescence to occur sooner and thus reduce the fracture resistance. It is also worth commenting on the relationship between the work of fracture determined by integrating the area under the true-stress true strain curve up to fracture with the UPEd0-1 determined from the Kahn tests, i.e. the data shown in Figure 8. At first, it might be expected that this would be strongly correlated since they are both measures of energy to fracture the material. Indeed, in Figure 8 it can be observed that there is a general trend of both measures increasing in a similar manner. However, there are clearly some microstructures where the UPEd0-1 is much lower than the tensile work of fracture. This appears to be the case for samples with a high fraction of the MA phase and where the MA phase is spatially distributed in along prior austenite grain boundaries (for example, see Figure 9a). Here, we speculate the much higher level of tensile triaxiality found in the Kahn test is promoting the nucleation, growth and coalescence of microvoids, thereby decreasing the resistance to crack propagation. Finally, it is worth emphasizing that all fracture tests conducted failed in a slow, ductile manner at ambient temperature. As such, the susceptibility of these microstructures to brittle failure has not been determined. Future work will involve repeating the tensile and Kahn tests in the temperature range of -20-30 oC to evaluate the effect of temperature on strength and fracture resistance. SUMMARY Microstructures of relevance to the HAZ of X80 steel produced by thermal simulations have been studied with respect to their mechanical behaviour and fracture properties. The lowest tensile strength, tear strength and UPEd0-1 is the case with Nb in precipitates, austenite grain size of 42 m with a cooling rate of 10 C/s. The case with Nb in solution, austenite grain size of 42 m with a cooling rate of 50 C/s proved to be the highest tensile strength, tear strength and UPEd0-1 microstructure tested. ACKNOWLEDGMENTS The authors would like to acknowledge NSERC (Canada), Evraz Inc. NA, and TransCanada PipeLines Ltd. for their support of this project. Jennifer Reicherts and Reza Taftehs microstructure characterization work has been of great use to this study.

From the Kahn tests, a similar pattern to that seen from the tensile tests emerges. The tear strength and UPEd0-1 are the highest for the condition with the greatest tensile strength, and lowest for the condition with the lowest tensile strength. These conditions are Nb in solution, 42 m austenite grain size with 50 C/s cooling and Nb in precipitates, 42 m austenite grain size with 10 C/s cooling rate respectively. While being the least ductile sample in tensile testing, the first cases good fracture properties can be expected by the fine bainite microstructure with almost no MA phase. In contrast, the second cases coarse granular bainite microstructure where the MA phase is found extensively throughout may explain the significantly poorer fracture properties of this condition. Fig. 9 shows LePera micrographs of Nb in precipitate and solution at 42 m austenite grain size and a cooling rate of 10 C/s. Fig. 8 shows significantly that the increase in cooling rate for a given condition generally correlates to an increase in both tensile toughness and UPEd0-1. It shows that the cases with Nb

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