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

IPC2012-90064

DEVELOPMENT OF MODERN HIGH STRENGTH HEAVY PLATES FOR LINEPIPE APPLICATIONS

Heike Meuser , Florian Gerdemann, Fabian Grimpe Salzgitter Mannesmann Grobblech GmbH Wiesenstrasse 36 45473 Mlheim, Germany 1 Contact Author Charles Stallybrass Salzgitter Mannesmann Forschung GmbH Ehinger Strae 200 47259 Duisburg, Germany
1

ABSTRACT High strength linepipe steels have to fulfil increasing property demands in modern pipeline applications. The transport of large gas volumes at high pressures from remote areas to the market is achieved in the most economical way by large diameter pipelines. For the last 30 years, high strength heavy plates for pipes and pipe bends were developed and produced at Salzgitter Mannesmann Grobblech. These products were steadily improved for example in terms of toughness and fracture behaviour at low temperatures. This is a strong focus of materials development around the world. Modern high-strength heavy plates used in the production of UOE pipes are generally produced by thermomechanical rolling followed by accelerated cooling (TMCP). The combination of high strength and high toughness of these steels is a result of the bainitic microstructure realised by TMCP and are strongly influenced by the rolling and cooling conditions. This paper gives an overview of the development of high strength plates for line pipe application at Salzgitter Mannesmann Grobblech. From comparably thin-walled X80 plates with no or medium DWTT requirements to recent requirements for approx. 28 mm thick X80 plates with requirements of 75/85% shear area fraction at -30C and more than 250 J Charpy energy at -40C the development work and the result of the last five years are described and presented. Classical light-optical characterisation of the microstructure of these steels is at its limits because the size of the observed features is too small to allow reliable quantitative results. Therefore Salzgitter Mannesmann Grobblech and Salzgitter

Mannesmann Forschung (SZMF) developed alternative methods with the aim of a quantification of microstructure features and a correlation of those with the mechanical properties and processing conditions. In several investigations, the information is related to the mechanical properties of the plate material. It was found that a variation of the processing conditions has a direct influence on parameters that are accessible through the EBSD method and correlates with mechanical properties. The detailed correlations vary depending on steel grade and TMCP strategy. The results have to be carefully interpreted and help understanding the connection between processing and properties. Consequently this can be used as valuable input for the definition of the processing window for heavy plate production with optimized properties. INTRODUCTION Salzgitter Mannesmann Grobblech GmbH (SMGB), a member of the Salzgitter group, operates a 5.1-meter heavy plate rolling mill which is specialised in the production of plate for pipe. More than 90 percent of its approximately 800,000 tons annual plate production is delivered to large diameter pipe mills all over the world. The most important and biggest customer is the German pipe producer EUROPIPE which is a joint venture of the two steel manufacturers Salzgitter and Dillinger Htte. Forced by the market demand for high strength arctic linepipe steels, SMGB developed and improves ultra high strength heavy plates in cooperation with the customers. All important steps of this development take place integrated within

Copyright 2012 by ASME

companies that are members of the Salzgitter group: the steel is produced at Httenwerke Krupp Mannesmann (HKM), the plates are rolled at SMGB, the pipes are manufactured at EUROPIPE, bends can be manufactured at SMGBs own pipe bending plant. Last but not least, the whole research and development for this production chain is performed in cooperation with Salzgitter Mannesmann Forschung (SZMF) which is the development centre of the Salzgitter group. The development of microalloyed steels for linepipe applications is a focus of research efforts of SMGB/SZMF. The research centre is equipped with the facilities to produce laboratory heats of up to 300 kg by vacuum induction melting and to perform thermomechanical rolling trials with accelerated cooling using two hot rolling mills. The typical weight of ingots used for heavy plate development is 100 kg. These ingots can then be divided into several coupons making it possible to investigate a broad range of compositions and processing parameters, in order to identify ideal rolling parameters for industrial scale rolling trials. An extensive database of results of rolling trials has been gathered, ranging up to the X120 strength level. The analysis of these data and of results of heavy plate production forms the basis for the optimisation and development of new processing strategies. This is complemented by numerical tools that are used for alloy design. Since the beginning of the 1980s, plates, pipes and pipe bends of steel grade API X80 were developed and produced at SMGB and have become daily business. In recent years, the complexity of requirements for line pipe materials has increased steadily with regard to toughness and weldability. For this reason, the X80 products were steadily improved by development along the entire process chain. Figure 1 gives an impression of the produced tonnage of heavy plates up to date in API Grade X80. In the beginning of the 1990s, both partners (SMGB and Europipe) started to work on the development of API X100 plates and pipes. While X80 today is daily business for both companies, X100 plates and pipes were only produced on a trial scale up to now. Some 1000 tons of X100 plates and pipes of different dimensions were manufactured so far.

width was 4470mm which corresponds to a 56 inch pipe.

25-29,9mm; 180,67kt

20-24,9mm; 112,53kt 15-19,9mm; 30,41kt

10-14,9mm; 32,35kt

30-34,9mm; 2,05kt 35-39,9mm; 0,06kt >=40mm; 0,18kt

Figure 2: Thickness distribution of X80 plates produced at SMGB

The first SMGB X80 plates were developed and produced according to specifications with a focus on elevated strength level with no special requirements on base-material toughness or heat-affected zone toughness. During the 25 years of development, however, more and more emphasis was laid on toughness behaviour [1-3]. Since 2002, SMGB has produced X80 plates above 25mm wall thickness, which poses an additional challenge compared to the first X80 plates with lower wall thickness. The toughness development for these plates since 2002 is illustrated in Figure 3 and 4. The requirements regarding minimum Charpy impact energy as well as the shear area fraction in Battelle drop-weight-tear tests increased constantly. The Charpy impact energies in Figure 3 show that the energy in the upper shelf reached values of approximately 230 to 250 J down to a test temperature of 10C in the period from 2002 to 2006. In 2007, the determined upper shelf energy was 270 J and in 2008 more than 300 J were achieved. At the same time, the upper shelf was extended to -40C in 2007 and finally to -50C in 2008. Recent results from production even reached an upper shelf energy of 450 J up to a testing temperature of -60C.

Figure 1: Development of X80 production at SMGB

Figure 3: Development of Charpy properties and requirements for SMGB X80 plates since 2002 (plate thickness from 25 to 30 mm)

The thickness range of X80 plates produced at SMGB, see Figure 2, varied from 10mm to 40mm, while the maximum

A similar trend can be seen in the development of the shear area fraction of the BDWT-test results, which shows that the temperature for 85 % of shear area fraction decreased from 0C

Copyright 2012 by ASME

in 2002 to -20C in 2006 to -40C, which was reached in 2008. In 2009, it was possible to extend the range for 85% shear area fraction even to a temperature of -50C (Figure 4).

Light-optical microscopy offers only limited possibilities for quantitative characterisation of the microstructure because of the low size of the features that have an influence on mechanical properties and the limited resolution. Scanning electron microscopy (SEM) with its inherent higher resolution is far better suited to characterise such microstructures, as illustrated in Figure 6. The image in Figure 6 which was taken at a magnification of 20,000:1 shows carbon-rich constituents that were found to be finely dispersed in the microstructure of high-strength heavy plate material.

Figure 4: Development of BDWTT requirements for SMGB X80 plates since 2002 for a plate thickness from 25 to 30 mm

These challenging requirements were met by constant material and process development while the alloying content was reduced at the same time. This reduction improved the weldability of the plate material and allowed material costs to remain in a reasonable range. The Effect of Processing Conditions on the Texture and Low Temperature Toughness The processing strategy of SMGB for the production of X80 with excellent low-temperature toughness consists of thermomechanical rolling above the Ar3-temperature followed by accelerated cooling (TMCP). The microstructure that is typically obtained using this procedure consists predominantly of bainite with a volume fraction of 80% or higher and minor volume fractions of ferrite and martensite, as shown exemplarily in the light-optical micrograph of a production sample in Figure 5. The resulting grain size is in the range of 25 m.

Figure 6: Microstructure of an X80 plate at a magnification of 5,000:1 (top) and carbon-rich constituents at a magnification of 20,000:1 (bottom) obtained by scanning electron microscopy

Figure 5: Typical microstructure of an X80 heavy plate at a magnification of 500:1 obtained by light-optical microscopy

Because of the lower solubility in the bainite, carbon is redistributed to the austenite during the phase transformation. This leads to a significant local enrichment of carbon which can stabilise the austenite down to room temperature or lead to the formation of martensite or high-carbon bainite. If these carbonrich regions are distributed homogeneously and remain small, they do not lead to a reduction of the toughness of the plate material. In addition to microstructure characterisation by SEM, the use of electron backscatter diffraction (EBSD) has gained

Copyright 2012 by ASME

increasing significance for the characterisation of the microstructure of bainitic steels in the last years, see e.g. [4-6]. The EBSD method provides information on the local crystal orientation. By generating a map out of EBSD spot measurements, the orientation differences or misorientations can be calculated. This makes it possible to determine the local misorientation and locate grain boundaries. This method is used extensively to characterise the microstructure of high-strength steels, and to correlate the results with the mechanical properties, see e.g. [5, 6]. EBSD measurements can also be used to characterise the crystallographic texture of a steel sample. In the present case, the measurements used for texture investigations were carried out with a step size of 2.5 m over an area of 600x600 m2 and were aimed at analysing the effect of processing parameters on texture using orientation distribution functions (ODF). It has been reported, that a high volume fraction of grains with a texture close to the rotated cube texture {001}<110> has a negative effect on the toughness and the formation of separations [7-10]. TM processing parameters were, however, not discussed in these investigations. In an earlier investigation, it has been found that texture differs significantly if the final rolling temperature is above or below the Ar3-temperature and is more pronounced for final rolling temperatures in the twophase region [7]. For this reason, samples taken from laboratory trials in which the processing parameters were varied were investigated. In these laboratory trials, plates were rolled in the laboratory on a two-high rolling mill to a final wall thickness of 27 mm, followed by accelerated cooling. The composition of the lab material produced by vacuum induction melting is given in Table 1. The intermediate thickness (IT), the final rolling temperature (FRT) and the cooling stop temperature (TCS) were varied in order to investigate the effect on mechanical properties. The intermediate thickness was increased from IT1 to IT2 by 20%. The final rolling temperature was increased from FRT1 to FRT2 by around 20 K. Both were selected above the temperature of the onset of the austenite to ferrite transformation in order to ensure a predominantly bainitic structure after accelerated cooling. The cooling stop temperature increased from TCS-1 to TCS-2 by roughly 100 K. In addition, the microstructure of the sample taken from X80 production at SMGB was investigated.
Table 1: Composition of the investigated lab material Composition , wt.% C Si Mn Lab. mat. <0,05 0,20 1,8 Others Cu, Ni, Mo Nb 0,050 Ti 0,02 CE IIW 0,44

were only found in pressed-notch Battelle drop-weight-tear (DWT) tests at -20C in transverse direction using specimens with the full wall thickness. In these tests, both the shear area and the total energy were evaluated. The variation of the processing conditions was found to affect the DWT test results significantly. In order to ensure arrest of long-running ductile cracks, a combination of high shear area and total energy is desirable [10]. The best combination of both parameters was realised for the lower final rolling and cooling stop temperature at both intermediate thickness levels (FRT1 and TCS1), as shown in Figure 7. These results of the laboratory trials were used as a basis for the industrial scale rolling trials at SMGB [6, 11].

Figure 7: Effect of the variation of processing parameters on the shear area and total energy in the DWT test

The Effect of Processing Conditions on the Texture and Low Temperature Toughness The EBSD method provides information on the local crystal orientation. By generating a map out of EBSD spot measurements, the orientation differences or misorientation can be calculated. This makes it possible to determine the local misorientation and locate grain boundaries. This method was used to characterise the microstructure of high-strength steels and to correlate the results with the mechanical properties, see e.g. [5, 6]. EBSD measurements can also be used to characterise the crystallographic texture of a steel sample. In the present case, the measurements used for texture investigations were carried out at the mid-wall position with a step size of 2.5 m over an area of 600x600 m2 and were aimed at analysing the effect of processing parameters on texture using orientation distribution functions (ODF). It has been reported, that a high volume fraction of grains with a texture close to the rotated cube texture {001}<110> has a negative effect on the toughness and the formation of separations [7-10]. TM processing parameters were, however, not discussed in these investigations.

Materials testing showed that the variation of processing parameters in the laboratory trials did not have a significant effect on tensile properties or the Charpy impact energy. The yield strength was around 550 MPa and the tensile strength was around 620 MPa. The Charpy impact energy was around 300 J down to a temperature of -80C. Differences between the plates

Copyright 2012 by ASME

In laboratory trials that were carried out with the aim to find optimum processing conditions for the production of X80 plate material with excellent low-temperature properties in the drop weight tear (DWT) test, the best results were obtained at final rolling temperatures (FRT) slightly above the Ar3-temperature, while higher final rolling temperatures led to a lower shear area [11]. An increase of the reheating temperature was also found to have a detrimental effect on DWT-test properties. This is believed to be related to a higher austenite grain size prior to rolling below the non-recrystallization temperature which affects the grain size in the final product. Texture investigations showed that the improvement in toughness was a result of a reduced volume fraction of the {001}<110> rotated cube texture component [8]. Based on these trials, the processing window for heavy plate production at SMGB was modified and the texture of X80 heavy plate material with a wall thickness of 23.8 mm and 27.7 mm was subsequently investigated. A comparison of the ODF at 2=45 of the laboratory-rolled material with high and low FRT and with material produced at SMGB is shown in Figure 8. The most characteristic texture components that were observed were {001}<110> (rotated cube texture), {113}<110>, {112}<110>, {554}<225>, {332}<113>.

12 10 8 Lab trial, low FRT Lab trial, high FRT Mill material, X80 27.7 mm Mill material, X80 23.7 mm 6 4 2 0 0 10 20 30 40 50 60 70 80 90 Angle []

Figure 9: Skeleton plot along the alpha-fibre (1=0, 2=45) of laboratory-rolled plates and mill material at mid-thickness

The skeleton plots for the epsilon-fibre (1=90, 2=45) in Figure 10 show that the material rolled at a higher FRT showed the highest intensity at an angle around =0. This case corresponds to the rotated cube texture. Another peak was observed around the {332}<113> component around =60.
9 Lab trial, low FRT Lab trial, high FRT Mill material, X80 27.7 mm Mill material, X80 23.7 mm 5 4 3 2 1

Intensity
8 7 6
Intensity

Low FRT

High FRT

X80 27.7 mm

X80 23.8 mm

{001} <110> {113} <110> {112} <110> {554} <225> {332} <113>

0 0 10 20 30 40 50 60 70 80 90
Angle []

Figure 8: ODFs at 2=45 of laboratory-rolled plates and mill material at mid-thickness

Figure 10: Skeleton plot along the epsilon-fibre (1=90, 2=45) of laboratory-rolled plates and mill material at mid-thickness

An increase of the volume fraction of the rotated cube texture component relative to the {113}<110> and {112}<110> components, which is believed to be linked to the formation of separations and a reduced low-temperature toughness, was observed at higher FRT. All other materials showed a maximum intensity that was shifted away from the rotated cube texture. This is also illustrated in the skeleton plots for the alpha-fibre (1=0, 2=45) in Figure 9. The samples taken from X80 production at SMGB showed a slightly higher volume fraction around the rotated cube orientation compared to material from the laboratory trials. This was, however, counterbalanced by high volume fractions around the {113}<110> (=25) and around the {112}<110> (=35) components.

In the case of the laboratory trial at a lower FRT, on the other hand, the intensity at 0 was reduced and a peak at around 65 close to the {554}<225> component became dominant. A similar behaviour was observed in the X80 heavy plate material, where the intensity at =0 was less dominant. These results indicate that lowering the final rolling temperature in the austenite region, as proposed for the production of heavy plate material based on the results of the DWT tests, indeed leads to an increase of the volume fraction of beneficial texture components compared to the rotated cube component. Precise knowledge of the relationship between processing parameters and the resulting microstructure is therefore essential, in order to optimise the rolling parameters for excellent low-temperature toughness.

Copyright 2012 by ASME

Results of X80 Heavy Plate Production Heavy plates optimised with regard to low-temperature toughness are designed for use in arctic environments, where beside the strength, the capability to arrest long-running ductile cracks is a major concern. The recently developed plate product is designed to guarantee fully ductile failure behaviour at temperatures as low as -40C in combination with high crack arrest capabilities due to its bainitic microstructure with optimised texture. Compared to ferritic-pearlitic microstructures, where the appropriate microstructures are developed by minimizing the austenite grain size, the bainitic microstructures are controlled by a combination of rolling and cooling parameters. In order to create the optimum microstructure for low-temperature application, exact control of the processing parameters such as the rolling parameters below the non-recrystallisation temperature, the cooling rate during accelerate cooling and the final cooling temperature is required, as shown in the microstructure investigation. The arctic grades produced at SMGB have a bainitic microstructure that consists predominantly of granular bainite, a low volume fraction of ferrite and very fine secondary phase particles, which are enriched with carbon. The granular primary phase nucleates at high temperatures and grows rapidly due to the high undercooling, which leads to a high number of low-angle grain boundaries in the microstructure. Due to this structure with a low grain size and a high dislocation density of the predominant phase, the generated microstructure has an ideal combination of strength and toughness. The granular primary phase and finely dispersed second phase particles lead to high energy absorption and thereby ensure excellent crack arrest behaviour while maintaining a high strength and optimum strain hardening behaviour. In the following, the results of a recent production campaign for plates with a thickness of 28 mm for arctic application are shown. The alloy composition is shown in Table 2.
Table 2: Composition of the investigated mill material Composition , wt.% C Si Mn Mill mat. <0,05 0,20 1,8 Others Cu, Ni, Mo Nb 0,050 Ti 0,02 CE IIW 0,45

of a single order of 24.000 tons in Figure 11 und 12.

Figure 11: Production data for the achieved distribution of the yield strength in transverse direction of 28mm plate

Figure 12: Production data for the achieved distribution of the tensile strength in transverse direction of 28mm plate As for all arctic grades, the main focus during the development and production lies on the toughness properties. The impact energy obtained in Charpy V-notch tests, which is a measure of the toughness, is shown in Figure 13.
Energy, Joule/cm2

The required mechanical properties of the pipes are summarised in Table 3.

Table 3: Pipe requirements (X80, wt = 28mm) YStransv. MPa min. 555 YSlong. MPa. min. 500 TStransv.MPa min. 640 TSlong.MPa min. 610 A5 % min. 18,0 Y/T CVN@40C, J/cm2 min. 250

500 450 400 350 300 250 200 -70 -60 -50 -40 -30

max. 0,92

Testing temperature, C -20 -10

The BDWT requirement was 75/85% shear area at a testing temperature of -30C. The statistically achieved values in the production of more than 84000 tons only in the year 2011 are represented by the values

Figure 13: Measured energy consumption in Charpy Vnotch tests of the last production campaign of X80-plate with a thickness of 28 mm

Copyright 2012 by ASME

The energy in the upper shelf was determined to be approximately 350 J/cm on average. Results of pressed notch BDWT-tests using specimens with the full wall thickness are shown in Figure 14. An average shear area above 85% was safely reached and the average total energy was around 7500 J.

CONCLUSIONS
SMGB has been constantly involved in the improvement of high strength grades since the early 1980s and has produced more than 450,000 tonnes of X80 up to a wall thickness of 40 mm and a width of 4,500 mm. While the initial focus was mainly on the yield strength and tensile strength, the requirements have become increasingly challenging with regard to low-temperature toughness, field weldabilty and material costs. As there is currently a high interest to develop gas fields in arctic environments, a high level of low-temperature toughness and excellent crack arrest capabilities have to be realised. This was achieved by constant alloy and process development. Laboratory trials showed that it is essential to maintain tight control of the rolling and cooling parameters, in order to achieve excellent toughness and crack arrest capabilities. The formation of beneficial texture components is favoured at final rolling temperatures slightly above the austenite-ferrite transformation. Today, the upper shelf in Charpy tests on X80 plates produced at SMGB can be extended down to a test temperature of below -50 C and 85 % shear area fraction in the BDWT test was reached safely at -40 C in the wall thickness range from 25 mm to 30 mm. At the same time, it was possible to reduce the alloy content and thereby improve the weldability significantly. This facilitates pipe production and field welding and leads to a reduction of costs. REFERENCES [1] Meimeth, S., Grimpe, F., Meuser, H., Siegel, H. Stallybrass, C., Heckmann, C.J. Development, state of the art and future trends in design and production of heavy plates in X80 steel-grades, Proc. 9th International Rolling Conference, Paris, France (2006). [2] Grimpe, F., Meuser, H:, Muthmann, E., Gerdemann, F. Improvement of mechanical properties of heavy plates for high strength linepipe applications i.e. in arctic regions, 2nd International Conference Super-High Strength Steels, Peschiera del Garda, Italy (2010). [3] Gerdemann, F., Meuser, H., Grimpe, F., Stallybrass, C., Frommert, M., Microstructure and Mechanical Properties of Heavy Plate Optimized for Low-Temperature Service, 2011 International Symposium on the Recent Developments in Plate Steels, Colorado, 19-22 June 2011

Figure 14: Measured BDWTT shear area at -30C of the last production campaign of X80-plate with a thickness of 28 mm plate Precise control of the accelerated cooling process is essential in the production of high-strength heavy plates on the X80 level or above, in order to guarantee homogeneous properties in all positions of the plate. The distribution of the mechanical properties, tested over the length of an arbitrarily selected plate from the production, is shown in Figure 15. This variation in local properties is similar to that of plates rolled without accelerated cooling and show that the mechanical properties are homogeneous over the complete plate length, as the average deviation for all strength parameters is less than 5 MPa.
Strength, [MPa] 750
725 700 675 650 625 600 575 550 525 500 475 450 0 2500 5000 7500 10000 12500 Plate length, mm

YS trans.

TS trans.

YS long.

TS long.

Figure 15: Strength distribution over the plate length

[4] Zajac, S., Schwinn, V., Tacke, K.-H. Characterisation and Quantification of Complex Bainitic Microstructures in High and Ultra-High Strength Linepipe Steels, Proc. Int. Conf. on Microalloying for New Steel Processes and Applications, Donostia-San Sebastian, Spain (2005). [5] Konrad, J., Stallybrass, C., Schneider, A., Meuser, H., Meimeth, S., Grimpe, F., Characterisation of the

Copyright 2012 by ASME

Microstructure of X80 Heavy Plate for Pipeline Applications using the EBSD Method, Proceedings of the 3rd International Conference on Thermomechanical Processing of Steels, Padua (2008) [6] Stallybrass, C., Konrad, J., Meuser, H., Grimpe, F. High Strength Heavy Plate Optimised for Application in Remote Areas and Low-Temperature Service, Proc. 8th International Pipeline Conference, Calgary (2010), IPC201031227 [7] Baczynski, G.J., Jonas, J.J., Collins, L.E., The influence of rolling practice on notch toughness and texture development in high-strength linepipe, Metallurgical and Materials Transactions A, Boston (1999), 3045-3054 [8] Hara, T., Shinohara, Y., Asahi, H., Terada, Effects of microstructure and texture on DWTT properties for high strength line pipe steels, Proceedings of the Sixth International Pipeline Conference, Calgary (2006), IPC2006-10255 [9] Hara, T, Fujishiro, T., Terada, Y., Inoue, T., Asahi, H., Doi, N. Development of high-strength heavy-wall line pipe, Pipeline Technology Conference, Ostend (2009), Ostend2009015. [10] Pyshmintsev, Y., Arabey, A.B., Gervasyev, A.M., Boryakova, A.N., Effects of microstructure and texture on shear fracture in X80 linepipes designed for 11.8 MPa gas pressure, Proceedings of the Pipeline Technology Conference, Ostend (2009), Ostend2009-028 [11] Stallybrass, C., Grimpe, F., Meuser, H., Hillenbrand, H.-G., Development of high strength heavy plate optimised for low temperature toughness for linepipe applications, Pipeline Technology Conference, Ostend (2009), Ostend2009-003

Copyright 2012 by ASME