METAL 2001 15. - 17. 5.

2001, Ostrava, Czech Republic

TRANSFORMATION BEHAVIOUR AND MICROSTRUCTURE OF AN

API X80 LINEPIPE STEEL SUBJECTED TO SIMULATED
THERMOMECHANICAL PROCESSING

P. Cizek

UNIVERSITY OF OXFORD, Department of Materials, Parks Road, Oxford OX1 3PH, GB

Abstract

The transformation behaviour and microstructural characteristics of the transformation

products were studied in an API X80 linepipe steel subjected to simulated controlled rolling
followed by controlled cooling. Deformation dilatometry was employed to investigate the
transformation characteristics of both recrystallised and heavily deformed austenite during
cooling at rates from 0.1°C/s to about 100°C/s and the corresponding CCT diagrams were
constructed. The transformation product microstructures were studied in detail using optical,
scanning electron, and transmission electron microscopy, complemented by a quantitative
image analysis. The detailed transformation and microstructural characteristics, obtained in
the present work, could be used for the optimisation of thermomechanical processing
schedules for API X80 and similar higher-grade linepipe steels.

1. INTRODUCTION

The constantly increasing demands of the pipeline industry for a more cost-effective pipeline
design has pushed the standard pipeline steel grade requirements up to API X80 and beyond.
Critical to the design of these steels is a low carbon equivalent for good field weldability [1].
To compensate for the loss in strength, additions of microalloying elements such as niobium,
titanium and molybdenum are used. These additions contribute to an increase in strength both
directly, through microstructural refinement, solid solution strengthening and precipitation
hardening, as well as indirectly, through enhanced hardenability and associated modification
of the resultant transformation microstructures [1,2]. Optimum product microstructures, with
a desired balance of mechanical properties at a given steel composition, are being achieved
through suitably designed thermomechanical processing schedules [2], which commonly
involve controlled rolling, followed by controlled accelerated cooling. The controlled rolling
step usually includes heavy deformation of the austenite, carried out in the non-
recrystallisation temperature region, which brings about significant refinement of the final
transformation microstructures. The accelerated cooling step aims to suppress the formation
of polygonal ferrite and, instead, encourage non-equilibrium, non-equiaxed ferrite
microstructures to be formed. The latter transformation products are known to contribute to
increasing strength, through both small effective grain sizes and increased dislocation
densities, while maintaining a reasonable level of toughness [1-3]. The non-equilibrium ferrite
microstructures do not contain cementite and possess some unique morphological features.
A specific terminology [4] has been adopted in the present work in an attempt to describe
all possible ferrite morphologies formed by the decomposition of austenite in these modern
microalloyed steels with very low carbon contents. Apart from martensite (M), this
terminology recognizes five separate forms of ferrite: (i) polygonal ferrite (PF), the
equilibrium microstructural constituent characterized by roughly equiaxed grains with smooth
boundaries, mostly containing a low dislocation density and no substructure; (ii)

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Widmanstätten ferrite (WF), defined by elongated crystals of ferrite with dislocation

substructure; (iii) quasi-polygonal ferrite (QF), characterized by grains with undulating
boundaries containing dislocation substructure and occasional martensite-austenite (M/A)
microconstituent; (iv) granular ferrite (GF), which consists of sheaves of elongated ferrite
crystals with low misorientations and a high dislocation density, containing roughly equiaxed
islands of M/A microconstituent; and (v) bainitic ferrite (BF), which consists of packets of
parallel ferrite laths (or plates) separated by low-angle boundaries and containing very high
dislocation densities. In contrast to GF, the M/A microconstituent retained between the ferrite
crystals in BF has an acicular morphology. The austenite decomposition products containing
cementite are generally classified as pearlite (P), degenerate pearlite (P’) and “classical”
bainite (B). In order to differentiate between conventional upper bainite (UB) and lower
bainite (LB), the classification scheme proposed by Ohmori et al. [5] has been adopted.
In order to obtain greater understanding of the processes that take place during industrial
processing of a modern API X80 linepipe steel, the aim of the present work was to
characterise the transformation behaviour and microstructures developed in this steel during
laboratory simulation of controlled rolling in conjunction with controlled continuous cooling.

2. EXPERIMENTAL PROCEDURES

The chemical composition of the steel studied was 0.065 mass% C, 0.29% Si, 1.55% Mn,
0.018% P, 0.003% S, 0.28% Mo, 0.076% Nb, 0.020% Ti, and the balance Fe. The steel was
supplied by BHP Integrated Steel, Port Kembla Works, Australia. Deformation dilatometry
was performed using a computerized high-speed quenching and deformation dilatometer. The
dilatometry specimens were solid cylinders with a diameter of 4 mm and a length of 8 mm.
Each steel was subjected to the simulated recrystallisation and non-recrystallisation rolling
schedules depicted schematically in Fig. 1, followed by controlled cooling at rates from
0.1°C/s to approximately 100°C/s. Both rolling schedules included a simulated “roughing”
step performed at a temperature of 1100°C using a strain of 0.30, followed by post-
deformation holding on the above temperature for 120 s to ensure complete recrystallisation.
The simulated non-recrystallisation rolling schedule contained an additional “finishing” step
performed at a temperature of 875°C, which was situated in the non-recrystallisation
temperature region, using a strain of 0.47 in compression. The cooling rates were defined by
the time interval required for the specimens to cool from 800°C to 500°C. The mean grain
diameter of the initial austenite was about 35 µm. All specimens were Vickers hardness tested
using a 5 kg load and examined by optical microscopy after being etched with 2% nital. The
information obtained was used to construct continuous cooling transformation (CCT)
diagrams. A more detailed metallographic examination was performed on selected specimens
using both scanning electron microscopy and transmission electron microscopy (TEM).

3. RESULTS

3.1 Transformation Behaviour

The CCT diagrams obtained are presented in Fig. 2. In the case of the transformation from the
recrystallised austenite (Fig. 2a), the presence of PF within the resulting transformation
microstructure was restricted to the cooling rates below approximately 1°C/s. At a cooling
rate of 0.3°C/s, PF formation was followed by the conversion of the remaining untransformed

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TR: 1200°C 120s TR: 1200°C 120s

1200 2°C/s 1200 2°C/s
1100°C 30% 120s 1100°C 30% 120s
1000 2°C/s 1000 2°C/s

Temperature (°C)
Temperature (°C)

875°C 875°C 46.7%

800 800
Controlled cooling Controlled Cooling
600 to 200°C 600 o
10°C/s to 200 C
10°C/s
400 400

200 200

0 0
0 200 400 600 800 1000 1200 0 200 400 600 800 1000 1200
(a) Time (sec) (b) Time (sec)

Figure 1. Schematic of simulated rolling schedules: (a) recrystallisation schedule; (b) non-
recrystallisation schedule involving a reduction of 46.7% at 875°C.

Figure 2. CCT diagrams obtained for the recrystallised (a) and deformed (b) austenite.

austenite into GF. The formation of a mix of QF and GF was observed to spread over a wide
interval of cooling rates ranging from 1°C/s up to 34°C/s. At a cooling rate of 95°C/s, the
transformation microstructure was dominated by BF accompanied by a small amount of M.
Heavy deformation of the prior austenite brought about a significant expansion of the PF
transformation field in the CCT diagram at the expense of a mix of QF and GF (Fig. 2b). The
corresponding transformation start temperatures underwent a noticeable increase, as illustrated
by the deviations of the transformation points (marked by solid circles) from the
superimposed open triangles. The transformation temperatures represented by the triangles
were derived from the CCT diagram of the recrystallised austenite at roughly comparable
microstructures. Following the same way of comparison, the transformation start temperatures
of a mix of QF and GF were found to increase slightly, whereas the corresponding
transformation finish temperatures underwent a marginal decrease. This brought about slight
widening of the corresponding temperature interval of transformation. Also, as a result of the
austenite deformation, the formation of BF was noticeably suppressed and that of M entirely
eliminated within the studied range of cooling rates.
Measurements of the bulk Vickers hardness of each of the dilatometer specimens were
superimposed on the corresponding CCT diagrams in Fig.2. As expected, the lowest hardness
values observed corresponded to the microstructures dominated by PF, which formed at the
highest transformation start temperatures. Conversely, the highest hardness value was

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displayed by the microstructure composed of BF and martensite, forming at the lowest

transformation start temperature from the recrystallised austenite. The hardness data obtained
for QF and GF, characterised by intermediate formation temperatures, were situated between
the above limits. The transformation microstructures formed from the deformed parent
austenite were generally observed to display slightly increased hardness values compared to
the equivalent microstructures created from the recrystallised austenitic matrix.

3.2 Transformation Microstructures

In the following, the microstructural characteristics of the transformation products obtained

from the recrystallised austenite (see Fig. 2a) will be first discussed in detail and some
comments on the impact of the austenite deformation on these characteristics will be
subsequently made. The microstructure of PF grains was observed to contain carbon-enriched
islands comprising a complex mixture of austenite decomposition products. At the lowest
cooling rate of 0.1°C/s, the carbon-enriched regions largely displayed quite uniform dark-
etching contrast in optical micrographs (Fig. 3a) and TEM showed that they were
predominantly composed of bainite, accompanied by a small amount of fine P or P`. The
observed bainite morphology could be best classified as a mixture of BII and BIII upper
bainite according to the scheme proposed by Ohmori et al. [5]. The BII sheaves were
composed of highly-dislocated ferrite laths separated by continuous cementite layers, while
the BIII sheaves, which were observed much more frequently than BII, contained discrete
cementite platelets aligned along a common direction within the ferrite matrix (Fig. 4a). When
increasing cooling rate to 0.3°C/s, PF volume fraction decreased and the rest of the

Figure 3. Optical micrographs of the microstructures transformed from the recrystallised

austenite: (a) 0.1°C/s, PF+B; (b) 0.3°C/s, PF+GF; (c) 1°C/s, QF+GF; (d) 18°C/s, GF; (e)
95°C/s, BF+M.

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microstructure became characterized by dark-etching microregions scattered within white

ferritic areas (Fig. 3b). In the TEM, the microregions displaying the dark-etching response in
optical micrographs were composed predominantly of bainite, with only a small fraction of
fine P’. The ferrite matrix, in which the dark-etching particles were embedded, contained a
high dislocation density and was subdivided into fragments separated by low-angle
boundaries. Thus, such a microstructure appeared to be similar to that observed within the GF
sheaves formed at higher cooling rate regimes (see below), apart from the second-phase
microregions being coarser and composed largely of bainite rather than M/A
microconstituents typical of GF.

Figure 4. TEM micrographs of the transformation products obtained from the recrystallised
austenite: (a) 0.1°C/s, BII; (b) 1°C/s, QF; (c) 18°C/s, GF; (d) 95°C/s, BF.

When the cooling rate reached 1°C/s, PF ceased to be formed and the transformation
microstructure became dominated by QF, accompanied by GF (Fig. 3c). For the
microstructures predominantly composed of QF, there was no clear indication of the locations
of prior austenite grain boundaries. The QF grains were characterised by undulating
boundaries and the presence of clearly etched sub-boundaries in their interiors. These grains
occasionally contained second-phase microregions, composed of a mixture of dark-etching
bainite particles and grey M/A microconstituents. TEM analysis revealed that QF grains were
composed of corse fragments, separated by low-angle boundaries and containing significant
dislocation densities (Fig. 4b). A gradual increase in cooling rate was accompanied by a
parallel increase in the volume fraction of GF in the microstructure, at the expense of QF, and
the distributed microregions became dominated by M/A microconstituents. When the
microstructure contained a significant volume fraction of GF, the locations of the prior

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austenite grain boundaries remained largely preserved (Fig. 3d). Observed by TEM, the GF
sheaves were composed of both elongated and roughly equiaxed fragments, separated by low-
angle boundaries and having high internal dislocation densities, and contained approximately
equiaxed regions of M/A microconstituent (Fig. 4c). The latter comprised a number of
variants of highly-dislocated lath martensite, accompanied by barely detectable retained
austenite. In contrast to the substructural characteristics of QF grains, the fragments present
within GF sheaves were generally finer and the corresponding dislocation densities
comparatively higher. An increase in cooling rate to 95°C/s brougt about a transition from GF
to BF, as well as the formation of a small volume fraction of lath martensite (see Fig. 2a). In
optical micrographs, BF was characterised by packets of parallel laths (or plates), containing
fine acicular M/A microregions along their boundaries, and the locations of the original
austenite boundaries remained entirely retained (Fig. 3e). The substructure of BF packets was
characterised by sympathetically nucleated, nearly parallel laths separated by low-angle
boundaries and containing very high dislocation densities in their interior (Fig. 4d).
The microstructures obtained after the transformation from the deformed, unrecrystallised
austenite essentially remained similar in character to those originated from the recrystallised
austenite matrix. However, as a result of austenite deformation, both PF and QF grains
became significantly refined and a similar trend was observed for both GF sheaves and BF
packets. The GF substructures were found to be slightly more fragmented, but there was no
obvious incease in corresponding dislocation densities as a result of transformation from the
heavily-deformed austenite. The BF laths generally became shorter, along with the decrease in
the corresponding packet dimensions.

4. DISCUSSION

4.1 Transformation Behaviour

Heavy deformation of austenite, carried out at a temperature (875°C) situated below the non-
recrystallisation limit, resulted in a pronounced shift of the PF transformation field in the CCT
diagram towards higher cooling rates (see Fig. 2), which is in good correspondence with the
published data [2,6]. The observed enhanced formation of PF may be attributed to both an
increase in the austenite stored energy due to deformation and a concomitant rise in the
density of ferrite nucleation sites, as well as to the lowering of the amount of Nb in solid
solution due to strain-induced precipitation of Nb carbonitrides, which decreases austenite
hardenability [6]. It is well known that the presence of PF in the microstructure of high-
strength linepipe steels needs to be minimised [1]. From the inspection of the CCT diagrams
in Fig. 2 it follows that, in the present case, the minimum cooling rate values required to avoid
PF formation were around 1°C/s and 10°C/s for transformation from the recrystallised and
deformed austenite respectively. It is necessary to note that both the above values, the latter
one in particular, might be slightly higher in the industrial processing of similar steels due to
both a finer prior austenite grain size and a larger amount of strain within the austenite, known
to decrease hardenability. Once the cooling rate exceeded the above limits, PF formation was
avoided and a variety of non-equilibrium ferrite microstructures was obtained. In contrast to
PF, the transformation characteristics of these non-equilibrium transformation products
generally appeared rather insensitive to deformation of the parent austenite in the steel
investigated (see Fig. 2), which is in agreement with findings presented in [7].

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4.2 Transformation Microstructures

The formation of PF grains, characterised by rather low internal dislocation densities, was
accompanied by the presence of carbon-enriched austenite regions, stabilized against further
PF formation. This was a result of the carbon content of the steel that exceeded the solubility
limit in PF. The carbon-enriched austenite was found to subsequently undergo complex
decomposition during further cooling, presumably due to variation in carbon enrichment.
Small fractions of P or P’, observed within the carbon-enriched islands at the very low cooling
rates, suggest that the pearlite transformation field was occasionally intersected in some local
volumes during cooling. The bulk of the carbon-rich austenite transformed into a mix of BII
and BIII types of classical bainite [5]. As already mentioned above, the presence of larger
amounts of PF in the microstructure of the linepipe steels should be avoided [1]. This is for
the reason that PF is detrimental to strength, as documented by the hardness values presented
in Fig. 2, and also brings about discontinuous yielding that might cause some problems during
pipe forming due to the Bauschinger phenomenon [1,3].
Unlike the PF grains described above, the non-equilibrium ferrite microstructures were
generally observed to contain significant internal dislocation densities, which is consistent
with continuous yielding displayed by these transformation products [1-3]. It seems
reasonable to suggest that the increased dislocation densities found within both QF grains and
GF or BF sheaves/packets originated mainly from accommodation of the stresses, caused by a
volume change accompanying the transformation at the relatively low temperatures involved.
The frequently observed low-angle boundaries, subdividing the above grains or
sheaves/packets into smaller fragments, appear to have largely resulted from mutual
impingement of several growing ferrite crystals, formed by separate nucleation events or
sympathetically [8]. Consequently, it could be expected that some carbon-enriched austenite
regions, stabilized against further transformation to ferrite, might become entrapped locally
between the growing non-equilibrium ferrite crystals. Indeed, such local volumes, transformed
during subsequent cooling to either bainite or M/A microconstituents, were frequently
observed in the present study. On the basis of careful comparisons of the ferrite
microstructures classified as QF or GF in the present work with those available in the
literature, it appears that these constituents might essentially be products of WF
transformation, undergoing some subsequent degeneration [8,9]. A possible reason why QF
requires relatively higher temperatures for its formation compared to GF has been suggested
in [9]. The results of the present investigation suggest that BF might perhaps represent a
genuine “bainitic” microstructure, alternatively classified as BI carbide-free upper bainite
having a different formation mechanism [5].
The transformation microstructures dominated by QF are known to have slightly lower
strength, compared to those formed at comparatively higher cooling rates and composed
predominantly of GF, as also indicated by the corresponding hardness values presented in Fig.
2. However, these microstructures possess superior toughness [2,3], thanks to the elimination
of the prior austenite grain boundaries, lower internal dislocation densities and fewer carbon-
rich distributed microconstituents. Further increase in cooling rate brings about a progressive
rise in GF volume fraction at the expense of QF, which gradually enhances strength (see
hardness values in Fig. 2) whereas toughness is expected to decrease [2,3]. When the cooling
rate is high enough for BF to be formed, the strength is further enhanced but the toughness is
known to deteriorate [3]. Thus, the results of the present study indicate that, through a careful
control of continuous cooling, microstructures with a balance of properties potentially suitable
for higher-grade linepipe steel development can be obtained.

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5. CONCLUSIONS

The transformation behaviour and the transformation product microstructures have been
studied in an API X80 linepipe steel during simulated recrystallisation and non-
recrystallisation controlled rolling, followed by controlled cooling at rates from 0.1°C/s to
about 100°C/s. Deformation dilatometry in conjunction with advanced metallographic
techniques were employed in the investigation and the corresponding CCT diagrams were
constructed. It was observed that severe plastic deformation of the parent austenite (>0.45)
markedly enhanced PF formation indicating a significant effective decrease in austenite
hardenability. In contrast, the non-equilibrium ferrite microstructures, classified as QF, GF
and BF, generally appeared rather insensitive to deformation of the parent austenite in the
steel investigated. The detailed transformation and microstructural characteristics, obtained in
the present work, could be used for the optimisation of thermomechanical processing
schedules for API X80 and similar higher-grade linepipe steels.

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