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https://doi.org/10.1007/s12540-020-00841-3
Abstract
Four Nb–V–Ti steel plates of API 5LX70 linepipe were produced with changing accelerated cooling rate and finish rolling
temperature using thermomechanical controlled process. The changes in ductile fracture surface, brittle fracture surfaces,
including initial cleavage fracture and inverse fracture, arrowhead marking surfaces, and delamination were investigated
using drop-weight tear test at temperatures of 0 °C and − 10 °C. Based on the drop-weight tear test results, an increase in the
accelerated cooling rate, resulting in an increase in the volume fraction of quasi polygonal ferrite, fine polygonal ferrite, and
granular ferrite microstructures, increased the percentage of ductile fracture surface and decreased the percentage of brittle
fracture surfaces. Moreover, a reduction in the finish rolling temperature led to similar changes in the ductile fracture surface
and brittle fracture surfaces due to an increase in the volume fraction of aciculae ferrite. Arrowhead markings surfaces,
caused by the presence of banded structures, their percentage was reduced by increasing the accelerated cooling rate and
decreasing the finish rolling temperature at the temperature of 0 °C. Furthermore, as the accelerated cooling rate increased,
the number, length, thickness, and depth of delaminations were reduced at temperatures of 0 °C and − 10 °C.
Keywords Drop-weight tear test · Thermo-mechanical controlled process · High-strength low-alloyed steel · Arrowhead
markings · API 5LX70
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and drop-weight tear test (DWTT). Each experiment has 2 Materials and Methods
its applications.
DWTT is used to evaluate abrupt and rapid propaga- 2.1 Materials
tion of cracks, which can cause ductile or brittle fracture
surfaces [9]. Therefore, it is recommended to perform this Nb–V–Ti microalloyed slab was produced by electric arc
test for the pipes known as production specification level furnace and continuous casting machine, and except for
2 (PSL 2), which are supposed to carry gaseous fluids, if vacuum degases, secondary steelmaking processes such as
the average shear fracture area or ductile fracture surface control of sulfur, chemical analysis, hydrogen, and calcina-
(DF) are equal to or greater than 85% at the temperature tion were conducted on it. Then, using the TMCP rolling line
of 0 °C [10]. of Khuzestan Oxin Steel Company (Oxin Company), four
Investigating the fracture surfaces was another goal of ferrite-pearlite plates of 19 mm thickness were produced
performing this test. The brittle fracture can be divided whose schematic, chemical composition, and parameters
into initial cleavage fracture (ICF), arrowhead marking are shown in Fig. 1 and Tables 1 and 2, respectively. Fur-
surfaces (AHMs), inverse fracture (IF), and delamination thermore, it was attempted to change only the ACC rate in
(also known as separation), while DF and shear lips are plates A and B and FRT in plates C and D by keeping other
recognized as the ductile fracture [11–13]. Examination of parameters constant to investigate their effects on the DWTT
these surfaces can reveal whether the casting and forming results. It should be mentioned that the values of critical
stages of the plates are appropriately conducted according temperatures, including Tnr (non-recrystallization tempera-
to their application or not. For example, delamination is a ture) and TAr3 (austenite to ferrite transition temperature) in
mode of fracture surface that occurs due to inclusions like Fig. 1, were calculated by Oxin Company, and the authors
MnS and segregation of elements, which create banded did not participate in calculating them.
structures [8, 12, 14]. Hence, the evaluation of these sur-
faces can offer guidance for the plates that should be free 2.2 DWTT Conditions
of any banded structures.
AHMs are known as a type of brittle fracture surface that After the plates were produced with the intended param-
can be seen in DWTT. According to the previous studies, R. eters of Table 2, DWTT was conducted on them to exam-
Schofield et al. [15], who investigated control rolled micro- ine their toughness. The test procedure, number of times it
alloyed steel, used the term arrowhead for the first time. was performed, dimensions of the specimens, whether the
According to the results of their study, the reasons for the specimens were accepted or rejected, and how to examine
formation of this surface were high impact transition tem- the fracture surfaces of the samples were all in accord-
perature (ductile–brittle transition temperature) and high ance with API 5L, API RP 5L3, and ASTM E436 stand-
yield strength of the steel. Another research attributed the ards [9–11]. Thus, the specimens with the dimensions
occurrence of AHMs to the existence of delamination and 19 mm × 76.2 mm × 305 mm (thickness × width × length),
the changes in the strain at moving crack-tip [16]. In another which were prepared perpendicular to the rolling direction,
study, after conducting crack tip opening angle (CTOA) tests
on APIX100 samples, chevron-shaped fractures, which were
very similar to the shape of AHMs, were observed due to
the banded structure leading to the growth of crack [17].
Thus, based on the reviewed studies, which are limited in
this subject, it was concluded that no research had been con-
ducted on this subject so far, and it has not been clear that
why these AHMs are formed and why they have such shapes.
Therefore, this research is the first of its kind.
In this research, four Nb–V–Ti plates of non-sour API
5LX70 linepipe were produced with different accelerated
cooling (ACC) rates and finish rolling temperature (FRT)
parameters using TMCP. Afterward, DWTT was performed
at temperatures of 0 °C and − 10 °C to clarify the effects of
these parameters on the percentages of brittle fracture sur-
faces (BFs), DF, delamination, and especially AHMs, and
determine the correlation between the results and micro-
structures. In addition, an effort was made to discover why
the AHMs were formed and why they had such shapes. Fig. 1 Schematic of TMCP program
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Table 1 Chemical composition
of API 5LX70 steel plates C Mn Si P S Nb Ti V Ni
(wt%) 0.085 1.52 0.32 0.011 0.001 0.054 0.015 0.036 0.154
Mo Cr Cu Al Ca N O Fe
0.094 0.017 0.008 0.032 16 ppm 47 ppm 18 ppm Bal.
2.3 Microstructure Evaluation
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3.2 Banded Structures
Table 3 Volume fraction, grain Plate Volume fraction, (wt%) Overall grain Shape
size and shape determination size (μm)
A F* P F P*
90 ± 1 10 ± 1 9 ± 2 CP
PF QPF AF GF
88 ± 2 2 ± 1 0 0
B 95 ± 1 5 ± 1 2 ± 1 FP
PF&FPF QPF AF GF
87.5 ± 2 5 ± 1 Nil 2 ± 1
C 88 ± 1 12 ± 1 4 ± 2 CP
PF&FPF QPF AF GF
78.5 ± 2 6 ± 2 Nil 3 ± 1
D 95 ± 1 5 ± 1 1.5 ± 0.5 FP
PF&FPF QPF AF GF
84.5 ± 2 1.5 ± 1 6 ± 1 3 ± 1
*F ferrite, P pearlite
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Besides, probable elements in ferrite-pearlite and pearl- as well as a large volume of DWTT fractured samples; how-
ite–pearlite boundaries were investigated using point analy- ever, slight studies have been done this issue [16].
sis. According to the results of Fig. 7a, b, iron existed mostly These areas themselves were subdivided into six types of
in the ferrite-pearlite boundary, while in pearlite–pearlite fracture surfaces: (1) ICF near the pressed notch, (2) delami-
boundary, there were silicon and chromium in addition to nations, which were distributed in different parts of the sur-
iron. Similar studies have been conducted to examine ele- face, (3) AHMs, which mostly appeared in the second area,
ments in or across grain boundaries [26, 27]. (4) IF, which referred to the appearance of DF instead of
brittle fracture surface according to the API RP 5L3 stand-
ard [11] and appeared in the third area, (5) DF, which could
3.3 Appeared Areas and Surfaces in DWTT appear in all areas and was the most appropriate fracture
surface, and (6) the shear lips that mostly appeared in the
Based on Figs. 8 and 9, which show the fracture surfaces of second and third areas and it should be noted that they were
plates A-D at the temperatures of 0 °C and − 10 °C, the frac- present outside the surface of the samples.
ture surfaces can commonly be subdivided into three areas. All of the fracture surfaces, except for the DF and shear
The first area was caused by the effect of the pressed notch lips, were considered as a reaction to ductile fracture, so they
that resulted in ICF, and the completion of this fracture was were brittle fractures. In order to have a better understanding
the end of this area. The second area was a combination of of the types of fracture surfaces in DWTT, some samples
AHMs and DF or only DF that resulted from continued crack with clearly identifiable fracture surfaces were selected,
growth. The third area formed due to the work hardening of whose schematics are shown in Figs. 10 and 11 beside their
the hammer impact, which had caused the appearance of IF. fracture surfaces.
Imaging of DWTT fractured surfaces, by means of SEM is a From Figs. 10 and 11, it can be concluded that after the
rare analysis due to the limited volume of the SEM chamber hammer impacts on the specimens, the crack began to grow
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(a) (a)
(b) (b)
O
C
C O Nb
Mn Nb Mn
Fig. 5 a The location of the linear analysis of the specified sample Fig. 6 a The location of the linear analysis of the specified sample
perpendicular to rolling the direction. b The results of the linear anal- perpendicular to rolling the direction. b The results of the linear anal-
ysis of the specified location in Fig. 5a ysis of the specified location in Fig. 6a
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Fig. 10 Schematic of DWTT
fracture surfaces for plates of a
A at 0 °C and b B at − 10 °C
plates [18, 19]. Among these microstructures, the AF as in the FRT were more effective in the formation of GF and
the best candidate for the microstructure of pipeline plates AF, respectively.
has more influence on balancing the strength and tough- As shown in Figs. 8 and 9, AHMs appeared in crack
ness because of its finest ferrite grain as well as the high- propagation direction (perpendicular to rolling direction).
est dislocation density. Moreover, the GF, FPF, and QPF Accordingly, it is evident in Figs. 8, 9 and 11 that AHM
respectively have more impact on increasing the strength initially grew in the direction of 90 degrees relative to the
and toughness [18, 19, 31]. In addition, the volume frac- applied stress and their bottom side formed. Afterward, they
tion and the size of the cementite of pearlite, which is had the final growth in the direction of 45 degrees relative to
a proper spot for nucleation and growth of cracks, were the applied stress, and their topsides formed, which created
reduced. Hence, the microstructures withstood further AHM. However, in some of AHMs, the angle of 90 degrees
crack growth, the DF increased, and the BFs and AHMs was approximate due to the presence of a delamination at the
decreased. Furthermore, based on Table 3, it was con- beginning of the bottom side. The steps towards the forma-
cluded that the increase in the ACC rate and the reduction tion of an arrowhead are similar to those of the crack growth
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Fig. 11 Schematic of DWTT
fracture surfaces for plates of a
C and b D at 0 °C
A 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C
80 ± 1 68 ± 1 6 ± 2 31 ± 2 14 ± 1 × × 1 ± 1 ✓ ✓
B 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C
85 ± 1 74 ± 1 5 ± 2 11 ± 2 7 ± 1 11 ± 1 3 ± 1 4 ± 1 ✓ ✓
C 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C
76 ± 1 79 ± 1 13 ± 4 9 ± 2 11 ± 1 12 ± 1 × × ✓ ✓
D 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C 0 °C − 10 °C
98 ± 1 87 ± 1 2 ± 1 6 ± 1 × × × 7 ± 1 ✓ ✓
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until ductile fracture in the tensile test so that after necking After conducting DWTT at the temperature of 0 °C, less
and then the formation and growth of cavities, the cracks than four delaminations with medium or short lengths, and
grew at an angle of 90 degrees at first, and then 45 degrees low thicknesses and depths were observed in the fracture
relative to the applied stress [32]. Thus, it can be concluded surfaces of plates B and D, which had a DF percentage
that although this type of fracture surface had brittle nature, equal to or above 85% and fulfilled the API 5L standard
its mechanism of shape formation was similar to that of the [10] requirement for transmission of gas fluids. Hence,
ductile fracture in the tensile test. it can be concluded that in plates with a DF equal to or
The start and stop of the growth of the AHMs can also be above 85%, the number, length, depth, and thickness of
examined in the DWTT fracture surface. For this purpose, delaminations were low, and the casting and fabrication
the mechanism of formation and growth of brittle fracture processes were appropriately performed. Furthermore, to
surfaces needs to be studied. Initially, the pressed notch is examine the banded structures at the DWTT fracture sur-
created as a fault and starting position of the crack under face for plates to be used in sour environments, delamina-
work hardening. After the hammer impacts the specimen, tions were a better criterion than the AHMs, because with
the crack appears and starts to propagate from the pressed the presence of banded structures in the microstructure of
notch due to the energy generated by the hammer along with all plates, one would expect the appearance of AHMs and
the stored elastic strain energy. However, by reducing the delaminations at the fracture surfaces of all plates. Never-
stored energy, crack stops, or slows down, but as this energy theless, with improving the properties of plates, only the
rises again, the crack growth rate increases, and the crack delaminations remained at the fracture surfaces, and the
starts to grow again [33]. A reduction, increase, or stop of AHMs were eliminated.
the crack growth affects the fracture surface, which means
the brittle fracture surface extends, stops, or decreases by
increasing, stopping, or reducing the crack rate, respectively.
Factors such as modification of the microstructure or elimi- 5 Conclusions
nation of the banded structures have a significant effect on
decreasing the crack growth and consequently reducing the After conducting DWTT at the temperatures of 0 °C and
brittle fracture surface. − 10 °C on four Nb–V–Ti microalloyed steels produced with
One of the modes that appeared at the fracture surfaces TMCP, it was concluded that:
of the DWTT samples is the delaminations. By examining
Figs. 8 and 9, it is observed that delaminations appeared in 1. With increasing the ACC rates and decreasing the FRT,
areas and surfaces such as (1) close to and inside the ICF, (2) the DF increased, and consequently, the BFs decreased
at the entire second area, (3) inside the AHMs, (4) close to due to the formation of QPF, FPF, GF, and AF micro-
the IF. In addition, the delaminations can be compared based structures that had fine grains and more dislocations
on their length, thickness, depth, and number in each plate. within themselves, as well as a reduction in pearlite,
Therefore, the number, depth, length, thickness, presence or which meant that the cementite decreased as they
absence of delaminations at the DWTT fracture surfaces can become smaller.
provide the suitable guidance to recognize whether casting, 2. The AHMs, as brittle fracture surfaces, appeared in
solidification, and TMCP of the slab are performed appropri- complete and incomplete forms and were reduced with
ately and according to customer requirements or not. an increase in the ACC and a decrease in the FRT. The
Given that the delaminations were all in the crack growth number, length, thickness, and depth of the delami-
direction, by examination of the fracture surface of plate nations also declined with increasing the ACC and
B, it was concluded that the number, length, thickness, and decreasing the FRT.
depth of delaminations decreased with increasing ACC rate 3. Based on the investigations, it was realized that the
due to the formation of QPF, FPF, and AF microstructures AHMs formed due to banded structures, which were
at the temperatures of 0 °C and − 10 °C. Nevertheless, with observed in the microstructures and approved by segre-
reducing FRT in Plate D, no changes were made in number, gation of the elements Nb, Mn, O, and C.
length, thickness, and depth of delaminations. Generally, 4. According to API 5L standard and DWTT results, since
by examining plates A-D, it was found that the number, plates B and D had less than four delaminations of low
length, and thickness of delaminations in plates C and D length, depth, and thickness, and a DF equal to or more
were lower than those in plates A and B. This result indicates than 85% at the temperature of 0 °C, they had the capa-
that plates C and D underwent a more appropriate casting bility for transmitting gas fluids, with plate D being the
process and TMCP and were able to withstand the occur- best choice. Moreover, instead of AHMs, the delamina-
rence and growth of the delaminations due to the presence tions were chosen as the best criterion for detecting the
of FPF and AF microstructures. banded structures.
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