Available online at www.sciencedirect.

com
@

_-

ScienceDirect

JOURNAL OF IRON AND STEEL RESEARCH, INTERNATIONAL. 2011, 18(2): 57-63

Microstructural Evolution and Mechanical Properties of Nb-Ti Microalloyed Pipeline Steel

LAN Liang-yun,

QIU Chun-lin,

ZHAO De-wen,

GAO Xiu-hua

(State Key Laboratory of Rolling and Automation, Northeastern University, Shenyang 110004, Liaoning, China)

Abstract: The correlation between microstructures and mechanical properties of a Nb-Ti microalloyed pipeline steel was investigated. T h e results revealed that with decreasing the finish rolling temperature and the cooling stop temperature, the matrix microstructure was changed from quasi-polygonal ferrite to acicular ferrite, as a result of improvement of both strength and low temperature toughness. By means of electron backscattered diffraction observation, an effective acicular ferrite packet contained several low angle boundaries or subboundaries plates which made important contributions to improvement of strength. It was found that many fine quasi-polygonal ferrite grains with high angle boundaries as the toughening structure were introduced into the acicular ferrite matrix to refine effective grain size and improve the toughness. Key words: pipeline steel; acicular ferrite; mechanical property; electron backscattered diffraction

T o improve the transmission efficiency, pipeline steels must have high strength, high toughness, and excellent corrosion Recently many studies have been carried out by optimizing chemical composition and thermomechanical control processing (TMCP) in order to obtain excellent mechanical properties of pipeline steelsC2-67. When pipeline steels are subjected to different rolling processes, the microstructures obtained usually consist of polygonal ferrite ( P F ) , quasi-polygonal ferrite ( Q F ) or massive ferrite, granular bainitic ferrite (GF) and bainitic or acicular ferrite ( B F or AF) in terms of ferrite microstructures classified by Krauss and other r e s e a r c h e r ~ ~ ~ -T h e AF, first described in the early ~I. 1 9 7 0 ~ has ,been well known as the optimum mi~~ crostructure with an excellent combination of high strength and good low temperature toughness in weld steels. Recently many researches have been done on the AF formed in pipeline steels, because its morphology and properties were to some extent simHowever, ilar to the AF formed in weld steelsC0-163. the morphological feature and crystallographic orientation of such kind of microstructure formed in pipeline steels are still controversial issues according to

Ref. [ll], Ref. [15] to Ref. [18]. In this work, different multiphase microstructures, such as AF together with QF and dispersed martensite/austenite ( M / A ) constituent, were obtained by applying different rolling processes. T h e purpose of this study is comparative analysis of the effects of different multiphase microstructures on mechanical properties of an API X70 pipeline steel and confirmation of the AF microstructure crystallographic characteristics by means of electron backscattered diffraction ( EBSD) and scanning electron microscope (SEM).

Materials and Experimental Procedure

Chemical composition for the experimental steel is listed in Table 1. In order to obtain low cost and high strength of hot rolled plate, the amount of carbon element was controlled slightly high but much lower
Table 1 Chemical composition of the experimental steel
(mass percent, % I
C 0.12 Mn 1.13

S
0.003

P
0.017

Si
0.25

A1 0.035

Nb 0.028

Ti
0.019

Foundation Item: Item Sponsored by National Natural Science Foundation of China (51074052) ; Fundamental Research Funds for Central Universities of China (N100607001) Biography:LAN Liang-yun(l983-), Male, Doctor Candidate; E-mail: lly. 1iangyunBgmail. com; Received Date: November 3, 2009

58

Journal of Iron and Steel Research, International

Vol. 18

than the maximum value prescribed in the API spec 5L standardC6'. T h e Nb and Ti elements as main microalloyed elements were added in it. In view of the elements of S and P great damage to toughness, these contents ( i n mass percent) were limited to 0. 003% and 0. 017% respectively. T h e materials, 100 m m X 100 m m X 150 mm in size, for hot rolling were cut from the forged slabs. The hot rolling experiment was carried out through varying TMCP conditions on pilot rolling mill with twin rolls of 450 mm in diameter. Details of rolling conditions are shown in Table 2. All steels were hot rolled to 10 mm-thick plates through a two-stage controlled rolling process. T h e first stage rolling was controlled in the recrystallized austenite region
Table 2
Steel

at high temperature with heavy reduction in order to refine the original austenite size, while the second stage rolling was controlled in non-recrystallized austenite in low temperature region above Ar3. Specimens for tensile and impact tests were cut from middle of the rolled plates in the transversal direction. Round tensile specimens with a gauge diameter of 8 mm and a gauge length of 40 mm were tested at ambient temperature at a crosshead speed of 5 mm/min using a SANS 10 kN servo-hydraulic machine. To evaluate the Charpy impact energy, sub-size (7. 5 mm X 10 mm X 10 m m ) standard Charpy V-notch specimens were conducted over a temperature range from -60 "C to room temperature in accordance with the standard method of ASTM-E 8M.

The rolling schedule and measured processing temperatures of the experimental steels
Rough rolling region Finishing temperature/% Finish rolling region Beginning temperature/% Finishing temperature/C Acceleration cooling Cooling stop temperature/% Cooling rate/ (% *
s-1)

A
B C

1040 1040 1060 1060 100--73+50+33

940 940 870 868 33+25+19.5+15.5+12+10

925 840 820 810

680 675 590 560

33 22 32 34

D
Schedule/mm A-D

T h e longitudinal direction plates of the hot rolled steels were polished and etched by 2 % of Nital solution, and microstructures were observed by FEI Quanta 600-scanning electron microscope ( SEM ). After SEM observation all the specimens were electrochemically polished in a solution containing 70 % of ethanol, 22% of distilled water and 8 % of perchloric acid (in volume percent), operating at 30 V and -25 O . EBSD analyses were carried out in SEM C equipped with a conventional EBSD system at the resolution step of 0.2 pm on the area of 70 pmX80 pm. T o quantify the effective grain size ( d ) between high-angle boundaries (>15") defined by M D Fuentes et alCln1,misorientation profiles were obtained from lines traced on orientation imaging maps, and a linear intercept method was used to compute this value. In order to examine cleavage facet size which is closely related to the toughness of material, cleavage fracture surfaces of the CVN specimens fractured at -60 'C were also observed by SEM.

properties of pipeline steels by optimizing microstrucIn tures subjected to different rolling this experiment, microstructures are composed of many different phases including QF, P (pearlite) , G F and AF or BF. T h e microstructures of the A and B steels rolled at high finish rolling and cooling stop temperature are shown in Fig. 1 (a) and ( b > respectively. T h e microstructures are mainly composed of

2
2.1

Results and Discussion

Microstructures It is a valid way to achieve excellent mechanical
(a) A steel;

(b) B steel;

(c) C steel;

(d) D steel.

Fig. 1

SEM micrographs of all the steels

Issue 2

Microstructural Evolution and Mechanical Properties of Nb-Ti Microalloyed Pipeline Steel

59

QF, together with P and little AF. T h e QF grains

have irregular and jagged boundaries with high dislocation density and little dispersed M / A constituentC7. Since the QF transformation can be accomplished by short-diffusion of interstitial (C) and substitutional ( N b ) atom across transformation interfacesC8, it can be observed that carbides discontinuously appear at the QF grain boundaries. The microstructures of the C and D steels are shown in Fig. 1 (c) and (d) respectively. As low finish rolling and cooling stop temperature, the AF formed in middle temperature is the major microstructure together with GF and QF. The AF with excellent mechanical properties may be an optimal microstructure for pipeline steels
Table 3
Steel Yield strength/MPa
485 490 545 580

because it includes high dislocation density and dispersed M/A constituent between the ferrite plates.

2.2

Tensile properties

T h e tensile properties of all the steels tested at room temperature are listed in Table 3 , as well as their stress-strain curves are represented in Fig. 2. T h e strength of AF together with G F and QF microstructures is much higher than that of QF together with P and AF microstructures. By decreasing the finish rolling and cooling stop temperature the substructure and dislocation with the high density are formed and retained in austenite, which increase the nucleation sites of the AF and promote the AF transfor

Tensile properties and impact absorbed energy of all the steels

Tensile strength/MPa
595 600 670 700

Elongation/ %
23 20 25 20

Yield ratio/ %
0. 82 0. 82 0. 8 1 0. 83

Absorbed energy/J
-10 75 77 135 147

-40 55 65

-60 47 40

A B C D

145
160

130 114

0.02

0.06

0.10 True strain

0.14

01 .8

Fig. 2

True strain-true stress curves of all experimental steels

mation, and it is beneficial to refine the microstructure and improve the ~ t r e n g t h ~ ~Meanwhile the . yield ratios, the ratio of yield strength to tensile strength, maintain a low constant about 0. 82 rather than increase with the increase of yield strength. That is to say, the microstructures of AF together with GF and QF can improve the yield strength and keep the low yield ratio. This is consistent with the result of Kim studiedC7.

2.3

Impact toughness and fracture behaviors

The CVN impact toughness of all the steels tested at various temperatures are also listed in Table 3. T h e toughness of the A and B.steels is very low at

all test temperatures, while the C and D steels having AF matrix perform excellent low temperature toughness. Fig. 3 ( a ) and ( b ) show SEM fractographs of CVN specimens of the A and D steels fractured at -60 O respectively. Cleavage facet size, an C important factor influencing the toughness of material, can be measured by fractographs, and it is related to but appears to be somewhat larger than the effective grain size which will be discussed below since cleavage cracks are deflected at the high misorientation b o u n d a r i e ~ ~ ~ -T h e cleavage facet size of the A ~~ steel is measured to be about 10 pm, larger than that of the D steel (about 6 pm). On the other hand, the fractions of cleavage fracture area of the A and B steels are larger than that of the C and D steels according to macrofractograghs. Especially no cleavage fracture phenomenon appears on the C steel fractograph fractured at - 60 C, which illustrates that the C steel has the best excellent toughness in this experiment. According to Eqn. (1) derived for the ductile-brittle transition temperatures T D B T of low-alloy ferritic steels established by F B P i ~ k e r i n g ~ ~ , the T D B T of material can be improved by 22 C when containing P of 10% in microstructures. Therefore it can be inferred that the P causes a great damage to the toughness of A and B steels. T~~~=-19+44zela+700wNtn-11. 5d-+2. 2 ~ (1)

60

Journal of Iron and Steel Research, International

Vol. 18

Fig. 3

( a ) A steel; ( b ) D steel. SEM fractographs of CVN specimens fractured at -60 c

where, wN(f) nitrogen not combined as a stable niis tride; and d is effective grain size. 2.4

EBSD analyses It is well known that good toughness of the mi-

crostructures is closely related t o small effective grain size or high density of high angle grain boundaries which can be measured by EBSD technique. High angle boundaries can act as obstacles to cleavage propagation, forcing the cleavage crack to change

the microscopic plane of propagation. Low angle boundaries seem to have no influence on the toughness of steels. From this reason, in order t o discuss fracture mechanics, it is more convenient t o use the concept of crystallographic packet, defined by A F Gourgues et alc13*191, corresponding t o grains or sets of adjacent units sharing the same crystallographic orientation. Fig. 4 ( a ) to ( d ) represent image quality maps and orientation image maps of the A and D steels. The

Fig. 4

( a ) , (b) A steel; ( c ) . (d) D steel. Image quality maps and orientation image maps

Issue 2

Microstructural Evolution and Mechanical Properties of Nb-Ti Microalloyed Pipeline Steel

61

image quality maps are built up by grain orientation contrast. Owing to the overlapping of the Kikuchi pattern coming from the small size of AF plates analyzed in the conventional EBSD system, the shape of AF plates could not be accurately represented in the Fig. 4 (c). T h e orientation image maps display grain orientations in unique colors dedicated to each crystallographic plane index, and each point that belongs to these planes exhibits with its neighbor points a misorientation lower than a certain ( 15") tolerance angle. Some dispersed dark gray colors corresponding to the low pattern quality are usually caused by lath boundaries or carbide particles, even pearlite phase shown in orientation image map of the A steel. Fig. 5 ( a ) to ( d ) reveal misoriention maps of the A to D steels respectively after cleaning up the low pattern points. Light grey lines represent low angle boundaries (10" - 15") , while dark grey lines represent high angle boundaries (15" or more). According to the misorientation maps of the A to D steels shown in Fig. 5 , the fraction of high angle boundaries bf the A to D steels is 87.7%, 86.5%, 89. 7 % , and 87. 8% respectively. High angle boundaries play an important part in the toughness of material because they are usually thought as a sufficient

(a)

A steel; (b) B steel; (c) C steel; (d) D steel. Fig. 5 Misorientation maps of all steels
IW

condition for the crack arrest which can force the cleavage clacks to change the microscopic plane of p r o p a g a t i ~ n " ~ - ' ~ ]In terms of the linear intercept method, the effective grain size of the A to D steels is 6. 6 , 6. 9 , 4 9 , and 5. 8 pm respectively. The . small effective grain size is the primary determinant attribution to excellent toughness of material. In a word, these results can properly explain that the toughness of the C and D steels are more excellent than that of the A and B steels, because the crack propagation path in AF matrix steel is much more bent than that in QF matrix steelCzo1. Comparing the orientation image maps and the misorientation maps with the SEM microstructures, it is interesting observed that each QF grain become effective grain because of its high angle boundaries with misorientation of 15" or more, which can be confirmed by Fig. 6 ( b ) . An AF grain size shown in the image quality figures does not become an effective grain size, but the AF packet containing several adjacent grains with low misorientation becomes the effective grain, which can be confirmed by Fig. 6 (a). And it is worth pointing out that each AF crystallographic packet contains several morphological packets formed by parallel plates observed by SEM. Therefore the SEM images define much finer microstructures than those visualized in the orientation image maps. Misorientation profiles of different microstructures were investigated along lines selected in orientation image maps of the D steel, as shown in Fig. 6 ( a ) to (c). Fig. 6 ( a ) represents the misorientation angle varied within an A F packet along the line ( a b ) . It is revealed that the point to point and point to origin misorientation angles are lower than 7. 5" and 15" respectively. And the curves exhibit a fluctuant variation which indicates that the AF microstructures consist of high intricate plates with lots of internal low angle boundaries and high density of dislocation. It is a major factor to result in the improvement of the strength of the C and D steels. Meanwhile the length of this AF packet is more than 20 pm, which indicates that the size of AF packets to some extend enl-

LU

15

60
20
0

10 5 4

Point to origin

1 2 1 6 2 0

12

16 0

Fig. 6

Misorientation profiles of different microstructures corresponding to different lines selected in Fig. 5 (d)

62

Journal of I r o n a n d Steel Research, International

Vol. 18

arge instead of refining the effective grain size. The AF plates in pipeline steels, for this feature, are different from the AF plates in weld steels where each AF plate is considered as the effective grain. T h e reason is that the nucleation sites of the AF in pipeline steels are not so many as that in weld steels according to relevant literatureC'0"4-'7~21-2z1 Fig. 6 ( b ) represents the misorientation angle varied along the line ( c d ) across several QF grains. T h e misorientation angle abruptly boosts up to 60" when encountering QF grains boundaries and the distance between two adjacent high angle boundaries is about 2 . 5 4 pm. Therefore QF as the toughening structure in the C and D steels makes a significant contribution to refine the effective grain size. T h e misoriention angle varied along the line ( e f ) selected in a GF grain is shown in Fig. 6 (c). A few low angle boundaries in the G F grains are much less than those in the AF packets. T h e cleavage crack propagation in multiphase microstructures of AF together with QF is schematically described by Fig. 7c223.From the fracture viewpoint , the AF crystallographic packets and fine QF grains act the effective grains and their boundaries can effectively deflect the cleavage crack propagation resulting in excellent low temperature toughness.

2 ) T h e fine QF grains as the toughening structure in A F matrix were the effective grains with high
angle boundaries, while an AF packet containing several similar crystallographic orientations plates could become the effective grain. This kind of AF in crystallographic properties was different from the AF formed in weld steels because of the different nucleation mechanisms.
References:

c11

QF

Fig. 7 Schematic illustration of cleavage crack propagation in microstructures AF and QF

Conclusions

In this experiment, the pipeline steels with different microstructures were produced by varying the hot rolling conditions and the effects of different microstructures on mechanical properties were investigated by mechanical properties tests and EBSD analysis. 1) T h e steels rolled at low finish rolling temperature composed of AF and G F together with fine QF presented excellent mechanical properties ; but those rolled at high finish rolling temperature mainly composed of QF together with P and little AF showed low impact absorbed energy values since irregularly dispersed P and carbides in QF grain boundaries caused the low temperature toughness.

Nagahama Y, Yamamoto S. High Performance Steel Pipes and Tubes Securing and Exploiting the Future Demands [J]. NKK Tech Rev, 2001, 88: 81. C2l Shiga C, Hatomura T, Kudoh J I , et al. Development of Large Diameter High Strength Line Pipes for Low Temperature Services [J]. Kawasaki Steel Tech Rep, 1981, 4: 97. ZHAO Ming-chun, YANG Ke, SHAN Yi-yin. The Effects of C3l Thermo-Mechanical Control Process on Microstructures and Mechanical Properties of a Commercial Pipeline Steel [J]. Mater Sci Eng, 2002, 335A: 14. c41 Hwang B, Kim Y G , Lee S. Effective Grain Size and Charpy Impact Properties of High-Toughness X70 Pipeline Steels [J]. Metall Mater Trans, 2005, 36A: 2107. Kim Y M, Kim S K , Lim Y J , et al. Effect of Microstructure C5l on the Yield Ratio and Low Temperature Toughness of L i n e pipe Steels [J]. ISIJ Int, 2002, 42: 1571. [el American Petroleum Institute. API Specification 5L-2007 Specification for Line Pipe [S]. Washington: API, 2007. Krauss G, Thompson S W. Ferritic Microstructures in Continc71 uously Cooled Low- and Ultra-Low Carbon Steels [J]. ISIJ Int, 1995, 35: 937. Shanmugam S, Misra R D K , Hartmann J , et al. MicrostrucC8l ture of High Strength Niobium-Containing Pipeline Steel [J]. Mater Sci Eng, 2006, 441A: 215. Shibata K , Asakura K. Transformation Behavior and Microc91 structures in Ultra-Low Carbon Steels [J]. ISIJ Int, 1995, 35: 982. C l O l Smith Y E , Coldren A P, Cryderman R L. Mn-Mo-Nb Acicular Ferrite Steels With High Strength and Toughness [C] // Toward Improved Ductility and Toughness. Tokyo : Climax Molybdenum Company (Japan) Ltd, 1972: 119. Clll Xiao F R , Liao B, Shan Y Y, et al. Challenge of Mechanical Properties of an Acicular Ferrite Pipeline Steel [J]. Mater Sci Eng, 2006, 431A: 41. Wang W, Yan W, Yang K. Relation Among Rolling Parame t e n , Microstructures and Mechanical Properties in an Acicular Ferrite Pipeline Steel [J]. Mater and Design, 2009, 30: 3436. Gourgues A F, Flower H M, Lindler T C. Electron Backscattering Diffraction Study of Acicular Ferrite, Bainite, and Martensite Steel Microstructure [J]. Mater Sci Tech, 2000, 16: 26. Fuentes M D, Mendia A I, Gutierrez I. Analysis of Different Acicular Ferrite Microstructures in Low-Carbon Steels by Electron Backscattered Diffraction. Study of Their Toughness Behavior [J]. Metall Mater Trans, 2003, 34A: 2505. Kim Y M , Lee H , Kim N J. Transformation Behavior and c151 Microstructure Characteristics of Acicular Ferrite in Linepipe Steels [J]. Mater Sci Eng, 2008, 478: 361. Mabuchi H , Uemori R , Fujioka M. The Role of Mn Depletion C161 in Intra-Granular Ferrite Transformation in the Heat Affected Zone of Welded Joints With Large Heat Input in Structural

Issue 2

Microstructural Evolution and Mechanical Properties of Nb-Ti Microalloyed Pipeline Steel

Steels [J]. ISIJ Int, 1996, 36: 1406. Honeycornbe R W K , Pickering F B. Ferrite and Bainite in Alloy Steels [J]. Metal Trans, 1972, 3A: 1099. Edmonds D V, Cochrane R C. Structure-Property Relationships in Bainitic Steels [J]. Metell Trans, 1990, 21A: 1527. Nohava J , Hausild P, Karlik M. Electron Backscattering Diffraction Analysis of Secondary Cleavage Cracks in a Reactor Pressure Vessel Steel [J]. Mater Character, 2003, 49: 211. WANG Wei, SHAN Yi-yin, YANG Ke. Study of High

63

[17] [18] [19]

[21]

[22]

[20]

Strength Pipeline Steels With Different Microstructures [J]. Mater Sci Eng, 2009, 502A: 38. Gianetto J A , Braid J E M, Bowker J T, et al. Heat-Affected Zone Toughness of a TMCP Steel Designed for Low-Temperature Applications [J]. ASME, 1997, 119: 134. Kim Y M, Shin S Y ,Lee H , et al. Effects of Molybdenum and Vanadium Addition on Tensile and Charpy Impact Proper ties of API X70 Linepipe Steels [J]. Metal1 Mater Trans, 2007, 38A: 1731.