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603 © 2011 ISIJ ISIJ International, Vol. 51 (2011), No. 4, pp. 603–611 F460 Heavy Steel Plates for Offshore Structure and Shipbuilding Produced by Thermomechanical Control Process Dongsheng LIU, Binggui CHENG and Mi LUO Institute of Research of Iron and Steel (IRIS), Shasteel, Jinfeng Town, Zhangjiagang City, Jiangsu Province, 215625 P. R. China. (Received on August 19, 2010; accepted on December 25, 2010) Key parameters for controlled rolling and accelerated cooling process have been determined to indus- trially produce 45–50 mm heavy plates of microalloyed low carbon-equivalent SiMnCrNiCu steel for off- shore structures and shipbuilding. The plates were hot rolled from continuously cast slabs with a four-high 5000 mm width mill and cooled with an accelerate-cooling system. The process was characterized by heavy finish rolling reduction ratio over 63% in austenite non-recrystallization region and interrupted accel- erated cooling at 460°C to form quasipolygonal ferrite and acicular ferrite as majorities of microstructure. Yield-strength greater than 460 MPa was achieved at room temperature, and Charpy V notch impact energies of 150 to ~300 J were secured even at –80°C. Coarse granular bainite and/or degenerate upper bainite were identified harmful, causing cleavage fracture. The correlation between the fraction of high- angle grain boundaries (15 deg) and ductile-brittle transition temperature was derived quantitatively for the advanced heavy plates. The effect of heat input during heavy plate welding on the microstructure and mechanical properties in the coarse-grained heat affect zone was discussed. KEY WORDS: low carbon-equivalent steel; thermomechanical control process; advanced heavy plates; shipbuilding. 1. Introduction Significant industrial progress has been made in thermo- mechanical processing of plate steels since 1980’s. 1–6) Con- ventional TMCP, i.e., the combination of controlled rolling and accelerated cooling was employed to enhance micro- structure-refinement. The installations of advanced acceler- ated-cooling (AcC) equipment with precise control of the start- and end-cooling temperatures and cooling rate provid- ed means to produce advanced high plate steels with lean steel composition to maximize the weldability. 7) The novel combination of accelerated-cooling and on-line heat-treat- ment process was used to pave the ways to produce dual- or multiple-phase microstructures to enhance the toughness in high-strength advanced steels. 3,6) The transformed micro- structure can now be modified from ferrite-pearlite to range of complex low-temperature microstructures (i.e., acicular ferrite, bainite, austenite-martensite constituents, and the multiple-phase microstructures) by means of the accelerated cooling technology in advanced high-strength high-tough- ness plate steels. Grain-refinement simultaneously increase yield strength and toughness while other strengthening mechanisms (solute-hardening, precipitation-hardening, bainite transformation-hardening, etc.) deteriorates the toughness. 4) For advanced steel plates with the aforemen- tioned complex microstructures, however, better under- standing and quantifying the relationships among process- ing conditions, resultant-microstructure, and microstructure- properties relationships are still required. Extensive studies have been done to obtain in-depth understanding on the correlation among chemical composi- tion, process condition, microstructure and mechanical properties in linepipe steel plates and other structural steels. 8–10) Fine grained microstructures including quasispo- lygonal ferrite (QPF), homogenous acicular ferrite (AF), lower bainite (LB) and lath martensite (LM) with small effective grain size are preferred to achieve good combina- tion of high strength and low temperature toughness. Coarse granular bainite (GB), degenerate upper bainite (DUB) in association with coarse martensite-austenite (MA) constitu- ents give larger effective grain size, deteriorating the low temperature CVN impact performance. The studies were, however, restricted to laboratory and specific in-house scale process conditions. Advanced heavy steel plates with room temperature yield-strength (YS) of 420 MPa and above for offshore structures and ship in frigid sea area are required to secure high strength and superior low temperature toughness. These plates are developed word wide to meet the market demand. 7,11–17) The heavy plates with YS greater than 460 MPa and ductile fracture behaviour during Charpy V notch (CVN) impact tests at –40°C are of major developments. 13–17) Few steel producers have developed advanced steel plates with required CVN property at –60°C. 7,12) Recently, plates in conformity with Det Norske Veritas NV–F460 specifica- tions, i.e., a minimum yield strength of 460 MPa, and secured minimum CVN impact energy of 31 J at tempera- tures down to –60°C, have been developed using TMCP with lean steel composition and low carbon equivalent to achieve maximized weldability. 18,19) In view of limited

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Page 1: F460 Heavy Steel Plates for Offshore Structure and

603 © 2011 ISIJ

ISIJ International, Vol. 51 (2011), No. 4, pp. 603–611

F460 Heavy Steel Plates for Offshore Structure and Shipbuilding Produced by Thermomechanical Control Process

Dongsheng LIU, Binggui CHENG and Mi LUO

Institute of Research of Iron and Steel (IRIS), Shasteel, Jinfeng Town, Zhangjiagang City, Jiangsu Province, 215625 P. R. China.

(Received on August 19, 2010; accepted on December 25, 2010)

Key parameters for controlled rolling and accelerated cooling process have been determined to indus-trially produce 45–50 mm heavy plates of microalloyed low carbon-equivalent SiMnCrNiCu steel for off-shore structures and shipbuilding. The plates were hot rolled from continuously cast slabs with a four-high5000 mm width mill and cooled with an accelerate-cooling system. The process was characterized byheavy finish rolling reduction ratio over 63% in austenite non-recrystallization region and interrupted accel-erated cooling at 460°C to form quasipolygonal ferrite and acicular ferrite as majorities of microstructure.Yield-strength greater than 460 MPa was achieved at room temperature, and Charpy V notch impactenergies of 150 to ~300 J were secured even at –80°C. Coarse granular bainite and/or degenerate upperbainite were identified harmful, causing cleavage fracture. The correlation between the fraction of high-angle grain boundaries (≥15 deg) and ductile-brittle transition temperature was derived quantitatively forthe advanced heavy plates. The effect of heat input during heavy plate welding on the microstructure andmechanical properties in the coarse-grained heat affect zone was discussed.

KEY WORDS: low carbon-equivalent steel; thermomechanical control process; advanced heavy plates;shipbuilding.

1. Introduction

Significant industrial progress has been made in thermo-mechanical processing of plate steels since 1980’s.1–6) Con-ventional TMCP, i.e., the combination of controlled rollingand accelerated cooling was employed to enhance micro-structure-refinement. The installations of advanced acceler-ated-cooling (AcC) equipment with precise control of thestart- and end-cooling temperatures and cooling rate provid-ed means to produce advanced high plate steels with leansteel composition to maximize the weldability.7) The novelcombination of accelerated-cooling and on-line heat-treat-ment process was used to pave the ways to produce dual- ormultiple-phase microstructures to enhance the toughness inhigh-strength advanced steels.3,6) The transformed micro-structure can now be modified from ferrite-pearlite to rangeof complex low-temperature microstructures (i.e., acicularferrite, bainite, austenite-martensite constituents, and themultiple-phase microstructures) by means of the acceleratedcooling technology in advanced high-strength high-tough-ness plate steels. Grain-refinement simultaneously increaseyield strength and toughness while other strengtheningmechanisms (solute-hardening, precipitation-hardening,bainite transformation-hardening, etc.) deteriorates thetoughness.4) For advanced steel plates with the aforemen-tioned complex microstructures, however, better under-standing and quantifying the relationships among process-ing conditions, resultant-microstructure, and microstructure-properties relationships are still required.

Extensive studies have been done to obtain in-depth

understanding on the correlation among chemical composi-tion, process condition, microstructure and mechanicalproperties in linepipe steel plates and other structuralsteels.8–10) Fine grained microstructures including quasispo-lygonal ferrite (QPF), homogenous acicular ferrite (AF),lower bainite (LB) and lath martensite (LM) with smalleffective grain size are preferred to achieve good combina-tion of high strength and low temperature toughness. Coarsegranular bainite (GB), degenerate upper bainite (DUB) inassociation with coarse martensite-austenite (MA) constitu-ents give larger effective grain size, deteriorating the lowtemperature CVN impact performance. The studies were,however, restricted to laboratory and specific in-house scaleprocess conditions.

Advanced heavy steel plates with room temperatureyield-strength (YS) of 420 MPa and above for offshorestructures and ship in frigid sea area are required to securehigh strength and superior low temperature toughness.These plates are developed word wide to meet the marketdemand.7,11–17) The heavy plates with YS greater than 460MPa and ductile fracture behaviour during Charpy V notch(CVN) impact tests at –40°C are of major developments.13–17)

Few steel producers have developed advanced steel plateswith required CVN property at –60°C.7,12) Recently, platesin conformity with Det Norske Veritas NV–F460 specifica-tions, i.e., a minimum yield strength of 460 MPa, andsecured minimum CVN impact energy of 31 J at tempera-tures down to –60°C, have been developed using TMCPwith lean steel composition and low carbon equivalent toachieve maximized weldability.18,19) In view of limited

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availability of relevant information, however, further inves-tigation is necessary to correlate the process parameters ofindustrial operation to microstructure-mechanical propertiesrelationship for optimizing the productivity and quality sta-bility of the plate products with thickness (t) of ∼50 mm.

The production of NV-F460 class ultra high strengthheavy-thickness (45–50 mm) steel plates via TMCP routewith lean steel composition is challenging when the maxi-mum continuously cast slab thickness and mill configura-tion are limited. Key parameters for specific TMCP aredependent upon steel composition to achieve desired micro-structures consisted of QPF, AF, GB, DUB and MA, and tar-get mechanical properties. Integrated consideration anddetailed database are necessary to bridge the considerablegap between laboratory observations and industrial process.However, such information is not adequate for the advancedheavy steel plates with the thickness of ~50 mm. In thepresent work, therefore, a series of full scale industrial pro-duction trials was conducted to quantify the correlation ofTMCP processing, microstructures and mechanical proper-ties in the NV-F460 class shipbuilding plates. 50 mm thickplates with room temperature yield-strength greater than460 MPa, and assured low temperature CVN toughness of~300 J even at –80°C were produced providing a new areafor the technology. The microstructural factors were charac-terized and quantitatively correlated with the ductile-brittletransition temperature in the industrially produced steel plates.

2. Experimental

The chemical composition of the continuously cast (CC)slabs used for industrial rolling trials is shown in Table 1.Carbon equivalent of 0.38 and Pcm value of approx. 0.17were chosen to maximize the weldability. Slabs of 320 mmthickness were produced by an integrated system consistedof basic oxygen furnace, ladle furnace, RH degassing unitand vertical-bending slab caster. Measures were taken toachieve sufficient steel cleanliness to meet the demandingtoughness. Soft reduction was applied to reduce centre seg-regation in the slabs.

The layout of the process and facilities with pusher typeslab furnaces, four-high 5000 mm width heavy plate mill,accelerated cooling system (MULPIC-AcC), hot leveling,etc, is presented in Fig. 1. After reheating the slab at 1200°Cfor two hours, the slab was subjected to descaling, roughrolling, delay, finish rolling, lamellar water flow cooling,hot leveling, and ultrasonic detection. Two-stage rolling,

i.e., hot deformation at austenite recrystallization region andnon recrystallization region with systematically variedfinish rolling reduction ratio (FR) of 44%, 63% and 69%,was conducted. For convenience, the plates are referred asFR44, FR63, and FR69, in accordance with the low (44%),moderate (63%) and high (69%) FR, respectively.

Polished surface along thickness (ND) and finish rollingdirection (RD) at center thickness (t/2) and quarter thickness(t/4) was etched in a 4% nital solution and observed by anoptical microscope (OM) and a field emission scanningelectron microscope (SEM) equipped with an EBSD camera(FEI’s model Quanta 3D FEG). The EBSD analysis(resolution: 0.2 μ m) was conducted and the data were theninterpreted by HKL technology Channel 5 software. Thesesamples were also subjected to micro-hardness measure-ments at 10 kg load employing a digital closed-loopcontrolled Vickers hardness tester (model: Tukon 2100B,Instron). To examine the cleavage fracture facets, thefractured surfaces of the CVN samples fractured at –196°Cwere observed by the SEM.

Mechanical properties in transverse-direction (TD) andRD at t/2 and t/4 were tested for the 45 and 50 mm plates.Round tensile samples with 8 mm gage diameter weremachined and tested at room temperature at a crossheadspeed of 5 mm/min by a 250-kN Instron machine (modelInstron 5585H, Instron Corp., Canton, MA). The yieldstrength was measured at the 0.2% offset stress. CVNimpact tests were performed on standard samples (size:10×10×50 mm) with the V notch parallel to ND at –196°Cto 0°C by a 450-J instrumented pendulum impact tester(model IMP450J Dynatup, Instron). A regression analysisfor absorbed impact energy versus test temperature was con-ducted with a hyperbolic tangent curve fitting method.

The hot rolled plates were further heat treated under strainaging conditions. For that, samples were taken at t/4 of theplates in RD and TD and subjected to elongation strains (εe)of 5% and 10%, respectively, and then aged at 250°C for 1h. Standard CVN samples were tested at –60°C.

To investigate the microstructure and properties of thecoarse grained heat affect zone (CGHAZ) of welds, rectangu-lar specimens of 10×10×75 mm were made from the 50 mmthick plate (FR69) in 10 mm sections of the plate at t/4 andt/2. The HAZ simulations were performed using a Gleeble3800 thermomechanical simulator employing the Rykalin-3D(thick plate) heat transfer model. A Pt-10 pct Rh thermocou-ple was spot welded at the central length of the specimens forrecording the temperature. The specimens were heated at130°C/s to a peak temperature (Tp) of 1350°C, held, for 0.1second, and cooled at different cooling times for the stipulat-ed range of 800°C to 500°C (t8/5) to be equivalent to a weldheat input of 1.5 to 30.0 kJ/mm. CVN specimens were madewith the notch at the central length, i.e., the spot welded ther-mocouple position along the original ND-TD orientation of

Table 1. Chemical composition of the experimental steel (mass, %).

C Si Mn P S Al Nb+V+Ti Cu+Ni+Cr Ceq Pcm

0.062 0.23 1.47 0.008 0.002 0.040 0.094 0.60 0.38 0.17

Fig. 1. Schematic layout of the 5000-mm width heavy-plate shop in Shasteel.

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the plates, and the CVN impact energies were measured at–60°C in the same way aforementioned.

3. Results

3.1. Industrial TMCP-AcC ProcessKey TMCP-AcC parameters for each plate investigated

including the total rough rolling reduction ratio (RR), thetotal FR, finish rolling entry temperature (Tin) and exittemperature (Tout), AcC cooling rate (φ) and AcC finishtemperature (TF) are listed in Table 2. All the recordedtemperatures were measured on the plate top surface. Roughrolling was finished at temperatures higher than 980°Cresulting in 90 mm, 120 mm and 160 mm thick transfer bars.The transfer bars were held and cooled on the cooling bed(delay) to meet finish-rolling temperature, and then finish-rolled as plates FR44, FR63 and FR69, respectively.

Austenite hot deformation constitutive behaviour andstatic recrystallization have been studied for the NV-F460grade shipbuilding steel.18) A peak strain observed on thestress-strain curves which indicated the start of dynamicrecrystallization was 0.35 at 1100°C at the strain rate of 1s–1. Stress-strain curves of austenite with a grain size (dγ) of100 μ m were measured at 1150 and 1200°C in the presentwork employing the same approach described in Ref. [18].The results are presented in Fig. 2 where the peaks on stress-strain curves indicate the occurrence of dynamic recrystal-lization. According to the individual pass rolling schedules(the maximum pass strain was less than 0.22 with strainrates of 2 to 4 s–1, which is less than the peak strains), there-fore, static recrystallization should be the dominant soften-ing and grain refinement mechanisms during rough rollingfor which the solute drag mechanism of microalloying ele-ments is taken into account at temperatures higher than950°C. As expected, work-hardened (pancaked) austenitemicrostructure is achieved during finish rolling.

3.2. MicrostructureFor the 50 mm plate FR44, the results of microstructure

characterization are shown in Figs. 3 and 4. The OM image(Fig. 3(a)) along the ND×RD section at t/2 presents themicrostructures consisted of fine QPF grains, predominanceof coarse GB associated with secondary phases (Fig. 3(b))which were identified by SEM as martensite-austenite (MA)constituents. The sample used for the OM and SEM obser-vations was further examined by EBSD analysis. The orien-tation image map (OIM) with high-angle (≥15 deg) grainboundaries marked in dark lines indicates the coexistence offine QPF grains (≤6 μ m) and coarse GB colonies at approx-imately 70 μ m at the t/2, as shown in Fig. 4. The subgrainsin the coarse GB formed in identical austenite grain havesimilar crystallite angles to one another and thus the effec-tive grain size of the GB is large.

Figures 5(a) and 5(b) are OM micrographs of plate FR69with FR of 69%. Various phases presented in the microstruc-tures are marked in the micrographs. The Vickers hardness(HV) data are also indicated. The microstructures at the t/4section are more refined than those at the t/2 leading to high-er hardness. The near surface materials may be exposed tothe cooling rate which is faster than that of the bulk resultingin finer microstructure and higher hardness. The effect ofFR on microstructure has been revealed by comparing themicrostructures in Figs. 3 and 5. The FR of 69% led to thepredominance of AF+QPF and refined GB in plate FR69.The secondary phases are mainly degenerate pearlite (DP)instead of MA constituents as it is the case for plate FR44.Inverse pole figure (IPF) maps obtained by EBSD analysisare shown in Figs. 6(a) and 6(b) for t/2 and t/4. The effectivegrain size of GB is refined to approximately 20 μ m at t/2due to the increased FR.

Figures 7(a) and 7(b) are OM images showing AF andDUB grains in plate FR63 at t/2 and t/4. SEM images, show-ing the difference of the microstructures at t/2 and t/4 andthe secondary phases of DP, are given in Figs. 7(c) and 7(d).

Table 2. Key TMCP-AcC parameters in the industrial rolling trials.

PlateNo.

t RoughRolling Finish Rolling Accelerated cooling

(AcC)

mm RR (%) Tin (°C) Tout (°C) FR (%) φ (°C/s) TF (°C)

FR44 50.0 72.0 835 793 44.0 13.0 490

FR63 45.0 63.0 855 829 63.0 13.0 460

FR69 50.0 50.0 777 808 69.0 11.3 463

Fig. 2. Flow stress behaviour of austenite observed during single hitcompression tests at the deformation condition as indicated.

(a)

Fig. 3. (a) OM and (b) SEM images for microstructure in plateFR44 at t/2.

(b)

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The microstructure at t/4 is finer than that at t/2. IPF mapobtained by EBSD analysis at t/2 is shown in Fig. 8. CoarseDUB grains are observed which formed in elongated (pan-caked) austenite grains with low angle grain boundaries.

3.3. Mechanical PropertiesThe mechanical properties including yield strength (YS),

ultimate tensile strength (UTS), total elongation (EL), yieldratio (YR=YS/UTS) and CVN impact energies measured at–40°C to –80°C are given in Table 3.

Fig. 4. OIM (Euler angle color scheme) with misorientation angle(≥15 deg) for ferrite domain boundaries (thick black lines)at t/2 of plate FR44.

(a) FR69, t/2

(b) FR69, t/4

(c) FR69, t/4Fig. 5. OM and SEM images for microstructures in plate FR69. (a)

OM, t/2; (b) OM, t/4; (c) SEM, t/4.

(a) FR69, t/2

(b) FR69, t/4Fig. 6. IPF map showing grains and high angle (≥15 deg) grain

boundaries (thick black lines) in plate FR69 at (a) t/2 and(b) t/4.

(a) FR63, t/2 (b) FR63, t/4

(c) FR63, t/2 (d) FR63, t/4

Fig. 7. OM and SEM images for microstructures produced in plateFR63 at t/2 and t/4.

Fig. 8. IPF map showing grains and high angle (≥15 deg) grainboundaries (thick black lines) in plate FR63 at t/2.

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The room temperature tensile properties of all the platesinvestigated met the specification for NV-F460 steel. Figure9 shows room-temperature stress-strain curves of the plates.Plate FR44 shows a continuous yielding behavior. This isdue to the high fraction of MA constituents (see Fig. 3)which promotes mobile dislocations at boundaries betweenthe hard secondary phases and the nearby soft phases. Otherplates show discontinuous yielding behaviour because ofless MA particles as observed in Figs. 5 and 7. The effectof rolling process on the yield strength may be negligible.The YS at t/4 is, however, 40–60 MPa higher than that at t/2which is consistent with the previous microstructure obser-vations and hardness measurements for all the plates.

The increase of FR during rolling leads to significantimprovement on the CVN performance. Brittle fractureswere observed during Charpy impact testing at temperaturesbelow –40°C showing CVN impact energies lower than 31J in plate FR44. As a result, the plate cannot meet the min-imum requirement for NV-F460 grade. In the other twoplates (FR63 and FR69), the CVN impact energies at –60°Cwere well above the 31-J, exceeding the minimum require-ment for F460 steel. The CVN impact performance at t/4 isgenerally better than that at t/2 (see CVN energies measuredat –80°C). Some CVN samples taken at t/2 of plate FR63,where GB grains were observed, exhibited brittle fracturebehaviour at –80°C. All CVN samples taken from the FR69plate, however, exhibited ductile fracture behaviour withimpact energy ranged from 150 to ~300 J even at –80°C.

Figures 10(a) through 10(d) show the Charpy absorbedenergy data as a function of the test temperature from whichan upper-shelf energy (USE) of approximately 330 J isdetermined for all the plates and the energy transition tem-peratures (ETT) are indicated, accordingly.

During the construction of ship hull structures, the platesare subjected to cold leveling, roll bending, press forming,etc. Strain aging occurs that results in increased strength anddecreased ductility and toughness. The CVN testing wastherefore conducted according to the procedures defined inthe approval of manufacturer and the CVN impact energiesat –60°C are listed in Table 4. The CVN properties of plateFR69 meet the target for F460 steel with sufficient margineven under the strain aging conditions.

The curves of CVN impact-load combined with impact-energy versus hammer displacement were plotted and ana-lyzed according to the data recorded by the instrumentedCharpy machine.20–22) The effects of tested temperature andstrain aging on the CVN impact properties are shown inFigs. 11(a) and 11(b). The CVN samples taken from plateFR44 exhibited different load-displacement behaviours atthe temperatures of 0°C and –40°C (see Fig. 11(a)). A duc-tile behaviour was observed at 0°C, where a 70-J crack-ini-tiation energy, a 150-J crack-propagation energy and a 100-J post fracture energy were differentiated from the curves.The post fracture energy may be a measure of crack arrestcapacity. A brittle behaviour was observed at –40°C, indi-cating that the absorbed energy in association with only thecrack-initiation stage without energy consumed during theabrupt brittle crack. In Fig. 11(b), the CVN load-displace-ment plots are given for the samples taken from RD- 1/4 tof plate FR69 tested at –60°C, –80°C, strain-aged with 10%

Table 3. Mechanical properties of the plates produced by theindustrial-scale rolling trials.

PlateNo.

t(mm) Location YS

(MPa)UTS

(MPa)EL(%) YR

CVN absorbed energy (J)*

–40°C –60°C –80°C

FR44 50 TD-t/2 472 613 23 0.77 45 (27) 28 (21) 11 (8)

TD- t/4 545 645 23 0.85 92 (26) 13 (10) 13 (9)

FR63 45 TD- t/2 493 621 23 0.79 302 (258) 317 (310) 173 (84)

TD- t/4 562 666 23 0.84 294 (253) 302 (300) 198 (80)

RD- t/2 481 613 23 0.79 311 (304) 198 (138) 68 (23)

RD- t/4 544 649 24 0.84 323 (316) 261 (217) 315 (303)

FR69 50 TD- t/2 477 606 21 0.79 305 (255) 282 (265) 227 (153)

TD- t/4 525 643 26 0.82 292 (261) 287 (277) 271 (240)

RD- t/2 465 599 24 0.78 291 (259) 293 (282) 243 (219)

RD- t/4 508 608 23 0.84 305 (269) 329 (318) 303 (295)

* Average energy of three specimens followed by parentheses with the minimum value.

(a)

(b)

(c)Fig. 9. Stress-strain curves measured at room temperature for

plates (a) FR44, (b) FR63, and (c) FR69 at t/2 and t/4,respectively.

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elongation strain (εe) and tested at –60°C. All the samplesdemonstrated ductile-fracture behaviour. The absorbed ener-gy at crack-initiation stage was 60 J for all the samples. Theenergies absorbed during crack-propagation were 270 J, 243J and 233 J, respectively, for the three tested conditions. Thepost-fracture energy for the strain aged sample was 60 J at–60°C.

Figures 12(a) and 12(b), 13(a) and 13(b) show SEM frac-tographs of the CVN samples at t/2 and t/4 taken from platesFR63 and FR69, respectively, fractured at –196°C. The fea-ture of the cleavage surface is dependent upon the micro-structures of each sample. At t/2 of plate FR63 where coarseDUB grains were observed, large cleavage facets sized ~50μ m were found (Fig. 12(a)). The lath structure and inter-lathbright particles indicate that the large cleavage facet origi-nated from a coarse DUB. At t/4 of plate FR63 where more

(a) ETT = –30°C (b) ETT = –60°C

(c) ETT = –80°C (d) ETT = –95°C

(e) ETT = –85°CFig. 10. Charpy absorbed energy versus test temperature. (a) FR44 at TD-t/2, ETT= –30°C; (b) FR63 at RD-t/2, ETT=

–60°C; (c) FR69 at TD-t/2, ETT= –80°C; (d) FR69 at TD-t/4, ETT= –95°C; (e) FR69 at RD-t/2, ETT= –85°C.

Table 4. CVN properties of plate FR69 under the strain aging con-ditions.

LocationCVN absorbed energy at –60°C (J)

εe= 0 εe= 5% εe=10%

TD- t/4 305, 277, 278 (287) 302, 315, 311 (309) 259, 266

RD- t/4 330, 339, 318 (329) 241, 286, 296 (274) 274, 304, 286

(a) FR44, TD- t/2

(b) FR69, RD- t/4Fig. 11. Load and Charpy impact energy versus hammer displace-

ment curves obtained in the instrumented impact tests forplates: (a) FR44 tested at 0°C and –40°C; (b) FR69 tested at–60°C, –80°C, strain aged and tested at –60°C, respectively.

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refined microstructures were observed (see Fig. 7), the max-imum size of cleavage facets were reduced to ~20 μ m (Fig.12(b)). Because the microstructures are more refined inplate FR69, the size of the maximum cleavage facet is below20 μm at t/2 and 10 μm at t/4, as shown in Fig. 13. Largecleavage facet is associated with long unit crack propagationpath and reduced ductile crack resistance. Fine-grained QPF,AF and refined DUB/GB are therefore required to decreasethe ETT in the advanced plates.

4. Discussion

4.1. TMCP ProcessAdvanced heavy plates with YS of 460 MPa and secured

ductile fracture at –60°C, i.e., NV-F460 steel plates, are pro-duced in the present work. Integrated TMCP-AcC specifi-cation has been defined to produce advanced F460 thickplates with the thickness of 45 to 50 mm based on the resultsof a series of industrial rolling. For the two-stage controlledrolling, one of the key process parameters is the FR of min-imum 63% to produce heavily work-hardened and non-recrystallizaed austenite to facilitate the transformation intofine-grained QPF, AF and refined DUB/GB microstructuresduring AcC. The best mechanical properties are achieved inplate FR69 with the highest FR. Long delay time is unavoid-able during rolling, and hence sequential multiple-platescross rolling strategy is recommended (e.g., three plates aresimultaneously on delay while one plate is being rolled).The productivity can be improved by 300% compared withsingle plate rolling method in mass production. In addition,AcC process is another key process step which shouldensure the entire continuous cooling transformation com-pleted at the defined cooling rates.18)

4.2. Effect of Microstructure Factors on MechanicalProperties

The microstructures vary when the FR changes in the aus-tenite non-recrystallization region. Different microstructuresare also observed at different locations across the plate thick-ness that results in the difference in mechanical properties. Forexample, coarse GB/DUB microstructures (Figs. 3 and 12)deteriorate the low temperature toughness while refined QPF/AF grains yield the best combination of strength and low tem-perature toughness in the heavy plates (see Fig. 13).

The microstructure factor, i.e., the distribution of grain-boundary misorientations taken from each EBSD measure-ment (see Figs. 4, 6 and 8) is quantified as shown in Figs.14(a) through (d). The average grain-boundary angle

(a) FR63, t/2 (b) FR63, t/4

Fig. 12. SEM fractographs of Charpy impact samples fractured at–196°C taken from plate FR44 at (a) t/2, and (b) t/4.

(a) FR69, t/2 (b) FR69, t/4

Fig. 13. SEM fractographs of Charpy impact samples fractured at–196°C taken from plate FR69 at (a) t/2, and (b) t/4.

(a)

(b)

(c)

(d)Fig. 14. Distribution of grain-boundary misorientations of (a) plate

FR44 at t/2, (b) plate FR69 at t/2, (c) plate FR69 at t/4, and(d) plate FR63 at t/2.

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(AGBA) and the fraction of high-angle grain boundaries(HAGB, which is greater than 15 deg) are also indicated.The AGBA and the fraction of HAGB increase as the FRincrease, leading to more refined microstructures. Further-more, the AGBA and the fraction of HAGB at t/4 are greaterthan those at t/2. The corresponding ETT data (TD-t/2 ofplate FR44, RD- t/2 of plate FR63, TD-t/2 and t/4 of plateFR69) are linearly correlated to the AGBA, and the fractionof HAGB, as shown in Figs. 15(a) and (b). The high AGBAand the high fraction of HAGB are correlated to low ETT.The ETT is more dependent on the AGBA than on the frac-tion of HAGB. Similar trends were found by Han et al.9) inthe experimental X80 steels. The present study, however,indicates that the ETT of the industrial NV-F460 plates ismore sensitive to the microstructure factors, i.e., the AGBAand the fraction of HAGB, because larger absolute slopesare observed (see Fig. 15) than these observed by Han etal.9) The above analysis emphasizes once again the signifi-cance of applying heavy FR to facilitate the formation offine microstructures with small effective grain size, highAGBA, and high fraction of HAGB. Insufficient FR leadsto the formation of coarse DUB and GB microstructureswith low AGBA, low fraction of HAGB, which are detri-mental to the low temperature toughness and give rise tohigh ETT.

4.3. WeldabilityThe coarse-grained heat affected zone (CGHAZ) adjacent

to the fusion line has the lowest toughness within the HAZ

because of large prior austenite grains. Appropriate heatinput must be employed during welding to control themicrostructures produced during continuous cooling andmechanical properties of the CGHAZ. Table 5 shows thehardness, CVN impact toughness measured under variousheat input conditions. Either the hardness or the CVNabsorbed energy decreases as the heat input increases. Whenthe heat input is 1.5 to 3.0 kJ/mm, excellent toughness val-ues are observed even at –60°C. At 5.0 kJ/mm and above,however, the impact toughness decreases substantially, notachieving the targets as defined for the parent F460-steelplates. The microstructures of the bulk materials at t/2 cor-responding to different CGHAZ conditions are shown inFig. 16. Similar series of microstructures were observed in

(a)

(b)Fig. 15. Relationship between (a) ETT and average grain boundary

angle, (b) ETT and the fraction of high-angle grain bound-aries.

Table 5. Mechanical properties in the simulated CGHAZ conditions.

Thickness t(mm) Location Heat input

(kJ/mm)Tp

(°C)t8/5(s)

Hardness(HV)

CVN absorbedenergy at –60°C (J)*

50

t/2 1.5 1350 3.9 310 341 (309)

t/4 1.5 1350 3.9 316 362 (331)

t/2 3.0 1350 7.7 278 254 (207)

t/4 3.0 1350 7.7 276 321 (285)

t/2 5.0 1350 12.9 254 179 (105)

t/4 5.0 1350 12.9 253 74 (21)

t/2 10.0 1350 25.7 230 32 (22)

t/4 10.0 1350 25.7 230 25 (23)

t/2 30.0 1350 77.2 205 11 (9)

t/4 30.0 1350 77.2 207 11 (10)

* Average energy of three specimens followed by parentheses with the minimum value.

(a) 1.5 kJ/mm (b) 3.0 kJ/mm

(c) 5.0 kJ/mm (d) 10.0 kJ/mm

(e) 30.0 kJ/mmFig. 16. The effect of heat input on microstructures in the CGHAZ

conditions.

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611 © 2011 ISIJ

the samples taken from t/4. At 1.5 kJ/mm, the microstruc-tures are mainly LB+LM that have high fraction of highangle grain boundaries23) and reduced effective grain size, asa result, give rise to the high strength (hardness) andenhanced ductile fracture resistance. At 3.0 kJ/mm, similarmicrostructure and hardness are observed that lead again toexcellent toughness even at –60°C. At 5.0 kJ/mm andabove, however, microstructures are featured by UB+GBassociated with coarse M/A constituents, that have low frac-tion of high angle grain boundaries and large effective grainsize,8–10,23) leading to decreased hardness and toughness.The present study suggests that the upper limit of heat inputduring welding practice for the investigated plate is 3.0 kJ/mm, which is generally consistent with the early study.18)

5. Conclusions

The effect of process parameters of industrial productionon microstructure and mechanical properties in amicroalloyed SiMnCrNiCu steel with lean composition hasbeen investigated to commercially produce heavy (45–50mm thick) plates of NV-F460 grade via thermomechanicalcontrol process (TMCP) for offshore structures andshipbuilding:

(1) Key TMCP parameters are determined to be (a)applying minimum 63% finish rolling reduction ratio in aus-tenite non-recrystallization region (Ttop≤850°C) followed by(b) accelerated cooling to ensure phase transformation com-pleted before (c) the interrupted cooling at 460°C on theplate surface.

(2) Best mechanical properties are achieved when 50mm thick plate is rolled heavily at 69% finish rolling reduc-tion ratio in austenite non-recrystallization region. The roomtemperature yield strength exceeds 460 MPa, and CVNimpact energies range from 150 J to 300 J even at –80°Cwith ductile fracture behaviour.

(3) The finish rolling reduction ratio affects the finalmicrostructure and mechanical properties of the heavyplates significantly. At 44%, coarse granular bainite anddegenerate upper bainite associated with MA constituentsare formed across the plate thickness. At 63%, acicular fer-rite grains are dominant, but coarse degenerate-upper-bain-ite grains of 40 μm are still observed at center thickness. At69%, fine-grained quasipolygonal ferrite and acicular fer-rite, refined degenerate-upper-bainite/granular-bainite grainsand degenerate-pearlite are produced as main secondary phas-es. The microstructures at quarter thickness are finer thanthose at center thickness leading to increased fraction ofhigh angle grain boundaries.

(4) The fractographs revealed by SEM indicate thatcoarse degenerate-upper-bainite grains create large cleavagefacets leading to deteriorated CVN properties. The low tem-

perature CVN properties are improved by the formation offine quasipolygonal ferrite, acicular ferrite and refineddegenerate-upper-bainite/granular-bainnite with high anglegrain boundaries due to increased finish rolling reductionrate.

(5) Linear relationships are found between the energytransition temperature and the average grain boundaryangle, and the energy transition temperature between thefraction of high-angle grain boundaries in the industriallyproduced NV-F460 plates.

(6) The upper limit of heat input during welding is 3.0kJ/mm to secure the CVN toughness of the coarse grainedheat affect zone at –60°C.

The above results, (1)–(6) have made it possible to indus-trially produce NV-F460 heavy plates.

AcknowledgementThe authors acknowledge financial support received from

Shasteel. Professor T. Emi is thanked due to constructivesuggestions about the project work and continuingencouragements. The authors are indebted to Ms. S. Chenand Dr. X. Zhang for arranging the industrial production.Able help received from Mr. H. Zhu and Mr. N. Xu, iswarmly appreciated.

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