DEVELOPMENT OF A HOT-DIP GALVANISED HIGH-STRENGTH, DEEP-DRAWING IF STEEL FOR MODERN AUTOMOTIVE APPLICATIONS

Marcel Lamberigts* and Frank E. Goodwin Centre de Recherches Mtallurgiques (CRM) * International Lead Zinc Research Organization (USA) INTRODUCTION Carmakers now tend to reduce the weights of their vehicles, or at the very least, to curb weight increases deriving from the introduction of additional safety and comfort pieces of equipment. The trend is clearly driven by environmental laws on fuel consumption and exhaust emission control. In this framework, the competition between materials will be intensified and, in the future, some long-held steel positions may start looking somewhat insecure. This is particularly true for frames and car body components, for which various manufacturers have already experienced with aluminium-based solutions. It is now generally recognised that the steel industry can only protect its market share by proposing new stronger grades, making it possible to go thinner and lighter. These materials must not only exhibit the desired level of mechanical strength, but also maintain an adequate deep drawing capability, as commonly measured by average Lankford coefficient r , isotropy r, and strain hardening coefficient n. At present, practically all car models feature electrogalvanised (EZ), pure zinc hotdip galvanised (GI) or galvannealed (GA) body protective coatings, allowing longterm anticorrosion guarantees. Combining high strength, deep drawing performances and adequate galvanisability however often proves challenging, and implies mastering all metallurgical mechanisms put in operation at every step of the production sequence. The steelmaking community has actively addressed this problem, as is testified by an impressive body of publications and international scientific conferences. In this context, the response of several high-strength deep-drawing steels to hotdip galvanising was investigated in the course of an earlier Rhesca simulationbased ILZRO project1. The target was to achieve yield strengths between 200 and 400 MPa, tensile strengths of about 500 MPa, elongations higher than 20%, Lankford coefficients over 2 and strain hardening coefficients of more than 0.2. It was concluded that, although these steels are somewhat more difficult to galvanise than reference IFs, conditions could always be worked out to obtain good quality coatings. This paper reports on a subsequent piece of work involving Rhesca simulation and pilot line continuous annealing and hot-dip galvanising. It was carried out on an experimental steel that had been shown to qualify as a satisfactory non-ageing, high-strength, deep-drawing material in the uncoated, cold-rolled and annealed condition. PILOT LINE EXPERIMENTS The experimental steel was cast by Willan Metals, Rotherham, UK, from a classical ULC-Ti IF feedstock supplied by British Steel Strip Products, now part of Corus Group (table 1). The material was then hotrolled at Corus Group, Brinsworth, UK, under conditions chosen to achieve fine ferrite grain and precipitate sizes, while minimising FeTiP precipitation. The material was supplied to CRM as a 0.6-mm thick coil in

the full-hard cold-rolled condition, to be hot-dip galvanised on the CRM pilot line C 30 N 20 S 90 P 400 Si 100

(figure 1).

Table 1: Experimental cast chemistry (ppm) Mn 14000 Al 400 Ti 300 Nb 220 B 20

Figure 1: CRM pilot line layout Because 0.6-mm thick coils can only be processed at a speed of 15 m/min, the cooling rate was always close to 25C/s between soaking and overageing. Annealing peak temperatures (780C, 800C and 820C) and N2-5%H2 protective atmosphere dew points (-22C and +5C) were selected to control pre-dip steel surface condition. Poorly reactive, oxidising element-containing steels can indeed be made amenable to hot-dip galvanising provided surface selective oxidation is made more internal than external in nature. Two composite coils were made of 3 small experimental steel sections (10 m in length) that had been welded to head, middle and tail ends of some commercial quality steel of exactly the same thickness. This way, all three annealing peak temperatures could be tested on each coil that was treated under the same protective atmosphere dew point (either 22C or +5C). It must be pointed out here that strip temperatures were measured by means of monochromatic optical pyrometers [System 4 Detector, Ge wavelength ( = 1.55 m)] located at fixed positions in the radiant-tube furnace, just below the gas jet cooling section and in the snout (figure 1). The coil processed at a dew point of 22C was under good control in terms of both temperature cycle and protective atmosphere oxidising potential. The situation was unfortunately definitely worse for the other coil, for which the measured annealing peak temperatures of experimental steel sections tended to raise way over the set point, in spite of the line operators efforts to moderate it (table 2). Table 2: Temperature control inaccuracy during high dew point annealing Taver (C) 816 870 879 Tmin (C) 790 813 851 Tmax (C) 848 923 896

It must be appreciated that the output signals [V (T, )] of monochromatic pyrometers are highly dependent on surface emissivity . Introducing inadequate emissivity values in the computation (est) can only result in grossly erroneous temperature readings (Test)2.
C V (T, ) = C1 5 exp 2 T C Test 2 Ttrue (K) = C 2 Test ln est true

before undergoing very fast cooling to preserve their surface condition. Thus treated panels exhibited a heterogeneous visual aspect, with some brighter and darker areas. They were also submitted to emissivity measurements carried out in a black body furnace, which led to widely scattered results (from 0.43 for both materials to 0.67 and 0.685 for the commercial quality and experimental steels, respectively). This strongly suggests that surface condition heterogeneity problems generated in the higher dew point protective atmosphere could account for the far-from-perfect in-line temperature control mentioned above. Depending on local emissivity and set point temperature, pilot line readings could indeed be overestimated by anything between 10C and 80C. Coating weight (expressed in g/m) was measured on-line with a Boyle RX detector (241Am source) placed along the strip axis between location 11 and exit bridle 12 (figure 1). It was shown to be under control, in spite of some degree of side-by-side heterogeneity. Slight differences between coils reflect variations in corresponding surface reactivity, in relation with emissivityaffecting modifications. Coating adhesion was furthermore excellent, as evidenced by cup-test mass losses comprised between 0.0003 and 0.0006 g/cup.
600
Tm ax = 870C

C1 and C2 are constants, while true and Ttrue are the true emissivity and temperature values, respectively. In an attempt to assess what the true emissivity was in the annealing furnace, specimens from both the experimental and commercial quality steels were submitted to the heat cycle of figure 2 in the Rhesca simulator.
1000
Air P u rg e N 2-5 % H 2 / D P = +5 C 8 00 C 1 33 C /m in

Temp erature (C )

800 600 400

7 C /s 2 0 C /s 2 0 C /s 6 00 C 5 00 C -1 s

200 0 0 1 2 3 T im e (m in ) 4 5

9 0 C /s

Figure 2: Rhesca surface conditioning The latter involved an oxidising preheating to 500C in air, to try and achieve an initial surface condition similar to that prevailing at the exit of the direct-fired furnace of the pilot line. The simulator chamber was evacuated, and an N2-5%H2 reducing atmosphere characterised by a dew point of +5C was established in it. The specimens were then rapidly reheated to 600C, and subsequently to 800C, at a rate similar to that prevailing in the radiant-tube section
(MPa)

500 400 300 200 100 0 0% D P = +5C 10% 20%

(% )
Tm ax = 816C

30%

40%

Figure 3: Typical true stress-true strain tension curves after high dew point annealing and hot-dip galvanising

Almost all test pieces machined from the experimental steel sections of the coils exhibited some limited yield point elongation (YPE), which turned exceptionally high for higher dew point and high apparent temperature annealing (figure 3). This situation should however not be considered negative, insofar as it reflects the materials expected resistance to secondary cold work embrittlement (CWE) and bake hardening (BH) capability. YPE can indeed be got rid of efficiently after adequate skin passing (figure 4).
600 500

on Lankford coefficient r (figure 5). Moreover, it does not affect coating adhesion (cup test mass loss between 0.0002 and 0.0006 g/cup). It is then fair to say that the experimental material meets the definition of high-strength, deep-drawing steel (YS 250 MPa, Eltot 30% and rTD 2). PROCESS OPTIMISATION The metallurgical reasons behind the property evolutions described above were sought for through a series of Rhesca simulations that were also designed to explore the ultimate performance limits allowed by the steel chemistry under consideration. More particularly, the effects of annealing peak temperature (between 800C and 920C) and cooling regime (slow cooling at 4.5 C/s or fast cooling at 115 C/s) on tensile properties, microstructure and texture were investigated. Rhesca panels were cut in the transverse direction from the full-hard, cold-rolled material. They were then subjected to the annealing cycles given by figure 6.
1000
800C 920C

(MPa)

400 300 200 100 0

TD DD RD

0% D P = +5C T m a x = 870C

10%

20%
(% )

30%

40%

Figure 4: Longitudinal (RD), transverse (TD) and diagonal (DD) true stress-true strain curves measured after skin passing As a matter of fact, skin passing always led to continuous tension curves, no matter how long the initial yield point elongation may have been. The treatment results in increased yield and tension strengths, but decreases uniform elongation and strain hardening, while remaining essentially neutral
2.8 2.6

N 2 -5% H 2 D P = -20C

Temp erature (C )

800
~ 133C/m in

600 400

600C

20C/s

200 0 0 60

Fast c ooling (115C/s)

S low c ooling (4.5C/s )

120

180

240

300

T im e (s)

r B efore SK P

2.4 2.2 2.0 1.8 1.6 1.4 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8

DP- 20C/RD DP- 20C/TD DP- 20C/Diag. DP+5C/RD DP+5C/TD DP+5C/Diag.

Figure 6: Annealing cycles imposed to full-hard Rhesca panels The latter, which were all carried out under the same protective atmosphere made of an N2-5%H2 mixture characterised by a dew point of 20C, were designed as an approximation to those actually undergone by the composite coils during pilot line processing. They consisted of a fairly rapid heating to 600C, to simulate direct-fired

r After S K P

Figure 5: Effect of skin passing on Lankford coefficients measured after hot-dip galvanising

furnace preheating, followed by a slower temperature ramp to annealing peak regu380 360 340

larly distributed between 800C and 920C (T = 10C).

24 22 20
S low Cooling

Fas t Cooling

YS (MPa)

300 280 260 240 220 780 800 820 840 860 880

ElU (% )

320
S low Cooling

18 16 14 12 10 8
Fas t Cooling

900

920

940

780 Afte r S K P 0 .3 0 .3

800

820

840

860

880

900

920

940

Afte r S K P 3 .5

T an n e al (C )

T an n e al (C )

3 .0
S low Cooling

rT

2 .5

0 .2 0 .2

S low Cooling

2 .0
Fas t Cooling

Fas t Cooling

1 .5 780 Afte r S K P 800 820 840 860 880 900 920 940

0 .1 780 Afte r S K P 800 820 840 860 880 900 920 940

T an n e al (C )

T an n e al (C )

Figure 7: Effects of annealing peak temperature and cooling rate on tensile properties measured after skin passing met, due to carbon diffusion (all cases) and Figure 7 illustrates the effects of annealing out-of-equilibrium microstructures (fast peak temperature and final cooling rate on cooling). As expected, these variations are some of the transverse mechanical propersmaller after slow - than after fast - cooling. ties measured after skin passing. These properties remain essentially constant be3.75 600 tween 800C and 880C, which suggests complete recrystallisation and structure sta500 3.5 bility. The only remarkable fact is that yield 400 strength is affected by the cooling rate after 300 3.25 annealing, presumably due to some carbon 200 having been made available by carbide dis3 r 100 solution and having an opportunity to precipitate again only under slow cooling con0 2.75 0% 10% 20% 30% 40% ditions.
(MPa)
T

It is worth noticing here that, based on the chemistry of table 1, the experimental steel under consideration is characterised by a theoretical / equilibrium transformation temperature of about 870C (Ae3). For annealing sequences carried out over the latter, yield and tensile strengths increase dramatically, and ductility features plum-

After S K P

(% )

890C

4.5C /s

Figure 8: Impact of Hutchinson effect on true stress-true strain tension curve and Lankford coefficient variation

rT

The most important observation concerns transverse coefficient rTD, which exhibits a sharp maximum around 890C, thus strongly suggesting some austenite memory effect (Hutchinson effect), whatever the cooling rate may have been3. It must however be pointed out that these extreme aver-

age transverse Lankford coefficients derive from highly variable instantaneous values, but such a material would certainly be particularly well suited for deep drawing (figure 8).

810C - 4.5C/s

810C - 115/s

890C - 4.5C/s

890C - 115C/s

Figure 9: Effects of annealing peak temperature and cooling rate on optical microstructure Figure 9 illustrates part of the evolution of the bulk microstructure with annealing peak temperature and cooling rate. Complete recrystallisation seems to be achieved already at 810C, but allotropic transformation does apparently not take place below 890C. Once austenisation has finally occurred, subsequent cooling leads to either a coarse isotropic polygonal or clearly acicular ferrite structure, depending on whether it is performed at 4.5C/s or 115C/s. Optical micrographs are certainly no sufficient evidence to assess full recrystallisation and incipient transformation temperatures. It is also necessary to discriminate between rolling-inherited and annealinginduced grain orientation features. This can be done reliably by way of texture analysis under the scanning electron microscope. The method is based on the so-called Kikuchi pattern created by continuous electron back scattering diffraction (EBSD), which can be interpreted in the form of orientation distribution functions (ODF), describing the frequency of occurrence of particular grain orientations in a threedimensional Euler space (rotation angles , and 2)4. It is common practice to focus attention on a particular section in the Euler

space (2 = /4), where most of the interesting texture components of cold-rolled and annealed steels can be found5. The main texture components lie along two axes, respectively called fibre (typical of

rolled materials, with all <110> directions parallel to the rolling direction) and fibre (typical of recrystallised materials, with all {111} planes parallel to the sheet surface.

810C - 4.5 C/s 2 = /4 PHI2= 45

810C - 115 C/s 2 = /4 PHI2= 45

890C - 4.5 C/s 2 = /4 PHI2= 45

890C - 115 C/s 2 = /4 PHI2= 45

Figure 10: Effects of annealing peak temperature and cooling rate on texture Figure 10 illustrates part of the evolution of texture with annealing peak temperature and cooling rate. The fibre is strong in all cases, although annealing at 810C leaves enough of rolling-inherited fibre components to question the complete recrystallisation condition that was supposed to prevail on the basis of optical micrographs commented on above (figure 9). An almost perfect fibre texture is achieved by annealing at 840C, followed by slow cooling (not shown in figure 10). Surprisingly enough, a similarly good result cannot be obtained in the case of fast cooling, which results in a strong polarisation. This is reason to believe that the optimum texture went complete in the last time interval spent at high temperature during slow cooling. After annealing at 880C, fibre components come back with some degree of polarisation, which suggests incipient austenitic transformation during soaking, as was predicted theoretically (Ae3 temperature given earlier), against metallographic evidence (figure 9). This situation is clearly improved upon by further raising the annealing temperature (to 890C), which leads to an almost perfect fibre texture through some austenite memory effect, no matter what the cooling rate was. DISCUSSION AND CONCLUSIONS In this study, an experimental high-strength, deep-drawing steel, based on a highmanganese ULC-TiNbP chemistry was subjected to pilot line continuous hot-dip galvanising, to assess how serious surface

reactivity problems could be with this sort of material. Two composite coils were made of three small experimental sections welded to head, middle and tail ends of a commercial quality steel of exactly the same thickness. They were annealed under protective atmospheres characterised by dew points of 22C and +5C, before hot dipping in a Zn-0.17%Al bath maintained at 460C. High dew point annealing led to temperature control problems associated with emissivity variations resulting from either incomplete residual oil burnout in the directfired furnace or reinforced surface oxidation. Coating thickness was nonetheless always under control, and coating adhesion excellent. Prior to skin passing, all corresponding tension curves exhibited some limited yield point elongation, which turned exceptionally high for high dew point-high temperature annealing. The effect could probably be attributed to some loss of carbide forming Ti in the creation of undesired TiFeP phosphides, or to carbide or carbo-nitride dissolution. Yield point elongation can be efficiently removed by adequate skin passing, leading the experimental steel to qualify as a fairly isotropic, high-strength, deep-drawing grade that could be used in the asgalvanised and skin-passed condition for lightweight automotive applications. As a complement to the trials just mentioned, a Rhesca simulation campaign was also carried out, in an attempt to optimise the annealing sequence before hot-dipping. From a purely metallurgical point of view, the austenite memory effect could be taken advantage of, by performing recrystallisation annealing at about 890C, where Lankford coefficient soars and yield strength increases dramatically under the effect of phase transformation. In this framework,

slow cooling is certainly more attractive than fast cooling, because it ensures that ductility features (ElU and Eltot) and strain hardening coefficient (n) be maintained at a sufficiently high level. It must however be mentioned that very high annealing temperatures pose serious problems concerning strip flatness or furnace heating capacity limits. In those cases where they remain out of reach, the treatment should be performed at any temperature over 810C to ensure full recrystallisation, followed by accelerated cooling to take advantage of the otherwise nondamaging extra strengthening suggested by figure 7. ACKNOWLEDGEMENTS The authors express their gratitude to their colleagues from companies having sponsored this ILZRO project, for many stimulating and fruitful discussions. LIST OF REFERENCES
1

M. Lamberigts, F.E. Goodwin, Galvanising High Strength Deep Drawable Steels for Modern Automotive Applications, Modern LC and ULC Sheet Steels for Cold Forming, Aachen, Germany, March 30-April 1, 1998, pp 437-448. 2 L. Landau, E. Lifchitz, Physique Statistique, UDC-530/022=60, Mir, 1967. 3 B. Hutchinson, L. Ryde, D. Artymowicz, Effect of Phase Transformation on Texture during Continuous Annealing, Modern LC and ULC Sheet Steels for Cold Forming, Aachen, 1998, pp 203-210. 4 L.H.J. Bunge, Crystallographic Texture and its Application in the Steel Industry, Cold Rolling: Technology and Products, Jamshedpur, India, February 2000, pp 3947. 5 B. Hutchinson, L. Ryde, Principles and Practice of Texture Control in Cold Rolled and Annealed Sheet Steels, Cold Rolling: Technology and Products, Jamshedpur, India, February 2000, pp 61-73.