Metallurgical Plant and Technology

November 2007 Original verffentlicht in MPT 6/2007

INTERNATIONAL
SPECIAL PRINT

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Quality aspects of hydrogen annealed steel strip

Furnaces and Services for Metals.

Reprint from Metallurgical Plant and Technology 6 (2007), pages 54162 2007, Verlag Stahleisen GmbH, Dsseldorf

Quality aspects of hydrogen annealed steel strip

In the past, the bell-type annealing process has often been seen as the sole cause of stickers although there are a number of different types of stickers caused by many different factors. This article discusses the various types of stickers, the mechanisms that produce them and the precautions which can be taken to prevent their occurrence. Throughout the world, there are companies which suffer losses of up to 10% as a result of stickers. Leading rolling mills which have focussed on the problem of stickers and the processes that produce them have been able to reduce the average share of stickers to less than 1%. Stickers have therefore lost the prominence among surface defects that they had in the 1990s.

Figure 1. Modern batch annealing plant supplied by LOI Thermprocess GmbH

Introduction
Sheet steels annealed in state-of-theart Bell-Type Annealing Furnaces (BAF) fulfil highest quality requirements. The mechanical properties have been optimised in respect of drawability, for low yield strength, high elongation and high Lankford values. With the same importance the BAF has to ensure best surface quality without any defects. Since soft grades tend to be very sticker sensitive the avoidance of sticker marks is a major issue of quality aspects.

anisms. However, a number of different types of stickers have been observed. In some cases, the processes which create these defects have been identified. Ridge stickers are sharply limited defects over the width of the strip. These stickers are mainly caused by strip profile anomalies (such as ridges), which can cause high radial pressures within the windings. Spot stickers are limited to localized spots on the strip. The main cause of these stickers is the local application of high pressures (by coil tongs, for example) and the unintentional winding of foreign objects into the coil, which become apparent when the coil is unwound. Edge stickers, as the name implies, occur at the edge of the strip. They are sharply limited flaws on the strip edge caused by relative movement between the windings of the coil and convector plates or charge carriers as a result of differences between the heating and cooling rates of the coil and these parts. Damage caused by coil handling, such

Classification of stickers
"Sticker" is an overall term for the plastic deformations or flow and kink marks already apparent on steel strip on the temper mill during the uncoiling of the windings of the coil before it reaches the rolling gap. Stickers are produced by the pressure welding of bare metal surfaces. It has not yet been decisively established whether this welding is caused by diffusion welding processes between two surfaces, sintering processes or other adhesion mech-

Dr.-Ing. Peter Wendt, Director of Sales; Dipl.-Ing. Frank Maschler, Senior Process Engineer; Dr.-Ing. Peizhong Wang, Senior Sales Manager, LOI Thermprocess GmbH LOI Italimpianti, Essen, Germany Contact: www.loi-italimpianti.com E-mail: peter.wendt@loi-italimpianti.de

MPT International 6/2007

Heat treatment
as positioning on a surface which is not level, may also cause edge stickers. Edge stickers can be reduced by using convector plates with a higher manganese content, which are harder. The design of the convector plates [1] and charge carriers is also important. The use of intermediate convector plates with a carrying area of 50% or more and machined intermediate convector plates can help to minimize edge stickers on thin strip (thickness less than 0.7 mm). General stickers are irregular kinked lines which take on a sickle-shaped appearance with increasing width (50 to 400 mm wide) and are mainly distributed over a large area in the centre of the strip, with reference to its width. They are also referred to as flowing material shapes or Lders lines (figure 2). Because of the crown of the strip and the resulting higher pressure on the strip centre, the flaw is positioned in a large area at the centre of the strip width in the case of strips with an optimum symmetrical profile. If the crown of the hot strip, which determines the profile of the cold strip, is too high or too sharp, the result may be a narrow but very pronounced track of stickers along the centre of the strip width. Strips with profiles which are too low or too flat may have very wide sticker areas or sticker tracks in the outer thirds of the strip width. In the case of strips which have a slightly wedge-shaped, asymmetrical cross section, the stickers will be located away from the central position at the highest part. The creation of general stickers is affected by a wide variety of process parameters, some of which have contrary effects. The causes of stickers and possible countermeasures are considered below.

Figure 2. Sticker marks

28

Coils with stickers, %

24 20 16 12 8 4 0

Influence of yield stress

Critical Not critical

0 120-149 150-179 180-209 210-239 240-269 >270

Yield stress, N/mm2

400 350

Yield stress, N/mm2

300 250 200 150 100 50 0 Soft quality High-strength quality IF quality Separation force

Figure 3. Effect of the yield strength on the sensitivity to sticker formation

General stickers and their causes

Stickers are created on the temper mill when coils annealed in a bell-type plant are uncoiled and the force required to open or separate the coil windings is in excess of the yield strength of the annealed material. In other words, general stickers depend both on the stress applied to the coil during unwinding and on the yield

strength of the annealed material. As a result, "welds", between the windings of the strip which can be separated by applying force below the material yield strength do not result in stickers. Investigations have shown that the formation of sticker marks is largely determined by the actual value of the yield strength and by the behaviour of the material at stress approaching the yield strength (figure 3). An evaluation of experience obtained with stickers at a German cold rolling mill over a period of several years shows that: - sticker frequencies are higher with soft grades (yield strength < 200 N/mm2),

- no or virtually no stickers occur with higher-strength grades (yield strength > 220 N/mm2), - no or virtually no stickers occur with soft IF steels because of the lack of a precisely defined yield strength. The effective local force acting on the strip during uncoiling in the hatched area of the above diagram must therefore be 120 - 220 N/mm2 (figure 3). This force results from the separation force and the additional effects of uncoiling speed and geometry. Higher separation forces are caused by strong adhesion between the strip windings resulting in the "welding" of tightly packed strip surfaces. These adhesion forces are affected by condiMPT International 6/2007

Heat treatment
tions during the annealing process (temperature, pressure and annealing time). The causes of these welding phenomena were comprehensively investigated for the first time by Pawelski et al. [2]. To date, knowledge of the causes of stickers in Europe is still based on this report, published in 1989. The effects of pressure on maximum separation force are considerably increased at higher temperatures. At temperatures up to about 600 C, practically no welding occurs, irrespective of the tension on the strip. This conclusion is confirmed by practical experience, although temperatures up to a maximum of 620C are generally regarded as uncritical with regard to stickers. In general, the higher the annealing temperature, the less time is required for welding the samples. strength and micro-alloyed steels are considered to be less susceptible to stickers. Strip profile. The profile of the coldrolled strip reflects that of the hotrolled strip. A steel strip with a profile optimized to avoid stickers has a crown of 40-60 m. Significantly lower crowns (flatter profiles) lead to increased sticker rates in the edge or central sections as a result of higher pressures. Asymmetric (for example, wedge-shaped) cross sections and cross section anomalies such as ridges also result in higher pressures and produce more intensive welding between the windings of a coil during the batch annealing process. Coiling tension. Coiling tension is a key factor in determining the stress in the coil and therefore also the sticker rate. Minimal coiling tension (near to the collapsing limit) helps to reduce overall compressive stress during the annealing process. Lower limits to the coiling force are set by the need to ensure safe handling during removal from the coiler and transfer to the belltype annealing furnace, the need for a stable coil and the avoidance of scratches caused by slippage during annealing and dressing. Leading cold rolling mills are in a position to reduce the coiling tension applied to a minimum (~ 22 N/mm2). The coiling tension must be optimized for the individual coil dimensions, widths and thicknesses. Strip roughness and topography. The roughness of the strip surface has considerable impact in minimizing welding and reducing the separation force required. Pawelski et al. [2] have already investigated these effects. The results of their experiments are shown in figure 3. The separation forces determined for roughened strip samples in the temperature range from 670 to 700C were only about half the corresponding figure for smooth sheet which had not been roughened prior to annealing. Apart from the roughness value, the texture of the surface roughness is also important. Surface irregularities which are more pointed and have a finer structure are more effective in reducing welding than coarser structures with a plateau configuration. For O5 surface qualities, leading cold rolling mills in Germany aim for a preroughened structure with a roughness of Ra > 1.2 m and a minimum number of peaks of Pc > 50 /cm (> 127 ppi). In order to avoid stickers, the values should not fall below Ra >1.0 m and Pc > 40 /cm (> 100 ppi). Strip cleanliness. As a general principle, the cleaner the strip, the greater is the risk of welding. The strip cleanliness of a rolled strip is normally defined in terms of oil residues and iron fines in mg/m2. The introduction of HPH (High Performance Hydrogen) annealing technology significantly improved strip cleanliness and therefore led to an increased tendency towards sticker formation with otherwise unchanged conditions. High strip cleanliness, which is desirable for downstream process stages, is therefore counterproductive in terms of sticker formation. If electrolytic strip cleaning systems (ECL) are used upstream from the annealing furnace, oil deposits can be reduced to 5 mg/m2 at the same time as forming a silicate layer of the order of 4 - 8 mg/m2 SiO2, which forms a barrier and prevents welding between the windings. An Asian cold rolling mill has reported that it was able to halve the sticker rate (from > 6% to < 2.9%) simply by optimizing the thickness of the silicate layer. A number of attempts have been made and are still being made to apply separating layers to the strip surface to prevent pressure welding without any detrimental impact on the production process. Tests with the addition of a silicate to the rolling emulsion for the last stand of a five-stand tandem line were at least partially successful. If this approach is adopted, it is necessary to ensure that the pH and stability of the emulsion are not impaired. There must be no adverse effect on corrosion

Factors affecting sticker formation

Although the pressure welds which lead to stickers are always produced in the batch annealing process, the degree of welding and the resulting severity of the stickers are determined to a very large extent by upstream and downstream production stages. The factors concerned can be divided into those related to - upstream process stages, - the annealing process itself, and - downstream process stages. As shown in table 1, the main factors can be summarised in three categories: before, during and after annealing. Steel grade. Soft, unalloyed steels of grades DC 04 (DDQ) and DC 05 (EDDQ) are sensitive to sticker formation [3]. IF steels without a clearly defined yield strength after annealing, higher-strength structural steels, high-

Factors affecting sticker formation Before annealing Steel grade Hot strip profile Coiling tension Strip roughness Strip cleanliness Strip dimensions Coil dimensions During annealing Cooling rate Heating-up gradient Coil position After annealing Uncoiling speed Uncoiling tension Uncoiling geometry

Table 1. Important factors affecting sensitivity to sticker formation

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and welding behaviour or on downstream production stages such as phosphating, painting, hot-dip galvanizing or electrolytic galvanizing. A German customer has reported that the sticker rate could be reduced from about 2% to about 0.2% by applying a silicon layer of 2 - 3 mg/m2 SiO2 in the last rolling stand [4]. The DEFOX process in which an oxide layer only effective in the critical first few hours of cooling is applied during the annealing process, did not prove to be effective in practice and has now been discontinued by many process, temperature differences are therefore higher, resulting in more severe thermal stress. Experience indicates that coils with strip thicknesses below 0.7 mm are especially sensitive to stickers. The negative impact of strip width is slightly less severe than that of thickness. Current statistics show that the risk of stickers already increases at strip widths above > 1,100 mm. As the outer diameter of the coil increases, temperature differences during the heating and cooling process also rise, leading to higher stress on the coil and welding is influenced directly by the annealing and cooling process or the time-temperature plot and indirectly by the thermal stress in the coil resulting from the temperature gradient. The risk of sticker formation can be reduced by the following measures taken during the annealing process. The heating rate shall be reduced when a control temperature of 600 C has been reached. This approach reduces stress caused by heating-up and also has a positive impact on strip cleanliness. However, it should be noted that stickers caused purely by heating-up are rare. The time-temperature regime has a greater effect. Very long soaking times shall be avoided. As there is a considerable tendency towards welding at high temperatures, even relatively low stress within the coil can result in sticker formation. The soaking time must be set so that the critical coil in the stack reaches the core temperature required. Cooling under the heating hood shall occur for a maximum of 6-8 hours. When the heating hood is removed, the charge is naturally cooled very rapidly. By allowing the charge to cool under the heating hood, the cooling shock is reduced and shifted to a lower temperature range, where the risk of welding and sticker formation is reduced. The same also applies to the starting temperature for rapid cooling. At any rate, the bypass or spray cooling system should not be started up until the coil core temperature is lower than 600C.

Figure 4. Concept of StickerMod

rolling mills. The main reasons were adhesion problems caused by incomplete reduction of trivalent iron oxide components in the layer applied, in addition, this process had less effect in reducing stickers than the furnace cooling stage which it replaced. Other possibilities which have been considered or tested include the use of QUERL separating layers containing nitrates, iron or iron oxide fines to provide spacers with a thickness in the m range between the windings. To date, none of these approaches has been widely adopted in practice. Strip dimensions, coil dimensions. As a general principle, thinner, wider strips and larger coil diameters tend to be more critical with regard to stickers. Strip thickness is the key parameter in this connection. The main reason is that coils of thinner strip have a larger number of windings, with an adverse effect on radial heat transmission through the coil. During the cooling

a greater risk of welding between the windings. Sticker rates are already significantly higher for coils with diameters above 1,600 mm. After annealing. Stickers are detected after first uncoiling after annealing. Therefore the uncoiling conditions are evident, mainly the uncoiling geometry and the uncoiling speed. A proper uncoiling geometry ensures a well defined, constant separation point. One measure of implementation is an anti-sticker roller [3]. Because the yield strength increases with the speed of force increase, high uncoiling speed above 500 m/min, better 800 m/min, helps to reduce stickers.

StickerMod - a model for avoiding stickers

Until recently it has not been possible to predict the occurrence of stickers in advance. As a result, the efficiency of the production process may be impaired, for example if the charge is cooled with the heating hood longer than is necessary for sticker prevention. StickerMod was developed by LOI Thermprocess [5, 6] as a tool for predicting stickers in individual stacks and for the analysis of individual annealing cycles. It is based on the investigations of Pawelski et al. [2], who considered the theoretical background (i.e. calculation of thermal stresses) and performed a number of
MPT International 6/2007

Measures during annealing to prevent stickers

Strip welding is caused during the annealing of thin sheet coils in belltype annealing furnaces. Pressure

Heat treatment
experiments on the influence of pressure, temperature and annealing time. Thermal stresses result from temperature differences in the coil. To calculate thermal stresses, information on local temperature distribution during the whole annealing cycle is necessary. LOI's thermodynamic mathematical model HeatMod calculates temperature distribution during the annealing cycle with high precision and was therefore used as the basis for the StickerMod model (figure 4). However, sticker calculations cannot be made solely on the basis of stress values. The effects of temperature and duration are represented by the equivalent separation force (ESF), which is an indicator of the uncoiling forces required and therefore also of sticker creation. The ESF is calculated on the basis of the coil width: 1,250 mm outer diameter: 1,855 mm inner diameter: 610 mm strip thickness: 1 mm stack weight: 94.6 t heating-up gradient from 350C to 710C in 17 h soaking temperature: 710C end of heating: 10 h equivalent time cooling with heating hood: 3 h start of rapid cooling: 450C Outer diameter and width of coils. The higher width results in higher separation forces increasing with increasing diameter. The reasons for this behaviour are the temperature differences, which increase with increasing width and outer diameter. The base stack is marked by circles. Cooling with the heating hood. A heating hood is often used to prevent stickers. Increasing the duration of cooling with the heating hood reduces the ESF by up to 18%. An increase in the duration of cooling with the heating hood beyond six hours has no further effect on the separation force, but only increases the cycle time. As a second result, the separation force increases if the charge is only cooled under the heating hood for one hour. The reason for this effect is the rising core temperature at the start of cooling with the heating hood. If the heating hood is removed at maximum core temperature, temperature differences are maximized, resulting in maximum pressure at a high temperature level. Rapid cooling start temperature. The control temperature at the start of rapid cooling has only a slight influence on the separation force. A reduction in the start temperature below 450C has no effect on the base stack. Above 450C, the separation force increases by about 4%. This can be explained by the geometry of the furnace. Due to the arrangement of the burners the second coil is heated up fastest. When rapid cooling is started, cooled purge gas is heated up by the first coil before reaching the second one. Core temperature. It was expected that separation force would increase with core temperature. However, cooling with the heating hood becomes more effective with increasing core temperatures. This can be explained by the increase in the ESF not only with the pressure level but also with the temperature level. Soaking temperature. The separation force decreases very strongly with a decreasing soaking temperature (up to 37%, compared to the base stack), while the total cycle time increases only by 7%. To make results comparable, all calculations were performed with an equivalent time of 10 h.

Evaluation of process parameters

The results of the base geometry calculation are shown in figure 5. As a result of the geometry of the furnace, which will not be discussed here, the highest gradients and therefore also

Temperature, C- Stress, N/mm2

800

4 coil stack 94.6 t 1,250 mm Outer diam. 1,855 mm Thickness 1.0 mm 600

8,000 7,000 6,000 5,000 4,000 3,000 2,000 1,000 0 -1,000 60

700 Width 500 400 300 200 100 0 -100 0

Control temperature Core coil 2 Edge coil 2 Temp. difference Total stress coil 2 2/3 pos. Sep. force coil 2 2/3 pos.

ESF, N

10

20

30

40

50

Figure 5. Annealing cycle for base stack by StickerMod

Time, h

investigations by Pawelski et al. [2], who measured the separation forces as a function of stress, temperature and annealing duration. Stickers occur if the ESF reaches a critical value. Parameters influencing stickers. As mentioned above, stickers are influenced by a number of parameters. StickerMod can take some of these into account: - coiling tension, - outer diameter, width of strip, - heating-up gradient, - cold spot temperature, - soaking temperature, - cooling with heating hood, - start temperature for rapid cooling, - material properties (yield strength). The influence of some of these parameters is indicated below taking the example of a 4-coil stack with the geometry and annealing cycle data as follows: 6
MPT International 6/2007

the highest equivalent separation forces (ESF) under these specific conditions can be seen on the second coil. For this reason, only curves for the second coil are shown in the diagrams. The bold blue line represents the local ESF for coil 2 two-thirds of the way from the inner diameter to the outer diameter at the centreline (2/3 position). During heating and soaking tensile stress (total stress > 0) at 2/3 position is in evidence. Therefore there is no increase in the ESF. Approximately one hour after the start of cooling with the heating hood, the core temperature becomes higher than the edge temperature. The layers are pressed together (total stress < 0) and pressure welding starts. Five hours after the end of soaking the ESF reaches its maximum. After this time less pressure will be expected.

Heat treatment
StickerMod validation. To verify the StickerMod programme, calculations were performed for 59 stacks which had already been annealed at a German plant. In 30 stacks one coil of each stack showed sticker marks, while 29 stacks were annealed without any marks. The maximum equivalent separation force occurring during the annealing cycle was calculated for each coil of all the stacks. Assuming a critical separation force of 6,000 N, 80% of the coils with sticker marks were detected correctly. The calculation of stacks without any sticker marks resulted in correct results for 86%. For 14% of stacks without sticker marks the model calculated a sticker warning. In view of the fact that the calculations are based on experimental data with deviations of up to 1,700 N and that these curves were approximated by mathematical functions, 80% represents good agreement. Furthermore it must be considered that the input variables of StickerMod are only a part of the influence factors listed in table 1. throughput by keeping the limits given by the upstream process steps.

Conclusion
Although sticker occurrence is always related to bell-type annealing, the main influences come from the upstream and downstream process steps as well as from the annealing process itself. Many of these factors are subjects of improvements, but some of them remain as input parameters to be considered in the design of the belltype annealing process. High heating and cooling speed is favourable for the throughput, but they could be detrimental in respect of stickers. Productivity as a combination of quality and throughput depends on how close and how safe certain limits can be used out. StickerMod is a kind of process intelligence which supports the design of annealing cycles. The resulting furnace cycles enable to achieve high

References
[1] Dr. Scheuermann, W.; Maschler, F.; Dr. Wendt, P.: Aspects of HPH-Hydrogen Batch Annealing, Paper published on LOI International Customer Convention on Heat Treatment of Steel Strip and Wire, 2004 [2] Pawelski, O.; Rasp, W., Martin, G.: Entstehung von Bandklebern bei haubengeglhtem Kaltband (Origins of sticker marks on batch annealed cold rolled sheet), Stahl u. Eisen 109 (1989), No. 4, p. 178-184 [3] Emde, E.; Dzafic, A.; Frech, W.: Sticker-prevention measures in HPH BAF and in upstream and downstream process steps, Paper published on LOI International Customer Convention on Heat Treatment of Steel Strip and Wire, 2004 [4] Henkel, Product Information, P3-percy [5] Dr. Leifgen, U.; Sinter, A.: Sticker Prevention in Batch Annealing - StickerMod: Basics and Results, Paper published on LOI International Customer Convention on Heat Treatment of Steel Strip and Wire, 2004 [6] Dr. Wendt, P.; Frech, W.; Dr. Leifgen, U.: Cold rolling defect "Stickers" and countermeasures, Heat Processing (5), Issue 2, 2007, p. 127-135

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