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Applied Surface Science 253 (2007) 6769–6777

www.elsevier.com/locate/apsusc

On texture, corrosion resistance and morphology of hot-dip


galvanized zinc coatings
H. Asgari *, M.R. Toroghinejad, M.A. Golozar
Department of Materials Engineering, Isfahan University of Technology, Isfahan 8415683111, Iran
Received 19 November 2006; received in revised form 10 January 2007; accepted 23 January 2007
Available online 31 January 2007

Abstract
Texture is an important factor which affects the coating properties. Chemical composition of the zinc bath can strongly influence the texture of
hot-dip galvanized coatings. In this study, lead content of the zinc bath was changed from 0.01 wt.% to 0.11 wt.%. Specimens were prepared from
zinc baths of different lead content and its texture was evaluated using X-ray diffraction. Corrosion behaviour was analyzed by Tafel extrapolation
and linear polarization tests. To study the corrosion products of the specimens, salt spray test was employed. Also, the spangle size of the specimens
was determined using line intercept method. From the experimental results it was found that (00.2) basal plane texture component would be
weakened by increasing the lead content of the zinc and conversely, (20.1) high angle pyramidal texture components strengthened. Besides,
coatings with strong (00.2) texture component and weaker (20.1) component have better corrosion resistance than the coatings with weak (00.2)
and strong (20.1) texture components. In addition, surface morphology would be changed and presence of basal planes decreases at the coating
surface due to the increase of lead in the zinc bath. Furthermore, spangle size would be increased by increasing the lead content of the zinc bath.
Investigation on the effects of skin pass rolling showed that in this case, (00.2) basal texture component and corrosion resistance of the skin passed
specimens, in comparison with non-skin passed specimens, have been decreased.
# 2007 Elsevier B.V. All rights reserved.

Keywords: Texture; Corrosion resistance; Skin pass rolling; Tafel/linear polarization test; Morphology; Hot-dip galvanizing

1. Introduction more advantageous for coiled products such as sheet, wire and
tube [1].
Zinc coatings are predominantly used to improve the In a large number of continuous hot-dip galvanizing lines,
aqueous corrosion resistance of steel by two methods, barrier lead is usually incorporated into the zinc bath. This addition not
protection and galvanic protection. In barrier protection, the only causes an increase in the bath fluidity and a decrease in its
zinc coating, which separates the steel from the corrosion surface tension but also, in small concentrations (0.04–
environment, will first corrode before the corrosive environ- 0.2 wt.%) improves the zinc coating uniformity and its
ment reaches the steel. In galvanic protection, zinc is less adhesion to steel sheet [2]. However, this also induces the
noble to iron at ambient conditions, and will sacrificially excessive growth of the zinc crystals and dendritic type
corrode to protect the substrate steel, even if some of the steel solidification in the form of spangles [3]. These spangles seem
is exposed as cut edges or scratches in the coating. Typical to grow from a nucleus and with an important solute
processing methods used in producing zinc coatings include segregation, with one of the most common structures being
hot-dip galvanizing, thermal spraying and electrodeposition. the six-pointed star or snowflake [4–6]. The spangles are the
This study will be concentrated on hot-dip galvanizing, i.e. the result of dendritic solidification of zinc [7]. Spangle size is
immersion of a steel article in a liquid bath of zinc or zinc influenced by cooling conditions during solidification. The
alloy, by continuous processing. The continuous process is three surface finishes commonly produced are regular spangle,
minimum spangle and extra-smooth spangle [1]. With preferred
nucleation sites at the liquid Zn/substrate interface, growth of
* Corresponding author. Tel.: +98 861 2776316; fax: +98 311 3912752. Zn spangles occurs in three stages including: (1) The initial
E-mail address: asgari.ha@gmail.com (H. Asgari). growth stage (0.1 s) involves sideways growth of Zn basal plane
0169-4332/$ – see front matter # 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.apsusc.2007.01.093
6770 H. Asgari et al. / Applied Surface Science 253 (2007) 6769–6777

Table 1
Production parameters of specimens
Specimen Chemical composition of the zinc bath Jet wiper distance Sheet Zinc bath Strip-entry Galvanizing
from sheet thickness temperature temperature line speed
(%)Pb (%)Fe (%)Al surface (mm) (mm) (8C) (8C) (m/min)
A 0.010 0.023 0.195 100 0.5 461  1 466  1 100
B, Bs 0.045 0.027 0.191 100 0.5 461  1 461  1 100
C, Cs 0.065 0.021 0.188 100 0.5 461  1 461  1 100
D 0.110 0.023 0.190 100 0.5 461  1 461  1 100

parallel to the interface in ½1 1̄ 0 0 growth direction. The entire composition of the steel substrate are shown in Tables 1 and 2.
steel surface is covered by a solid layer of zinc dendrites, As it can be seen in Table 1, the variations of Al and Fe wt.% are
whereas the surface remains liquid. (2) The second stage very small and negligible and thus, they are considered to have
involves slow thickening of the solid zinc grain which is no effect on texture and corrosion resistance. Specimens Bs and
dependent on grain orientation. (3) The third stage, or Cs are two specimens which were skin passed and have the
continuous thickening of the zinc grain, causes solute same chemical composition of the zinc bath as specimens B and
enrichment of the remaining liquid and finally Pb precipitation C, respectively (Table 1).
between Zn dendrite arms [8]. Large spangles are generally The crystallographic orientation of the coatings was
associated with solute additions to the galvanizing bath and Pb, determined using X-ray diffraction (Philips XL Model 30,
at concentrations greater than 0.04 wt.%, is the solute generally Cu Ka radiation, step size of 0.038 and counting time of 1 s). A
added to molten Zn to produce spangles [9]. 2-theta scan was performed between 208 and 1408 and the
The preferred crystallographic orientation (texture) depends integrated intensities of several reflections were determined,
strongly on external factors such as cooling rate gradient, these are termed Ihkil. It should be noted that integrated
surface condition of steel substrate during the coating intensities require background subtraction. Each Ihkil is
solidification process and bath chemical composition [10]. normalized by dividing it by its structure factor or random
0 n 0
Concerning the coating corrosion resistance, this depends in intensity, Ihkil , giving Ihkil . The values of Ihkil were obtained
n n
particular on the zinc layer chemical composition and also is from powder zinc pattern. In this study, only Ið00:2Þ and Ið20:1Þ
affected by the crystallographic orientation. were considered.
When a metal is exposed to a corrosive environment, the Tafel/linear polarization tests were conducted in a 5% NaCl
corrosion resistance of each grain varies because of the solution at room temperature using an EG&G Princton Applied
difference in the binding energy of atoms between the Research Model 263A potentiostat. A standard corrosion cell
crystallographic planes. According to Scully, the total energy kit with the working electrode, two graphite counter electrodes
involved in the breaking of the bonds and the subsequent and a saturated calomel reference electrode (SCE) was used.
dissolution of atoms is higher for the crystallographic planes The volume of the electrolyte for each test was 500 ml.
which have a higher number of nearest neighbor atoms. Thus, Potentiodynamic scanning was performed by stepping the
the close packed planes, or low-index planes, are known to be potential at a scan rate of 1 mV/s from 250 mV (SCE) to
more resistant to dissolution because of the higher binding 500 mV (SCE). The edges of specimens were covered by a
energy of the surface atoms [11]. plastic lacquer to prevent the corrosion of steel. Salt spray test
Skin pass rolling is used after galvanizing process to roughen were performed using a salt spray cabinet according to ASTM
the surface of hot-dip galvanized sheet to be prepared for standard B117. The salt spray test was done in 5% NaCl
subsequent chromating and painting process. Skin pass rolling solution at 35 8C.
has some influences on texture and corrosion behaviour of hot- The morphology of corrosion products (obtained from salt
dip galvanized coatings. spray cabinet after 72 h exposure) was studied using scanning
The aim of this study is to assess the effects of skin pass electron microscopy (SEM) and X-ray diffraction (XRD). SEM
rolling and different concentrations of lead in the zinc bath on studies were carried out using a Philips XL Model 30 and XRD
(00.2) and (20.1) texture components, corrosion resistance,
spangle size and morphology of hot-dip galvanized zinc
coatings. Table 2
Chemical composition of steel substrate

2. Experimental procedure Grade JIS G3302


%C 0.038
%Ti 0.001
All the tests were carried out three times with commercially %S 0.005
available JIS G3302 hot-dip galvanized steel sheets and the %Mo 0.002
average of results considered as the final report. In this research, %P 0.007
lead content of the zinc bath was changed from 0.01 wt.% to %V 0.001
%Si 0.009
0.11 wt.%. The coating thickness for all specimens was the
%Al 0.048
same and about 44 mm. Production parameters and chemical
H. Asgari et al. / Applied Surface Science 253 (2007) 6769–6777 6771

n
Fig. 1. Effects of lead content of zinc bath on Ið00:2Þ n
and Ið20:1Þ of non-skin Fig. 2. Effect of lead content of zinc bath on corrosion current density of non-
passed specimens. skin passed specimens.

n
studies were done employing a Philips Xpert-MPD Model is recognized that Ið00:2Þ of specimen A is 12 times higher than
3040. The surface morphology was studied using Nomalski that of specimen D.
differential interference method and employing an optical Fig. 2 shows that increasing the lead content of zinc bath
microscopy equipped with polarized light. would result in the increase of corrosion current density.
The size of spangles was determined using line intercept Therefore, the best corrosion resistance was experienced for
method. In this method, several lines (10 cm in length) are specimen A and the worst one was that of specimen D.
drawn on different regions of the specimen surface and the After 72 h of exposing two specimens (B and D) to salt spray
intersected spangles are counted. Then the length of every cabinet, XRD analysis of corroded specimens shows that the
line is divided by the number of intersected spangles (by the main corrosion products were Simonkolleite, Zincite, Hydro-
line) and the average of results considered as the spangle zincite and aluminum oxide. It shows that increasing the lead
size. content of zinc bath (from 0.045 wt.% to 0.11 wt.%) has no
Cross sections of the coatings were studied using scanning effect on the present phases in corrosion products. Also, SEM
electron microscopy. The composition of the coating layers was micrographs obtained from these specimens showed that a
determined using EDS analysis. relatively thick and continuous layer of corrosion products
covered the whole surface of the specimen D whereas the
3. Results surface of specimen B presented not only less voluminous
corrosion products but also a partially attacked area. In the
3.1. Non-skin passed specimens latter case (specimen B), noncorroded zinc crystals (basal
plane) were present in different zones of the surface (Fig. 3) and
As it was noted above, the texture of the coating depends it was not seen for the former case (specimen D).
strongly on the chemical composition of the zinc bath. It can be Fig. 4 shows the relationship between the lead content of
seen from Fig. 1 that by increasing the lead content of zinc bath, zinc bath and polarization resistance (Rp) of specimens. As it
relative intensity of (00.2) basal plane texture component is can be seen, increasing the lead content would decrease the
decreased. This means that basal plane texture component is polarization resistance of specimens and consequently,
weakened. Conversely, in Fig. 1, it is clear that increasing the decreases the corrosion resistance of galvanized zinc coatings.
lead content of zinc bath results in increasing the relative The results were in good agreement with that of Tafel
intensity of (20.1) pyramidal plane texture component. Thus, it polarization tests.

Fig. 3. (a) and (b) Noncorroded zinc crystals (basal planes) remained on the surface of specimen B after 72 h exposure in salt spray.
6772 H. Asgari et al. / Applied Surface Science 253 (2007) 6769–6777

Fig. 4. Effects of lead content of zinc bath on linear polarization (Rp) of non- Fig. 5. Effects of lead content of zinc bath on spangle size of non-skin passed
skin passed specimens. specimens.

In Fig. 5, increasing in the spangle size due to increasing Figs. 6–8 show the optical morphology of Zn crystals
the lead content of the zinc bath can be observed. It is evident deposited on the steel substrate in the specimens B, C and D,
that specimen A has a very small spangle size and the spangle using Nomalski differential interference method. Zn crystals
size difference between specimens A and D is about 9 mm. In are thin plates and their edges lie in one direction on each grain
addition, it was seen that by increasing the lead content of and there is a clear change in morphology from one grain to
zinc bath, number of dull spangles was increased and another grain (Fig. 6(a)). Other figures such as Figs. 6(c) and
conversely, number of bright spangles decreased and the 7(b) show the rows of the thin zinc crystals which were aligned
surface of the specimens became more opaque; that is, a large in two directions as if they fell down like dominoes. In Figs.
number of the spangles were smooth and very reflective with 6(b) and 7(a), layered thin hexagonal platelets of zinc crystals
a higher bright coating in specimens A and B but, specimens can be observed. It should be noted that these morphologies are
C and specially D had a dull appearance because most of the the general morphology of the surfaces of specimens B, C and
spangles were opaque and poorly reflective. Specimens A and D and as can be seen, by increasing the lead content of the zinc
B contained a higher percentage of smooth spangles than bath the presence of basal planes parallel to the surface
specimens C and D. decreases and these planes are substituted with other planes

Fig. 6. (a), (b), (c) and (d) Surface morphology of specimen B.


H. Asgari et al. / Applied Surface Science 253 (2007) 6769–6777 6773

Fig. 7. (a) and (b) Surface morphology of specimen C.

Fig. 8. (a) and (b) Surface morphology of specimen D.

which are thought to be prism or high angle planes (Figs. 6(b),


7(a) and 8(b)). These morphologies confirm the results of X-ray
diffraction that showed the decreasing of basal planes by
increasing the lead content of the zinc bath.
Fig. 9 illustrates the XRD diagrams of specimens A and D
with different spangle sizes and texture components. It is
obvious that increasing the lead content of the zinc bath,
accompanied by the increase of spangle size, has leaded to
decrease of basal plane intensity of specimen D and increasing
of other components (note to the units of the diagrams).

n n
Fig. 9. XRD diagrams of specimens (a) A and (b) D with different spangle size Fig. 10. Effects of lead content of zinc bath on Ið00:2Þ and Ið20:1Þ of skin passed
and texture intensities. specimens.
6774 H. Asgari et al. / Applied Surface Science 253 (2007) 6769–6777

3.2. Skin passed specimens

Fig. 10 shows the decrease in relative intensity of (00.2)


basal texture component with addition of lead to the zinc bath.
Also, in figure, it can be distinguished that relative intensity of
(20.1) pyramidal plane texture component increases as the lead
content of zinc bath increases.
Fig. 11 indicates the corrosion current densities of skin
passed specimens and it is seen that by addition of lead to zinc
bath, corrosion current density has been increased. In Fig. 12,
n n
polarization resistance (Rp) of skin passed specimens are Fig. 13. Comparison of Ið00:2Þ and Ið20:1Þ between skin passed and non-skin
depicted and it can be observed that increasing the lead content passed specimens.
of zinc bath results in the decrease of polarization resistance.
In Fig. 13, relative intensities of (00.2) and (20.1) texture (Fig. 16). Spangle size determination of skin passed specimens
components of skin passed and non-skin passed specimens are showed that spangle size has been decreased in comparison
compared. It can be concluded that skin passed specimens have with non-skin passed specimens (Fig. 17). This could be due to
lower relative intensity of (00.2) basal texture component but the breaking of the spangles via skin pass rolling.
higher relative intensity of (20.1) pyramidal plane texture
component with respect to non-skin passed specimens. 4. Discussion
Figs. 14 and 15 compare the corrosion current density and
polarization resistance between skin passed and non-skin Although hot-dip galvanized zinc coatings often show a
passed specimens. As it is evident, skin passed specimens have strong (00.2) basal plane texturing [1], in the case of lead
higher corrosion current density but lower polarization additions, the (00.2) texturing disappears [12]. It is evident in
resistance in comparison with non-skin passed specimens. n
Fig. 1 that by increasing the lead content of zinc bath, Ið00:2Þ was
Comparison between SEM micrographs of skin passed and n
decreased and conversely, Ið20:1Þ was increased. This is due to
non-skin passed specimens shows that in the case of skin pass the fact that lead decreases the nucleation sites of basal planes
rolling, some microcracks have been established in the coating and conversely, increases the nucleation sites of other planes
and therefore, the continuity of the coating is deteriorated such as (20.1) pyramidal planes [13]. Thus, when the lead
content of zinc bath is increased, less nuclei of basal planes
form and consequently, less basal planes will be formed and

Fig. 11. Effects of lead content of zinc bath on corrosion current density of skin
passed specimens. Fig. 14. Comparison of corrosion current density between skin passed and non-
skin passed specimens.

Fig. 12. Effects of lead content of zinc bath on polarization resistance of skin Fig. 15. Comparison of polarization resistance between skin passed and non-
passed specimens. skin passed specimens.
H. Asgari et al. / Applied Surface Science 253 (2007) 6769–6777 6775

Fig. 16. Comparison of SEM micrographs of (a) skin passed and (b) non-skin passed specimens.

words, surface becomes electrochemically less active because


surface energy, that its value is inversely proportional to the
atomic spacing (d), is lowest for basal plane with respect to
other planes in hcp structure (for example: 1/d = 0.41; 0.89 and
0.85 for (00.2), (20.1) and (11.2) planes, respectively) [3].
Because of this excellent dissolution resistance, coating with
higher relative intensity of (00.2) basal plane texture
component will be corroded much slower than those of lower
relative intensity of (00.2) basal texture component [11].
However, when the relative intensity of (00.2) basal plane
Fig. 17. Comparison of spangle size between skin passed and non-skin passed texture component decreases, it is concluded that the basal
specimens. planes at the surface are substituted with other planes such as
high angle pyramids (e.g. (20.1)) or prism planes. The corrosion
lower area of the surface would be covered by these planes resistance of these planes, because of their higher surface
parallel with the surface. energy and lower interatomic binding energy, is low and
From Figs. 18 and 19 it can be inferred that in both skin therefore, the coating becomes weaker against corrosion
passed and non-skin passed cases, the coatings with a higher attacks [11]. It was mentioned above, the surface of specimen
relative intensity of (00.2) basal plane texture component and D was completely covered by corrosion products after 72 h
lower relative intensity of (20.1) high angle pyramidal plane exposure in salt spray because of very low corrosion resistance
texture component have better corrosion resistance. When the of the coating. It means that approximately all of the zinc
relative intensity of (00.2) basal plane texture is high, it can be coating on the steel sheet is corroded by corrosive environment,
concluded that the surface is mainly covered by basal planes but the partially corroded surface of specimen B revealed that
parallel with the sheet surface. The basal planes have the there are some noncorroded zones (planes) yet. These
highest binding energy of the surface atoms and the total energy noncorroded zinc crystals, in fact, are basal planes remained
involved in the breaking of the bonds and the subsequent on the surface (Fig. 3) and showed the better corrosion
dissolution of atoms is highest for these planes [11]. In the other resistance of the coatings obtained from zinc baths with lower

n n n n
Fig. 18. Relationship between lead content of zinc bath, icorr, Ið00:2Þ and Ið20:1Þ in Fig. 19. Relationship between lead content of zinc bath, icorr, Ið00:2Þ and Ið20:1Þ in
non-skin passed specimens. skin passed specimens.
6776 H. Asgari et al. / Applied Surface Science 253 (2007) 6769–6777

lead content. Also, results of Tafel polarization test confirmed the zinc dendrite to increase, resulting in larger spangles [8].
that the corrosion resistance is decreased by increasing the lead Skin passed specimens, due to the breaking of their spangles,
content of zinc bath (Fig. 2). have lower spangle size than non-skin passed specimens. Also,
n n
Decrease in Ið00:2Þ and increase in Ið20:1Þ of skin passed it was noted that by increasing the lead content of the zinc bath,
specimens in comparison with non-skin passed specimens is the surface became more opaque and dull spangles increased.
associated with the cold work done on the specimen and This happens because lead segregates towards the coating
changing in crystallographic orientations due to skin pass surface and precipitates as some globules in dull spangles and
rolling (Fig. 13). Therefore, as it was explained before, darken their color [18]. Thus, by increasing the lead content of
because of decreasing the (00.2) basal plane texture zinc bath, number of dull spangles increases. However, lead
component, corrosion resistance of skin passed specimens also precipitates in bright spangles but in this case, the diameter
has been decreased [11]. Thus, one of the reasons for higher of the lead globules is smaller and the amount of precipitated
corrosion current density and lower polarization resistance of lead is lower in comparison with dull spangles [16–18]. More
skin passed specimens with respect to non-skin passed opaque surface of dull spangles and coatings that obtained from
specimens (Figs. 14 and 15) would be more decrease in high zinc baths with higher lead content can also be ascribed to their
corrosion resistant (00.2) basal plane texture component textures. It has been discerned that in dull spangles, the
(Fig. 13). predominant texture component is (20.1) and texture coefficient
Another reason for less corrosion resistance of skin passed of (00.2) basal plane texture component is very low in these
specimen in comparison with non-skin passed specimens is the spangles [3]. On the contrary to dull spangles, bright spangles
presence of microcracks in the coating (Fig. 16). These have highest texture coefficient of (00.2) basal planes and
microcracks destroy the continuity of the coating, cause its (20.1) high angle pyramid texture coefficient is very low in
simpler spalling and faster achievement of corrosive environ- these spangles [3]. Therefore, in dull spangles, planes with
ment to the steel substrate. In fact, in the presence of these lower number of atoms (packing factor) are parallel to the
microcracks, accelerated corrosion occurs [13]. surface and during the radiation of light to their surfaces, they
As it was seen in Figs. 6–8, basal planes decreased in the have not enough ability for ordered and completed reflection of
surface of the specimens as the lead content of the zinc bath the light and then seems to be opaque. It should be noticed that
increases. The morphologies confirm the results obtained for this inhomogeneous distribution of lead promotes the localized
(00.2) basal texture component. Every spangle on galvanized corrosion of the material [14], affects the topography of the
coating consists of many grains growing from several nuclei coating surface [15] and changes the surface reactivity of the
which are related to each other in orientation, thus as it is coating [3].
obvious in these figures (such as Figs. 6(b), 7(a) and 8(b)),
decreasing the nucleation sites of the basal planes due to the 5. Conclusions
increase of lead content of the zinc bath has resulted in the
decreasing of basal planes at the surface [13]. In Figs. 6(c) From the results presented in this paper, the following
and 7(b) the rows consisting of the layered zinc crystals have conclusions can be drawn:
grown until the impingements with other rows because of the
lack of nucleation sites in some parts of all the specimens 1. Increasing the lead content of zinc bath results in the
n n
and have taken the shape that is called ‘dominoes’ by some decrease of Ið00:2Þ and the increase of Ið20:1Þ in both skin
authors [19]. It should be mentioned that these types of passed and non-skin passed specimens.
n n
morphologies have been observed also in the electrodepos- 2. Skin passed specimens have higher Ið20:1Þ and lower Ið00:2Þ in
ited zinc coatings and in the case of electrodeposited zinc comparison with non-skin passed specimens.
n n
coatings, presence of grain boundaries is ascribed to the 3. As Ið00:2Þ increases and Ið20:1Þ decreases, corrosion resistance
epitaxial growth of Zn crystals on the steel substrate and of both skin passed and non-skin passed specimen increases.
certain relationship between zinc crystals and ferrite grains 4. Non-skin passed specimens have better corrosion/polariza-
[19], but in the case of hot-dip galvanizing, because of tion resistance in comparison with skin passed specimens.
having different intermetallic layers and separation between 5. Increasing the lead content of zinc bath would change the
eta layer and the substrate due to the presence of these morphology of the surface; i.e. the presence of basal planes
intermetallic layers, it seems to be not true for discussion at the surface decreases.
and consideration of the epitaxial or nonepitaxial growth of 6. Spangle size increases by addition of lead content in the zinc
the zinc crystals. It seems that in the hot-dip galvanizing, bath.
these boundaries are the boundaries of zinc crystals (Fig. 6(a)
and (d)). Acknowledgements
As can be seen in Fig. 17, the spangles are enlarged by
increasing the lead content of zinc bath in both skin passed and The authors would like to thank Mobarakeh Steel Company
non-skin passed specimens. This is because lead has lower laboratories staff and R&D unit engineers for helping with the
surface tension and promotes spangle formation [6]. In specimens. Assistance received from SEM and XRD labora-
addition, this element segregates ahead of the growing dendrite, tories staff of Materials Engineering Department of Isfahan
lowering surface tension and allowing the growth velocity of University of Technology is also appreciated.
H. Asgari et al. / Applied Surface Science 253 (2007) 6769–6777 6777

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