Surface & Coatings Technology 364 (2019) 218–224

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Surface & Coatings Technology

journal homepage: www.elsevier.com/locate/surfcoat

Effect of shot-blasting pretreatment on microstructures of hot-dip galvanized T

coating
⁎ ⁎
Jiaojiao Li, An Du, Yongzhe Fan, Xue Zhao, Ruina Ma , Jianjun Wu
School of Materials Science and Engineering, Hebei University of Technology, Key Lab for New Type of Functional Materials in Hebei Province, Tianjin Key Lab Materials
Laminating Fabrication and Interface, Tianjin 300132, People's Republic of China

A R T I C LE I N FO A B S T R A C T

Keywords: This study investigates the effect of shot-blast pretreatment on the microstructure of hot-dip galvanized coating
Shot-blasting of steel. The morphology, roughness, residual stress, phase composition and microhardness of the samples were
Hot-dip galvanizing measured to evaluate the effect of shot-blasting on the steel matrix. In comparison with pickled samples, the
Plastic deformation surface layer of the shot-blasted samples showed severe plastic deformation, and the tensile stress on the surface
Compressive residual stress
was transformed into compressive residual stress. In addition, both the surface roughness and microhardness
Grain refinement
increased greatly. Results showed that the microstructure of the hot-dip galvanized coating was influenced by
the compressive residual stress, roughness, grain size and crystal defect of the steel matrix. The compressive
residual stress inhibits the dissolution of Fe atoms, resulting in a thinner coating. Grain refinement and crystal
defect promoted the diffusion of Fe and Zn at the earlier stage of reaction and shortened the reaction time,
thereby increasing the coating thickness. The thickness of the entire coating of the samples decreases with the
increase in surface roughness.

1. Introduction
Hot-dip galvanizing is a common practice for protecting steel
components from corrosion in construction, automotive, and electrical
applications [1–5]. The protective layer not only acts as a barrier
against corrosive media, but also provides protection as a sacrificial
anode [6]. Rust removal is a very important step in the pretreatment
before hot-dipping. Pickling in acid is the most widely used method for
rust removal; however, over-pickling often occurs, and the process is
also environmentally hazardous because of the production of waste acid
[7]. Hence, shot blasting and shot peening are extensively employed for
mechanical rust removal. However, a prolonged and deep shot-blast
process is necessary to achieve the cleanliness required for hot-dip
galvanization. Therefore, excessive cleaning may occur, resulting in a
series of changes in the structure and performance of the sample sur-
face. Shot blasting and shot peening can result in high plastic de-
formation of surface layers, high surface roughness, compressive re-
sidual stress, work hardening, and high dislocation density [8–19]. The
change of the substrate described above exerts a great influence on the
structure and corrosion resistance of the coating.
Induction of plastic deformation of steels has already been im-
plemented for preprocessing for diffusion-based surface-modification
techniques such as plasma-carburizing [20], boriding [21,22], nitriding
[23–27], and gas nitriding [28]. The surface plastic deformation
treatment can accelerate the atomic diffusion rate, nucleation rate, and
diffusion kinetics [29–32]. Growth activation energy can decrease after
the surface plastic deformation treatment [33]. Wettability is also af-
fected by the surface plastic deformation treatment [34].
Based on a literature review, the surface plastic deformation treat-
ment was successfully used as a preprocessing method for diffusion-
based surface-modification techniques [20–28]. The surface plastic
deformation treatment could facilitate diffusion during ion nitriding,
boronizing, etc. However, previous studies have focused on the effect of
plastic deformation on diffusion. To the best of our knowledge, no
previous studies have examined the effect of surface plastic deformation
treatment on the structure of hot-dip galvanized coating. Hence, in this
study, hot-dip galvanization pretreatment by pickling and shot blasting
was compared, and the effect of plastic deformation on the structure of
hot-dip galvanized coating was analyzed.
2. Materials and methods
2.1. Sample preparation
Q235 steel samples (60 mm × 40 mm × 2.5 mm) were used in the
experiments, with chemical composition as given in Table I. The

⁎
Corresponding authors.
E-mail addresses: maryna@126.com (R. Ma), hbgdwjj@126.com (J. Wu).

https://doi.org/10.1016/j.surfcoat.2019.02.075
Received 18 September 2018; Received in revised form 19 February 2019; Accepted 22 February 2019
Available online 23 February 2019
0257-8972/ © 2019 Elsevier B.V. All rights reserved.
J. Li, et al.
Table I
Composition of Q235 steel (wt%).
C Mn Si S P Cr Ni
0.12–0.20 0.30–0.67 ≤0.30 ≤0.045 ≤0.045 ≤0.30 ≤0.30
samples were precleaned by shot blasting or pickling. Both operations
were performed at room temperature. The pickling treatment involved
placing the steel sample in hydrochloric acid with a concentration of
18–20% for 20 min. The pickled sample was cleaned in distilled water
and dried in air.
Shot blasting was performed on a shot-blast machine by steel balls
with 0.6 mm diameter for 60 min. Five of the shot-blast samples were
annealed at 200–600 °C for 2 h in an argon protective atmosphere,
followed by furnace cooling to room temperature at a rate of 2 °C min−1
to eliminate the residual stress. The samples were then cleaned in dis-
tilled water and dried in air.
To study the effect of surface roughness on the coating thickness,
samples with different surface roughness values were prepared by slight
grinding with 400 mesh and 2000 mesh abrasive paper. Thus, the in-
fluence on the galvanized coating of compressive residual stress, grain
size, and crystal defects from shot-blasting could be neglected.
Subsequently, hot-dip galvanizing of all the above samples was
carried out by dipping into a molten Zn bath at 460 °C for 40 s.
2.2. Measurements and observations
The surface morphology of the samples and the thickness of zinc
coating were measured by using an optical microscope. The cross-sec-
tion of the samples was polished to a mirror surface and then etched.
The microstructures of the samples were observed by a scanning elec-
tron microscope (SEM). Surface roughness of the pickled and shot-
blasted samples expressed in arithmetic average (Ra) was assessed
using a surface roughness tester. The XRD data were identified by using
a D8 FOCUS X-ray diffractometer (XRD), which was operated with Cu
Kα radiation (λ = 1.54056 Å), with a step width of 0.02°. Residual
stress profile in the surface region of the samples was measured by X-
ray diffraction. The microhardness was measured using a Vickers mi-
crohardness tester with a loading force of 0.1 N for 15 s.
3. Results and discussion
3.1. Microstructure and morphology of steel matrix
The cross-sectional SEM micrographs of steel matrix with different
pretreatments are shown in Fig. 1. The microstructure, composed of
equiaxed grains, did not change after pickling. However, severe plastic
deformation appeared in the shot-blasted samples [11], to a depth of
Fig. 1. SEM micrographs of the steel matrix with different pretreatment. (a) Pickled; (b) shot blasted.
Surface & Coatings Technology 364 (2019) 218–224
about 12 μm. The microstructure changes gradually from elongated
grains to the equiaxed grains in the matrix with increased distance from
Fe the surface [35].
The 3D morphology and surface profiles of pickled and shot-blasted
Bal. samples are shown in Fig. 2. It can be seen that the pickled surface is
much smoother than the shot-blasted surface. The significant changes
to surface morphology can be observed after the shot-blasting treat-
ment. Comparatively large dimples appear on the surface of the shot-
blasted samples because of high velocity impacts on the surface by shots
[36]. In addition, a great deal of pile-ups are produced around the
dimples [11]. Compared with the pickled samples, the shot-blasted
samples showed increased average surface roughness. The roughness
values (Ra) increased from 0.18 to 0.32 μm.
3.2. Surface residual stress and XRD analysis
The surface stress of the pickled samples is tensile stress, the value
of which is 15.86 ± 26.03 MPa. On the contrary, significantly high
stress is generated in the surface after shot blasting, of
−336.58 ± 19.78 MPa. Meanwhile, the shot blasting converts the
surface tensile stress to surface compressive residual stress. A similar
result was reported by Pandey et al. [10].
The X-ray diffractograms of the pickled and shot-blasted samples are
shown in Fig. 3. No phase change occurs after the shot-blasting treat-
ment, and the location of diffraction peaks is almost the same as in the
pickled samples [8]. An evident broadening of the diffraction peaks of
shot-blasted samples can be seen in Fig. 3. The result can be ascribed to
the grain refinement, lattice deformation, and/or an increase in the
atomic-level microstrain [11,37].
3.3. Variation trend of microhardness
The thickness of the affected layer of samples with different pre-
treatment is shown in Fig. 4. Compared with the pickled samples, the
shot-blasted samples showed significantly increased surface hardness
[38]. The microhardness decreases rapidly as the depth increases to
8 μm, and then more gradually decreases to a stable value around
12 μm. It is reasonable to deem that this result is caused by the com-
pressive residual stress and refined grains caused by shot blasting [13].
3.4. Morphology of coatings
Cross-sectional SEM micrographs of the galvanized coating after the
pickling and shot-blasting pretreatments are shown in Fig. 5. The
FeeZn “outbursts” are formed at the raised areas of steel matrix surface
after shot blasting [39], which is coarser and looser than that in the flat
surface and the pickled samples. The thickness of the δ phase on the
raised areas of the surface is much thinner than that of the flat surface.
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J. Li, et al.
Fig. 2. 3D morphology and surface profiles of samples treated by pickling and shot-blasting. (a) Pickled; (b) shot blasted.
Fig. 3. X-ray diffractograms of pickling and shot-blasting samples. (a) Pickled;
(b) shot blasted.
It is obvious that the coating thickness is uniform after pickling.
However, the coating thickness is inhomogeneous after shot blasting,
which is loose at the bulge of the steel substrate. Shot blasting enables
the coating thickness to decrease in comparison to that of the pickled
samples. The coating consists of η phase, ζ phase, and δ phase from the
surface to the inside of the sample [6]. The average thickness of each
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Surface & Coatings Technology 364 (2019) 218–224
Fig. 4. Thickness of the affected layer of samples with different processes. (a)
pickled; (b) shot blasted.
phase in the galvanized coating without outbursts is also measured. For
the pickled galvanized sample, the thickness of the galvanized reaction
coating is about 31.3 μm, and the ζ phase has an average thickness
about 28.5 μm. The average thickness of the δ phase is even more
uniform, about 2.8 μm. Meanwhile, for the shot-blasted sample, a gal-
vanized reaction coating of about 27.1 μm is observed. The average
thickness of the ζ phase in the flat part of the surface is slightly de-
creased, being about 24.5 μm. The average thickness of the δ phase is
about 2.6 μm.
There are four factors that can influence the coating thickness:
roughness, surface compressive residual stress, refinement of grain size,
and high dislocation density. It is common sense that the refinement of
grain size and high dislocation density generated from the grain
boundaries provide a fast diffusion channel for the diffusion of FeeZn
[34,40,41] and increase the rate of nucleation of iron atoms [33],
which will cause a thicker coating.
J. Li, et al. Surface & Coatings Technology 364 (2019) 218–224

Fig. 5. Cross-sectional SEM micrographs of galvanized coating with the pickled and shot-blasted pretreatment. (a) and (c) Pickled; (b) and (d) shot blasted.

3.5. Effect of the compressive residual stress on the microstructure of the

coating

The effect of compressive residual stress on the microstructure of

the coating is analyzed by annealing the shot-blasted sample at the
recrystallization temperature. The surface roughness of the shot-blasted
samples at room temperature and after annealing at different tem-
peratures from 200 to 600 °C is shown in Fig. 6. It can be seen that the
surface roughness of shot-blasted samples remains unchanged after
annealing at different temperatures. The thickness of the affected layer
of the shot-blasted samples with and without annealing at different

Fig. 7. Thickness of the affected layer of shot-blasted samples with non-an-

nealing and annealing at different temperatures.

temperatures is shown in Fig. 7. The thickness of the affected layer

Fig. 6. Surface roughness of shot-blasted specimens at room temperature and
after annealing at different temperatures from 200 to 600 °C.
decreases gradually with the increase in annealing temperature. Some
researchers [42] pointed out that the trend of compressive residual
stress is very similar to that of the hardening thickness. Therefore, it can
be assumed that most of the residual stress is released and almost dis-
appears after annealing. As shown in Fig. 8, the Bragg diffraction peak
remains unchanged after annealing at 200 °C and becomes narrow after
300 °C. This shows that there is no change in the grain size and crystal
defects in preliminary annealing. After annealing at 300 °C, the crystal
defects gradually decrease. Wu et al. [13] reported similar results.
The variation in the thickness of the galvanized coating after

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J. Li, et al. Surface & Coatings Technology 364 (2019) 218–224

Fig. 8. X-ray diffractograms of shot-blasted samples at room temperature and

after annealing at different temperatures from 200 to 600 °C.
Fig. 9. Thickness variation of each phase in galvanized coating annealed at
different temperatures.
annealing at different temperatures is presented in Fig. 9. The average
thickness of the galvanized coating on the annealing samples gradually
increases as annealing temperature is increased, for temperature up to
400 °C. With annealing temperature at or above 500 °C, the thickness of
the coating decreases slightly. After annealing at 200 °C, the influence
of surface roughness and grain size on galvanized coating can be ne-
glected. In the hot-galvanizing process, iron dissolves first. The surface
compressive residual stress induced by the shot blasting acts as a sur-
face barrier that inhibits the dissolution of Fe atoms from the steel
matrix and results in the thinning of the coating [43,44]. Subsequently,
the residual stress is gradually released and the thickness of the coating
increases with increasing annealing temperature. However, the thick-
ness of the coating fluctuates and is not thickened continuously. Fig. 10
shows the morphology of the galvanized layer after annealing at 600 °C.
It can be seen that there are still outbursts in the coating. This may
indicate that residual stress is not the only factor affecting the coating.
The cross-sectional SEM micrographs of the shot-blasted steel ma-
trix after annealing at 300 °C and 600 °C are shown in Fig. 11. No re-
crystallization occurs at 300 °C. After annealing at 600 °C, the deformed
grains almost disappear and smaller equiaxed grains appear. After an-
nealing at 300 °C, the microstrain and dislocation density decline [42], Fig. 10. Morphology of the galvanized layer after annealing at 600 °C.
resulting in a reduction in the rate of the FeeZn reaction. With an-
nealing at 400 °C, the recrystallization of part of the yielding grain
3.6. Effect of the grain size and crystal defect on the microstructure of the
occurs and grain refinement is initiated. An increased amount of in-
coating
termetallic phases will nucleate at the grain boundary. After annealing
at 500 °C, the crystal defects are basically eliminated and the accel-
As shown in Fig. 12, the grain refinement zone is retained under-
eration of the FeeZn reaction disappears.
neath the galvanized coating on the shot-blasting sample. Sun et al.
[28] also found that the deformation layer was retained after nitriding
treatment at 520 °C. This shows that the grain refinement zone does not

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J. Li, et al.
Fig. 11. Cross-sectional SEM micrographs of shot-blasted steel matrix at 300 °C and 600 °C.
Fig. 12. Cross-sectional SEM micrographs of shot-blasted steel matrix after hot-
dip galvanizing.
disappear completely in the galvanizing process, and it still affects the
coating structure.
3.7. Effect of the roughness on the microstructure of the coating
Balusamy et al. [32] suggested that the increase in surface rough-
ness induced by the plastic deformation impacts the subsequent diffu-
sion. However, the effect of roughness on the microstructure needs to
be further explored. The surface roughness of the non-shot-blasted
samples was changed by slight grinding with different types of me-
tallographic abrasive paper. In this process, the sample surface is only
mildly polished; hence, the influence of compressive residual stress and
crystal defect on the galvanized coating can be neglected. Fig. 13 shows
variation in the thickness of each phase in the galvanized coating with
different roughness values. The thickness of the entire coating of the
samples decreases with the increase in the surface roughness. Singh
et al. [45] reported similar results. For surfaces with higher roughness,
both the spreading area and time reduced because of weak wettability
[46]. In addition, the increase in roughness would decrease the diffu-
sion coefficient [47]. These might be the reasons why the coating
thickness became thinner with the increase in roughness.
4. Conclusion
A shot-blasting pretreatment was performed on the surface of the
steel substrate followed by hot-dip galvanizing. The characterization of
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Surface & Coatings Technology 364 (2019) 218–224
Fig. 13. Thickness of each phase in the galvanized coating varying with the
roughness.
the steel surface after the shot-blasted treatment was investigated.
Following these characterization studies, the effect of the change of the
steel surface on the microstructure of galvanized layer was analyzed.
The main conclusions are as follows:
(1) Shot blasting could change the properties of a part of the steel
matrix. The grain size reduction and compressive residual stress on
the surface of the sample were induced by shot blasting. Non-uni-
form microscopic strain and crystal defects such as dislocation
density of the steel matrix were increased after shot blasting. The
surface hardness and surface roughness of the steel matrix also
significantly increased.
(2) The morphology of grains on and near the surface of the steel
substrate was changed by shot blasting. The shot-blasted samples
had a large number of small dimples and pile-ups on the surface,
and the undulating degree of the interface was intensified. A 12-μm
depth of plastic deformation layer was produced in the near surface
area, and the grains on the surface were elongated perpendicular to
the deformation direction with disk shape. With the increase in
depth, the grains gradually became equiaxed, and the morphology
became close to that of the pickled samples.
(3) Compared with the pickled samples, the outbursts were formed on
the raised areas on the surface of the shot-blasted samples, and the ζ
phase was coarser and looser than that on the flat surface and the
pickled samples. The thickness of the coating decreased in the flat
parts of the sample, and outbursts were formed by subsequent
J. Li, et al.
diffusion.
(4) The compressive residual stress inhibited the thickening of the
coating. The roughness had a deleterious influence on the thickness
of the coating. Four factors, including the grain size and crystal
defects, led to the formation of a thinner galvanized coating.
Future work should consider the mechanism of the effect of
roughness on coating thickness.
Funding
This work was supported by the National Natural Science
Foundation of China (grant numbers 51601056); and the Natural
Science Foundation of Hebei Province of China (grant number
E2017202012).
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