Surface & Coatings Technology 342 (2018) 29–36

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Surface & Coatings Technology

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

Aluminizing mechanism on a nickel-based alloy with surface nanostructure T

produced by laser shock peening and its effect on fatigue strength
⁎
Luo Sihaia, He Weifenga,b, , Zhou Liuchenga, Nie Xiangfana, Li Yinghonga,b
a
Science and Technology on Plasma Dynamics Laboratory, Air Force Engineering University, Xi'an, Shaanxi 710038, China
b
School of Mechanical Engineering, Xi'an Jiaotong University, Xi'an, Shaanxi 710049, China

A R T I C L E I N F O A B S T R A C T

Keywords: A nanocrystalline surface layer with grain sizes ranging between 30 and 150 nm was fabricated on a K417 nickel-
K417 nickel-based alloy based cast alloy by means of laser shock peening (LSP). The effect of the surface nanostructure on the gas
Laser shock peening aluminizing process was investigated through microstructure characterizations, carried out by transmission
Surface nanostructure electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results
Gas aluminizing
showed that, following the LSP treatment, a higher amount of Al diffused into the matrix and a thicker-alu-
Diffusion mechanism
minizing layer was produced. The diffusion mechanism was that the thermal stability of surface nanostructure
Fatigue strength
and high-density dislocation induced by LSP increased its surface activity and made more channels available for
element diffusion during the high temperature gas aluminizing processing. The specimens in different surface
treatments (aluminizing and LSP + aluminizing) were then subjected to vibration fatigue load. The fatigue
strengths of the aluminizing specimens and LSP + aluminizing specimens were 226 MPa and 335 MPa, respec-
tively. All the results indicated that LSP-induced surface nanostructure increased the efficiency of the alumi-
nizing process and the fatigue resistance.

1. Introduction
The nickel-based alloys blades of modern gas turbine aero-engines
operate in the extreme rigorous conditions, exposed to severe me-
chanical and thermal stress, which would cause fatigue failure. In the
absence of protective coatings, these may cause fatigue failure, oxida-
tion and hot corrosion, seriously damaging the components of the aero-
engine and potentially leading to its failure. Nickel aluminide coatings
are commonly applied on nickel-based alloys to improve their fatigue,
oxidation and corrosion resistance [1–4].
The gas aluminizing process is one of the most cost-effective pro-
cesses used to form a nickel alumina coating on the surface of engine
components. In particular, due to the possibility of using this technique
on the components with different sizes and shapes, it is widely used to
form a dense aluminum compound protective layer on the surface of
metallic alloys. During the process, the diffusing Al atoms react with the
substrate elements and form the more strengthening γ′ phases.
Consequently, the global mechanical properties and fatigue resistance
are improved. Many investigations have been carried out and it has
been found that the thickness and concentration of the diffusion layer
developed during the thermochemical treatment process depend on the
processing conditions and the surface microstructure of the substrate
alloy [3–6]. For example, Gleiter [7] and Lu et al. [8] suggested that a
large number of grain boundaries in the ultrafine grains, especially in
nanocrystalline materials, act as fast atomic diffusion channels and
enhance the surface activity. Shen et al. [9] found that the atomic
diffusivity was enhanced in nanocrystalline materials compared to their
coarse grained counterparts. Moreover, various kinds of non-equili-
brium defects presented in the nano-grain boundaries could act as a
high-energy storage and further enhance the surface diffusivity [10,11].
Hence, we believe that surface microstructure change, especially sur-
face nanocrystallization, is a good option for accelerating the produc-
tion of diffusion layers.
Severe plastic deformation (SPD) induced by surface mechanical
treatments, such as surface mechanical attrition treatment (SMAT) and
shot peening, is recognized as an effective method to produce a surface
nanostructure that can promote diffusion [12–19]. Xiang et al. [15]
found that the SMAT treatment induced the formation of nanoscale
grains and high-density dislocations, and promoted the diffusion pro-
cess as well as the formation of a thicker diffusion layer. Hong et al.
[16] utilized ultrasonic nanocrystal surface modification on Pt-modified
aluminide coatings of nickel-based alloys to form a surface nanos-
tructure layer, which resulted in higher Al concentrations in the
coating. Similar results had also been reported in previous works

⁎
Corresponding author at: Science and Technology on Plasma Dynamics Laboratory, Air Force Engineering University, China, 1St Baling road, Xi'an, Shaanxi 710038, China.
E-mail address: hehe_coco@163.com (H. Weifeng).

https://doi.org/10.1016/j.surfcoat.2018.02.083
Received 1 November 2017; Received in revised form 5 February 2018; Accepted 21 February 2018
Available online 15 March 2018
0257-8972/ © 2018 Elsevier B.V. All rights reserved.
L. Sihai et al.
[17–19]. These studies indicated that surface refined-grains or surface
nanocrystallization induced by SPD could effectively improve the
atomic diffusivity and mechanical properties of diffusion layers. How-
ever, the industrial application of these methods to turbine blades is
limited by their uncontrollability and the significant surface toughness
deriving from the severe plastic deformation.
Laser shock peening (LSP) is one of the most commonly SPD
methods and has been previously proposed as a technique to produce
the surface nanocrystalline layer on nickel-based alloys, titanium alloys
and stainless steels [20–30]. Compared with other surface mechanical
treatment technologies, LSP has the advantages of not requiring contact
with the substrate, of affecting a deep layer, and having excellent
controllability. In addition, this technique results in a surface with
lower toughness, making it applicable to complex aero-engine compo-
nents [31]. In our previous works, we found that the surface nanos-
tructure produced by LSP in nickel-based alloy has good thermal sta-
bility at 900 °C [24,25]. On the other hand, LSP can introduce
compressive residual stress that improves the resistance to fatigue and
hot corrosion [32–36]. Thus, laser shock peening is considered as one of
the most promising methods for improving the atomic diffusion of Al in
nickel-based alloy turbine blades.
In this work, we investigated the surface nanostructure produced by
laser shock peening and the atomic diffusion of Al in a modified gas
aluminizing process. The microstructure of the coatings was char-
acterized and the effect of surface nanostructure on the gas aluminizing
process was investigated. Moreover, the fatigue strength of the alumi-
nide coatings was examined.
2. Experiments and methods
2.1. Materials
The experimental material is the K417 nickel-based cast alloy,
which has been broadly applied in aero-engine turbine blades due to its
excellent fatigue, corrosion and creep resistance. It mainly consists of γ
solid solution, strengthening phase γ′ and (γ + γ′) eutectic, as shown in
Fig. 1a. To further justify the presence of the γ and γ′ phases, TEM
observation was adopted, as shown in Fig. 1b and c. The nominal
chemical composition is listed in Table 1 and the atomic scale structure
of γ and γ′ phases can be seen in reference [36]. The alloy elements,
such as Co, Cr, Mo, V, play a positive role in solid solution strength-
ening; the precipitation phase can be formed by the additions of alloy
elements, such as Ti and Al, which has precipitation strengthening ef-
fect; and the alloy elements, such as B, C and Zr, have a beneficial effect
on the grain boundary strengthening.
2.2. Experimental process of LSP
To evaluate the effect of surface nanostructure on the gas
Fig. 1. Surface microstructure in the substrate of K417 nickel-based alloy. (a) SEM image, (b) TEM image and (c) the corresponding SAED image of (b).
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Surface & Coatings Technology 342 (2018) 29–36
aluminizing process, LSP treatment was adopted previously. Prior to
LSP treatment, the samples surface was polished with SiC paper with
the grit number from 500 to 2400, and then ultrasound cleaning in
ethanol was used to degrease the surface of samples. The LSP procedure
was performed on a Q-switched Nd:YAG laser designed by the company
of TYRIDA, Xi'an, Shaanxi (SGR-EXTRA/25J). The corresponding ex-
perimental set-up and detail procedures were previously described in
the literature [37]. A laser with the following listed parameters was
used: energy is 10.8 J, pulse width is 20 ns, laser beam diameter is
3.4 mm, and power density is 6 GW/cm2. In order to avoid the bend by
one-sided LSP and improve the efficiency of LSP process, two-sided LSP
was used on the standard vibration specimens. The paths of laser spots
and LSP region are shown in Fig. 2.
2.3. Gas aluminizing process
Both the samples pre-treated or pre-untreated by LSP treatment
were washed carefully using the acetone and absolute alcohol and then
immediately being subjected to gas aluminizing treatment, carried out
in a homemade device, as shown in Fig. 3. Gas aluminizing process was
carried out in a special pit furnace with a pre-evacuated vacuum me-
chanical pump and the materials were embedded in a birdcage clamp.
Al-Fe powder was used as infiltration agent, ammonium chloride
(NH4Cl) was used as activator and aluminum oxide (Al2O3) powder was
used as filler. Subsequently, the samples were aluminized at high
temperature condition. To avoid surface oxidation and ensure inert
atmosphere conditions during the whole process duration, the furnace
was vacuumed to 10−3 mbar and then filled with argon. The process
was carried out at 900 °C + 10 °C and lasted 2 h.
2.4. Microstructural observations
The phase analysis of aluminide coatings was characterized by MFS-
7000 X-ray diffraction (XRD) equipment with Cu-kα radiation
(λ = 1.5406 nm), operated at a voltage of 50 kV, a current of 40 mA
and a take-off angle of 6°. The diffraction data were collected over a 2θ
range of 20°–100°, with a step width of 0.02°. The grain sizes and in-
tegrated areas for β-phase and δ-phase diffraction peaks in the XRD
spectra were determined by using the MDI Jade 6 software.
To precisely characterize the surface microstructure of K417 nickel-
based alloy after LSP treatment, transmission electron microscopy
(TEM) observation was used. TEM was performed in JEM 2100F with
the experimental parameters: FEG (field emission gun): 200 kV; point
resolution: 0.23 nm and line resolution: 0.14 nm. The thin foils for TEM
observations were cut by electro-spark discharge from the surface layer
with a thickness of 1 mm, then mechanically grinded on the untreated
sides to obtain thin plates with a thickness of about 20 μm, and finally
single electro-polished from the untreated side. Microstructural mor-
phological images were observed by JEOL/JSM-6360LV scanning
L. Sihai et al.
Table 1
Composition of K417 cast nickel-base superalloy.
Composition Cr Co Mo Ti
Percentage (wt%) 8.5–9.5 14–16 2.5–3.5 4.5–5.7
Fig. 2. The shape and size of vibration fatigue test specimen.
Fig. 3. Schematic representation of the gas aluminizing device.
electron microscope (SEM) operated at a voltage of 20 kV, an equipped
energy dispersive spectroscopy (EDS) system was used to determine the
compositions within the aluminizing coatings.
2.5. High cycle fatigue method
High cycle fatigue (HCF) is one of main failures modes in modern
military aircraft gas turbine engines. The vibration fatigue tests were
designed and carried out using the D-300-3 electric vibration system at
resonant frequency of first order, room temperature and in air. The size
and shape of the fatigue specimens is shown in Fig. 2. Before the ex-
periment, the frequency sweeping method was adopted to obtain the
natural frequency of the samples at room temperature. The experiment
showed that the resonant frequency of K417 samples was about 293 Hz.
During the fatigue testing, the specimen tip amplitude was obtained by
displacement transducer (optical microscope and eddy current dis-
placement sensor). Gauges were glued on the center of the notch region
of the specimen, which were used to monitor the strain in the vibration
process.
An up-down method was adopted to determine the fatigue strength.
If the cumulative excitation frequency dropped to 1% of resonant fre-
quency before the number of fatigue cycles reached the 107, the test
Surface & Coatings Technology 342 (2018) 29–36
Al C V B Zr Mn Si Ni
4.8–5.7 0.13–0.22 0.6–0.9 0.012–0.022 0.05–0.09 < 0.5 < 0.5 Bal.
was stopped and the specimen was defined as “Break”. If the frequency
decreased cumulatively below 1%, and the fatigue cycles number was
higher than 107 cycles, the test was stopped and the specimen was
defined as “exceeded”.
3. Results and discussion
3.1. Microstructure evolution induced by LSP
Fig. 4 shows the typical TEM images at different depths of the K417
nickel-based alloy sample after LSP treatment. Surface nanocrystallines
with sizes of 30–150 nm were produced after LSP treatment, as shown
in Fig. 4a and b. The corresponding circles selected area electron dif-
fraction (SAED) pattern indicates the nanocrystallines with random
orientations. In addition, the nanocrystallines are obviously elongated
in the direction perpendicular to that of the LSP process. As is known,
during the shock wave propagation, the pressure on the material de-
creases as with the depth increases. At a depth of ~2 μm from the
treated surface, dislocation cells and high-density dislocations are
generated (Fig. 4c). With a further increase in the depth to 5 μm, lower
but still significant density dislocations are found (Fig. 4d). We notice
that the dislocation activity caused by the laser-induced shock wave is
the main reason for the formation of surface nanocrystals. The com-
prehensive explanation of the surface nanocrystallization mechanism
induced by LSP has been described in detail in a previous study [23].
The formation of the nanocrystalline and the high-density disloca-
tions in the surface layer of nickel-based alloy after LSP treatment led to
the formation of a large number of defective grain boundaries and the
aluminizing process was carried out under 900 °C high temperature
conditions. Thus, the thermal stability of the surface nanostructure and
high-density dislocations induced by LSP are the key issues. In a pre-
vious work, we investigated thoroughly the thermal stability of the
surface nanostructure layer on the K417 nickel-based alloy in detail
[25]. The results showed that at 900 °C, the surface nanostructure can
maintain a good thermal stability for a long time. In particular, at the
annealing temperature of 900 °C, the largest grain size in the surface
nanostructure layer increased from 140 nm to 220 nm and some of the
smaller grains, with the size of around 50 nm, could still be found after
the annealing process. The reasons for the good thermal stability of the
surface nanostructure induced by LSP are the lower cold work hard-
ening rate of LSP, the large volume fraction of grain boundaries present
in the surface nanocrystalline layer and the stability of the high-density
dislocations. The high thermal stability, along with the dislocation
density, provides suitable conditions for and plays an active part in high
31
L. Sihai et al.
temperature gas aluminizing. A more detailed discussion is presented in
the following section.
3.2. Aluminizing and microstructure characterization
To investigate the effect of the surface nanostructure induced by LSP
on the formation of the aluminide coatings, the XRD peaks of the sur-
face coatings obtained with different treatments were analyzed and the
results are shown in Fig. 5. The surface coatings in the aluminizing and
LSP + aluminizing samples both contain strong diffraction peaks re-
lative to the β-NiAl phase, as well as weak diffraction peaks associated
to the δ-Ni2Al3 phase. According to the “high activity” formation me-
chanisms [38], it may be concluded that the diffusion layers are pri-
marily developed by inward diffusion of Al inside the Ni matrix, rather
than outward diffusion of nickel, which leads to the formation of the
dense β-NiAl phase. Ehtemam–Haghighi et al. [39,40] proposed a
method to calculate the volume factions of alloy phases based on the
Fig. 5. The XRD patterns of the K417 nickel-based alloys after aluminizing processing
with and without pre-LSP treatment.
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Surface & Coatings Technology 342 (2018) 29–36
Fig. 4. Typical microstructures at different depths of the
K417 nickel-based alloy after LSP treatment. (a) bright-
field image of the surface nanocrystalline with the grain
sizes ranging from 30 to 150 nm, (b) the corresponding
dark-field image of image (a), (c) dislocation cells and
high density dislocations at the depth of 2 μm, (d) dis-
locations at the depth of 5 μm. The inset in (a) shows the
corresponding SAED pattern.
integrated areas of diffraction peaks. Due to there exists two phases in
several diffraction peaks, the quantitative volume factions of β-NiAl
phase and δ-Ni2Al3 have difficult to be estimated based this the method.
But we concluded that more Al element diffusion into the matrix for the
sample treated by pre-LSP based on the integrated areas of diffraction
peaks obtained by MDI Jade 6 software.
In addition, the full width at half maximum (FWHM) and the cor-
responding location of the aluminizing and LSP + aluminizing samples
were shown Table 2. The results showed that the FWHM of aluminizing
samples with pre-LSP treatment was broader compared with that of
aluminizing samples without pre-LSP treatment. Based on the XRD
patterns, the grain size of LSP + aluminizing sample changed from
several micrometers of the aluminizing only sample to 32 nm. Mean-
while, the locations of the diffraction peaks shows only small deviations
between the two samples. The small deviations of diffraction peaks
locations was mainly due to the thermal stability of the micro-strain
and nanoscale grains introduced by pre-LSP treatment.
To further analyze the difference between the aluminizing and
LSP + aluminizing samples, the cross-sectional microstructures were
observed by SEM (Fig. 6). Three layers, referred to as inner, middle and
outer, could be found in the aluminide coatings of both samples. Fig. 6a
shows the cross-sectional microstructure of the aluminide coating in the
original aluminizing sample. The thickness of the diffusion coating was
~17 μm. The thickness and microstructural characteristics of the
Table 2
The FWHM and the corresponding locations of the diffraction peaks for the aluminizing
and LSP + aluminizing samples.
hkl FWHM/2θ
Aluminizing LSP + aluminizing
100 0.198/31.04 0.314/30.98
110 0.236/44.50 0.279/44.46
111 0.251/55.26 0.292/55.22
200 0.325/64.72 0.458/64.66
211 0.394/81.92 0.547/81.90
220 0.455/98.32 0.525/98.28
L. Sihai et al.
Fig. 6. SEM images of the K417 nickel-based alloy aluminizing diffusion layer structure under different surface treatments. (a) Aluminizing diffusion layer structure of the aluminizing
treatment, and particles in the diffusion layers were deposited randomly; (b) Diffusion layer structures of LSP + aluminizing treatment, and particles in diffusion layers were deposited
orderly and acicular crystal appeared in local area of diffusion layers.
diffusion coating in LSP + aluminizing sample were different. During
the high temperature aluminizing processing, Al2O3 can be produced on
the material surface, hindering the diffusion of Al atoms into the ma-
terial. On the other hand, the stable β-NiAl phase was formed on the
surface. This is why there was no change in the outer layer thickness
between the aluminizing sample and the LSP + aluminizing sample
(Fig. 6b), i.e. the outer layer thickness of the two samples was always
~10 μm. The random distribution microstructure in the diffusion layer
of the aluminizing sample has a tendency to transform into an orderly
distribution, with a preferential growth direction and the formation of
an acicular structure, in the LSP + aluminizing sample (Fig. 6b). This is
because the severe plastic deformation induced by LSP provides the
energy required for the acicular crystal growth. At the beginning of the
aluminizing processing, the grain nucleation locations of the β-NiAl and
δ-Ni2Al3 phases were formed on the surface of the nickel and chromium
atoms, respectively. Under the same aluminizing conditions, the refined
nickel particles formed during the LSP treatment significantly increased
the NiAl nucleation rate and shortened the distance between different
NiAl nucleation sites. In other words, the formation of a surface na-
nostructure and dislocation defects induced by LSP could effectively
shorten the formation time of the dense NiAl layer. In addition, the
refined nickel particles also increased the diffusion rate of Al into the
matrix, resulting in the rapid formation of the NiAl layer. This is why
the thickness of the inner layer was increased from ~7 μm to ~10 μm.
3.3. Element distribution in the aluminizing coatings
The cross-sectional SEM images and related EDS results at different
depths of aluminizing and LSP + aluminizing samples are shown in
Fig. 7. At the beginning of aluminizing process, the Al diffusion coef-
ficient was orders of magnitude larger than that of Ni [3]. This means
that vapor phase deposited Al diffused into the matrix and reacted with
Ni, resulting in the formation of the δ-Ni2Al3 phase. With the increase in
temperature and stabilizing heating treatment, the metastable δ-phase
(Ni2Al3) further transformed into the stable dense β-phase (NiAl). The
formation of δ-Ni2Al3 and β-NiAl could be demonstrated by the increase
in Al content at point 1 (Fig. 7a) of the outer layer (Fig. 7b) and XRD
results (Fig. 7). When the temperature increased to 900 °C, the diffusion
coefficient of Ni also increased significantly, but the δ-Ni2Al3 layer,
especially the dense β-phase layer, formed previously prevented the
outward-diffusion of Ni. Therefore, the outward-moving Ni reacted
with Al, which diffused across the δ-Ni2Al3/β-NiAl layer, resulting in
the formation of the γ′-Ni3Al phase, as seen from the element dis-
tribution at point 3 (Fig. 7a) of the inner layer (Fig. 7b). It is worth
noting that a “low activity” process also exists in the aluminizing pro-
cess. According to the “low activity” mechanism [3], the alloy elements,
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Surface & Coatings Technology 342 (2018) 29–36
such as Ti, Cr and Co, will precipitate at the interface between the β-
NiAl layer and the substrate, and then react with the outward diffusing
C element, forming an interdiffusion layer containing some carbides,
such as M23C6 and M7C3. This was proved by the EDS result at point 2 of
the middle layer in Fig. 7b. The presence of a large amount of alloy
elements could further restrict the outward diffusion of Ni and promote
the formation of γ′-Ni3Al phase, which contributes to increasing the
fatigue property during the cycle loading. Due to the outward-diffusion
of alloy elements, the contents of Cr, Co and Mo decreased at the
substrate (point 5 in Fig. 7b) and increased at and near the inner layer
(point 3 and 4 in Fig. 7b) compared with that in original samples
(Table 1).
3.4. Diffusion mechanism in a surface nanostructured layer
Nanostructured materials have numerous grain boundaries and an
enhanced diffusivity compared to the original materials because of the
lower activation energy at grain boundaries [5]. Moreover, in a pre-
vious work [25], we found that the surface nanostructure induced by
LSP in K417 nickel-based alloy can keep a good thermal stability even
at high temperature. Therefore, the sample with pre-LSP treatment can
provide a large number of fast diffusion channels during the high
temperature gas aluminizing process. In addition, the number of nu-
cleation sites is evidently higher in nanostructured materials, due to the
large amount of grain boundaries and high-density dislocations. These
are the main reasons for which the β-NiAl phase and a small amount of
the δ-Ni2Al3 phase on the surface were found at point 1 of the outer
layer (Fig. 7c and d): a larger amount of Al atoms diffuse into the
substrate compared to the original sample. Underneath the diffusion
layer (point 4 in Fig. 7c), the contents of Ni and Al were higher than
they were in the same location of the original aluminizing sample. This
indicates that some Al atoms are capable of diffusing across the surface
of the NiAl layer due to the LSP-induced surface nanocrystallization.
Moreover, carbides also existed in the interdiffusion layer, and the
contents of Cr and Co were higher in the inner layer, as seen in point 3
(Fig. 7b and d). The increase of Al and Cr contents had a positive role on
the oxidation resistance [41]. On the other hand, the presence of a large
amount of alloy elements restricted the outward diffusion of Ni, which
is why there was a higher Ni content at point 4 (Fig. 7d) compared with
that at the same point of the original aluminizing sample (Fig. 7b).
Accordingly, the SEM micrographs and related EDS results indicated
that there existed three layers in both the original aluminizing and
LSP + aluminizing samples. The outer layer was formed by the δ-Ni2Al3
and Al-rich β-NiAl phases; the middle layer consisted of β-NiAl, en-
riched by some alloy elements; the inner layer consisted of γ′-Ni3Al. The
difference between the original aluminizing and LSP + aluminizing
L. Sihai et al. Surface & Coatings Technology 342 (2018) 29–36

Fig. 7. SEM cross-sectional images and associated element distributions at different depths of the aluminizing layer of the K417 nickel-based alloy. (a, b) aluminizing sample; (c, d)
LSP + aluminizing sample.

samples was only in the element distributions in the three layers.

Therefore, the diffusion mechanism during the two aluminizing pro-
cesses could be described in the same manner.
According to the results of Goward [42], the Al atoms diffusion rates
in the δ-Ni2Al3 phase are three to four orders of magnitude higher than
that in the γ′-Ni3Al and β-NiAl phase at the low temperature, so the
inward diffusion of the active Al atoms inside the sample surface oc-
curs, leading to the formation of metastable δ-Ni2Al3. The metastable δ-
phase (Ni2Al3) further transformed into the stable dense β-NiAl phase
during the heating treatment. This is why the outer layer consists of δ-
Ni2Al3 and Al-rich β-NiAl phases. For a short time further inward alu-
minum diffusion must occur, and the aluminum content of the advan-
cing interface must decrease to a value at which formation of the β-NiAl
by the Al diffusion can no longer occur at some point (middle layer). At
the high temperature condition, the Ni diffusion coefficient increased
significantly. The large amount of outward-moving Ni reacts with the
inward diffusion Al atoms, and then promoted the formation of γ′-Ni3Al
in the inner layer (point 3 in Fig. 7).
Fig. 8. Fatigue strengths of K417 nickel-based alloy with different surface treatments.

3.5. High cycle fatigue strength

To further verify the effects of different surface treatments on the
fatigue strength of K417 nickel-based alloy, the high cycle fatigue test
was designed and adopted according to the Chinese technology stan-
dard (HB5277-84). Thirty standard vibration fatigue specimens were
machined into the dimensions shown in Fig. 2. Half of the prepared
specimens was treated by aluminizing and the other half was treated by
LSP + aluminizing.
The fatigue strength of the K417 nickel-based alloys with different
surface treatments is shown in Fig. 8. We had previously investigated
the effect of LSP treatment on the fatigue strength of K417 nickel-based
alloys [24]. The results showed that the fatigue strength was increased
from 110 MPa, relative to the original samples, to 285 MPa after LSP
treatment. The fatigue strength improvement was attributed to the high
amplitude and larger depth compressive residual stress and to the mi-
crostructural change. In addition, the fatigue strength of the LSP-treated
K417 nickel-based alloy was still increased to 230 MPa after a 10 h
heating treatment at 900 °C. Although most of the compressive residual
stress generated by LSP was relaxed at high temperature, the additional
increase in fatigue strength was mainly attributed to the surface na-
nostructure induced by LSP with relatively good thermal stability at this
temperature.
In this work, the fatigue strength of the sample not subjected to LSP
increases from 110 MPa to 226 MPa after aluminizing. The fatigue
strength increases to 335 MPa for the aluminizing sample subjected to
pre-LSP treatment, which is higher than that of aluminizing samples
(226 MPa) and LSP + 900 °C samples (230 MPa). The improvement
mechanism of aluminizing with or without pre-LSP treatment on fa-
tigue strength are different from the mechanism of LSP, the detailed
discussions are as follows.
It is well known that the γ′ phase in nickel-based alloys is the main

34
L. Sihai et al.
strengthening phase. During the aluminizing process, some Al atoms
could diffuse into the substrate and then react with Ni to form new γ′
phase. Moreover, the diffusion of Ti could replace the Al atoms of the γ′-
Ni3Al phase and form Ni3(Al, Ti) compounds, which could increase the
content of the γ′ phase in the surface layer. On the other hand, the
addition of Al element can change the solubility of other alloy elements,
such as Ti, Co and Cr. This is why there was a higher content of alloy
elements in the diffusion layer (Fig. 7). The alloy elements may cause
the solid solution strengthening effect in the diffusion layer, which ef-
fectively improves the mechanical properties of nickel-based alloys. The
surface microstructure change, especially the increase of γ′ phase and
element distribution changes (mainly the increase of alloy elements)
are the main reasons for fatigue strength improvement after the alu-
minizing treatment.
For the LSP + aluminizing samples, the improvement mechanism is
similar with that of aluminizing, but it has some special features.
Firstly, the SEM observations show that the microstructure in the dif-
fusion layer changes from a random distribution in the original alu-
minizing samples (Fig. 7b) to an orderly distribution, with an acicular
structure distribution, in the LSP + aluminizing sample (Fig. 7d). Sec-
ondly, the LSP-induced surface nanostructure and high-density defects
can provide more diffusion channels and nucleation locations, leading
to the formation of higher amounts of β-phase and γ′ strengthening
phase and to a thicker diffusion layer (Fig. 6). Thirdly, Xu et al. [43]
showed that the compressive residual stress could change the diffusion
coefficient of alloy elements. The existence of residual stress resulted in
more alloy elements diffusing into the surface aluminide layer of
LSP + aluminizing sample (Fig. 7). The increase of alloy elements can
increase the content of solid solution strengthening phase. Moreover,
the larger amount grain boundaries produced by LSP are beneficial for
the diffusion of alloy elements (Zr, Ti, Cr, Mn) into the γ′ strengthening
phase, which act as pinning effects and improve the bonding strength of
diffusion layers. The microstructural changes induced by aluminizing is
one main reason for the fatigue strength improvement.
It is worth noting that the surface nanostructure and high-density
dislocations induced by LSP had good thermal stability, which has a
positive role for the fatigue strength. The effect of grain size and dis-
locations on fatigue strength can be expressed by Hall-Petch equation
[44]:
σ = σ0 + kd−1/2 + αGbρ1/2 (1)
where σ0 is the original strength of the material, k is the Hall–Petch
constant, and d is the grain size, α is a constant, G is the shear modulus,
b is the Burgers vector and ρ is the dislocation density. Thus, the
thermal stability of surface nanostructure and high density dislocations
at the surface resulted in the high strength for the LSP + aluminizing
samples. The high strength created a barrier and restricted the dis-
locations movement during the fatigue load, which resulted in the
much higher required cycles to crack initiation. All in all, the fatigue
strength improvement of LSP + aluminizing samples is due to the in-
crease of Al content and the decrease of grain size induced by the two
treatments of LSP and aluminizing.
4. Conclusions
In this study, the high temperature gas aluminizing process on the
K417 nickel-based alloy, with a surface nanostructure layer produced
by means of LSP, was investigated. The influence of the LSP treatment
on the aluminizing process was examined by comparing and assessing
the microstructural characteristics and fatigue strength of specimens
that had been pre-treated by LSP and specimens that have not been pre-
treated. The main conclusions are summarized as follows:
(1) A nanocrystalline layer was produced in the K417 nickel-based
alloy by means of LSP. The grain sizes at the top of surface were in
the range 30–150 nm. Beneath the nanostructure layer, dislocation
35
Surface & Coatings Technology 342 (2018) 29–36
cells and high-density dislocations were generated.
(2) SEM micrographs and related EDS results indicated that three layers
existed in both samples after the aluminizing process. The outer
layer was consisted by δ-Ni2Al3 and Al-rich β-NiAl phase; the
middle layer consisted of β-NiAl and alloy elements, and the inner
layer consisted of γ′-Ni3Al.
(3) The fatigue tests showed that the aluminizing treatment could im-
prove the fatigue strength of the K417 nickel-based alloy from
110 MPa to 226 MPa. The improvement is mainly attributed to the
changes in microstructure and element distribution in the surface
layer. The fatigue strength of the LSP + aluminizing samples in-
creased to 335 MPa, which is higher than that of the original alu-
minizing samples, the reason is the combined effect of LSP and
aluminizing.
Author contributions
W.F. He and Y.H. Li designed the project. W.F. He, S.H. Luo, L.C.
Zhou and X.F. Nie performed the microstructure observation and fa-
tigue experiments and supervised S.H. Luo and W.F. He analyzing the
data and presenting the results. S.H. Luo, W.F. He and Y.H. Li wrote the
paper. All authors contributed to discussions of the results.
Acknowledgements
The authors are indebted to the Center for Advancing Materials
Performance from the Nanoscale, State Key Laboratory for Mechanical
Behavior of Materials, Xi'an Jiaotong University for the cooperation in
the TEM observations. This work was supported by the National Key R&
D Program of China (grant numbers 2016YFB1102600), National Basic
Research Program of China (grant numbers 2015CB057400) and
National Natural Science Foundation of China (grant numbers
51405507).
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