Journal of Alloys and Compounds 882 (2021) 160701

Contents lists available at ScienceDirect

Journal of Alloys and Compounds

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

In-situ warm shot peening on Ti-6Al-4V alloy: Effects of temperature on

fatigue life, residual stress, microstructure and mechanical properties ]]
]]]]]]
]]

⁎
Su Hui Lim a,b, Zheng Zhang a, , Debbie Hwee Leng Seng a, Ming Lin a, Siew Lang Teo a,
Fengxia Wei a, Augustine Kok Heng Cheong a, Shijie Wang a, Jisheng Pan a
a
Institute of Materials Research and Engineering, A⁎STAR (Agency for Science, Technology and Research), #08-03, 2 Fusionopolis Way, Innovis 138634, Singapore
b
Singapore Institute of Food and Biotechnology Innovation, A⁎STAR (Agency for Science, Technology and Research), #01-02, 31 Biopolis Way, Nanos 138669,
Singapore

a r t i cl e i nfo a bstr ac t

Article history: Shot peening (SP) is a matured surface enhancement technique to improve fatigue strength and fatigue lives
Received 10 April 2021 of cyclically loaded metallic components at room temperature. In order to achieve enhanced beneficial
Received in revised form 17 May 2021 effects beyond SP’s conventional performance, SP has been attempted at elevated temperatures or under
Accepted 2 June 2021
tensile stress loading on spring steel with some success. In this work, SP on α/β Ti-6Al-4V alloys has been
Available online 5 June 2021
carried out when they were heated at elevated temperatures up to 400 °C. The effects of such in-situ warm
SP on fatigue life of Ti-6Al-4V at different temperatures have been evaluated and correlated with respective
Keywords:
Warm shot peening development in compressive residual stress distribution, microstructure and hardness. The optimum in-situ
Ti-6Al-4V warm SP condition was achieved at 100 °C after a trade-off between compressive residual stress relaxation
Thermal softening and enhanced grain refinement, both of which are affected by thermal softening but to different degrees.
EBSD © 2021 Elsevier B.V. All rights reserved.
Stress relaxation
Grain refinement
Crystallographic orientation mapping

1. Introduction technique, which has been widely used in many industries including
automobile, aerospace, biomedical and many more. SP is a cold
Enhancing fatigue strength can extend the service lives of cycli­ working process, where shots made of metal, glass or ceramic ma­
cally loaded components (such as springs, suspension coils, crank­ terials strike metallic components’ surface and act as small peening
shafts, gears, gun barrels, turbine blades) and thus have considerable hammers to induce permanent plastic deformation, which leads to
economic impacts. A wide range of methods have been adopted to work-hardening and CRS on the peened surfaces. Surface CRS is
improve fatigue strengths and fatigue lives of these components, balanced by tensile stress in the interior. Besides improving fatigue
such as optimizing geometric design, using stronger materials, per­ resistance, CRS can also offer some degree of stress corrosion re­
forming surface enhancement treatment, etc. Surface enhancement sistance to the Mg components [9].
treatment can improve fatigue life significantly by introducing The potential increase in the fatigue strength for a given material
compressive residual stress (CRS) in the surface layers of metallic by using conventional SP treatments is limited to a depth between
components without increasing their dimension or demanding 150 and 250 µm under a set of the optimized key process parameters
stronger materials. CRS can inhibit surface micro-cracks from nu­ including shot media, compressed air pressure, shot peening dis­
cleation and propagation into the bulk of the components, reducing tance, coverage, etc. Therefore, if greater beneficial results are de­
the probability of pre-matured component failure. Various surface sired from SP instead of investing on new equipment like laser shot
treatment techniques including shot peening [1–3], autofrettage [4], peening, it is necessary to modify the conventional SP process. The
deep cold rolling / burnishing [5–7], laser shot peening [5], waterjet first possible modification is to preload the component with tensile
peening [8], etc, have been developed over the years. Among them, stress while shot peening, which induces higher compressive re­
shot peening (SP) is by far the most common and the least costly sidual stresses in longitudinal direction close to the surface. Such
practice is termed stress shot peening (SSP) and has already been
adopted in the spring industry for many years [10,11].
The second plausible method is to carry out the SP process at
⁎
Corresponding author.
elevated temperatures, and is termed as warm shot peening (WSP).
E-mail address: [email protected] (Z. Zhang).

https://doi.org/10.1016/j.jallcom.2021.160701
0925-8388/© 2021 Elsevier B.V. All rights reserved.
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

Fig. 1. (a) Image of an as-received rectangular Ti-6Al-4V block (top) and a flat dog-bone Ti-6Al-4V coupon (bottom) used in this work; (b) Geometry of the dog-bone Ti-6Al-4V
coupon.

It was initially proposed for spring steel due to their remarkably high [2,3,28]. The CRS peaked around − 749 ~ − 845 MPa. Such CRS in­
yield strength, which requires very large impact velocity to initiate creased the fatigue life of Ti64 materials [2,3] significantly by frag­
plastic deformation. Shots are frequently fractured after peening menting surface grains [28] and moving the fatigue cracks initiation
spring steel and WSP is thus designed to reduce the flow stress of point from surface in pristine specimens to sub-surface in peened
spring steel [12,13]. Indeed, it has been demonstrated that WSP has specimens [3].
introduced higher and deeper CRS in SUP9 (Mn-Cr) spring steel up to Recently, a thermo-mechanical coupled finite element modeling
300 °C [14]. Further increasing the shot peening temperature to (FEM) has predicted a slightly deeper CRS if Ti64 was WSP at a
400 °C led to CRS relaxation [14]. In addition to higher magnitude of thermal flux of 3.0 × 106 W/m2, which raised the surface tempera­
CRS, WSP on AISI 4140 steel at 310~330 °C also led to a much stable ture to 218 °C [29]. Surface CRS would relax if the thermal flux was
CRS during quasi-static and cyclic loading, incurring only minimal further increased to 6.0 × 106 W/m2, which raised the surface tem­
CRS relaxation after the cyclic loading [10,15,16]. Inspired by the perature to 417 °C [29]. Despite their technological importance and
prominent beneficial effects on spring steel, others materials such as wide applications, to the best of our knowledge, there have been no
Mg alloys [9,17], SiCw/Al composites [18], TiB2/Al composite [19], etc, actual experimental studies of WSP on Ti64 alloys yet, which could
have also been attempted with WSP to expand its application areas. possibly produce similar beneficial effect as spring steel [10,14–16].
The third possible modification is to combine various SP Therefore, a customized heating stage has been designed in this
methods, such as double shot peening (DSP) [11,20], warm stress work in order to carry out in-situ WSP studies of Ti64 up to 400 °C in
shot peening (WSSP), warm stress double shot peening (WSDSP) a commercial SP booth. The resultant fatigue life performance has
[11], etc. DSP is to peen the component surface using a smaller shot been correlated with development in CRS distribution, micro­
at a lower intensity after the initial conventional SP treatment. Si­ structure and mechanical properties after such WSP treatment, in
milar to micro-shot peening (MSP) which uses shots with much order to determine the optimum in-situ WSP condition for Ti64 alloy.
smaller size (0.1 mm in diameter compared to the conventional shot
with 0.3 mm in diameter), both DSP and MSP aim to reduce surface 2. Experimental methods
roughness caused by the crater edges or known as notch effect [21].
DSP also targets to induce work-hardening at deeper layers [11,20]. 2.1. Materials
WSSP and WSDSP are an effective combination of the different de­
rivatives of SP methods mentioned above while peening the com­ Two geometries of commercial-grade α/β Ti-6Al-4V (Ti64) have
ponents at elevated temperatures [11]. Among these three possible been used in the current work (Fig. 1(a)). The top rectangular coupon
modifications, WSP outperforms SSP as it can be applied to com­ had a dimension of 50 (length) × 30 (width) × 10 (thickness) mm3,
ponents with irregular or asymmetry geometries, where a uniform while bottom flat dog-bone had a dimension of 124.3 (length) × 19.0
stress over the targeted area is very difficult to achieve. (width) × 2.5 (thickness) mm3. The dog-bone shape coupon's de­
Although several derivatives from conventional SP has been de­ tailed dimension can be found in Fig. 1(b). Both types of coupons
veloped, the target material so far has been predominately spring were ground to have arithmetic roughness (Ra) below 0.3 µm. No
steel. Ti-6Al-4V or Ti64 alloy is another important metal alloy, which heat treatment was performed on the as-received Ti64 prior to the
has considerable technological and commercial values due to its shot peening (SP).
wide range of applications in automotive [22], aerospace [23,24] and
medical [25,26] industries thanks to its high strength-to-weight 2.2. In-situ warm shot peening (WSP) setup
ratio, excellent corrosion resistance and compatibility with compo­
site structure. Room temperature SP has also been routinely per­ There were several designs in the literature to modify either the
formed on Ti64 components subjected to periodic loading such as SP gun [29] or the entire SP booth [10,14–18] in order to carry out in-
springs, axles, shafting, aircraft landing gears since 1970s [27] to situ stress and/or warm shot peening. As the current study is only a
increase their fatigue strengths and resistance to stress-corrosion preliminary feasibility study, an in-situ heating setup based on
cracking. However, the impact of SP on the Ti64 alloys’ fatigue life hotplate is proposed (Fig. 2). A protective cover was designed to
have been very sparely investigated [1,2,5,28]. It has been reported contain the entire hotplate (Fig. 2(a)) in order to mitigate the col­
that SP at 6~8 A intensity with 100~125% coverage can produce lateral peening by the shot balls on the Matcor MS7-H550-Pro pre­
190~200 µm thick layers with CRS beneath the α/β Ti64 alloy surface cision hotplate, which can heat up to 550 °C. Two adaptors were

2
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

Fig. 2. Pictures of (a) hotplate (right) and its protective cover (left), and back-side of adapters to hold the (b) rectangular block and (c) the flat dog-bone Ti64 coupon. (d) The
complete setup for shot peening dog-bone coupon.

designed for fixing both rectangular coupons (Fig. 2(b)) and flat dog- corresponding load (F0.2) after offsetting 0.2% strain of as-received
bone shape coupons (Fig. 2(c)) onto the hotplate during shot pe­ Ti64 were determined to be 823.3 MPa and 14.801 KN from the
ening. Care must be taken to hold the samples firmly during the previous tensile test [28]. The HCF tests were subsequently carried
forceful impact of the shot metals introduced by the compressed air out on a MTS Bionix 370 servohydraulic HCF system at three sinu­
at a pressure of 35 psi. The adaptors were specially designed in order soidal loadings equal to 0.9, 0.7 and 0.5 times of F0.2 at a frequency of
to minimize the heat dissipated from hotplate to the surrounding 20 Hz and a load ratio (R, minimum load/maximum load) of 0.1 at
protective cover through the Ti64 samples. Without minimizing room temperature. Each condition was repeated on at least three
contact area, the Ti64 samples can only reach up to 80 °C, even coupons for consistency.
though the hotplate was heated up to 550 °C. Thanks to the two The rectangular blocks (Fig. 1) were used for the other analysis
adaptors, the same protective cover can be used to accommodate including average surface roughness (Ra) via KLA Tencor P-10 surface
both types of Ti64 samples (Fig. 2(d)) and can be placed inside the profilometer, surface residual stress by Stresstech Xstress G3 X-ray
commercial shot-peening booth. The actual temperature on the stress measurement and its depth profile via center hole drilling
sample surface was measured by a thermocouple and was mon­ (CHD) method, etc. The hardness and young’s modulus of the Ti64
itored to be stable for 5 min before the routine SP process was car­ coupons were investigated using a nano-indentation system (Agilent
ried out in this SP booth manufactured by Clemco Industries Corp, G200 Nanoindenter XP). A Berkovich diamond tip was positioned
which has been described in [28]. over cross-sectional Ti64 coupons with indentation down to
High hardness cast steel shots with average diameter of 0.34 mm 1000 nm. Each line scan has the first indentation point at 20~35 µm
were peened at a pressure of 35 psi from a duckbill nozzle 4″ ver­ away from the surface. The subsequent 4 indentation points were
tically above the Ti64 coupon surface. 7 strokes were swiped across 30 µm apart and the next 10 points were 100 µm apart.
the coupon surface at a speed of 60 in./min in order to reach a target Coupon’s crystallinity was examined using Bruker D8 Advance X-
intensity between 6 and 9 A and a coverage of 125%. At least 3 pieces ray diffraction (XRD) with Cu Kα X-ray (λ = 1.54 Å) at a voltage of
of type A Almen strip were used to verify that the intensity was 40 kV and a current of 40 mA. Phase quantification was performed
stabilized prior to actual peening. Only one side of the rectangle via Rietveld phase analysis using TOPAS v5 software and deploying
coupon was peened at the targeted temperatures from 100 to 400 °C. full axial model and fundamental parameters approach. JEOL 7600F
For dog-bone samples, the adaptor was loosened after the first side field emission scanning electron microscope (FE-SEM) equipped
was peened so that the sample can be flipped upside down manually with X-Max 50 energy dispersive spectroscopy (EDS) detector and
to peen the other side's surface. Oxford Instrument NordlysNano electron backscattering diffraction
(EBSD) detector was used for microstructural characterization. EDS
2.3. Characterization was performed to determine the elemental composition, while EBSD
was carried out to reveal the grain orientations from cross-section
The details of various equipment employed to characterize the surface of the coupon and to analyze the deformation depth from
Ti64 coupons were reported in our earlier publication [28]. In a shot peening surface. The EBSD measurement was acquired with
nutshell, flat dog-bone Ti64 samples (Fig. 1) were meant for tensile 20 kV electron accelerating voltage and a scan step size of 1 µm. Ti
test and high cycle fatigue (HCF) test. The yield stress (σ0.2) and the hexagonal close packed (HCP) and body centered cubic (BCC) phases

3
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

were selected for indexing the EBSD patterns of the α- and β- the higher temperature, respectively. However, the TiO2 layer after
phase Ti. in-situ WSP at 300 °C can be completely removed from surface after
FEI Helios Nanolab 450 S dual beam focused ion beam (FIB) 8 min of Ar+ ion sputtering within X-ray photoelectron spectro­
system was used to prepare cross-sectional Ti64 samples for trans­ scopy’s chamber (Fig. S1). Hence, it indicates that the TiO2 layer
mission electron microscopy (TEM) characterization, which was formed on the surface after in-situ WSP was quite thin (less than
performed using FEI Titan 80–300 TEM system operating at 200 kV. 22 nm) and it was likely to be amorphous given the low formation
TEM phase and crystallographic orientation mapping was carried temperature (≤ 400 °C). Hence, it was unlikely to affect the Ti64′s
out using JEOL-2100 TEM. It was operated at 200 kV and had a fatigue and mechanical properties significantly.
double tilt low-background TEM holder, an Oxford EDS detector, a Surface profiler measurement also detected a consistent increase
DigiSTAR Precession electron diffraction (PED) system and in both craters’ average depth (H) and diameter (D) over the tem­
Nanomegas ASTAR™ phase and orientation mapping system. The perature (Table 1), which led to an increase in the ratio of H/D. The
crystallographic orientation mapping was obtained through scan­ stress concentration factor (Kps7) under a single direction stress field
ning the area of interest at Nano-beam diffraction mode with step can be estimated using the following equations from [30]:
size of 10 nm and actual beam size of ~6 nm using a 10 µm size
H
condensed aperture. The electron diffraction patterns were indexed Kps7 = 1 + 2.1 × (for H/D 0.30)
D (1)
by comparison with standard α-Ti (space group of P63/mmc with
a = 2.925, c = 4.667 Å) and β-Ti (space group of Im-3m with H 1.3
a = 3.211 Å) crystal structures. The final process maps in both EBSD Kps7 = 1 + 4.0 × (for H/D < 0.15)
D (2)
and TEM were analyzed using HKL Channel 5 (Oxford Instruments)
software. As our H/D is less than 0.15, Eq. (2) is used to calculate Kps7 , which
can be seen to increase slightly (about 4.7%) from 1.057 after shot
3. Results peening at room temperature to 1.107 after shot peening at 300 °C
(Table 1). Clearly, the small increases in the stress concentration
3.1. Surface morphology, roughness and composition factor was attributed to deeper and larger craters at higher in-situ
WSP temperature. By contrast, Kps7 increased up to 55.6% when shot
Ti64 rectangular coupons were in-situ warm shot peened (WSP) diameter increased from 0.3 to 1.4 mm or when shot velocity in­
at 100, 200, 300 and 400 °C. They are shown in Fig. 3 together with creased from 40 to 100 m/s (Fig. 23 in [31]). Ridges between craters
the as-received Ti64 and after shot peening at room temperature. are known to serve as the preferential crack initiation points, the so-
There was clear discoloration after in-situ WSP at 400 °C due to the called notch effect [21]. Nevertheless, no vibro-polishing was per­
severe oxidation in air. Therefore, the subsequent maximum in-situ formed on these samples, as vibro-polishing can modify the micro­
WSP temperature was kept at 300 °C to avoid undesired excessive structure and decrease the thickness of layer with compressive
surface oxidation, and the characterization of samples after in-situ residual stress (CRS) while reducing the surface roughness [2]. In
WSP at 400 °C were not included. addition, the increase in stress concentration factor by the surface
The SEM images of Ti64 surfaces after in-situ WSP were shown in roughness was minor in the current case (Table 1), as CRS is reported
Fig. 4, with the surface morphology of the as-received Ti64 coupon to exercise a leading role than surface roughness in the modification
shown as inset in Fig. 4(a). After shot peening from room tempera­ of fatigue properties [32].
ture up to 300 °C, the initial flat surface has been changed into
dented surfaces with numerous craters from the impacting shots. 3.2. High cycle fatigue life
Upon inspection under surface profiler, there was a monotonic in­
crease of arithmetical roughness (Ra) values with the heating tem­ High cycle fatigue test is a gatekeeper in determining the effec­
perature from 1.34 µm after shot peening at room temperature to tiveness of such WSP. Upon determining the load corresponding to
2.93 µm after WSP at 300 °C. The higher roughness is attributed to as-received Ti64′s yield strength after offsetting 0.2% strain (F0.2,
the reduced flow stress and hence larger degree of plastic de­ 14.801 KN) in our earlier work [28], three loads equal to 0.9, 0.7 and
formation as the Ti64 coupons were heated up to a higher tem­ 0.5 times of F0.2 were chosen as the high, medium and low loads to
perature. The as-received Ti64 coupon had Ti, Al, V, O, C, Fe and Si evaluate the fatigue life of the Ti64 dog-bone coupons after different
elements in weight percentage (wt%) as measured by EDS of 82.4, in-situ WSP temperatures. At least three dog-bone samples were
5.2, 3.5, 7.1, 1.6, 0.1 and 0.1, respectively [28]. After WSP, these ele­ tested for each condition with each point in the stress-life (SN)
ments were still present (Fig. 4(f)), except that both O wt% and Fe wt curves representing one sample. The vertical axis represents stress
% increased from 7.1 to 0.1 on the as-received surface to 24.1 and 8.4 amplitude (Δσa, in MPa), which is defined as half of the difference
after in-situ WSP at 300 °C. The increases in O wt% and Fe wt% were between maximum stress (σmax) and minimum stress (σmin) during
× (1 R)
attributed to heavier oxidation at the surface and higher diffusivity loading (Δσa= max 2 min = max 2 ). R is the load ratio (0.1 in cur­
of Fe from the high hardness cast steel shots into the Ti64 surfaces at rent study). The horizontal axis is the number of cycles to failure

Fig. 3. Picture of six pairs of Ti64 rectangular blocks before and after in-situ warm-shot-peening (WSP) from room temperature (32 °C) up to 400 °C. At each condition, two
coupons were shot peened to ensure repeatability.

4
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

Fig. 4. SEM images of Ti64 after shot peening at (a) 32, (b) 100, (c) 200, (d) 300 °C. The inset on the top right corner in (a) shows the as-received Ti64′s surface prior to SP. (e)
Average surface roughness and (f) surface composition in weight percentage after warm shot peening from room temperature up to 300 °C.

Table 1
Average crater depth (H) and diameter (D) on Ti64 surfaces after shot peening at different temperatures.

Shot peening Crater depth Crater diameter H/D Kps7

temperature (°C) (H, µm) (D, µm)

32 3.260 ± 1.460 85.927 ± 25.918 0.038 1.057

100 4.766 ± 2.986 92.042 ± 23.477 0.052 1.085
200 6.225 ± 2.744 116.614 ± 27.932 0.053 1.089
300 8.302 ± 3.328 134.522 ± 35.399 0.062 1.107

(Nf). The Nf of all Ti64 coupons increased as the load decreased beneficial and generally led to shorter Nf. At medium load of 0.7 F0.2,
(Fig. 5), while the as-received Ti64 dog-bone samples showed the in-situ WSP at 100 °C had a noticeable higher Nf than that SP at room
lowest Nf at all the three loads. After shot peening at room tem­ temperature while in-situ WSP at 200 °C and 300 °C had slightly
perature, the Nf at all three loads increased (represented by red lower Nf values. However, at low load of 0.5 F0.2, in-situ WSP at
circles) compared to those without shot peening (represented by 100 °C resulted in run-outs (beyond 106 cycles) for all three samples,
black squares), which is expected as shot peening is well known to while in-situ WSP at 200 and 300 °C had generally comparable re­
extend the Nf of components under cyclic loadings [2,33]. sults with that SP at room temperature. There was one run-out case
Compared with the Nf after SP at high load of 0.9 F0.2 (13.321 KN) for in-situ WSP at 200 °C. As the Nf from all samples were more than
at room temperature, in-situ WSP at 100, 200 and 300 °C were not 104 cycles, the current fatigue failure is high cycle failure and hence

5
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

Fig. 5. The stress-life (SN) curves from as-received dog-bone shaped Ti64 coupons (black squares) and after shot peening at 32, 100, 200 and 300 °C at three loads of 13.321, 10.361
and 7.401 KN. Each symbol presents one sample. Basquin’ equation was used to fit SN curves in log-log scale and the fitting results were shown at the bottom of the figure.

Basquin’s power law equation (Eq. (3), [34,35]) can be employed in 3.3. Depth profile of compressive residual stress (CRS) and hardness
its log scale format (Eq. (4)) in order to fit the stress-life curve in log-
log scale: Firstly, the Ti64 coupons’ crystalline phases after in-situ WSP
were examined under XRD. As shown in Fig. 6, the as-received Ti64
= × Nf b
a f (3) was comprised of strong patterns from Ti17Al3 (blue ticks, α-Ti
phase) and weak patterns from Ti0.7V0.3 (green ticks, β-Ti phase).
After shot peening from room temperature up to 300 °C, there was
log ( a) = log ( f) b × log (Nf ) (4) no obvious change in the XRD patterns, suggesting an intact crys­
tallinity of the Ti64 and hence absence of possible phase transfor­
where σ'f is the fatigue strength coefficient and b is the fatigue
mation despite the high temperature WSP treatment. Nevertheless,
strength exponent. The fitting results are shown at the bottom of
Rietveld phase analysis shows that the weight percentage of the α-Ti
Fig. 5, where b is the absolute value of the slope. Fatigue strength
phase inside the coupon has consistently increased from 74.9 wt% in
exponent (b) is reported to increase with decreasing hardness and
as-received coupon up to 87.1 wt% after WSP at 300 °C, accom­
inclusion size [35] and is also related to the cyclic hardening [34]. SP
panying with a concurrent decrease in β-Ti phase (Table 2). No TiO2
reduces the grain size in the surface layer, but it does not change the
phase was detected by XRD due to its small thickness (< 22 nm) and
inclusion size significantly. Hence, the inclusion size can be taken as
likely amorphous structure.
constant in the current case. The change of b will reflect the change
Residual stress is a key property in determining the fatigue
of hardness, and the fitting results table in Fig. 5 suggests a max­
performance after various surface enhancement treatment. Upon
imum hardness after in-situ WSP at 100 °C, which decreases with an
confirming that coupon’s dominant phase after in-situ WSP up to
increase in in-situ WSP temperature.
300 °C was still α-Ti phase, X-ray stress measurement was carried
High cycle fatigue tests show beneficial results for Ti64′s fatigue
out to detect the shift of α-phase Ti (213) plane at 2θ of 141.7 ° in
life after in-situ WSP at 100 °C at medium and low loads (Fig. 5),
order to determine the surface residual stress on both rectangle
while in-situ WSP at higher temperature of 200 and 300 °C did not
(Fig. 7(a)) and dog-bone Ti64 coupons (Fig. 7(b)). The as-received
introduce additional benefits despite a higher cost of thermal
Ti64 rectangular coupon had already a CRS of − 148.0 MPa (Fig. 7(a)),
budget. The trend is similar to an optimum in-situ WSP for steel
arising from the grinding process [28]. Upon shot peening at room
between 200 and 300 °C, with a further increase in WSP temperature
temperature, the CRS increased substantially to − 775.0 MPa. When
to 400 °C deteriorating the fatigue performance [14,16]. The me­
the rectangular coupons were in-situ warm shot peened at 100 °C,
chanism in extending the fatigue life of steel by WSP are usually
the surface CRS decreased slightly to − 746.3 MPa, indicating occur­
attributed to the creation of deeper or larger compressive residual
rence of stress relaxation at 100 °C. Such stress relaxation was more
stress (CRS) region in the components [12,14,19], while deterioration
pronounced when the in-situ WSP temperatures increased to 200
above this optimum WSP temperature was attributed to CRS re­
and 300 °C, where the surface CRS further decreased monotonically
laxation at higher temperature [14,16]. To understand the micro­
to − 661.0 and − 556.4 MPa, respectively.
scopic mechanism behind the additional beneficial effect after in-
Two sides of several dog-bone coupons after in-situ WSP at 100,
situ WSP at 100 °C, Ti64 coupons after WSP at different temperatures
200 and 300 °C were also examined under X-ray stress measurement
were subjected to a series of characterization as described in the
(Fig. 7(b)). The side which was WSP first was plotted in the left half
following sessions.
panel, while the other side peened later was plotted in the right half

6
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

α(0002)
α(1011)

α(1010)

α(1012)

α(1013)
α(1120)
WSP@300oC

Intensity (arb. unit)

WSP@200oC

WSP@100oC

β(110) SP @ 32oC

β(211)
β(200)
No SP

40 50 60 70 80 90
2θ (o)
Fig. 6. XRD patterns from the as-received Ti64 (bottom) and Ti64 after shot peening at 32, 100, 200 and 300 °C. They are scaled to have the same height for easy comparison.

Table 2
Rietveld phase analysis result of the Ti64 coupons’ XRD patterns after WSP.

Samples α-Ti (P63/mmc) β-Ti (Im-3 m) Goodness of

fit (GOF)
a (Å) c (Å) Composition (wt%) a (Å) Composition (wt%)

As-received 2.93191 ± 0.00019 4.67026 ± 0.00031 74.95 ± 0.17 3.20919 ± 0.00047 25.05 ± 0.17 1.64
SP @32 °C 2.93973 ± 0.00022 4.67788 ± 0.00037 82.83 ± 0.95 3.22669 ± 0.00051 17.17 ± 0.95 1.26
WSP @100 °C 2.94103 ± 0.00024 4.67929 ± 0.00039 84.76 ± 0.78 3.22878 ± 0.00050 15.24 ± 0.78 1.23
WSP@200 °C 2.93893 ± 0.00021 4.67614 ± 0.00034 85.75 ± 0.82 3.22743 ± 0.00042 14.25 ± 0.82 1.24
WSP@300 °C 2.93753 ± 0.00020 4.67472 ± 0.00033 87.08 ± 0.72 3.22522 ± 0.00040 12.92 ± 0.79 1.27

panel. A decrease in the magnitude of the CRS with an increase in significantly lower than the corresponding CRS after SP at room
WSP temperature can be seen clearly in Fig. 7(b), with average value temperature, although their CRS from 112 to 352 µm were margin­
at each temperature close to the value detected on rectangular ally larger than that after SP at room temperature. In-situ WSP led to
coupons in Fig. 7(a). More importantly, the two sides showed com­ a shift of maximum CRS to a deeper depth, while the decreasing
parable CRS values at each in-situ WSP temperature, suggesting trend in CRS with WSP temperature measured by center hole drilling
absence of stress relaxation on the first side when it was pressed agrees well with that observed by X-ray stress measurement in
against the hotplate when the other side underwent the WSP pro­ Fig. 7(a & b). Such a decrease in WSP temperature agrees with the
cess. Hence, Fig. 7(b) demonstrates that the current WSP setup in FEM calculation about relaxation in CRS below when the Ti64 sur­
Fig. 2 can produce reliable and consistent results despite different face temperature was increased from 119.2 to 218.4 and 416.9 °C,
geometries of samples. especially at 100 µm deep below the surface [29].
The rectangular coupons were also subjected to center hole Shot peening (SP) is a cold working process, which introduces
drilling test in order to find out the residual stress distribution along CRS and work hardens the surface layers at the same time. Fig. 7
depth in both longitudinal and transverse directions represented by shows that in-situ WSP did induce CRS at the surface layer and hence
σ1 (Fig. 7(c)) and σ3 (Fig. 7(d)), respectively. The overall residual it likely work-hardened the surface layer as well. As a result, nano-
stress distribution along these two directions were similar, in­ indentation in line scan pattern was set up (Fig. 8(a)) to probe the
dicating the isotropic nature of the shot peening treatment. There­ hardness and Young’s modulus along the depth of the rectangular
fore, the residual stress profile along the longitudinal direction (σ1) blocks subjected to SP at different temperatures. The resulting
will be used as an example for discussion. For the as-received Ti64 hardness and Young’s modulus in Fig. 8(b & c) were divided into two
coupons, the maximum CRS is − 130.6 MPa at the first point near regions: near surface region (≤ 500 µm) and bulk region (≥ 600 µm).
top-surface region at a depth of 8 µm. It gradually reduced to zero at The as-received Ti64 coupons had a near-surface hardness of 4.2 GPa
a depth of 144 µm. For the coupon shot peened at room temperature, and Young’s modulus of 125.3 GPa. They were lower than the aver­
the CRS increased from − 774.0 MPa near-surface to a maximum aged values from the bulk at the depth between 600 and 1200 µm
value of − 877.7 MPa around 24 µm deep, before the CRS gradually (4.8 GPa and 135.6 GPa, respectively), which were close to the values
decreased to nearly zero at 208 µm deep. For Ti64 coupons warm directly measured from the top surface (4.7 GPa for hardness and
shot peened at 100 °C, there was a reduction in CRS from − 774.0 MPa 132.1 GPa for Young’s modulus, represented by the 2 dash lines). The
at surface to a maximum CRS of − 807.1 MPa at 72 µm deep. However, similar hardness and Young’s modulus in these two orthogonal di­
from a depth of 56 µm onwards, WSP at 100 °C had a larger CRS rections shows close mechanical strength of Ti64 coupons in these
compared to that SP at room temperature, and its CRS decreased to two perpendicular directions. Upon shot peening at room tem­
zero at a much deeper depth of 352 µm. WSP at 200 and 300 °C perature, near-surface hardness and Young’s modulus increased
further decreased the surface CRS to − 659.5 MPa and − 497.3 MPa at slightly to 4.5 and 127.3 GPa, respectively, which suggests presence
8 µm depth, respectively. Their CRS between 8 and 88 µm was of surface hardening caused by the shot peening process.

7
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

(a) -100 (b) -400

300oC
-148.0
-200 -450 200oC
1st Side
100oC

Residual Stress, σ (MPa)

-300
Residual stress (MPa)

In-situ heating + Shot-peening -500 2nd Side

-400
-550
-500
-600
-556.4
-600
-650
-661.0
-700
-700
-746.3
-800 -775.0
-750
-900
0 50 100 150 200 250 300 350 0 4 8 12 16 20 24 28 32
Temperature (oC) Samples

Longitudinal Direction (σ1) Transverse Direction (σ3)

(c) 100 (d) 100
0 0
-100 -100
Residulal Stress (MPa)

Residulal Stress (MPa)

-200 No SP -200 No SP
-300 SP @ 32oC -300 SP @ 32oC
WSP @ 100oC WSP @ 100oC
-400 -400
WSP @ 200oC WSP @ 200oC
-500 -500
WSP @ 300oC WSP @ 300oC
-600 -600
-700 -700
-800 -800
-900 -900
0 100 200 300 400 500 600 700 800 9001000 0 100 200 300 400 500 600 700 800 9001000
Depth (μm) Depth (μm)

Fig. 7. Residual stress on (a) the Ti64 rectangular coupons and (b) dog-bone coupons measured by X-ray stress measurement before and after shot peening treatment. Each point
in (b) represents one sample with the results from first side plotted on the left panel, while the results from second side plotted on the right panel. Residual stress depth profile
below the surface as probed by center hole drilling for Ti64 after warm-shot-peening from 32 up to 300 °C in (c) longitudinal (σ1) and (d) transverse (σ3) directions.

After in-situ WSP at 100 °C, the coupons showed consistently suggest that WSP is still a surface enhancement treatment, with
higher hardness and Young’s modulus values (blue lines in Fig. 8(b effect limited to the top 500 µm.
and c)) at the near-surface region from 37 to 500 µm compared to
those in the bulk region from 600 to 1200 µm. Moreover, the hard­ 3.4. Fractography and microstructural development in top surface
ness and Young’s modulus at near-surface region (37~500 µm) was region after in-situ WSP
also much higher than the values after SP at room temperature.
Although an increase in in-situ WSP temperature to 200 and 300 °C The cross-section of the current dog-bone samples was rectangle
did not lead to such a dramatic increase in the hardness and Young’s (7.00 × 2.50 mm2) and not in circular shape. Hence, the samples were
modulus near the surface region, they were slightly higher than both not axial symmetry. Nevertheless, the fracture surface morphology
as-received and SP at room temperature. It can be seen that the from Ti64 dog-bone samples before and after shot peening at dif­
trend of hardness development measured by nano-indentation ferent temperatures were still examined under SEM (Fig. 9) in order
agrees nicely with a maximum hardness after in-situ WSP at 100 °C to have a glimpse about the fatigue fracture initiation point. The
as predicted by the fatigue strength component (b) after fitting of fracture morphology at medium load of 0.7 F0.2 was selected for
Fig. 5. While SP affects the hardness and Young’s modulus near discussion, as all samples had fatigue fracture at this loading and
surface region, it did not affect the bulk hardness and Young’s there was a large difference in the cycles to failure (Nf) at different
modulus after SP at different temperatures, which were always close temperatures. For the as-received Ti64, the fatigue initiation point
to the initial values of 4.8 and 135.6 GPa from the as-received was at the surface of the width of the rectangle (marked by the
sample. Hence, the stable bulk hardness and Young’s modulus dotted ellipse). The whole fracture surface showed smooth

8
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

(a) Point scan measured

at top surface Line scan measured
along cross-section from
near-surface to bulk

(b) Surface region (≤ 500μm) Bulk region (≥ 600μm) (c) 160 Surface region (≤ 500μm) Bulk region (≥ 600μm)
6.0
150

Young's modulus (GPa)

5.5
Hardness (GPa)

140
5.0

4.5 130

4.0 As-received coupon 120 As-received coupon

SP @ 32oC SP @ 32oC
3.5 WSP @ 100oC 110 WSP @ 100oC
WSP @ 200oC WSP @ 200oC
WSP @ 300oC WSP @ 300oC
3.0 100
0 200 400 600 800 1000 1200 0 200 400 600 800 1000 1200
Distance from surface (μm) Distance from surface (μm)

Fig. 8. (a) A schematic showing the indentation measurement from the top surface and the line scan profile along the cross-sectional sample with starting point at near surface to
the bulk. (b) Hardness and (c) Young’s modulus probed at the cross-section of the rectangular coupons from near-surface down to a depth around 1200 µm. The hardness and
Young’s modulus measured at as-received Ti64 coupon’s top surface (black arrow in (a)) are plotted as black dash lines in (b and c) as reference.

transgranular fracture (highlighted by dotted square box) and characteristics of transgranular fracture [36]. Upon shot peening at
faceted intergranular fractures (Fig. 9(a)). By using a higher 32 °C, the crack initiation point was moved to sub-surface, around
magnification, the typical fatigue striations which was next to the 109 µm beneath the surface (Fig. 9(c)), representing by the circled
ductile fracture can be seen clearly in Fig. 9(b), where river line “fish-eye” feature. This agrees with previous reports that shot
patterns represented as plateaus connected by shear ledges are peening pushes the crack initiation point from surface to sub-surface

Fig. 9. SEM images from the surfaces after fatigue fracture of (a and b) as-received Ti64 (σa = 266.4 MPa, Nf = 20,236) and Ti64 after shot peening at (c) room temperature (32 °C,
σa = 258.9 MPa, Nf = 36,007), (d) 100 °C (σa = 261.5 MPa, Nf = 50,694), (e) 200 °C (σa = 264.7 MPa, Nf = 21,588) and (f) 300 °C (σa = 261.9 MPa, Nf = 20,048). The white arrows represent
surfaces which have been shot peened.

9
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

Fig. 10. Forward scatter electron Images (FSD, 1st row), the band contrast (2nd row) and Kernel average misorientation (KAM, 3rd row) maps from respective areas labeled by
white boxes in 1st row for(a) as-received Ti64 and after shot peening at (b) 32, (c) 100, (d) 200 and (f) 300 °C. The insets in 2nd row are the inverse pole figures (IPF) from the same
areas where the band contrast maps were taken. The 4th row displays the overlaid KAM maps and respective FSD images. The scale bars in all the images represent 100 µm. Grain
boundaries are represented by black lines for band contrast and KAM maps.

[3,32]. When the shot peening temperature was further raised up to phase with random orientations. The red, green and blue colors in
100 and 200 °C, the fatigue crack initiation points were measured to IPF represent [0001], [1210] and [0110] directions perpendicular to
be 200 and 147 µm beneath the surfaces (Fig. 9(d & e)), respectively. analyzed surface, respectively. The Kernel average misorientation
After shot peening at 300 °C, fatigue crack initiation point surpris­ (KAM) map (3rd row) shows that the top of 17 µm in the as-received
ingly went back to the top surface (Fig. 9(f)). It then explained the Ti64 coupon had greater local misorientation values (marked in
close Nf values between the as-received Ti64 and after in-situ WSP at green, 1.5~2°, scale bar in the inset) compared to that in the bulk
300 °C in Fig. 5, since both of them had fatigue crack initiation points (represented in blue, 0°). From the overlaid KAM map and FSD image
at the surface. It is worth mentioned that the fatigue striations and (4th row in Fig. 10), it can be seen that some of the non-indexed
ductile fracture features described in Fig. 9(b) were similarly ob­ (black) region are located within the higher misorientated (green)
served on the fracture surfaces in Fig. 9(c–f). Fig. S2 in the regions. The non-indexed region was attributed to unsuccessful in­
Supplementary Information provides additional fractography images dexing in this region due to very fine grain size from grinding pro­
between the fatigue propagation and final fracture regions. In the cess as revealed in our earlier work [28].
fracture regions, voids, secondary cracks and faceted cleavages can After shot peening at room temperature, the thickness of non-
be seen clearly in column (ii) of Fig. S2. indexed black region increased significantly to 24 µm (4th row,
Although the fatigue crack initiation points were all at sub-sur­ column (b), Fig. 10), due to a refinement of the surface grains under
face after shot peening from 32 to 200 °C, their microstructures at severe plastic deformation [28]. By highlighted with pink lines, the
the top surface regions were likely to be modified by the direct {1012} deformation twinning boundaries appeared in high density in
forceful impact at different temperatures to various degrees, which the top surface region (~ 63 µm), although they were not visible in
affected the distribution of CRS (Fig. 7), surface hardness (Fig. 8) and as-received Ti64′s band contrast. As hexagonal close packed α-Ti has
the cycle to failure (Fig. 5) eventually. Hence, the top surface region only 3 slip systems [37] (far less than 12 independent slip systems in
in Ti64 coupons have been investigated under electron back­ face-center-cubic metals), twinning serve as a main mechanism to
scattering diffraction (EBSD, Fig. 10). The detailed microstructures accommodate the severe plastic deformation induced by shot pe­
before and after shot peening at room temperature have been dis­ ening. The thickness of greater misorientation region in KAM also
cussed in our previous work [28]. The results are briefly summarized increased significantly to ~62 µm (3rd row, column (b), Fig. 10), si­
here. The Ti64 coupons consisted mainly of large grains milar to the depth with presence of {1012} twinning.
(3.7~201.3 µm) with irregular shapes. For as-received coupon, the The microstructural changes with in-situ WSP at higher tem­
band contrast map (2nd row, column (a) Fig. 10) acquired from peratures from 100 to 300 °C were quite similar as seen from the
boxed area of the forward scattered electron image (1st row, column band contrast and KAM images. The {1012} deformation twinning
(a) in Fig. 10) shows a well indexed area throughout except at the top boundaries were again observed only at the top surface after in-situ
edge region of about 8 µm thick (non-indexed dark strips). The in­ WSP at 100 and 200 °C. The top surface layers were comprised of
verse pole figure (IPF) in the inset shows that the as-received coupon black non-indexed top region followed by green region and then the
was dominantly comprised of hexagonal-close-packed (HCP) Ti underlying blue region with large and irregular α-Ti grains. The black

10
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

Fig. 11. Bright field TEM images from (a) as-received Ti64 and after shot peening at (b) 32, (c) 100 and (d) 300 °C.

region was 24~31 µm thick, while the green region was 56~70 µm observed area. Upon in-situ WSP at 100 °C (Fig. 11(c)), the entire area
when measured from the top surface. Unlike for shot peening at under TEM’s observation turned into fine and uniform grains with
room temperature which had a few indexed strips (high local mis­ average size about 70 nm. However, when the in-situ WSP tem­
orientations) present right from top surface, shot peening at high perature was further increased to 300 °C (Fig. 11(d)), the grain size
temperature (100~300 °C) resulted in a nearly continuous top black under the TEM observation appeared to be non-uniform again:
region without any indexed green strips, which seem suggesting a smaller at the top surface but larger at the underlying layer
denser fine grain distribution. WSP at 300 °C also led to very few (Fig. 11(d)).
{1012} twining boundaries formation, indicating that more active TEM-based crystallographic orientation mapping was employed
slips were activated to accommodate the severe deformation when to visualize the α-Ti and β-Ti grain distribution at the surface layer
the Ti64 was heated to high temperature. from the same set of samples examined in Fig. 11 (prepared via FIB).
The black non-indexed regions in EBSD and KAM mapping were The top 0.4 µm layer was comprised of very fine α-Ti grains which
attributed to refined grains which had sizes far below the EBSD step was below the step size and hence beyond the detection limit of
size of 1 µm described in our earlier work [28]. As SEM-based EBSD EBSD (row (a), column (i), Fig. 12). Under this layer, large α-Ti grains
is unable to provide further direct observation about microstructural with uniform orientation in z-direction can be seen clearly in as-
change after in-situ WSP at 100 °C, which significantly increased the received Ti64. In between the α-Ti grains were the curvy β-Ti strips
fatigue life at medium to low loads (Fig. 5), we similarly resort to (row (a), column (ii), Fig. 12). Each of them was comprised of dom­
TEM and TEM-based crystallographic orientation mapping to unveil inantly single orientation. The β-Ti grains had a width below 0.3 µm,
the mechanism behind the beneficial effect of in-situ WSP at 100 °C. far smaller than the step size in SEM-based EBSD. Hence, they were
The as-received Ti64 had a surface layer about 0.4 µm thick with also not indexed under EBSD. Upon SP at room temperature (row (b),
very fine grains (<100 nm) due to the grinding process (Fig. 11(a)). Fig. 12), the α-Ti grains at the top surface layer (<1.7 µm) were clearly
Below this layer (marked by dotted white line), the coupons were fragmented into smaller size with random orientation, while the
comprised of large α-Ti grains separated by curvy β-Ti strips. Such underlying layer (~5 µm) was comprised of slightly bigger grains, but
large α-Ti grains were similarly observed under SEM-based EBSD, their sizes were still far smaller than those in the as-received Ti64
except that the top 0.4 µm was unable to be indexed by EBSD and coupons. The top β-Ti curvy strip was broken (row (b), column (ii),
hence appeared black (Fig. 10(a)). After shot peening at room tem­ Fig. 12), while the lower two β-Ti curvy strips were bombarded to
perature (Fig. 11(b)), the large α-Ti grains at the surface have been have multiple orientations, representing by several different colors.
fragmented into smaller grains at the top surface less than 1.7 µm Upon in-situ WSP at 100 °C, both α-Ti grains and the β-Ti strip at
thick (marked by dotted white line) but was bigger at the underlying the whole image frame with 5 × 3 µm2 were refined into small grains
substrate (2~4 µm). The grain size was non-uniform throughout the with random orientations (row (c), Fig. 12). Visually, the grain sizes

11
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

Fig. 12. TEM orientation map in z direction of α-phase Ti1.7Al0.3 (column i) and β-phase Ti0.7V0.3 (column ii) from (a) as-received Ti64 and after shot peening at (b) 32, (c) 100 and
(d) 300 °C. The scale bars in the images represent 1 µm. The overall imaging area is 5 × 3 µm2.

were much smaller than those after SP at room temperature (32 °C). This was accompanied by appearance of grains below 0.05 µm and a
Increasing in-situ WSP temperature had little effects in further re­ clear reduction in overall grain size. After in-situ WSP at 100 °C, there
ducing the grain size. Instead, large portion of bigger grains can be was a further increase in the relative abundance of grains blow
seen at the lower surface. The images of α-Ti grains and the β-Ti strip 0.05 µm at the expense of grains between 0.05 and 0.10 µm for both
after in-situ WSP at 300 °C were shown in row (d), Fig. 12. α- and β-grains. As a result, the average grain size of α- and β-Ti64
Each grain’s size can be extracted from Fig. 12 and the resultant decreased from 0.068 and 0.065 µm after SP at room temperature to
grain size distribution histogram are plotted in Fig. 13. The histogram 0.066 and 0.059 µm at 100 °C, respectively. With an increase in WSP
shows that the α-phase grains larger than 0.7 µm in the as-received temperature to 300 °C, the relative abundance of grains between
Ti64 vanished after shot peening at room temperature (Fig. 13(a)). 0.05 and 0.10 µm increased for both α- and β-grains. The average α-

12
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

Fig. 13. Grain size distribution based on TEM orientation map in Fig. 12 of (a) α-phase Ti1.7Al0.3 and (b) β-phase Ti0.7V0.3 from as-received Ti64 and after shot peening at 32, 100
and 300 °C.

Ti64 grain increased to 0.073 µm while average β-Ti64 grain size was further increased to 400 °C [14]. For Ti64, however, raising the
remained around 0.059 µm (Fig. 13). These observations thus suggest in-situ WSP temperature from room temperature to 100 °C im­
occurrence of grain recrystallization after WSP at 300 °C. mediately led to a decrease in CRS in the top 52 µm layer, as measured
by both center hole drilling and X-ray stress measurement (Fig. 7).
4. Discussion Further increasing in-situ WSP temperature to 200 and 300 °C led to
significant decrease in CRS (Fig. 7), although 300 °C is far below Ti64′s
Shot peening (SP) at room temperature enhances fatigue life by recrystallization temperature. The difference between the effect of
confining the inwards diffusion of micro-cracklines via compressive in-situ WSP on spring steel and Ti64 was attributed to the inherently
residual stress and prolonging cracklines’ diffusion distance via grain different mechanical properties. While the Young’s modulus, yield
refinement, which also work hardens the surface layer. Besides in­ strength and ultimate tensile strength (UTS) of the SUP9 spring steel
troducing these two effects, warm shot peening (WSP) is also af­ were reported to be 190 GPa, 1080 MPa and 1225 MPa, respectively
fected by thermal softening effect, which lowers flow stress and [39], the Young’s modulus, yield strength (σ0.2) and UTS of the present
hardness. Thermal softening can lead to higher degree of deforma­ Ti64 were measured by tensile test to be 122.4 GPa, 823.3 MPa and
tion and stress relaxation, both of which are more prominent at 897.8 MPa, respectively [28]. Spring steels typically have very high
higher temperatures. As a result, initial increase of surface roughness Young’s modulus and yield strength, which allows them to return to
with WSP temperature have been commonly observed in steel original shapes after repeated elastic deformation. Compared to SUP9
[14,15], Mg alloy [9,17] as well as the current Ti64 (Fig. 4(e)). Thermal spring steel, Ti64 has lower Young’s modulus and yield strength. As a
softening also facilitates deformation by slip, as well as dislocation result, thermal softening led to the stress relaxation at much lower
migration and dislocation annihilation at high temperatures. temperature for Ti64 (100 °C) than for spring steel (400 °C).
Therefore, the grains’ dynamic recrystallization can take place, re­ Although slightly relaxing the CRS at the surface, in-situ WSP at
sulting in small grains growing into bigger grains, if the WSP tem­ 100 °C resulted in a larger CRS compared to that SP at room tem­
perature is above the metals’ recrystallization temperatures, which perature from a depth of 56 µm onwards. Its CRS decreased to zero at
is approximately half the melting points, i.e. 0.5 Tm [38]. For ex­ a much deeper depth of 352 µm compared to 208 µm after SP at
ample, WSP of Mg AZ31 at 240 and 360 °C led to larger grains of 9.2 room temperature (Fig. 7). In addition, both TEM images (Fig. 11) and
and 13.2 µm, respectively, compared with that after SP at room TEM-based crystallographic orientation mappings (Fig. 12) show
temperature (3.6 µm) [9]. The growth of grain size after WSP of Mg that the surface layer after WSP at 100 °C has led to a much finer α-Ti
AZ31 alloys suggested occurrence of significant dynamic re­ grains at the top surface compared to those after SP at room tem­
crystallization during the WSP. The eventual in-situ WSP outcome perature. In-situ WSP at 100 °C increased the surface grain density
will be a trade-off among these effects and will be material- significantly, which effectively prolongs the diffusion distance of
dependent rather than a generalized rule. cracklines before they cause the coupons’ breakdown. Further in­
For SUP9 (Mn-Cr) spring steel, in-situ WSP introduced larger and creasing the WSP temperature to 200 and 300 °C led to easier dis­
deeper compressive residual stress (CRS) with an increase of tem­ location movement and annihilation and reduced the CRS
perature up to 300 °C, compared to CRS after shot peening at room significantly. As a result, in-situ WSP at 100 °C led to best fatigue
temperature. Its CRS only relaxed when the shot peening temperature performance of Ti64 coupons with three run-outs at low load

13
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

(Fig. 5). The fine balance between mild CRS relaxation and enhanced Acknowledgment
grains refinement results in an optimum in-situ WSP temperature
for Ti64 at 100 °C. At this temperature, the CRS and refined grains This research is supported by the Agency for Science, Technology
also work hardened the surface layer down to 500 µm and increased and Research (A*STAR), Singapore, under its Aerospace Program
the surface hardness observed under nano-indentation (Fig. 8). Thus, (A1715a00079) and Structural Metal Alloy Program (A18b1B0061).
in-situ WSP at 100 °C could also increase the wear resistance of the Dr. Thomas Haubold and Mr. Abhay Gopinath from Rolls-Royce as
Ti64 components. well as Dr. Dennis Tan Cheng Cheh and Prof. Upadrasta Ramamurty
from IMRE are acknowledged for their insightful discussion. Mr. Koh
5. Conclusion Li Teck and Mr. Kelvin Kuan from ST Aerospace Engines Pte Ltd are
acknowledged for their assistance with the shot peening.
In summary, Ti64 coupons have been in-situ warm shot peened
(WSP) at 100, 200 and 300 °C, and compared with the coupons after Appendix A. Supporting information
shot peening at room temperature (RT). The surface roughness,
oxygen weight percentage and α-Ti phase percentage increased lin­ Supplementary data associated with this article can be found in
early with an increase in the WSP temperature due to severer plastic the online version at doi:10.1016/j.jallcom.2021.160701.
deformation at higher temperatures, while both surface compressive
residual stress (CRS) and maximum CRS in the bulk decreased with References
WSP temperature. Fatigue crack initiation point was pushed from
[1] S.J. Lainé, K.M. Knowles, P.J. Doorbar, R.D. Cutts, D. Rugg, Microstructural char­
surface at as-received condition to sub-surface after shot peening acterisation of metallic shot peened and laser shock peened Ti–6Al–4V, Acta
from 32 to 200 °C. It moved back to surface after shot peening at Mater. 123 (2017) 350–361.
300 °C. Although in-situ WSP at 100 °C led to a relaxation of CRS at [2] Z.G. Liu, T.I. Wong, W. Huang, N. Sridhar, S.J. Wang, Effect of surface polishing
treatment on the fatigue performance of shot-peened Ti–6Al–4V alloy, Acta
the surface from − 775.0 to − 746.3 MPa and a reduction in the Metall. Sin. (Engl. Lett.) 30 (2017) 630–640.
maximum CRS from − 877.7 to − 807.1 MPa, it produced a larger CRS [3] X.P. Jiang, C.S. Man, M.J. Shepard, T. Zhai, Effects of shot-peening and re-shot-
compared to that SP at room temperature from a depth of 56 µm peening on four-point bend fatigue behavior of Ti-6Al-4V, Mater. Sci. Eng. A 468
(2007) 137–143.
onwards, and thickened surface layer with CRS from 208 to 352 µm.
[4] A.P. Parker, Autofrettage of open-end tubes - pressures, stresses, strains, and
In addition, it resulted in much refined grains with high density of code comparisons, J. Press. Vessel Technol. Trans. ASME 123 (2001) 271–281.
{1012} twining boundaries at the top surface. These refined grains [5] R.K. Nalla, I. Altenberger, U. Noster, G.Y. Liu, B. Scholtes, R.O. Ritchie, On the
increased the hardness of the surface layer significantly and pro­ influence of mechanical surface treatments - deep rolling and laser shock pe­
ening - on the fatigue behavior of Ti-6Al-4V at ambient and elevated tempera­
longed the diffusion pathways of the micro cracklines. The overall tures, Mater. Sci. Eng. A 355 (2003) 216–230.
results effectively led to much higher fatigue life at medium (0.7 F0.2) [6] A. Lim, S. Castagne, C.C. Wong, Effect of deep cold rolling on residual stress
and low (0.5 F0.2) loads, although effects at high load (0.9 F0.2) were distributions between the treated and untreated regions on Ti-6Al-4V alloy,
J. Manuf. Sci. Eng. 138 (2016).
marginal. Therefore, an optimum in-situ WSP temperature for Ti64 is [7] C.C. Wong, A. Hartawan, W.K. Teo, Deep cold rolling of features on aero-engine
determined to be 100 °C. components, in: Proceedings of the 2nd CIRP Conference on Surface Integrity
In addition to the studies of WSP on spring steel [10,14–16], Mg (CSI), Procedia CIRP 13, (2014) 350-354.
[8] D. Arola, M. McCain, S. Kunaporn, M. Ramulu, Waterjet and abrasive waterjet
alloys [9,17], SiCw/Al composites [18] and TiB2/Al composite [19], this surface treatment of titanium: a comparison of surface texture and residual
study demonstrates the applicability of WSP on another technolo­ stress, Wear 249 (2001) 943–950.
gically important Ti64 alloy. It also advocates future attempts for [9] L.B. Peral, A. Zafra, S. Bagherifard, M. Guagliano, I. Fernández-Pariente, Effect of
warm shot peening treatments on surface properties and corrosion behavior of
other prospective candidates such as aluminum lightweight alloys
AZ31 magnesium alloy, Surf. Coat. Technol. 401 (2020) 126285.
and the new high/medium entropy alloys, with the latter is reported [10] A. Wick, V. Schulze, O. Vohringer, Effects of stress- and/or warm peening of AISI
to have sluggish diffusion coefficient [40] and should have good 4140 on fatigue life, Steel Res. 71 (2000) 316–321.
potential in containing dislocation diffusion and annihilation at high [11] A. Tange, K. Ando, Improvement of spring fatigue strength by new warm stress
double shot peening process, Mater. Sci. Technol. 18 (2002) 642–648.
temperatures. [12] M. Schilling-Praetzel, F. Hegemann, P. Gomez, G. Gottstein, H. Indusa, M. Spain,
Influence of temperature of shot peening on fatigue life, Conf. Proc. ICSP-5
CRediT authorship contribution statement (1993) 227–238.
[13] N. Hasegawa, Y. Watanabe, Y. Kato, Effect of shot peening on fatigue strength of
carbon steel at elevated temperature, Conf. Proc. ICSP-5 (1995) 157–162.
Su Hui LIM: Investigation, Writing - original draft, Writing - re­ [14] Y. Harada, K. Mori, Effect of processing temperature on warm shot peening of
view & editing. Zheng ZHANG: Conceptualization, Methodology, spring steel, J. Mater. Process. Technol. 162–163 (2005) 498–503.
[15] A. Wick, V. Schulze, O. Vohringer, Effects of warm peening on fatigue life and
Formal analysis, Writing - review & editing, Supervision, Project relaxation behaviour of residual stresses in AISI 4140 steel, Mater. Sci. Eng. A
administration, Funding acquisition. Debbie Hwee Leng SENG: 293 (2000) 191–197.
Investigation, Writing - review & editing. Ming LIN: Investigation. [16] R. Menig, V. Schulze, O. Vöhringer, Optimized warm peening of the quenched
and tempered steel AISI 4140, Mater. Sci. Eng. A 335 (2002) 198–206.
Siew Lang TEO: Investigation. Fengxia Wei: Investigation, Writing - [17] Y. Huang, W.C. Liu, J. Dong, Surface characteristics and fatigue performance of
review & editing. Augustine Kok Heng CHEONG: Investigation. warm shot peened wrought magnesium alloy Mg-9Gd-2Y, Mater. Sci. Technol.
Shijie WANG: Writing - review & editing. Jisheng PAN: Writing - 30 (2014) 1481–1487.
[18] J.J. Huang, Z. Wang, J. Gan, Y. Yang, G. Wu, Q.S. Meng, Investigation of fatigue
review & editing.
performance improvement in SiCw/Al composites with different modified shot
peening treatments by considering surface mechanical properties, J. Alloy.
Data Availability Compd. 728 (2017) 169–178.
[19] W.Z. Luan, C.H. Jiang, V. Ji, Y.H. Chen, H.W. Wang, Investigation for warm peening of
TiB2/Al composite using X-ray diffraction, Mater. Sci. Eng. A 497 (2008) 374–377.
The raw/processed data required to reproduce these findings [20] B.G. Scuracchio, N.B. de Lima, C.G. Schön, Role of residual stresses induced by
cannot be shared at this time due to technical or time limitations. double peening on fatigue durability of automotive leaf springs, Mater. Des.
However, the data can be made available upon request. 47 (2013) 672–676.
[21] Y. Harada, Y. Saeki, K. Takahashi, Effect of different shot peening treatments on
fatigue life in Ti alloy, in: R. Shabadi, M. Ionescu, M. Jeandin, C. Richard, T.
Declaration of Competing Interest Chandra (Eds.) Thermec 2018: 10th International Conference on Processing and
Manufacturing of Advanced Materials, (2018), pp. 908–913.
[22] K. Faller, F.H. Froes, The use of titanium in family automobiles: current trends,
The authors declare that they have no known competing fi­ JOM 53 (2001) 27–28.
nancial interests or personal relationships that could have appeared [23] R.R. Boyer, An overview on the use of titanium in the aerospace industry, Mater.
to influence the work reported in this paper. Sci. Eng. A 213 (1996) 103–114.

14
S.H. Lim, Z. Zhang, D.H.L. Seng et al. Journal of Alloys and Compounds 882 (2021) 160701

[24] M. Peters, J. Kumpfert, C.H. Ward, C. Leyens, Titanium alloys for aerospace [33] R.O. Ritchie, D.L. Davidson, B.L. Boyce, J.P. Campbell, O. Roder, High-cycle fatigue
applications, Adv. Eng. Mater. 5 (2003) 419–427. of Ti-6Al-4V, Fatigue Fract. Eng. Mater. Struct. 22 (1999) 621–631.
[25] C.N. Elias, J.H.C. Lima, R. Valiev, M.A. Meyers, Biomedical applications of titanium [34] S. Hong, R. Weil, Low cycle fatigue of thin copper foils, Thin Solid Films
and its alloys, JOM 60 (2008) 46–49. 283 (1996) 175–181.
[26] H.J. Rack, J.I. Qazi, Titanium alloys for biomedical applications, Mater. Sci. Eng. C [35] Y.B. Liu, Y.D. Li, S.X. Li, Z.G. Yang, S.M. Chen, W.J. Hui, Y.Q. Weng, Prediction of the
26 (2006) 1269–1277. S–N curves of high-strength steels in the very high cycle fatigue regime, Int. J.
[27] W.J. Harris, The Influence of fretting on fatigue. Part III, in, Paris, France, (1972). Fatigue 32 (2010) 1351–1357.
[28] Z. Zhang, M. Lin, D.H.L. Seng, S.L. Teo, F. Wei, H.R. Tan, A.K.H. Cheong, S.H. Lim, [36] G.A. Pantazopoulos, A short review on fracture mechanisms of mechanical
S. Wang, J. Pan, Fatigue life enhancement in alpha/beta Ti-6Al-4V after shot components operated under industrial process conditions: fractographic ana­
peening: an EBSD and TEM crystallographic orientation mapping study of sur­ lysis and selected prevention strategies, Metals 9 (2019) 148.
face layer, Materialia (2020) 100813. [37] M. Peters, J. Hemptenmacher, J. Kumpfert, C. Leyens, Structure and properties of
[29] C. Wang, L. Wang, Thermo-mechanical coupled simulation of warm shot peening titanium and titanium alloys, in: C. Leyens, M. Peters (Eds.), Titanium and
of Ti6Al4V alloy, China Surf. Eng. 32 (2019) 143–153. Titanium Alloys: Fundamentals and Applications, Wiley-VCH, Verlag GmbH &
[30] J.K. Li, Y. Mei, W. Duo, W. Renzhi, An analysis of stress concentrations caused by Co. KGaA, 2003, pp. 1–36.
shot peening and its application in predicting fatigue strength, Fatigue Fract. [38] T. Sakai, A. Belyakov, R. Kaibyshev, H. Miura, J.J. Jonas, Dynamic and post-dy­
Eng. Mater. Struct. 15 (1992) 1271–1279. namic recrystallization under hot, cold and severe plastic deformation condi­
[31] G.I. Mylonas, G. Labeas, Numerical modelling of shot peening process and cor­ tions, Prog. Mater. Sci. 60 (2014) 130–207.
responding products: residual stress, surface roughness and cold work predic­ [39] H. Chandra, D.K. Pratiwi, M. Zahir, High-temperature quality of accelerated
tion, Surf. Coat. Technol. 205 (2011) 4480–4494. spheroidization on SUP9 leaf spring to enhance machinability, Heliyon 4 (2018)
[32] Y. Wen, P. Liu, L. Xie, Z. Wang, L. Wang, W. Lu, C. Jiang, V. Ji, Evaluation of me­ 01076.
chanical behavior and surface morphology of shot-peened Ti-6Al-4V alloy, [40] M.H. Tsai, J.W. Yeh, High-entropy alloys: a critical review, Mater. Res. Lett.
J. Mater. Eng. Perform. 29 (2020) 182–190. 2 (2014) 107–123.

15