Materials Science and Technology

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Microstructure and tensile behaviour of pure

titanium produced after high-energy shot peening

S. Dai, Y. Zhu & Z. Huang

To cite this article: S. Dai, Y. Zhu & Z. Huang (2016) Microstructure and tensile behaviour of
pure titanium produced after high-energy shot peening, Materials Science and Technology, 32:13,
1323-1329, DOI: 10.1080/02670836.2015.1121598

To link to this article: http://dx.doi.org/10.1080/02670836.2015.1121598

Published online: 08 Feb 2016.

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Microstructure and tensile behaviour of pure
titanium produced after high-energy shot
peening
S. Dai 1, Y. Zhu2 and Z. Huang1

In this study, the microstructure and tensile behaviour of pure titanium processed by means of high-
energy shot peening have been studied. The results show that a nanocrystalline surface layer is
prepared on the surface of pure titanium. During severe deformation, the dislocations, twins and
slip bands with single orientation are formed rst, then the intersections of twins and slip bands are
observed, and then the subgrains appear near or in the slip bands and nally the randomly oriented
nano-grains are formed due to the further breakdown. After high-energy shot peening, the ultimate
tensile strength and the yield strength increase by 27 and 40%, while the elongation decreases by
64% after treatment, due to the increasing dislocation density, micro-strain and the grain renement.
Keywords: Pure titanium, High-energy shot peening, Microstructure, Twins, Dislocations, Mechanical property

Introduction after treatment. A large number of defects are introduced

Owing to high specic strength, superior biocompatibility
and outstanding corrosion resistance, pure titanium and
Ti6Al4V alloy have been widely used as permanent
implant materials of damaged hard tissues.1,2 It is
known that the V element exhibits high cytotoxicity and
Al element may induce senile dementia for the latter
alloy.3 Pure titanium is considered as the one of the best
implanted materials as it is only composed of Ti element
without toxic elements.4 However, the strength of pure
titanium is a little lower than Ti6Al4V, leading to the
narrower application scope.
Surface nanocrystallisation (SNC) is an effective and
economical route to improve the strength for metal
materials.5 A variety of severe plastic deformation pro-
cesses have been proposed to produce SNC, such as shot
peening. Recent researches had successfully revealed that
particular shot-peening processes were applied to achieve
ultrane grained materials on the surface of treated
parts. Unal and Varol6 studied that the microstructure
and hardness of AISI 304 austenitic stainless steel per-
formed by different types of shot peening, including air
blast conventional shot peening, severe shot peening and
repeening. The results showed that the deformation layer
had nano-grain size distributions with much higher hard-
ness. Bagherifard and Guangliano7 focused on fatigue
strength of surface nonacrystallised low alloy steel
obtained by the application of severe shot-peening process
and the results testied the improvement of fatigue life
into the surface of the treated sample by means of shot
peening and the strength may increase due to the severe
plastic deformation. With regard to pure titanium, some
researchers have investigated the microstructure evolution
performed by means of surface mechanical attrition treat-
ment (SMAT). For example, Zhu et al.8 studied that the
microstructure of the surface layer after SMAT and dis-
cussed the mechanism of the formation of nano-grains on
the basis of recrystallisation process. Wen et al.9 investi-
gated the step of the defect evolution during SMAT inten-
sively. However, there are few investigations dealing with
the effect of shot peening on the microstructure and mech-
anical property of pure titanium. Compared with SMAT,
the stress and the deformation caused by particular shot
peening are larger, which is favourable for the improvement
of strength and the formation of nano-grains. Moreover, it
was reported that the nano-grained (NG) materials were
effective in improving the biological responses of bone-
forming cell, since there was a similarity in topography
scale between NG materials and bone.1012 Therefore,
pure titanium after shot peening may have better mechan-
ical property and biocompatibility.
High-energy shot peening (HESP) is the one of the hot-
test topic in the eld of severe plastic deformation pro-
cesses. The present study focused on microstructure
evolution of pure titanium obtained by means of HESP
and the nano-crystal layer was prepared on the surface.
Also, the hardness and strength of the sample after treat-
ment were investigated.

1
Nano Structural Materials Center, Nanjing University of Science and Tech- Experimental
nology, Nanjing 210094, China
2
Department of Materials Science & Engineering, North Carolina State Uni- The material used in this study was a 4-mm-thick plate
versity, Raleigh, NC 27695, USA made of pure titanium and the chemical composition in

Corresponding author, email daishijuan_1982@163.com weight percent was given as follows: 0.11Fe, 0.15O,

2016 Institute of Materials, Minerals and Mining

Published by Taylor & Francis on behalf of the Institute
Received 3 August 2015; accepted November 2015
DOI 10.1080/02670836.2015.1121598 Materials Science and Technology 2016 VOL 32 NO 13 1323
Dai et al. Behaviour of pure titanium produced after HESP
0.23Al and balance Ti. The plate was annealed in argon
atmosphere at 1023 K for 2 h and then air-cooled in fur-
nace to room temperature. The stainless steel balls with
the diameter of 3 mm were used and the shot velocity
was 60 m s1. Both sides of annealed specimen were
high-energy shot peened for 30 min at room temperature.
Optical microscope (OM) was used to examine the
microstructure evolution along sections perpendicular to
the treated surface of the specimens. The cross-sections
were mechanically polished using silicon carbide paper
and a polishing cloth, and nally etched at room tempera-
ture in a solution of 1 mL HF, 3 mL HNO3 and 7 mL dis-
tilled water. Then, the phase structure was analysed by an
X-ray diffractometer (XRD, D8 Discover) with Cu K
radiation and graphite monochromator operated at 40
KV and 40 mA, and the grain size and micro-strain of
the samples were calculated from line broadening of
Bragg diffraction peaks using equations (1) and (2),
respectively.13,14
Kl
Size = cos u
b layer thickness (approximately 150 m) was close to that
b limitation to the increase in the deformed layer depth
1= tan u
4 due to the balance between the elasticplastic defor-
where Size means the grain size; K means constant,
usually K=1; means the X-ray wavelength; means
the full width at half maximum of the peak; is the
Bragg angle of the [h k l] reection and means the
micro-strain.
Transmission electron microscopy (TEM) investi-
gations were carried out on FEI Tecnai 20 microscopes
operating at 200 KV. The plane-view TEM foils of layers
at different depths were obtained rst by polishing the
corresponding surface layer, then mechanically polishing
the sample on the untreated side until it was approxi-
mately 50-m thick and followed by electro-polishing
using a twin-jet technique. Shimadzu HMV-G microhard-
ness tester was used for determining the hardness altera-
tion from shot-peened surface to the interior with a load
of 1 N and duration of 10 s. The mechanical property of
the sample was obtained by an electronic universal test
machine (CMT 5105).
1 Cross-sectional OM images of the sample a before and b after HESP
1324 Materials Science and Technology 2016 VOL 32
Results and discussion
Microstructures
Cross-sectional OM images of the samples are shown in
Fig. 1. Before HESP, grains with no deformation can be
clearly seen in the matrix and the grain size of the matrix
is approximately 2030 m (Fig. 1a). After HESP, the
microstructure close to the surface cannot be indentied
and severe deformation layers are observed in Fig. 1b.
The thickness of the surface deformation layer is not uni-
form (80140 m) and the reason may be attributed to the
heterogeneous nature of plastic deformation within and
between grains.15,16 The microstructures of the treated
sample can be separated into three layers accordingly:
(1) severe deformation layer; (2)minor deformation layer
and (3)strain-free matrix, and the three layers have no
obvious boundaries. The strain decreases gradually from
the surface to the interior, leading to the fact that the gra-
dient microstructure exhibits nano- to submicro- to
micro-structure. In the reference,17 pure titanium speci-
mens were severe shot peened and the obtained deformed
(1)
in this study. It can be referred that there seems to be a
(2)
mation and the dynamic restoring.18
X-ray diffractometer results
X-ray diffractometer proles of the surface layers before
and after HESP are shown in Fig. 2. Test condition is con-
tinuous scanning with 2 min1 from 10 to 90. It is clear
that no phase transition occurs after HESP. The broaden-
ing of the diffraction peaks obtained by means of HESP
can be attributed to small crystallite size and micro-strain.
Meanwhile, (101) crystal plane is the main slip plane
during deformation for pure titanium, which is easier to
slip compared with other slip planes.19 As shown in Fig.
2, the diffraction peak on (101) crystal plane changes
more signicantly, which means the grain renement
effect caused by slipping on this plane is relatively larger.
In addition, the average grain size and micro-strain are
investigated by analysing the XRD proles. Obviously,
the average grain size close to the surface is effectively
NO 13
 Dai et al. Behaviour of pure titanium produced after HESP

this study, the micro-strain increases up from 0.058 to

0.325% after HESP, due to the enhancement of the lattice
distortion, as shown in Table 1. The increase in the defects
caused by severe deformation leads to the increase in
micro-strain after treatment.

Transmission electron microscopy images

At a depth of 250 m below treated surface
The typical microstructure with dislocation tangles and
deformation twins is found at the depth of 250 m
from the treated surface. Figure 3a shows that the
tangled dislocations are evident due to the large strain
and strain rate. Meanwhile, parallel bands approxi-
2 X-ray diffractometer proles of the sample before and after mately 100-nm width are observed, as shown in Fig.
HESP 3b. Selected area electron diffraction (SAED) patterns
taken from areas containing two adjacent bands reveal
that they are twins with respect to the (-2112) plane.
rened to nano-meter scale after HESP, which shows that The deformation twins (-2112) are a common type for
a higher strain and strain rate are more effective in caus- pure titanium with hexagonal close-packed (HCP)
ing to the formation of nano-grains (Table 1). After severe crystal structure. The similar result was obtained in the
plastic deformation, micro-strain obtained by using X-ray literature,22 which showed that the twins (-2112) were
diffraction can help to investigate the inuence of the active during plastic deformation. Munroe and Tan23
deformation process. Micro-strain alteration after shot theoretically investigated the orientation of deformation
peening has been studied in a lot of literatures.20,21 In twinning in HCP metals and they found that (-2112) and
(1012) twins were dominant under compressive loading.
A great amount of small balls with high kinetic energy
Table 1 Average grain size and micro-strain of the sample
impacting on the surface of samples causes elastic and
before and after HESP plastic deformation in the process of HESP, leading to
the formation of the twins with respect to the (-2112)
Sample Average grain size/nm Micro-strain/% plane. Moreover, it can be seen that the twins generally
run across the entire grain and stop at the boundary,
Before HESP 23500 0.058
but one of the ends terminates inside the grain occasion-
After HESP 65 0.325
ally, as shown in Fig. 3b.

3 Transmission electron microscopy images of the sample by HESP at the depth of 250 m from the treated surface a dislo-
cation tangles; b parallel twins; c SAED which is taken from b

Materials Science and Technology 2016 VOL 32 NO 13 1325

Dai et al. Behaviour of pure titanium produced after HESP
4 Transmission electron microscopy images of the sample by HESP at the depth of 150 m from the treated surface a twins with
different orientations and b twins and slip bands
At a depth of 150 m below treated surface
Transmission electron microscopy examination of the
layer approximately 150 m below the surface is shown
in Fig. 4 and the microstructure differs from that at the
depth of 250 m. As shown in Fig. 4a, the intersections
of strip twins are observed. The twins with a variety of
orientations are formed in one grain and they cut across
each other. Moreover, a larger number of parallel slip
bands with 400500-nm width can be found (Fig. 4b)
and some twins go across the slip bands, where a lot of
dislocation pile-ups exist. It can be inferred that the inter-
sections of the twins and slip bands with different orien-
tations improve the grain renement.
At a depth of 100 m below treated surface
Figure 5 shows the TEM images of the layer at the depth
of 100 m from the surface. The deformation twins disap-
pear and the width of slip bands narrows down to 200
300 nm at this time (Fig. 5a). The corresponding SAED
shows undeveloped arcs with well-dened diffraction
spots, suggesting that slip bands are low angle disorienta-
tions. As shown in Fig. 5b, the boundary of the slip band
is not straight as that of the twins and the formation of the
5 Transmission electron microscopy images of the sample by HESP at the depth of 100 m from the treated surface a slip
bands; b cross-slip and c subgrains in the slip band
1326 Materials Science and Technology 2016 VOL 32 NO
cross-slip is known by analysing the corresponding
SAED. In the present study, the cross-slip occurs on (1
102) and (2111) planes, but they are not the conven-
tional slip planes for pure titanium and the detailed mech-
anism has not been found out. Meanwhile, it is observed
that some subgrains with the size of 100200 nm exist in
the interior of the slip band, which indicates that the inter-
sections of the slip bands start to change into the equiaxed
subgrains gradually due to the larger strain.
At a depth of 30 m below treated surface
Figure 6 shows the TEM images of the layer at the depth
of 30 m from the surface. The bright and dark eld
images show that the microstructure is characterised by
distributed nano-meter scale grains (Fig. 6a and b). The
corresponding SAED patterns composed of continuous
rings (Fig. 6c) show that grains of the original sample
have been broken down to equiaxed nano-sized
grains and these grains are random in crystallographic
orientation. The histogram of grain size distribution
(Fig. 6d ), calculated using the method mentioned in the
literature,24 shows that the sizes of 35% of the grains
close to the surface are less than 100 nm. From Fig. 6,
13
 Dai et al. Behaviour of pure titanium produced after HESP

6 Transmission electron microscopy images of the sample by HESP at the depth of 30 m from the treated surface a bright eld
image showing nano-grains; b dark eld image corresponding to a; c SAED pattern of a and d histogram of grain size
distribution

it can be seen that HESP is a useful way for the prep- after HESP were 545 and 695 MPa, 405 and 567 MPa,
aration of nano-grains on the surface of the sample. and 31 and 12%, respectively. The UTS and the yield
strength increase by 27 and 40%, while the elongation
Summary of microstructure evolution decreases by 64% after treatment. However, the
The microstructure evolution of pure titanium processed elongation is still far larger than 8%, which meets the
by means of HESP at a shot velocity of 60 m s1 can be requirements of biomedical metal materials.28 The
separated into the following steps: (1) formations of dislo- increasing strength and decreasing elongation could be
cation tangles and twins with the single orientation; (2) attributed to the increasing dislocation density and
intersections of twins and slip band with different orien- micro-strain. During HESP process, a large number of
tations; (3) disappearance of the twins and formation of balls impact on the surface of specimen and the intersec-
the subgrains near or in the slip band and (4) the ran- tions of dislocations caused by elastic and plastic defor-
domly oriented nano-grains are formed due to the further mations are formed in the near-surface region. The
breakdown. increasing micro-strain leads to the enhancement of lat-
tice distortion. It is well known that the interactions of
dislocations and lattice distortion, which increase the
Hardness resistance of dislocation movement, can make the
Figure 7 depicts the hardness distribution of the samples strength increase and the elongation decrease. On the
along cross-section after HESP. The hardness close to the
surface is the maximum and the value is up to approxi-
mately 362 HV. The substantial increase in hardness
close to the surface is attributed to the increase in the dis-
location density and the decrease in the grain size, result-
ing in working hardening.2527 Owing to the formation of
gradient structure layer after being treated by HESP, the
hardness declines gradually from the surface to the
interior part of the sample. The value of the hardness
tends to be stable until the depth is 500 m, but it is still
higher than that of the untreated specimen. It indicates
that the structure of the matrix has no obvious change
after HESP (seen in Fig. 1), but the residual stress is intro-
duced into the matrix due to severe plastic deformation.

Tensile properties and fracture behaviour

Figure 8 shows stressstrain curves of the samples before
and after HESP. The ultimate tensile strength (UTS), the
yield strength and the elongation of the sample before and 7 Hardness distribution of the sample along cross-section

Materials Science and Technology 2016 VOL 32 NO 13 1327

Dai et al. Behaviour of pure titanium produced after HESP
8 a Stressstrain curves and SEM images of the fracture for the sample b before and c after HESP
other hand, the surface grains have been rened greatly
due to the serious plastic deformation, and ne grain
strengthening is another main factor for the improvement
of mechanical property.
In order to correlate the mechanical properties with
their structure, the failures close to the surface of the
untreated and treated specimen are observed by SEM.
As shown in Fig. 8b and c, both of the samples show
the characterisations with clear ductile features. Before
HESP, the dimples are uniform and the mean size is
approximately 100 m. In addition, it is also clear that
there are some large dimples with the size of 200300
m. The sample after HESP shows a lot of dimples with
the size varying from 10 to 100 m from the treated surface
to strain-free matrix and it has dimples with different sizes in
the different layers. It is known that the larger dimple indi-
cates that material has good plasticity and the size of the
dimples decreases after treatment, indicating the worse plas-
ticity, which is in accordance with the result of Fig. 8a.
Conclusion
(i) The deformation layer with the depth of 80140 m
was formed on the surface of pure titanium after HESP.
The average grain size close to the surface was rened
to nano-meter scale according to the XRD results.
(ii) A nanocrystalline surface layer was prepared by
means of HESP. During severe deformation, the dislo-
cations, twins and slip bands with single orientation
were formed rst, then the intersections of twins and
slip bands are observed, and then the subgrains appear
near or in the slip bands, lastly the randomly oriented
nanograins were formed due to the further breakdown.
(iii) After HESP at a shot velocity of 60 m s1 for
30 min, the UTS and the yield strength increased by
1328 Materials Science and Technology 2016 VOL 32 NO
27 and 40%, respectively, while the elongation
decreased by 64% after treatment, due to the increasing
dislocation density, micro-strain and the grain
renement.
Acknowledgement
This work was partly supported by Jiangsu Planned Pro-
jects for Postdoctoral Research Funds (grant no.
1402008A).
References
1. H. N. Liu and T. J. Webster: Nanomedicine for implants: a review of
studies and necessary experimental tools, Biomaterials, 2007, 28,
354369.
2. R. D. K. Misra, C. Nune, T. C. Pesacreta, M. C. Somani and L. P.
Karjalainen: Understanding the impact of grain structure in auste-
nitic stainless steel from a nanograined regime to a coarse-grained
regime on osteoblast functions using a novel metal deformation
annealing sequence, Acta Biomater., 2013, 9, 62456258.
3. R. Sahoo, B. B. Jha and T. K. Sahoo: Effect of primary alpha phase
variation on mechanical behavior of Ti6Al4V alloy, Mater. Sci.
Technol., 2015, 31, 14861494.
4. A. Thorfve, A. Palmquist and K. Grandeld: Three-dimensional
analytical techniques for evaluation of osseointegrated titanium
implants, Mater. Sci. Technol., 2015, 31, 174179.
5. K. Lu and J. Lu: Nanostructured surface layer on metallic materials
induced by surface mechanical attrition treatment, Mater. Sci. Eng.
A, 2004, 375, 3845.
6. O. Unal and R. Varol: Surface severe plastic deformation of AISI
304 viaconventional shot peening, severe shot peening and repeening,
Appl. Surf. Sci., 2015, 351, 289295.
7. S. Bagherifard and M. Guangliano: Fatigue behavior of a low-alloy
steel with nanostructured surface obtained by severe shot peening,
Eng. Fract. Mech., 2012, 81, 5668.
8. K. Y. Zhu, A. Vassel, F. Brisset, K. Lu and J. Lu: Nanostructure for-
mation mechanism of -titanium using SMAT, Acta Mater., 2004,
52, 41014110.
13

9. M. Wen, G. Liu, J. F. Gu, W. M. Guan and J. Lu: Dislocation evol-
ution in titanium during surface severe plastic deformation, Appl.
Surf. Sci., 2009, 255, 60976102.
10. G. Balasundaram and T. J. Webster: An overview of nano-polymers
for orthopedic applications, Macromol. Biosci., 2007, 7, 635642.
11. T. J. Webster, E. L. Hellenmeyer and R. L. Price: Increased osteo-
blast functions on theta+deltananober alumina, Biomaterials,
2005, 26, 953960.
12. T. J. Webster and J. U. Ejiofor: Increased osteoblast adhesion on
nanophase metals: Ti, Ti6Al4V, and CoCrMo, Biomaterials,
2004, 25, 47314739.
13. Z. Wang, W. Z. Luan, J. J. Huang and C. H. Jiang: X-ray diffraction
line prole analysis of iron ball milled powders, Mater. Sci. Eng. A,
2004, 366, 229238.
14. N. S. Goncalves, J. A. Carvalho, Z. M. Lima and J. M. Sasak: Size-
strain study of NiO nanoparticles by X-ray powder diffraction line
broadening, Mater. Lett., 2012, 72, 3638.
15. G. H. Majzoobi and A. R. Ahmadkhani: The effects of multiple re-
shot peening on fretting fatigue behavior of Al7075T6, Surf. Coat.
Technol., 2010, 205, 102109.
16. W. B. Liu, C. Zhang, Z. G. Yang and Z. X. Xia: Microstructure and
thermal stability of bulk nanocrystalline alloys produced by surface
mechanical attrition treatment, Appl. Sur. Sci., 2014, 292, 556562.
17. O. Unal, A. Cahit Karaoglanli, R. Varol and A. Kobayashi:
Microstructure evolution and mechanical behavior of severe shot
peened commercially pure titanium, Vacuum, 2014, 110, 202206.
18. H. L. Chan, H. H. Ruan, A. Y. Chen and J. Lu: Optimization of the
strain rate to achieve exceptional mechanical properties of 304 stain-
less steel using high speed ultrasonic surface mechanical attrition
treatment, Acta Mater., 2010, 58, 50865096.
Dai et al. Behaviour of pure titanium produced after HESP
19. M. Wen, J. F. Gu, G. Liu, Z. B. Wang and J. Lu: Formation of
nanoporous titania on bulk titanium by hybrid surface mechan-
ical attrition treatment, Surf. Coat. Technol., 2007, 201, 6285
6289.
20. Q. Feng, C. Jiang, Z. Xu, L. Xie and V. Ji: Effect of shot peening on
the residual stress and microstructure of duplex stainless steel, Surf.
Coat. Technol., 2013, 226, 140144.
21. L. Xie, C. Jiang and W. Lu: The inuence of shot peening on the
surface properties of (TiB+TiC)/Ti6Al4V, Appl. Surf. Sci.,
2013, 280, 981988.
22. D. H. Shin, I. Kim, J. Kim, Y. S. Kim and S. L. Semiatin:
Microstructure development during equal-channel angular pressing
of titanium, Acta Mater., 2003, 51, 983986.
23. N. Munroe and X. L. Tan: Orientation dependence of slip and twin-
ning in HCP metals, Scripta Mater., 1997, 36, 13831386.
24. L. M. Wang, Z. B. Wang, S. Guo and K. Lu: Annealing-induced
grain renement in a nanostructured ferritic steel, J. Mater. Sci.
Technol., 2012, 28, 4145.
25. S. Bagherifard, I. Fernandez-Pariente, R. Ghelichi and M.
Guagliano: Effect of severe shot peening on microstructure and
fatigue strength of cast iron, Int. J. Fatigue, 2014, 65, 6470.
26. D. K. Yang, P. Cizek and P. D. Hodgson: On the deformation mech-
anism of ultrane-grained titanium with multilayered hierarchical
structure, Mater. Sci. Eng. A, 2013, 582, 162169.
27. J. Lu, H. L. Chan, A. Y. Chen and H. N. Kou: Mechanics of high
strength and high ductility materials, Procedia Eng., 2011, 10,
22022207.
28. H. Y. Kim, T. Sasaki, K. Okutsu, J. I. Kim, T. Inamura, H. Hosoda
and S. Miyazaki: Texture and shape memory behavior of Ti22Nb
6Ta alloy, Acta Mater., 2006, 54, 423433.
Materials Science and Technology 2016 VOL 32 NO 13 1329