Accepted Manuscript

Characterization on Surface Mechanical Properties of Ti-6Al-4V after Shot Peening

Lechun Xie, Yan Wen, Ke Zhan, Liqiang Wang, Chuanhai Jiang, Vincent Ji

PII: S0925-8388(16)30120-7
DOI: 10.1016/j.jallcom.2016.01.119
Reference: JALCOM 36470

To appear in: Journal of Alloys and Compounds

Received Date: 14 December 2015

Revised Date: 7 January 2016
Accepted Date: 16 January 2016

Please cite this article as: L. Xie, Y. Wen, K. Zhan, L. Wang, C. Jiang, V. Ji, Characterization on Surface
Mechanical Properties of Ti-6Al-4V after Shot Peening, Journal of Alloys and Compounds (2016), doi:
10.1016/j.jallcom.2016.01.119.

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Relationship between two surface principal stress σ 1 , σ 2 and applied tensile strain
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εa for Ti-6Al-4V.
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Characterization on Surface Mechanical Properties of Ti-6Al-4V

after Shot Peening

Lechun Xie a, b *, Yan Wen c, Ke Zhan d, Liqiang Wang a, b *, Chuanhai Jiang a,

Vincent Ji e

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a
State Key Laboratory of Metal Matrix Composites, School of Materials Science and

Engineering, Shanghai Jiao Tong University, No. 800 Dongchuan Road, Shanghai

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200240, P.R. China

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b
Collaborative Innovation Center for Advanced Ship and Deep-Sea Exploration,

Shanghai 200240, P.R. China

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c
School of Physics and Optoelectronic Engineering, Nanjing University of

Information Science and Technology, Nanjing, Jiangsu 210044, P.R. China

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d
School of Materials Science and Engineering, Shanghai University for Science and
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Technology, 516 Jungong Road, Shanghai 200093, P.R. China

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e
LEMHE/ICMMO, UMR 8182, Université Paris-Sud 11, 91405 Orsay, France
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* Corresponding author: lechunxie@yahoo.com; wang_liqiang@sjtu.edu.cn

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Abstract

The surface mechanical properties of Ti-6Al-4V after shot peening (SP) were

investigated in this work. Firstly, the surface yield strength was obtained from the

in-situ X-ray stress analysis method combined with the tensile test technique, and the

value was increased to 1080 MPa, which was improved about 27% compared with the

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unpeened bulk material. It was ascribed to the surface work-hardening during the

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process of SP. Secondly, after SP, the hardness increased obviously and the

compressive residual stress was introduced in the surface layer, which were beneficial

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to the surface properties of Ti-6Al-4V. Even so, the compressive residual stress was

relaxed under cyclic loading. So thirdly, the relaxation of residual stress on the peened

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surface was studied under cyclic loading. The fast relaxation took place in the first

few cycles then became stable gradually in further cycles. When the applied tensile
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stress was approaching to the yield strength, the relaxation was drastic and distinct.

The behaviors of residual stress relaxation under different applied stresses were
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quantified by a function. The results indicated that the relaxation behavior was mainly
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influenced by the original magnitude, the applied stress and the cycling numbers. In

view of all analysis, it can be found that the method of combining in-situ X-ray stress
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analysis and the tensile test is an effective method to characterize the surface
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mechanical properties of metal materials after SP treatment.

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Keywords: Surface yield strength; X-ray stress analysis; Residual stress relaxation;

Cyclic loading; Shot peening; Ti-6Al-4V

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1．Introduction

Titanium alloys have received considerable attention because of their good

physical and mechanical properties [1-6]. However, during the process of

manufacturing and subsequent heat treatments, the tensile stresses always generate

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and may deteriorate the fatigue properties [7]. Some researches [7, 8] show that the

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fatigue failure often initiates from the surface. And the increment of surface strength

could effectively improve the resistance against fatigue failure [9]. As an effective

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and important surface treatment method, shot peening (SP) is a widely used cold

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working process in which the surface strength of a metal component is improved
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[10-14]. During the process of SP, a great amount of small balls with high kinetic

energy impact on the surface of components which causes the elastic and plastic
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deformation on the surface layer. The repeated impacts not only induce compressive
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residual stress but also refine the microstructure at surface and sub-surface regions,
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which makes the nucleation and propagation of fatigue crack more difficult. Several
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studies [15-17] have illustrated the beneficial effects of surface compressive residual

stresses on fatigue life of component. So the surface mechanical properties after SP

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treatment are crucial to the application of materials.

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Usually, the stress–strain relationship can be utilized to describe the mechanical

properties of materials. For bulk materials, the stress–strain relationship can be

obtained via the tensile test directly. However, for the film materials, the coating

materials or the surface treatment materials, the direct tensile testing is not available.

Therefore, the technology of X-ray diffraction (XRD) is adopted and utilized for

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evaluating the surface mechanical properties of materials [18-20] because the

diffraction beam penetrates into the metallic materials only in a limited depth,

generally about 10 µm. After SP treatment, the residual stress and microstrain on the

surface can be also obtained via XRD methods [21, 22]. The residual stress in such a

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thin surface layer usually exhibits a plane stress state, for one of the principal

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directions vertical to the surface plane with the stress value almost being zero. Even

so, above limited XRD methods cannot reveal the stress–strain relationship of the

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surface deformed layer after SP. Recently, a modified XRD method has been

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developed to measure the stress–strain relationship of thin films with a biaxial stress
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state by in-situ X-ray stress analysis method [23, 24]. This method is based on the von

Mises stress criterion instead the use of the maximum principal stress, and it has
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shown the availability. So based on the theory of in-situ X-ray stress analysis method,
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the experimental technique in our work will be improved by combining the X-ray
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stress analyzer and the tensile tester at the same time. Then the combined equipment

will be utilized to investigate the stress–strain relationship of shot peened surface

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layer, and determine the surface yield strength after SP.

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In addition to the stress-strain relationship, the residual stress on the surface is a

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significant mechanical parameter. After SP treatment, the compressive stresses are

introduced, which are beneficial in increasing resistance to stress corrosion cracking

[25], corrosion fatigue [26], fretting, galling and erosion caused by cavitations [27,

28]. However, during component operation, any static or cyclic residual stress

relaxation reduces the achievable benefits, because the beneficial compressive

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residual stresses at the surface are often imposed to a cyclic loading with tensile

stress. In some cases, the rate of residual stress relaxation may be drastic in the early

stages of cyclic loading, even more than 50% in extreme cases [29]. Moreover, it is

critical that the improvement of fatigue properties depends mainly on the stability of

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the residual stresses under on the tension-loaded state [30]. In spite of the

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considerable research, the technical challenge of understanding and accurately

quantifying residual stress relaxation under different cyclic loading still need to be

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investigated and overcome.

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Ti-6Al-4V is one of the developed titanium alloys, and SP as a surface
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strengthening method could greatly improve its surface mechanical properties. So in

this report, the surface mechanical properties of shot peend Ti-6Al-4V will be studied
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and analyzed in details. By using in-situ X-ray stress analysis method, the
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stress–strain relationship of shot peened surface layer will be obtained via the
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combined equipment. And the surface yield strength can be determined from the

stress–strain relationship. Meanwhile, the residual stress on the surface after SP will
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be measured and the relaxation behaviors under cyclic loading will be studied. All
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results will be analyzed and discussed in detail.

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2. Experimental

The specimens of Ti-6Al-4V used in this study were obtained via

high-temperature synthesis. In order to obtain the even composition, the process of

melt was more than three times. The yield strength of Ti-6Al-4V is about 850 MPa at

room temperature. The specimens were processed into the dog-bone shape with the
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effective dimension of 25×5×2 mm3 and then polished. One group of specimens

was treated by SP, and the other group was not done for comparison. The schematic

configuration and dimension of specimen was presented in Fig. 1. SP treatments were

carried out on both sides of the specimens by an air blasting machine (Carthing

Machinery Company, Shanghai, China). The diameter of peening nozzle was 15 mm

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and the distance between the nozzle and the sample was 100 mm. The intensity of SP

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was measured by the arc height of Almen specimen (A type), which was mainly

determined by jet pressure, SP time and SP medium. In this work, the coverage of

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each SP was 100%. The surface coverage of SP is very important in the process of SP,

and in order to control the surface coverage, the invariable jet pressure and SP time

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should be set. The velocity of the movement of nozzle should be slowly and equably.
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Additionally, the computer numerical control has been introduced in the process of
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SP, which plays a very significant role in controlling the surface coverage. In the

process of SP, the medium was Al2O3 ceramic balls with average diameter of 0.3 mm.
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Other parameters were given as follows: 0.55 MPa of jet pressure, 30 s of SP time and
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0.2 mmA of SP intensity.

Residual stresses were measured by X-ray stress analyzer (LXRD, Proto,

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Canada) with Cu-Ka radiation under 30 kV/ 25 mA and Ni filter. In the process of
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calculation, the elastic diffraction constants of Young’s modulus (E) and Poisson ratio

(ν ) are 114 GPa and 0.31 respectively. According to the residual stress calculation
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method, the planar stresses of the alpha phase of Ti-6Al-4V are determined finally.

The diffraction peak of Ti (213) were detected in measurement and then the residual

stresses were determined according to the sin2ψ method [31], and the range of tilting

angles was 0o – 45o. From the point of view of mechanics properties, there are only

several slip planes in titanium alloys, which results in elastic anisotropy under

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external loading, besides, textures may be introduced in the process of manufacture,

which is also an important factor in inducing elastic anisotropy. However, in this

work, the process of melt is repeated three times, which can reduce textures in

titanium alloys, especially in surface layers. So from the point of view of XRD

analysis, in this work, the titanium alloy is polycrystal materials and elastic isotropy

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in surface layers can be admissive. Absolutely the choice of (213) plane to calculate

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the residual stress is justified. The original residual stress after SP, and the

longitudinal stress σ1 and transverse stress σ2 under different loading were measured.

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At each step, the applied strain along the longitudinal direction were measured by

strain gage technique and the different loading was implemented by the tensile tester

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(Gopoint Testing Equipment Company, Shenzhen, China) in experiments. The length
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of reduced section of the sample was 25 mm (shown in Fig. 1). Based on the theory of
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in-situ X-ray stress analysis method, the experimental technique was improved by

combining the X-ray stress analyzer and the tensile tester at the same time, and then
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utilized to investigate the stress–strain relationship and determine the surface yield
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strength. The photo of combined equipment was shown in Fig. 2 and the related parts

were indicated.
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In terms of residual stress relaxation on the shot peened surface, the combined
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equipment was also used in our experiment. As for the cyclic loading, the applied
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stresses were 700, 750, 800 MPa, respectively. At each time after unloading, the

residual stresses were measured by X-ray stress analyzer. Besides, after SP, the

hardness distribution in the surface layer was measured by Digital Microhardness

Tester (DHV-1000, Beijing, China) with loading weight 2.94 N and holding time 20

s, and three times of each point were carried out and then the average values were

selected for description. In order to obtain the depth distribution of hardness and

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residual stress, the thin top surface layers were removed one by one via the method of

chemical etch with a solution of distilled water, nitric acid, and hydrofluoric acid in

proportion of 31:12:7. All experiments were carried out at room temperature.

3. Results and discussion

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3.1 Stress–strain relationship and surface yield strength

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The stress–strain relationship and surface yield strength can be determined by the

in-situ X-ray stress analysis method. It is assumed that the longitudinal and transverse

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directions of plate specimen are two principal directions of biaxial residual stress in

the surface (see Fig. 1). When external stress is applied to the longitudinal directions,

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the surface stress states are still biaxial and the principal directions do not change. On

the basis of the Von Mises yielding criterion [32], only the equivalent stress vs
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equivalent strain curve can be properly characterizes the mechanical properties of

specimen surface under biaxial stress state. The surface equivalent stress σ under
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each load can be defined as Eq. (1).

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σ = (σ 12 − σ 1σ 2 + σ 22 )1 2 (1)

In which, the σ 1 and σ 2 represent the stress in longitudinal and transverse

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directions measured by X-ray stress analyzer. About the uniaxial equivalent strain ε ,
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it can be expressed as Eq. (2) in the elastic deformation stage.

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ε = εe = σ E (2)

Where E is the Young’s modulus and ε e is the elastic strain. In the plastic

deformation stage, the ε can be shown as Eq. (3)

ε = εe + ε p (3)

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in which ε p is the plastic strain. Using σ 1′ , σ 1′′ , σ 2′ , σ 2′′ , ε a′ , ε a′′ , σ ′ and σ ′′ to

indicate the measured values of σ 1 , σ 2 , the applied strain ε a , and σ of two adjacent

measurement points. The increments of equivalent plastic strain ∆ε p for all intervals

is determined as

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σ ′ + σ ′′ ∆σ 1 − v∆σ 2
∆ε p = ∆ε a − (4)
σ 1′ + σ 1′′ − (σ 2′ + σ 2′′) / 2 E

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Where ∆σ 1 = σ 1′′ − σ 1′ , ∆σ 2 = σ 2′′ − σ 2′ , ∆ε a = ε a′′ − ε a′ . Then the total equivalent plastic

strain ε p for each measurement point can be obtained by successive summation.

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Firstly, two surface principal stress σ1, σ2 and the applied tensile strain εa for

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Ti-6Al-4V before SP are measured and shown in Fig. 3. Before measurement, the
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surface layer affected by the machining process was removed by chemical etch

polishing to eliminate the influence of surface defects. Before SP, there is little
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residual stress on the surface, therefore, the measured surface stress in longitudinal
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direction by X-ray method in Fig. 3 just reveals the value of external loading.
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However, the variation of stress values is negligible in the transverse direction. Fig. 4

is the stress–strain curves calculated by X-ray stress analysis method and the tensile
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test according to the results in Fig. 3. It indicates the good agreement between the

results by the proposed method and those of the tensile tests.

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The process of this work is descript as follow. Firstly, using the proposed method
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to calculate the surface stress-strain curve of sample before SP. For the unpeened

samples, the surface stress-strain curve should be according with the bulk stress-strain

curve by general tensile test because the material is homogeneous. Secondly, the bulk

stress-strain curve can be obtained easily, and the curve is shown in Fig. 4. Thirdly,

using this curve to verify the proposed method, it reveals that the method is suitable to

test the surface stress-strain curve of Ti-6Al-4V. Finally, utilizing the proposed
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method to determine the surface stress-strain curve of sample after SP because the

deformation of material is inhomogeneous after SP. This is the main purpose of this

work.

After SP, the original residual stresses without external loading can be regarded

as the primary stresses σ 1 and σ 2 in the longitudinal and transverse directions.

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While increasing the load, the variation of σ 1 and σ 2 , and the relation between

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stresses and the applied strain εa are displayed in Fig. 5. At beginning, σ 1 in

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longitudinal direction is compressive stress, which is due to the effect of SP on

improving the compressive stress on surface. With the increase of external load, the

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compressive stress σ 1 decreases with the increment εa in the elastic stage, and then
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gradually transforms to tensile stress during the plastic region. But the stresses σ 2

change slightly and the variations are not obvious during the uniaxial tension.
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According to the linear regression using the data of σ 1 in the elastic region in Fig. 5,
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the elastic modulus can be calculated [33]. The slope of shot peened state is around
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112 ± 5 GPa, which is approximated to the E of the bulk Ti-6Al-4V. During the stage

of plastic deformation, the σ 1 − εa curve shows nonlinear behaviors.

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Based on the data in Fig. 5 and the calculated method described above, the

relationship between the equivalent stress σ and the uniaxial equivalent strain ε
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of the surface can be calculated, which has been shown in Fig. 6. The yield strength

σ 0.2 of shot peened surface can be determined corresponding to the permanent plastic

strain 0.2%. As shown in Fig. 6, the surface yield strength σ 0.2 of Ti-6Al-4V is

about 1080 MPa while the SP intensity is 0.2 mmA. Compared with the yield strength

of unpeened bulk Ti-6Al-4V (850 MPa), the surface yield strength increases about

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27% after SP treatment. The results indicate that SP can effectively raise the surface

yield strength of Ti-6Al-4V.

3.2 Hardness and residual stress

After SP, hardness measurements indicate significant increments in the surface

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layer, and the related results have been shown in Fig. 7. It reveals that the hardness

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reaches the maximum at the top surface and then decreases gradually along the

increase of depth. The hardness on the shot peened surface is about 571 HV, which is

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more than 50% higher than the unpeened sample’s value (350 HV). Because SP is a

process of work-hardening which can induce refined domain size, high density

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dislocations, even the nano-crystalline layer on the surface layer [34]. These variation
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are beneficial to the surface hardness and strength of metal materials. The
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improvement of hardness on surface is consistent with the result of surface yield

strength.
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After SP treatment, the depth distribution of residual stress along the variation of
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depth is shown in Fig. 8. It can be found that the residual stresses are compressive

stress on the deformation layer, and the depth of deformation layer is about 150 µm.
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The values of residual stress increase to the max value, and then decrease and trend to
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stable at last. The max compressive residual stress appears on the subsurface of 15 µm,
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and the value is -795 MPa. Additionally, the residual stresses are very high and the

variation is not obvious in the near surface layer (d < 25 µm). The decline of residual

stress is obvious at the middle surface layer ( 25 µm < d < 125 µm), and it decreases

monotonously. At the deep surface layer (d > 125 µm), the decrease of residual stress

is gently and the values trend to stable. Since the plastically stretched surface layer

wants to expand and the adjacent elastically responding material around and below

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the impact restrains the expansion, therefore, the compressive residual stress is

generated in the surface layer. Moreover, the plastically restriction in the near surface

layer is more severe than that in the deep surface layer because of the direct impact

with shot balls during the process of SP, which leads to the higher compressive

residual stress in the near surface layer.

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3.3 Residual stress relaxation under cyclic loading

According to the results in Fig. 5, it can be found that the variation of stress in

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transverse direction is not obvious under loading. Therefore, in this part, the

investigation on residual stress relaxation under cyclic loading are mainly focused on

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the longitudinal direction. The relaxation behaviors under different applied stresses of
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700, 750 and 800 MPa along the longitudinal direction are displayed in Fig. 9. The
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same equipment is utilized in the experiment of relaxation behaviors and the

experiment of testing surface yield. The applied stress values are calculated based on
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the external loading. Three specimens under the same SP intensity (0.2 mmA) are
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chosen as experimental samples, and the surface residual stresses are measured as

-707, -649 and -657 MPa, respectively. Three samples are used at the same time
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during the process of SP treatment, so the errors are introduced between these three
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samples, even though under the same SP intensity. Moreover, during the measurement
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of residual stress, the second error is introduced by X-ray Stress Analyzer. Thus, the

initiation stress of these three samples are different in Fig. 9. Although the difference

exists, the error range is about 0-50 MPa, which can be ignored during this

measurement. Consequently, there is little influence of the difference on the results

and discussion.

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From Fig. 9, it indicates that the relaxation of residual stress depends on both the

applied stresses and the cycling number N. With the increase of N, the residual stress

starts to relax and the relaxation rate is fast in the initial stage for all three applied

loadings, which is consistent with the references [35, 36]. During the first few cycles,

the tensile cold working can improve the tensile yield strength, and the tensile yield

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strength is direct proportion to the tensile cold working [37]. Because of the existence

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of tensile cold working, the deformation under loading decreases in further cycles,

and the residual stresses trend to stable gradually after first few cycles. SP treatment is

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also the process of cold working, and the effect of SP is more obvious than that of

tensile cold working in this work, so after 30 times of cyclic loading, the stable

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residual stresses are still the compressive residual stress.
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In order to quantify the residual stress relaxation behavior under cyclic loading,
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the linear logarithm relationship proposed by Kodama is adopted to description [38],

which is expressed as Eq. (5).

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σ NRS = A + m log N (5)

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where σ NRS is the surface residual stress after N cycles. A and m are materials
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constants depending on the applied stress amplitude. Fig. 10 shows the relationship

between the residual stress and the logarithm of cycling number. Combining the
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datum in Fig. 10 and Eq. (5), the residual stress relaxation under three different
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applied loading can be expressed as: σ NRS = −662 + 176log N , σ NRS = −532 + 165log N ,

σ NRS = −394 + 113log N , which are corresponding to 700, 750 and 800 MPa

respectively. Based on above results, it can be found that the residual stress relaxation

is mainly influenced by the original magnitude, the value of applied stress and the

cycling numbers. The relaxation usually occurs easily while the applied stress is
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approaching to or bigger than the yield strength of the bulk materials. For Ti-6Al-4V,

the yield strength is 850 MPa, the applied stresses along the longitudinal direction are

700, 750 and 800 MPa in this work. Therefore, under the applied stress of 800 MPa,

the relaxation rate of compressive residual stress is fastest during the first few cycles.

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4. Conclusion

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Combining the X-ray stress analyzer and the tensile tester at the same time, the

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combined equipment was utilized to investigate the stress–strain relationship of shot

peened surface layer of Ti-6Al-4V, and determine the surface yield strength. The

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results showed that the surface yield strength σ 0.2 was about 1080 MPa while the SP
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intensity was 0.2 mmA. Compared with the yield strength of unpeened bulk

Ti-6Al-4V (850 MPa), the σ 0.2 increased about 27% after SP treatment, which
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indicated that SP can effectively raise the surface strength. In addition, the hardness
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increased obviously and the compressive residual stress was introduced after SP,
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which were beneficial to the surface properties. However, the compressive residual

stresses were relaxed under cyclic loading, and the results indicated that the relaxation
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behavior was mainly influenced by the original magnitude, the value of applied stress
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and the cycling numbers. The behaviors of stress relaxation were quantified as
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σ NRS = −662 + 176log N , σ NRS = −532 + 165log N and σ NRS = −394 + 113log N ,

which were corresponding to the applied stresses of 700, 750 and 800 MPa,

respectively. The stress relaxation usually occurs easily while the applied stress was

bigger than or approaching to the yield strength of bulk material, therefore, under the

applied stress of 800 MPa, the relaxation rate was fastest during the first few cycles.

Based on all results, the experimental method of combining in-situ X-ray stress

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analysis and the tensile test is an effective method and can be utilized as a

complementary approach to investigate the surface mechanical properties of metal

materials after SP treatment.

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Acknowledgment

This work is supported by the projects of National Natural Science Foundation of

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China (Grant No. 51302168 and 51502142), the 973 Program under Grant

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No: 2014CB046701 and Shanghai Pujiang Program (Grant No: 15PJD017). The

financial support of the General Program of Natural Science Foundation of the

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Jiangsu Higher Education Institutions of China (Grant No. 15KJB430021) and the
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Startup Foundation for Introducing Talent of NUIST (No. 2014r036) are gratefully
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appreciated. The authors also thank to the financial support of the National Natural

Science Foundation of China (NSFC) (No. 51405356), the Research Fund for the
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Doctoral Program of Higher Education of China (No. 20130143120015), and the

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Hujiang Foundation of China (B14006).

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[38] S. Kodama, Proc. Int. Conf. on Mechanical Behavior of Metals II, Kyoto, Society

of Material Science, 2 (1972) 111-118.

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Figure captions:

Fig. 1 Schematic configuration and dimension of specimens.

Fig. 2 Photo of the combined equipment with X-ray stress analyzer and the tensile

tester under in-situ tensile loading.

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Fig. 3 Relationship between two surface principal stress σ1, σ2 and the applied tensile

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strain εa for Ti-6Al-4V before SP.

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Fig. 4 Stress-strain curve of Ti-6Al-4V without SP by X-ray stress analysis method

and tensile test.

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Fig. 5 Relationship between two surface principal stress σ 1 , σ 2 and applied tensile
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strain εa for Ti-6Al-4V.

Fig. 6 Surface stress-strain curve between the equivalent uniaxial strain ( ε ) and the
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equivalent stress ( σ ) of Ti-6Al-4V after SP.

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Fig. 7 Depth distribution of hardness on Ti-6Al-4V surface layer after SP.

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Fig. 8 Depth distribution of residual stress on Ti-6Al-4V surface layer after SP.
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Fig. 9 Relationship between residual stress in longitudinal direction and the number

of cycles under different applied stresses in shot peened surface layer of Ti-6Al-4V.
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Fig. 10 Relationship between the residual stress and the logarithm of cycling number.
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Radius of fillet
Width 5 mm z (Vertical axis)
Width 5 mm
of grip 20 mm y (Transverse axis)
section

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2 mm x (Longitudinal axis)
25 mm
Thickness
Length of reduced section

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65 mm
Over-all length

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X- ray Stress Analyzer

X- ray emission tube

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Detector 1 Detector 2

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Tension Tension

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The sample
Tensile Tester

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Research highlights:

1. In-situ X-ray stress analysis method is used to study the surface yield strength.

2. Experiment is improved by combining X-ray stress analyzer and the tensile tester.

3. Surface yield strength is 1080MPa, increasing 27% compared with original sample.

4. Under load of 800MPa, the stress relaxation rate is fastest during first few cycles.

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5. Stress relaxation behavior under different loading can be quantified by a function.

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