International Journal of Fatigue 103 (2017) 258–263

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International Journal of Fatigue

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

Prediction of the surface finishing roughness effect on the fatigue

resistance of Ti-6Al-4V ELI for implants applications
Paulo Sergio Carvalho Pereira da Silva, Leonardo Contri Campanelli ⇑, Cesar Adolfo Escobar Claros,
Tales Ferreira, Diego Pedreira Oliveira, Claudemiro Bolfarini
Federal University of São Carlos, Department of Materials Engineering, Rod. Washington Luís km. 235, 13565-905 São Carlos, SP, Brazil

a r t i c l e i n f o a b s t r a c t

Article history: Based on the theors of elasticity for linear elastic materials and strain partitioning, a method was devel-
Received 8 May 2017 oped to predict fatigue lives of load bearing Ti-6Al-4V ELI implants with surfaces modified in the microm-
Received in revised form 4 June 2017 eter scale to promote bioactive materials and accelerate osseointegration. Notched fatigue specimens
Accepted 5 June 2017
were characterized by confocal laser scanning microscopy (CLSM) and subjected to axial fatigue tests
Available online 7 June 2017
at a constant maximum stress to determine the Siebel and Stieler’s C constant. The mean value obtained
for C was employed to determine the fatigue resistance (Kf factor) allowing the life prediction of samples
Keywords:
with different sized notches. The method was validated by performing fatigue tests with samples mod-
Fatigue
Notch effect
ified at two scales, 2 lm and 10 lm, typical values that can be produced in industrial conditions. It was
Titanium confirmed that the prediction method was in agreement with the experimental results. In addition, the
Implants prediction method clarified the strong reduction in the fatigue resistance from 850 MPa to 594 MPa due
to small differences in surface roughness, a result unexplained in the literature so far.
Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction monotonic effect (known as the Kt factor) that continuously

increases as the radius of curvature of the notch r decreases, the
Surface modification techniques have been developed in order influence on the fatigue resistance (known as the Kf factor) reaches
to promote the bioactivity of titanium implants and consequently a maximum for a critical radius value, as illustrated in Fig. 1. The
the osseointegration process [1]. In spite of the clinical benefit definition of Kf is:
related to the generation of micrometer or even nanometer fea-
fatigue limit without notch
tures on the surface, the increase in roughness that results from Kf ¼ ð1Þ
fatigue limit with notch
the surface treatments causes a great concern to the design of
implants, mainly because the fatigue performance of metallic This is readily understood when it is considered that, in the case
materials is very sensitive to the surface condition. Grit blasting of the fatigue resistance, the value of the maximum stress at the
and chemical treatment are typical techniques that alter the metal- notch region, which increases with the decrease of the radius of
lic surface without formation of brittle coatings, but the effect of curvature r, must be balanced by the volume of material affected
these treatments on the fatigue performance is contradictory. For by the stress concentration (Kf), which decreases with the decrease
example, acid etching employed by Pazos et al. [2] decreased the of the radius of curvature [8]. Differences between Kf and Kt factors
fatigue resistance of pure titanium, whereas acid + alkali treatment are that the first one depends on the materials properties and the
performed by Escobar Claros et al. [3] on Ti-6Al-4V kept the fatigue second one does not. For this reason, the Siebel and Stieler
resistance unchanged. approach describes the Kf behavior by Eq. (2), based on the factor
The changing of the fatigue response of a surface modified v related to the radius of curvature r, as in Eq. (3), and the material
implant depends on the magnitude of the produced surface modi- parameter C (Siebel):
fications, which can be approximately considered as mechanical pffiffiffiffiffiffiffiffiffiffiffiffi
Kt
notches. In fact, the influence of notches in the fatigue resistance ¼1þ Cv ð2Þ
Kf
of metals has been studied for many years [4–7]. Unlike the elastic
where
⇑ Corresponding author at: Rod. Washington Luís km. 235, P.O. Box 60, 13565- 2
905 São Carlos, SP, Brazil. v¼ ð3Þ
r
E-mail address: leoccampa@hotmail.com (L.C. Campanelli).

http://dx.doi.org/10.1016/j.ijfatigue.2017.06.007
0142-1123/Ó 2017 Elsevier Ltd. All rights reserved.
 Paulo Sergio Carvalho Pereira da Silva et al. / International Journal of Fatigue 103 (2017) 258–263 259

Fig. 1. Demonstrative plot from Eq. (1) for an arbitrary C = 0.0020 mm, a specimen Fig. 2. Schematic drawing of the fatigue specimen with detail in the dotted circle
with diameter D = 3.6 mm and a semicircular surface notch. for the notched region, which is amplified (all dimensions in millimeters).

when Kt varies between 2 and 5 [6]. C and r units are mm and v unit dimension strong enough to allow the machining operation on
is mm1. the fatigue specimens. As shown in Fig. 2, the notch had a radius
The C parameter depends on the notch radius r and on the of approximately 90 µm.
material properties. Although this constant is well established for Confocal laser scanning microscopy (CLSM) in an Olympus Lext
steels of several strengths, in the case of Ti-6Al-4V it is still not OLS 400 equipment was used to measure the actual dimensions of
found in the literature. Ploeg et al. [9] have published an extensive the produced notches. Image sizes of 645 lm  645 lm were ana-
study for the determination of the constants from the deformation lyzed at a magnification of 20. Table 1 shows the measured
partitioning method [10] for Ti-6Al-4V samples without notches, height h and width w of each notch, along with the standard devi-
and, therefore, without entering into considerations the C parame- ation values resulting from three measurements in each case, as
ter. The prediction of the surface effect on the fatigue life depends well as the mean radius r calculated as the average between the
on experimental tests of real components, comprising an exercise height and half width.
of trial and error. Such procedure is time consuming and may lead The fatigue tests of these specimens were conducted in air using
to delays in the development of surface modified implants that will a MTS Bionix servo hydraulic testing machine at a maximum stress
be subjected to cyclic loadings. Thus, in the case of real compo- Smax = 800 MPa, frequency f = 10 Hz and stress ratio R = 0.1. The
nents, such as hip femoral stems, there are still gaps in the litera- maximum stress value was determined based on the work of Esco-
ture to explain and to allow, prior to the tests, an analysis of the bar Claros et al. [3], in which the staircase method was employed
material’s behavior with a surface modification in a scale on the to compare the fatigue resistance of chemically treated specimens
order of few microns and of the large difference in the mechanical with polished ones, with 8 specimens in each case. The fatigue
behavior resulting from small surface variations. Such differences, limit for a run-out of 5  106 cycles was not statistically altered
if overlooked, might lead to catastrophic failures of the stems in and, for the surface modified condition, was equal to
the clinical use. 850 ± 26.5 MPa. By using the Student’s t-distribution for a sample
Therefore, the purpose of this work is to develop a method for size of 8 specimens and with 90% confidence interval (t = 1.860),
predicting the influence of the surface finishing on the fatigue it is possible to state that, for a peak stress of 800 MPa (850–
resistance of Ti-6Al-4V ELI, particularly in the micrometer scale, 1.860  26.5), only 5% of the specimens would fail in a sampling
by determining the C constant of Eq. (2), which is a measure of with a large number of specimens.
the notch sensitivity.
2.1.2. Determination of Kf factor
In the prediction method, for the application of Eq. (2), Kt values
2. Materials and methods
were calculated from classical equations based on the theory of
elasticity for linear elastic materials [13]. Eq. (4) is applied to an
2.1. Prediction method
elastic stress condition under axial loading in the case of a semicir-
cular notch in a cylindrical shape:
2.1.1. Determination of the C parameter
The material used in this work was taken from rounded bars of
the alloy Ti-6Al-4V ELI, with chemical composition, microstructure Table 1
and mechanical properties in accordance with the ASTM F136 Mean radius of the mechanical notches.
standard [11]. It is noteworthy that the alloy belongs to the same Specimen h (lm) w (lm) r (lm)
lot employed in the previous work of Escobar Claros et al. [3]. Eight
1 96.6 ± 1 161.3 ± 2 89.75
cylindrical fatigue specimens were machined with diameter
2 125.9 ± 1 174.2 ± 1 107.25
D = 3.6 mm in the test section following the dimensional require- 3 114.7 ± 2 163.5 ± 2 99.75
ments of the ASTM E466 standard [12], as illustrated in Fig. 2, 4 101.6 ± 6 168.3 ± 1 96.25
and subjected to a grinding and polishing step in order to remove 5 89.0 ± 1 169.4 ± 4 88.25
6 122.0 ± 6 210.9 ± 4 117.75
the machining marks. A circumferential and semicircular
7 99.7 ± 6 163.5 ± 1 94.00
mechanical notch was then machined in a lathe with a special 8 99.0 ± 4 168.6 ± 1 94.00
cutting tool fabricated by electrical discharge machining, with a
260 Paulo Sergio Carvalho Pereira da Silva et al. / International Journal of Fatigue 103 (2017) 258–263

   2  3
2h 2h 2h 2.2. Further chemical treatment
K t ¼ 3:04  5:42 þ 6:27  2:89 ð4Þ
D D D
In previous work reported by Escobar Claros et al. [3], a light
In the case of Kf calculation, it is necessary to consider two chemical treatment (Rz = 2 lm) showed that the fatigue resistance
stress and strain distributions. The first one comprises the nominal was maintained. Thus, to validate the notch effect on Ti-6Al-4V
stress amplitude (S) and elastic strain amplitude (De) acting far samples, a more aggressive chemical treatment was performed.
from the notch that results from the alternation of the applied This surface modification induced an Rz value higher than a critical
stresses, as follows: Rz value calculated that should cause a reduction on fatigue resis-
tance. For this step, Ti-6Al-4V ELI alloy bars were machined and
DS
S¼ ð5Þ polished to produce eight cylindrical specimens according to the
2
ASTM E466 standard [12]. The surface modification of the speci-
mens was carried out in two steps: initially with HCl, and subse-
DS quently with NaOH. For acid etching, a temperature of 60 °C and
De ¼ ð6Þ
E two hours were employed. The alkaline treatments were per-
The second distribution comprehends the elasto-plastic stress formed using 45 mL of NaOH 10 mol L1 solution to each sample
(Dr) and strain (De) acting at the notch tip. The total strain is cal- and a temperature of 60 °C during 24 h. These samples were ana-
culated from the theory of strain partitioning [10] and the total lyzed and compared to the results obtained by Escobar Claros
stress from the equation of the hysteresis loop, as follows: et al. [3]. Table 3 summarizes the nomenclatures employed
throughout the following sections for each surface condition.
De r0f þ rm The fatigue tests of Ti64-AE 2 specimens were conducted by the
¼ ð2NÞb þ e0f ð2NÞc ð7Þ
2 E staircase test method according to ISO 12107 standard [16] on a
MTS Bionix servo hydraulic testing machine, at a frequency
  10 f = 10 Hz and stress ratio R = 0.1, with immersion in a saline solu-
Dr Dr n
De ¼ þ2 ð8Þ tion (9 g/L) at 37 °C. The stress amplitude increment (Ds) was
E 2K 0
50 MPa (always testing a new specimen) and a predefined fatigue
with rm = 0 due to the stress shake-down effect in the plastic life (Nc) of 5  106 cycles was selected. Dixon and Mood method
regime and E = 110 GPa. The constants for Ti-6Al-4V ELI were taken was used to determine the fatigue stress mean value and the stan-
from the work of Ploeg et al. [9] and are shown in Table 2. These val- dard deviation.
ues correspond to Ploeg’s results obtained from tests in air at room The developed topography was examined by scanning electron
temperature, unlike the results applied to femoral stems, which microscopy (SEM), using a Philips XL-30 FEG microscope; rough-
were obtained from tests on Ringer’s solution (page 898 of [9]). ness measurements were obtained by CLSM using a Olympus Lext
From Neuber’s rule for plastic regime: OLS 4000 microscope. In this case, image sizes of
130 lm  130 lm were analyzed at a magnification of 50.
pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
Kf ¼ Kr  Ke ð9Þ
3. Results and discussion
Dr
Kr ¼ ð10Þ
DS 3.1. Mechanical notched specimens

De Table 4 presents the number of cycles N up to the rupture

Ke ¼
De
Other possible effects, such as residual stresses and resulting
microstructural alterations in a layer of around 300 lm deep from
the surface, are not considered in the prediction method as the
effect of residual stresses is well known, although many doubts
still remain, concerning, for instance, the type of residual stresses
(macro or micro residual stresses) and their effects on the various
stages of fatigue (nucleation of a micro crack, propagation of a
micro crack, propagation of a macro crack) [14,15]. The develop-
ment of a method to predict fatigue behavior without considering
the effect of residual stresses has an additional advantage since, if
the method predicts correctly the effect of surface modifications, it
is easily concluded that residual stresses have, in the specific case
applied, a negligible influence compared with the one of the
notches.
Table 2
Ti-6Al-4V ELI constants [9].
Constant
r0 f
e0 f
b 0.0407
c 0.648
K0
n0
ð11Þ
obtained in the fatigue tests of the notched specimens, the values
of Kt and Kf and the calculation of the C constant from Eq. (2).
With these results, the most probable value of C was calculated
(C = 0.0058 ± 0.0012 mm), allowing the determination of the val-
ues presented in Table 5, which will be the basis for further
discussions.
From Table 5, using greater approximation in the calculation
(omitted in the table for easier visualization of the results), the
radius of curvature 120 µm renders the maximum value of Kf,
and around this value the sensitivity of Kf to the radius of curvature
is minimum. Although this result was not known a priori, it was
convenient for the determination of the C constant since the mean
value of the machined notches (90 µm) was close to this value.
From Eq. (2), the calculated value of the C constant allowed the
construction of a curve relating the ratio Kt/Kf and factor v for Ti-
6Al-4V, which is presented in Fig. 3 and compared with the curves
of several steels (adapted from [8]). The Ti-6Al-4V curve falls
between the curves of steels with yield strength in the range 500
–900 MPa, suggesting that the calculation of the C constant
Value
819 MPa Table 3
0.886 Nomenclature adopted for the surface conditions.
Nomenclature Surface condition
825 MPa Ti64-AE 0.5 HCl (0.5 h) + NaOH (24 h) [3]
0.0629 Ti64-AE 2 HCl (2 h) + NaOH (24 h)
 Paulo Sergio Carvalho Pereira da Silva et al. / International Journal of Fatigue 103 (2017) 258–263 261

Table 4
Summary of the calculation of the C constant.

Specimen 2r/D Kt N (cycles) Kf Kt/Kf  1 v (mm1) C (mm)

1 0.0499 2.78 2668 2.06 0.35 22.1607 0.0056
2 0.0596 2.74 1886 2.18 0.25 18.6480 0.0035
3 0.0554 2.76 2491 2.08 0.32 20.0501 0.0053
4 0.0535 2.77 3031 2.02 0.37 20.7792 0.0066
5 0.0490 2.79 3469 1.98 0.41 22.6629 0.0074
6 0.0654 2.71 2793 2.04 0.33 16.9851 0.0063
7 0.0522 2.77 2877 2.03 0.36 21.2766 0.0062
8 0.0522 2.77 2626 2.06 0.34 21.2766 0.0055

Table 5
Values of Kt and Kf for several radius of curvature of the notch with C = 0.0058 mm.

r (mm) Kt v (mm1) Kf
0.0010 3.04 2000 0.69
0.0020 3.03 1000 0.89
0.0022 3.03 909 0.92
0.0024 3.03 833 0.95
0.0026 3.03 769 0.97
0.0028 3.03 714 1.00
0.0029 3.03 690 1.01
0.0030 3.03 667 1.02
0.0040 3.03 500 1.12
0.0050 3.02 400 1.20
0.0060 3.02 333 1.26
0.0070 3.02 286 1.32
0.0080 3.02 250 1.37
0.0090 3.01 222 1.41
0.0100 3.01 200 1.45
0.0120 3.00 167 1.51
0.0140 3.00 143 1.57
0.0160 2.99 125 1.61
0.0180 2.99 111 1.65
0.0200 2.98 100 1.69 Fig. 3. Comparison of the relation between the ratio Kt/Kf and factor v for Ti-6Al-4V
0.0400 2.92 50 1.90 and steels with different yield strength values (adapted from [8]).
0.0600 2.87 33 1.99
0.0800 2.81 25 2.03
0.1000 2.76 20 2.06
0.1100 2.73 18 2.06 On the other hand, the longer exposure time to acid etching for
0.1200 2.71 17 2.06 the Ti64-AE 2 sample (Fig. 4b) produced a surface having greater
0.1300 2.68 15 2.06 micro porosity when compared to Ti64-AE 0.5 sample (Fig. 4a),
0.1400 2.66 14 2.06
which is assumed to be detrimental to the performance in fatigue
0.1500 2.63 13 2.06
0.2000 2.51 10 2.02 [2,23].
0.4000 2.11 5 1.81 Average peak-to-valley roughness (Rz) obtained on surfaces of
0.6000 1.82 3 1.60 Ti64-AE 0.5 and Ti64-AE 2 samples with their standard deviation
0.8000 1.62 3 1.44
are reported in Table 6. It is noteworthy that, before HCl etching,
1.0000 1.47 2 1.33
all samples were polished until a homogenous surface was
obtained (RZ < 0.100 µm). The Ti64-AE 0.5 and Ti64-AE 2 samples
showed a significant increase of Rz during acid etching to
performed in this work is reasonable since Ti-6Al-4V has a strength 2.040 ± 0.200 µm and 9.955 ± 1.550 µm, respectively. The subse-
value comparable to 900 MPa yield strength steel, but with higher quent immersion into NaOH solution developed on both surfaces
toughness. nanoscale topography, but maintained the surface roughness gen-
erated by the previous acid etching. Fig. 5 shows the 3D topo-
graphic images.
3.2. Application to chemical etched specimens The surface modification of Ti64-AE 0.5 [3] led to a surface
roughness Rz = 2.04 µm, which may be modeled as semi-circular
Fig. 4 shows SEM images of the surface morphologies of Ti64-AE surface notches with radius r = 2 µm. As noted in Fig. 5, the longer
0.5 and Ti64-AE 2 samples, previously etched with HCl and then exposure time to acid etching resulted in a Rz value 79.5% higher
immersed in NaOH. Both samples presented a homogenous when compared to Ti64-AE 0.5 sample, meaning that the Ti64-AE
sponge-like structure on the surface (Fig. 4a and b) [17–19]. The 2 sample produced semi-circular surface notches with radius of
formation mechanisms of these structures are associated with approximately r = 10 µm. It is known that increasing the radius of
exposure of the passive TiO2 layer to NaOH solution. At first, the curvature means a reduction on the maximum stress at the notch
passive layer is partially dissolved to form HTiO3. At the same tip region, but this must be balanced with the greater volume of
time, the metallic titanium is hydrated forming HTiO3nH2O. material affected by stress concentrator, due to a higher stress field
Finally, positively charged alkali ions Na+ react with negatively gradient, which can lead to the reduction on the fatigue resistance
charged groups to produce an alkali titanate hydrogel layer [8].
[20,21]. This homogeneous bioactive sodium titanate structure The staircase diagram for the Ti64-AE 2 samples is presented in
formed on both surfaces of Ti64-AE 0.5 and Ti64-AE 2 samples is Fig. 6. According to the Kf results presented in Table 5 for a notch of
favorable for apatites precipitation [22]. approximately 10 lm and using Eq. (1), it was possible to predict
262 Paulo Sergio Carvalho Pereira da Silva et al. / International Journal of Fatigue 103 (2017) 258–263

Fig. 4. SEM image of: (a) Ti64-AE 0.5 [3] and (b) Ti64-AE 2.

Table 6
Rz measurements for Ti64-AE 0.5 and Ti64-AE 2 samples.

Sample Rz (µm)
Ti64-AE 0.5 2.04 ± 0.20 [3]
Ti64-AE 2 9.95 ± 1.55

the fatigue limit for this notch as 580 MPa. Based on this informa-
tion, a stress of 550 MPa was therefore chosen for the initial tests.
By applying the Dixon and Mood method to the resulted values
[16,24], the fatigue limit was calculated as 594 ± 74 MPa, confirm-
ing that the semi-circular notches of 10 lm caused a drop on the
fatigue resistance of around 30% when compared to the resistance
of the same alloy without chemical treatment, equal to
842 ± 27 MPa [3].
From values of r (or Rz), v, Kt and Kf, in addition to the C param-
eter previously determined for Ti-6Al-4V alloy, the application of
Eq. (1) provided the curve of theoretical rf in function of a semi-
circular notch Rz, as shown in Fig. 7. The experimental rf values Fig. 6. Plot of staircase testing results for Ti64-AE 2 with run-out of 5  106 cycles.
for Ti64-AE 0.5 and Ti64-AE 2 samples (Rz = 2 lm and 10 lm
respectively) were plotted as well. samples. On the other hand, the samples subjected in the present
Agreeing with Fig. 1, the theoretical curve in Fig. 7 reveals that, work to a more aggressive treatment (Ti64-AE 2) that led to
when the notch radius decreases, the peak stress at the notch tip Rz = 10 lm, which is larger than the critical value, produced a
increases. Nevertheless, the volume of material where the stresses higher Kf value than Ti64-AE 0.5 samples. This means that a greater
are larger than a critical value, associated to a notch, decreases volume of material is subjected to the maximum stress level.
with the notch radius to a critical value Rcr z , where Kf = 1 (Table 5). In this case, it is higher the probability of finding a worst
So, for semi-circular notches smaller than Rcr z = 2.8 lm, the volume metallurgical condition or defect ahead of the notch tip that would
of material affected by the local peak stress is not significant to make the material fail at lower stresses, resulting in an inferior
influence the fatigue resistance. In other words, the prediction fatigue strength.
method establishes that samples with roughness lower than Rcr z Based on the above discussion, it can be seen that the prediction
behave as samples without notches. This behavior was observed method is in good agreement with the experimental results. These
in the work of Escobar Claros et al. [3], where samples with results are of extreme importance for the design of load-bearing
Rz = 2 lm that resulted from acid etching and alkaline treatment implants with modified surface that are submitted to cyclic
(Ti64-AE 0.5) presented similar performance of surface polished loadings since, depending on the method employed for the surface

Fig. 5. 3D topographic image of: (a) Ti64-AE 0.5 [3] and (b) Ti64-AE 2.
 Paulo Sergio Carvalho Pereira da Silva et al. / International Journal of Fatigue 103 (2017) 258–263
Fig. 7. Plot of rf in function of Rz.
modification, the roughness scattering (i.e. notches) from the lower
to the upper level can lead to huge differences in the fatigue
response of the component and to unexpected failures in clinical
use. Therefore, according to these results, it is recommended to
know more precisely the process being used for the surface modi-
fication in regard to the variation of the roughness that can be pro-
duced in an industrial scale, and take into consideration the
changes in the Kf value and, consequently, in the design of the
component.
4. Conclusions
The discussion showed that the prediction method presented in
this work for Ti-6Al-4V ELI alloy, summarized in Table 5 and Fig. 7,
justifies the relation between the surface finishing and the fatigue
life, in case of negative influence and of no influence. As observed
in Fig. 7, a small variation of the surface roughness above the crit-
ical value may result in a large variation of the fatigue resistance,
which helps to explain the strong differences in the fatigue lives
observed by slightly changing the roughness in the low µm range
(2–10 µm). In the case of orthopedic implants, the method may
abbreviate the development stage of the project by predicting
the effect of different surface conditioning methods on the fatigue
life. In addition, it can establish more reliable safety factor for the
design of load-bearing implants supporting cyclic loadings and
help avoid catastrophic failures in clinical use.
Acknowledgements
The authors acknowledge the financial support from the Brazil-
ian institutions CAPES (scholarship PVNS 028/2013) and FAPESP
(scholarship 2016/12995-5).
263
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