Materials Today: Proceedings xxx (xxxx) xxx

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Materials Today: Proceedings

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In vitro tribological investigation and osseointegration assessment for

metallic orthopedic bioimplant materials
Sachin Solanke a, Vivek Gaval b,⇑, Sahil Sanghavi c
a
Department of General Engineering, Institute of Chemical Technology, Mumbai 400019, India
b
Faculty of General Engineering Department, Institute of Chemical Technology, Mumbai 400019, India
c
Knee and Hip Surgeon, Sancheti Institute for Orthopaedic & Rehabilitation, Pune, India

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

Article history: This research study is aimed at finding a suitable uncoated metallic biomaterial based on its wear prop-
Received 1 October 2020 erties and osseointegration ability for orthopedic implants. In the present work, wear tests were carried
Received in revised form 9 October 2020 out on uncoated metallic biomaterials such as Co-Cr-Mo, SS316L, Ti6Al4V and Titanium grade 2. The wear
Accepted 19 October 2020
tests were performed to determine friction coefficient and wear loss in the presence of simulated body
Available online xxxx
fluid having a common pH of 7.25 similar to human plasma. The wear resistance was found to be highest
for Co-Cr-Mo material followed by SS316L, Ti6Al4V and Titanium grade 2 material. To grow an apatite
Keywords:
layer, uncoated metallic substrates were immersed for two weeks in a simulated body fluid having ion
Bioimplant materials
Simulated body fluid
concentration equivalent to human blood plasma. Adhesive bonding strength of the apatite layer formed
Wear test on the different bioimplant substrates was evaluated under tensile stress. The worn metallic surfaces post
Wear loss wear tests and metallic substrates with apatite layer were analyzed using scanning electron micrographs.
Apatite layer From the results it was found that uncoated Ti6Al4V material is more suitable for orthopedic implants as
Adhesive strength compared to other materials studied in this work.
Ó 2020 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Confer-
ence on Advances in Materials Processing & Manufacturing Applications.

1. Introduction and chemical characteristic are being studied pertaining to

biomedical field. Out of this only a few biomaterials are presently
From the literature survey it is clear that in the present scenario used for orthopedic bioimplant surgery. For bone replacement the
total hip and knee arthroplasty replacement is most common most commonly used metallic biomaterial are titanium, stainless
orthopedic surgery performed throughout the world. It was steel and cobalt-chromium alloys. Metallic biomaterials for ortho-
reported in the literature that total hip and knee replacement pedic implants should have good mechanical properties such as
would increase by 175% and 674% respectively between 2005 high strength, high fracture toughness and high wear resistance.
and 2030 [1,2]. Near about five lakh and more hip and knee joint [7,8]. The wear property is important as far as metallic bioimplant
surgery replacement are being performed per year in the world functioning and performance in length of service is concerned. The
[3]. The short life span of modern artificial bioimplant joint or release of metallic debris or ions due to wear in components of
arthroplasty is major drawback in current scenario, so researchers prosthesis leads to harmful or adverse effect in the human body.
are trying to improve lifespan of artificial bioimplant joints. Gener- So high wear resistance becomes primary requirement of metallic
ation of wear debris due to articulating movement of components bioimplant materials. In recent years short life and inadequate per-
in the implanted metallic arthroplasty leads to the aseptic lessen- formance of artificial prosthesis has been associated to a phe-
ing [4]. As a result, longevity of artificial arthroplasty would nomenon called stress shielding effect [9]. The stress shielding is
decrease and becomes unstable [5]. It was reported that 75%-85% caused due to mismatch of elastic modulus between artificial
artificial prostheses were made from metal alloys [6]. Several types and natural bone. Elastic modulus of cortical bone is generally in
of orthopedic implant biomaterials and alloys with their physical the range of 15–25 GPa [10,11]. Stress shielding effect can be min-
imized by selecting metallic biomaterial with an elastic modulus
⇑ Corresponding author. similar to human natural bone [12]. Torsional stiffness and modu-
E-mail address: [email protected] (V. Gaval).
lus of elasticity of titanium alloys is comparable less than other

https://doi.org/10.1016/j.matpr.2020.10.528
2214-7853/Ó 2020 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Conference on Advances in Materials Processing & Manufacturing Applications.

Please cite this article as: S. Solanke, V. Gaval and S. Sanghavi, In vitro tribological investigation and osseointegration assessment for metallic orthopedic
bioimplant materials, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.10.528
S. Solanke, V. Gaval and S. Sanghavi Materials Today: Proceedings xxx (xxxx) xxx

metallic alloys such as SS316L and CoCrMo alloy which helps in of SS316L, TI6Al4V, Co-Cr-Mo and TIGR2 are 7.98 gm/cm3, 4.43
reducing the stress shielding of bone. Modulus of elasticity of gm/cm3, 8.3 gm/cm3 and 4.52 gm/cm3 respectively. The metallic
cobalt alloy is twice that of the titanium alloy [13–15]. Bone is a samples were polished by rough sand paper and washed ultrason-
dynamic tissue that is continually being built, broken down and ically in acetone. After that samples were dried in an oven at 75 °C
rebuilt in a process called bone remodeling. Osteoblast and osteo- for 10 h.
clasts which both have a role in bone remodeling. Osteoblasts
attachment and proliferation better on rough surface. Whereas
fibroblasts and epithelial cells prefer smoother surfaces. High sur- 2.2. In vitro wear test
face roughness values also lead to a greater coating dissolution
rate. [16,17]. From the reported data, it is clear that the wear prop- Wear ball on disk machine (DUCOM, Bangalore, India) was used
erties of metallic bioimplant materials play an important role in to study the weight wear loss of different metal samples. The pro-
the effective working of bioimplants inside the living body. The dif- cess parameters for wear test are as presented in Table 1.
ferent methodology and test arrangement has been adopted by A steel ball (counterface) of 10 mm diameter was used for wear
researchers to check the wear properties of materials. Therefore test. The wear tests were performed under a load of 5 N and 10 N,
it is necessary to study the different metallic bioimplant materials at linear velocity of 0.05 m/s and 0.1 m/s. The wear parameters are
in terms of their mechanical, tribological and biological properties. selected based on the wear conditions faced by the femoral head
It has been reported in the literature that the weight% of alloying inside the acetabular cup. The stress induced in a hip joint during
elements have significant effect on mechanical and tribological walking is in the range of 0.8–2.5 MPa [29]. Hip joint is expected to
performance of metallic bioimplants. It is reported that 4 wt% addi- withstand high frictional forces for a minimum of 20 to 25 years
tion of Mo in the Co-Cr showed good mechanical and wear charac- [30]. Since wear experiments cannot be continued for such a long
teristics as compared to 1 wt%, 2 wt ℅ and 3 wt ℅ addition of Mo period, the applied normal load during the test is kept at a high
[18]. The addition of 2 wt% of tungsten (W) in recently developed value of 5 N and 10 N so as to obtain significant wear loss data.
Co- 30 Cr- 4 Mo- 1Ni alloy exhibited better corrosion behavior The wear test was carried out as per procedure given in ASTM G-
and biological response [19,20]. Recently it was investigated that 99 standard [31] for determining the wear of materials during slid-
performance of ceramic hip implant was influenced by the varying ing using ball on disk apparatus. Three repeat experiments were
wt ℅ of silicon nitride. The improvement in physical, mechanical performed and average value of three tests was considered.
and wear properties were observed for 2.5 wt ℅ silicon nitride
as compared to 5 wt% and 7.5 wt ℅ of silicon nitride [21].
Biocompatibility and osseointegration are the important and 3. Results and discussions (in vitro wear test)
unique properties of metallic biomaterials. When metallic bioma-
terials are implanted into the human body they always show The value of mean COF was obtained from the wear test data
non-toxic and nonallergic reactions. For effective osseointegration, recorded in the form of an excel sheet file from the WINDUCOM
an essential prerequisite for a successful metallic orthopedic 2010 machine software. The values of the COF are plotted as a
bioimplant is the formation of new bone on its surface [22]. function of sliding distance as shown in Fig. 1. The result demon-
Immersing of metal sample in simulated body fluid (SBF) in vitro strates highest COF value for SS316L substrate and lowest COF
study is very useful for evaluating the biocompatibility and tissue value for Co-Cr-Mo substrate. The wear test result demonstrate
response of metallic biomaterials. This helps in reducing the num- that the value of wear loss for the different substrates did not
ber of living animals and the long span of living animal experi- change perceptibly with the increase in load and siding distance.
ments [23]. The bioactivity of material is related to its strength The less wear loss and COF of the C0-Cr-Mo alloy is by virtue of
to produce the apatite layer on the metallic surface immersed in its higher hardness (315 HV) and wear resistance characteristics.
SBF. Apatite formation is an essential requirement to check the The hardness of different metal substrates such as Co-Cr-Mo,
bone-bonding strength ability of artificial metallic bioimplant TIGR5, TIGR2, SS316L is 470 HV, 315 HV, 209 HV and 203 HV
material [24–26]. SBF is used for examining the apatite formation respectively [32]. The higher wear rate and moderate COF of the
on the surface of artificial bioimplant material. The apatite forming Ti6Al4V and TGR2 substrates may be due to its low shear strength
ability on the metallic surface is evaluated by immersing it in SBF. and hexagonal closed packed structure. Table 2 shows wear resis-
SBF was innovated by kokubo et al. whose ion concentration/inor- tance offered by various substrates under SBF condition.
ganic similar to the human plasma blood [27,28]. From the results it is observed that the weight loss increases
The aim of this study is to investigate the tribological and marginally with increase in applied normal load and sliding veloc-
osseointegration characteristics of the most commonly used ity. With the increase in these parameters, the temperature
metallic biomaterials such as SS316L, TI6Al4V, Co-Cr-Mo and Tita- between the substrate material and indenter increases resulting
nium grade 2 (TGR2) under in vitro condition. In the present study in oxidation of metal substrates due to low thermal conductivity
all these metallic biomaterials have been tested for wear properties of these alloy materials. This oxidized surface of substrate material
as per ASTM G-99 standard and bonding/ adhesive strength of the becomes stable to some extent reducing the weight loss [33]. The
apatite layer was examined which was formed on the surface of formation of oxide islands during sliding contact at some locations
metal samples when immersed in SBF. is evident from SEM micrographs. This oxidized surface gets frag-
mented or becomes stable to some extent. The formed fragmented
oxide layer or particles sometimes acts as lubricating agent and
2. Materials and method thus reduces weight loss. The formation of metal oxide was
observed at more location in SS316L sample as evident from SEM
2.1. Preparation of samples micrograph. This has resulted in less wear loss in SS316L as com-
pared to Ti6Al4V and TGR2 sample. This is attributed to low ther-
Metallic raw materials such as SS316L, TI6Al4V, Co-Cr-Mo and mal conductivity among other substrates and the same pairing of
TIGR2 were procured in solid form from the Belmount Industrial material physical characteristic between substrate and indenter
Solutions, Mumbai. The samples with a size of 40 mm diameter [34,35]. Also in SS316L substrate wear test, contact surface of the
and 6 mm thickness were prepared for in vitro wear test using counterface/ indenter used in testing was observed more markedly
laser technology at Dalvi Engineering Works, Mumbai. Densities darkened as compared to other metallic substrates wear test. From
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S. Solanke, V. Gaval and S. Sanghavi Materials Today: Proceedings xxx (xxxx) xxx

Table 1
Process parameter as per ASTM standard for ball on disk wear test.

Substrate sample Sliding velocity (m/s) Applied normal load (N) Sliding distance (m) Radial Track diameter (mm)
Co-Cr-Mo, SS316L, Ti6Al4V, TGR2 0.05 m/s, 0.1 m/s 5 N, 10 N 200 m 30 mm

Fig. 1. (a) Graph illustrating the variations in COF vs. Sliding distance under 5 N and 0.05 m/s; (b) Graph illustrating the variations in COF vs. Sliding distance under 10 N load
and 0.1 m/s.

Table 2
Wear weight loss (Gram) and mean coefficient of Friction.

Substrate sample Average Wear weight loss (for 5 N and 0.05 m/s) Average Mean coefficient of Friction
Co-Cr-Mo 0.0020 0.35
SS316L 0.0038 0.59
Ti6Al4V 0.0055 0,41
TGR2 0.0069 0.49
Substrate sample Average Wear weight loss (for 10 N and 0.1 m/s) Average Mean coefficient of Friction
Co-Cr-Mo 0.0021 0.37
SS316L 0.0035 0.62
Ti6Al4V 0.0059 0.44
TGR2 0.0073 0.47

literature, it was found that in titanium alloy at higher load and were washed gently with pure acetone and dried on a clean bench.
sliding distance there was formation of oxide islands or layers [36]. After, the samples were taken out for surface morphology charac-
terization using SEM. Comparison of human blood plasma and SBF
3.1. SEM characterization for wear tested specimen ion concentrations is as shown in Table 3.
The apatite formation was lead up by presence of calcium and
SEM images were taken at MMMF lab, IIT Bombay (Carls Zeiss phosphate ions in the SBF adsorbed on the surfaces of samples.
Microscopy Ltd. Cambridge CB 1 3JS, United Kingdom). More visi- After immersing for some time, calcium and phosphate ions gets
ble ridging of the wear traces was observed in Ti6Al4V and TGR2 attracted towards the metallic surface to form the apatite crystals.
material which may be attributed to the presence of b phase in Once the apatite crystals or nuclei are formed, they spontaneously
the material leading to increase in localized plastic deformation grow by consuming the calcium and phosphate ions from the sur-
[37]. The dominant mechanism of wear includes the ridging and rounding SBF in the conical flask. Tiny leaf like apatite crystals
abrasion. In addition, the traces of wear characterized by chipping, were observed after initial soaking of 1 or 2 days. After few more
crack (microcrack) and delamination were observed showing days a prominent increase in the number of crystalline nuclei
adhesive and abrasive wear (Fig. 2). was observed. After prolonged immersion whole surface was cov-
ered with apatite layer without leaf like crystals due to increase of
4. Result and discussion (in vitro apatite formation and Ca and P ion concentration. Apatite crystal length was measured
adhesive strength measurement) after formation of dense structure of apatite precipitate in two
weeks. Majority of the apatite crystals have a length of 20–25 nm
4.1. In vitro apatite formation after 14 days of soaking. No significant difference was observed
in the apatite layer thickness formed on the surfaces of different
For in vitro apatite layer formation, prepared bioimplant metal- metallic samples. Almost same apparent reaction rate for apatite
lic samples were immersed in conical flask containing 200 mL of formation was observed in different metallic samples. Approxi-
SBF (Kelkar Scientific Research Centre, Mumbai). The conical flask mately 8 lm to 9 lm thick apatite layer was formed on one side
was then kept in constant temperature (37 °C) water bath for of the uncoated metallic samples after soaking in SBF for 14 days.
14 days. After soaking for two weeks, different metallic substrates This apatite layer have the similar chemical composition and

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S. Solanke, V. Gaval and S. Sanghavi Materials Today: Proceedings xxx (xxxx) xxx

Fig. 2. SEM Images of worn surfaces such as Co-Cr-Mo, Ti6Al4V, SS316L and TGR2.

Table 3
Comparison of human blood plasma and SBF ion concentrations (mmol/L).

Sample Na+ K+ Ca2+ Mg2+ HCO3 Cl- HPO2-

4 SO24
Blood plasma (Human) 142 5 2.5 1.5 27 103 1 0.5
SBF 142 5 2.5 1.5 4.2 147.8 1 0.5

structure to the natural apatite in the bone [38]. Based on apatite 4.2. Measurement of bonding/adhesive strength
crystals length measurement and observation from SEM images,
it can be concluded that there was no preferred environment and The adhesive strengths between the formed apatite layer and
crystallographic orientation for apatite nucleation on different different metallic samples were checked/ examined at Kelkar
uncoated metallic substrates. The SEM images of apatite layer for- Scientific Research Centre, Mumbai. Researchers have developed
mation on the surfaces of different uncoated metallic surfaces are several methods for evaluating the adhesive strength of coating-
as shown in Fig. 3. substrate interface. The most commonly used methods are

Fig. 3. SEM images of different surfaces of the metallic substrates Co-Cr-Mo, Ti6Al4V, SS316L and TGR2 soaked in SBF for 14 days.

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S. Solanke, V. Gaval and S. Sanghavi Materials Today: Proceedings xxx (xxxx) xxx

Table 4
Adhesive strength at the interface between apatite- uncoated metallic samples.

Test Sr. No. Substrate Material Failure Adhesive load (N) Adhesive Strength (Mpa) Avg. Adhesive Strength (Mpa)
1 SS316L 13 0.01034 0.010
2 SS316L 13.2 0.01059
3 SS316L 13.3 0.01058
4 Ti6Al4V 15.4 0.01225 0.012
5 Ti6Al4V 15.8 0.01257
6 Ti6Al4V 15.6 0.01241
7 Co-Cr-Mo 13.7 0.01090 0.010
8 Co-Cr-Mo 13.8 0.01098
9 Co-Cr-Mo 13.7 0.01090
10 TGR2 14.5 0.01153 0.011
11 TGR2 14.7 0.01169
12 TGR2 14.9 0.01185

Fig. 4. Arrangement for measurement of adhesive strength between metallic substrate and formed apatite layer.

indentation test, shear test, ASTM F 1147, ISO 14916, EN 582 and adsorbs the negative charged phosphate ions on Ti substrate sur-
tensile adhesive strength like ASTM C633. In the current study face. The surface of Ti alloys becomes negatively charge due to
the adhesive strengths of apatite layer to metallic samples was accumulation of phosphate ions from SBF. After it combines with
found out by using ASTM C- 633 method [39]. This method is positive charged calcium ions resulting in formation calcium phos-
selected owing to its simplicity and good efficiency. Tensile stress phate which transforms into stable crystalline nuclei or apatite.
was applied to the different metallic samples at crosshead speed of Although Ti6Al4V and TGR2 possess friendly advantages from
1 mm/min until fracture occurred. The sample with apatite layer the viewpoints of biomedical requirements such as close elastics
on one side was fixed between the two cylindrical stainless steel modulus to natural bone, high strength to weight ratio, enhanced
jigs using Araldite glue. The testing set up is as shown in Fig. 3. biocompatibility and osseointegration. These specific properties
Tensile load was applied normally to metallic samples until frac- play an important role in longevity of artificial bioimplant material.
ture occurred generally at apatite- metal sample interface. Tensile However, considering all these specific properties use of TI6Al4V
load was then gradually increased from zero to the then load of and TGR 2 substrate materials is recommended. To induce bioac-
failure. The adhesive strength is ratio of load of failure to failure tivity and osseointegration of metallic materials, hydroxyapatite
area. The ultimate load that has been applied to the different (HA) modified ceramics provide an alternate solution of long term
metallic samples was then recorded. This method is not recom- fixation. Stable fixation of the implant to bone decide the long-
mended for high temperature application due to its limitation term success of joint replacement. HA has the same chemical and
relating to the strength of adhesive bonding agent. Fig. 4 depicts crystallographic structure as the living bone structure. The pres-
schematic arrangement for measurement of adhesive strength ence of calcium and phosphate ions at the HA surface creates the
between metallic substrate and formed apatite layer (Table 4). bioactive surrounding with living bone. Few research studies
In adhesive strength test, three measurements were recorded reported that sintered apatite form very tight adhesive bond with
for each metallic substrates and average value of adhesive/bonding living bone and avoid the significant biodegradation.
strength was considered. Under tensile stress, the fracture
occurred at the interface between the metallic substrate and the
formed apatite layer. The computed adhesive strengths between 5. Conclusion
the formed apatite layer and uncoated metallic samples was found
to be in the range of 0.010 to 0.012 Mpa. These results reveals that 1. The wear loss in Ti6Al4V material is not significantly higher as
the apatite layer formed on different metal surfaces may be loosely compared to other metallic biomaterials in this study. Because
bonded. The results shows that the adhesive strength of titanium of less density of Ti6Al4V and higher adhesive strength of apa-
alloys is marginally more as compared to other substrates. This tite layer, uncoated Ti6Al4V is found to be more suitable metal-
may be due to specific crystalline phase and positive surface lic biomaterial for orthopedic implants.
charge, positively charged titanium oxide on titanium metal alloys 2. From the SEM micrograph, it is evident that the dominant wear
forms apatite layer on its surface in the vitro environment [40]. mechanisms were adhesive and abrasive for all metallic sub-
This positively charged titanium oxide of Ti alloys first selectively strates. In addition, for Ti6Al4V and TGR2 the dominant mech-

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S. Solanke, V. Gaval and S. Sanghavi Materials Today: Proceedings xxx (xxxx) xxx

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