A Review On Plasma Sprayed Titanium and Hydroxyapatite Coatings On Polyetheretherketone Implants

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A review on plasma sprayed titanium and hydroxyapatite

coatings on polyetheretherketone implants
Article in International Journal of Surface Science and Engineering · January 2019

DOI: 10.1504/IJSURFSE.2019.103923
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Int. J. Surface Science and Engineering, Vol. 13, No. 4, 2019 237
A review on plasma sprayed titanium and

hydroxyapatite coatings on polyetheretherketone
implants
Ali Tekin Guner* and Cemal Meran

Faculty of Technology,
Pamukkale University,
Denizli, 20160, Turkey
Email: alitekinguner@pau.edu.tr
Email: cmeran@pau.edu.tr
*Corresponding author
Abstract: Polyetheretherketone (PEEK) is a biocompatible polymer with good

mechanical strength, thermal and chemical stability and is suitable for magnetic
resonance and X-ray imaging. Moreover, density and elasticity of PEEK is
closer to bones compared to metals. Nevertheless, the hydrophobicity of the
PEEK surface causes a soft tissue formation at the bone/implant interface that
prevents direct bone apposition. Although numerous methods have been
developed for improving PEEK’s bioactivity, the most widely used and
accepted method have been coating the surface with a thin layer of
osseointegrative material by thermal spraying. Most widely used coating
materials in the manufacture of orthopaedic implants have been hydroxyapatite
(HAp) and titanium. Thus, this review focuses on the recent progress on HAp
and Ti coatings deposited by plasma spraying methods on PEEK implants.
Keywords: plasma spray; coating; polyetheretherketone; PEEK;

hydroxyapatite; HAp; titanium.
Reference to this paper should be made as follows: Guner, A.T. and Meran, C.
(2019) ‘A review on plasma sprayed titanium and hydroxyapatite coatings on
polyetheretherketone implants’, Int. J. Surface Science and Engineering,
Vol. 13, No. 4, pp.237–262.
Biographical notes: Ali Tekin Guner has been working as a Research

Assistant at the Pamukkale University, Faculty of Technology, Department of
Biomedical Engineering in Turkey since 2013. He has completed his MSc in
Mechanical Engineering from the Pamukkale University in 2013 and he is
pursuing his PhD in Mechanical Engineering at the same university. His current
research fields are thermal spray coatings and biomaterials used in orthopaedic
implants.
Cemal Meran holds a PhD in Mechanical Engineering from the Pamukkale

University, Turkey. He carried out all experiments of his PhD study at the
Fachochschule Regensburg in Germany. Then he took an academic position
at the Pamukkale University in 2002-present. He was promoted to Professor
of Mechanical Engineering in 2013. He also carries administrative
responsibilities including Manager of the Center of Materials Research and
Application of Pamukkale University since 2009. He has organised several
conferences, symposiums and academic activities. He is the Chair of the
International Materials Symposium (IMSP) which is held every two years at
Copyright © 2019 Inderscience Enterprises Ltd.

238 A.T. Guner and C. Meran
the Pamukkale University. He has authored numerous peer-reviewed scientific

journal and conference papers and has presented in around 40 national and
international symposiums and congresses in mechanical engineering and
materials engineering fields.
1 Introduction
Biomaterial can be defined as a material designed for the development, treatment or

replacement of a tissue, organ or body function. Implant is a medical device made of
biomaterials that is deliberately placed into the body, completely or partially under the
epithelium surface (Williams, 2011). The transition of biomaterials from lab to clinical
applications requires a long and meticulous procedure, starting from the synthesis of the
materials to design, production and clinical testing of the implants (Sukaryo et al., 2016).
In orthopaedics, biomaterials are used to stabilise the fractured bones or joints by a
trauma or to replace the joints or bones that are degenerated by a disease such as
osteoporosis (Mahyudin et al., 2016). While most of them are metals (e.g., titanium,
cobalt-chrome and stainless-steel alloys), most used non-metallic materials can be
divided into three as ceramics (e.g., alumina, zirconia, CaP-based ceramics and bioactive
glasses), polymers [e.g., polyethylene, polyetheretherketone (PEEK), acrylic bone
cements] and composites (e.g., carbon fibre or glass fibre reinforced polymers) (Niinomi,
2002; Elias et al., 2008; Chen and Thouas, 2015; Mahyudin et al., 2016; Lin et al., 2017).
There are some basic properties that are required in biomaterials to be used in the
manufacture of orthopaedic implants. These are mechanical properties (tensile,
compression, bending, fatigue, abrasion resistance, elasticity, etc.) and chemical
properties (corrosion resistance, solubility or insolubility etc.) that are well known for
engineers and properties like biocompatibility, bioinertness, bioactivity which are of
interest to medical and biological sciences.
Bioactive ceramics provide a very high biocompatibility and rapid recovery, but they
are also very hard and brittle to limit their usage. Metals and polymers have superior
mechanical properties, but the common disadvantage of these materials is the lack of
bioactivity. Metallic and polymeric materials used in orthopaedic implants cannot form
chemical bonds with human bones. When a cementless prosthesis is implanted in human
bone, initial mechanical stability is provided by an interference fit. But the strength of
this fixation decreases with time as the crushed necrotic bone is removed around the
implant. For this reason, the long-term fixation of the implant highly relies on the rapid
formation of the new bone (Furlong and Osborn, 1991; Junker et al., 2009; Goriainov
et al., 2014). HAp, a ceramic with a chemical composition that is very similar to the
mineral content of human bone, has exceptional biocompatibility and with bioactive
properties like osteoconductivity and osteoinductivity (Mahyudin et al., 2016b; Szcześ
et al., 2017; Tang et al., 2018). However, the strength and fracture toughness of HAp are
not enough to replace load bearing skeletal system components. To overcome this
disadvantage, HAp is generally used as a thin coating on other substrate materials in
orthopaedic implants (Junker et al., 2009; Mediaswanti et al., 2014; Xiao et al., 2017;
Harun et al., 2018). The purposes of coating orthopaedic implants are to be able to fix the
implant without using additional bone cement or screws, reduce post-operative hospital
A review on plasma sprayed titanium and hydroxyapatite coatings 239
stay, increase biointegration, stimulate bone ingrowth, prevent allergic reactions and
consequently prolong the life of the prosthesis (Espallargas, 2015).
Various methods have been developed for HAp coatings including thermal spraying
[plasma spraying (Levingstone et al., 2015; Heimann, 2016; Xu et al., 2016; Harun et al.,
2018; Gkomoza et al., 2019), flame spraying (Yang et al., 2017; Mardali et al., 2019),
high velocity oxy-fuel spraying (Bolelli et al., 2007a, 2007b; Mardali et al., 2019),
detonation gun spraying (Gledhill et al., 1999, 2001; Sapra et al., 2008) and so on],
sputter deposition (Mediaswanti et al., 2014; Vladescu et al., 2016; Ozeki et al., 2017;
Surmenev et al., 2017; Qadir et al., 2019), pulsed laser deposition (Koch et al., 2007;
Pereiro et al., 2012; Duta et al., 2013; Rajesh et al., 2013; Popescu-Pelin et al., 2017;
Hidalgo-Robatto et al., 2018; Rau et al., 2018), ion-beam assisted deposition (Choi et al.,
2000; Hamdi and Ide-Ektessabi, 2003; Cotrut et al., 2018) dip coating (Khalid et al.,
2013; Javadi et al., 2019), sol-gel coating (Asri et al., 2016; Javadi et al., 2019),
electrophoretic deposition (Manoj Kumar et al., 2016; Farrokhi-Rad, 2017, 2018;
Farrokhi-Rad et al., 2017; Göncü et al., 2017; Baştan et al., 2018; Patel et al., 2019;
Pawlik et al., 2019) and hot isostatic pressing (Onoki and Hashida, 2006; Harun et al.,
2018). Among them, atmospheric plasma spraying (APS) has been the most frequently
used and commercially accepted method of HAp coatings on orthopaedic implants
(Surmenev, 2012; Levingstone et al., 2015; Heimann, 2016, 2017).
PEEK is an organic thermoplastic polymer in the polyaryletherketone (PAEK) family
introduced in the early 1980s. As a biomaterial approved for use in implants, PEEK was
first offered commercially in 1998 by Invibio Ltd., a member of the Victrex Group (Kurtz
and Devine, 2007). There have been a large number of studies reporting the successful
clinical performance of PEEK polymers to date (Williams et al., 1987; Brantigan et al.,
2000; Glassman et al., 2001; Kärrholm et al., 2002; Brantigan et al., 2004; Akhavan
et al., 2006; Toth et al., 2006; Panayotov et al., 2016). PEEK has superior mechanical
properties and thermal stability compared to most of the polymeric biomaterials, has high
chemical stability, is non-magnetic and thus is suitable for magnetic resonance imaging
(MRI) and it does not create shadows in X-ray imaging as it is radiolucent. Moreover,
density and elasticity of PEEK is closer to that of the human bones compared to metals
thus it has the potential to prevent stress-shielding and bone resorption around the
implant (Kurtz and Devine, 2007; Kurtz, 2012; Anguiano-Sanchez et al., 2016;
Panayotov et al., 2016). PEEK is used in orthopaedic applications such as fracture
fixation plates, screws, total joint replacement prosthesis parts and spinal implants. It can
be used in neat form, as well as with reinforcements like carbon fibre to increase strength
or bioactive additives or coatings such as HAp. CFR-PEEK materials have been
recommended for use as an alternative material to metals in femoral stems to eliminate
the stress shielding effect and has also been suggested as an alternative to ultra-high
molecular weight polyethylene (UHMWPE) for use in the acetabular socket of total hip
arthroplasty to provide higher wear resistance (Davim and Marques, 2001).
The hydrophobic surface of PEEK causes a fibrous tissue formation at the
bone/implant interface that prevents bone apposition (Almasi et al., 2016). To prevent
this tissue response numerous studies have been done on osteoinductive and
osteoconductive coatings of HAp and porous Ti on PEEK implants. This review focuses
on recent progress on HAp and Ti coatings deposited by plasma spraying methods on
PEEK substrates.
2 Plasma spray deposition technology
The first thermal spray coatings were produced with oxy-acetylene torches modified for
powder and wire feed in the early 1900s, and since then thermal spray coating technology
has been rapidly developed with improvements in raw materials, equipment and
application methods (Sampath, 2009; Malek et al., 2014). Today thermal spray
technology is widely used in many specialised industries such as biocompatible coatings
of surgical implants. In biomedical applications, surface modification is of great
importance to establish a stable integration of biomaterials into the living tissue. Since the
1990s, plasma spray deposition of biocompatible materials such as HAp, TiO2, Ti on
CoCr, Ti alloy and stainless steel joint replacement prosthesis parts is a well-known and
clinically accepted method (Driver, 2012; Espallargas, 2015). In thermal spray coating
processes, the coating material in the form of a solid rod, wire or powder fed to the spray
gun is heated to the melt or the semi-melt temperature and accelerated through to the
surface to be coated as shown in Figure 1. The molten/semi-molten particles are
deformed in so called ‘splat’ form by the effect of heat and kinetic energy during the
collusion and the building-up of successive droplets form a laminated coating on the
surface. First, they are locked with the roughened surface to be coated and then with each
other. Gaps may occur in the coating if air is trapped in between, underheated solid
particles may remain in the coating and overheated particles can be oxidised in the spray
jet (Davis, 2004; Pawlowski, 2008; Fauchais et al., 2014; Espallargas, 2015).
Figure 1 The basic operating principle of thermal spray coatings (see online version for colours)
In the plasma spray method, the plasma arc spray torch contains a tubular copper anode
and a tungsten cathode, and generally these two electrodes are cooled with water. Gases
heated with a high current arc between these electrodes are ionised into plasma state and
powdered coating material is sent into this plasma jet (Figure 2). This method is used
in heat-resistant coatings with high melting temperatures (ceramic, carbide, high
temperature alloys), wear resistant coatings, electrical and thermal insulation coatings and
biocompatible coatings for surgical implants. Almost all coating materials that will not
degenerate in plasma temperatures (reaching to ~20,000 K) can be used with this method.
It has the advantages of high coating density, high adhesion strength, low heat transfer to
the coating surface. High investment costs and large equipment requirements are the
disadvantages of this method. On the other hand, vacuum plasma spraying (VPS) method
is applied in a chamber that is vacuumed and filled with inert gas at a very low pressure.
Higher gas velocities are achieved as the plasma diameter and length are larger under low
pressure. This results in high density, high adhesion strength and low oxide content.
Disadvantages of the method are high heat transfer to the substrate, expensive equipment,
and impossibility of manual application (Davis, 2004; Driver, 2012; Fauchais et al., 2014;
Espallargas, 2015).
Figure 2 The basic operating principle of plasma spray process (see online version for colours)
3 Validation of the coatings, guidelines and requirements
Metallic and ceramic plasma spray coatings for orthopaedic implants are subject to
various international standards and guidelines. These standards and guidelines explain the
characterisation of the materials to be coated, the details of the coating process, the
characterisation of the coating and the testing methods of the coating properties as
detailed below. The two most commonly used materials that have a successful history of
clinical testing for plasma spray coatings of orthopaedic implants are Ti and HAp. These
standards and guides have been developed primarily for coatings applied to metallic
substrates but can also be used for plasma sprayed Ti and HAp coatings on polymeric
substrates such as PEEK.
3.1 Requirements for plasma sprayed Ti coatings on surgical implants

The required properties of Ti powder to be used as a raw material for the coating of
surgical implants are described in the ASTM F1580 standard specification for titanium
and titanium-6 aluminum-4 vanadium alloy powders for coatings of surgical implants
(ASTM, 2012). The requirements of Ti coatings applied to orthopaedic implants are
specified by ISO 13179-1 standard implants for surgery – plasma-sprayed unalloyed

titanium coatings on metallic surgical implants (ISO, 2014) and food and drug
administration (FDA) centre for devices and radiological health’s (CDRH) guidance
document guidance for industry on the testing of metallic plasma sprayed coatings on
orthopaedic implants to support reconsideration of postmarket surveillance requirements
(CDRH, 2000). Based on these guidelines and specifications, the following properties of
plasma sprayed Ti coatings on PEEK substrates must be determined in order to assess the
reliability of the coatings:
• chemical properties of substrate and coating material such as composition and trace
element amounts
• microstructural properties of the substrate and the coating such as grain size, phase
ratios, porosity etc.
• roughness and thickness of the coated surface
• static tensile, static shear and fatigue shear strength of the coating
• abrasion resistance of the coating.
These tests and analyses shall be carried out in accordance with procedures described in
the following ASTM and ISO standards in order to obtain comparable and viable results:
• ASTM F1147 standard test method for tension testing of calcium phosphate and
metallic coatings (ASTM, 2017b)
• ASTM F1044 standard test method for shear testing of calcium phosphate coatings
and metallic coatings (ASTM, 2017a)
• ASTM F1160 standard test method for shear and bending fatigue testing of calcium
phosphate and metallic medical and composite calcium phosphate/metallic coatings
(ASTM, 2017c)
• ASTM F1978 standard test method for measuring abrasion resistance of metallic
thermal spray coatings by using the Taber Abraser (ASTM, 2018)
• ASTM F1854 standard test method for stereological evaluation of porous coatings
on medical implants (ASTM, 2015)
• ASTM E2371 standard test method for analysis of titanium and titanium alloys by
direct current plasma and inductively coupled plasma atomic emission spectrometry
(performance-based test methodology) (ASTM, 2013)
• ISO 9220 metallic and related coatings: scanning electron microscope method for
measurement of local thickness of coating by examination of cross sections
(ISO, 1988)
• ISO 4287 geometrical product specifications (GPS) – surface texture: profile method
– terms, definitions and surface texture parameters (ISO, 1997).
The mechanical properties of Ti coatings should be tested according to international
standards and fulfil the requirements in regulations shown in Table 1. Required chemical
properties of Ti coatings according to ISO standards are listed in Table 2.
Table 1 Required mechanical properties of plasma sprayed Ti coatings on surgical implants
Properties Test methods Specifications Requirements

Tensile adhesion ASTM F1147 ISO 13179-1 (ISO, 2014), >22 MPa
strength (ASTM, 2017b) FDA guidance (CDRH, 2000) (CDRH, 2000; ISO, 2014)
Shear adhesion ASTM F1044 ISO 13179-1 (ISO, 2014), >20 MPa
strength (ASTM, 2017a) FDA guidance (CDRH, 2000) (CDRH, 2000; ISO, 2014)
Shear fatigue ASTM F1160 ISO 13179-1 (ISO, 2014) >10 MPa @ 107 cycles
strength (ASTM, 2017c) (ISO, 2014)
Abrasion ASTM F1978 ISO 13179-1 (ISO, 2014), Mass loss < 65 mg @
resistance (ASTM, 2018) FDA guidance (CDRH, 2000) 100 cycles
(CDRH, 2000; ISO, 2014)
Table 2 Chemical composition requirements of plasma sprayed Ti coatings on surgical

implants
Requirements
Elements Test methods Specifications
(mass fraction)
Carbon (C) ASTM E2371 ISO 13179-1 (ISO, 2014) ≤0.10% (ISO, 2014)
(ASTM, 2013)
Hydrogen (H) Shall be determined ISO 13179-1 (ISO, 2014) ≤0.20% (ISO, 2014)
Iron (Fe) by combustion using ISO 13179-1 (ISO, 2014) ≤0.60% (ISO, 2014)
a recognised
Nitrogen (N) validated method ISO 13179-1 (ISO, 2014) ≤5.00% (ISO, 2014)
Oxygen (O) (ISO, 2014). ISO 13179-1 (ISO, 2014) ≤10% (ISO, 2014)
The sum of N, ISO 13179-1 (ISO, 2014) ≤10% (ISO, 2014)
O, H, C and Fe
Titanium (Ti) ISO 13179-1 (ISO, 2014) Balance
3.2 Requirements for plasma sprayed hydroxyapatite (HAp) coatings on

surgical implants
Apatites are a group of minerals with hexagonal crystal system and general empirical
formulas as Ca10(PO4)6X2. In the case of HAp X is replaced by OH → Ca10(PO4)6(OH)2.
HAp, also known as hydroxylapatite, is very similar to the mineral structure of both
human bones and tooth enamel (biocompatible) and promotes new bone formation on the
surface by osteoblast cells (bioactive). Pure crystalline HAp is little or no soluble in the
body. While the crystallinity of HAp is the most important factor that affects the
formation of bone tissue and dissolution rate of the coating within the body, other factors
affecting bone formation are microstructure of the powder, phase composition and
surface topography of the coating (Espallargas, 2015). The required properties of HAp
powder to be used as a raw material for the coating of surgical implants are described in
the ASTM F1185 standard specification for composition of hydroxylapatite for surgical
implants (ASTM, 2014a) and ISO 13779-6 implants for surgery – hydroxyapatite –
part 6: powders (ISO, 2015).
The properties needed to be obtained in HAp coatings on orthopaedic implants are
defined by ASTM F1609 standard specification for calcium phosphate coatings for
implantable materials (ASTM, 2014b), ISO 13779-2 implants for surgery –
hydroxyapatite – part 2: coatings of hydroxyapatite (ISO, 2008a) and FDA guidance
510(K) information needed for hydroxyapatite coated orthopaedic implants (FDA, 1997).
Based on these guidelines and specifications, the following properties of HAp coatings
must be determined in order to assess the reliability of the coatings:
• chemical composition of the raw powder and the coating
• phase composition and crystallinity of the raw powder and the coating
• the tensile and shear strength of the coating
• thickness and porosity amount of the coating
• the size of the powder
• the solubility products and dissolution rate of the raw powder and the coating
• X-ray diffraction patterns of the raw powder and the coating.
Infrared spectroscopy of the raw powder and the coating. Tests of these properties shall
be carried out in accordance with procedures described in the following ASTM and ISO
standards in order to obtain comparable and viable results:
• ISO 13779-2 implants for surgery – hydroxyapatite – part 2: coatings of
hydroxyapatite (ISO, 2008a)
• ISO 13779-3 hydroxyapatite – part 3: chemical analysis and characterisation of
crystallinity and phase purity (ISO, 2008b)
• ISO 13779-4 implants for surgery – hydroxyapatite – part 4: determination of
coating adhesion strength (ISO, 2002)
• ASTM F1147 standard test method for tension testing of calcium phosphate and
metallic coatings (ASTM, 2017b)
• ASTM F1044 standard test method for shear testing of calcium phosphate coatings
and metallic coatings (ASTM, 2017a)
• ASTM F2024 standard practice for X-ray diffraction determination of phase content
of plasma-sprayed hydroxyapatite coatings (ASTM, 2016)
• ASTM F1854 standard test method for stereological evaluation of porous coatings
on medical implants (ASTM, 2015)
• ASTM F1926 standard test method for dissolution testing of calcium phosphate
granules, fabricated forms, and coatings (ASTM, 2014c).
The mechanical properties of HAp coatings should be tested according to international
standards and fulfil the requirements in the regulations shown in Table 3.
Required chemical properties of HAp coatings and test methods used for
determination of these properties according to international standards are listed in
Table 4.
Table 3 Required mechanical properties of plasma sprayed HAp coatings on surgical implants
and test methods used for determination of these properties

Tensile adhesion ISO 13779-4 ISO 13779-2 ≥ 15 MPa
strength (ISO, 2002), ASTM (ISO, 2008a), ASTM (ISO, 2008a)
F1147 (ASTM, 2017b) F1609 (ASTM, 2014b)
Shear adhesion ASTM F1044 ASTM F1609 -
strength (ASTM, 2017a) (ASTM, 2014b)
Shear and bending ASTM F1160 ASTM F1609 -
fatigue strength (ASTM, 2017c) (ASTM, 2014b)
Table 4 Chemical requirements of plasma sprayed HAp coatings on surgical implants and test
methods used for determination of these properties

Arsenic (As) ISO 13779-3 ISO 13779-2 ≤3 mg/kg
(ISO, 2008b) (ISO, 2008a), ASTM (ISO, 2008a;
F1609 (ASTM, 2014b) ASTM, 2014b)
Cadmium (Cd) ISO 13779-3 ISO 13779-2 ≤5 mg/kg
F1609 (ASTM, 2014b) ASTM, 2014b)
Mercury (Hg) ISO 13779-3 ISO 13779-2 ≤5 mg/kg
F1609 (ASTM, 2014b) ASTM, 2014b)
Lead (Pb) ISO 13779-3 ISO 13779-2 ≤30 mg/kg
F1609 (ASTM, 2014b) ASTM, 2014b)
Total harmful metals ISO 13779-3 ISO 13779-2 ≤50 mg/kg
F1609 (ASTM, 2014b) ASTM, 2014b)
Ca/P atomic ratio ISO 13779-3 (ISO, ISO 13779-2 1.67–1.76
2008b) (ISO, 2008a), ASTM (ISO, 2008a)
F1609 (ASTM, 2014b)
HAp mass fraction ISO 13779-3 ISO 13779-2 ≥50%
(ISO, 2008b), ASTM (ISO, 2008a), ASTM (ISO, 2008a)
F2024 (ASTM, 2016) F1609 (ASTM, 2014b)
α-TCP, β-TCP, ISO 13779-3 ISO 13779-2 ≤5% (ISO, 2008a)
TTCP and CaO mass (ISO, 2008b), ASTM (ISO, 2008a), ASTM
fraction1 F2024 (ASTM, 2016) F1609 (ASTM, 2014b)
Crystallinity ratio ISO 13779-3 ISO 13779-2 ≥45%
(ISO, 2008b), ASTM (ISO, 2008a), ASTM (ISO, 2008a)
F2024 (ASTM, 2016) F1609 (ASTM, 2014b)
Notes: 1α-TCP: α-tricalcium phosphate, β-TCP: β-tricalcium phosphate,
TTCP: tetracalcium phosphate.
4 Evolution and comparison of thermal spray coatings on PEEK

substrates
Before the commercial introduction of PEEK as a biomaterial approved for use in

medical implants by Invibio Ltd. in 1998, industrial grade or custom carbon fibre
reinforced PEEK materials were used in the preliminary studies. The first study on the
coating of PEEK implants with plasma spraying method were performed by Ha et al. in
1994. A highly carbon fibre reinforced PEEK substrate (59% vol.) was coated with a
200 µ thick layer of HAp by APS. Tensile adhesion strength of the coating was very low
(2.8 MPa) at that time. Low adhesion strength was associated with a possible vapour film
preventing close contact of substrate and the coating caused by vaporisation of PEEK
matrix upon contact with the first HAp particles at very high temperature (Ha et al.,
1994). In the study published by the same team in 1997, two different coatings were
deposited on CFR-PEEK samples, a Ti coating and a HAp coating with an intermediate
layer of Ti (Figure 3). Rough Ti coatings (Ra ≈ 28.29 µm, Rz ≈ 145.35 µm) with a
varying thickness of 10–150 µm were produced. On this titanium bond layer HA coatings
with a varying thickness of 50–150 um were deposited. A good interlocking between
HAp, Ti bond layer, Ti coating and PEEK substrate was reported though no mechanical
tests were performed. VPS was assessed as a suitable method for HA/Ti deposition on
CFR-PEEK implants by Ha et al. (1997).
Figure 3 Vacuum plasma sprayed, (a) Ti (b) Ti/HAp coatings on CFR-PEEK
Source: Ha et al. (1997)

About ten years later Beauvais and Decaux demonstrated that HAp coatings with a
suitable chemical composition, phase ratios and a crystallinity of 74% could be produced
by APS without degrading the PEEK substrate in an international conference. Coating
thickness was ~150 µm and tensile adhesion strength was improved to 7.5 MPa. Tensile,
impact and flexural strengths of PEEK substrate were not significantly affected during
the process, only tensile elongation decreased from 32% to 15%. It was suggested that the
coating adhesion strength can be increased by optimising the surface roughening process
or by using a titanium bond layer produced by VPS method and a better assessment of
strength can be made with the use of high viscosity room temperature curable adhesives
(Beauvais and Decaux, 2007).
In 2008, Devine et al. presented a study on VPS-Ti coatings on PEEK screws for
improved bone apposition in a scientific meeting. Ti coating increased the removal torque
of the screw from 2.3 ± 0.81 Nm to 4.97 ± 1.54 Nm and bone-implant contact area from
1 to 50% (Devine et al., 2008).
In 2009, Bureau et al. (2009a, 2009b) presented two different studies about APS-HAp
coating on PEEK in international congresses. The first study was about the effect of APS
parameters on the crystallinity and phase content of CaP-based coatings (HAp, α-TCP
and β-TCP). APS parameters modulated the crystalline content considerably (from 55 to
15%) and the trace phases (TTCP and CaO) for HAp coating (Bureau et al., 2009a). In
the second study a new preparation method for APS-HAp coatings on PEEK was
presented. PEEK substrate was overmolded with a 100 µm thick composite layer
composed of 30% wt. HAp and PEEK. Over this layer an 85 µm thick HAp coating was
produced by APS with a crystalline index of ~0.53 and Ca/P atomic ration of 1.66.
Tensile adhesion strength was measured to be 20.9 ± 2.1 MPa which is considerably
above the values obtained in previous studies (Bureau et al., 2009b). In the same year
Gisep and Wieling presented a study on mechanical and biological investigation of
VPS-Ti coating on CFR-PEEK (50% vol. CF) substrate. Tensile and shear adhesion
strength of the 70 μm thick Ti coating were measured as 22.2 ± 1.3 and 29.7 ± 6.5 MP
respectively. The removal torque of the coated screws was significantly higher. Less soft
tissue was formed around coated samples and better bone integration and contact were
reported. So, it was concluded that VPS-Ti coating is a good method to increase the
osteointegration of long-term CFR-PEEK implants like joint replacement prostheses and
spinal cages by Wieling (2009). Meanwhile, the effects of APS parameters, such as
plasma power, distance, gas flow and powder rate were investigated by Wu et al. (2009).
It was reported that HAp particle velocity increased with both He carrier gas addition to
Ar and increasing current. And the velocity decreased with both increasing powder
feeding rate and spraying distance (Wu et al., 2009).
Between 2008 and 2010, the studies conducted with the cooperation of the University
of Trento and Eurocoating S.p.A. on Ti and HAp coatings on neat and carbon fibre
reinforced biocompatible PEEK substrates were presented in scientific congresses
(Vedova et al., 2008; Robotti et al., 2009; Zappini and Robotti, 2010). On neat PEEK
substrate, the bond strength values of 19 ± 3 MPa for HAp coatings and 28 ± 4 MPa for
Ti coatings were obtained with APS method. On the CFR-PEEK substrate, adhesion
strength values of 22 ± 5 for HAp coatings and 32 ± 7 MPa for Ti coatings were reported.
In the case of VPS-Ti coatings applied to PEEK samples reinforced with 60% of long
carbon fibres the adhesion strength of 36 ± 7 MPa was reported (Zappini and Robotti,
2010). Initial mechanical properties of the substrates were not significantly affected, and
the coatings met the regulatory requirements in terms of phase composition, crystallinity
and chemical composition. The same experiments were also published in a book section
(Robotti and Zappini, 2012). Eurocoating S.p.A. has commercialised these coatings with
the brand Spondycoat®.
After the successful production and subsequent commercialisation of mechanically
and chemically sufficient Ti and HAp coatings on PEEK substrates, the studies tended to
focus on the in vivo behaviour of these coatings. In 2013, Devine et al. published a paper
in which they implanted Ti coated PEEK screws in a sheep tibia by two
different methods, namely physical vapour deposition (by Ionbond A.G.) and VPS
(by Medicoat A.G.). VPS Ti coated screws demonstrated a significantly higher removal
torque and direct bone apposition compared to uncoated and PVD-Ti coated screws
(Devine et al., 2013).
In 2014, Suska et al. examined in vivo behaviour of CR-PEEK implants coated with a
dual layered Ti/HAp coating in a rabbit model. Before the coating process the samples
were sand blasted with 250 μm sized Al2O3. A commercial VPS process (Medipure® dual
Ti/HA) applied to Ti alloy substrates was modified to suit the lower thermal properties of
PEEK substrate compared to Ti alloys by using of a smaller powder particle size
(15–45 μm sized Ti powder for bond layer and 15–50 μm sized HAp powder for top
layer) and longer plasma spraying distance. Tensile adhesion strength of the dual layered
200 μm thick coating was measured to be 28.5 ± 2.3 MPa. Ca/P and crystallinity ratios
were measured to be ~1.67 and 58.7% respectively. A better direct bone contact was
reported in the histological investigation of the coated samples compared to uncoated
samples. In conclusion, Ti/HAp coated CFR-PEEK implants were found to have equal
osseointegration to HAp coated Ti alloy implants which are accepted as the industrial
standard by Suska et al. (2014).
In 2015, Walsh et al. examined the effects of a commercial 200 µm thick VPS Ti
coating (Ti-Bond®, Spinal Elements Inc.) with a surface roughness (Ra) value of 33.7 µm
on osseointegration of PEEK implants. It was reported that the porous Ti coating
significantly improved the pull-out test results at 4 weeks and continued to improve in
12 weeks compared to neat PEEK (Walsh et al., 2015).
In 2016, Stübinger et al. compared in vivo response of different plasma sprayed
coatings (APS-Ti, VPS-Ti, dual layered APS-HAp on VPS-Ti) on PEEK and CFR-PEEK
implants. 108 PEEK rods were implanted in the pelvis bones of six sheep and after 2 and
12 weeks the surgical sites were investigated histologically and tested by pull-out tests.
The surface coating of PEEK and CFR-PEEK resulted in a significant improvement in
osseointegration compared to uncoated implants. Coated implants showed significantly
higher pull-out values, especially after 12 weeks compared to uncoated ones. The dual
layered coating (HAp on Ti) resulted in the most positive results. They concluded that
commercially available medical devices made of PEEK-based materials for spinal
applications can be improved by plasma sprayed HAp bioactive coatings. Though, details
of the coating processes and tests for the adhesion strength of these coatings were not
included in the study (Stübinger et al., 2016).
More recently, in 2017, Sclafani et al. published a review of clinical performance of
plasma sprayed Ti coated PEEK implants used in anterior lumbar interbody fusion
(ALIF) in 44 patients. A clinically significant decrease in post-operative pain and
successful arthrodesis with a solid fusion rate of 96%, which was found to be superior to
the previous studies on standard PEEK interbody spacers in the literature was reported.
It was concluded that VPS-Ti coating (Ti-Bond®, Spinal Elements, Inc.) on PEEK
implant provides rapid and stable fixation at the bone-implant interface. Though there is
still a need for a direct comparison of clinical outcomes between neat PEEK and plasma
spray coated PEEK spinal implants to evaluate the efficiency of the coatings (Sclafani
et al., 2017).
Finally, two more studies (Oliveira et al., 2018; Vogel et al., 2018) were published on
the effect of plasma spraying process on the initial mechanical properties of PEEK
substrates in 2018. Oliveira et al. (2018) compared PEEK substrates in unmodified,
exposed to plasma and APS-HAp coated conditions in terms of short-term and fatigue
strengths. While tensile strength was not affected significantly, flexural strength and
fatigue stress decay rate was increased slightly (Oliveira et al., 2018). However, tensile
elongation at break significantly reduced, from 24% in unmodified condition to 21% and
18% in plasma-exposed and HA-coated condition in accordance with Beauvais and
Decaux’s (2007) findings. Vogel et al. (2018) investigated the effect of 200 ± 50 μm
thick VPS-Ti coatings using two different powder sizes on physical and chemical
properties of PEEK substrate as well as the adhesion strengths of the coatings.
Two variations of VPS-Ti coatings were produced, using Ti powders with a mean particle
size of 90 μm and 180 μm. Smaller particle size resulted in lower surface roughness
(Ra = 30.2 μm vs. 64.1 μm), lower adhesion strength (30.3 MPa vs. 37.8 MPa) but a
more uniform distribution of the coating with a higher porosity (33.3 vs. 30%). While
tensile strength of PEEK was not affected significantly, fracture strain reduced from
28.2% in unmodified condition to 9.6% in sand-blasted condition by inducing a notch
effect, and subsequently VPS coating further reduced fracture strain to 9.2 and 7.8% for
90 and 180 μm sized powders respectively (Vogel et al., 2018).
Table 5 A summary of the adhesion strengths of the plasma sprayed Ti and HAp coatings on
PEEK implants
Adhesion strength
Author Coating type Substrate
(MPa)
Ha et al. (1994) APS-HAp ICI® PEEK APC-2 Tensile: 2.8
(59% long carbon fibre
reinforced)
Beauvais and APS-HAp PEEK Optima® Tensile: 7.5
Decaux (2007)
Bureau et al. APS-HAp coating over Victrex® PEEK Tensile: 20.9 ± 2.1
(2009b) 30% wt. HAp added 150CA30 (30% short
PEEK composite layer carbon fibre reinforced)
Wieling (2009) VPS-Ti CFR-PEEK (50% long Tensile: 22.2 ± 1.3
carbon fibre reinforced) Shear: 29.7 ± 6.5
Zappini and APS-HAp PEEK Optima® LT1 Tensile: 19 ± 3
Robotti (2010)
APS-Ti PEEK Optima® LT1 Tensile: 28 ± 4
APS-HAp PEEK Optima® Tensile: 22 ± 5
LT1CA30 (30% short
carbon fibre reinforced)
APS-Ti PEEK Optima® Tensile: 32 ± 7
LT1CA30 (30% short
carbon fibre reinforced)
VPS-Ti PEEK Endolign® (60% Tensile: 36 ± 7
long carbon reinforced)
Suska et al. (2014) Dual layer VPS-Ti/HA CFR-PEEK Tensile: 28.5 ± 2.3
(Invibio Inc.)
The coating adhesion strengths have been significantly improved to date by modifying
the plasma spray coating process parameters to suit PEEK substrates. A summary of the
studies on the mechanical properties of plasma sprayed Ti and HAp coatings on PEEK
implants is shown in Table 5. While coatings that meet the regulatory requirements
[tensile strength of 22 MPa (CDRH, 2000; ISO, 2014) for Ti and 15 MPa (ISO, 2008a)
for HAp coatings] have been produced with both atmospheric and vacuum plasma spray
methods, the highest adhesion strengths have been obtained by VPS method.
A comparison of the studies on the effect of plasma spraying process on the initial
mechanical properties of PEEK substrates is shown in Table 6. While the effect on tensile
strength and modulus was insignificant, fatigue performance was reduced moderately,
and elongation was reduced severely coming close to minimum requirement of 5% in
ASTM F2026 – 17 standard specification for polyetheretherketone (PEEK) polymers for
surgical implant applications (ASTM, 2017d). It is thought that the main reasons for the
decrease in mechanical properties are the notch effect on the surface caused by sand
blasting and exposure to UV irradiation during the plasma spray process.
Table 6 A summary of the effect of plasma spraying processes on the mechanical properties of
PEEK and CFR-PEEK substrates
Author Coating type Effect on mechanical properties

Beauvais and APS-HAp on Tensile strength was not affected significantly.
Decaux (2007) PEEK Impact, flexural strength and flexural modulus were
slightly increased.
Elongation was reduced significantly (~53%).
Vedova et al. PS-HAp on PEEK tensile strength was slightly reduced, elastic
(2008) PEEK and modulus was slightly increased.
CFR-PEEK CFR-PEEK tensile strength and elastic modulus were
both slightly reduced.
Fatigue limits were slightly reduced.
Zappini and APS-HAp and Tensile strength was not affected significantly.
Robotti (2010) APS-Ti on PEEK Elongation is significantly reduced, especially for HAp
and CFR-PEEK coating on PEEK (~40%).
Fatigue strength was reduced, especially for
CFR-PEEK (between 17–27%).
Oliveira et al. APS-HAp on Tensile strength was not affected significantly.
(2018) PEEK Flexural strength and fatigue stress decay rate was
improved slightly.
Elongation significantly reduced (~12% as plasma
exposed, ~25% as coated).
Vogel et al. VPS-Ti on PEEK Tensile strength was not affected significantly.
(2018) Elongation significantly reduced (~66% in
sand-blasted condition, between 67–72% after coating).
Animal studies report improved bone apposition compared to uncoated PEEK implants
and good results were reported in clinical trials of Ti coated spinal implants though
further clinical trials are needed to prove the long-term stability and benefits of the
coatings. A summary of the animal studies and clinical performance of the plasma
sprayed Ti and HAp coatings on PEEK implants is shown in Table 7.
Table 7 A summary of the available articles on biological response of plasma sprayed Ti and
HAp coatings on PEEK implants
Author Method Results Conclusions

Sclafani et al. Post-surgical Coated implants exhibited VPS-Ti coating on PEEK
(2017) follow-up of a clinically significant implant provides rapid and
44 patients that improvement in stable fixation at the
received a VPS-Ti post-operative pain. bone-implant interface,
coated PEEK ALIF Successful arthrodesis with though there is still a need
implant. a solid fusion rate of 96% for a direct comparison of
at an average of 7.3 ± 2.3 clinical outcomes between
months was observed. neat PEEK and plasma
spray coated PEEK spinal
implants to evaluate the
efficiency of the coatings.
Stübinger et al. Uncoated, Ti coated Higher bone-to-implant Coated implants
(2016) and dual layered contact rates and pull-out demonstrated significant
Ti/HAp coated values were demonstrated improvement in
implants were placed especially after 12 weeks osseointegration compared
in the pelvis bones of compared to uncoated to uncoated implants.
six sheep. implants. The dual layered Commercially available
coating (HAp on Ti) surgical implants made of
resulted in the most PEEK for spinal
positive results. applications can be
improved by plasma
sprayed HAp coatings.
Walsh et al. VPS Ti coated PEEK Porous Ti coating The formation of a fibrous
(2015) implants were placed significantly improved the tissue interface between
into distal femur and pull-out test results at hydrophobic PEEK surface
proximal tibia of four 4 weeks and continued to and host bone can be
sheep. improve in 12 weeks inhibited, and mechanical
compared to neat PEEK. properties can be improved
Direct bone on-growth in by a VPS-Ti coating.
cancellous and cortical
sites were demonstrated in
histological examination.
Suska et al. Six HA/Ti coated A better direct bone Ti/HAp coated CFR-PEEK
(2014) PEEK implants were contact was reported for implants were found to
placed into femur and coated samples compared have equal
tibia of each eleven to uncoated samples in osseointegration to HAp
adult rabbits. histological investigation coated Ti alloy implants
of the surgical sites after which are accepted as the
six weeks. industrial standard.
Devine et al. VPS and PVD-Ti VPS Ti coated screws VPS-Ti coating improved
(2013) coated CFR-PEEK demonstrated a the quantity and quality of
screws were significantly higher bone on-growth. Ti coating
implanted in a sheep removal torque and direct may broaden indications of
tibia. bone apposition compared PEEK implants, including
to neat and PVD Ti coated situations where improved
screws. bone apposition is
required.
5 Conclusions
PEEK is an organic thermoplastic polymer with successful clinical performance in

orthopaedic applications such as fracture fixation plates, screws, total joint prosthesis
parts and spinal implants. PEEK has several advantages over metallic implant materials
like radiolucency, non-magneticity, density and elastic modulus close to that of the bone
to prevent stress-shielding and bone resorption. PEEK’s hydrophobic surface can be
coated with porous Ti and HAp to improve osteoconductivity and osteoinductivity
properties. Plasma spray deposition is the accepted method in the production of these
coatings.
The important properties of HAp coatings, such as phase composition (Ca/P ratio),
crystallinity ratio, microstructural properties and adhesion strength depend on various
parameters of the plasma spray process such as flowrates of the plasma gases, powder
size and feed rate, plasma power and spray distance (Chang et al., 1998; Fazan and
Marquis, 2000; Heimann, 2006; Wang et al., 2007; Su et al., 2018). These characteristics
significantly affect the mechanical strength and chemical stability of these coatings as
well as the biological response upon implantation into bone (Yang et al., 1995; Heimann,
2006). Studies on HAp coatings on metallic implants report that while higher electric arc
power, higher gas flow rate and smaller powder size lead to a homogeneous structure
with lower porosity; lower plasma power, lower plasma gas flowrate and larger powder
size result in a non-homogeneous and porous microstructure. As the spray distance
increases to a certain value, the homogeneity of the coating increases, and after a certain
distance, the homogeneity decreases (Wang et al., 2007). For PEEK implants a smaller
particle size and a longer spraying distance compared to that are used for metallic
substrates are recommended because of the lower melting and decomposition
temperatures of PEEK material.
APS is the most cost-effective method and there are conference papers that report
biocompatible Ti and HAp coatings conforming the international standards could be
produced on PEEK substrates with APS, but there are no peer-reviewed articles
published in international journals reporting adhesion strengths above the lower limit
specified in the standards to our knowledge. On the other hand, VPS provides higher
purity and higher adhesion strength than APS but is a more expensive and
time-consuming process. Coatings with different roughness and porosity levels can be
produced with VPS and Ti/HAp dual layer VPS coatings combine the bioactivity of HAp
with the mechanical strength of Ti. Plasma sprayed Ti coatings are commonly used to
improve osseointegration and the stability of the biomechanical fixation by increasing
wettability and surface area for bone apposition on the implant surface (Le Guéhennec
et al., 2007). Roughness is essential for improving implant integration with the bony
tissue (Bagno and Di Bello, 2004) and many studies have reported that the initial and also
the long-term fixation of the implant can be enhanced by increased roughness (Buser
et al., 1991; Le Guéhennec et al., 2007). Very high roughness and porous Ti coatings on
PEEK implants can be achieved by VPS.
To improve the performance of APS coatings on PEEK implants, alternative methods
such as suspension plasma spraying (Bolelli et al., 2015; Fan and Bai, 2016; Ročňáková
et al., 2018; Bai et al., 2019; Hameed et al., 2019; Zhang et al., 2019) or shrouded plasma
spraying (Planche et al., 2007; Kim et al., 2010; Morks and Berndt, 2010; Wei et al.,
2012; Erfanmanesh et al., 2014; Matthews, 2014b, 2014a) may be used. In suspension
plasma spraying method, fine powders are injected into the plasma by a liquid carrier.
Lower spraying temperatures provide higher crystallinity and the higher speed of the
particles provides better adhesion strength. Moreover it possible to produce very thin
coatings using fine powders with this method (Fan and Bai, 2016; Hameed et al., 2019).
In the shrouded plasma spraying method, a gas or solid shield is used to prevent the
sprayed particles from coming into contact with oxygen present in the surrounding air.
Thus, better mechanical properties may be achieved with lower oxide content and higher
purity without the use of a vacuum chamber. Moreover, it is possible to use a longer
spraying distance leading to lower substrate temperatures.
This study attempted to present a focused review and the evolution of the available
scientific research on plasma sprayed Ti, HAp and dual layered Ti/HAp coatings applied
to PEEK and CFR-PEEK substrates. Since 1994, major progress has been made in the
field of osseointegrative plasma sprayed coatings on PEEK substrates. With the plasma
spray deposition method, Ti and HAp coatings with the properties specified in
international standards have been obtained. In vivo studies show improved results over
uncoated PEEK materials. Likewise, there are studies demonstrating the decent clinical
performance of Ti coatings on PEEK implants, although there is still a need for
comparison of the osseointegration capacity of Ti and HAp coatings PEEK implants
between each other and versus uncoated PEEK implants. In addition, the plasma spraying
method is still open to improvement, especially on surface preparation of PEEK
substrate. However, most of the plasma spray coatings applied to PEEK implants are
commercial products and the process details are not open access, this is thought to slow
down the scientific development in this area to some extent.
Acknowledgements
This study was supported by Scientific Research Coordination Unit of Pamukkale

University under the project number 2018FEBE065.
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A Review On Plasma Sprayed Titanium and Hydroxyapatite Coatings On Polyetheretherketone Implants

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A review on plasma sprayed titanium and hydroxyapatite

Article in International Journal of Surface Science and Engineering · January 2019

Ali Tekin Guner Cemal Meran

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A review on plasma sprayed titanium and

Ali Tekin Guner* and Cemal Meran

Abstract: Polyetheretherketone (PEEK) is a biocompatible polymer with good

Keywords: plasma spray; coating; polyetheretherketone; PEEK;

Biographical notes: Ali Tekin Guner has been working as a Research

Cemal Meran holds a PhD in Mechanical Engineering from the Pamukkale

Copyright © 2019 Inderscience Enterprises Ltd.

the Pamukkale University. He has authored numerous peer-reviewed scientific

Biomaterial can be defined as a material designed for the development, treatment or

2 Plasma spray deposition technology

3 Validation of the coatings, guidelines and requirements

3.1 Requirements for plasma sprayed Ti coatings on surgical implants

specified by ISO 13179-1 standard implants for surgery – plasma-sprayed unalloyed

Table 1 Required mechanical properties of plasma sprayed Ti coatings on surgical implants

Properties Test methods Specifications Requirements

Table 2 Chemical composition requirements of plasma sprayed Ti coatings on surgical

3.2 Requirements for plasma sprayed hydroxyapatite (HAp) coatings on

Properties Test methods Specifications Requirements

Properties Test methods Specifications Requirements

4 Evolution and comparison of thermal spray coatings on PEEK

Before the commercial introduction of PEEK as a biomaterial approved for use in

Figure 3 Vacuum plasma sprayed, (a) Ti (b) Ti/HAp coatings on CFR-PEEK

Source: Ha et al. (1997)

Author Coating type Effect on mechanical properties

Author Method Results Conclusions

PEEK is an organic thermoplastic polymer with successful clinical performance in

This study was supported by Scientific Research Coordination Unit of Pamukkale

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