Author's Accepted Manuscript Comparative Investigation on the Adhesion of Hydroxyapatite coating on Ti-6Al-4V Implant: A Review Paper E. Mohseni, E. Zalnezhad, A.R. Bushroa PII: S0143-7496(13)00168-1 DOI: http://dx.doi.org/10.1016/j.ijadhadh.2013.09.030 Reference: JAAD1419 To appear in: International Journal of Adhesion & Adhesives Accepted date: 17 July 2013 Cite this article as: E. Mohseni, E. Zalnezhad, A.R. Bushroa, Comparative Investigation on the Adhesion of Hydroxyapatite coating on Ti-6Al-4V Implant: A Review Paper, International Journal of Adhesion & Adhesives, http://dx. doi.org/10.1016/j.ijadhadh.2013.09.030 This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting galley proof before it is published in its final citable form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain. www.elsevier.com/locate/ijadhadh
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Author's Accepted Manuscript
Comparative Investigation on the Adhesion ofHydroxyapatite coating on Ti-6Al-4V Implant:A Review Paper
To appear in: International Journal of Adhesion & Adhesives
Accepted date: 17 July 2013
Cite this article as: E. Mohseni, E. Zalnezhad, A.R. Bushroa, ComparativeInvestigation on the Adhesion of Hydroxyapatite coating on Ti-6Al-4VImplant: A Review Paper, International Journal of Adhesion & Adhesives, http://dx.doi.org/10.1016/j.ijadhadh.2013.09.030
This is a PDF file of an unedited manuscript that has been accepted forpublication. As a service to our customers we are providing this early version ofthe manuscript. The manuscript will undergo copyediting, typesetting, andreview of the resulting galley proof before it is published in its final citable form.Please note that during the production process errors may be discovered whichcould affect the content, and all legal disclaimers that apply to the journalpertain.
Hydroxyapatite (HA) has been used in clinical bone graft procedures for the past 25 years. Although a biocompatible material, its poor adhesion strength to substrate makes it unsuitable for major load-bearing devices. Investigations on various deposition techniques of HA coating on Ti-6Al-4V implants have been made over the years, in particular to improve its adhesion strength to the metal alloy and its long-term reliability. This review comprehensively analyzes nine techniques mostly used for deposition of HA onto Ti-6Al-4V alloys. The techniques reviewed are Plasma sprayed deposition, Hot Isostatic Pressing, Thermal Spray, Dip coating, Pulsed Laser deposition (PLD), Electrophoretic deposition (EPD), Sol-Gel, Ion Beam Assisted deposition (IBAD), and Sputtering. The advantages and disadvantages of each method over other techniques are discussed. The adhesion strength and the factors affecting the adhesion of HA coating on Ti-6Al-4V implants are also compared. Keywords: Adhesion; Hydroxyapatite; coating; Ti-6Al-4V implant
1. Introduction
Biological fixation is defined as the process where prosthetic components become firmly
bonded to the host bone by ongrowth or ingrowth without the use of bone cements [1-3]. In the
late 1960s, the concept of biological fixation of load-bearing implants using bioactive
2
hydroxyapatite (HA) coatings was proposed as an alternative to cemented fixation.
Hydroxyapatite (HA: Ca10(PO4)6(OH)2), a pure calcium phosphate phase, is a preferred
biomaterial for both dental and orthopedics use due to its favorable osteoconductive and
bioactive properties [4, 5]. HA has a similar chemical composition and crystal structure as the
apatite in the human skeletal system, and is therefore suitable for bone substitution and
reconstruction [6]. Furthermore, HA has shown significant success in implants due to its
favorable in vivo behavior [7, 8] and the presence of HA films prolongs the lifetime of
prostheses [9]. However, HA coatings are susceptible to fatigue failure, making it unsuitable for
load bearing implants [10, 11].
Nevertheless, there is a large demand for implants with excellent mechanical properties.
These implants should possess similar properties to the human bones, such as in the value of its
Young’s modulus, which result in less stress shielding effect [12] and extends its service life.
The implants can made into different shapes such as plates, rods, screws and pins [13].
Historically, titanium-based alloys are the most common material for this purpose since it is
known to be a tolerable metal in the human body [14].
Titanium (Ti) and its alloys are the most commonly used metallic materials for medical
implants in orthopedic and dental applications, due to their low density, high strength, non-
toxicity and excellent corrosion resistance [15]. However, there have been reports on
inflammatory reaction around these implants as a result from the creation of an avascular fibrous
tissue that encapsulated the implants [16, 17]. A coating of hydroxyapatite layer can be deposited
on the metal alloy to assist the osseointegration of these implants with surrounding tissues [16].
The bond strength between the coating layer and the metal substrate is a very critical
factor. Separation of the coating layer from the implant during service in the human body results
3
in adverse effects on the implants and the surrounding tissue caused by detached particles [18].
The main reason of using HA coating on metallic substrates is to keep the mechanical properties
of the metal such a load-bearing ability and, at the same time, to take advantage of the coating’s
chemical similarity and biocompatibility with the bone [19].
According to Blind et al., the HA coating allows rapid osteointegration as a result of
bone tissue bonding properties [20]. The first clinical results from HA coatings on titanium
dental implants were promising, showing excellent results, even with poor bone quality.
However, after a long period, mechanical failure would occur at the interface of HA and metallic
substrate [21]. The HA coating dissolves as a result of poor crystallized structure [22, 23],
decrease of adherence with the titanium surface and dramatic late implant failure [23, 24].
Moreover, HA itself has poor mechanical properties, with a bending strength of less than 100
MPa [25]. Thus, it can be concluded that the stability of the HA coating is the most critical
factor to ensure the success of this type of implant. Furthermore, the method used to deposit HA
powder onto the substrate could influence the coating characteristics such its adhesion strength
and reliability.
Several techniques have been used to create the HA coating on metallic implants, such as
gel, ion beam assisted deposition (IBAD), and sputtering were evaluated and discussion were
made on the coating parameters affecting the adhesion strength of the coating. Advantages and
disadvantages of each method were discussed and a quantitative comparison was made on the
different techniques of HA coating on Ti-6Al-4V substrate. Based on this review, the best
adhesion of HA coating to substrate is obtained by sputtering deposition technique while the
worse bonding strength was obtained by PLD at 1000 laser pulses. Using an interfacial layer
(such as TiO2 or TiN) as the initial coating layer on the substrate followed by HA coating layer
can enhance the bonding strength. Pretreatments such as nitriding, followed by etching, can
enhance the adhesion strength in PLD. Moreover, post-treatments also have similar effects on
other techniques such as IBAD and thermal spray.
Acknowledgement
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The authors would like to acknowledge the University of Malaya for providing the necessary
facilities and resources for this research. This research was fully founded by the Ministry of
Higher Education, Malaysia with the high impact research grant number of
um.c/625/1/HIR/MOHE/ENG/27.
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Table 1 Thermal spray condition of HA powders [92].
Parameters Argon
(l/min)
Helium
(l/min)
Current Voltage Powder
Rate
(g/min)
Spray
Distance
(mm)
Surface
Speed
(m/min)
Travers
Speed
(mm)
Cooling
Setting 41 60 700 52 30 115 75 8 yes
Table 2 Bond strength test results with different pretreatment and cryogenic treatment [92].
Coating Bonding Strength ( MPa)
Without Cryogenic
Treatment
With Cryogenic Treatment
Ultrasonic High
Pressure Air
Ultrasonic High
Pressure Air
HA 26.56 18.91 36.65 29.30
53
Table 3 Adhesion strengths of HA coated samples with and without TiO2 inner layer
deposited using different voltages [160].
Samples
(substrate + inner layer + Ha)
Shear Strength
(MPa)
Ti-6Al-4V + ----- + HA 13.8 ( s=1.8)
Ti-6Al-4V + TiO2 (50 V)+ HA 11.9 ( s=1.8)
Ti-6Al-4V + TiO2 (20 V)+ HA 13.1 ( s=1.8)
Ti-6Al-4V + TiO2 (10 V)+ HA 21.0 ( s=1.8)
Note. S: standard deviation.
Table 4 Adhesion Strength and Failure Mode of Coatings [220].
Table 5: Different techniques to deposit HA coating.
Technique Thickness Advantages Disadvantages
Plasma Spraying < 20 µm rapid deposition ; sufficiently low cost; fast bone healing, less risk for coating degradation
Poor adhesion, alternation of HA structure due to coating process; non- uniformity in coating density; extreme high temperature up to 1200 ºc, phase transformation and grain grow of substance due to high temperature procedure; increase in residual stress; unable to produce complete crystalline HA coating
Thermal Spraying
30- 200 µm High deposition rates; low cost;
Line of sight technique; high temperatures induce decomposition; rapid cooling produces amorphous coatings; lack of uniformity; crack appearance; low porosity; coating spalling and interface separation between the coating and the substrate
Sputter Coating 0.5- 3 µm Uniform coating thickness on flat substrates; dense coating; homogenous coating; high adhesion
Line of sight technique; expensive time consuming; produces amorphous coatings; low crystallite which accelerates the dissolution of the film in the body
Pulsed Laser Deposition
0.05- 5 mm Coating with crystalline and amorphous; coating with dense and porous; ability to produce wide range of multilayer coating from different materials; ability to produce high crystalline HA coating; ability to restore complex stoichiometry; high degree of control on deposition parameters
Line of sight technique; splashing or particle deposition; need surface pretreatment; lack of uniformity
Dip Coating < 1 µm Inexpensive; coatings applied quickly; can coat complex substrates; high surface uniformity; good speed of coating;
Requires high sintering temperatures; thermal expansion mismatch; crack appearance
Sol-gel 0.1- 2.0 µm Can coat complex shapes; Low processing temperatures; relatively cheap as coatings are very thin; simple deposition method; high purity; high corrosion resistant; fairly good adhesion
Some processes require controlled atmosphere processing; expensive raw materials; not suitable for industrial scale; high permeability; low wear resistance; hard to control the porosity;
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Electrophoretic Deposition
0.1- 2.0 mm Uniform coating thickness; rapid deposition rates; can coat complex substrates; simple setup, low cost, high degree of control on coating morphology and thickness, good mechanical strength; high adhesion for n-HA
Difficult to produce crack-free coatings; requires high sintering temperatures; HA decomposition during sintering stage
Hot Isostatic Pressing
0.2- 2.0 mm Produces dense coatings; produce net-shape ceramics; good temperature control; homogeneous structure; high uniformity; high precision; no dimensional or shape limitation
Cannot coat complex substrates; high temperature required; thermal expansion mismatch; elastic property differences; expensive; removal/interaction of encapsulation material
Ion Beam Assisted Deposition
<0.03 µm Low temperature process; high reproducibility and reliability; high adhesion; wide atomic intermix zone are coating-to-substrate interface
Crack appearance on the coated surface
Figure 1 Tensile bond strength result of plasma sprayed Ti-6Al-4V/ 20 wt.%
hydroxyapatite coating (as sprayed and HIPed) [79].
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Figure 2 A schematic diagram of thermal spray coating [82].
Figure 3 Fundamental stages of dip coating (the finer arrows indicate
the flow of air) [94].
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Figure 4 SEM micrographs from cross-sectional view of HA coatings (via SOL 2) on Ti-
6Al-4Vsubstrates after heating at 840°C [96].
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Figure 5 Comparison of adhesion strength for HA on substrates with different pre-treatments
[119].
Figure 6 Average surface roughness of titanium substrates treated with different laser pulses and
HA coating compared with control sample [132].
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Figure 7 Failure values obtained by scratch test (Lc1, Lc2 and Lc3) for the HA coatings on
different irradiated and non-irradiated titanium substrate [132].
Figure 8 Electro-polarization corrosion curves for both EPD n-HA coating and HA thermal
sprayed coating [151].
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Figure 9 Cross section SEM micrograph of the EPD deposited under the identified optimum
suspension condition [140].
Figure 10 SEM micrograph of the uncrack deposit surface [140].
100µm
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Figure 11 Steps in the sol-gel process for ceramic materials [169].
Figure 12 X-ray diffraction of sol-gel coatings preferred to 500˚C on titanium substrates and
then fired at various temperatures [179].
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Figure 13 A scanning electron micrograph of a coating fired to 800˚C for 10 min, the field of
view is 250 nm × by 250 nm [179].
Figure 14 Coefficient of friction in terms of relative voltage as a function of normal load while
scratching (a) pure HA coating; (b) fluoridate HA (FHA6) coating on Ti-6Al-4V [174].
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Figure 15 Adhesion strength of pure HA and fluoridated HA coatings on Ti-6Al-4V substrates
as indicated by upper critical load in scratch test. Firing temperatures are indicated [174].
Figure 16 Pull-out adhesion strength of FHA coating before and after soaking in TPS solutions.
* indicates a significant increase of adhesion strength with respect to F0 (as prepared coatings);
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** indicate a significant increase of adhesion strength with respect to F0 (after soaking in TPS
for 21 days) [186].
Figure 17 Pull-out strength of coatings with different F content [190].
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Figure 18 Fz-Fy curve of scratch test from specimen prepared by (a) IBSD and (b) IBAD [207].
Figure 19 Layer-metal substrate bond strengths, before and after heat treatment, as a function of
ion beam current [207].
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Figure 20 SEM micrographs of the coating layer (A) before and (B) after the heat treatment
[208].
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Figure 21 Adhesion strength of the IBASVD samples at different elevated temperatures [197].
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Figure 22 Bone bonding strengths of sputtered films [217].
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Figure 14 Adhesion strength of coatings [220].
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Figure 24 Quantative comparison of different coating techniques.