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7

Bioinert ceramic biomaterials:


advanced applications
DOI: 10.1533/9781782422662.173
Abstract: First-generation, inert ceramics exhibit excellent mechanical
strength, corrosion and wear resistance. This chapter reviews the fundamental
properties that make alumina, zirconia, titania and pyrolytic carbon the
materials of choice for the production of numerous load-bearing implants. The
shortcomings of these materials, namely their relative brittleness and limited
ability to be integrated with soft and hard tissues in vivo, are also discussed as a
limiting factor for their clinical application.
Key words: bioinert ceramics, alumina, zirconia, leucite, bioinert refractory
polycrystalline compounds.

7.1

Introduction

Ceramics are inorganic materials that are generally formed by a high-temperature


synthesis process. They are comprised of non-directional ionic and covalent bonds,
and are typically crystalline in nature (Bauer et al., 2013). The first generation of
ceramics was hard, stabile and inert under a wide range of environmental conditions,
often displaying superior properties to metallic biomaterials.
Metal-based alumina, zirconia and titania are amongst the most highly studied
ceramics. The high compressive strength, low friction, corrosion and wear resistance
of alumina, zirconia, titania and pyrolytic carbon makes these ceramics an excellent
material for the fabrication of load-bearing implants. The high abrasive strength of
these ceramics renders them highly suitable for use as bearing balls in artificial
joints. When compared to metallic ball heads, ceramic heads lead to less long-term
wear when used in conjunction with a polyethylene cup, reduce aseptic loosening,
and therefore exhibit a reduced degree of osteolysis within the peri-implant space
(Ihle et al., 2011). Despite these advantages, ceramics suffer from the disadvantage
that they can be brittle (due to the nature of ionic bonds), which somewhat limits
their use in clinical applications (Bauer et al., 2013). However, their excellent osteoconductive properties also make ceramics a coating of choice for the encapsulation
of metallic load-bearing implants, such as titanium and stainless steel.

7.2

Hardness, high compressive strength and wear


resistance of bioinert refractory polycrystalline
compounds

Alumina (Al2O3) and zirconia (ZrO2) oxides represent two examples of the most
widely used inert ceramics, with applications in the construction of orthopaedic
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joint replacement and load-bearing implants, for example prosthesis, implant


coatings and dental implants. These are discussed in the following sections,
together with leucite-containing ceramics.

7.2.1 Alumina
Alumina-based ceramics are typically prepared from very fine-grained
polycrystalline -Al2O3 using hot isostatic pressing, followed by sintering at
temperatures of 1600 to 1800 C. The compressive strength of alumina is notably
higher than that of zirconia at 4250 and 2000 MPa for -Al2O3 and tetragonal
zirconia stabilised with yttria, respectively. The Youngs modulus and hardness
for the former was greater, at 400 GPa and 2400 HV, respectively, compared to
208 GPa and 1130 HV. However, for zirconia, the bending strength was found to
be higher for the zirconium oxide (1000 MPa) compared to 595 MPa for -Al2O3.
In comparison, the bending and compressive strengths of dense hydroxyapatite
ceramics are 20 to 80 MPa and 100 to 900 MPa, respectively, with a Youngs
modulus of 70 to 120 GPa and hardness of 500 to 800 HV.
The mechanical properties, strength and corrosion resistance in crystalline
materials is known to depend on the grain size within the material. Studies have
demonstrated that for alumina to maintain its favourable mechanical and wear
properties, the grain size should be kept below 4 m, since an increase in the grain
size to more than 7 m has been shown to reduce the mechanical strength of the
ceramic by close to 20% (Bauer et al., 2013). Addition of magnesium oxide to the
-Al2O3 facilitates the preservation of the fine-grained structure during the sintering
process, contributing to the increased strength, resistance to dynamic and impact
forces, fracture toughness and subcritical crack growth resistance. Figure 7.1 shows
differences in microstructure and alumina doped with Ca, Mn and Cr (Pabbruwe et
al. 2004). However, the use of such sintering agents should be kept to a minimum,
since their excessive use may result in precipitation at the grain boundary and a
consequent loss of fatigue resistance. In addition, implant materials that have a
Youngs modulus that is relatively compared to that of natural bone tissue have
been associated with aseptic loosening of the implant, with this behaviour being
typically observed in metallic implants, such as those based on titanium.
Ceramics based on alumina are used in clinical applications such as dental bridges
and implants, joint prosthesis, bone screws, alveolar ridge and maxillofacial
reconstructions (Cruz-Pardos et al., 2012; Huet et al., 2011). Under load
conditions that are typical for load-bearing applications (12 kN), alumina-based
implants are expected to perform for 30 years, with their lifetime being limited by
the material properties and the environment in which the ceramics are required to
operate (Ritter et al., 1979). The fracture mechanics theory used to make this
projection assumes that fatigue failure is controlled by the slow crack growth
of pre-existing flaws in the structure when placed in biological environments.
For example, the long-term strength of glass-infiltrated alumina- and various

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7.1 Differences in microstructure of the internal surface of alumina


tubes (1.3 mm outer diameter, 0.6 mm inner diameter, 15 mm length)
doped with Ca, Mn, or Cr: (a) pure alumina; (b) 0.5 mol% Ca-doped
alumina; (c) 5.0 mol% Ca-doped alumina; (d) 0.5 mol% Mn-doped
alumina; (e) 5.0 mol% Mn-doped alumina; (f) 0.5 mol% Cr-doped
alumina; and (g) 5.0 mol% Cr-doped alumina. The scale bars are 5 m.
The doping significantly altered tissue ingrowth, differentiation and
osteogenesis within a porous implant when implanted into femoral
medullary canals of female rats for 16 weeks (Pabbruwe et al., 2004).

zirconia-ceramics for applications in an oral cavity environment differed significantly


(Tinschert et al., 2007). The study found that under moist environmental conditions,
the glass-infiltrated alumina- and some zirconia-ceramics have a high susceptibility
to subcritical crack growth, while zirconia ceramics containing 0.25 wt% alumina
oxide demonstrated the highest initial and most favourable long-term strength.

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7.2.2 Zirconia
As with Al2O3 ceramics, zirconia is biocompatible, exhibiting good corrosion
resistance under normal physiological conditions. As mentioned previously,
zirconia has higher bending strength and fracture toughness compared to alumina,
making it highly suitable for load-bearing implant applications. Furthermore, the
stress shielding between the bone and the zirconia is reduced compared to that of
alumina, owing to the notably lower tensile modulus of the former material.
Monoclinic at room temperature, zirconia crystallises to form a tetragonal phase
at temperatures between 1000 and 1170 C. Subsequent heating to a temperature
of 2370 C causes the zirconia to transform from a tetragonal to cubic phase.
During the sintering process, zirconia also undergoes a volumetric expansion of 3
to 5%. As the material cools, the mechanical stresses within the structure form.
This mechanical stress has been linked to the formation of cracks in ceramics that
are based on pure zirconia. Sintering agents may be introduced to stabilise the
phases during these temperature changes. Introduction of magnesium oxide,
calcium oxide and yttrium oxide results in the formation of a partially-stabilised
zirconia microstructure, that is, it is comprised primarily of cubic zirconia with
minor monoclinic and tetragonal zirconia precipitates. For example, incorporation
of CuO into zirconia ceramics resulted in a significant reduction of friction in a
sliding test against Al2O3 balls, with the coefficient of friction reducing from 0.8
to values between approximately 0.2 and 0.3 (Pasaribu et al., 2003). The flexural
strength of partially-stabilised zirconia has been reported to be further affected by
the fabrication methodology and the properties of the powders used (Adolfsson
and Shen, 2012). The introduction of low amounts of Y2O3 (23 %mol) into a
tetragonal zirconia polycrystal yields a ceramic structure with typical grain size of
under 1 m and narrow size distribution.
As a result of their superior mechanical properties arising from its high
crystallinity, yttrium oxide stabilised tetragonal zirconia polycrystals are attractive
candidates for various load-bearing dental applications (Crisp et al., 2012; Tarumi
et al., 2012). However, the same degree of crystallinity renders yttria-stabilised
tetragonal zirconia polycrystals highly opaque, which is undesirable for dental
restoration from an aesthetic point of view. Clinically speaking, the stability of an
yttria partially-stabilised tetragonal zirconia implant will be highly dependent on
the adhesive bond strength that exists between the zirconia-based core and the
resins used for dental restorations (Jevnikar et al., 2012). In contrast to silicabased ceramics, chemically-inert zirconia ceramics exhibit resistance to etching
with acids, such as hydrofluoric acid and functionalisation. A host of methods
have been trialled to establish a long-term bond with this substrate, including
mechanical and chemical roughening of the surface to create micro-scale retention,
for example particle abrasion, tailoring bonding cements, for example zincphosphate, composite resin, glass ionomer and resin-modified glass ionomer
cements, and deposition of thin layers, such as alumina coatings.

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7.2 Schematic representation depicting how the tetragonal to


monoclinic (t m) transformation of ZrO2 increases fracture
toughness. When a section containing metastable tetragonal zirconia
(t -ZrO2) is subjected to a remote macroscopic tensile stress, the stress
intensification due to the presence of the crack tip is sufficient to
transform some t -zirconia grains to the monoclinic form. Since this
transformation entails a volumetric expansion, which is constrained
by the surrounding materials, the net result is compressive stress
acting on the surfaces of the crack, whose propagation is thus
hindered (Lughi and Sergo, 2010).

The addition allows for the stabilisation of the tetragonal phase at room
temperature, with the size of the grain and the amount of yttrium oxide present
affecting the proportion of the tetragonal phase retained. The retention of the
metastable tetragonal phase is favourable, since it limits the extent of crack
propagation. Specifically, the application of stress and resultant crack formation

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induces the metastable tetragonal zirconia grains located at the crack tip to
transform to the stable monoclinic phase (Fig. 7.2). The expansion associated with
the phase transformation works to offset the compression stress onto the materials,
thus enhancing the mechanical roughness of the ceramics. In order to expand the
desirable crack limiting characteristics of zirconia materials, these ceramic
particles have been dispersed into the Al2O3 bulk ceramics to ensure mechanical
pre-stressing of the resultant ceramics as the material loses its temperature after
the sintering treatment. The resultant materials are characterised by a favourable
flexing strength of over 900 MPa and a hardness of 1500 HV. However, it is not
clear if the improvement in mechanical properties is associated with the microcrack
formation. Furthermore, the wear resistance of alumina-containing zirconia
particles has been shown to be less than that of pure Al2O3. In order to overcome
this limitation, the zirconia particle size was reduced to a nanoscale.
Adding SrO and Cr2O3 to this nanoparticle zirconia-toughened alumina allows
the formation of an alumina matrix composite ceramic (Bahraminasab et al.,
2012). The mechanical properties of the composite are even more superior,
exhibiting bending and compressive strengths of 1150 and 4700 MPa, respectively,
Youngs modulus of 350 GPa and hardness of 1975 HV. The enhanced mechanical
strength allows for the development of more reliable, thinner walled components
with a comparable load-bearing capacity. In orthopaedic applications, these
materials could facilitate the fabrication of large ball heads to decrease the
incidence of implant dislocation. In vivo studies using a sheep model showed a
stable osseo-integration of porous coated alumina matrix composite ceramic
monoblock cups (Schreiner et al., 2012). Clinical studies of the alumina matrix
composite/alumina matrix composite-bearing surfaces showed no evidence of
abnormal wear, osteolysis or implants migration (Lazennec et al., 2012).

7.2.3 Leucite
Leucite (KAlSi2O6) is a mineral composed of potassium and aluminium
tectosilicate, with the crystals conforming to a polygonal shape and ranging in
size from 1 to 5 micrometres (Fig. 7.3). At ambient temperatures, leucite
crystallises to tetragonal structure, which is transformed to a cubic structure at
625 C. A volumetric expansion of over 1% takes place during the displacive
phase transformation, which is where a structural change is associated with the
coordinated movement of atoms relative to their neighbouring atoms. Leucite is a
major crystalline phase in ceramics that are used for dental veneers, termed
feldspathic porcelains, where the amorphous phase is a feldspar-derived
glass. Since the coefficient of thermal expansion of the glass phase is significantly
lower than that of the underlying metallic implant, it is not suitable for veneering
applications on its own. The incorporation of leucite notably increases the
coefficient of thermal expansion. In terms of fabrication, leucite-containing
ceramics can be prepared via the incongruent melting of naturally-occurring

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7.3 Surface crystallisation of leucite in a SiO2-Al2O3-K 2O-Na2O glass.


Dendritic crystals grow like petals of a flower. SEM, etched sample
(3% Hydrofluoric acid, 10 s), Au sputtered (Hland et al., 2007).

feldspars at temperatures between 1150 and 1530 C (Bauer et al., 2013). As with
other ceramics, microcracking within leucite-containing ceramics occurs as a
result of the mismatch in the coefficient of thermal expansion between the
crystalline and amorphous phases, causing a decoupling of crystals from
the ceramic matrix. The thermal behaviour and the resultant mechanical
properties and stability of leucite-based ceramics are dependent on the amount
of the crystalline phase present. Typically, due to the presence of an extensive
amorphous phase, leucite-based materials have been found to exhibit inferior
mechanical properties compared to that of other biologically relevant inert
ceramics.

7.3

Techniques for the fabrication of bioinert ceramic


implants

The fabrication methodologies employed to manufacture finished implant


products are vast, with the choice of method being dependent on the material and

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operation environment requirements. For instance, ceramic-based dental implants


can be fabricated by heat pressing, slip casting, computer-aided hard machining of
completely sintered ceramic units, or by sequential soft machining of partially
sintered porous ceramic units and sintering (Denry and Holloway, 2010). Vacuumaided sintering is commonly used for deposition of ceramic veneers, most
commonly leucite-based feldspathic porcelains (1525 vol% leucite) onto metallic
dental implants. The technique is used to minimise the porosity of the ceramic
veneer, as well as to reduce the presence of defects (cracks, inclusions) that may
evolve into microcracks under operating pressure. Within the porcelain, the
leucite particles have been shown to be partially encircled by the microcracks
formed as a result of a thermal expansion mismatch between the leucite crystalline
phase and the surrounding glass matrix, with the magnitude of the stress at the
particlematrix interface independent of the leucite particle size (Mackert et al.,
2001). The firing/cooling cycles have been reported to influence the leucite
concentration within the ceramic veneer, thus affecting the mechanical properties
of the product. Slow cooling has been demonstrated to increase the proportion of
crystalline leucite within the porcelain (Mackert and Evans, 1991). The ratio of
crystalline leucite to amorphous feldspar glass affects the coefficient of thermal
expansion of the resultant ceramic, and is fine-tuned to ensure that the thermal
contraction of the veneer is less than that of the underlying metal unit (Mackert
and Williams, 1996). In addition to tempering, ion-exchange treatments of
feldspathic porcelains (via application of ion exchanging agents to the porcelain
surface) have been demonstrated to create a surface less prone to crack initiation
(Anusavice et al., 1992).
Heat pressing is an easy and inexpensive technique that has mostly been used
to produce ceramics based on leucite and lithium disilicate with a reinforcing
crystalline phase. The ceramics produced in this fashion contain a significantly
higher proportion of crystalline component (3545 vol% leucite), resulting in
an enhanced bending strength and fracture toughness compared to that of
veneers (Denry and Holloway, 2010). The observed improvement in the
mechanical performance of heat pressed ceramics can be partially attributed
to the dispersion of fine leucite crystals throughout the ceramic matrix and the
difference in tangential compressive stresses around the crystal phase as a
consequence of cooling. According to Guazzato et al. (2004), the highly localised
residual stresses can arise in a region with thermal expansion anisotropy in
polycrystalline materials with elongated grains and/or thermal expansion or
elastic mismatch in polyphase materials and/or in transforming materials. These
residual stresses induce the microcrack toughening of the material, where
microcracks emerge along the lowest energy path, such as the lower modulus and
toughness glassy phase in a glass-ceramic. However, the negative aspect of the
microcrack evolution is the potential decoupling of the crystalline phase from the
porcelain matrix, which can result in an untimely loss of strength and facture
resistance.

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While the typical porosity of heat pressed leucite-based ceramics is


approximately 10%, a significantly lower porosity (~1%) can be attained using
lithium disilicate (Li2Si2O5)-based ceramics (65 vol%). The heat pressing-induced
crystallisation of lithium disilicate yields a highly interlocked crystal phase
with nanosized dimensions, with lithium metasilicate (Li2SiO3) and cristobalite
(SiO2) intermediates forming prior to the formation of lithium disilicate crystals.
As with leucite-based ceramics, the formation of tangential compressive
stresses at the boundary between Li2Si2O5 crystals and surrounding amorphous
phase is associated with improved crack deflection and mechanical stability
(Borom et al., 1975). The high proportion of the Li2Si2O5 to glassy phase and
applied heat and pressure lead to crystal alignment, with the mechanical fracture
toughness anisotropy. Specifically, the susceptibility to crack formation and
propagation is significantly reduced in the direction perpendicular to crystal
alignment.
As with other processes, the addition of a sintering aid into the ceramics
precursor allows for property tunability of the resultant material. For example, hot
pressing was used to produce fully dense ceramics from magnesium aluminate
spinel (MgAl2O4) with a good optical transparency (>80% throughout the visible
spectrum). The determining parameter in attaining the high transparency was the
addition of 0.25 wt% LiF agent prior to hot pressing at 1600 C under vacuum and
20 MPa uni-axial load, followed by hot isostatic pressing at 1850 C under
200 MPa Ar atmosphere (Sutorik et al., 2012). Other variables that affect the
transparency of the resultant MgAl2O4 ceramics include heating rate, temperature,
powder treatment and pressure at which the processing takes place. Recently,
spark plasma sintering has been suggested as a good method for the production of
transparent MgAl2O4 ceramics, which was found to be a superior technique
compared to both hot pressing and hot isostatic pressing methodologies (Fu et al.,
2013). Within a few minutes, the technique promises to achieve an almost full
densification, resulting in a restricted grain growth and uniform grain-size
distribution compared to that obtained using hot pressing.
Another approach used to produce dense ceramics is sequential dry pressing
and sintering, where an over-sized specimen (1020% larger than the final
implant) is first fabricated using a computer-designed die and then sintered at a
temperature of about 1550 C. This production method is commonly used on high
purity Al2O3-based ceramics and results in a high degree of crystallinity and a
small distribution of grain size around a mean of 4 m, the bending strength of
approximately 600 MPa, and good in vivo stability for many years of use. Since
the high crystallinity of the bulk material renders it opaque and not aesthetically
pleasing for dental applications, the resultant product often undergoes finishing
coating using a translucent porcelain veneer. The methodology is also suitable for
fabrication of fine stabilised zirconia powders (Laberty-Robert et al., 2003). Uniaxial dry pressing and sintering (14001550 C, 2 hrs) of yttria partially stabilised
tetragonal zirconia yielded ceramics with a mean grain size of 0.26 to 0.57 m

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(Kosma and Kocjan, 2012). The temperature at which sintering took place
affected the ageing characteristics of different ceramics. Furthermore, the
properties of the powdered precursors had the greatest effect on ageing when
sintered at lower temperatures, and minimal effect at higher sintering temperatures.
Important powder characteristics include their ability to flow freely into the die
and be packed with a minimal gradient; these will depend on the size and
distribution of ceramic particles within the powder, their granular conformation
(size, shape, distribution), the deformation that these granules undergo during
pressing, etc.
For the fabrication of glass-infiltrated ceramics of spinel (MgAl2O4), alumina
and ceria-stabilised ZrO2/Al2O3 nanocomposite, a process involving slip-casting,
sintering and infilling is used (Bajpai and Bhargava, 2012; Della Bona et al.,
2008). Slip-casting is first used to produce a highly porous three-dimensional
structure from the aforementioned crystalline materials, which are then sintered at
the temperatures appropriate for the chosen crystalline phase to produce a highly
stable crystalline network. Then a lanthanum-based glass is introduced into the
structure to produce the glassy phase network (Yang et al., 2012b). Sandblasting
can be used to remove any excess glass. For Al2O3-based ceramics, the glassy
phase represents approximately 27% of the material by volume at 5% porosity.
The crystalline phase is composed of grains with wide size and shape distribution.
As with previously discussed ceramics, the difference in the coefficient of
thermal expansion between the crystalline and glassy phases accounts for the
microcrack formation and bridging, thus enhancing the mechanical properties of
the material. Among the glass-infiltrated ceramics, MgAl2O4 has superior
translucidity compared to Al2O3-based ceramics; however, the strength and
fracture resistance is higher in the former material (Sutorik et al., 2012). Glassinfiltrated ceria-stabilised ZrO2/Al2O3 structures consist of 34 vol% Al2O3, 33
vol% of ceria-stabilised ZrO2 and 23 vol% glass phase, with a resultant porosity
of approximately 8 vol%. The use of two different crystalline phases improves the
mechanical toughness of the resultant ceramics, where zinc grains contribute to
microcrack nucleation (due to compressive and circumferential tensile stresses
associated with zirconia grains) and alumina grains provide crack deflection,
contact shielding and crack bridging.
Hard machining involves the computer-aided machining of fully sintered
ceramics in order to produce implantable components. The process is associated
with considerable tool wear and results in the abundance of surface defects that
may compromise the in vivo stability and compatibility of the material. A range of
ceramics are based on feldspar, leucite, sanidine (Na,KAlSi3O8), lithium disilicate,
alumina and zirconia (Denry et al., 2001). However, soft machining uses partially
crystallised ceramics that can be post-treated with glass-infiltration, sintering, hot
pressing, etc. to attain final mechanical strength. The obvious benefit is the ease
with which these ceramics can be machined. For example, partially crystallised
lithium disilicate-based ceramics, containing both metasilicate (Li2SiO3) and

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disilicate (Li2Si2O5) crystals, are characterised by a lower strength of 130 MPa.


Both soft and hard machining processes incur a notable amount of wastage of the
ceramic material, and involve a ceramic preform containing a high degree of
detail regarding the implant uniformity, compaction density and robustness to
enable computer machining.
A number of additive production methodologies have been developed to
fabricate complex ceramic structures in a more time and economically efficient
manner and increase the accuracy with which the implant is manufactured. The
methodologies are based on the availability of small modular elements that can be
assembled quickly yet reliably. Stereolithography is a cost-effective method that
involves laser polymerisation of an UV curable monomeric system followed by
removal of organic particles (Chartier et al., 2002). Robocasting is another
computer-aided design/computer-aided manufacturing process, where ceramic
paste is deposited in a layer-by-layer sequence to build up core and fixed partial
denture structures (Silva et al., 2011). Selective laser sintering is a type of solid
freeform fabrication in which a ceramic part is generated in layers from powder
using a computer-controlled laser/scanning apparatus and power feed system
(Bourell et al., 1992). Three-dimensional printing allows for manufacture of
tooling and functional prototype parts directly from computer models via the
deposition of powdered material in layers and the selective binding of the
powder by ink-jet printing of a binder material (zkol et al., 2012; Sachs et al.,
1992).

7.4

Conclusion

Inert ceramics are characterised by a favourable combination of mechanical


strength, corrosion and wear resistance, making them well suited for a wide range
of load-bearing applications, most notably as integral components of artificial
joints and in dentistry. Indeed, alumina ceramics are frequently used for the
fabrication of femoral joint heads to be used in conjunction with an ultra-high
density polyethylene acetabular liner in hip arthroplasty. From a mechanical wear
point of view, a ceramicceramic pairing would be even more beneficial, since it
would reduce the incidence of the aseptic loosening associated with polymer
wear. However, limited in vivo soft and hard tissue integration of alumina and
other bio-inert ceramics leads to loosening of all-ceramics-based acetabular
sockets in the pelvic bone. Along with brittleness, such poor osseo-integration
hinders the potentially beneficial clinical applications of these ceramics. To
circumvent these issues, several bio-activation strategies have already been
reported. Among them, sodium hydroxide treatment and surface immobilisation
of biological agents have already been demonstrated to successfully improve cell
adhesion, proliferation and secretion of osteocalcin in the absence of the
deteriorating effect on the short- and long-term strength behaviour. However,
more research into the surface modification of ceramics is required to ensure that

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sufficient levels of cementbone interaction take place if these materials are to be


used clinically. This has resulted in second- and third-generation ceramic
materials, which are discussed in Chapter 8.

7.5

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