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Zirconia based dental ceramics: structure,

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Cite this: DOI: 10.1039/c6dt03484e

mechanical properties, biocompatibility and
applications
Chandkiram Gautam,*a,b Jarin Joyner,a Amarendra Gautam,b Jitendra Raoc and
Robert Vajtaia

Received 7th September 2016,
Accepted 30th October 2016
DOI: 10.1039/c6dt03484e
www.rsc.org/dalton
Zirconia (ZrO2) based dental ceramics have been considered to be advantageous materials with adequate
mechanical properties for the manufacturing of medical devices. Due to its very high compression
strength of 2000 MPa, ZrO2 can resist differing mechanical environments. During the crack propagation
on the application of stress on the surface of ZrO2, a crystalline modification diminishes the propagation
of cracks. In addition, zirconia’s biocompatibility has been studied in vivo, leading to the observation of no
adverse response upon the insertion of ZrO2 samples into the bone or muscle. In vitro experimentation
has exhibited the absence of mutations and good viability of cells cultured on this material leading to the
use of ZrO2 in the manufacturing of hip head prostheses. The mechanical properties of zirconia fixed
partial dentures (FPDs) have proven to be superior to other ceramic/composite restorations and hence
leading to their significant applications in implant supported rehabilitations. Recent developments were
focused on the synthesis of zirconia based dental materials. More recently, zirconia has been introduced
in prosthetic dentistry for the fabrication of crowns and fixed partial dentures in combination with compu-
ter aided design/computer aided manufacturing (CAD/CAM) techniques. This systematic review covers
the results of past as well as recent scientific studies on the properties of zirconia based ceramics such as
their specific compositions, microstructures, mechanical strength, biocompatibility and other applications
in dentistry.

1. Introduction ZrO2 is a bioceramic that was first investigated by the

The etymology of the word ‘ceramic’ derives from the Greek
word keramos, which means pottery or burnt article. Today, the
word ‘ceramic’ has a more expansive meaning and includes
materials such as glass, advanced ceramics and cement
systems as well. Ceramics are generally inorganic, nonmetallic
solids synthesized by proper heat treatment and subsequent
cooling. They are related to a combination of covalent, ionic,
and seldom metallic bonding. Ceramic materials may be crys-
talline, partly crystalline or non-crystalline.1 Crystalline cer-
amics are composed of either pure or glass ceramics. ZrO2
based ceramics have been considered to be very important
materials for medical device applications.2–6
a
Department of Material Science and Nano Engineering, 6100 Main MS-325,
Rice University, Houston, Texas 77005, USA
b
Department of Physics, University of Lucknow, Lucknow - 226007, Uttar Pradesh,
India. E-mail: gautam_ceramic@yahoo.com
c
Department of Prosthodontics, Faculty of Dental Sciences, King George Medical
University, Shah Mina Road, Chowk, Lucknow - 226003, Uttar Pradesh, India
German chemist Martin Heinrich Klaproth in 1789.7 The first
research paper on the use of ZrO2 as a biomaterial was pub-
lished by Helmer and Driskel in 1969.8 In the last ten years,
the use of ZrO2 based ceramics as a biomaterial for implants
and dental crowns in dentistry has risen significantly, due to
the superior mechanical properties of ZrO2, such as its high
mechanical strength, biocompatibility, as well as its very high
wear resistance and friction.9,10 In the research field of dentis-
try, the use of ZrO2 in dental restoration applications has been
a practice since 1998 due to its very high strength for load
bearing as dental crowns, fixed partial dentures (FPDs) and
dental implants.11,12 Therefore, ZrO2 takes a remarkable
place amongst the various oxide ceramics due to its excellent
mechanical as well as biocompatible properties. It is well
known that the different stages of ZrO2 polymorphs are temp-
erature dependent; at ambient pressure, zirconia can assume
three crystallographic forms. Pure zirconia is monoclinic (m),
under ambient conditions. With increasing temperature, the
material transforms to a tetragonal crystal structure (t) at
∼1170 °C and then to a cubic crystal structure (c), followed by
a fluorite structure at ∼2370 °C with melting at 2716 °C.13–16

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Fig. 1 Crystallographic phase change with the variation of temperature of the three ZrO2 phases.17,18

The ZrO2 ceramic shows a hysteretic, martensitic t → m trans-
formation during the heating and cooling processes, while its
reversible transformation occurs at ∼950 °C upon cooling.
Pure zirconia along with various stabilizing oxides such as
CaO, MgO, Y2O3 or CeO2 allows the retention of the tetragonal
structure at room temperature. Therefore, it controls
stress-induced transformations. It is reported that ZrO2 has a
high temperature stability and melting point (2680 °C), high
hardness (1200–1350 HVN), a high thermal expansion
coefficient (>10 × 10–6 K−1), low thermal conductivity
(<1 W m−1 K−1) and a high thermo-shock resistance (ΔT =
400–500 °C).10 All possible crystallographic phase changes
with temperature are shown in Fig. 1.17,18
2. Stabilizing high temperature
phases of zirconia
The doping of various oxides that are dissolvable in zirconia
(CaO, MgO, Y2O3) lowers the crystal structure from tetragonal
to monoclinic (t–m) and cubic to tetragonal (c–t) phase trans-
formation temperatures. This doping is therefore said to be
stabilizing the high temperature phases. The amount of alloy-
ing oxide required to produce this respective stabilization is
determined from the relevant phase diagram, which can be
seen in Fig. 2 for the zirconia–yttria system.19 In principle, any
composition which is sintered in the cubic phase and retains a
wholly cubic crystal structure on cooling is considered to be
fully stabilized. The continued possession of the tetragonal
phase at room temperature will also be feasible, provided that
the tetragonal to monoclinic phase transformation is inhib-
ited. This can be achieved by a combination of fine powders,
matrix constraints and stabilizing additions of dopants.
In the recent years, the use of bioceramic restorations has
increased due to their superior aesthetic appearance, bio-
compatibility, machinability and the absence of any metal content
as compared to other materials.20 Zirconia based bioceramic
materials, especially yttria-tetragonal zirconia polycrystals
(Y-TZPs), have recently been included for prosthetic rehabilita-
tions as a core material for single crowns, and conventional as

Dr Chandkiram Gautam, a senior Jarin Joyner received his

Assistant Professor of Physics,
received his BSc and MSc in
Physics from CCS University,
Meerut in 1995 and 1997 respect-
ively. Dr Gautam did an MPhil in
Physics at IIT Roorkee. He received
his MTech in Materials
Technology in 2000 and a PhD
degree in Ceramic Engineering in
2005 from IIT BHU, Varanasi. He
received the Raman Post-Doctoral
Chandkiram Gautam Research Award Fellowship
(2014–2015) from UGC, India
and completed at Rice University, Houston, Texas, USA. He was
awarded the UGC Research Fellowship during 2012–2013.
Dr Gautam is a recipient of the ‘Young Scientist’ Award from UPCST,
Lucknow (2007). His research area is glass and nano-bioceramics.
Bachelor’s degree in chemistry
from Oberlin College and his
Master’s degree in organic chem-
istry from Georgia State
University. His research pursuits
are concentrated in energy
storage, and investigating
polymer composites to be uti-
lized as separators and binders
in lithium ion battery systems at
high temperatures. Jarin enjoys
Jarin Joyner spending his free time as a free-
lance classical violinist.

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Fig. 2 Phase equilibrium diagram for the zirconia yttria system and
showing the phase transformation with variation temperature vs. mol%
of Y2O3.19
well as resin-bonded fixed partial dentures (FPDs) in dental
implantology.21,22 Nowadays, the combination of Y-TZP and
computer aided designs and computer aided manufacture
(CAD/CAM) systems is a new worthy approach that reduces the
number of steps in prosthetic manufacturing and eliminates
the variables introduced by the manual procedures of the
Amarendra Gautam did his B.Sc.
in Science at the University of
Lucknow in 2009. He received
his M.Sc. degree from Baba
Saheb Bhimrao Ambedkar
University, Lucknow in 2014 in
Applied Physics. Currently he is
pursuing a Ph.D. under the
supervision of Dr C. R. Gautam,
Department of Physics,
University of Lucknow and he is
working on HAP based nano-
Amarendra Gautam bioceramic materials for bone
implants.
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Fig. 3 Representation of the (a) milling process of zirconia Cercon; (b)
the core of zirconia Cercon.29
dental technician. Y-TZP exhibits unusual physical and mech-
anical properties, such as high flexural strength, fracture
toughness, hardness, corrosion resistance, wear and tear
under both acidic as well as basic ambient conditions, translu-
cency, color stability, greater effectiveness of diagnostic radio-
graphs and high biocompatibility.23–25 To enhance the
bonding between zirconia frameworks and veneering porce-
lain, surface roughness is increased with variable grained
alumina based abrasives and the use of interlayers is also in
current practice. Furthermore, in spite of the use of CAD/CAM,
the final steps involving strong mechanical action on zirconia
components must continue to be performed by dental tech-
nicians.26,27 One of the first researchers who used CAD/CAM
techniques for the fabrication of tooth restoration devices was
Duret in the 1970s.28 Fig. 3 shows a tooth crown fabricated
from a pre-sintered zirconia core, which was milled using
CAD/CAM (Cercon, Dentply).29 Different important mechan-
ical, thermal and electrical parameters of zirconia are listed in
Table 1.
Dr Jitendra Rao, MDS
(Prosthodontics), is currently
working as a professor in KGMU,
Lucknow. Implant dentistry and
clinical prosthodontics are his
major areas of interest. After
postgraduation from KGMC, he
joined as a senior resident (SR)
in the same department followed
by a SRF in a WHO collaborative
project with the Ministry of
Health & Family Welfare (GOI),
Jitendra Rao before joining as a lecturer in the
same department. He has been
honored with a certificate of excellence for his work and conduct
during his senior residency by the Dean, Faculty of dental sciences.
He received the Science and Technology innovation award from
the Hon’ble Chief Minister of UP in 2016. He also has to his credit
about 42 national and international publications.
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Table 1 Mechanical, thermal and electrical properties of zirconia

Minimum Maximum Minimum Maximum

Property value (S.I.) value (S.I.) Units (S.I.) value (Imp.) value (Imp.) Units (Imp.)
−1
Atomic volume (average) 0.02 0.021 3
m kmol 1220.47 1281.5 in3 kmol−1
Density 5 6.15 Mg m−3 312.14 383.932 lb ft−3
Energy content 200 300 MJ kg−1 21667.7 32501.6 kcal lb−1
Bulk modulus 72.3 212 GPa 10.4862 30.748 106 psi
Compressive strength 1200 5200 MPa 174.045 754.196 ksi
Elastic limit 115 711 MPa 16.6793 103.122 ksi
Endurance limit 107 640 MPa 15.519 92.8241 ksi
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Fracture toughness 1 8 MPa m1/2 0.910047 7.28037 ksi in1/2

Hardness 5500 15 750 MPa 797.708 2284.35 ksi
Loss coefficient 0.0005 0.001 0.0005 0.001 Null
Modulus of rupture 177 1000 MPa 25.6717 145.038 ksi
Poisson’s ratio 0.22 0.32 0.22 0.32 Null
Shear modulus 53.4 86.4 GPa 7.74501 12.5313 106 psi
Tensile strength 115 711 MPa 16.6793 103.122 ksi
Young’s modulus 100 250 GPa 14.5038 36.2594 106 psi
Latent heat of fusion 700 820 kJ kg−1 300.944 352.535 BTU lb−1
Maximum service temperature 1248 2522 K 1786.73 4079.93 °F
Melting point 2823 2973 K 4621.73 4891.73 °F
Minimum service temperature 0 0 K −459.67 −459.67 °F
Specific heat 420 540 J kg−1 K−1 0.32502 0.417883 kJ/kg °K
Thermal conductivity 1.7 2.7 W m−1 K−1 3.18246 5.05449 W K−1 m−1
Thermal expansion 2.3 12.2 10−6 K−1 4.14 21.96 10−6 °F−1
Breakdown potential 4 6 MV m−1 101.6 152.4 V per mil
Dielectric constant 10 23 10 23 Null
Resistivity 3.16 × 1013 3.16 × 1018 10−8 ohm m 3.16 × 1013 3.16 × 1018 10−8 ohm m

3. Advantages of zirconia and of zirconia based ceramics may be compromised when

zirconia based ceramics
Zirconia is considered to be a suitable ceramic material for
dental and other biomedical applications due to its high resist-
ance to corrosion and light weight. In addition, zirconia based
ceramics have superior properties such as high biocompati-
bility compared to other ceramics.30,31 However, the properties
Dr Robert Vajtai joined Ajayan’s
group at the Rensselaer
Polytechnic Institute in July 2000
to spend his sabbatical with a
NATO-NSF Fellowship. Robert
received his M.S. degree in
physics and his Ph.D. degree in
solid-state physics from the
University of Szeged, Hungary, in
1986 and 1997, respectively. He
received the Bolyai Fellowship of
the Hungarian Scientific
Robert Vajtai Academy from 1999 to 2000. He
also spent his sabbatical time as
a Fellow of the Swedish Institute in The Ångström Laboratory in
Uppsala, Sweden, from 1998 to 1999; as an Eötvös Fellow at the
EPFL in Lausanne, Switzerland, from 1995 to 1996, and he also
visited the Max Planck Institute in Göttingen, Germany in 1993
via the Max Planck Fellowship. His work is focused on the syn-
thesis and applications of nanomaterials.
exposed to considerable heat and moisture.32,33 In the late
1960s, zirconia was studied as a potential biomaterial known
as tetragonal zirconia polycrystals (TZPs). It was found that its
properties were ideal for the construction of hip prostheses as
well as for dental restorations. In 1975, British physicist Ron
Garvie found that the tetragonal structure of ZrO2 could be
stabilized by doping of ∼5.5% yttrium oxide, resulting in an
extremely hard and tough ceramic material. This process
improved its mechanical properties and enhanced its high bio-
logical stability. Furthermore, zirconium’s sheer strength
prompted its nickname, ‘ceramic steel’, and over the past two
decades it has debuted in the field of dentistry first for the fab-
rication of strong crowns, and more recently as a strong, tooth-
colored and metal-free dental implant material. Zirconia has
mechanical properties very similar to that of stainless steel. Its
resistance to traction lies in the range of 900–1200 MPa and its
effective compression resistance is ∼2000 MPa.34 Decades of
research have shown that a zirconia bridge can retain its
strength even after a time period of 50 years. In addition,
studies have also reported that zirconium is extremely bio-
compatible, and does not cause allergic symptoms to human
beings during implantation processes.35
Other significant advantages of ZrO2 over other ceramics
include: (i) natural: zirconium implants are extremely advan-
tageous over titanium or any other metal implants for the jaw
in order to create fixed teeth replacements. Therefore, ZrO2
implants are a holistic, natural choice for dental implants.
(ii) Hygienic: zirconium dental implants are shown to retain
less plaque than their titanium counterparts, which will
promote healthier gums around the implant. (iii) Aesthetics:

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zirconium has the advantage of its bright and white tooth like
color, which as a base for a tooth replacement, appears even
more natural than crowns with metal implants underneath.
The white color of ZrO2 implants also eliminates the possi-
bility of a darkened gum line that sometimes occurs due to
metal implants. (iv) Strength: zirconium is the second stron-
gest material found in nature (next to diamond), and the
strength of zirconium implants is equal to that of titanium
implants. (v) Biocompatible: zirconium is inert in nature and
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(1680–1800 °C) than other composites. Furthermore, Mg-PSZ
has poor stability, which may slightly lower the energy for
tetragonal to monoclinic phase transformation. The micro-
structure of Mg-PSZ consists of an array of cubic zirconia par-
tially stabilized by 8 to 10 percent (by mol) of magnesium
oxide. Due to the difficulty in obtaining free silica, Mg-PSZ pre-
cursors (SiO2), magnesium silicates can form a low content of
magnesia, favoring the tetragonal to monoclinic phase trans-
formation and resulting in lower mechanical properties and

therefore it does not cause any allergic reactions. Moreover, it
shows extraordinary toughness and resistance against wear
and tear. The comparative characteristics of some ceramics for
biomedical applications have been listed in Table 2.36,37
4. Types of zirconia used in dentistry
stability of the synthesized material. Fully sintered blocks have
been manufactured with this material and require rigid and
strong machining systems. A dental ceramic system called
Denzir-M (Dentronic AB, Skellefteå, Sweden) is an example of
a fully sintered Mg-PSZ ceramic for dental crown and bridge-
work.40 Fig. 4 shows the microstructural features of the major
categories of transformation of toughened zirconia with

In spite of the fact that there are so many different types of

zirconia, only three types of ZrO2 are used to date in dentis-
try.38,39 The first of these types are zirconia ceramics with at
least two ZrO2 tetragonal phases as a minor phase dispersed
and precipitated, respectively. The origin and details of the
stabilization of the tetragonal phase differ among these three
toughened microstructures. These have evolved as researchers
and manufacturers have sought to exploit the different pro-
perties of the various phases of ZrO2 that form at different
temperatures (as discussed in section 1). These phases are
stable at high temperatures and need to be frozen in such a
manner that they can be used at room temperature, while
others exploit toughening mechanisms that are only found in
these and a few other materials. The three materials share the
requirement of stabilizing the tetragonal phase whereas tough-
ening involves the martensitic transformation. The raw
materials of zirconia are the minerals zircon (ZrSiO4) and bad-
deleyite (β-ZrO2).

4.1 Magnesium partially stabilized zirconia (Mg-PSZ)

Mg-PSZ is reportedly an unsuitable composite for use in den-
tistry because of its high porosity and large grain size, which
may lead to surface wear and large crack propagation. The sin-
tering temperature of this type of zirconia is also much higher
Fig. 4 Microstructural features of the major categories of transform-
ation-toughened zirconia: (a) zirconia toughened alumina (ZTA), (b) Mg
partially stabilized zirconia (Mg-PSZ), (c) yttria-stabilized tetragonal zir-
conia polycrystalline (Y-TZP) and (d) fully stabilized zirconia (FSZ) with
large grains of ZrO2.41–44

Table 2 Characteristics of some ceramics for biomedical applications31,32

Silicon
Property Units Alumina Mg-PSZ TZP TZP-A Hydroxyapatite carbide

Chemical composition 99.9%+ ZrO2 + 8–10 mol% ZrO2 + 3 mol% ZrO2/Y2O3/Al2O3 Ca10(PO4)6(OH)2 SiC
MgO MgO Y2O3 95/5/0.25
Density g cm−3 ≥3.97 5.74–6 >6 6.05 3.1 3.2
Porosity % <0.1 — <0.1 0 — —
Bending strength MPa >500 450–700 900–1200 1200 600 —
Compression strength MPa 4100 2000 2000 2000 ∼1000 2000
Young’s modulus GPa 380 200 210 210 100–200 410
Fracture toughness, KIC MPa m−1 4 7–15 7–10 12 ∼3 —
Thermal expansion K−1 8 × 10−6 7–10 × 10−6 11 × 10−6 11 × 10−6 — 4.3
coefficient
Thermal conductivity W m−1 K−1 30 2 2 2 — 84 × 10−6
Hardness HVN 0.1 2200 1200 1200 1200 350 —

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different morphologies of grains and grain boundaries which
are fully developed and uniformly distributed throughout the
matrix.41–44 More recently, Mg-PSZ systems have been investi-
gated in order to achieve favorable mechanical properties by
using powder processing methods and post sintering aging
treatments above and below the eutectoid temperature in sub
and pro-eutectoid ageing treatments. The composition ranges
studied successfully, along with the aging temperatures used
are shown in Fig. 5.45 It was soon realized that the aging kine-
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tics of sintering and appropriately cooled Mg-PSZ materials
above the eutectoid temperature was too rapid to control the
tetragonal precipitate crystal growth and therefore enabled the
production of material properties suitable for a variety of
industrial applications.
4.2 Zirconia toughened alumina (ZTA)
It is reported that the nanocomposites of Al2O3–ZrO2 have a
high resistance with respect to crack propagation, which can
improve the lifetime and reliability of ceramic joint pros-
theses.46,47 At room temperature, the stability of the tetragonal
phase did not initially involve the use of doping, but instead is
controlled by the grain size, morphology and particle size (intra-
or inter-granular). The possibility to synthesize Al2O3–ZrO2 nano-
composites has been evidenced by refining powder processing
using a new colloidal synthetic route.48,49 These new composites
can exhibit not only greater toughness but more importantly, a
greater threshold for the stress intensity factor, under which
crack propagation does not take place. Although there is a rela-
tively low concentration of zirconia, i.e. 10 percent in volume, in
these composites, they show a similar hardness value in com-
parison with other materials such as Al2O3 and are not suscep-
tible to the hydrothermal instability observed in some cases of
stabilized zirconia bioceramics. In ZrO2 toughened alumina, for
example, particles above a critical size will transform to the
monoclinic symmetry upon cooling to room temperature.50
Since, this tetragonal to monoclinic phase transformation is
known to be martensitic, thus, a useful way to describe particle
size effects is to examine their influence on the martensitic start
Fig. 5 Zirconia rich end of the ZrO2–MgO phase equilibrium diagram
indicating the composition range for Mg-PSZ ceramics. Arrows indicate
the sub and proeutectoid ageing temperatures.45
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(Ms) temperature; essentially all tetragonal phase stabilization
can be viewed as decreasing the value of Ms to below room
temperature. Such investigations have suggested that the particle
size effect is likely due to difficulties in nucleating the phase
transformation. However, consideration has also been given to
the possible effects of surface and strain energy and chemical
free energy driving forces. In contrast to the other two classes,
the stability of the tetragonal* (*indicating metastability) phase
at room temperature does not primarily involve the use of
dopants, but rather is controlled instead by the particle size, par-
ticle morphology and location (intra- or inter-granular; Fig. 4a).
4.3 Yttria full stabilized tetragonal zirconia polycrystal
(3Y-TZP)
The addition of approximately 2 to 3 percent of yttria, Y2O3 by
mol as a stabilizing agent in ZrO2 allows the sintering of fully
tetragonal fine-grained zirconia ceramic materials made of 100
percent small metastable tetragonal grains, known as Y-TZP.51
The TZP stabilized with 3 mol percent of 3Y-TZP zirconia has
been utilized for different dental applications since the mechan-
ical properties are similar to that of metals, whereas the
color approximates that of natural teeth. To date, studies on
the potential of 3Y-TZP zirconia bioceramics in dental appli-
cations continue to increase. Therefore, more information and
further detailed studies are needed to identify the capabilities
of these materials as bio-compatible. 3Y-TZP has superior
mechanical properties than those of other ZrO2 based
materials. Like poly-crystalline materials, 3Y-TZP shows low
porosity and very high density.52 The grain size significantly
influences the mechanical properties of zirconia 3Y-TZP,
whereas high temperature and longer sintering periods
produce larger grain sizes and will subsequently diminish the
mechanical properties due to large pore sizes.53 Therefore,
higher sintering temperatures lead to larger grain sizes.
Consequently, the sintering process becomes the determining
factor and thus the process control needs to be emphasized.
The 3Y-TZP bioceramic consists of an array of partially
stabilized zirconia with 2 mol percent of Y2O3. The ZrO2 fine
grains (usually <0.5 mm) with small concentrations of Y2O3
stabilizers can contain up to 98 percent of the metastable tetra-
gonal phase after sintering. The main feature of this micro-
structure is to be formed by tetragonal grains of uniform dia-
meter in the order of nanometers, sometimes combined with
a small fraction of the cubic phase. As explained above, the
yttria-stabilized zirconia (YSZ) is suitable for optical and solid
oxide fuel cell (SOFC) applications due to its high refractive
index and electrical conductivity, low absorption coefficient
and high opacity in the visible and infrared spectra. The criti-
cal grain size for this material is in the order of 1 μm, i.e. if the
size exceeds 1 μm, then 3Y-TZP becomes prone to phase trans-
formation toughening because of the its lower stability.
Meanwhile, if the grain size is smaller than 1 μm, this
phenomenon does not occur. In addition, zirconia having a
grain size below 0.2 μm does not undergo this phase trans-
formation toughening and thus its fracture toughness
decreases.54 3Y-TZP was first applied in the medical field of
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Fig. 6 (a and b) Micrographs of different zirconia 3Y-TZP ceramic
blocks showing well interconnected fine grains of ZrO2 embedded with
Y2O3 grains.55
orthopedics, with significant success due to its good mechan-
ical properties and biocompatibility. Prosthetic restorations
with 3Y-TZP are obtained by milling pre-sintered blocks, fol-
lowed by either another subsequent sintering performed at a
high temperature, or by machining sintered blocks completely.
Fig. 6(a and b) display the scanning electron micrographs
(SEM) of different zirconia 3Y-TZP bioceramic blocks.55 The
blocks are machined with the help of CAD/CAM systems and
in the case of pre-sintered blocks, prosthetic restorations are
pre-shaped into a size 25 to 30 percent higher than desired
(depending on the batch compositions) to compensate for the
sintering, or shrinkage in the final product. The final sintering
temperature is between 1350 and 1550 °C.56 This processing
reduces the level of tension present and prevents the trans-
formation from the tetragonal to monoclinic phase, which
leads to a final surface virtually free of the monoclinic phase.
5. Biocompatibility of zirconia and
zirconia composite ceramics
The allergic reaction produced by some metal alloys is a disad-
vantage of metal ceramic restorations which in turn has led
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to the increase in the demand of more biocompatible
ceramic implants for restorations. However, the degree of cyto-
toxicity of the metal alloys largely depends on the type of
dental alloy used in the fabrication of metal ceramic restora-
tions.57 Generally, zirconia based ceramics are chemically
inert materials, which have no adverse effect or general tissue
reactions. As the ceramic prostheses are made with highly
polished surfaces, they can contact the gum tissue and assist
in the maintenance of the gingival architecture. Depending on
the smoothness, the ceramics prevent the build-up of plaque,
creating a favorable surface for gingival tissues. Zirconia based
materials, allowing good cell adhesion and no adverse sys-
temic reactions have been associated with it. However, par-
ticles from the degradation of zirconia at low temperatures or
from the manufacturing processes can be released, promoting
an immune localized inflammatory reaction.
The biocompatibility of ZrO2 has been extensively evaluated
and both in vitro and in vivo studies have confirmed the high
biocompatibility of Y-TZP with the use of very pure zirconia
powders that have been purged of their radioactive
content.58–65 No local or systemic adverse reactions were
reported to this material.66,67 Recent studies have demon-
strated that fewer bacteria accumulate around the Y-TZP
material than titanium, which can be potentially explained by
different protein adsorption properties.68–71 Additionally, the
release of metal ions may cause gingiva discoloration, which
would further decrease the visual aesthetics.72 Besides promot-
ing high cosmetic requirements, other advantageous pro-
perties of ceramic materials are the biocompatibility and
chemical stability. The strongest dental ceramic commercially
available is 3 mol percent of yttria stabilized tetragonal zirco-
nia polycrystals (3Y-TZPs), shortened as zirconia. This material
has become the most popular choice for the dental core and
multiple units’ framework.73 The biocompatibility of the
(Y,Nb)-ZrO2/Al2O3 composite was evaluated by means of an
in vitro cytotoxicity test and an in vivo subcutaneous implant
test.74,75 Recently, Joon Kim et al. reported the biocompatibil-
ity of the (Y,Nb)-TZP/Al2O3 composite abutments for dental
implants. This biocomposite material was prepared by using
20 mol percent of Al2O3 as a dopant and exhibited a highest
strength of the order of 700 MPa, toughness of 8.1 MPa m1/2
and showed no hydrothermal degradation while aging in an
autoclave. The biocompatibility of the composite ceramic
exhibited no cytotoxicity and no significant adverse soft tissue
response for up to a 3 month implant period in guinea pigs.
The cell growth and survival test micrographs are shown in
Fig. 7(a and b) and exhibit a favorable response of L929
fibroblast cells on (Y,Nb)-TZP/Al2O3 specimens, such as an
increased cell number according to the culture time and main-
tenance of a normal cell morphology.76 ZrO2 bio-composite
ceramic was successfully processed via spark plasma sintering
(SPS) at 1200 °C for 5 min. They reported that the strong
adherence and the absence of cracking at the interfaces indi-
cated the matching of fracture toughness gradation, providing
a cushioning between composite layers of functionally graded
materials (FGM). However, a desired variation in porosity
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Fig. 7 Cell growth and survival test: (a) fibroblasts cultured in the (Y,Nb)-TZP/20 vol% Al2O3 composite for 4 days (×100), (b) fibroblasts cultured in
the (Y,Nb)-TZP/20 vol% Al2O3 composite for 6 days (×100) and (c) cell (Saos-2) adhesion, (d) control sample, (e) HAp–Al2O3, (f ) Al2O3–YSZ.76,77
could not be achieved. Successive cell culture experiments
using L929 fibroblast and Saos-2 osteoblast like cells provided
clear evidence of cell adhesion and cell proliferation on the
surface of FGM, indicating good cyto-compatibility as shown
in Fig. 7(c–f ).77 In vitro and in vivo studies have also confirmed
a high biocompatibility of zirconia and composite dental cer-
amics based on it, especially when it is completely purified of
its radioactive contents.78,79 The biocompatibility of alumina–
zirconia composites was investigated by Konduk et al.80 Tissue
reactions of test materials were performed using rats for a two
month duration. As the amount of ZrO2 is increased, mullite
formation became visible on the particle boundaries. Animal
studies have revealed that these ceramic composites do not
have any adverse effects on the tissue investigated histo-
logically. Zeng et al. developed a new type of gradient ceramic
biomaterial.81 ZrO2 was selected as the substrate and the
Na2O–SiO2–B2O3–CaO glass system was chosen as a medium
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Dalton Transactions
for bonding HAp and ZrO2. After a 3 month implantation
period in the leg bone of a canine, the gradient bioactive
implant bonded with the bone and the bonding strength
between the gradient bioactive material implant and bone was
much higher than that between a pulse titanium implant and
bone. In vivo studies of carbon–carbon composites showed the
accumulation of platelets on the exposed surface material with
any surface morphology, whereas platelet concentration in the
blood remained constant.82
5.1 Biocompatibility in soft tissues
Several studies on various animals like rabbits, rats, mice,
dogs and monkeys have reported on the behavior of zirconia
based ceramics implanted into soft tissues. These in vivo tests
performed with different physical pins, bars, wear particles
and structural forms (TZP, PSZ, or coatings) of zirconia in
different sites of implantation led to the analysis of systemic
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Dalton Transactions Perspective

toxicity and adverse reactions in the implanted soft tissues.
Only a few studies have dealt with PSZ in rodent muscles com-
pared with alumina. When implanted in the para-spinal
muscles of rats for up to 12 weeks, zirconia polycrystals
(Y-PSZ) tended to become encapsulated with fibrous tissue as
observed for alumina control samples. Similarly, Y-PSZ
ceramic elicited the same response to alumina controls when
implanted subcutaneously into rats for a period of up to
12 months. Both materials became encapsulated by a thin
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hydroxyapatite was observed in direct contact with cell viability
and MTT assays. These observations were confirmed succes-
sively91 when the cytotoxicity of ZrO2–Y2O3 on human lympho-
cyte mitogens was compared with the one observed in cultures
of alumina and titania powders. All the materials tested (grain
size ≤44 µm) showed a dose dependent lymphocyte mitogen
inhibition. Alumina and zirconia cytotoxicities were similar
and both were lower than that of TiO2 rutile. Specially, the
cytotoxicity of ZrO2 powders (ceramic precursors) was higher

layer of fibrous tissue, which was independent of the implan-
tation time. In all cases, ZrO2 did not bring out any form of
adverse tissue reaction, suggesting that zirconia is a biocompat-
ible ceramic material. In conclusion, zirconia (despite the
physical form tested) does not succeed in causing cytotoxicity
in soft tissues even if fibers were found in lymph nodes after
intraperitoneal injection.83–85 Degidi et al. compared soft
tissue reactions to ZrO2 and titanium; they reported that
inflammatory infiltrate, micro-vessel density and vascular
endothelial growth factor expressions appeared higher
throughout the titanium implant than around those of ZrO2.
Moreover, cellular proliferation on ZrO2 surfaces is higher
than that on titanium ones.86
In vitro biocompatibility is also evaluated using cell cultures
which interact with the biomaterial; zirconia is currently used
as the femoral ball head in total hip replacements (THR) and
thus will make contact with soft tissues and blood cells
in vivo.87 Zirconia powders were tested with different cell lines
(Table 3) and some authors observed that ZrO2 has no cyto-
toxic effects when fibroblasts were co-cultured with it or with
extracts using different methods (viability of cells and MTT
assay).88,89 Scanning electron microscopy studies also reported
the adhesion and spreading of 3T3 fibroblasts.90 On the other
hand, a higher inhibition of cellular growth using zirconia and
tricalcium phosphate (TCP) powders rather than alumina or
than the cytotoxicity of powders obtained by the crushing and
milling of sintered ZrO2 ceramics. Ion release was tested in a
saline solution at a temperature of 37 °C (to 0.12 µg cm−2)
from plates of high density sintered materials (HIP, 160 MPa,
1225 °C, 2 h). In an acid solution, (lactic acid 0.02 M at 37 °C)
yttrium and zirconium ions increased (to 3 µg cm2), leading to
the conclusion that ZrO2 ceramics cannot be used in an acidic
environment i.e. the oral cavity.
5.2 Biocompatibility in hard tissues
The first comparative results with ZrO2 and other implanted
materials like Al2O3 have previously been reported by Wagner
and Christel, who used pins of zirconia (Y-TZP) or alumina
inserted into the femurs of rabbits and did not observe any
difference in the bone reaction to implants.92,93 Bar and cylin-
der forms of the implants were also implanted in the bones of
rats, rabbits, and mice without inducing or causing any local
or systemic toxic effects after the insertion of yttria-stabilized
zirconia. Finally, it appeared that the various forms of zirconia
tested in hard tissues do not induce any adverse reaction or
global toxic effects. Moreover, in light of these biocompatibility
tests, it became evident that zirconia, no matter the physical,
or structural form tested, is a biocompatible material.

Table 3 Details of the in vitro test on zirconia and zirconia based ceramics and powders

Material name Physical form Cell type Test name Observations Remarks Ref.

ZrO2 Particles Macrophages Cytotoxicity at Zirconia less toxic Higher phagocytosis 89

24 hours than polyethylene of zirconia than PE
CaPSZ Sintered ceramic 3T3 Fibroblasts SEM observation Adhesion and After 72 h cell monolayer 90
(30% porosity) spreading of cells onto (30% porosity)
ceramic samples
HAp–Al2 Spark plasma L929 fibroblast cells Cell viability MTT SEM Cell adhesion and cell 77
O3–YSZ sintered and Saos-2 proliferation
osteoblast cells
Y-PSZ Ceramic Human oral Colony forming Powders more toxic Toxicity related to specific 85
precursor and fibroblasts efficiency, MTT, than crushed and surfaces and ion release
sintered dissolution test milled ceramic
Y-PSZ Wear particles L929 fibroblasts Cell growth in the Wear product Toxicity is related to the 89
of UHMWPE presence of PECFs of UHMWPE presence of particles of
vs. Y-PSZ more cytotoxic zirconium hydroxides
than UHMWPE vs.
Ti6Al4V
Y-PSZ Powder Human lymphocyte Inhibition of cell Dose dependent Toxic effect of Y-PSZ similar 88
mitogenesis after cytotoxicity to alumina and lower than
PHA induction the ones of titania
Y-PSZ Powder Balb 3T3 and human Cell viability, MTT No cytotoxic effects Different levels of 85
osteoblasts sensitivity among the
tests used

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6. Dental applications of zirconia
based composite ceramic materials
6.1 Zirconia based implants
The reported studies demonstrate a bone implant contact for
zirconia dental implants, very similar to those of titanium
implants, and these findings suggest that ZrO2 dental
implants can reach firm stability in bones. More recently, the
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osseo-integration of zirconia dental implants was histologically
demonstrated in one human patient.94 In this study, a two-
piece zirconia implant was placed in the maxilla of a healthy
woman and 6 months after surgery, the retrieval of the dental
implant was performed. The surrounding soft and hard
tissues were gathered and processed for histological evaluation
and the processed sample of ZrO2 dental implants provided
the histological evidence of osseo-integration. Moreover, the
SEM analyses exhibited very good maintenance of the crestal
bone level; in fact, it was possible to evaluate the observations
that the first bone-to-implant contact was occlusal to the
implant abutment junction. This finding can be related to the
excellent characteristics of ZrO2 dental implants which present
high biocompatibility and low plaque adhesion.95 Another
retrospective study suggests that ZrO2 endosseous implants
can achieve a survival rate similar to that of titanium implants
with healthy and stable soft and hard tissues. In the work by
Brüll et al.,96 121 zirconia implants (66 two-piece implants and
55 one-piece implants) were inserted in 74 patients. After a
mean observation period of 18 months, the cumulative
implant survival rate was 96.5%. The clinical examination
revealed that the probing pocket depth (PPD) and bleeding on
probing (BOP) were significantly lower around implants than
around the teeth (mean PPD of 1.8 ± 0.4 mm; mean BOP
scores of 4.1% ± 4.2%), whereas the radiographic evaluation
demonstrated that peri-implant marginal bone levels were
stable (mean bone loss of 0.1 ± 0.6 mm) after the three-year
follow-up.
Kohal et al. reported an all ceramic custom made ZrO2
implant crown system for the replacement of a single tooth.97
The experimental study which was carried out on the mean
bone implant surface of rabbits was reported to be ∼68.4%.
Sennerby compared the osseo-integration and removal torque
of ZrO2 implants, titanium oxide implants, and zirconia with a
modified surface when these were inserted in the tibia and
femur of rabbits. He concluded that although osseo-
integration appeared similar between the different samples,
the removal torque of the pure zirconia implant was lower
than those of the other two implants, suggesting that surface
modification can improve ZrO2 implant stability.98 Titanium
implants with a coronal base in ZrO2 are also available, the
aim of which is to combine the safety of titanium with the aes-
thetic features of ZrO2.99 Moreover, an in vitro experimental
study pointed out that ZrO2 implants are able to sustain
chewing stresses nicely. The cyclical mechanical resistance of
ZrO2 implants with ceramic restorations in comparison with
that of traditional implant prosthodontic restorations was
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reported. The mean fracture load after cyclical stress in tita-
nium–porcelain fused to metal restorations amounted to 668.6 N,
whereas for zirconia implants with all ceramic restorations
fracture occurred at a mean load of 555.5 N. It was concluded
that ZrO2 implants are able to bear fatigue and stresses
sufficiently well for anterior teeth implant replacements.
Suarez studied the outcome 3 years after the placement of
ZrO2 ceramic restorations on 18 teeth. Only one tooth failed
after the experimental period because of radicular fracture.
According to this study, it is possible to consider ZrO2 resto-
rations as reliable and durable for clinical applications.100 In
terms of periodontal health, none of the studies reported any
difference or noted any changes in the biological character-
istics of the soft and hard tissues around the zirconia-based
restorations. Although some data quantified and explored dis-
tinction in the biocompatibility of ZrO2, no instances of gingi-
val inflammation or periodontitis could be shown.101 These
findings have led to the suggestion that ZrO2 may be a suitable
material for manufacturing implant abutments with a low
bacterial colonization potential. Recently, Zafiropoulos et al.
reported in their clinical study over a period of 3 years of study
that none of the patients reported any unusual pain or discom-
fort, nor the presence of abscesses, swelling, or allergic reac-
tions during the course of treatment. In addition, no implants
or natural teeth were lost during the observation period.
Furthermore, no fractures and failures were observed in the
ZrO2 abutments, the superstructures, or the ceramic veneers
as shown in Fig. 8.102
In further studies, a randomized controlled clinical trial
comparing zirconia and titanium abutments supported by 40
single implants was published.103 After being in function for
three years, 18 zirconia and 10 titanium abutments were fol-
lowed up in a study. Both abutment materials exhibited survi-
val rates of 100% as well as similar biological and esthetic out-
comes. In an adult pig animal study, it was shown that the col-
lagen fiber orientation was similar around ZrO2 and titanium
implant necks. For both ceramic as well as metallic materials,
the fibers run parallel-oblique and parallel to the implant
surface.104 More recently, in a clinical study, a similar degree
of plaque accumulation was found at ZrO2 and titanium abut-
ments for the period of three years. In the same study, when
ZrO2 abutments were used as a restoration support, there was
no significant difference in bone levels between ZrO2 and tita-
nium abutments after a 3-year follow-up.105
6.2 Zirconia based esthetic orthodontic brackets
Orthodontic brackets are passive components of fixed ortho-
dontic appliance bonded to the enamel which provide the
means to transfer the force applied by the activated arch-wire
to the tooth. Besides the dental applications that were men-
tioned previously, ZrO2 has also been applied for the fabrica-
tion of esthetic orthodontic brackets.106 The recent introduc-
tion of ZrO2 based ceramics as a restorative dental material
has generated considerable interest in the dental community.
According to Koutayas et al.,107 ZrO2 based orthodontic brack-
ets can be technologically feasible with the development of
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Fig. 8 Three-year clinical view. (a) Zirconia copings. (b) Zirconia implant abutment.102
CAD/CAM systems. High-strength ZrO2 frameworks can be
viable for the fabrication of full and partial coverage crowns,
fixed partial dentures, veneers, posts and cores, primary
double crowns, implant abutments, and implants. Heravi
states that in the future, the reduction in the curing time and
change in the light direction may increase the bond strength
and reduce enamel fracture during debonding processes.108
Polycrystalline ZrO2 brackets, which reportedly have the
greatest toughness amongst all ceramic materials, have been
offered as an alternative to Al2O3 ceramic brackets.109 They are
cheaper than crystalline Al2O3 ceramic brackets but are very
opaque and can exhibit intrinsic colors making them less
aesthetically favorable. Favorable sliding properties have been
reported with both stainless steel and nickel–titanium arch-
wires along with reduced plaque adhesion and clinically accep-
table bond strengths and bond failure loci at the bracket/
adhesive interface.110 Therefore, Y-TZP orthodontic brackets
provide enhanced strength, superior resistance to deformation
and wear, reduced plaque adhesion and improved
aesthetics.111
6.3 Zirconia-based crowns and bridges
Dental crowns are the caps that mimic the teeth by capping
and encircling the teeth, reconstructing their shape, size and
durability. The crowns are bonded to the tooth using dental
cement (resin or acid–base cements, the powder is a metal
oxide or silicate and the liquid is acidic), hiding the visible
part of the tooth below and above the gum line.112 Advanced
zirconium based crowns are taking the place of ordinary metal
and porcelain crowns. The advantage of this combination is
the natural translucency of the crown, which makes it possible
to successfully mimic a natural tooth. ZrO2 is often used for
anterior teeth due to the metal base not being able to be seen
in a ray of light. ZrO2 based restoration has superior mechan-
ical properties (fracture toughness, strength and hardness)
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comparable to that of the metal based materials113,114 which is
why it is feasible to prepare all ceramic crowns, bridges and
implants,115 making it a hot issue in stomatology.116–120 The
ZrO2 crown for dental applications is shown in Fig. 9.121
Tsalouchou carried out a study of 50 ZrO2 crowns, comparing
fracture resistance of two types of veneer ceramic: injected
ceramic and stratified ceramic over ZrO2 cores. The mean
resistance for the groups was ZirCAD + ZirPress (2135.6 ± 330.1 N)
and ZirCAD + IPS e.max Ceram (2189.9 ± 317.6 N), without
a statistically significant difference.122 Another important argu-
ment is the durability of a crown compared to all ceramic
crowns, which are also aesthetically favorable, but are totally
unacceptable for the posterior teeth. Clinical studies have
revealed a high rate of fracture for porcelain veneered ZrO2
based restorations that varies between 6 and 15% over a 3–5
year-period.123 These are high values compared to the 4% frac-
ture rate shown by conventional metal ceramic restorations
over 10 years, as shown in Fig. 10a.124 The cause of these frac-
tures is still a mystery, but might be associated with bond
failure between the veneered porcelain and the ZrO2 structure.
The ZrO2 porcelain interface may be involved in crazing and
Fig. 9 Zirconia crown for dental applications.121
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Fig. 10 Different grades of the crowns: (a) chipping of the ceramic
veneer on ceramo-metallic restoration, (b) grade 1 chipping of a zirconia
full-coverage crown (tooth 41) and (c) grade 2 of a zirconia full-coverage
crown (tooth 44).123
chipping during its functioning. Stresses could be related to
surface properties, as bulk thermal expansion or contraction
mismatches do not appear to be the cause.125 According to
Heintze and Rousson,126 the chipping of veneered porcelain
can be classified by severity and the treatment required for
repair as follows:
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Grade 1: small surface chipping. Treatment: polishing the
restoration surface (Fig. 10b). Grade 2: moderate surface chip-
ping. Treatment: use of a resin composite repair system
(Fig. 10c). Grade 3: severe veneer ceramic chipping with
exposure to the ZrO2 core. Treatment: replacement of the
damaged prosthesis. Literature reviews show that the most fre-
quent types of ZrO2 based fixed dental prosthesis chipping are
grades 1 and 2, which do not show restoration failure.127
After these observations regarding ZrO2 based crowns and
bridges we shift the focus to the behavior of ZrO2 as an abut-
ment material. The clinical applications of ZrO2 for abutment
can be divided into two main areas: first are the pre and
custom fabricated ZrO2 posts for endodontic treated roots.
Although, this procedure has been advocated by few dental
clinicians, the use of single visit fiber posts has proven to be
the method of choice when an endodontic treated tooth needs
to receive an endodontic post and build up a ZrO2 abutment
for oral implant reconstructions. Zirconia as an implant abut-
ment material as shown in Fig. 11, was first introduced in
1996.128 Based on its mechanical properties with the high frac-
ture toughness compared to all other ceramics,129 zirconia
seems not to be prone to fractures in clinical practice. In fact,
until today there has been no report on fractures of zirconia
implant abutments in any clinical study.130 However, long term
clinical trials on zirconia abutments are scarce and based on
observation periods of three to six years.131,132 Furthermore, most
of the studies on ZrO2 abutments are case reports. For example,
only four patients with six implants were treated in one of the
aforementioned studies with the longest follow up time of six
years.133 Sailer et al. investigated 58 zirconia bridges fabricated
Fig. 11 This sequence of clinical images shows a titanium implant
(Straumann, Basel, Switzerland) placed (a) in the left central incisor area
(segmented white arrow). (b) illustrates the occlusal view (black solid
arrow) and front view (white solid arrow) of a zirconia abutment (Cares
Abutment, Straumann, Basel, Switzerland) screw-retained on the
implant. (c) and (d) are the front and occlusal views respectively of the
final restoration cemented on the abutment.12
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by the direct ceramic machining system clinically.133 Their
results exhibited a survival rate of 84 percent in a period of
3.5 years. Minor porcelain chipping was reported in 11 percent
of the bridges. Tinschert et al. fabricated 65 zirconia bridges
with the DCS President® system and observed the zirconia
bridges for a mean period of three years and reported a small
chipping of the veneering material in 6 percent of the bridges,
which showed a cumulative survival rate of 86 percent.134 More
recently, Rismanchian et al. reported that both Biodenta (ZrO2,
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Al2O3, Y2O3) and Cercon (ZrO2, Y2O3, HfO2, SiO2, Al2O3)
systems can withstand biting force (even para functions) in
posterior implant supported ZrO2 based bridges and no sig-
nificant differences were observed between the two systems.135
6.3.1 Thermal induced residual stress effect in zirconia
veneer crowns. Residual stresses within the veneer are linked
to the high prevalence of veneer chipping observed in clinical
trials of ZrO2 prostheses.136 Belli et al. hypothesized that the
thermal mismatch between the ZrO2 infrastructure and the
veneer porcelain, as well as the rate used for cooling zirconia
veneer crowns, would be directly proportional to the magni-
tude of residual stresses built within the veneer layers. Two
porcelains with different coefficients of thermal expansion
were used to veneer ZrO2 copings in order to create high or low
thermal mismatches.137
Lohbauer et al.137 reported the results on the fracture of a
veneered ZrO2 dental prosthesis from an inner thermal crack
fractographic analysis and showed that the fracture of dental
prostheses may initiate from internal thermal flaws, and not
exclusively from contact cracks, radial cracks or marginal
defects. The fracture origin in the presented research work was
a thermal flaw that resulted from the layering technique.
Fracture was induced by sliding contact loading and expedited
by an internal flaw embedded in the veneering material under
considerable thermal residual stresses. Other manufacturing
techniques that avoid incremental sintering of the veneer
might come as a more reliable option.138 Overall, the resultant
residual stresses in bilayer prostheses are a superimposition of
stresses generated during cooling and stresses due to the mis-
match (Δα) in the coefficients of thermal expansion (CTE)
between the core and the veneer. The low thermal diffusivity of
the framework in zirconia veneer bilayer systems results in
higher temperatures at the interface during cooling in com-
parison with other infrastructure materials.139 Thermal gradi-
ents within the veneer are aggravated for faster cooling rates
due to the less relaxed state of the veneer as the temperature
falls through the glass transition temperature, Tg range.140
These conditions place ZrO2 based prostheses under a high
risk of veneer fracture and the high incidence of chipping
reported in clinical trials seems to support the mathematical
predictions only.141,142 However, available data on the magni-
tude and spatial distributions of residual stresses in zirconia
veneer bilayers are usually analytical or experimentally
measured using simple geometries.143–145
Later on a third variable was introduced in the form of
surface treatment, where copings were sandblasted or left sin-
tered prior to veneering. Through differences in core exposure
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experiences after failure, the effect of sandblasting on the
bonding between the core and veneer can be qualitatively evalu-
ated afterwards. A conventional static load to failure test
and a more clinically relevant chewing simulation cyclic fatigue
test were used and compared. A four to five-fold stress increase
was observed for the high CTE mismatch in comparison with
the low mismatch combination. The higher cooling rate had a
small influence on the stress increase, especially for the low
mismatch combination. The mechanical data evaluation
showed that while the compression test could not show clear
differences between variables, the fatigue test showed a higher
sensitivity to detect reliability variations regarding states of
thermal stress within the veneers. Differences in the magnitude
and distribution of cooling and thermal mismatch induced
stresses within the veneer layer of bilayer systems affect crack
behavior and theoretically print their effects on the fracture sur-
faces.146 However, this effect can be seen using indentation
tests on tempered or slowly cooled porcelain discs, which result
in differences in crack lengths for surfaces under compressive
or tensile residual stresses.147–149 Under the same applied load,
residual tensile stresses result in longer cracks, while compres-
sive stresses tend to shorten them. A significant increase in the
characteristic cycles to failure was observed for crowns that were
built using a veneer with a coefficient of thermal expansion
close to that of the zirconia core, indicating that the lifetime of
zirconia based prostheses could benefit from low thermal mis-
match combinations. That was the case, however, only for the
condition of a fast cooling rate, so that slow cooling protocols
may be employed to minimize stresses arising from large
thermal mismatches. Before stronger evidence could be sup-
plied, some authors have suggested that sandblasting the ZrO2
surface prior to veneering could improve the interfacial quality
by increasing its roughness.150 In vitro studies on dental cer-
amics have used fractography, so as to locate crack initiation
sites and calculate fracture toughness and stress at failure from
crack size measurements.151–155 Eventually, the results on the
fracture of a veneered ZrO2 dental prosthesis from an inner
thermal crack fractographic analysis showed that fractures of
dental prostheses may initiate from internal thermal flaws, and
not exclusively from contact cracks, radial cracks or marginal
defects. The fracture origin was a thermal flaw that resulted
from the layering technique. Fracture was induced by sliding
contact loading and expedited by an internal flaw embedded in
a veneering material under considerable thermal residual stres-
ses. Other manufacturing techniques that avoid incremental
sintering of the veneer might come as a more reliable option.
6.3.2 Surface treatments of zirconia. In spite of the high
mechanical strength, zirconia based ceramics have poor bond
strength after conventional bond cementation procedures,
requiring different surface treatment methods.156 The clinical
success of ceramic restorations depends on the cementation
process.157 Adhesive cementation to ZrO2 ceramics is desir-
able158 since it improves retention,159,160 marginal adaptation,
and fracture resistance,161 reduces the possibility of recurrent
decay,162,163 and enables more conservative cavity prep-
arations. Different methods to promote adequate adhesion
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between the resin cement and ZrO2 have been proposed. These
methods include the use of a phosphate modified monomer
(MDP) in the resin cement,164–168 laboratory or chair side air-
abrasion with 110 and 30 μm Si-coated aluminum
particles,169–171 the use of zirconate coupler primers,172 tetra-
ethoxysilane flame treat device usage,173 the use of organo
functional silanes,174,175 laser irradiation,176 the Si vapor
phase deposition method,177 and the selective infiltration
etching procedure.178–180
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The most common surface treatment method (STM) for
adhesive cementation to ceramic restorations is based either
on micromechanical bonds that is bonds obtained with hydro-
fluoric acid (HF) etching and particle sandblasting or on
chemical bonds, which is obtained by the application of a
silane coupling agent. HF removes the glassy matrix of glass
ceramics creating a high surface energy substrate with micro-
porosities for the penetration and polymerization of resin com-
posites, which is enabling a micromechanical interlocking.
However, HF etching does not produce any change in the
arithmetic roughness of ZrO2.181 The negligible effect of the
HF on the ZrO2 surface occurs due to the absence of the glassy
matrix, resulting in low bond strength values.182–184 The
surface treatment with primers containing functional mono-
mers such as MDP (Alloy Primer and Clearfil Ceramic Primer,
Kuraray Medical Inc., Japan) or other phosphoric acid acrylate
monomers (Metal/Zirconia Primer, Ivoclar Vivadent) is often
recommended to improve the bonding strength of ZrO2. Since
results are not always significant, the combination of primers
and air abrasion methods tends to produce a better bond
strength, especially in the long term.185–188 The use of new
zirconia primers (a mixture of organophosphate and carboxylic
acid monomers) or a phosphonic acid monomer (6-MHPA) has
been tested showing good immediate results.189 Different
types of silanes have been studied, but none of them was able
to show high effectiveness in surfaces with an absent or
reduced Si content as the surface of ZrO2.190–194 In addition,
siloxane bonds may be sensitive to hydrolytic degradation,
affecting the stability of the adhesive interface.195,196
Organosilanes were also tested (3-methacryloyloxypropyl
trimethoxysilane, 3-acryloyloxypropyltrimethoxysilane, or
3-isocyanatopropyltriethoxysilane) with better results for the
two first ones. The silane organo-functional groups are gener-
ally a methacrylate molecule, but acrylate groups are known to
be more reactive than methacrylates. The 3-isocyanatopropyl-
triethoxysilane is a rare silane, which has not been reported to
be used as an adhesion promoter in dental materials research.
Si deposition by air abrasion might produce a more silane
reactive surface,197 but it also tends to produce a surface with
lower roughness and consequently a lower possibility of mech-
anical interlocking with resin cement. Some authors do not
show lower roughness,198 but considering this might be a true
observation, the enabled chemical interaction to resin cement
or coupling agents would justify its use.199 Recent studies have
shown promising results on the bond strengths of Y-TZP/resin
cement after the glazed ceramic surface is subjected to air par-
ticle abrasion with Al2O3 and silanization or etching with HF
Dalton Trans.
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Dalton Transactions
acid,200 but a stable bond promoted by these methods is ques-
tionable and needs more studies.
Kosmac et al.201,202 have reported the effects of dental
grinding and sandblasting on the ageing and fatigue behavior
of pressureless sintered biomedical grade Y-TZP ceramics. It
was found that upon dental grinding and sandblasting, the
surface of the material was heavily damaged and partially plas-
tically deformed, but the amount of transformed monoclinic
ZrO2 was low. The partitioned tetragonal zirconia grains and
pre-existing ZrO2 zirconia in the ground and sandblasted sur-
faces hindered the propagation of the diffusion controlled
transformation during subsequent ageing. Dental grinding at
a high rotation speed lowered the mean strength under static
loading and the survival rate under cyclic loading. Scherrer
et al.203 showed that sandblasting yttria stabilized zirconia
with 30 μm silica coated AlO3 particles at 2.5 bar also improved
the fatigue limits and survival probabilities of the Y-TZP
materials tested. It can therefore be recommended as a last
clinical step before cementation.
6.4 Zirconia based dental posts
For more than 250 years, dental clinicians have written about
the placement of posts in the roots of teeth to retain restor-
ations.204 As early as 1728, Pierre Fauchard described the use of
tenons, which were metal posts screwed into the roots of teeth
to retain bridges. In the mid-1800s, wood replaced metal as the
post material, and the pivot crown, a wooden post fitted to an
artificial crown and to the canal of the root, was popular among
dentists.205 Often, these wooden posts would absorb fluids and
expand, frequently causing root fractures. In the late 19th
century, the Richmond crown, a single piece post retained
crown with a porcelain facing, was engineered to function as a
bridge retainer. During the 1930s, the custom cast post and core
was developed to replace the one piece post crowns. This pro-
cedure required casting a post and core as a separate component
from the crown. This 2-step technique improved marginal adap-
tation and allowed for a variation in the path of insertion of the
crowns. The nonmetallic prefabricated posts have been develo-
ped as alternatives, including ceramic (white ZrO2) and fiber
reinforced resin posts. ZrO2 posts have a high flexural strength,
are biocompatible, and are highly corrosion resistant. However,
this material is difficult to cut intra-orally with a diamond
cutter, and to remove from the canal for retreatment.206 The
inherent high flexural strength of ZrO2 makes it useful not only
for crowns, fixed partial dentures and implant abutments, but
also for posts. In dental applications, ZrO2 is used mostly in
tetragonal crystalline phases that are partially stabilized with
Y2O3, providing flexural strength greater than 1000 MPa. This
makes ZrO2 suitable also as a post material. Zirconia posts are
available today in cylindrically, as well as conically, shaped
designs. In terms of the surface quality, zirconia posts with
slightly roughened finishes are preferred for good micromecha-
nical retention to adhesive cements. While zirconia posts
provide excellent radiographic opacity, the reported strength
becomes a significant disadvantage if the post later needs to be
retrieved. The likelihood of endodontic re-intervention therefore,
This journal is © The Royal Society of Chemistry 2016

Dalton Transactions
needs to be considered. Clinical long term success, however,
appears to be excellent for adhesively cemented zirconia posts
with direct composite buildups.207 The Metoxit AG company has
been reported to produce root posts made of zirconia, which
were produced starting in 1991. The key to their success was the
hardening and tempering of the material by the HIP process.
The advantage of the ‘Metoxit process’ is that root posts can be
manufactured with very small diameters (as low as 1.4 mm),
very narrow tolerances and high resistance to fracture. To date,
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this quality has not been matched either by injection moulding
methods or by extrusion (Fig. 12a–c).207
Fig. 12 (a) Example of a product: root post made of zirconia ceramic,
(b) root posts made of zirconia ceramic in the root canals for the build-
ups and (c) the root posts can be fitted with ceramic build-ups by using
the press technique.207
This journal is © The Royal Society of Chemistry 2016
View Article Online
Perspective
Recently, Abu Kasim et al.208 patented three types of multi-
layered composite materials that were produced using powders
of ZrO2, Al2O3, HAp, and Ti to develop newly designed func-
tionally graded dental posts. Likewise, Abu Kasim et al.209 also
investigated the stress distribution of a newly designed func-
tionally graded dental post which consisted of a multilayer
design of ZrO2-Ti-HAp and was compared to posts fabricated
from a homogeneous material such as titanium and zirconia.
They reported that this new dental post exhibited several
advantages in terms of stress distribution compared to posts
fabricated from a homogeneous material. The stress and strain
distribution at the post dentine interface of FGDP was better
than that of homogeneous posts.
6.5 Zirconia in removable prosthodontics
The use of ZrO2 for the fabrication of a zirconia bar on
implants and of a corresponding zirconia complete denture
has also been reported. The technique utilizes a copy milling
unit, that is a manually operated machine for the manufacture
not only of frameworks but also of completely removable den-
tures.210,211 Removable partial dentures are for patients who are
missing some of their teeth on a particular arch. Fixed partial
dentures, also known as a crown and bridge, are made from
crowns that are fitted on the remaining teeth to act as abut-
ments and prosthodontics made from materials to resemble
the missing teeth. Fixed bridges are more expensive than
removable appliances but are more stable. Removable prostho-
dontics are used when fixed prosthodontics are not possible.
7. CAD/CAM and zirconia restoration
7.1 Applications of dental CAD/CAM systems
Currently, a stone model of crowns and FPDs is being pro-
duced, as was done with conventional methods, and this
serves as the starting point for the CAD/CAM process to ensure
digitizing accuracy.212 After the stone model is digitized,
restorations can be designed on the monitor and fabricated by
various processing machines. Dental laboratory technicians
can use this system as a laboratory tool. This flow is most com-
monly followed by the current commercial dental CAD/CAM
systems available for crown and FPD restorations. There are
also systems that complete the wax up, as in the conventional
method, and then digitize the wax patterns followed by auto-
matic processing. Recently, networked CAD/CAM systems that
were originally based on the Procera® system have garnered
attention, especially for the fabrication of high strength
ceramic frameworks. The roles of digitizing a stone model and
that of CAD/CAM processing are separated in this system.
Frameworks fabricated at the center are then delivered to the
satellite office to complete the restorations by layering porce-
lains. This is an important application of the CAD/CAM
technology in a specialized field within a total process. This
application holds promise for the fabrication of ZrO2 frame-
works. Later, networked CAD/CAM systems were available, and
all ceramic frameworks using industrial dense sintered
Dalton Trans.
 View Article Online

Perspective Dalton Transactions

polycrystalline Al2O3 were available in the clinic. Since these

production

Available

Available

Available

Available

Available

Available

Available
high strength industrial ceramics were not available in the

Central

center
conventional dental laboratory, the application of networked

O
O
CAD/CAM, located in a processing center, was a tremendous

Noncomposite
innovation in the history of dental technology. Such networked
production systems are currently being introduced by a

Zirconia
number of companies worldwide. Currently, the production of
zirconia frameworks is the most popular use of this approach

O
O

O
in the world market (Table 4). Furthermore, the veneering part
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Alumina
of zirconia all ceramic FPDs was also fabricated by a CAD/CAM
process from a block of glassy materials and thus a new fabri-
cation system for digital veneering was introduced.213

O
Porcelain
7.2 Availability of zirconia based materials for CAD/CAM
CAD/CAM has become somewhat synonymous with zirconia,

O
O

O
but systems are available that can machine any type of ceramic

Gold
materials i.e. glass ceramics, interpenetrating (infiltration cer-

O
amics) materials and solid-sintered monophase ceramics like

Titanium
Materials
zirconia. The material used depends on the functional and
aesthetic demands and on whether a chair side or laboratory
CAD/CAM restoration is fabricated. For chair side CAD/CAM

O
O

O
restorations, an aesthetic, strong material requiring minimal

Resina
post milling aesthetic adjustment to minimize the chair side

O
time is needed. Currently, most of the commercially available
CAD/CAM systems in the world use zirconia based materials
Bridge
(Y-TZP) to fabricate the frameworks of FPDs214–221 and are
O

O
O

O
O
O
shown in Table 4. There are two types of zirconia blocks cur-
Crown

rently available for distinct CAD/CAM applications. The first

application is the use of fully sintered dense blocks for direct
O

O
O

O
O
O
machining using a dental CAD/CAM system with a grinding

CCD/color
machine with higher stiffness. The second application is the
Veneer

use of partially sintered blocks for CAD/CAM fabrication fol-

light
Prostheses
Current dental CAD/CAM systems in the world available for zirconia214–221

O
lowed by post sintering to obtain a final product with
sufficient strength. The former has the advantage of a superior
Inlay

fit because no shrinkage is involved in the process, but has the

O

O
disadvantage of inferior machinability associated with the
machine

Original

Original
Original

Original

Original

Original

Original

Original

Original
Milling

wear of the tool. In addition, micro-crack formation on the

OEM

OEM
material during the milling procedure might deteriorate mech-
anical durability.222
Original

Original
Original

Original

Original

Original

Original

Original
Scanner

& OEM

& OEM

& OEM

& OEM
OEM

OEM

OEM
7.3 CAD/CAM used in zirconia supraconstruction
CAD/CAM is also an important technique to produce supra-
Touch probe

construction for teeth restoration. Recently, Zafiropoulos et al.

CCD/white
CCD/white

CCD/white

CCD/color
CCD/laser

CCD/laser

CCD/laser

CCD/laser
Digitizing

PSD/laser

have reported the results using CAD/CAM to fabricate zirconia

method

supraconstruction.102 The CAD/CAM fabricated zirconia supra-

light

light

light

light
—

construction processes are shown in Fig. 13. The zirconia

framework (ZENO Discs, Wieland Dental) was then milled
C-Pro system (Panasonic dental)

using a CAD/CAM system (M4820, I-MES, Eiterfeld, Germany)

electrotechnical work GmbH)

Pro 50, Wax Pro® (SYNOVAD)

ZENO® Tec System (Wieland

Lava® (3M ESPE Dental AG)

Hint-ELs system (Hint-ELs

and sintered in an electrical furnace (ZENO Fire, Wieland

CEREC AC (Sirona Dental

Dental & Technik GmbH)

Katana (Kuraray Noritake
Procera® (Nobel Biocare

Dental Supply, Co., Ltd)

Everest & Arctica (KaVo

Cercon smart ceramics

Dental) for 14 hours at 1500 °C (Fig. 13a). To veneer the

Denta CAD systems)
(Degu Dent GmbH)

implant retained supraconstruction, a high fusing micro

Etkon® (Etkon AG)

Aadva system (GC)

of system GmbH)
CAD/CAM system

Germany GmbH)

ceramic (Vintage ZR, Shofu Dental, Ratingen, Germany) was

(manufacture)

used. To veneer the natural tooth retained supraconstruction,

a lightly cured indirect ceramic polymer (Ceramage, Shofu
Table 4

Dental) and a bonding system (Bond I and II, Shofu Dental)

were used (Fig. 13b–e). The zirconia superstructure possessed

Dalton Trans. This journal is © The Royal Society of Chemistry 2016


Dalton Transactions
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Fig. 13 (a) CAD/CAM fabricated zirconia supraconstruction. (b and c)
Finished/veneered supraconstruction for the PERIO patient. (d and e)
Finished/veneered supraconstruction for the IMPL patient.102
a wall thickness of 0.6 mm, an occlusal distance of 1.5 mm
and 3 × 3 mm proximal connecting elements.
8. Future prospect of zirconia
restorations
In dental healthcare, the use of ZrO2 implants as a treatment
option is a new topic compared to the other dental appli-
cations described. Titanium has been the material of choice
for the fabrication of oral implants, and many investigations
have shown its long term effects. However, more recently,
tooth colored ceramic materials have been gaining popularity
with dentists as well as with patients. The possible side effects
of metallic materials and the trend away from the use of
metals in the human body have promoted the search for more
biocompatible materials. Zirconia has been used as an ortho-
pedic implant material for many years and lately has been
emerging in dentistry in the form of orthodontic brackets,
post and core systems, all ceramic prosthetic restorations,
implant abutments and more recently as a material for oral
implants. Because of the rapid development of both materials
and processing technologies, the application of zirconia based
FPDs seems promising. However, dentists and dental tech-
nicians must collaborate and perform the proper clinical pro-
cedures even if the CAD/CAM system can neglect some parts of
the conventional manual work. It is a challenge to comment
on ‘aging free’ zirconia since the transformation occurring
upon aging consists of a ‘natural’ return to the monoclinic
equilibrium state. However, it is still not clear whether the
tetragonal to monoclinic phase transition phenomenon com-
This journal is © The Royal Society of Chemistry 2016
View Article Online
Perspective
promises the final dental restoration. The addition of alumina
to zirconia, creating zirconia/alumina composites has been
advocated to reduce the aging kinetics maintaining good
mechanical properties and is being explored as one of the
possible options. In order to improve the lifetime and the
reliability of the prostheses, carbon nanotubes (CNT) are also
added. Zirconia–MWCNT nanocomposites were also proposed
for biomedical applications.223 Nanocrystalline materials are
expected to show improved mechanical properties and the
nanometric features on the surface of the prostheses seem to
reduce the risk of rejection and enhance the proliferation of
osteoblasts (bone-forming cells).224 Due to metastability, zirco-
nia is prone to ageing in the presence of water. For the
development of new ageing system, ceramics (absence of ZrO2)
are the key for gaining confidence in mechanical property
degradation known as ageing which is due to the progressive
spontaneous transformation of the metastable tetragonal phase
into the monoclinic phase. As reported in the present article,
zirconia is being widely applied in dentistry starting from oral
implant fabrication to the manufacturing of dental crown and
bridgework. Zirconia and zirconia supported ceramics are
worthy of being further evaluated particularly with improved
production methods. More long term clinical evaluation must
be performed to understand the behavior and reliability of ZrO2
compared with porcelain fused to metal restorations that are
currently the most reliable system for FPD restorations.
9. Summary
In this article, past, current and future perspectives of zirconia
and zirconia based ceramic materials have been reviewed.
These materials have potential applications in dental restor-
ations, dental CAD/CAM and some specific and special
implants. Extensive in vitro and in vivo studies have confirmed
their high fracture resistance and use in stress bearing areas.
Due to the excellent physical properties of zirconia, its white
color and superior biocompatibility, it is being evaluated as an
alternative framework for the full coverage of all ceramic
crowns and fixed partial dentures. The properties of ZrO2 sur-
faces, such as the low plaque adhesion on zirconia dental
implants, and the absence of micro-gaps between fixtures and
abutment restorations, which are a promising prosthodontic
alternative to metal based restorations and the biological,
mechanical and clinical studies published to date seem to
indicate that zirconia restorations are both well tolerated and
sufficiently resistant. Ceramic bonding, luting procedures,
ageing and wear of zirconia restorations need to be further
evaluated in order to guide the adequate use of this material.
The biocompatibility of zirconia has been well documented
and in vitro and in vivo tests on Y-TZP have revealed good bio-
compatibility with no adverse reactions with cells or tissues.
Existing clinical studies demonstrated a promising survival
potential regarding tooth-supported restorations but also
revealed significant complications such as the high incidence
of early fractures of either the veneering or the core materials.
Dalton Trans.

Perspective
Longitudinal studies will help to determine the degree of clini-
cal benefits or severity of complications. The fracture origin in
the presented research work was a thermal flaw that resulted
from the layering technique. Fracture was prompted by sliding
contact loading and expedited by an internal flaw embedded
in the veneering material under considerable thermal residual
stresses. Other manufacturing techniques that avoid incremen-
tal sintering of the veneer might come as a more reliable
option. New aesthetic, restorative materials demand adhesion
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and recreating the dentin–enamel junction; their success is a
function of addressing the needs of the individual substrates
involved (enamel, dentin, and indirect materials such as zirco-
nia). The use of adhesives on the tooth substrate and the use
of primers on the indirect substrate in conjunction with
quality resin-based cements are crucial in optimizing clinical
outcomes of these new restorative materials.
Zirconia applications seem to consolidate a well-established
position in clinical dentistry, due to the improvements in CAD/
CAM technology and due to the materials’ exceptional physical
properties. There is no doubt that the application of the CAD/
CAM technology in dentistry provides innovative results, and
contributes to the health and QOL of people in aging societies.
CAD–CAM methods of production produce consistent quality,
a superior marginal fit and can also satisfy critical aesthetic
needs of the patients. The application of dental CAD/CAM
systems is promising, not only in the field of crowns and
FPDs, but also in other fields of dentistry, even if its contri-
bution is limited at present. Basic research should be con-
ducted in the fields of aging, veneering, framework design,
bonding, surface modification and esthetic performance to
further understand the observed complications and provide
solutions that will accelerate expected clinical outcomes. As
many new trends and applications for zirconia are being dis-
covered, the future of this biomaterial appears to be very prom-
ising. Lastly, we are confident that by using zirconia ceramics
in dental restorative and prosthetic devices, we have helped
patients to recover and maintain their oral function and
health.
Conflict of interest
The authors declare no competing financial interest.
Acknowledgements
The present review study was fully supported under the Raman
Post Doctoral Research Award Fellowship, Award no. F5-65/
2014 (IC), University Grant Commission, New Delhi, India. The
authors would like to acknowledge Prof. P. M. Ajayan,
Department of Materials Science and Nano Engineering, Rice
University, Houston, Texas, USA for providing all the necessary
facilities which were required to carry out this work. The
authors also gratefully acknowledge the publishers for giving
Dalton Trans.
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Dalton Transactions
permission to reproduce the cited works for academic pur-
poses as review articles.
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