Journal Identication = DENTAL Article Identication = 1791 Date: April 21, 2011 Time: 2:49pm

dental materi als 2 7 ( 2 0 1 1 ) 527534

avai l abl e at www. sci encedi r ect . com
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A novel polymer inltrated ceramic dental material
Li-Hong He

, Michael Swain
Sir John Walsh Research Institute, School of Dentistry, University of Otago, Dunedin, New Zealand
a r t i c l e i n f o
Article history:
Received 26 March 2010
Received in revised form
30 September 2010
Accepted 7 February 2011
Keywords:
Polymer inltrated ceramic
Mechanical properties
Nanoindentation
CAD/CAM
a b s t r a c t
Objectives. To evaluate the mechanical behavior of a prototype porous ceramic interpene-
trating polymerceramic material containing 1520% polymer.
Methods. After sample preparation, elastic modulus, hardness, stressstrainrelationshipand
indentation creep response were measured by a nanoindentation system. Fracture tough-
ness was measured by the single-edge-notched beam (SENB) method. SEM was employed
to observe the fractured surface and analyze the fracture mechanisms.
Results. The polymer inltrated ceramic material has elastic modulus, hardness, and frac-
ture toughness values of 30.14GPa, 2.59GPa, and 1.72 MPam
1/2
, respectively. The material
illustrates a signicant indentation size effect for elastic modulus and hardness, and has
similar indentation creep behavior to human enamel. Manufacturing procedures such as
the density of pre-inltrated porous ceramic and processing pressure inuence the nal
properties of the material.
Signicance. This polymer inltrated ceramic material is anticipated to become a new mem-
ber of the dental CAD/CAM family.
2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
1. Introduction
Recent trends in esthetic dentistry include the reduction or
elimination of metals and increasing use of CAD/CAM tech-
nology [1]. These trends have led to increased usage of ceramic
and composite materials and have contributed to the growth
of the CAD/CAM market. However, although tougher ceramics
such as zirconia and alumina have been used in dentistry, all-
ceramic systems, especially those with veener porcelains, still
experience a relatively high failure rate due to the brittleness
of the veneering layer. As a result, all-ceramic restorations
have an inferior life span equivalent to that of metalceramic
restorations [2]. Another potential hazard of current ceramic
restorations is excessive wear of the opposing teeth due to
the high hardness of the veneering materials [3]. Conse-
quently, the development of novel dental esthetic materials

Corresponding author at: Sir John Walsh Research Institute, School of Dentistry, University of Otago, PO Box 647, Dunedin 9054, New
Zealand. Tel.: +64 3 4797084; fax: +64 3 4795079.
E-mail address: lihong.he@otago.ac.nz (L.-H. He).
has switched to more polymer based resin-composites. How-
ever, traditional dental composites are compromised by their
curing shrinkage, low mechanical properties and poor wear
resistance. Thus there is an urgent need to develop a new
composite system to support the emerging indirect restora-
tive material market. There have been some developments in
this area with the release of Paradigm
TM
MZ100 Block (3M
TM
)
for CEREC

as a CAD/CAM composite for inlay, onlay, veneer

and full crown.
Recently, anewinterpenetrating networkmaterial inwhich
a porous ceramic is inltrated by a polymer has been devel-
oped by the VITA company (VITA Zahnfabrik, Bad Sckingen,
Germany) based on the glass inltrated ceramic (In-ceram)
systems theypioneeered. The aimof this studywas toevaluate
the mechanical properties of this new material and identify
parameters inuencing the mechanical properties of this fam-
ily of materials.
0109-5641/$ see front matter 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2011.02.002
Journal Identication = DENTAL Article Identication = 1791 Date: April 21, 2011 Time: 2:49pm
528 dental materi als 2 7 ( 2 0 1 1 ) 527534
Table 1 Descriptions of different samples.
Material ID Description
P Pure polymerized resin processed at higher pressure
M1 Pre-inltrated ceramic with density of 1.66g/cm
3
M2 Pre-inltrated ceramic with density of 1.80g/cm
3
C1 Polymer inltrated M1 under lower pressure
C2 Polymer inltrated M1 under higher pressure
C3 Polymer inltrated M2 under higher pressure
2. Materials and methods
Materials evaluated in this study were prototypes provided
by the VITA company (VITA Zahnfabrik, Bad Sckingen,
Germany). Porous pre-inltrated ceramic blocks with two dif-
ferent apparent densities were inltrated by a polymer and
heat polymerized under different pressures to fabricate the
polymer inltrated ceramics. Details of the testing materials
are described in Table 1.
One centimeter thick slices were sectioned from different
blocks of the materials listed in Table 1 for nanoindentation
tests and 20mm3.5mm4.5mm beams were cut from dif-
ferent blocks for fracture toughness testing. Cutting of the
specimens was done with a high speed cutting machine
(Accutom-50, Struers, Copenhagen, Denmark) witha diamond
cut-off wheel (331CA, Struers, Copenhagen, Denmark) at a
spindle speed of 3000rpm and feeding speed of 0.05mm/s
under water irrigation. The slices were polished (TegraPol-21,
Struers, Copenhagen, Denmark) to 1m with diamond pol-
ishing paste and the beams were polished to 2400# SiC paper
(Struers, Copenhagen, Denmark) to the nal dimension of
20mm3mm4mm.
The beams for fracture toughness test were pre-notched
with the high speed cutting machine (Accutom-50, Struers,
Copenhagen, Denmark) to a depth of 1.9mm through the
width of 4mm. Then, a purpose built compressive-air-driven
cyclic movement machine with a xed razor blade and 3m
diamond paste was employed to sharpen the notch and
extend it an additional 100200m. The nal length of the
notch was measured with an optical microscope (YS2-H,
Nikon, Japan) equipped with an objective micrometer (Olym-
pus, Japan) to an accuracy of 1m. To minimize the notch
blunting effect, the tip of every notch was double checked to
ensure the radius of the notch tip was less than 10m.
2.1. Nanoindentation tests
The indentation experiments were performed using a nano-
based indentation system (Ultra Micro-Indentation System,
UMIS-2000, CSIRO, Australia). The polished specimens were
mounted on metal bases which contained a strong magnet to
ensure adequate contact was obtainedwiththe test base inthe
UMIS. All the tests were performed under standard laboratory
conditions.
The elastic modulus and hardness of the specimens were
measured with a calibrated Berkovich indenter. The force
applied during the experiments was xed at 30 and 300mN.
Sixteen indents were made in a 44 array with the interval of
50mbetweenindents at eachload value. The maximumload
was held for 30s to minimize the effect of creep onthe unload-
ing curve. The OliverPharr analysis method [4] was used by
the UMIS software to calculate the elastic modulus (E) and
hardness (H). The rst four indents were discarded from the
calculation, because of thermal drift inuences, and twelve
data points were collected for each test.
In the book Hardness of metals, Tabor [5] showed that
an equivalence existed between conventional stressstrain
curves and that generated by plotting hardness versus con-
tact radius divided by indenter radius (a/R) using a spherical
tipped indenter. The nanoindentation stressstrain relation-
ship was measured based on the previous described method
[6,7]. Three calibrated spherical tips with the nominal radius
of 5, 10 and 20m were employed. Contact stress, or hardness
(H), is calculated by its denition,
H =
P
A
(1)
where P is the maximum load and A is the contact area. The
contact strain (a/R) is determined from the sin value of the
contact angle , which is derived from the indenter tip cali-
bration function a=f(h
p
) and its derivative tan =a

=f

(h
p
). As
a result, a/R can be expressed as [6,7],
a
R
= sin =
1

(tan
2
+1)
(2)
With Eqs. (1) and (2), the nanoindentation stressstrain
relationship can be plotted from the results with the different
spherical indenters.
For the indentation creep test, the Berkovich indenter was
used with a maximum force of 250mN. One-step loading and
unloading method with a maximum-force (250mN) hold time
of 900s and upon unloading at a minimum-force (5mN) also
with hold time of 900s was followed [8]. All tests commenced
after at least 2h thermal soak period in the instrument, and
thermal drift was deemed to be almost negligible (<0.05nm/s)
before each experiment.
2.2. Fracture toughness test
Standard single-edge-notched beam (SENB) method was used
to measure the fracture toughness (K
1c
) [9]. The prepared sam-
ples were loaded in a three-point bending format with the
support span of 16mm at a cross-head speed of 0.5mm/min
till failure in a universal test machine (Model 3369, Instron,
Norwood, MA, USA). The following equation was used to cal-
culate the K
1c
,
K
1c
=
FL
BW
3/2
f

a
W

(3)
in which F is the fracture load, L is the lower supporting span,
B is the breadth of the beam, W is the width of the beam, and
a is the length of the notch. Geometrical factor f(a/W) can be
calculated by Eq. (4),
f

a
W

= 2.9

a
W

1/2
4.6

a
W

3/2
+21.8

a
W

5/2
37.6

a
W

7/2
+38.7

a
W

9/2
(4)
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dental materi als 2 7 ( 2 0 1 1 ) 527534 529
Five samples were prepared and tested for each material
and the data were analyzed statistically with Microsoft Excel
2007.
2.3. Brittleness index
Following Lawn and Marshall [10], the brittleness index is cal-
culated by:
B =
H
K
1c
(5)
where His the hardness to quantify the resistance to deforma-
tion, and K
1c
is the fracture toughness to dene the resistance
to fracture. In the current study, the average values of H and
K
1c
were used for calculation.
2.4. SEM observation
Representative fractured samples were gold coated for scan-
ning electron microscope (SEM) observation. Cambridge S360
SEM (Cambridge Instruments, Cambridge, UK) and a sec-
ondary electron detector was employed to observe both
polished and fractured surfaces of the sample.
2.5. Statistical analyses
Differences between means were tested for statistical signif-
icance using analysis of variance (ANOVA); one-way ANOVA
(with Turkey post hoc comparison) was used to determine
which groups differed from one another. Analyses were con-
ducted using SPSS 18 (SPSS Inc., Chicago, IL, USA).
Table 2 Nanoindentation elastic modulus and
hardness of polymer ceramics under two different loads.
Sample Load (mN) Elastic
modulus (GPa)
Hardness
(GPa)
P 30 3.48 0.05 0.20 0.002
300 3.40 0.03 0.19 0.001
M1 30 21.53 11.56 2.31 2.13
300 12.26 3.09 0.97 0.72
M2 30 28.53 11.31 2.77 2.08
300 21.17 5.78 1.15 0.60
C1 30 32.21 9.48 3.18 2.15
300 29.87 4.41 2.45 1.02
C2 30 35.79 6.27 3.52 1.14
300 28.47 4.05 2.59 1.01
C3 30 40.06 17.97 2.92 1.92
300 30.14 2.96 2.36 0.57
Note: Number of data for each group and load was 12.
3. Results
3.1. Nanoindentation elastic modulus and hardness
The results for the Berkovich derived hardness and elastic
modulus values for the various materials are listed in Table 2.
The statistical analysis did not showany signicant difference
between groups C1, C2, and C3 for either E or Hat 300mNload.
Values for H and E from different indentation loads illus-
trate a clear indentation size effect for all specimens except
the bulk polymer sample. The indentation size effect (ISE) is
clearly illustrated in Fig. 1 with C3 specimen as the example.
The data shown in Fig. 1 indicates a degree of scatter of the
results which is also reected in the standard deviations.
Fig. 1 Nanoindentation hardness and elastic modulus of C3 sample plotted against the effective contact radii of the
Berkovich indenter at different loads.
Journal Identication = DENTAL Article Identication = 1791 Date: April 21, 2011 Time: 2:49pm
530 dental materi als 2 7 ( 2 0 1 1 ) 527534
Fig. 2 Stressstrain relationship (Ha/R) generated with the three spherical tipped indenters for the samples listed in
Table 1.
3.2. Nanoindentation stressstrain relationships
The nano-indentation derived stressstrain curves for all the
materials with the three indenters are shown in Fig. 2.
The highly repeatable data points for the polymer sam-
ple (P) conrm and validate the method. However, due to the
porosity of the porous ceramic preforms and big differences
between two phases of the polymer inltrated ceramics, all
ceramic and composite specimens (M1, M2, C1, C2, and C3)
show considerable scatter in the stressstrain relationships.
3.3. Nanoindentation creep behavior
The nanoindentation derived creep (at maximum load) and
backcreep (recovery at minimum load) response with the
Berkovich indenter for three of the materials; the polymer
matrix (P), porous ceramic matrix (M2) and polymer inltrated
composite (C3) are shown in Fig. 3.
All the curves in Fig. 3 are the average response of at least
3 tests. The relative penetration depth, h
t

, was calculated by
subtracting the initial penetration depth at the beginning of
the holding time from the increasing depths during the hold-
ing period at maximum and minimum loads.
Creep data at maximum-load exhibits increasing penetra-
tion depth with time. Pure polymer (P) shows the maximum
creep (0.6mover 900s), followed by inltrated-ceramic (C3).
Incontrast, the pre-inltrated porous ceramic (M2) shows very
limited indentation creep response (less than 0.04m dur-
ing the 900s holding period). Such limited creep response,
0.06nm/s, is at the lower limit of UMIS system thermal
drift stability and implies that the viscous response of these
ceramic materials is virtually absent.
At the minimum-load hold period (this behavior is called
backcreep), recovery is prominent only for polymer sample
Fig. 3 Indentation creep response versus time for the
polymer matrix (P), porous ceramic matrix (M2) and
polymer inltrated material (C3). The change in depth at
maximum load and at the minimum load, h
t

t, curves of
creep and recovery are shown.
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dental materi als 2 7 ( 2 0 1 1 ) 527534 531
Table 3 Fracture toughness and brittleness index of
different samples.
Sample Fracture toughness
(MPam
1/2
)
Brittleness
index (m
1/2
)
P 0.80 0.05 0.24
M1 0.44 0.04 0.80
M2 0.66 0.03 1.74
C1 1.46 0.21 1.68
C2 1.65 0.11 1.57
C3 1.72 0.09 1.37
Note: Number of fracture toughness data for each group was 6.
(P) whereas for the porous ceramic and polymer inltrated
ceramic the backcreep rate remained within the instruments
stability range (<0.05nm/s) (Fig. 3).
3.4. Fracture toughness and brittleness index
The fracture toughness and brittleness index derived from
Eqs. (3) and (5) are listed in Table 3.
Table 3 clearly illustrates that the fracture toughness of the
polymer inltrated-ceramics were signicantly higher than
the pre-inltrated ceramics performs (p<0.01 by one-way
ANOVA). One-way ANOVA indicated a signicant difference
between groups C1 and C3 with respect to fracture toughness.
The density of pre-inltrated ceramics and processing pres-
sure had an inuence on the fracture toughness of the nal
product.
The average hardness at 300mN was chosen for the cal-
culation of brittleness index after considering the ISE of the
material. The value of hardness from heavier loads might be
more comparable to the macro-scale properties of the mate-
rial.
3.5. SEM observation
The microstructure of pre-inltrated porous ceramic (M2) are
shown in Fig. 4AD, which reveals that the material was made
from irregular shaped ceramic phase resulting in irregular
pores withinthe structure whichwere typically less than3m.
The SEM images (Fig. 4EH) of polymer inltrated-ceramic
sample (C3) did not show any obvious pores and voids, which
indicate that the polymer inltration was successful. Other
specimens had similar microstructure and fractographic fea-
tures, therefore were not included here.
4. Discussion
It has long been the goal for dental material scientists to
develop a material with similar mechanical behavior to that
of natural human enamel and dentin. The polymer inltrated
ceramic investigated suggests a successful step toward such a
goal.
Firstly, the material illustrated similar ISE behavior as
observed for human enamel, namely, not only the hardness
but also more importantly the elastic modulus of the mate-
rial have a relationship to indentation depth or contacting
area [7]. Although ISE of dental materials has been docu-
mented previously [11], to our knowledge, this is the rst
dental material with signicant ISE for elastic modulus, which
indicates the mechanical behavior of the material are depen-
dent on the contacting area in functional situations and the
material becomes stiffer under smaller contact and higher
pressure. Considering the porous structure of the ceramic
and the composite nature of the polymer inltrated-ceramics,
it is reasonable to suggest that lower loads result in higher
elastic modulus and hardness with greater data scatter. For
porous pre-inltrated ceramics (M1 and M2), this is because
the surface roughness (porosity in this case) had a signicant
inuence on the result, which is similar to what Bobji and
Biswas mentioned [12]. For the polymer inltrated-ceramics,
lower indentation load generated smaller contacting areas
with limited affected zones around the indentations. As a
result, the indentation responses especially at low loads for
the inltrated material were dominated by either the ceramic
particles or the polymer regions, depending onthe initial point
of contact. Due to the relative small volume fraction of the
polymer phase indents had more chance to fall on ceramic
particles than inltrated polymer. In contrast, at heavy load
with the contact area much greater than the dimension of
the polymer regions a more averaged response of the two
phase nature of the ceramicpolymer is obtained. Therefore,
the average E and H at lower loads were higher than at heavier
loads.
Secondly, the hardness values of the polymer inltrated-
ceramics is much lower than typical dental ceramics and
veneering porcelains. For example, Vita Mark II ceramic and
Vita VM9 veneering porcelain have indentation hardness val-
ues of 10.640.46 and 9.50.35GPa, respectively [6], which
are three times higher than the tested novel inltrated mate-
rial. Several wear test studies have indicated that dental
porcelains and ceramics generated greater antagonist tooth
wear than other restorative materials [1315]. Moreover, it
is generally accepted that harder material may cause more
severe wear on the antagonist [16]. Therefore, the signicantly
lower hardness value of the polymer inltrated-ceramic than
most commercial dental ceramics may be of considerable
advantage in order to protect the opposing teeth from exces-
sive wear. However, specic studies are needed to conrmthis
speculation.
Thirdly, the material has similar indentation creep ability
as that of human enamel (0.1mover 900s) [8]. However, the
material did not recover automatically as did human enamel
uponunloading. Whenconsideredinmore detail, it is interest-
ing to note that polymer inltrated-ceramic (C3) did not show
any recovery even though it has been inltrated by polymer.
The possible reason could be, the ceramic particles fractured
during loading become interlocked with each other, which
blocked the recovery of the polymer during the unload hold-
ing period. This aspect reveals that the inltrated-ceramic has
a somewhat similar viscous response as human enamel but
lacks the ability of auto-recovery. In human enamel the pres-
ence of the near theoretical strength of the nano-crystallites
of hydroxyapatite coupled with the ability of the remnant pro-
teins that glue these crystallites together to unfold and refold
imparts such recovery ability [17]. By comparing with typical
porcelains that do not exhibit creep [8], the creep response
of the polymer inltrated-ceramic, which is similar as that
of human enamel [8], implies that these materials will have
Journal Identication = DENTAL Article Identication = 1791 Date: April 21, 2011 Time: 2:49pm
532 dental materi als 2 7 ( 2 0 1 1 ) 527534
Fig. 4 SEM observation of M2 (images AD) and C3 (images EH) samples. Images A and E were surfaces after high speed
diamond saw cutting during notch preparation; images B, C and F, G were fractured surfaces after fracture toughness tests;
images D and H were of cracks propagated through the polished surface during sample preparation. Ceramic phase and
polymer phase in image H have been marked by C and P, respectively.
better stress redistribution ability than porcelain based dental
restorations.
Fourthly, in comparison with other restorative dental
materials, the inltrated-ceramic material has high fracture
toughness, which is slightly higher than MZ100 CAD/CAM
composite (K
1c
1.4MPam
1/2
) [18]. Moreover, all of the poly-
mer inltrated-ceramic specimens share similar brittleness
index values, which are all lower than 4.3m
1/2
, the sug-
gested value for good machinability [19]. The slight decreasing
trend of brittleness index from C1 to C3 may have originated
from the increasing fracture toughness associated with the
higher processing pressure and ceramic density. By compar-
ing the brittleness index values with that of other commercial
CAD/CAM dental materials reported by Tsitrou et al. [20],
the polymer inltrated-ceramics have comparable values with
ProCAD (Vivadent-Ivoclar) (B=1.7m
1/2
) and VITA Mark II
Journal Identication = DENTAL Article Identication = 1791 Date: April 21, 2011 Time: 2:49pm
dental materi als 2 7 ( 2 0 1 1 ) 527534 533
(VITAZahnfabrik) (B=1.6m
1/2
), and are better than IPS e.max
(Vivadent-Ivoclar) (B=2.9m
1/2
). This indicates that the poly-
mer inltrated ceramics are suitable candidates for CAD/CAM
purposes.
Fifthly, the density and processing pressure had an inu-
ence on the nal properties of the materials. As listed in
Tables 2 and 3, higher initial density of the pre-inltrated
ceramic and higher inltration pressure gave better mechani-
cal properties, although there was no statistical difference for
E and H. Similar trends can be found for stressstrain response
as well. However, too high a density of the pre-inltrated
ceramic may result in incomplete polymer inltration. Thus,
the density of pre-inltrated ceramic and inltration pressure
must be optimized.
Lastly, SEM observations of the microstructure of the
material indicate that the porous pre-inltratedblockwas suc-
cessfully inltrated. Polymer inltration did not change the
fracture pattern of the ceramic preforms signicantly. Fig. 4E
illustrates that some of the ceramic grains were chipped out
during high speed cutting as a result of the crack propagation
within the low fracture toughness polymer phase. However,
due to the crack deection effects of tough ceramic parti-
cles, the chances for chipping out of the whole particle are
much less than those of pre-inltrated ceramics. Therefore, it
is reasonable to nd that the cutting surface of polymer inl-
trated ceramic (Fig. 4E) is smoother than that of pre-inltrated
ceramic (Fig. 4A). Moreover, the at facets in Fig. 4Aand E were
believed to be the outcome of grinding with the cutting wheel
rather thandirect cutting throughthe toughceramic particles.
In short, for pre-inltrated porous materials, cracks propa-
gated along the boundaries of the ceramic crystals (M2), and
for polymer inltrated ceramics cracks propagated within the
polymer phase (C3) except for penetrating through the weak
part of the irregular ceramic isthmus as indicated by the black
arrow in Fig. 4H. This suggests that, similar as with other two
phase composite systems, the high fracture toughness of the
poly-ceramic is due to crack deection.
In summary, the material has several advantages as a new
dental restorative material. (1) Reasonable brittleness index
with satisfactory fracture toughness makes the material a
suitable CAD/CAM candidate; unlike a number of partially
sintered CAD/CAM materials which require additional ring,
the one-step manipulation helps ensure a high degree of
dimensional accuracy of the nal products. (2) Lower hardness
compared with traditional veneering porcelains may better
protect the opposing teeth from excessive wear and should
enable more rapid machining in CAD/CAM instruments. (3)
Similar creep response as enamel and low hardness endows
the material withlower contact stresses and good stress redis-
tribution ability when used as a dental restorative. (4) Higher
E and H more closely matching natural tooth structure than
current dental composites and acrylics make the material a
good replacement of current inlay materials. More equivalent
mechanical properties to enamel and dentin make the mate-
rial a highly appropriate choice for implant supported denture
teeth as well as phantomteeth for simulation and dental edu-
cation purposes.
Finally, this preliminary study only evaluated the mechan-
ical properties of the material. Other aspects of the material
such as fatigue response, color stability and biocompatibility
should be thoroughly investigated before the material can be
released for clinical applications.
5. Conclusions
These novel polymer inltrated ceramic restorative materi-
als have averaged elastic modulus, hardness, and fracture
toughness values of 30.14GPa, 2.59GPa, and 1.72MPam
1/2
,
respectively, depending onthe manufacturing conditions. The
density of pre-inltrated ceramic and polymer pressure of
processing inuence the nal properties of the materials,
especially the fracture toughness (p<0.05 between C1 and C3
groups by one way ANOVA). The materials illustrate ISE for
both E and H, and have similar indentation creep response as
humanenamel. SEMobservationindicates that the inltration
of polymer was successful and the high fracture toughness of
the material was due to a crack deection mechanism.
Acknowledgements
We thank Vita Zahnfabrik for supply of this material and to
discussions with N. Thiel, E. Bojemueller, A. Coldea and K.
Klemm about these composite materials. Statistical analysis
assistance from Prof. Murray Thomson is greatly appreciated.
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