d e n t a l m a t e r i a l s 2 7 ( 2 0 1 1 ) 527–534

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A novel polymer infiltrated 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 a b s t r a c t

Article history: Objectives. To evaluate the mechanical behavior of a prototype porous ceramic interpene-
Received 26 March 2010 trating polymer–ceramic material containing 15–20% polymer.
Received in revised form Methods. After sample preparation, elastic modulus, hardness, stress–strain relationship and
30 September 2010 indentation creep response were measured by a nanoindentation system. Fracture tough-
Accepted 7 February 2011 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 infiltrated ceramic material has elastic modulus, hardness, and frac-
Keywords: ture toughness values of 30.14 GPa, 2.59 GPa, and 1.72 MPa m1/2 , respectively. The material
Polymer infiltrated ceramic illustrates a significant indentation size effect for elastic modulus and hardness, and has
Mechanical properties similar indentation creep behavior to human enamel. Manufacturing procedures such as
Nanoindentation the density of pre-infiltrated porous ceramic and processing pressure influence the final
CAD/CAM properties of the material.
Significance. This polymer infiltrated 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.

has switched to more polymer based resin-composites. How-

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 metal–ceramic
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
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 ParadigmTM MZ100 Block (3 MTM )
for CEREC® as a CAD/CAM composite for inlay, onlay, veneer
and full crown.
Recently, a new interpenetrating network material in which
a porous ceramic is infiltrated by a polymer has been devel-
oped by the VITA company (VITA Zahnfabrik, Bad Säckingen,
Germany) based on the glass infiltrated ceramic (In-ceram)
systems they pioneeered. The aim of this study was to evaluate
the mechanical properties of this new material and identify
parameters influencing the mechanical properties of this fam-
ily of 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).
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
528 d e n t a l m a t e r i a l s 2 7 ( 2 0 1 1 ) 527–534
Table 1 – Descriptions of different samples.
Material ID Description
P Pure polymerized resin processed at higher pressure
M1 Pre-infiltrated ceramic with density of 1.66 g/cm3
M2 Pre-infiltrated ceramic with density of 1.80 g/cm3
C1 Polymer infiltrated M1 under lower pressure
C2 Polymer infiltrated M1 under higher pressure
C3 Polymer infiltrated M2 under higher pressure
2. Materials and methods
Materials evaluated in this study were prototypes provided
by the VITA company (VITA Zahnfabrik, Bad Säckingen,
Germany). Porous pre-infiltrated ceramic blocks with two dif-
ferent apparent densities were infiltrated by a polymer and
heat polymerized under different pressures to fabricate the
polymer infiltrated 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 20 mm × 3.5 mm × 4.5 mm 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) with a diamond
cut-off wheel (331CA, Struers, Copenhagen, Denmark) at a
spindle speed of 3000 rpm and feeding speed of 0.05 mm/s
under water irrigation. The slices were polished (TegraPol-21,
Struers, Copenhagen, Denmark) to 1 ␮m with diamond pol-
ishing paste and the beams were polished to 2400# SiC paper
(Struers, Copenhagen, Denmark) to the final dimension of
20 mm × 3 mm × 4 mm.
The beams for fracture toughness test were pre-notched
with the high speed cutting machine (Accutom-50, Struers,
Copenhagen, Denmark) to a depth of 1.9 mm through the
width of 4 mm. Then, a purpose built compressive-air-driven
cyclic movement machine with a fixed razor blade and 3 ␮m
diamond paste was employed to sharpen the notch and
extend it an additional 100–200 ␮m. The final 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 1 ␮m. 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 10 ␮m.
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 obtained with the test base in the
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 fixed at 30 and 300 mN.
Sixteen indents were made in a 4 × 4 array with the interval of
50 ␮m between indents at each load value. The maximum load
was held for 30 s to minimize the effect of creep on the unload-
ing curve. The Oliver–Pharr analysis method [4] was used by
the UMIS software to calculate the elastic modulus (E) and
hardness (H). The first four indents were discarded from the
calculation, because of thermal drift influences, and twelve
data points were collected for each test.
In the book Hardness of metals, Tabor [5] showed that
an equivalence existed between conventional stress–strain
curves and that generated by plotting hardness versus con-
tact radius divided by indenter radius (a/R) using a spherical
tipped indenter. The nanoindentation stress–strain relation-
ship was measured based on the previous described method
[6,7]. Three calibrated spherical tips with the nominal radius
of 5, 10 and 20 ␮m were employed. Contact stress, or hardness
(H), is calculated by its definition,
P
H= (1)
A
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(hp ) and its derivative tan  = a = f (hp ). As
a result, a/R can be expressed as [6,7],
a 1
= sin  =  (2)
R (tan−2  + 1)
With Eqs. (1) and (2), the nanoindentation stress–strain
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 250 mN. One-step loading and
unloading method with a maximum-force (250 mN) hold time
of 900 s and upon unloading at a minimum-force (5 mN) also
with hold time of 900 s was followed [8]. All tests commenced
after at least 2 h thermal soak period in the instrument, and
thermal drift was deemed to be almost negligible (<0.05 nm/s)
before each experiment.
2.2. Fracture toughness test
Standard single-edge-notched beam (SENB) method was used
to measure the fracture toughness (K1c ) [9]. The prepared sam-
ples were loaded in a three-point bending format with the
support span of 16 mm at a cross-head speed of 0.5 mm/min
till failure in a universal test machine (Model 3369, Instron,
Norwood, MA, USA). The following equation was used to cal-
culate the K1c ,
FL
a
K1c = f (3)
BW 3/2 W
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),
a  a 1/2  a 3/2  a 5/2
f = 2.9 − 4.6 + 21.8
W W W W
 a 7/2  a 9/2
−37.6 + 38.7 (4)
W W
 d e n t a l m a t e r i a l s 2 7 ( 2 0 1 1 ) 527–534 529

Five samples were prepared and tested for each material

Table 2 – Nanoindentation elastic modulus and
and the data were analyzed statistically with Microsoft Excel
hardness of polymer ceramics under two different loads.
2007.
Sample Load (mN) Elastic Hardness
modulus (GPa) (GPa)
2.3. Brittleness index P 30 3.48 ± 0.05 0.20 ± 0.002
300 3.40 ± 0.03 0.19 ± 0.001
Following Lawn and Marshall [10], the brittleness index is cal-
M1 30 21.53 ± 11.56 2.31 ± 2.13
300 12.26 ± 3.09 0.97 ± 0.72
culated by:
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
H
B= (5) 300 29.87 ± 4.41 2.45 ± 1.02
K1c
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
where H is the hardness to quantify the resistance to deforma-
300 30.14 ± 2.96 2.36 ± 0.57
tion, and K1c is the fracture toughness to define the resistance
to fracture. In the current study, the average values of H and Note: Number of data for each group and load was 12.

K1c were used for calculation.

2.4. SEM observation

Representative fractured samples were gold coated for scan- 3. Results

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).
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 show any significant difference
between groups C1, C2, and C3 for either E or H at 300 mN load.
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 reflected 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.
530 d e n t a l m a t e r i a l s 2 7 ( 2 0 1 1 ) 527–534

Fig. 2 – Stress–strain relationship (H–a/R) generated with the three spherical tipped indenters for the samples listed in
Table 1.

3.2. Nanoindentation stress–strain relationships
The nano-indentation derived stress–strain 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) confirm and validate the method. However, due to the
porosity of the porous ceramic preforms and big differences
between two phases of the polymer infiltrated ceramics, all
ceramic and composite specimens (M1, M2, C1, C2, and C3)
show considerable scatter in the stress–strain relationships.
ing the 900 s holding period). Such limited creep response,
∼0.06 nm/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

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 infiltrated
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, ht  , 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- Fig. 3 – Indentation creep response versus time for the
tion depth with time. Pure polymer (P) shows the maximum polymer matrix (P), porous ceramic matrix (M2) and
creep (∼0.6 ␮m over 900 s), followed by infiltrated-ceramic (C3). polymer infiltrated material (C3). The change in depth at
In contrast, the pre-infiltrated porous ceramic (M2) shows very maximum load and at the minimum load, ht  –t, curves of
limited indentation creep response (less than 0.04 ␮m dur- creep and recovery are shown.
 d e n t a l m a t e r i a l s 2 7 ( 2 0 1 1 ) 527–534 531

dental material with significant ISE for elastic modulus, which

Table 3 – Fracture toughness and brittleness index of
different samples. indicates the mechanical behavior of the material are depen-
dent on the contacting area in functional situations and the
Sample Fracture toughness Brittleness
material becomes stiffer under smaller contact and higher
(MPa m1/2 ) index (␮m−1/2 )
pressure. Considering the porous structure of the ceramic
P 0.80 ± 0.05 0.24
and the composite nature of the polymer infiltrated-ceramics,
M1 0.44 ± 0.04 0.80
it is reasonable to suggest that lower loads result in higher
M2 0.66 ± 0.03 1.74
C1 1.46 ± 0.21 1.68 elastic modulus and hardness with greater data scatter. For
C2 1.65 ± 0.11 1.57 porous pre-infiltrated ceramics (M1 and M2), this is because
C3 1.72 ± 0.09 1.37 the surface roughness (porosity in this case) had a significant
Note: Number of fracture toughness data for each group was 6. influence on the result, which is similar to what Bobji and
Biswas mentioned [12]. For the polymer infiltrated-ceramics,
lower indentation load generated smaller contacting areas
(P) whereas for the porous ceramic and polymer infiltrated
with limited affected zones around the indentations. As a
ceramic the backcreep rate remained within the instruments
result, the indentation responses especially at low loads for
stability range (<0.05 nm/s) (Fig. 3).
the infiltrated material were dominated by either the ceramic
particles or the polymer regions, depending on the initial point
3.4. Fracture toughness and brittleness index
of contact. Due to the relative small volume fraction of the
polymer phase indents had more chance to fall on ceramic
The fracture toughness and brittleness index derived from
particles than infiltrated polymer. In contrast, at heavy load
Eqs. (3) and (5) are listed in Table 3.
with the contact area much greater than the dimension of
Table 3 clearly illustrates that the fracture toughness of the
the polymer regions a more averaged response of the two
polymer infiltrated-ceramics were significantly higher than
phase nature of the ceramic–polymer is obtained. Therefore,
the pre-infiltrated ceramics performs (p < 0.01 by one-way
the average E and H at lower loads were higher than at heavier
ANOVA). One-way ANOVA indicated a significant difference
loads.
between groups C1 and C3 with respect to fracture toughness.
Secondly, the hardness values of the polymer infiltrated-
The density of pre-infiltrated ceramics and processing pres-
ceramics is much lower than typical dental ceramics and
sure had an influence on the fracture toughness of the final
veneering porcelains. For example, Vita Mark II ceramic and
product.
Vita VM9 veneering porcelain have indentation hardness val-
The average hardness at 300 mN was chosen for the cal-
ues of 10.64 ± 0.46 and 9.5 ± 0.35 GPa, respectively [6], which
culation of brittleness index after considering the ISE of the
are three times higher than the tested novel infiltrated mate-
material. The value of hardness from heavier loads might be
rial. Several wear test studies have indicated that dental
more comparable to the macro-scale properties of the mate-
porcelains and ceramics generated greater antagonist tooth
rial.
wear than other restorative materials [13–15]. Moreover, it
is generally accepted that harder material may cause more
3.5. SEM observation
severe wear on the antagonist [16]. Therefore, the significantly
lower hardness value of the polymer infiltrated-ceramic than
The microstructure of pre-infiltrated porous ceramic (M2) are
most commercial dental ceramics may be of considerable
shown in Fig. 4A–D, which reveals that the material was made
advantage in order to protect the opposing teeth from exces-
from irregular shaped ceramic phase resulting in irregular
sive wear. However, specific studies are needed to confirm this
pores within the structure which were typically less than 3 ␮m.
speculation.
The SEM images (Fig. 4E–H) of polymer infiltrated-ceramic
Thirdly, the material has similar indentation creep ability
sample (C3) did not show any obvious pores and voids, which
as that of human enamel (∼0.1 ␮m over 900 s) [8]. However, the
indicate that the polymer infiltration was successful. Other
material did not recover automatically as did human enamel
specimens had similar microstructure and fractographic fea-
upon unloading. When considered in more detail, it is interest-
tures, therefore were not included here.
ing to note that polymer infiltrated-ceramic (C3) did not show
any recovery even though it has been infiltrated by polymer.
4. Discussion The possible reason could be, the ceramic particles fractured
during loading become interlocked with each other, which
It has long been the goal for dental material scientists to blocked the recovery of the polymer during the unload hold-
develop a material with similar mechanical behavior to that ing period. This aspect reveals that the infiltrated-ceramic has
of natural human enamel and dentin. The polymer infiltrated a somewhat similar viscous response as human enamel but
ceramic investigated suggests a successful step toward such a lacks the ability of auto-recovery. In human enamel the pres-
goal. ence of the near theoretical strength of the nano-crystallites
Firstly, the material illustrated similar ISE behavior as of hydroxyapatite coupled with the ability of the remnant pro-
observed for human enamel, namely, not only the hardness teins that ‘glue’ these crystallites together to unfold and refold
but also more importantly the elastic modulus of the mate- imparts such recovery ability [17]. By comparing with typical
rial have a relationship to indentation depth or contacting porcelains that do not exhibit creep [8], the creep response
area [7]. Although ISE of dental materials has been docu- of the polymer infiltrated-ceramic, which is similar as that
mented previously [11], to our knowledge, this is the first of human enamel [8], implies that these materials will have
532 d e n t a l m a t e r i a l s 2 7 ( 2 0 1 1 ) 527–534

Fig. 4 – SEM observation of M2 (images A–D) and C3 (images E–H) 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 infiltrated-ceramic material has high fracture
toughness, which is slightly higher than MZ100 CAD/CAM
composite (K1c ∼ 1.4 MPa m1/2 ) [18]. Moreover, all of the poly-
mer infiltrated-ceramic specimens share similar brittleness
index values, which are all lower than 4.3 ␮m1/2 , 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 infiltrated-ceramics have comparable values with
ProCAD (Vivadent-Ivoclar) (B = 1.7 ␮m1/2 ) and VITA Mark II
 d e n t a l m a t e r i a l s 2 7 ( 2 0 1 1 ) 527–534
(VITA Zahnfabrik) (B = 1.6 ␮m1/2 ), and are better than IPS e.max
(Vivadent-Ivoclar) (B = 2.9 ␮m1/2 ). This indicates that the poly-
mer infiltrated ceramics are suitable candidates for CAD/CAM
purposes.
Fifthly, the density and processing pressure had an influ-
ence on the final properties of the materials. As listed in
Tables 2 and 3, higher initial density of the pre-infiltrated
ceramic and higher infiltration pressure gave better mechani-
cal properties, although there was no statistical difference for
E and H. Similar trends can be found for stress–strain response
as well. However, too high a density of the pre-infiltrated
ceramic may result in incomplete polymer infiltration. Thus,
the density of pre-infiltrated ceramic and infiltration pressure
must be optimized.
Lastly, SEM observations of the microstructure of the
material indicate that the porous pre-infiltrated block was suc-
cessfully infiltrated. Polymer infiltration did not change the
fracture pattern of the ceramic preforms significantly. 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 deflection effects of tough ceramic parti-
cles, the chances for chipping out of the whole particle are
much less than those of pre-infiltrated ceramics. Therefore, it
is reasonable to find that the cutting surface of polymer infil-
trated ceramic (Fig. 4E) is smoother than that of pre-infiltrated
ceramic (Fig. 4A). Moreover, the flat facets in Fig. 4A and E were
believed to be the outcome of grinding with the cutting wheel
rather than direct cutting through the tough ceramic particles.
In short, for pre-infiltrated porous materials, cracks propa-
gated along the boundaries of the ceramic crystals (M2), and
for polymer infiltrated 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 deflection.
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 firing,
the one-step manipulation helps ensure a high degree of
dimensional accuracy of the final 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 with lower 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 phantom teeth 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
533
should be thoroughly investigated before the material can be
released for clinical applications.
5. Conclusions
These novel polymer infiltrated ceramic restorative materi-
als have averaged elastic modulus, hardness, and fracture
toughness values of 30.14 GPa, 2.59 GPa, and 1.72 MPa m1/2 ,
respectively, depending on the manufacturing conditions. The
density of pre-infiltrated ceramic and polymer pressure of
processing influence the final 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
human enamel. SEM observation indicates that the infiltration
of polymer was successful and the high fracture toughness of
the material was due to a crack deflection 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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