d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 769–775

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Characterization and surface treatment effects

on topography of a glass-infiltrated
alumina/zirconia-reinforced ceramic

Alvaro Della Bona a,∗ , Tiago A. Donassollo b , Flávio F. Demarco b ,

Allyson A. Barrett c , John J. Mecholsky Jr. d
a Dental School, The University of Passo Fundo, P.O. Box 611/613, Campus I, BR 285, Km171, Passo Fundo, RS 99001-970, Brazil
b Dental School, Federal University of Pelotas, RS, Brazil
c Department of Dental Biomaterials, University of Florida, Gainesville, FL, USA
d Department of Materials Science and Engineering, University of Florida, Gainesville, FL, USA

a r t i c l e i n f o a b s t r a c t

Article history: Objective. Characterize the microstructure, composition and some physical properties of a
Received 23 March 2006 glass-infiltrated alumina/zirconia-reinforced ceramic (IZ) and the effect of surface treatment
Accepted 20 June 2006 on topography.
Methods. IZ ceramic specimens were fabricated according to ISO6872 instructions and pol-
ished through 1 ␮m alumina abrasive. Quantitative and qualitative analyses were performed
Keywords: using scanning electron microscopy (SEM), backscattered imaging (BSI), electron dispersive
Microstructure spectroscopy (EDS) and stereology. The elastic modulus (E) and Poisson’s ratio () were deter-
Composition mined using ultrasonic waves, and the density () using a helium pycnometer. The following
Surface topography ceramic surface treatments were used: AP-as-polished; HF-etching with 9.5% hydrofluoric
Physical properties acid for 90 s; SB-sandblasting with 25 ␮m aluminum oxide particles for 15 s and SC-blasting
Ceramic with 30 ␮m aluminum oxide particles modified by silica (silica coating) for 15 s. An optical
profilometer was used to examine the surface roughness (Ra) and SEM–EDS were used to
measure the amount of silica after all treatments.
Results. The IZ mean property values were as follows:  = 4.45 ± 0.01 g/cm3 ;  = 0.26 and
E = 245 GPa. Mean Ra values were similar for AP- and HF-treated IZ but significantly increased
after either SC or SB treatment (p ≤ 0.05). The surface concentration of Si(K) increased 76%
after SC treatment.
Significance. HF is an inadequate surface treatment for bonding resins to IZ ceramic. Treating
IZ with either SB or SC produced greater Ra values and the SC showed a significant increase in
the surface concentration of silica, which may enhance bonding to resin via silane coupling.
© 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

1. Introduction rior mechanical properties. The development of new technolo-

gies and research are introducing these materials to dentistry.
Zirconia-based ceramics have been used for a great number of In-Ceram Zirconia (IZ) (In-Ceram Zirconia, Vita Zahnfab-
applications in the bioengineering field because of their supe- rik, Germany) was developed by adding partially stabilized

∗
Corresponding author. Tel.: +55 54 3311 5142; fax: +55 54 3316 8403.
E-mail address: dbona@upf.br (A. Della Bona).
0109-5641/$ – see front matter © 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2006.06.043
770 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 769–775
zirconia to In-Ceram Alumina, combining the toughening
mechanisms of zirconia with the established technology used
for the partially sintered glass-infiltrated alumina to produce
stronger, tougher metal-free ceramic restorations that can be
successfully used as posterior three-unit fixed bridges [1–4].
There are some studies reporting the microstructure, compo-
sition and mechanical properties of IZ [2–10]. However, none
of them present a complete characterization of the ceramic IZ
microstructure related to the effect on surface treatment.
Quantifying microstructural parameters is important
to develop structure/property relationships. Quantitative
microstructural analysis provides an association among the
constitution, physical properties, and structural characteris-
tics of materials [1,11,12].
There are several physical and mechanical properties con-
ventionally used to characterize the behavior of ceramics,
such as: elastic modulus (E), Poisson’s ratio () and density ().
The elastic or Young’s modulus (E) is a measure of the stiff-
ness or the material’s resistance to elastic deformation. The
greater the modulus, the stiffer the material, or the smaller
the elastic strain that results from the application of a given
stress. The modulus is an important design parameter used
for computing elastic deflections. Poisson’s ratio () is the ratio
of the lateral to axial strain. Theoretically, a typical  value
for isotropic materials is 0.25, but the maximum may be as
high as 0.50. It is related to the shear modulus (G) and elas-
tic modulus [E = 2G (1 + )] [13]. Since the velocity at which
sound travels through a solid can be readily measured by
ultrasonic wave transducers and receivers, the velocity of the
sound wave and the density () of the material can be used
to calculate the dynamic Young’s modulus and Poisson’s ratio
values [14].
The volume of crystalline materials and their volume
changes with temperature are closely related to the crystal
structures. The density () is directly determined by the crystal
structure, that is, the efficiency of atomic packing. The den-
sity, as usually measured (g/cm3 ), depends on the number of
atoms per cubic centimeter and on the atomic weight of the
constituents. The volume of a glass is largely determined by
the nature of the vitreous network. The density is a minimum
value for the pure network former and increases as modifier
ions are added [15].
Ceramic microstructure and composition are also control-
ling factors in the development of a micromechanical reten-
tive surface by acid etching, which is the most popular surface
treatment process leading to resin bonding [11]. However, the
high crystalline content ceramics are resistant substrates to
surface degradation by acid etching [16–18] and are difficult to
bond chemically to resins via silane coupling agents because
of the reduced silica-based matrix.
Silica coating the ceramic surface seems to be a promising
method to promote the bonding of acid-resistant ceramics to
resin. It has been suggested that this surface treatment pro-
cedure can increase the silica content on ceramics and metals
enhacing the bond to resins via silane agents [17–20]. How-
ever, there is limited knowledge regarding the surface topog-
raphy and chemical changes after treating the acid-resistant
ceramics.
The objective of this study is to characterize the microstruc-
ture, composition, and some of the physical properties
of a glass-infiltrated alumina/zirconia-reinforced ceramic
(IZ) (In-Ceram Zirconia, Vita Zahnfabrik, Germany) and
to examine the topography resulting from surface treat-
ments, testing the hypothesis that the silica content on
the high crystalline ceramic surface is increased by silica
coating.
2. Materials and methods
In-Ceram Zirconia specimens (12 mm × 2 mm) were fabricated
according to ISO6872 instructions and supplied by the man-
ufacturer (VITA Zahnfabrik, Bad Säckingen, Germany). The
specimens were polished through 1 ␮m alumina abrasive
before performing the analytical analyses.
The dynamic elastic modulus (E) and Poisson’s ratio () were
determined by means of ultrasonic waves and a computer pro-
gram (ECALC and Sigview-F software, Nuson Inc., Boalsburg,
PA, USA) based on a set of equations that uses the time of
flight, density (), and thickness (t). The specimen thickness (t)
was measured using a digital caliper (Digimatic caliper, Mitu-
toyo Co., Kawasaki, Japan) and the weight (w) of the specimen
was obtained using an analytical balance (Mettler H31, Mettler
Instrument Corp., Hightstown, NJ, USA). The density () of the
material was obtained using a Helium Pycnometer (Accupyc
1330, Micromeritics Instrument Co., Norcross, GA, USA) after
calculating the volume (V). Piezoelectric transducers/receivers
(Ultran Laboratories Inc., Boalsburg, PA, USA) and an ultra-
sonic pulse apparatus (Ultima 5100, Nuson Inc., Boalsburg)
were used to measure the time of flight through the ceramic
specimens. Longitudinal and shear (transverse) time of flight
values were obtained and used to calculate the  and E of the
ceramic.
Semi-quantitative and qualitative analyses were per-
formed using scanning electron microscopy (SEM), backscat-
tered imaging (BSI), electron dispersive spectroscopy (EDS) and
stereology principles.
As-polished (AP) IZ specimens were mounted on aluminum
stubs using carbon coating paste for better conductivity and
were carbon coated in a vacuum evaporation system (Ion
Equipment Co., Santa Clara, CA, USA). The thickness of the
carbon layer was approximately 250 Å. Secondary electron
and backscattered images (SEI and BSI) were recorded. The
composition of each ceramic phase was determined by elec-
tron dispersive spectroscopy (EDS) using a scanning electron
microscope (JSM-6400, Jeol LTD., Tokyo, Japan) and the ZAF
correction method. The analysis was performed at an acceler-
ating voltage of 15 kV. Each ceramic phase was analyzed three
times at different locations and average values of composi-
tion were determined. Compositional element concentrations
above 1 wt% were recorded.
The crystalline volume fraction (Vv) was estimated based
on stereological principles. An auto beam-area measure-
ment function was used based on intensity histograms from
backscattered electron images (Link ISIS program, Oxford,
England and Link ISIS Instruments, Microanalysis Group,
Bucks, England). Eight different areas from three specimens
were used and averaged for the Vv value.
As-polished (AP) IZ ceramic specimens were surface
treated as follows:
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 769–775 771

HF: Etching with 9.5% HF (Ultradent Products Inc., South Jor-

dan, UT, USA) for 90 s, rinse with water spray for 30 s, and dry
with oil-free air spray.
SB: Sandblasting with 25-␮m aluminum oxide particles
(Micro-Etcher - Danville Inc., San Ramon, CA, USA), using the
following parameters: blasting perpendicular to the surface
at a distance of 10 mm for 15 s, at a pressure of 2.8 bar.
SC: Blasting with 30 ␮m aluminum oxide particles modified
by silica (CoJet System, 3M-ESPE, MN, USA), using the same
blasting parameters applied for the SB.

Ceramic surface roughness parameters for AP, HF, SB, and

SC treated specimens were determined using an optical pro-
filometer (Wyko NT1000, Wyko Corp. and Veeco Instruments
Inc., Tuscon, AZ, USA) and software (Wyko Vision32, Version
2.210, Wyco and Veeco). The scan length of 50 ␮m collected 687
frames using a magnification of 10×. Five different locations
in three specimens (n = 15) were measured. Mean Ra values
were statistically analyzed using One-way analysis of variance
(Anova) and Tukey’s test (˛ = 0.05).
Some AP, HF, SB and SC treated IZ specimens were also
mounted on aluminum stubs as described above for SEM/EDS
analyses. Silica mappings were generated from all ceramic
treatments in addition to the compositional element analy-
sis.
3. Results
Fig. 1 – A Representative photomicrography (SEM in BSI
mode) of carbon coated AP treated In-Ceram Zirconia; the
light crystals identified with numbers 1 and 2 are zirconia,
the dark crystals are alumina (numbers 3 and 4), and the
glassy phase is in grey (number 5). The image is colored by
the ISIS software for volume fraction calculations. An
intensity histogram is produced from the percentage values
of red (zirconia) and green (alumina) as measured by the
Link ISIS computer program. Magnification is 5000× (For
interpretation of the references to color in this figure legend,
the reader is referred to the web version of the article.).

The mean and standard deviation values of volume fraction

shown in Fig. 3A–D. The mean surface silicon content val-
(Vv), density (), dynamic elastic modulus (E), and Poisson’s
ues (element percentage of Si) and the mean values of the
ratio () of the IZ ceramic are as follows: (Fig. 1).
roughness parameters for the IZ ceramic surface treatments
used in this study are summarized in Table 1. As alumina and
VV(alumina) = 63.7 ± 9.3%; VV(zirconia) = 32.4 ± 7.7%;
zirconia crystals are not etched by HF, similar mean Ra val-
VV(glass matrix) = 4.0 ± 2.1% ues are shown by AP- and HF-treated ceramic surfaces. The
latter showed a slightly higher value probably because the
acid etches the scarce glassy matrix, which can be observed
 = 4.45 ± 0.01 g/cm3 in the SEM image (Fig. 3B) and by the decrease in Si con-
tent on the HF-treated surface (1.25–0.87%) (Table 1). Yet, SEM
E = 245 ± 6 GPa images and roughness profiles show a higher retentive sur-
face pattern for SB- and SC-treated surfaces (Fig. 3C and D),
which agrees with the significantly increased mean Ra values
 = 0.26 ± 0.005
(Table 1). Such surface morphology should increase the bond
A representative SEM–BSI micrographs of the microstruc- to resin by micromechanical retention. In addition, the sili-
ture is depicted in Fig. 1. The different phases were identified con content increased 76% on the SC treated ceramic surface
and semi-quantitative EDS analyses were performed (Fig. 2)
at representative areas (numbers 1–5 in Fig. 1). EDS analysis of
the compositional element concentration of IZ ceramic phases
revealed alumina [Al(K) 49.4%] and zirconia [Zr(L) 31.8%] crys-
tals in a glassy matrix based on La2 O3 [22.5% La(L)]. The aver-
age composition of the zirconia phase (Fig. 2), without carbon
and oxygen is as follows: Zr(L) 82.0%; Ce(L) 16.5% and Al(K)
1.2%. The average composition of the alumina phase (with-
out carbon and oxygen) is Al(K) 99.8%. The results suggest
a zirconia-reinforced, alumina-based ceramic infiltrated by a
lanthanum oxide-based glass. In addition, the zirconia phase
is stabilized by cerium oxide.
Representative SEM photomicrographs and roughness pro- Fig. 2 – Representative semi-quantitative EDS analysis with
files of the ceramic surface treatments used in this study are ZAF correction of the composition of zirconia crystals.
772 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 769–775

Fig. 3 – Representative images of the treated IZ ceramic surface topography (SEM photomicrographs, magnification 5000×)
and surface roughness (optical profilometry, magnification 10×). (A) As-polished IZ ceramic surface. (B) HF-treated IZ
ceramic surface. (C) IZ surface sandblasted with 25 ␮m alumina particles. (D) Silica coated IZ ceramic surface.
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 769–775
Table 1 – Mean values of roughness parameters, statistical grouping for Ra and the amount of silica for the ceramic
surface treatments used on the In-Ceram Zirconia
Surface treatments Ra*
As-polished (AP) 207 ± 17 nm a
Hydrofluoric acid (HF) 231 ± 14 nma
Sandblasting (SB) 1.0 ± 0.2 ␮mb
Silica coating (SC) 836 ± 49 nmb
Ra, the average roughness as calculated over the entire measured array. * Different superscript letters (a and b) indicate statistical significant dif-
ferences (p < 0.05); Rq, the root-mean-squared roughness calculated over the entire measured array; Rt, the peak-to-valley difference calculated
over the entire measured array.
(1.25–2.20%) (Table 1). This should also increase the chemical
bond to resin via silane agents.
4. Discussion
Most of today’s high-strength ceramic materials are based
on alumina and/or zirconia. The In-Ceram system has been
developed using an alumina slip casting technique to build the
framework that is fired to form an open-pore microstructure,
which is infiltrated with lanthanum oxide-based glass. There-
fore, the values indicating the high mechanical properties of
this system depend upon the complete wetting of the porous
microstructure by glass infiltration. It has been reported that
an addition of about 33 wt% of zirconia (In-Ceram Zirconia)
resulted in an increase in flexural strength values from 500 to
about 750 MPa [2,9,21]. Therefore, as a different material, the
In-Ceram Zirconia (IZ) needs to be characterized and its prop-
erties well understood to estimate the clinical performance of
such ceramic.
Microscopic examination is useful for the study and char-
acterization of materials. Examination of microstructures is
often related to material properties and the information is
used to predict properties and improve the design of new
materials [11].
Structurally, all ceramic materials are either crystalline,
partially crystalline, or amorphous. Most crystalline ceram-
ics, except for single crystals, are actually polycrystalline
because they are composed of a large number of small
crystals, or grains, separated from one another by grain
boundaries. So, there are important relationships between
chemical composition, atomic structure, fabrication process,
microstructure, and the properties of polycrystalline ceramics.
Therefore, quantifying microstructural parameters is impor-
tant to develop structure/property relationships. Quantitative
microstructural analysis provides an association among the
constitution, physical properties, and structural characteris-
tics of materials [11].
Several methods can be used to determine ceramic compo-
sition. This study employed a semi-quantitative analysis using
electron dispersive spectroscopy (EDS), according to the pro-
tocol suggested by Della Bona and Anusavice [11]. According
to those authors, this is one of the more reliable methods to
analyze the composition of different ceramic phases.
Most dental ceramics with a high content of zirconia are
partially stabilized by yttria and show high strength values
[6,16,18,19,22]. This study showed that the zirconia in the IZ
773
Rq Rt Si(K) element %
321 ± 14 nm 12.5 ± 3.4 ␮m 1.25
330 ± 10 nm 24.2 ± 3.1 ␮m 0.87
1.6 ± 0.5 ␮m 63 ± 4 ␮m 0.98
1.6 ± 0.1 ␮m 55 ± 2 ␮m 2.21
ceramic is partially stabilized by ceria (Ce(L) 7.5%) with no
traces of yttrium (Y) in the ceramic composition.
The brittle nature of ceramics demands a greater margin
of safety in strength than with metals. All dental ceramics
tend to fail at the same critical strain of the order of 0.1%
[23]. For this reason, any increases in strength and toughness
have to be associated with an increase in the elastic modulus.
The mean Poisson’s ratio and dynamic elastic modulus values,
respectively 0.26 and 245 GPa, are very similar to the mean val-
ues reported by a previous study (0.26 and 240 GPa) [9]. These
same authors estimated the crystalline volume fraction (Vv)
of IZ based on stereology principles using transparent grids
and the line-intercept technique. The average percentage for
each phase had to be calculated due to the presence of mul-
tiple phases and the variety of grain shapes. Therefore, they
reported 33% of alumina, 34% of zirconia, 23% of glass and 8%
porosity [9]. The present study used an auto beam-area mea-
surement function based on intensity histograms from several
BSE images to estimate the average Vv value of the different
ceramic phases. The Vv analysis revealed 63% of alumina, 32%
of zirconia and 4% of glass matrix. The results are from AP
ceramics, so no porosity was observed, which may explain the
difference from results reported by Guazzato et al. [9], where
the IZ specimens were HF etched for 30 min.
A density value of 3.86 g/cm3 has been reported for In-
Ceram Alumina [21]. However, no other study has reported
the density value for IZ that seems to be a reasonable value
(4.45 g/cm3 ) for this type of ceramic [24].
Creating an effective micromechanical retentive ceramic
surface is crucial for an adequate adhesive bond and/or repair
of ceramic restorations [25]. Resin penetration and polymer-
ization into this retentive surface produce the most important
adhesion mechanism of the resin–ceramic systems [25–29].
Several procedures have been reported and used clinically
to produce a similar micromechanical retentive ceramic sur-
face. The most popular is acid etching with hydrofluoric acid
(HF). Laboratory and in-office airborne particle abrasion sys-
tems have also been applied. These systems generally use two
types of abrasives: alumina particles (SB) and silica modified
alumina particles (SC-silica coating systems). The goal of the
SC systems is to promote a retentive surface and to deposit a
silica layer on ceramic and metal surfaces [11,16,17,26,29–34].
However, a surface treatment can produce different retentive
patterns on ceramics with different microstructure and com-
position [11].
This study showed that treating IZ ceramic using 9.5% HF
for 90 s produced a similar surface topography as the non-
774 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 769–775
treated IZ ceramic (AP group), which is in agreement with
the mean Ra values obtained from the HF and AP treated sur-
faces (Table 1 and Fig. 3A and B). This result can be explained
because the HF preferably etches the glassy phases, usually
silica-based phases, to produce a retentive surface [35–41].
However, the IZ ceramic contains a small amount of a lan-
thanum oxide-based glassy matrix (4%), which hinders the HF
etching action and the production of micromechanical reten-
tive sites, in accord with previous works [7,27]. Yet, EDS anal-
ysis and silica mapping of the IZ ceramic surfaces showed
that there is a reduction in silicon [Si(K)] after HF treatment
(1.25–0.87%), supporting the assumption of the HF action on
the glass matrix.
Statistically significant ceramic surface changes were pro-
duced after either sandblasting with alumina particles (SB) or
silica coating (SC) the IZ ceramic surfaces (mean Ra values
in Table 1). The topography changes produced by SB and SC
ceramic treatments were also evident under the SEM (Fig. 3C
and D), supporting other studies [17,30]. In addition, EDS anal-
ysis and silica mapping of the SC treated IZ ceramic surface
showed that there is a 76% increase in the silicon [Si(K)] surface
content (2.2%) when compared with the AP surface (1.25%)
(Table 1), which should benefit the chemical bonding mech-
anism of resin to ceramic via silane coupling agents.
Many studies have shown that high alumina content
ceramics are resistant to HF etching and just minor topo-
graphic changes are observed after airborne particle abrasion
with alumina particles (SB) resulting in low bond strength
values to resin materials [16,17,20,29,31,33,34]. However, it
has also been suggested that the association of mechani-
cal (via micro-retention using silica coating) and chemical
(via silane coupling) adhesive mechanisms produce better
bond strengths of high crystalline content ceramics bonded
to resins [17,28–30,32]. Although the SB treated ceramic
surface showed the highest mean Ra value, there was a
reduction in the surface silicon [Si(K)] (from 1.25 to 0.98%),
which may reduce the efficiency of bonding to resin via
silane coupling, if the previously mentioned rationale is
used.
Compared to AP ceramic, the SC treated ceramic also
showed a significant increase in the mean Ra value, which
was no different from the mean value of SB treated ceramic
(Table 1). In addition, the silica coated IZ ceramic surfaces
showed a significant increase (76%) in the concentration of
surface silicon, confirming the hypothesis of this study. This
finding should improve both the mechanical and chemical
bond mechanisms to resin. This assumption agrees with bond
strength experiments that reported the highest mean bond
strength values for resin bonded to silica coated alumina-
based ceramics [16,17,26,29,31,34]. The mean Ra values from
this work are in agreement with the results from other studies
[30,33].
5. Conclusions
The characterization procedures showed that the In-Ceram
Zirconia (IZ) is a ceria stabilized zirconia-reinforced, alumina-
based ceramic infiltrated by a lanthanum oxide-based glass.
This polycrystalline material has a dynamic elastic modulus
(245 GPa) and Poisson’s ratio (0.26) compatible with this type
of ceramic.
For clinical purposes, the microstructural and composi-
tional analyses along with the optical profilometry, revealed
an acid resistant ceramic material, to which an HF treat-
ment produces an inadequate retentive surface pattern for
bonding to resins. However, treating the IZ ceramic with
the airborne particle abrasion systems (SB and SC) produced
significantly greater mean Ra values, which should bene-
fit the mechanical bond mechanism to resin-based materi-
als. In addition to the significant topography changes, the
SC treated ceramic produced a 76% increase in the concen-
tration of surface silicon [Si(K)], which should also benefit
the chemical bond mechanism to resins, via silane coupling
agents.
Acknowledgments
A preliminary report was presented at the 82th Meeting of the
International Association for Dental Research, in Honolulu,
USA.
The authors thank Major Analytical Instrumentation Cen-
ter (MAIC, Department of Materials Science and Engineering,
University of Florida) for the assistance with the analytical
procedures and instruments.
This study was partially supported by CNPq do Brasil grant
# 300659/2003-2.
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