Effect of particle size on the flexural

strength and phase transformation of an

airborne-particle abraded yttria-stabilized
tetragonal zirconia polycrystal ceramic
Renata Garcia Fonseca, DDS, MSc, PhD,a
Filipe de Oliveira Abi-Rached, DDS, MSc,b
José Maurício dos Santos Nunes Reis, DDS, MSc, PhD,c
Elisa Rambaldi, PhD,d and Paolo Baldissara, DDS, MSc, PhDe
Araraquara Dental School, São Paulo State University - UNESP,
Araraquara, São Paulo, Brazil; School of Dentistry, Alma Mater
Studiorum - University of Bologna, Bologna, Italy
Statement of problem. Because airborne-particle abrasion is an efficient method of improving the bond at the zirconia-
cement interface, understanding its effect on the strength of yttria-stabilized tetragonal zirconia polycrystal is important.

Purpose. The purpose of this study was to evaluate the effect of the particle size used for airborne-particle abrasion on the
flexural strength and phase transformation of a commercially available yttria-stabilized tetragonal zirconia polycrystal
ceramic.

Material and Methods. For both flexural strength (20.0
4.0
1.2 mm) (n¼14) and phase transformation (14.0-mm
diameter
1.3-mm thickness) (n¼4), the zirconia specimens were made from Lava, and their surfaces were treated in the
following ways: as-sintered (control); with 50-mm aluminum oxide (Al2O3) particles; with 120-mm Al2O3 particles; with 250-
mm Al2O3 particles; with 30-mm silica-modified Al2O3 particles (Cojet Sand); with 120-mm Al2O3 particles, followed by 110-
mm silica-modified Al2O3 particles (Rocatec Plus); and with Rocatec Plus. The phase transformation (%) was assessed by x-ray
diffraction analysis. The 3-point flexural strength test was conducted in artificial saliva at 37 C in a mechanical testing
machine. The data were analyzed by 1-way ANOVA and the Tukey honestly significant difference post hoc test (a¼.05).

Results. Except for the Cojet Sand group, which exhibited statistically similar flexural strength to that of the as-sintered group
and for the group abraded with 250-mm Al2O3 particles, which presented the lowest strength, airborne-particle abrasion with
the other particle sizes provided the highest values, with no significant difference among them. The as-sintered specimens
presented no monoclinic phase. The groups abraded with smaller particles (30 mm and 50 mm) and those treated with the
larger ones (110 mm and/or 120 mm particles and 250 mm) exhibited percentages of monoclinic phase that varied from 4% to
5% and from 8.7% to 10%.

Conclusions. Except for abrasion with Cojet Sand, depending on the particle size, zirconia exhibited an increase or a decrease
in its flexural strength. Airborne-particle abrasion promoted phase transformation (tetragonal to monoclinic), and the
percentage of monoclinic phase varied according to the particle size. (J Prosthet Dent 2013;110:510-514)

Clinical Implications
Although yttria-stabilized tetragonal zirconia polycrystal exhibits high
mechanical strength, some procedures, for example, airborne-particle
abrasion, indicated for improving the bond at the zirconia-cement
interface, may affect this property, depending on the particle size used.

a
Associate Professor, Department of Dental Materials and Prosthodontics, Araraquara Dental School, São Paulo State University - UNESP.
b
PhD Student, Department of Dental Materials and Prosthodontics, Araraquara Dental School, São Paulo State University - UNESP.
c
Assistant Professor, Department of Dental Materials and Prosthodontics, Araraquara Dental School, São Paulo State University - UNESP.
d
Researcher, Centro Ceramico Bologna.
e
Professor, Department of Oral Sciences, Division of Prosthodontics, School of Dentistry, Alma Mater Studiorum - University of Bologna.

The Journal of Prosthetic Dentistry Garcia Fonseca et al

December 2013
The use of yttria-stabilized tetragonal
zirconia polycrystal (Y-TZP) to manu-
facture ceramic-fixed prostheses has
increased substantially because of its
high fracture toughness1,2 and flexural
strength,2-4 which allows the use of
metal-free partial fixed dental prostheses
in areas of high masticatory load.5,6
However, some procedures such as
milling with computer-aided design and
computer-aided manufacturing (CAD/
CAM) technology,7 grinding with dia-
mond rotary instruments,8,9 and
airborne-particle abrasion3,7 may create
surface flaws on the zirconia, which act
as stress concentration sites.3,8 As a
consequence, the behavior of the zirco-
nia is unpredictable, increasing8,10,11 or
decreasing3,9,12 its strength, with the
latter resulting from crack initiation and
propagation toward the bulk of the
material.3,9,12
When airborne-particle abrasion is
used, the particle size may affect the
strength of the zirconia. Studies2,7,10,13
that evaluated the effect of different
particle sizes used in airborne-particle
abrasion on the strength of zirconia are
limited and have produced conflicting
results.8,9,14 Another aspect that could be
affected by particle size and, therefore,
should be investigated together with the
study of zirconia strength is its phase
transformation (tetragonal to mono-
clinic). Although this effect has been
investigated to a limited extent13,15 and
studies8,10,11,15 related to phase trans-
formation and strength have been per-
formed, their results are not conclusive.
Airborne-particle abrasion is one of
the most-efficient methods of promoting
micromechanical retention and conse-
quently improving the bond at the
zirconia-cement interface.16-19 This
method is indicated for minimally reten-
tive tooth preparations and the minimal
inherent mechanical retention of CAD/
CAM-milled zirconia. When considering
that the influence of airborne-particle
abrasion on the strength and phase
transformation of the Y-TZP ceramics
is not yet fully clarified in the literature,
the purpose of this in vitro study was
to analyze the effect of different Al2O3
particle sizes, silica modified or not,
Garcia Fonseca et al
on the flexural strength and phase trans-
formation of a commercially available Y-
TZP ceramic. The null hypotheses were
that different Al2O3 particle sizes do not
influence flexural strength.
MATERIAL AND METHODS
A total of 98 bar-shaped specimens
(20.0
4.0
1.2 mm) were prepared for
3-point flexural strength testing (ac-
cording to ISO 6872),20 and 14 disk-
shaped specimens (14.0-mm dia-
meter
1.3-mm thickness) were pre-
pared for x-ray diffraction analysis. The
specimens were obtained by cutting
presintered CAD/CAM zirconia milling
blocks (Lava Frame; 3M ESPE AG) with a
saw (Isomet 1000; Buehler Ltd) with
a diamond-coated disk (Diamond
Wafering Blade, Series 15LC Diamond
no. 11-4276; Buehler Ltd) under con-
stant water irrigation. The specimens
were washed in tap water to remove
the cutting debris and were finished
manually with a ceramic polisher (Exa
Cerapol 0361HP; Edenta AG) with a
slow-speed handpiece under wet con-
ditions. All the specimens were sin-
tered in an oven (Lava Furnace 200;
Dekema Dental-Keramiköfen GmbH)
according to the manufacturer’s in-
structions (heating rate ¼20 C/min:
0 C-1000 C; 10 C/min: 1000 C-1500 C;
holding time ¼2 hours and cooling rate ¼
15 C/min: 1500 C-800 C; 20 C/min:
800 C-250 C, the oven was opened
at 250 C).
1 Three-point flexural strength test.
511
One surface on each specimen was
treated as follows: as-sintered (control);
airborne-particle abraded with 50-mm
Al2O3 particles; with 120-mm Al2O3 par-
ticles; with 250-mm Al2O3 particles; with
30-mm silica-modified Al2O3 particles
(Cojet Sand; Al2O3 >97 wt% and amor-
phous silica <3 wt%); with 120-mm Al2O3
particles, followed by 110-mm silica-
modified Al2O3 particles (Rocatec Plus;
Al2O3 >95 wt% and amorphous silica 1
to 5 wt%); and with Rocatec Plus. For the
airborne-particle abrasion, the specimens
were mounted in special holders, ac-
cording to their shape (bar or disk), at a
perpendicular distance of 10 mm from
the tip of the airborne-particle abrasion
unit (Basic Classic; Renfert GmbH).21 The
specimens were then airborne-particle
abraded for 20 seconds at a pressure of
0.28 MPa. All specimens were ultrasoni-
cally cleaned in distilled water for 10
minutes.
Specimens from each group (n¼14)
were loaded into a 3-point flexural
strength fixture (15-mm span), with the
airborne-particle-abraded surface sub-
jected to the tensile force at a crosshead
speed of 1.0 mm/min and a 5 kN load
cell2 (Fig. 1). The test was performed in
artificial saliva at 37 C in a mechanical
testing machine (EMIC DL2000; EMIC
Equipment and Systems Testing Ltd).
The data (MPa) were analyzed by 1-way
ANOVA followed by the Tukey honestly
significant difference post hoc test
(a¼.05). The software used was SPSS
19.0 (Statistical Package for Statistical
Science Inc).
512 Volume 110 Issue 6
2000 reported similar behavior with 25-mm
Al2O3 particles. Qeblawi et al2
1800
also observed that the use of 30-mm
1600 silica-modified Al2O3 particles did not
Flexural strength (MPa)

1400 result in statistically higher flexural

strength when compared with the non-
1200 abraded specimens (control group) and
1000 explained this finding by saying that
these small particles may have been less
800
effective at inducing phase trans-
600 formation on the surface of the Y-TZP
400 ceramic. Indeed, in the present study,
abrasion with Cojet Sand resulted in a
200
slight (4%) phase transformation
0 (tetragonal to monoclinic) of zirconia,
120 µm
Cojet 50 µm Rocatec 120 µm Al2O3 + 250 µm which was not enough to influence its
as-sintered
Sand Al2O3 Plus Al2O3 Rocatec Al2O3 flexural strength. Borchers et al23 also
Plus found an increase in monoclinic phase
Mean 872.8 B 1028.6 B 1410.9 A 1535.7 A 1509.4 A 1497.9 A 618.0 C content, with no statistically significant
2 Flexural strength mean values (MPa), standard deviations, and statistical results. effect on the biaxial flexural strength of
Different uppercase letters indicate significant differences (P<.05). zirconia after storage in different hydro-
thermal conditions. According to these
X-ray diffraction analysis was used to abrasion conditions promoted the high- investigators,23 the transformation zone
assess the effect of the particle size used est flexural strength values, with no sta- has to extend to a certain depth of the
for airborne-particle abrasion on the tistically significant differences among zirconia to affect its strength. In addition
phase transformation of zirconia. Spec- them. to the smaller size of the Cojet Sand
imens from each group (n¼4) were The as-sintered specimens exhibited particles, according to Zhang et al,24 the
analyzed by an x-ray powder diffrac- no monoclinic phase, whereas the other silica particles are soft and round, which
tometer (D8 Advance; Bruker Axs Ltd) groups exhibited an amount of this may have also contributed to the
with graphite-monochromated Cu Ka phase that varied from 4% to 10%. The behavior of the zirconia in response to
radiation (l¼1.5406 Å, generator set at groups abraded with smaller particles airborne-particle abrasion with Cojet
40 kV and 40 mA). Scans were per- (30 mm and 50 mm) exhibited 4% and Sand particles.
formed from 10 to 100 degrees (2q) at a 5% of monoclinic phase, respectively. In contrast, abrasion with 250-mm
step size of 0.02 degrees, with a The groups abraded with 110- and/or Al2O3 particles provided a significant
measuring time of 6 seconds per step. 120-mm particles showed percentages decrease in flexural strength and 10% of
The monoclinic phase fraction was of monoclinic phase that varied from monoclinic phase content. According to
calculated according to the Garvie and 8.7% to 9%. Abrasion with 250-mm Zhang et al,24 when zirconia ceramic is
Nicholson method.22 Al2O3 particles provided 10% of airborne-particle abraded, the outward
monoclinic phase. The relationship be- expansion, as a result of the phase trans-
RESULTS tween particle size and monoclinic formation of the grains, promotes a
phase content (%) is demonstrated in plastic deformation of the surrounding
One-way ANOVA revealed that the 3- Figure 3. zirconia, which, in turn, provides
point flexural strength was affected by compressive stresses. Although airborne-
the particle size (df¼6, F¼54.2, DISCUSSION particle abrasion is considered to be a
P<.001). The flexural strength mean more gentle process, which results in
values (MPa), standard deviations, and The results of this study did not lower stresses and lower temperatures
the statistical groupings identified with provide evidence to support the when compared with grinding,10 it is
the Tukey honestly significant difference null hypotheses because the particle size possible that the compressive stresses that
test are presented in Figure 2. Except affected the flexural strength (P<.001) result from the phase transformation were
for the Cojet Sand, which provided sta- of zirconia. The abrasion with Cojet not able to counteract the propagation of
tistically similar mean flexural strength to Sand, which consists of 30-mm silica- cracks, which originated from severe
the as-sintered group and for airborne- modified Al2O3 particles, promoted alumina abrasion, decreasing the bulk
particle abrasion with 250-mm Al2O3 statistically similar flexural strength strength of zirconia.
particles, which exhibited the lowest when compared with the as-sintered Airborne-particle abrasion with
strength, the other airborne-particle group (control group). Curtis et al13 50-mm Al2O3 particles significantly
The Journal of Prosthetic Dentistry Garcia Fonseca et al
December 2013
12.0
Monoclinic phase content (%)
10.0
8.0
6.0
4.0
2.0
0.0
Cojet
as-sintered
Sand
Mean 0.0 4.0
3 Monoclinic phase content (%) of all groups.
increased the flexural strength of zirconia
and provided 5% of monoclinic phase.
Qeblawi et al2 also reported an increase
in flexural strength promoted by abra-
sion with 50-mm Al2O3 particles when
compared with the Cojet Sand and the
control groups. However, Karakoca and
Yilmaz8 highlight the fact that the abra-
sion of densely sintered core ceramics
with these small particles may not be
effective in providing irregularities on the
surface of the restoration; these irregu-
larities are essential for improving the
bond strength with resin cements by
means of micromechanical retention.
This limitation could be solved by using
120-mm Al2O3 particles, Rocatec Plus, or
the combination of both. Wang et al7
showed that abrasion with 120-mm
Al2O3 particles significantly increased the
surface roughness of zirconia in com-
parison with 50-mm Al2O3 particles. In
addition, the present study showed that
these larger particles (110 and 120 mm)
also provided an increase in flexural
strength when compared with the con-
trol group and were less aggressive than
250-mm Al2O3 particles. Kosmac et al10
and Guazzato et al11 also observed an
increase in biaxial flexural strength with
110-mm Al2O3 particles when compared
with the as-sintered groups.
Overall, the flexural strength results
of the present study indicate that,
Garcia Fonseca et al
120 µm
50 µm Rocatec 120 µm Al2O3 + 250 µm
Al2O3 Plus Al2O3 Rocatec Al2O3
Plus
5.0 9.0 8.7 9.0 10.0
except for abrasion with 250-mm Al2O3
particles, the mean flexural strength
values increased with increasing particle
size. Besides the particle size, Zhang
et al24 reported that its hardness and
shape may also influence the degree of
damage of the zirconia surface from
airborne-particle abrasion and that the
silica particles are softer and rounder
than the alumina particles. Therefore,
in the present study, a statistical
difference should have been found
between the groups abraded with
120-mm Al2O3 particles and with
Rocatec Plus, which have similar parti-
cle sizes. However, in this study, the size
of the particles outweighed the hard-
ness and the shape in determining the
flexural strength, and the behavior of
the zirconia with regard to flexural
strength was similar between hard and
soft airborne-particle abrasion.
Regarding the phase transformation,
the percentages of the monoclinic phase
found by Guess et al,3 Karakoca and
Yilmaz,8 and Guazzato et al11 are
corroborated by the results of this study.
For the IPS e.max ZirCAD zirconia, Guess
et al3 observed 0.0% for the as-sintered
group and 6.0% for the airborne-particle
abraded (50-mm Al2O3 particles) group.
Karakoca and Yilmaz8 reported 0.0%
for the Cercon zirconia as-sintered
and 9.4% for that abraded with
513
Rocatec Pre (110-mm Al2O3 particles).
Guazzato et al11 obtained 9.5% when
the DC-Zirkon zirconia was abraded
with Al2O3 particles of the same size as
those of Rocatec Plus, which, however,
were not silica modified.
In the present study, although the
monoclinic phase data were not statis-
tically analyzed, the percentage increase
seemed to have followed the size
enlargement of the particles used for
the airborne-particle abrasion. This
behavior also was observed by Curtis
et al,13 when the effect of 25-, 50-, and
110-mm Al2O3 particles was evaluated.
An interesting result of this study was
that 250-mm Al2O3 particles provided a
percentage of the monoclinic phase
content (10%) close to that found in
the groups abraded with 110-mm and/
or 120-mm particles (8.7% to 9%). This
behavior may indicate that, in the latter
groups, the compressive forces that
result from the phase transformation
were capable of preventing the propa-
gation of small flaws and cracks, which
did not occur in the group abraded
with 250-mm Al2O3 particles, probably
because the abrasion with these parti-
cles is more aggressive than those
performed with other particle sizes.
Although the aim of this study was
not to evaluate the existence of a possible
correlation between phase trans-
formation (tetragonal to monoclinic)
and flexural strength, in general, the in-
crease in the flexural strength seems to
have followed the increase in the mono-
clinic phase content. Guazzato et al11
observed that the increase in strength of
zirconia seems to result mainly from the
phase transformation and that a higher
flexural strength is related to a greater
amount of monoclinic phase content on
the zirconia surface. Sato et al15 also
noted that the increase in monoclinic
phase content was accompanied by an
increase in biaxial flexural strength.
However, some studies are not in agree-
ment with this statement.8,23 Borchers
et al23 found that submitting a Y-TZP
ceramic to different hydrothermal envi-
ronments and loading conditions
resulted in different percentages of
phase transformation (tetragonal to
514
monoclinic) but produced statistically
similar biaxial flexural strength values;
these investigators suggested that the
transformation zone did not reach deeply
enough into the material to affect its bulk
strength. This result could indicate
that the phase transformation is not al-
ways accompanied by an increase in
strength. Also, in the study of Karakoca
and Yilmaz,8 despite the statistical
strength similarity between the control
and airborne-particle-abraded groups, a
higher percentage of monoclinic phase
was found on the abraded zirconia
surface.
As commented by Wang et al,7
although airborne-particle abrasion
with some particle sizes had a beneficial
effect on the flexural strength of zirconia,
it could have a detrimental effect on the
fatigue life of this material because of
the in-depth growth of small flaws that
result from cyclic loading during masti-
cation. Moreover, factors such as tem-
perature changes and moisture, which
were not evaluated in the present study,
can also influence the behavior of zir-
conia regarding the different surface
treatments. Therefore, future studies are
needed to investigate how the groups of
this study behave when these factors are
included. Studies that investigate the
effect of the particle size used for
airborne-particle abrasion on other
properties of Y-TZP ceramics, such as
surface roughness, hardness, and frac-
ture toughness are also necessary to
confirm the efficacy of some particle
sizes over others.
CONCLUSIONS
Within the limitations of this in vitro
study, the following conclusions were
drawn:
1. The smaller silica particles (Cojet
Sand) and the largest alumina ones
(250 mm) did not affect or decreased
flexural strength, whereas the other parti-
cles studied increased this mechanical
property.
The Journal of Prosthetic Dentistry
2. Airborne-particle abrasion pro-
moted phase transformation (tetragonal
to monoclinic) and the percentage in-
crease of the monoclinic phase seems to
have followed the enlargement of the
particles.
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Corresponding author:
Dr Renata Garcia Fonseca
Departamento de Materiais Odontológicos
e Prótese
Faculdade de Odontologia de
Araraquara - UNESP
Rua Humaitá, n. 1680 - Araraquara
São Paulo 14801-903
BRAZIL
E-mail: renata@foar.unesp.br
Copyright ª 2013 by the Editorial Council for
The Journal of Prosthetic Dentistry.
Garcia Fonseca et al