RESEARCH AND EDUCATION

Effect of hydrofluoric acid concentration and etching duration

on select surface roughness parameters for zirconia
Beata Smielak, PhD, DDSa and Leszek Klimek, PhDb

An increasing number of metal ABSTRACT

ceramic restorations are being
Statement of problem. The surface of zirconia is resistant to chemical treatment. Roughening the
replaced with ceramic systems. surface of densely sintered zirconia still poses a challenge in dentistry.
The opaque metal coping re-
flects light, which produces Purpose. The purpose of the study was to examine the effects of hydrofluoric acid on the quality of
surface roughening of zirconia.
an artificial appearance of the
restoration. Metal blocks out Material and methods. One hundred cylindrical disks made from zirconia (Ceramill Zi; Amann
100% of light; thus, it does not Girrbach AG) were divided into 4 groups. Three groups (n=30) were distinguished on the basis of
pass through to the gingival hydrofluoric acid (HF) concentration: 40% HF, 9.5% HF, and 5% HF. The groups were then further
divided into 3 groups of 10 specimens, each based on etch time (1, 5, or 15 minutes). The control
tissue. Zirconia has excellent
group (n=10) consisted of specimens polished with SiC abrasive paper. The surface was examined
esthetic properties, is semi- with scanning electron microscopy, and the roughness was measured with a profilometer and
translucent, and is light in color. confocal laser scanning microscope. The mean arithmetic profile deviation (Ramean) and mean
Light transmission is approxi- maximum height of profile (Rzmean) results for the etched surfaces in relationship to the baseline
mately 48%, and the refractive surfaces were compared with the Student t test for averaged data (a=.05).
index is 2.3.1,2 Results. When etched with 40% HF concentration, the Ramean and Rzmean results were statisti-
Restorations performed with cally higher (P<.01) for the etched surfaces than for the baseline surfaces. When etched with
zirconia have excellent me- 9.5% HF concentration, the higher Ramean and Rzmean results were only statistically significant
chanical properties compared (P<.01) after 15 minutes. Etching with 5% HF concentration showed no significant differences
with other ceramic systems (P>.05).
3,4
used in dentistry. However, Conclusions. Etching with a 5% HF solution should not be recommended as a method for
the hardness of yttria- roughening zirconia surfaces. (J Prosthet Dent 2015;-:---)
stabilized zirconia (3Y-TZP)
causes problems with surface enhancement and of chemical bonds and by micromechanical inter-
makes it difficult to ensure appropriate preparation for locking.7-9
bonding between the luting cement and the prosthetic Several surface roughening and coating methods have
restoration. The homogenous, densely packed struc- been used to optimize the surface of zirconia and to
ture of zirconia crystals and the absence of a glass improve its bond strength with resin-based cements.
matrix make etching and silanization impossible. For However, they were not effective in significantly in-
this reason, bond strength is lower than for glass creasing the zirconia-resin bond strength.10 Aside from
ceramic restorations. 4,5
The minimum tensile bond mechanical retention, to date, the only effective method
strength acceptable in clinical conditions ranges be- for ensuring chemical bonding to zirconia surfaces is one
tween 10 and 13 MPa.6 A strong, durable resin-to- that requires the use of a modified bisphenol A glycidyl
ceramic bond is established through the formation methacrylate resin luting agent (Panavia 21; Kuraray).

a
Assistant Professor, Department of Dental Prosthetics, Medical University of Lodz, Poland.
b
Professor, Department of Materials Research, Institute of Materials Science and Engineering; Professor and Chairman, Department of Dental Technology, Medical
University of Lodz, Poland.

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2 Volume
Clinical Implications
Applying 5% hydrofluoric acid to zirconia restora-
tions does not ensure an acceptable degree of
surface roughness.
This agent contains the adhesive phosphate monomer
and self-etching universal resin cement (RelyX Unicem;
3M ESPE) and provides a stable bond that resists hy-
drolysis during different artificial aging procedures.7,11-13
Unfortunately, this stable bond is not sufficient to ensure
retention of adhesive zirconia restorations, thereby
resulting in debonding under function.14 In vitro aging is
used to study bond stability under controlled laboratory
conditions.6,15
The methods used to increase micromechanical
retention such as airborne-particle abrasion with Al2O3
causes insignificant surface modification but also induces
an unfavorable transformation of the material from a
tetragonal to monoclinic phase. This results in the buildup
of surface compression, subsurface tension, and residual
flaws. The disturbed phase stability increases susceptibility
to degradation, which can cause aging of the surface
with grains breaking off, formation of microcracks, and
reduced material fatigue strength.16-20 In addition, neither
airborne-particle abrasion nor grinding with abrasive
paper or diamond rotary instruments, despite being
technically simple to perform, significantly increased the
bond strength between ZrO2 and luting cements.10,21,22
Traditional silanes used in silica ceramics are not an
effective means of conditioning a polar zirconia surface,
which is characterized by hydroxyl ions bound both
chemically and mechanically to water. The absence of a
silica layer prevents both a reaction between the methoxy
silane groups and bonding with the ZrO2 surface.23
The CoJet and Rocatec systems (3M ESPE) consist of
a tribochemical silica coat, which forms as a result of
airborne-particle abrasion, where the abrasive material
contains the appropriate silica compounds in addition to
aluminum oxide. This results in the emergence of a
surface ceramic layer and micromechanical retention.
Taken together, this improves the bonding action with
the luting cement.23
One innovative surface roughening technique is se-
lective infiltration etching (SIE). SIE is based on the
principle of heat-induced infiltration, which can lead to
the rearrangement of zirconia crystals and also result in
the formation of intergrain nanoporosities, where low-
viscosity resinous materials can flow and interlock after
polymerization.24
Casucci et al25 devised an experimental method for
ZrO2 surface roughening. They used an acid with
methanol, 37% HCl, and ferric chloride at a temperature
of 100 C. This process increased the mean arithmetic
THE JOURNAL OF PROSTHETIC DENTISTRY
- Issue -
Table 1. Characteristics and origin of HF
Etching Origin
Etching with 5% HF for 1, 5, and 15 min IPS Empress Ceramic Etch;
Ivoclar Vivadent
Etching with 9.5% HF for 1, 5, and 15 min Porcelain Etch; Ultradent
Dental Products Inc
Etching with 40% HF for 1, 5, and 15 min Experimentally prepared
in laboratory
HF, hydrofluoric acid.
profile deviation (Ramean) roughness parameter. Never-
theless, there was an effect of weakness over time, which
may be due to the low concentration of silica on the
insufficiently abraded hard surface of ZrO2.14 The surface
of zirconia, which is resistant to chemical and mechanical
factors, is a suitable surface for experimental studies on
its enhancement by increasing the etching time and
concentration of HF.
MATERIAL AND METHODS
A total of 100 cylindrical specimens of 3Y-TZP (Ceramill
Zi; Amann Girrbach AG) were sintered in a furnace
(Ceramill Therm; Amann Girrbach AG) by using a uni-
versal program (8 C per minute from 200 C to 1450 C, 2
hours at a fixed temperature of 1450 C, and the correct
cooling time). The sintering process lasted approximately
10 hours. Material shrinkage amounted to approximately
21%. After sintering, the specimens had a diameter of 9
mm and height of 5 mm. Ninety of the specimens were
divided into 3 groups (n=30) on the basis of acid con-
centration and were further divided into 3 groups of 10
specimens, each based on etch time. Specimens were
etched with hydrofluoric acid (HF) in concentrations of
40%, 9.5%, and 5% for 1, 5, or 15 minutes. Table 1 shows
the characteristics of the acid and its commercial origin. A
concentration of 40% acid was prepared for experimental
purposes in a laboratory. The surface of the specimens
had been polished successively with 220, 400, 600, and
800 grit size abrasive paper with a Metasinex grinding
machine with water cooling. The specimens were then
washed in an ultrasonic cleaner (Quantrex 90 WT; L&R
Manufacturing Inc) in ethanol for 10 minutes and air
dried. A control group (n=10) consisted of specimens
polished with SiC abrasive paper.
Acid was applied to each of the 10 specimens for 1, 5,
or 15 minutes and then rinsed off with acetone in an
ultrasonic cleaner. The specimens were then neutralized
in a powder consisting of calcium carbonate and sodium
carbonate (CaCO3 and Na2CO3) for 5 minutes, rinsed
once more for 20 seconds in distilled water, and air dried.
The specimens were examined with a Hitachi S300N
scanning electronic microscope (SEM). Depending on the
type of registered signal emitted by the specimen (after
being stimulated by electron beams), 2 types of images
were registered in SE secondary electrons (surface
Smielak and Klimek
- 2015 3

Figure 1. SEM image of surface of specimen untreated at ×500 Figure 2. SEM image of surface of specimen after HF etching with 40%
magnification. HF concentrations after 15 minutes at ×500 magnification.

topography) and retrospectively in backscattered BSE

electrons (so-called material contrast).
Profilometric tests were made with a Nikon MA
200 confocal laser scanning microscope (CLSM) with
an image resolution of 512×512 pixels. The surfaces
of the specimens were scanned with an argon laser at
a wavelength of l=488 nm. Measurements were
made with a microscope at ×500 magnification. The
measured section was 275 mm in length. Three im-
ages (at 3 different sites) were obtained from each
specimen. These images were registered with EZ-C1
software. The data obtained with microscopy were
analyzed with software (Mountains Map Premium 6;
Digital Surf). A mean roughness profile was achieved
from each image, and the parameters were deter- Figure 3. CLSM image of surface of specimen after polishing (baseline
mined for Ramean and mean maximum height of surface).
profile (Rzmean). The mean value was then calculated
for each of these parameters.
presented in Figures 1, 2. The images revealed slight
Three 275×275 mm images were scanned for each
differences in the surface topography of the tested
tested specimen. Roughness profiles were determined for
specimens after etching with HF at concentrations of 5%,
each area with MMP software, that is, 512 profiles each
9.5%, and 40% each specimen had been etched for 1, 5,
in the north-south and east-west direction. Each indi-
and 15 minutes. The differences are expressed on a
vidual profile was used to establish roughness parame-
nanometric scale.
ters. To determine the final roughness parameters for the
Microscopic images obtained with CLSM are pre-
tested surfaces, the arithmetic mean was established for
sented in Figures 3, 4. Slight differences were observed in
values from all 1024 profiles for 3 scanning fields. These
the surface topography of the etched surfaces compared
results were analyzed by using the PQ Stat v1.4.2.324
with the baseline specimens. The data are expressed on a
statistical package. The Ramean and Rzmean results for the
nanometric scale.
etched surfaces in relationship to the baseline surfaces
The results of the numerical values of roughness
were compared with the Student t test for averaged data.
parameters and their standard deviations are presented
A test probability of P<.05 was regarded as significant,
in Tables 2-4. Figures 5, 6 feature the percentage
while a test probability of P<.01 was considered to be
changes in the increase in the values of roughness pa-
statistically significant.
rameters, Ramean and Rzmean, depending on the etching
time.
RESULTS
The images presented here show that the tested
Examinations performed with a SEM in an image of surfaces were poorly enhanced. An increase in acid
SE secondary electrons and dispersed BSE electrons are concentration and etching duration resulted in slightly

Smielak and Klimek THE JOURNAL OF PROSTHETIC DENTISTRY

4 Volume - Issue -

Figure 4. CLSM images of surfaces of specimens after HF etching with 5%, 9.5%, and 40% HF concentrations after 1 minute, 5 minutes, and 15 minutes
at ×500 magnification.

Table 2. Mean arithmetic roughness parameters Ramean and Rzmean for Table 3. Mean arithmetic roughness parameters Ramean and Rzmean for
baseline specimens and specimens etched with 40% HF concentration baseline specimens and specimens etched with 9.5% HF concentration
40% HF (mm) 9.5% HF (mm)
Baseline Surface Surface Treated Baseline Surface Surface Treated
Etching Etching
Time Ramean SD Rzmean SD Ramean SD Rzmean SD Time Ramean SD Rzmean SD Ramean SD Rzmean SD
1 min 0.002 0.000 0.013 0.003 0.005 0.001 0.026 0.003 1 min 0.002 0.000 0.013 0.002 0.002 0.000 0.011 0.002
5 min 0.003 0.000 0.022 0.003 0.007 0.002 0.040 0.014 5 min 0.002 0.000 0.012 0.002 0.002 0.000 0.013 0.002
15 min 0.001 0.000 0.008 0.002 0.007 0.001 0.039 0.005 15 min 0.002 0.000 0.013 0.003 0.003 0.000 0.017 0.002
Ramean, mean arithmetic profile deviation; Rzmean, mean maximum height of profile; Ramean, mean arithmetic profile deviation; Rzmean, mean maximum height of profile;
HF, hydrofluoric acid. HF, hydrofluoric acid.

greater surface enhancement, although the size, which is Table 4. Mean arithmetic roughness parameters Ramean and Rzmean for
expressed in nanometers, is most likely not sufficient to baseline specimens and surfaces etched with 5% HF concentration
ensure an effective bond between the luting cement and 5% HF (mm)

abutment teeth. Baseline Surface Surface Treated

Etching
Statistically significant differences (t=-6.71, P<.001) Time Ramean SD Rzmean SD Ramean SD Rzmean SD
1 min 0.002 0.001 0.014 0.006 0.002 0.000 0.012 0.003
were observed in the Ramean results between the baseline
5 min 0.002 0.001 0.014 0.003 0.001 0.000 0.008 0.001
surface and the surface etched with 40% HF concentra-
15 min 0.002 0.000 0.013 0.001 0.002 0.000 0.013 0.001
tion after 1 minute, with higher results observed for the
Ramean, mean arithmetic profile deviation; Rzmean, mean maximum height of profile;
etched surface. Statistically significant differences (t=- HF, hydrofluoric acid.
5.66, P<.001) were also observed in the Ramean results
between the baseline surface and the surface etched the Ramean results between the baseline surface and the
with 40% HF concentration after 5 minutes, with higher surface etched with 40% HF concentration after 15 mi-
results observed for the etched surface. Statistically sig- nutes, with higher results observed for the etched
nificant differences (t=-8.48, P<.001) were observed in surface.

THE JOURNAL OF PROSTHETIC DENTISTRY Smielak and Klimek

- 2015
900
800
HF40% HF9.5% HF5%
Percentage change in the values of Ramean
700
roughness parameter — ΔRamean (%)
600
500
400
300
200
100
0 0
0 1
Etching time (min)
Figure 5. Percentage change in roughness parameter Ramean in relation
to duration of etching.
Statistically significant differences (t=-9.69, P<.001)
were observed in the Rzmean results between the baseline
surface and the surface etched with 40% HF concentra-
tion after 1 minute, with higher results observed for
the etched surface. Statistically significant differences
(t=-3.97, P=.003) were also observed in the Rzmean results
between the baseline surface and the surface etched with
40% HF concentration after 5 minutes, with the higher
results noted for the etched surface. Statistically signifi-
cant differences (t=-18.20, P<.001) were also observed in
the Rzmean results between the baseline surface and the
surface etched with 40% HF concentration after 15 mi-
nutes, with higher results noted for the etched surface. In
summary, etching with 40% HF concentration produced
significantly higher (P<.01) Ramean and Rzmean results for
the etched surfaces in relationship to the baseline
surfaces.
No significant (t=0, P=1.000) differences were
observed in the Ramean results between the baseline
surface and the surface etched with 9.5% concentration
after 1 minute. Also, no significant (t=0, P=1.000) dif-
ferences were found in the Ramean results between the
baseline surface and the surface etched with 9.5% HF
concentration after 5 minutes. However, after 15 mi-
nutes, significant (t=-2.24, P<.038) differences were
observed in the mean Ramean results between the base-
line surface and the surface etched with 9.5% HF con-
centration, with higher results observed for the etched
surface.
Significant differences (t=-2.24, P=.038) were observed
in the Rzmean results between the baseline surface and the
surface etched with 9% HF concentration after 1 minute,
with higher results observed for the etched surface. No
significant differences (t=-1.11, P=.278) were found in the
Rzmean results between the baseline surface and the surface
etched with 9.5% HF concentration after 5 minutes. Sta-
tistically significant differences (t=-3.51, P=.003) were
observed in Rzmean results between the baseline surface
Smielak and Klimek
5
600
HF40% HF9.5% HF5%
500
Percentage change in the values of Rzmean
roughness parameter — ΔRzmean (%)
400
300
200
100
5 15 0 1 5 15
Etching time (min)
Figure 6. Percentage change in roughness parameter Rzmean in relation
to duration of etching.
and the surface etched with 9.5% HF concentration after 15
minutes, with higher results observed for the etched sur-
face. Higher Ramean and Rzmean results were observed for
the etched surfaces with 9.5% HF concentration for 15
minutes and were statistically significant (P<.01) compared
with baseline surfaces.
No significant differences (t=0, P=1.000) were
observed in the Ramean results between the baseline
surface and the surface etched with 5% HF concentration
after 1 minute. Also, no significant differences (t=-2.24,
P=.038) were found in Ramean results between the
baseline surface and the surface etched with 5% HF
concentration after 5 minutes, with higher results
observed for the baseline surface. No significant differ-
ences (t=-2.24, P=.038) in Ramean results were observed
between the baseline surface and the surface etched with
5% HF concentration after 15 minutes.
No significant differences (t=0.94, P=.363) were
observed in the Rzmean results between the baseline
surface and the surface etched with 5% HF concentration
after 1 minute. There were still no significant differences
(t=-1.58, P=.149) in Rzmean results between the baseline
surface and the surface etched with 5% HF concentration
after 5 minutes. There were no significant differences
(t=0, P=1.000) in Rzmean results between the baseline
surface and surface etched with 5% HF concentration
after 15 minutes. Taken together, no significant (P>.05)
differences were observed when the surfaces were etched
with 5% HF concentration. Figures 5, 6 show the per-
centage change in the increase in roughness parameters
Ramean and Rzmean compared with the duration of the
etching.
When etching was done with a 40% HF concentration,
the mean increase in parameters DRamean and DRzmean(t)
achieved significantly higher (P<.01) values over time.
Nevertheless, despite the increase in roughness, these
parameters still remained at the level of several to a dozen
nanometers and may have resulted in less bonding with
THE JOURNAL OF PROSTHETIC DENTISTRY
6 Volume
the luting cement. However, at HF 9.5% and HF 5%,
these changes were slight or nonexistent.
DISCUSSION
To ensure high retention, prevention of microleakage,
and increased fracture/fatigue resistance, bonding tech-
niques for zirconia-based systems must be improved.
Strong resin bonding relies on micromechanical inter-
locking and adhesive chemical bonding to the ceramic
surface and requires surface activation for chemical
adhesion. In some instances, high-strength ceramic res-
torations do not require adhesive bonding to a tooth
structure and can be placed using conventional cements,
which rely on micromechanical retention alone. How-
ever, resin bonding is desirable when the prepared tooth
structure is unusually short or tapered.23 Adhesion is
dependent on the type of luting cement used and its
bonding capacity between a suitably prepared ceramic
surface and the enamel and dentin.5,8
Many studies have focused on the problem of
selecting the appropriate cement to achieve the
optimal retention of crowns and partial fixed dental
prosthesis. Another factor of importance for strong and
long-term bonding is appropriate surface treatment.9 A
rough and irregular surface of 3Y-TZP creates micro-
retentive depressions for the bonding systems. Thus,
not only is the bonding surface greater, but the wetting
and surface energy are also greater.23 Airborne-particle
abrasion has been used in an attempt to enhance the
surface area available for bonding: although an
improvement in the average surface roughness has
been recorded on a micrometer scale, the treatment
appeared to be inadequate to establish reliable
ceramic/cement bonds.19,20
Alternative technologies are advocated to change
these high-strength ceramic cores into more retentive
substrates. SIE has recently been proposed because it
has achieved promising results in terms of bond
strength values at the zirconia-resin cement interfaces.
The use of SIE improved nanomechanical retention of
zirconia by increasing the surface area available for
bonding.24
Casucci et al25 have shown that a hot chemical
etching solution produces a surface roughness that is
significantly greater than when SIE is used. This tech-
nique could possibly enhance the mechanical retention of
ZrO2 and increase the Ramean roughness parameter of
the 3Y-TZP surface from 26 nm after 10 minutes to 103
nm after 60 minutes. In the same studies, etching with
9.5% HF also achieved a parameter value of Ramean 5 nm
after 90 seconds.
In the studies presented here, the value of the Ramean
parameter after etching with 9.5% HF was 0.002 after 60
seconds, and the same result was achieved after 5
THE JOURNAL OF PROSTHETIC DENTISTRY
- Issue -
minutes and 0.003 after 15 minutes. However, etching
with a 5% HF solution achieved Ramean parameter values
of 0.002 after 60 seconds, 0.001 after 5 minutes, and 0.002
after 15 minutes.
The majority of authors have reported that the
application of a 9.5% or 5% HF concentration to a zir-
conia surface does not cause any morphologic changes in
its structure and does not increase surface roughness and
that the roughness is less compared with conventional
ceramics.4,5,10,17 We obtained similar conclusions for our
study.
Significantly higher (P<.01) Ramean and Rzmean results
on the etched surfaces compared with the baseline sur-
faces were achieved with 40% HF concentration, and the
mean increase in parameters DRamean and DRzmean(t)
achieved statistically significant (P<.01) values over time.
The data obtained in this study were detectable on a
nanometric scale, which indicates that the quality of
surface enhancement may be insufficient to improve
bond strength with luting cements. Etching zirconia with
HF has limited effectiveness because of the dense crystal
network and the small amount of glass matrix and is
not recommended as a treatment method for this
material.5,13,21,23
CONCLUSIONS
Within the limitations of this in vitro study, the following
conclusions were drawn:
1. An increase in etching time has a positive effect on
the quality of the treated zirconia surface, although
it is also dependent on the concentration of acids
used for etching.
2. Etching with a 5% HF solution is not recommended
as a method for roughening zirconia surfaces.
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Corresponding author:
Dr Beata Smielak
The Medical University of Lodz
Pomorska 251, 92-213 Lodz
POLAND
Email: bsmielak@hotmail.com
Copyright © 2015 by the Editorial Council for The Journal of Prosthetic Dentistry.
THE JOURNAL OF PROSTHETIC DENTISTRY