Materials Research.

Study of the Influence of Acid Etching Treatments on the Superficial Characteristics of Ti

Bruno Ramos Chrcanovic*, Maximiliano Delany Martins
Laboratrio de NanoscopiaLabNano, Centro de Desenvolvimento da Tecnologia NuclearCDTN,
Comisso Nacional de Energia NuclearCNEN, Av. Presidente Antnio Carlos, 6627,
Campus da UFMG, Pampulha, CEP 31270-901, Belo Horizonte, MG, Brazil
Received: April 8, 2013; Revised: February 6, 2014

Modifications in texture and surface chemistry are commonly used to increase the biologic response
to implants. We evaluated the influence of five different acid etching treatments on the chemical and
topographical superficial characteristics of cpTi grade IV discs (test groups). One group of samples
were only polished (control group). The samples were analyzed by electron microscopy (SEM, EDS),
atomic force microscopy, and grazing incidence XRD. The acid etching treatments which produced
higher values for the amplitude roughness parameters showed a combination of strong acids (HF and
HCl/H2SO4) at high concentrations, with a relatively high temperature ( 60 C) for a considerable
time ( 60 min). Titanium and oxygen were the only elements detected by EDS on the surface in all
groups, whereas titanium hydride was detected when the samples were analyzed by GIXRD. Only the
group subjected to thermal treatment showed presence of rutile phase on the surface.
Keywords: titanium, surface modification, acid-etching, surface characterization

1. Introduction
Alterations in endosseous dental implant design have
been revisited extensively to decrease treatment time
frames by reducing the healing period for osseointegration
establishment. Thomas and Cook1 examined the variables
that potentially influence bone apposition to an implant
surface. Of twelve parameters studied, only surface
characteristics were shown to have a significant effect on
bone integration of an implant. Because the implant surface
is the first component to interact with the host, several
surface modifications have been extensively investigated
in the search for improved bone healing that would allow
immediate or early loading of dental implants2. Alterations
in surface texture and chemistry are modifications used
commonly to increase the biological response to implants.
The beneficial effect of rough implant surfaces on periimplant bone formation is considered to be based on the
changes in microtopography and subsequent alterations of
surface energy that result in increased interaction with the
adjacent biological environment by adsorption of proteins
and blood components which in turn can enhance cell
attachment and implant integration3.
Recently, commercially pure titanium (cpTi) has become
widely used as a biomaterial for dental implants, orthopaedic
implants, cardiovascular appliances, and implant-supported
dental crowns because of outstanding characteristics that
include high specific strength, high resistance to corrosion,
greater biocompatibility, low modulus of elasticity, and high
capacity to be osseointegrated with bone4. Furthermore,
the creation of roughened titanium surfaces has long
been demonstrated to be an effective way to promote the
interfacial biomechanical properties of bone-anchored
*e-mail: brunochrcanovic@hotmail.com

implants by means of increasing the interlocking capacity

of surface5. The literature shows that when micromechanical
anchorage is achieved, the bone-repair process switches
from slower bone corticalization around the implant surface
to more rapid bone trabeculization and bone ingrowth into
the rough surface6. Some biomechanical studies in animal
models found that the surface texture of titanium implants
has a significant influence on their anchorage in bone7,8.
Bone interlocking or micromechanical anchorage
at the interface is not a feature common to all surfaces;
to achieve it, a certain level of roughness seems to be
required. Some authors9 showed that machined surfaces do
not achieve micromechanical anchorage at the interface.
When torqued, bone was not found attached to the machined
surface, whereas anchorage has been documented for other
surfaces with physical and chemical surface modifications9.
The surface topography obtained by acid attack can be
modulated according to prior treatment as, for example,
by sandblasting, using acid mixtures, using different
temperatures, and using different etching times. Acid
etching is a subtractive method, wherein pits are created
in the titanium surface10. Acid etching of titanium is of
particular interest because it creates a microtextured surface
(fine rough surface with micro pits of 1-3 m and larger pits
of approximately 6-10m) that appears to enhance early
endosseous integration and stability of the implant7.
Some studies support the belief that the subtractive
surface modification by acid etching has a positive effect
on the strength of endosseous integration. Lazzaraetal.11
compared the bone response to Osseotite (an implant system
that has a machined and dual acid-etched surface-MDAS)
and machined surfaces (MS) placed in the human posterior
maxilla. After 6 months of healing, the bone contact at the

Chrcanovic & Martins

MDAS was significantly higher when compared to MS, and

the osteoconductive effect (the amount of bone apposition)
of the MDAS over the MS was particularly pronounced in
the softer trabecular bone. Klokkevoldetal.7 compared the
anchorage of MDAS and MS in the rabbit tibia model, and
observed a statistically significant higher mean removal
torque for the MDAS after 1, 2, and 3 months. Treating
titanium by HF/HNO3 or by HCl, HF, and H3PO4, Heetal.12
and Zareidoostetal.13 respectively, showed that acid-etched
titanium surfaces had higher roughness, lower cytotoxicity
level and better biocompatibility than the control samples
not submitted to acid etching.
Thus, considering the importance of this subtractive
method of surface modification, the aim of the present study
was to evaluate the influence of five different acid etching
treatments described in the literature on the chemical and
topographical superficial characteristics of cpTi grade IV.

2. Material and Methods

Eighteen machined cpTi grade IV discs (12.7 2.0 mm)
were used as the substrate material for the experiment. All
discs were cut from a rod using a IsoMet Low Speed Saw
(Buehler, Lake Bluff, USA) with a Diamond Wafering
Blade No. 11-4244 (diameter 4-102mm / thickness
0.0120.3mm) from the same manufacturer. The samples
were embedded in polymethyl methacrylate, in order to
be polished in a polishing machine until a #2000 silicon
carbide paper.
The discs were separated into a control group with
3 discs and 5 test groups with 3 discs each. Each test
group was acid-etched by a different acid treatment
(defined as groups AT1 to AT5) previously described in
the literature14-18. Table1 presents a detailed description of
these 5 acid-etching treatments. The firing in vacuum was
performed in a VITA Vacumat 40T vacuum furnace (VITA
Zahnfabrik H. Rauter GmbH & Co.KG, Bad Sckingen,
Germany).
The surface morphology of treated samples was
examined by scanning electron microscopy (SEM-JEOL,
model JSM-5310, Tokyo, Japan). The secondary electron
(SE) detection mode with an acceleration voltage of 25 kV
was selected for SEM analysis and the vacuum pressure
was maintained below 1 105 Torr. The load current (LC)
was approximately 85 A. For a direct comparison of the
surface morphology, the same magnification of 1000 was
selected for all samples.

Materials Research

In order to obtain quantitative analysis of the surface

roughness, atomic force microscopy (AFM - NTegra
Aura, NT-MDT, Moscow, Russia) of the samples was
performed. AFM images were acquired in air using
semicontact mode with a sharpened gold-coated silicon
tip (nominal spring constant of 2.5-10 N/m and nominal
resonance frequency of 110-200 kHz, NSG01 probe series,
NT-MDT, Moscow, Russia). The scanning area for the
measurements was 5050m2. The images obtained by
AFM were characterized by 2nd order extraction filter, using
the software Image Analysis 2.1.2 (NT-MDT, Moscow,
Russia). The seven amplitude surface roughness parameters
calculated by the software were evaluated (Sy, Sz, Sa, Sq, Ssk,
and Ska). The mean value and standard deviation of these
parameters was obtained from 15 satisfactory scans of each
group (5 from each of the 3 samples), from random sites
on the surface. A statistical analysis of the mean values
of the surface roughness parameters was composed and
compared with One-Way Analysis of Variance (ANOVA),
since a normal distribution of the variables was observed
by the Kolmogorov-Smirnov test. The Tukeys HSD
test was also performed, in order to find means that are
significantly different from each other. The degree of
statistical significance was considered P < 0.05. The
Statistical Package for the Social Sciences (SPSS) version
20 software (SPSS Inc., Chicago, USA) was used to perform
the statistical analysis.
The surface chemical composition was analyzed by
energy dispersive x-ray spectroscopy (EDS-JEOL, model
JXA-8900RJ, Tokyo, Japan). The most central area of the
samples was chosen, and the analysis was made with a
magnification of 200. The elemental chemical composition
was calculated by the mean value and standard deviation
from the 3 samples of each group.
Moreover, grazing incidence X-ray diffraction (GIXRD)
measurements were carried out in a Ultima IV X-ray
diffractometer (Rigaku, Tokyo, Japan), using Cu-K1
radiation at 30 kV and tube current of 20 mA, without any
filter or monochromator, in the angle range of 10 90
(2) with a grazing incidence of 3, making the diffraction
sensitive to the surface. The step of measurement was set to
0.05 with a scan rate of 0.5 per minute. The divergence slit
was set to 1 mm, with a Div H.L. Slit of 2 mm. The results
were analyzed in Search-Match software (Crystallographica,
Oxford, United Kingdom). GIXRD experiments were
carried out in order to distinguish chemical compounds at
the sample surface.

Table1. Details of the acid-etching groups.

Acid-etching
Group
AT1
AT2
AT3
AT4
AT5

Acid solution
1% HF / 30% HNO3
12% HF
70% HCl / H2SO4
70% HCl / 60% H2SO4
0.11 mol/L HF+0.09 mol/L HNO3
5.80 mol/L HCl+8.96 mol/L H2SO4
48% H2SO4

Temperature Etching
(C)
time (min)
RT
RT
80
60
RT
80
60

60
2
5
60
10
30
60

Additional treatment

Reference

dried in an oven at 50 C for 24 h

dried in an oven at 50 C for 24 h
firing in vacuum at 600 C for 10 min

Orsinietal.14
Cho and Park15
Carvalhoetal.18
Yangetal.17
Iwayaetal.16

Study of the Influence of Acid Etching Treatments on the Superficial Characteristics of Ti

3. Results
3.1. SEM analysis
Figures1a-f revealed characteristic differences at the
microscopic level according to the surface modification
methods used for the samples as measured by SEM.
Differences of the surfaces were obvious between the
groups due to differences of the etching processes.
The control group samples were mainly characterized
by multidirectional grooves as result of the polishing
process (Figure1a). Samples submitted to acid treatment
classified as AT1 showed a homogenous distribution of
irregularities throughout the surface (Figure 1b). AT2
(Figure 1c) showed the presence of ridges and valleys
with bigger dimensions as shown in AT1 samples, in
many regions resembling grooves with a width varying
from 1 to 2 m. AT3 samples showed a surface with a
great number of micro pits of 1-3 m and some larger
pits (Figure1d). AT4 showed an almost homogeneous
distribution of valleys and peaks with sharp edges
(Figure1e). Acid etching treatment AT5 did not eliminate
the multidirectional grooves (Figure1f), suggesting that
the acid treatment was not effective to change surface
morphology.

3.2. AFM analysis

The qualitative and quantitative surface topography
demonstrated different degrees of roughness. Table2 shows
the mean values of tridimensional roughness parameters for
the control group and acid-etched samples (groups AT1 to
AT5) as determined by AFM. It can be observed that the
surfaces of the samples from control group showed smaller

mean values of the amplitude roughness parameters than the

test groups. AT1 showed closest mean values of Sy, Sz, and
Average when compared to the control group, and the same
mean value of Sa and Sq as the control group. The samples
from AT2, AT3, and AT4 groups showed higher mean
values. The topographic maps obtained by AFM showed,
qualitatively, the difference in roughness between the six
surfaces: control group (Figure2a) and test groups AT1 to
AT5 (Figures2b-f, respectively).
The amplitude parameters characterize the surface based
on the vertical deviations of the roughness profile from
the mean line. The roughness parameter Ssk represents the
degree of symmetry of the surface heights about the mean
plane. The sign of Ssk indicates the predominance of peaks
(i.e. Ssk > 0) or valley structures (Ssk < 0) comprising the
surface. Thus, it can be observed that all groups but AT4
have a predominance of peaks. Sku indicates the presence
of inordinately high peaks/deep valleys (Sku > 3.00) or lack
thereof (Sku < 3.00) making up the texture. In this case,
groups AT1 and AT5 were the only ones with a presence of
inordinately high peaks/deep valleys.
Comparison of the mean values of the surface roughness
parameters with ANOVA showed that the difference of
the values between the groups revealed to be statistically
significant for all parameters. Groups AT2 and AT3 showed
statistically significant difference for the mean value of
the roughness parameters when compared to the other
groups, but not between themselves. The difference of
the mean values of the control, AT1 and AT5 groups were
also statistically significant for most of the parameters
when compared to the other study groups, but not between
themselves.

Figure1. SEM pictures of control group (a), AT1 (b), AT2 (c), AT3 (d), AT4 (e), and AT5 groups (f) (original magnification 1000xscale
bar 25 m).

Chrcanovic & Martins

Materials Research

Table2. Mean values ( SD) of tridimensional roughness parameters as determined by AFM (scanning area of 50 50 m2), and P-values
for one-way ANOVA comparisons.
Group
Control
AT1
AT2
AT3
AT4
AT5
P-value

Sy (m)

Sz (m)

Average-mean
height (m)

Sa (m)

Sq (m)

1.300.37a
1.540.41a
6.410.61b
6.830.41b
5.220.95
2.971.09
0.000

0.650.19a
0.760.20a
3.210.31b
3.420.23b
2.550.44
1.480.56
0.000

0.540.17a
0.690.24a
3.110.39b
3.250.41b
2.520.55
1.340.51
0.000

0.110.02a
0.110.02a
0.780.13b
0.850.15b
0.570.16
0.160.05a
0.000

0.140.03a
0.140.03a
0.970.16b
1.060.17b
0.730.19
0.220.08a
0.000

Ssk

Sku

0.620.62a
2.363.12a,b
0.290.82a,b,c 3.713.38b
0.150.21a,c 0.140.26a
0.160.21a,c 0.030.55a
0.160.30b,c
0.240.55a
0.450.58a
3.473.41b
0.002
0.000

Groups denoted with the same superscripted letter do not indicate statistically significant difference in surface roughness (P 0.05) between the groups,
according to the Tukeys HSD test.
a,b,c

Figure2. AFM topography maps for the control group (a), AT1 (b), AT2 (c), AT3 (d), AT4 (e), and AT5 groups (f) (scanning
area:5050m2).

Study of the Influence of Acid Etching Treatments on the Superficial Characteristics of Ti

3.3. EDS analysis

EDS analysis of the surfaces showed titanium and
oxygen to be the only elements in all groups, with a similar
average % atomic concentration of 60% and 40% ( 5%),
respectively. Figure3 shows a typical EDS spectrum of the
group AT2.

3.4. XRD analysis

Figure4 presents a typical GIXRD diffractogram for a
sample from the control group, where diffraction peaks were
labeled according to Miller indices, as described elsewhere19.
The diffractogram analysis confirmed only the presence of
titanium (Ti). The GIXRD results obtained for the samples
from groups submitted to acid etching showed the presence
of Ti and titanium hydride (TiH2) in groups AT1 to AT4
(Figures5a-d, respectively), and Ti, TiH2, and rutile (TiO2)
in group AT5 (Figure5e).

Figure3. Typical EDS spectrum of a sample from group AT2,

showing oxygen (O) and titanium (Ti).

4. Discussion
Chemical texturing is a method of surface roughening
through acid etching. This method has advantages compared
with current methods of roughening such as grit blasting,
plasma spraying, and beads. As the production process does
not stress the adjacent material, there is no risk of flaking
or delamination and the process does not leave particles
of grit20,21.
All test groups have been acid attacked; nevertheless,
due to the distinct treatment parameters, every implant
displayed distinct surface roughness characteristics and
a proper surface aspect that could not be mistaken. Seven
distinct roughness parameters have been reported for each
surface. However, their significance in terms of predicting
an enhanced bone response or an increased implant fixation
remains questionable10. Some studies have demonstrated
that increases in the numerical surface roughness of an
implant enhance biomechanical anchorage in bone, as
determined by torque removal tests8 and resistance to pushout forces22. These studies showed a tendency toward an
increase in bone contact, and resistance to removal, with
an increasing numerical implant surface roughness. In the
groups AT2, AT3, and AT4 it can be seen that the etching
created micropits, when the SEM image is compared with
the control group, which also reflected in the higher values
of the amplitude roughness parameters in these samples.
Groups AT2 and AT3 also showed statistically significant
difference for the value of the roughness parameters when
compared to the other groups. This was also true for the
group AT4 for some parameters, but not all. Specific
to dental implants, studies have shown that histologic
and biomechanical characteristics were improved due
to increase in the as-machined surface texture by varied
methods resulting in average implant surface roughness
(Sa) ranging from 0.5 to 2 m23,24. Thus, the values found
in the present study for the roughness parameter Sa seems
to be appropriate in these groups. Although biological tests
were not conducted in the present study, it can be suggested
that these surfaces with the highest values of roughness
parameters (AT2, AT3 and AT4) could also present a
greater osseous anchorage, if implants had been treated

Figure4. Typical GIXRD diffractogram for the control group

sample, showing peak identification (Miller indices). See text for
details.

with these acid etchings, and if could only consider the

surface topographic characteristics, based on results found
in the literature. Several studies reported a good correlation
between increased Ra (bi-dimensional correlate of the threedimensional Sa) and stronger anchorage7,9,22, although the
Ra is obviously insufficient by its own to characterize a
given surface25. Wongetal.22 evaluated pushed-out titanium
cylinders placed in the knee trabecular bone of mini-pigs
after 3 months, comparing four surfaces. The surface with
the highest Ra showed the highest anchorage; a strong linear
correlation, r2=0.90, was found between the Ra and the
push-out load. Gotfredsenetal.9 measured the anchorage
of four treated surfaces in a rabbit tibia model after 4, 6,
9, and 12 weeks with the torque test. The highest torque
values were observed at each time point for the roughest
surface, as determined by the Ra and Rt. At all time points,
these authors reported a high correlation of r=0.83 between
the Ra and implant anchorage. Klokkevoldetal.7 compared
the torque resistance to removal of screw-shaped titanium
implants having a MDAS with implants having either a
MS, or a titanium plasma spray surface (TPS), in a rabbit
model. Their results showed an enhanced bony anchorage to
MDAS implants as compared to MS implants (also showing
a much higher value of Ra for the MDAS implants), and

Chrcanovic & Martins

Materials Research

Figure5. Typical GIXRD diffractograms of samples from groups AT1 to AT5. Peak identification according to crystal structures: Ti(circle),
TiH2 (diamond), rutile (X).

that dual acid etching of titanium enhances early endosseous

integration to a level which is comparable to that achieved by
the topographically more complex TPS surfaces. However,
although the height-descriptive parameters of the surfaces
of the groups AT2, AT3, and AT4 were significantly higher
than the AT1 and AT5 surfaces, one cannot speculate on their
biological performance until their bone interlocking capacity
is demonstrated. It turns out that clinical implications cannot
be drawn by relying on roughness-descriptive parameters
alone10.
It has been reported that the etching process modifies
the Ti surface composition of SLA-treated implants, and

XRD and metallographic microscopy analysis indicated the

presence of 20 to 40% of titanium hydride (TiHx, x 2)
in addition to Ti[26]. Before attacking the metallic titanium,
the acids must first dissolve the protective titanium oxide
layer. During the course of the corrosion process of titanium,
native hydrogen ions (H+) are released. These small ions
diffuse rapidly into the metal because the latter is left without
its dense protective oxide layer; the sub-surface is therefore
enriched with hydrogen27. When saturation in hydrogen
is reached, titanium hydride is formed. Titanium hydride
may be biologically important because a hydride layer is
much better suited as a template for binding biomolecules

Study of the Influence of Acid Etching Treatments on the Superficial Characteristics of Ti

chemically onto a titanium surface28. In the present study,

as the surface of the samples were also modified by acid
etching, it was not surprising that titanium hydride was
found in all test groups (from AT1 to AT5) by GIXRD
analysis.
EDS analysis of the surfaces showed titanium and
oxygen to be the only elements in all groups, most probably
due to the natural formation of a titanium oxide passivation
layer (mainly TiO2) just after sample surface preparation.
The result (about 60%/40%) agrees with the mass percentage
of the TiO2, the main component of a typical titanium
oxide passivation layer. It was previously observed, by
using XPS analysis, that dental implants surfaces treated
only by sandblasting and acid-etching consists of oxidized
titanium29. Moreover, TiO2 can exist in three crystalline
forms called anatase, rutile, and brookite, all with different
physical properties. The quasi-amorphous oxides can be
crystallized by heating to temperatures of 400-500 C or
higher, which leads to transformation to more crystallized
phases30. Thus, the presence of rutile phase in group AT5
can be explained by the thermal treatment by which the
samples of this group were subjected (firing in vacuum at
600 C for 10 min).
The results showed that the acid etching treatments used
here produced a surface with different topographical and
chemical features compared to the polished one (control),
except for AT5. The present results demonstrated that
the acid etching can remove the grooves produced by the
polishing process. The etching can create a surface with
randomly distributed pits in a micron-scale (as seen with
AT3 Figure 1d), or homogeneously create ridges and
valleys throughout the surface (as seen with AT1, AT2, and
AT4), enlarging the surface area. Although the ultimate aim
of acid attack is to create pits to allow for bone ingrowth,
etching varies from weak to strong. The AT1 produced very
small pits. AT5 did not change the surface morphology when
compared with the control group. The surface aspect is
probably caused by the use of either a weak acid mixture, a
low etching temperature, or a short etching time10. In the case
of AT1, the room temperature might have been the cause,
whereas in the case of AT5, the cause was probably a weak
acid solution. The formation of great number of micropits
in the group AT3 probably resulted from a combination of
strong acids (HCl/H2SO4) at high concentrations, a relatively
high temperature (60 C), for a considerable time (60 min).
The result of an irregular surface with higher values of
roughness parameters in groups AT2 and AT4 may be the
consequence of a combination of 2 etching steps with strong

acids at high concentrations, and with high temperature

(80C) in at least one step of the etching bath.
This same research team conducted in 2013 a study
comparing the effect of the same five acid etching
treatment here described (Table 1) on the superficial
characteristics of cpTi grade IV, but after sandblasting the
samples with aluminum oxide21. Comparing the present
roughness parameters results with the ones obtained by
Chrcanovicetal.21, it can be observed that the values did
not significantly differ in groups AT2, AT3, and AT4. When
this is taken into account it can be suggested that for these
acid etching groups, at least when considering the amplitude
roughness parameters, there is no need to perform the
sandblasting procedure before the acid treatment in order to
increase the roughness of the surface; only the acid etching
treatment could be enough.
Although some of the surfaces here created using
specific acid etching methods resemble chemically and
topographically surfaces with osseointegration potential
described in the literature, further research is necessary
to clear up the influence of acid etching methods on the
biological response.

Eduardo Antnio de Carvalho (CDTN/CNEN) and Rolf

Ankli (Dental Atelier Rolf Ankli Art & Experience).

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5. Conclusions
Treating titanium surfaces with acid does not create
a standard topography. The latter varies according to
several parameters, such as prior treatment, acid mixture
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acid etching treatments here classified as AT2, AT3, and
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Acknowledgements
This work was supported by the Brazilian agencies
CNPq and FAPEMIG. The authors would like to thank

Chrcanovic & Martins

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