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New Acid Etched Titanium Dental Implant Surface

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 SCIENTIFIC ARTICLES
Stomatologija, Baltic Dental and Maxillofacial Journal, 5:101-105, 2003

New Acid Etched Titanium Dental Implant Surface

Gintaras Juodzbalys, Marija Sapragoniene, Ann Wennerberg

SUMMARY
The purpose of this investigation was to create an acid etched implant surface that results in a
surface similar to that gained by using sandblasting combined with acid etching and to compare it
with surfaces of commercially available screw-type implants.
Titanium grade V discs were machined in preparation for acid etching. Tests were carried out
using different acids and their combinations with variable time exposures. All etched surfaces were
scanned with electron microscope (JEOL JSM-5600, Japan) and digital images were made for
visual evaluation and description of the surfaces. The etched surfaces were evaluated for surface
morphology (combination of micro roughness and waviness) and were best attained by a combina-
tion of sulphuric and hydrochloric acids. The etched titanium discs were fixed in resin (two were cut
and polished and two – scored and fractured) and the surface profile was examined in.
The second part of the investigation used screw-shaped titanium implants. Twenty-eight screw-
shaped implants that were manufactured from commercially available titanium grade V, were se-
lected and divided into two groups: 3 implants as controls (machined surface) and 25 implants
processed using the etching methods used in the first part of the investigation. Magnifications of 27,
200 and 2000 were used to analyse the first two consecutive crests of threads, flanks and root of
threads of each implant with the treated surface. A three-dimensional optical interferometer (Micro-
Xam, Phase-Shift, USA) was used to characterize the surface roughness of both control and test
groups. Three screws were selected from each group and measured at 9 sites: 3 measurements
each on the crest, root and flank of the threads. To describe the surface roughness in numbers, the
following parameters were used: the average height deviation (Sa), the developed interfacial area
ratio (Sdr), the fastest decay autocorrelation length (Sal) and the density of summits (Sds). Surfaces
of 5 commercially available screw-type implants and the experimental ones were comparatively
analyzed. It was concluded that the new experimental etched titanium surface had features of a
roughened titanium surface with glossily micro-roughness and large waviness. In general, the ex-
perimental surface was significantly rougher than the selected commercially available implants and
similar to SLA treated surface (top Sa 2,08µm (SD 0,36); Sdr 1,34µm (SD 0,3); valley – 1,16µm (SD
0,1) and 0,68µm (SD 0,1); flank – 2,24µm (SD 0,8) and 1,27µm (SD 0,1) respectively).
Key words: commercial titanium, titanium dental implants, endosseous integration, surface
texture, acid etching.

INTRODUCTION
Brånemark et al. (1) started the new era of implantology confirmed these findings in a histological study. Many re-
when they published the findings about titanium dental im- searchers have been working during the last decade on the
plants in 1969. Since then this method still remains popular development of new surface textures in order to improve
and reliable, with only shape and surface of the titanium initial implant stability and bone healing (8, 9, 10, 11, 12, 13,
implants having changed. Excellent titanium biocompatibility 14).
assures good tissue integration (2, 3). Baier et al. (4) dis- Characteristics of titanium implant surfaces have been
cussed what features play the most significant role in early modified by additive methods (e.g. titanium plasma spray)
acceptance and immobilization of the implant in the tissue to increase the surface area and provide a more complex
bed. Texture, charge and chemistry of the surface as well as surface macro-topography. Subtractive methods (e.g. blast-
cleanliness were considered to be the most important re- ing, acid etching) have also been used to increase the sur-
quirements for the implant material (5). Predecki et al (6) ob- face area and to alter its micro-topography or texture (15).
served rapid bone growth and good mechanical adherence Buser et al. (16) analyzed the percentage of direct bone-
with an implant that had an irregular surface. Bowers et al. (7) implant contact for different surface modifications: sand-
blasted, hydroxyapatite, titanium plasma-sprayed and acid
etched. The highest percentage of bone-implant contact
was recorded with the sandblasted surface treated by acid
Gintaras Juodzbalys - D.D.S., PhD, assoc. prof., Clinic of Oral
etching (hydrochloric and sulphuric acids). Acid etching of
and Maxillofacial Surgery, Kaunas Medical University, Lithuania. titanium is of particular interest because it creates a micro-
Marija Sapragoniene – PhD, assoc.prof., Department of Analytic textured surface (fine rough surface with micro pits of 1-
and Toxicologic Chemistry, Kaunas Medical University, Lithuania. 3µm and larger pits of approximately 6-10µm) that appears
Ann Wennerberg - PhD, assoc.prof., Department of Biomaterials, to enhance early endosseous integration and stability of
Handicap Research and Department of Prosthetic Dentistry, Den- the implant (17). This may be related to a change in surface
tal Material Science, Goteborg University, Sweden. roughness and/or chemical composition (13). It has also
been shown in rabbits that implants with macro-textured
Address correspondence to Gintaras Juodzbalys: Clinic of Oral surface (significant waviness with large elements of 10-30µm
and Maxillofacial Surgery, Eiveniu 2, Kaunas, Lithuania.

Stomatologija, Baltic Dental and Maxillofacial Journal, 2003, Vol. 5., N. 3. 101
SCIENTIFIC ARTICLES G.Juodzbalys, M.Sapragoniene, A.Wennerberg

and peaks of different size) ensured better endosseous inte- Screw shaped titanium implants
gration (15). A sandblasted and acid etched surface (SLA) Thereafter we investigated the screw-shaped titanium
provides both a microroughness and waviness that seems implants. Twenty-eight screw-shaped implants with 4
to enhance bone contact with the implant surface. The tita- threads were manufactured from commercially available ti-
nium surface was first sandblasted with large particles cre- tanium grade V (3,5mm in diameter and 6mm in length). Three
ating a grossly rough surface followed by acid etching, form- of them were chosen as control (machined surface) and 25
ing a micro rough surface (18). implants were etched using the method, which was created
The purpose of this investigation was to create im- by the authors on the titanium discs. Five series of surface
plant surface using acid etching only, which would result in etching process were performed on 5 implants in each se-
a surface similar to that gained by using sandblasting com- ries. Exposition and temperature of etching process were
bined with acid etching. The experimental surface would controlled for creation of new standardized implant surface.
then be compared with surfaces of commercially available
screw-type implants. Topographical evaluation of the screw shaped titanium
implants
MATERIALAND METHODS Implants were ultrasonically cleaned prior to examina-
Acid etching procedure tion. Implants with the experimental surface were examined
Titanium grade V discs (8mm in diameter and 2mm in with electron microscope (JEOL JSM-5600, Japan) using 27,
height) were machined in preparation for acid etching. All 200 and 2000 magnification and digital images were made for
discs were etched using pure acids or in combination (Table visual evaluation according to the previously stated prin-
1). A series of etching processes were performed changing ciples. The first two consecutive crest of threads, flanks
the exposure duration and acid combination. Exposure times and roots of threads of each implant were analyzed.
were as follows: 12 hours initial exposure followed by 6 h A three-dimensional optical interferometer Micro-Xam,
increments until 72h of exposure was reached. Phase-Shift, USA was used to characterize the surface rough-
The titanium discs were etched with 4 different pure ness of both control and test group implants. The surfaces
acids or their combination at 11 different exposure times at of three implants were analyzed topographically according
+20o C, thus forming 44 experimental groups with 5 samples to the method proposed by Wennerberg (19). Three screws
in each group for a total of 220 discs. were selected from each group and each screw was mea-
Topographical evaluation of the titanium discs sured at 9 sites: 3 times on the thread crest, root and flank.
All surfaces were scanned with scanning electron mi- Each measured area was 200X200µm. Gaussian filter of
croscope (SEM) (JEOL JSM-5600, Japan) using 27, 200 and 50X50µm size was used to distinguish between roughness
2000 magnification and digital images were made for visual and form or undulations in accordance of the requirements
examination of the surfaces. of the standard (SS-ISO 11562:1996). To describe the sur-
The machined implant surfaces were first characterized face roughness in numbers, the following parameters were
using the SEM. The surfaces were oriented in the direction used: the average height deviation (Sa), the developed in-
of the machine grooves and the surface was rated on the terfacial area ratio (Sdr), the fastest decay autocorrelation
degree of etching. Surface orientation was unidirectional length (Sal) and the density of summits (Sds).
where the machining grooves were still present. When the
machining grooves could not be distinguished, the surface Statistics
was characterized as complex one. Statistical analyses were performed using the SPSS/
Another important indicator was regularity of etching. PC+ version 10.0.1 program (SPSS Inc., Chicago, Illinois,
If the surface was etched unequally and had intact areas, it USA). Standard deviations of the means were calculated.
was characterized as irregular surface. Equally etched sur-
face was characterized as regular or uniformly etched sur- RESULTS
face.
Digital photos were evaluated on the principle that Topographical evaluation of the titanium discs
darker spots represented pits and lighter ones – peaks. Pits The test titanium discs were examined visually is de-
were measured in diameter without estimating their depth. scribed as follows:
Micro pits of 1-3µm and bigger elements of approximately 6- The control group (machined surface) had regular uni-
10µm formed the microtexture of the surface. Microtexture directional grooves with some irregular shallow roughness
characterized the roughness of titanium surface while (Fig.1a);
macrotexture consisted of large elements of 10-30µm – it’s Group I (etched with HCl) had a microtexture that was
and was characterized as waviness. poor without evidence of micropits (Fig.1b);
From these results, the etching method that achieved a Group II (etched with HCl and H2SO4) yielding a rather
surface most similar to a SLA surface was selected as the rough surface but the microtexture was poor with few micro
most acceptable. The profile of the selected surface was pits and smooth waviness (Fig.1c). The length of time that
additionally evaluated visually. Prepared titanium discs were Group I and II were subjected to their respective acids did
fixed in resin. Two were cut and polished and two – scored not change the surface texture.
and fractured without polishing and a detailed examination Group III (etched with H2SO4/ HCl and H3PO4) yielded
of the surface profile was performed. Both profiles appeared an interesting surface hsowing distinct waviness without
to have significant roughness. microtexture (Fig.1d);
Group IV (etched with H2SO4 for 72h and HCl for 30h)
showed significant surface roughness with micro pits of 1-
10µm and large valleys of 20-30µm with peaks of different
sizes (Fig.1e). The waviness and roughness of the surface
Table 1. Application of different pure acids / their combination
was regular and without intact areas.
in the test groups. This acid etching method was selected for further in-
Group Acids vestigation with screw shaped titanium implants.
I HCl Evaluation of the surface profile in the cut and pol-
ished (Fig.2a) and scored and broken (Fig 2b) groups
II HCl and H 2SO 4 showed the surface to be rough with small depressions and
III H 2SO 4/HCl and H 3PO 4 prominences of 1 to 10µm in size, visible in the profile. Wide
IV H 2SO 4 and HCl trenches of 30µm could be seen (Fig. 2).

102 Stomatologija, Baltic Dental and Maxillofacial Journal, 2003, Vol. 5., N. 3.
G.Juodzbalys, M.Sapragoniene, A.Wennerberg SCIENTIFIC ARTICLES

Fig. 1. Scanning electron microscopy images

of titanium discs. (a) Disc with machined sur-
face. Regular machining grows apparent on
the surface. X2000 mag. (b) Disc with acid
etched (HCl) surface with poor microtexture
without micropits. (c) Disc with acid etched
(HCl and H 2 SO 4 ) surface. Poor microtexture
with few micropits and smooth waveness (d)
Disc with acid etched (H2SO 4/HCl and H3 PO4 )
surface. Clear expressed surface waveness with-
out microtexture. (e) Disk with acid etched
(H 2 SO 4 and HCl) surface with 1-10 µ m
micropits, large 20-30 µm valleys and differ-
ent size peaks.

Fig. 2. Scanning electron microscopy images

of titanium discs profile. (a) Cut incised-pol-
ished disc surface. (b) Cut-fractured disc sur-
face. Both surface profiles exhibited expressed
roughness.

Fig. 3. Digital images from the topographical

measurement. (a) Machined surface with clear
direction of the surface topography. (b) Acid
etched (H2SO4 and HCl) surface with the regu-
lar distribution expressed peaks and valleys.

Topographical evaluation of the screw shaped titanium over the entire surface (Fig.3b). Surface texture was charac-
implants. terized by regularly distributed on the peaks and valleys.
Digital topographical images (Fig. 3) were performed in Electron microscopy scans of the machined surface of
order to compare machined and acid etched surfaces on a control implant had grooves, which were more expressed
screw shaped titanium surfaces. The surfaces of the ma- on thread crests than at the root or flanks of the thread (Fig.
chined titanium implants were examined and shown that 4 a1). The unidirection of deep grooves and ridges remained
these implants had mainly unidirectional machining grooves from the machining process. The implant surface treated
and ridges (Fig.3a). The acid treated titanium implants with sulphuric and hydrochloric acids was found to have a
showed roughness and waviness that was evenly spread very complex surface without any intact areas. But the rough-

Table 2. Surface roughness measured with optical interferometer at different sites of thread on machined and experimental etched
thread
S a (SD) S al (SD) S ds (SD) S dr (S D)
Title
(µm) (µm) (/µm2) (%)
etched
flank 2,24 (0,81)* 5,44 (1,19) 0,06 (0,00) 127,06 (10,80)*
top 2,08 (0,36)** 7,85 (2,14) 0,07 (0,00) 134,45 (29,10)**
valley 1,16 (0,08)+ 6,37 (0,90) 0,07 (0,00) 67,78 (5,31)+
machined
flank 1,29 (0,98)* 8,01 (8,99) 0,12 (0,01) 29,75 (10,88)*
top 1,28 (0,70)** 10,12 (6,67) 0,11 (0,01) 31,76 (16,85)**
valley 0,62 (0,09)+ 6,66 (1,91) 0,09 (0,01) 20,83 (3,79) +
*,**,+p<0,04 *,**,+p<0,001
Sa - the average height deviation, Sal - the fastest decay autocorrelation length, Sds - the density of summits, Sdr - the developed interfacial area ratio,
SD - the standard deviation.

Stomatologija, Baltic Dental and Maxillofacial Journal, 2003, Vol. 5., N. 3. 103
SCIENTIFIC ARTICLES G.Juodzbalys, M.Sapragoniene, A.Wennerberg

Fig. 4. Scanning electron microscopy images of experimental titanium implants. (a) Implant with machined surface. X27 mag. Clear direction
of grooves and ridges as remnants from the machining process. (a1) Machined thread top with deep irregular grooves and ridges. X2000 mag.
(a2) A machined thread valley with less distinct ridges and grooves. X2000 mag. (a3) A machined thread flank with distinct ridges and grooves.
X2000 mag. (b) implant with acid etched surface X27 mag. Regular distribution of surface texture. (b1) Acid etched thread top with 1-10 µm
micropits and large features of approximately 30 µm and different size peaks. X2000 mag. (b2) Acid etched valley with 1-20 µm micropits and
small peaks. X2000 mag. (b3) Acid etched flank with clear expressed 1-10 µm micropits, large features of approximately 30 µm and different size
peaks. X2000 mag.

ness of the surface was more expressed at the crests and Table 3. Comparison of surface roughness measured at 5
flanks (Fig. 4 b1 and b3) than in the root areas (Fig. 4 b2). different sites on commercially produced screw-type
Measurements with an optical interferometer estab- implants and the experimental implant with optical
lished that the following parameters - height deviation of profilometry.
acid etched surface (Sa), the surface enlargement (Sdr), the
fastest decay autocorrelation length (Sal) and the density Implant
Sa (SD) Sdr (SD)
of summits (Sds), – were significantly bigger than of ma- /manufacturer
chined surfaces (Table 2). It is worth noting that common Nobel Biocare (Goteborg, Sweden)
top 0,99 (0,5) 1,29 (0,2)
roughness of surface was significant but the roots were valley 0,60 (0,3) 1,17 (0,1)
again smoother than the crests or the flanks. flank 0,65 (0,1) 1,26 (0,1)
The surfaces of 5 commercially produced screw-shaped TiO bl ast (Astra Tech AB, Molndal,Sweden)
implants (18) and the implant with the experimental surface top 1,27 (0,2) 1,32 (0,1)
were comparatively analyzed taking measurements at the valley 1,15 (0,2) 1,31 (0,1)
same sites (Table 3). Results showed that all commercially flank 0,84 (0,1) 1,25 (0,0)
available implants had the smoothest surface at the flanks, Osseotite (3i , Palm Beach Gardens, FL)
while flanks of the experimental implants were the roughest top 1,97 (1,0) 1,42 (0,2)
– Sa 2.24µm (SD 0.8). It is worth noting that the experimental valley 0,69 (0,1) 1,12 (0,0)
implant screws were generally rougher when compared to flank 0,54 (0,1) 1,13 (0,0)
other commercially available implants. However the surface SLA (Institut Straumann AG, Waldenburg, Switzerl and)
top 1,79 (0,2) 1,42 (0,1)
enlargement (Sdr) was rather similar to the implant with SLA valley 1,32 (0,1) 1,27 (0,0)
surface. flank 1,23 (0,1) 1,30 (0,1)
Bonefit (Institut Straumann AG)
DISCUSSION top 2,08 (0,1) 1,79 (0,0)
valley 2,12 (0,7) 1,91 (0,4)
Commercially available implants are available with sev- flank 2,09 (0,2) 1,88 (1,1)
eral surface texture types. This study resulted in the devel- Experimental implant
opment of a surface texture using acid etching technology. top 2,08 (0,4) 1,34 (0,3)
It has been shown that finely pitted (micro pits of 1-3µm and valley 1,16 (0,1) 0,68 (0,1)
larger elements of approximately 6-10µm in size) surfaces flank 2,24 (0,8) 1,27 (0,1)
had an early enhancement implant and bone integration (15). Sa - the average height deviation, Sdr - the developed interfacial
Studies by Wenneberg et al. (11, 19, 20, 21) demon- area ratio, SD - the standard deviation.

104 Stomatologija, Baltic Dental and Maxillofacial Journal, 2003, Vol. 5., N. 3.
G.Juodzbalys, M.Sapragoniene, A.Wennerberg SCIENTIFIC ARTICLES

strated optimal surface roughness of particles of 75µm made that this titanium surface was gained using two methods of
surface more resistant to torque and greater bone-to-metal processing – sandblasting and acid etching. Probability of
contact than small (25µm) or coarse (250µm) particles. The surface contamination and of micro-particle dissemination
optimal surface had an average height deviation of about into the surrounding tissues is extremely low (24).
1.5µm resulting in a surface enlargement of 50%. In our study we used one method – acid etching – to
Implants with macrotextured surfaces, e.g., plasma create a new titanium surface combining all the aforemen-
sprayed or hydroxyapatite coated, had more enhanced bone tioned surface texture features. The present study showed
to implant contact at late osseointegration period (15). Some that precise acid selection and the sequence of processing
authors have reported erosion of the hydroxyapatite layer played the main role in preparation of the rough titanium
(22) and peri-implant bone loss resulting in a higher failure surface. The surface was poorer if it was etched with hydro-
rate (12, 23) for implants with hydroxyapatite surface. On chloric acid and then with sulphuric one. The very similar
the other hand, Buser et al. (16) showed that implants with results were demonstrated processing implants only with
sandblasted and acid etched surfaces had higher bone to hydrochloric acid or with sulphuric/hydrochloric acids and
implant contact percentages than implants with titanium phosphoric one. Sulphuric and hydrochloric acids in se-
plasma sprayed surfaces. This confirms presumption that quence and time showed the best results. The newly cre-
significantly roughened surface itself (titanium plasma ated titanium surface according its topography was very
sprayed surface) does not stimulate early bone and implant much alike to a SLA surface. It combines the main properties
integration. The titanium surface was sandblasted at first of roughened titanium surface: glossily micro rough and
with large particles creating a significantly rough surface, large waviness. In general, the experimental surface was
which afterwards was acid etched, forming a finely rough rougher when compared to commercially available implants.
surface. This surface texture improved the initial implant Although the implant surface created using specific
stability in bone of low-density and increased the quality of acid etching methods resembles an SLA created surface,
the bone to implant interface (18). It should be emphasized further research is necessary to study the biological re-
sponse to it.

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Received: 2002 10 10
Accepted for publishing: 2003 09 27

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