Does Rinsing Following Particle Deposition Methods

Have a Negative Effect on Adhesion to Titanium?

Mutlu Özcana / Gurel Pekkanb / Ashkan Khanc

Purpose: This study evaluated whether air blasting or rinsing particle remnants with water would impair adhesion
of resin composite to metal.
Materials and Methods: Commercially pure titanium plates (1 mm x 25 mm x 50 mm) were wet polished down
to 1200-grit silicone carbide abrasive and ultrasonically cleaned. They were then embedded in auto-polymerizing
acrylic with the bonding surfaces exposed. Specimens were randomly assigned to one of the following particle
deposition protocols (N = 60, n = 10 per group): group 1: particle deposition with aluminum trioxide (50 μm
Al2O3) (AL) + air blasting + silane (ESPE-Sil); group 2: particle deposition with 30 μm SiO2 (CoJet) (CSC) + air
blasting + silane; group 3: particle deposition with Rocatec Pre 110 μm Al2O3+Rocatec Plus 110 μm SiO2 (LSC)
+ air blasting + silane. In groups 4 (AL-W), 5 (CSC-W) and 6 (LSC-W), the same protocols were used, but instead
of air blasting only, particle-deposited specimen surfaces were rinsed with water and air blasted. Adhesive resin
(VisioBond) was applied and resin composite (Quadrant Posterior, Cavex) was bonded using polyethylene molds
and photopolymerized. The specimens were then submitted to thermocycling (6000 cycles, 5°C–55ºC, dwell
time: 30 s, transfer time: 5 s). Pre-test failures during thermocycling were assigned a value of 0 MPa. Failure
modes were identified using an optical microscope. SEM images of particles were obtained. Bond strength data
(MPa) were statistically analyzed using two-way ANOVA and Tukey’s post-hoc tests (_= 0.05).
Results: Particle type significantly affected the bond results (p < 0.001). AL groups presented significantly lower
results (air blasting: 4.3 ± 3.3, rinsing: 11.8 ± 6.5) compared to those of CSC (air blasting: 27.7 ± 6.6, rins-
ing: 30.4 ± 9.3) and LSC (air blasting: 31.4 ± 8.7, rinsing: 28.7 ± 7.0). AL groups presented 5 spontaneous
debondings during thermocycling in the air-blasted group. Rinsing with water as opposed to air blasting only did
not decrease the results with any of the particle types (p > 0.05). While AL groups showed exclusively adhesive
failure between the resin composite and the substrate, the incidence of cohesive failures in the composite was
more frequent in groups CSC and LSC after either air blasting or rinsing. SEM images of particles showed sharp
morphology of the particles in AL compared to CSC and LSC.
Conclusion: Rinsing and air blasting following particle deposition methods did not impair adhesion of resin com-
posite to titanium. Particle deposition with silica particles provided better adhesion of resin composite to this
substrate compared to the use of alumina particles.
Key words: adhesion, air abrasion, bond strength, composite resin, particle deposition, repair, silane coupling
agent, surface conditioning, titanium.

J Adhes Dent 2013; 15: 307–310. Submitted for publication: 29.12.12; accepted for publication: 09.05.13
doi: 10.3290/j.jad.a30163

a Professor, University of Zurich, Dental Materials Unit, Center for Dental and
Oral Medicine, Clinic for Fixed and Removable Prosthodontics and Dental
Materials Science, Zurich, Switzerland. Designed the study, analyzed the
data, wrote the manuscript, discussed the results and commented on the
manuscript at all stages.
b Associate Professor, Department of Prosthodontics, Faculty of Dentistry,
Dumlupinar University, Kutahya, Turkey. Analyzed the data, performed the
experiments while guest researcher in Groningen, discussed the results and
commented on the manuscript at all stages.
c Dental Student, University Medical Center Groningen, Department of Dentistry
and Oral Hygiene, Groningen, The Netherlands. Performed the experiments,
discussed the results and commented on the manuscript at all stages.
Correspondence: Professor Mutlu Özcan, University of Zürich, Dental Ma-
terials Unit, Center for Dental and Oral Medicine, Clinic for Fixed and Re-
movable Prosthodontics and Dental Materials Science, Plattenstrasse 11,
CH-8032, Zürich, Switzerland. Tel: +41-44-63 45600, Fax: +41-44-63 44305.
e-mail: mutluozcan@hotmail.com
P article deposition protocols using abrasives of differ-
ent sizes increases the surface area and contributes
to micromechanical retention of resin-based materials to
metals during repair of metal-ceramic fixed dental pros-
theses (FDP),6 cementation of metal posts,12 frame-
works,8,11,13 or veneering indirect composites to metal
frameworks. 4 Particle deposition methods increase
wetting properties of adhesion promoters and improve
interfacial bonding between the resin-based materials
and the substrate.5 Today, it is possible to activate the
surface energy and increase the surface roughness of
metals using either alumina or silica-coated alumina
particles.10 Particle deposition methods applied under
propelled compressed air removes unfavorable oxides
and contaminants, thereby cleaning the surface. One

Vol 15, No 4, 2013 307

Özcan et al
rationale for the use of abrasive particles is to form co-
valent bonds between the resin and the hydroxyl groups
on the metal.3 The particle-deposited surfaces are then
coated with silane coupling agents for improved adhe-
sion of the resin-based materials.2,7 Silane coupling
agents improve wettability and promote covalent bonds,
thus enhancing the chemical adhesion between the
metals and resin composite.9 After particle deposition
on a given substrate, part of the particles penetrate the
surface due to the impact and some particles bounce
back from the surface.10 The loose particles create
undesirable debris in the mouth and may also impair
wettability of the silane and the successive adhesive
resin depending on the size of the abrasive. Thus, the
loose particles are typically air blasted, but this proced-
ure does not completely eliminate the particles from the
working environment. This is an important aspect as
the minimum space required at the bonding interface is
crucial to avoid clinical debonding failures and microle-
akage.5 Clinically, there are concerns whether removal
of particle remnants with water followed by air blasting
would impair adhesion compared to air blasting only.
The objectives of this study therefore were a) to evalu-
ate the effect of air blasting alone vs rinsing and then air
blasting of abrasives after particle deposition methods on
the adhesion of resin composite to metal and b) to identify
the failure modes after debonding. The null hypothesis
tested was air blasting alone or rinsing and air blasting
of abrasives after particle deposition methods would not
show significant differences in adhesion of resin compos-
ite to metal.
MATERIALS AND METHODS
Commercially pure titanium plates (Permascand; Ljung-
averk, Sweden) (1 mm × 25 mm × 50 mm) were wet
polished to 1200-grit silicone carbide abrasive (SiC)
(Struers; Willich, Germany) and ultrasonically cleaned
(Vitasonic II, Vita Zahnfabrik; Bad Säckingen, Germany)
in distilled water for 5 min and allowed to dry at room
temperature for 5 min. They were then embedded in auto-
polymerizing acrylic (Autoplast, Condular; Wangen, Swit-
zerland) with the bonding surfaces exposed. Specimens
were randomly assigned to one of the following particle
deposition protocols (Nplates = 15, Nspecimens = 60, n = 10
per group):
y Group 1 (AL): The specimens were particle deposited
with 50 μm Al2O3 (Korox, Bego; Bremen, Germany)
using an intraoral air-abrasion device (Dento-Prep,
RØNVIG; Daugaard, Denmark) perpendicular to the
surface from a distance of approximately 10 mm for
20 s/cm2 in circling motions at 2.8 bar.
y Group 2 (CSC): In this group, instead of ordinary
alumina particles, 30-μm alumina particles coated
with silica (SiO2) were used (CoJet Sand, 3M ESPE;
Seefeld, Germany). The particle deposition protocol
was as described in group 1.
y Group 3 (LSC): In this group, 110-μm Al2O3 (Rocatec
Pre, 3M ESPE) followed by 110-μm SiO 2 (Rocatec
308
Plus, 3M ESPE) was used (Rocatec System, 3M
ESPE). Deposition parameters were as described in
group 1.
y After particle deposition in groups 1 to 3, the rem-
nants of the abrasive particles were gently air blasted
for 20 s.
y In groups 4 (AL-W), 5 (CSC-W), and 6 (LSC-W), the
same protocols were performed, but instead of air
blasting, particle-deposited specimen surfaces were
rinsed with water using a multifunctional tip for 20 s
and air blasted for 20 s.
All specimens received one coat of silane coupling
agent (ESPE-Sil, 3M ESPE) which was left to react for
5 min. Subsequently, one coat of adhesive resin (Vi-
sioBond, 3M ESPE) was applied with a microbrush, air
thinned and photopolymerized (650 mW/cm2) for 40 s
using a photopolymerization device (Astralis 5, Ivoclar
Vivadent; Schaan, Liechtenstein). Resin composite
(Quadrant Posterior, Cavex Holland BV; Haarlem, The
Netherlands) was then placed and bonded incrementally
using polyethylene molds (height: 3 mm) and photopoly-
merized from the top for 40 s. The specimens were then
submitted to thermocycling (6000 cycles, 5°C–55ºC,
dwell time: 30 s, transfer time: 5 s). Pre-test failures
during thermocycling were assigned a value of 0 MPa.
Specimens were mounted in the jig of the universal
testing machine (Zwick ROELL Z2.5 MA 18-1-3/7; Ulm,
Germany) and shear force (crosshead speed: 1 mm/min)
was applied to the bonded interface until failure occurred.
Failure modes were identified using an optical microscope
(Stemi 2000-C, Carl Zeiss; Göttingen, Germany) at 100X
magnification. SEM (JSM-5500, JEOL; Tokyo, Japan) im-
ages of abrasive particles were obtained.
Failure types were categorized according to the modi-
fied Adhesive Remnant Index (ARI):1 score 0 = no com-
posite left on the surface, score 1 = < 1/2 of the surface
covered with composite, score 2 = >1/2 of the surface
covered with composite, score 3 = surface completely
covered with composite.
Bond strength data (MPa) were analyzed statistically us-
ing two-way ANOVA and Tukey’s post-hoc tests _ = 0.05).
RESULTS
Particle type significantly affected the bond strength
results (p < 0.001). AL groups presented signifi-
cantly lower results (air blasting: 4.3 ± 3.3, rinsing:
11.8 ± 6.5) compared to those of CSC (air blasting:
27.7 ± 6.6, rinsing: 30.4 ± 9.3) and LSC (air blasting:
31.4 ± 8.7, rinsing: 28.7 ± 7.0). AL groups presented 5
spontaneous debondings during thermocycling in the air-
blasted group (Fig 1).
Rinsing with water did not decrease the results with
any of the particle types as opposed to air blasting only
(p > 0.05).
While AL groups showed exclusively adhesive failures
between the resin composite and titanium, the incidence
of cohesive failures in the composite was more frequent
The Journal of Adhesive Dentistry
 Özcan et al

in groups CSC and LSC after either air drying or rinsing,

respectively (Table 1). Shear Bond Strength (MPa)
SEM images of particles showed sharp morphology of 45
the particles in AL compared to CSC and LSC (Fig 2). 40

35

DISCUSSION 30

25
Since rinsing with water and air blasting after particle 30.4
20
deposition with all particle types did not have an ad- 31.4
27.7
verse effect on the bond results, the null hypothesis 15
28.4
could be accepted. Yet bond strengths with the alumina 10
particles (AL) were significantly lower than with alumina 11.8
5
particles coated with silica (CoJet-CSC and Rocatec Sys- 4.3
tems-LSC), indicating that particle morphology affects 0
the adhesion to metal. Al CSC LSC
Although ordinary alumina particles and CoJet particles Dry
present similar particle sizes, the higher bond strengths Rinse
with the latter imply a greater importance of the chem-
ical aspect of adhesion than the micromechanical char- Fig 1 Means and standard deviations of the bond strength
acteristics. Principally, silane (oligomers) monomers (MPa) of resin composite to titanium after air-particle abrasion
or molecules, being chemically bifunctional, react with protocols where the particles were only air dried (Dry) or rinsed
each other forming siloxane bonds, -Si-O-Si-. With an and dried after deposition (Rinse).

Table 1 Distribution of the frequencies of failure types according to modified Adhesive Remnant Index (ARI) for
experimental groups (n = 10 per group)

Groups Score 0 Score 1 Score 2 Score 3 Dislodged*

AL 10/10 0/10 0/10 0/10 5/10

AL-W 10/10 0/10 0/10 0/10 0/10

CSC 0/10 4/10 4/10 2/10 0/10

CSC-W 0/10 2/10 6/10 2/10 0/10

LSC 0/10 1/10 5/10 4/10 0/10

LSC-W 0/10 1/10 5/10 4/10 0/10

Score 0 = no composite left on the surface, score 1 = <1/2 of the surface covered with composite, score 2 = >1/2 of the surface covered with composite,
score 3 = surface completely covered with composite. *Dislodged during thermocycling.

a b c

Figs 2a to 2c Typical SEM images of a) Al2O3 (10,000X), b) CoJet Sand (10,000X) and c) Rocatec Plus (3500X) particles. Note
the rough surface of individual Al2O3 particles compared to silica-coated Al2O3 particles in b and c. Morphology of individual particles
shows great variation.

Vol 15, No 4, 2013 309

Özcan et al
inorganic substrate (resin matrix) (ie, silica, metal ox-
ides that contain basic hydroxyl OH groups), they can
form -Si-O-M- bonds (M = metal).3 Hydrolytic degrada-
tion of -Al-O-Si- compared to -Si-O-Si- has been previ-
ously reported.7 Thus, the higher incidence of pre-test
failures during thermocycling in the alumina deposited
group can be explained based on this phenomenon.
Similarly, even though the particle size was much higher
in Rocatec (110 μm) as opposed to CoJet (30 μm), the
non-significant difference in all conditions between these
two systems cancels out the significance of microme-
chanical retention when better wettability of the silane is
achieved on less rough surfaces. Future studies should
look at the wettability aspect of silanes and their hydro-
lytic stability on different rough topographies. Also, the
necessary amount of Si vs Al needs to be established, as
the surfaces are not completely coated with Si in silica-
coating systems.10 Hydrolyzed alkoxy groups, ie, they
have reacted with water, turn into silanol groups; as a
byproduct, corresponding alcohol molecules are yielded.
The silanol groups bond covalently to the hydroxyl groups
(-OH) on titanium dioxide of the titanium surface.2 The
available amount of alumina or alumina particles coated
with silica on the titanium surface even after rinsing
was sufficient to obtain durable adhesion of the resin
composite tested. The embedded Si and Al particles on
the substrate surface, after deposition under the applied
parameters, do not seem to be removed by rinsing or
were sufficient to react with the silane.
The rinsing and subsequent air-blasting approach
could to be implemented after clinical particle abrasion
protocols during intraoral repair of metal-ceramic FDPs,
cementation of metal posts or veneering metal frame-
works. In this study, titanium was used as a screening
metal. Certainly, the results may change when a noble
alloy is used.
CONCLUSIONS
1. Rinsing with water after particle deposition of alumina
and alumina particles coated with silica did not im-
pair the adhesion of resin composite to titanium.
2. Both laboratory and chairside silica deposition sys-
tems delivered higher bond strength than particle
deposition with alumina, with which more hydrolytic
degradation and exclusively adhesive failures were
experienced.
310
3. The particle size of 30 or 110 μm in silica deposi-
tion systems tested did not affect the bond strength
results.
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Clinical relevance: Rinsing loose particle remnants
after particle deposition methods did not impair the
adhesion of resin composite to titanium. Chairside
or laboratory silica particle deposition should be
preferred to alumina particles for conditioning this
substrate.
The Journal of Adhesive Dentistry