Repair Bond Strength of a CAD/CAM Nanoceramic Resin

and Direct Composite Resin: Effect of Aging and Surface

Conditioning Methods
Dayanne Monielle Duarte Mouraa / Amanda Maria de Oliveira Dal Pivab / Ana Beatriz do
Nascimento Januárioc / Aretha Heitor Verissímod / Marco Antonio Bottinoe / Mutlu Özcanf /
Rodrigo Othávio Assunção Souzag

Purpose: To evaluate the effect of surface conditioning methods and aging on the repair bond strength between
resin composite and nanoceramic CAD/CAM resin.
Materials and Methods: Twenty-four blocks of nanoceramic CAD/CAM resin (NCR) (Lava Ultimate, 3M Oral Care)
(10 x 5 x 2 mm3) and resin composite (Filtek Z350, 3M Oral Care) (RC) were made, embedded in acrylic resin, polished
(#600, #800, #1200) and randomly divided into 8 groups (n = 12 each) according to surface conditioning methods
(air abrasion with 30-μm CoJet [CJ] or air abrasion with 50-μm Al2O3 [AB]) and aging prior to repair (without aging,
24 h in water at 37°C; with aging 6 months in water at 37°C). The blocks were air abraded (20 s, 2.5 bar, 10 mm)
using a standardized device. A layer of adhesive resin (Scotchbond Universal) was applied (20 s) and photopoly- y
merized for 20 s. RC cylinders (Ø = 2 mm; h = 2 mm) were then bonded to the NCR substrates using a Teflon ma-
trix and photopolymerized for 40 s. All specimens were thermocycled (10,000 cycles, 5°C-55°C) and submitted to
the shear bond test (50 kgf, 0.5 mm/min) to measure repair strength. Data (MPa) were analyzed using 3-way
ANOVA and Tukey’s test (α = 0.05). Failure analysis was performed using stereomicroscopy (20X).
Results: ANOVA revealed a significant effect of only the “material” factor (p = 0.00). The group NCR6mCJ pre-
sented bond strengths (29.37 ± 5.41) which were significantly higher than those of the NCR24hCJ (20.88 ± 5.74)
and RC groups (p < 0.05). The group RC24hCJ (19.71 ± 4.21) presented the lowest shear bond strength
(p < 0.05). Failure analysis revealed predominantly type B mixed failures (adhesive+cohesive in the substrate ma-
terial) except for the groups NCR24hCJ and NCR6mAB, where mainly type C failure (adhesive+cohesive at the RC)
was observed.
Conclusion: Air abrasion with Al2O3 particles or silicatization with CoJet followed by adhesive resin application are
effective surface conditioning methods for the repair of nanoceramic CAD/CAM resin with resin composite.
Key words: adhesion, nanoceramic resin, repair, resin composite, shear bond strength, surface conditioning.

J Adhes Dent 2020; 22: 275–283. Submitted for publication: 28.06.18; accepted for publication: 28.11.19
doi: 10.3290/j.jad.a44551

a PhD Student, Federal University of Rio Grande do Norte (UFRN), Department f Professor, University of Zurich, Center for Dental and Oral Medicine, Dental
of Dentistry, Natal, RN, Brazil. Hypothesis, performed the experiments, wrote Materials Unit, Clinic for Fixed and Removable Prosthodontics and Dental Ma-
the manuscript. terials Science, Zurich, Switzerland. Idea, consulting, evaluated the results,
b proofread the manuscript.
MSc Student, São Paulo State University (UNESP), São Paulo, Brazil. Per-
r
formed and interpretated of qualitative analyses, wrote manuscript. g Professor, Federal University of Rio Grande do Norte (UFRN), Department of
c Dentistry, Natal, RN, Brazil. Idea, consulting, evaluated the results, proofread
Dentist inPrivate Practice, Natal, RN, Brazil. Hypothesis, performed the experi-i
the manuscript.
ments, wrote the manuscript.
d MSc Student, Federal University of Rio Grande do Norte (UFRN), Department
of Dentistry, Natal, RN, Brazil. Hypothesis, performed the experiments, wrote
the manuscript.
Correspondence: Adjunct Professor Rodrigo O. A. Souza, Department of Den-
e Professor and Chair, São Paulo State University (UNESP), Institute of Science tistry, Federal University of Rio Grande do Norte (UFRN), Av. Salgado Filho,
and Technology, São José dos Campos, Brazil. Idea, consulting, evaluated the 1787, Lagoa Nova, Natal, RN, Brazil 59056-000. Tel: +55-84-3215-4104;
results, proofread the manuscript. e-mail: rodrigoothavio@gmail.com

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I n addition to the current ceramic materials such as feld-

spathic, crystal-reinforced, and zirconia ceramics,6 new
resin-based materials such as nanoceramic resins (NCR)
MATERIALS AND METHODS
The brands, material types, chemical compositions, batch
have been developed for use in CAD/CAM technologies.28 numbers, and manufacturers of the materials used in this
Lava Ultimate (3M Oral Care; St Paul, MN, USA), for ex- study are listed in Table 1.
ample, is an NCR with a chemical composition similar to The experimental groups formed were: NCR24hCJ: NCR
a conventional resin composite: 20% resin matrix re- aged for 24 h and treated with CoJet; NCR6mCJ: NCR aged
inforced with 80% silica particles 20 nm in diameter and for 6 months and treated with CoJet; NCR6mAB: NCR aged
particle size similar to zirconia, 4-11 nm in diameter.2,10 for 6 months and air abraded with Al2O3; RC24hCJ: resin
As it is prepolymerized under high pressure and tempera- composite aged for 24 h and treated with CoJet; RC24hAB:
ture during manufacturing, NCRs have better physicome- RC aged for 24 h and air abraded with Al2O3; RC6mCJ: RC
chanical properties, and present less discoloration38 and aged for 6 months and treated with CoJet; RC6mAB: RC
higher resistance to abrasion37 compared with conven- aged for 6 months and air abraded with Al2O3 (Table 2).
tional resin composites (RC). NCRs also have relatively
high flexural strength combined with a low flexural modu- Specimen Preparation
lus,2 resulting in a more flexible, less brittle material,32 Figure 1 presents the flowchart of the study design. Eight
with increased ability to withstand loads when compared blocks (12 x 5 x10 mm3) of CAD/CAM nanoceramic resin
to dental ceramics. (NCR, Lava Ultimate, 3M Oral Care) were sectioned with
The improved properties of such new resin-based mater- r using a double-sided diamond disk (Microdont no 34.570,
ials allow their use in a variety of clinical indications, such LB100, Beltec; São Paulo, Brazil) under air-water irrigation.
as inlays, onlays, and veneers.21 Although their clinical ap- In total, 24 rectangular specimens with dimensions of 10 x
plication has been shown to be feasible and predictable 5 x 2 mm3 as measured with a digital caliper (Eccofer, Curi-
even in complex situations, restorations may have a shorter tiba, Paraná, Brazil) were obtained. They were then flat-
longevity due to fractures of the material,29 adhesive inter- r tened with a series of silicon carbide (#600, #800, and
face failures, inadequate handling by the operator, or pa- #1200 grit, 3M Oral Care). In addition, 24 rectangular
tient-related problems such as occlusal overload,23 para- blocks (10 x 5 x 2 mm3) were made of conventional RC
functional habits,16,23 and risk of secondary caries. In such (Z350, 3M Oral Care) using a translucent silicone mold
cases, intraoral repair might be an advantageous, less inva- (Master, Talmax silicone; Curitiba, Brazil). Two-mm incre-
sive, quick alternative which costs less3 than complete re- ments of RC were inserted into the mold, compacted, and
placement of the restoration. Similar to conventional RC photopolymerized for 40 s from each direction (Radii Cal,
restorations, the repair of these materials requires ade- SDI; Victoria, Australia, 1200 mW/cm2). After 24 h, the sur-r
quate surface conditioning to create microretentions for faces were flattened with silicon carbide paper as described
micromechanical bonding with the repair material, thus en- above. Thereafter, the rectangular blocks of both materials
suring greater longevity.3 were embedded in chemically activated acrylic resin (JET,
Several in vitro studies have reported on the effect of Artículos Odontológicos Clássico; São Paulo, Brazil). After
surface conditioning methods on the repair bond strength of polymerization, the outer surfaces were polished with a se-
RC materials.18,20,25 Some of the most commonly used ries of silicon carbide papers (#600, #800 and #1200) in a
methods include diamond-bur roughening,19 air abrasion polishing machine (Labpol 8-12, Extec; Enfield, CT, USA).
with conventional or silica-coated aluminum oxide parti- All blocks were immersed in distilled water and cleaned in
cles,27 phosphoric acid conditioning,31 and the use of silane an ultrasonic device for 5 min (Cristófoli Equipamentos de
and universal adhesives.36 However, the results and tech- Biossegurança; Paraná, Brazil).
niques of these studies vary greatly, since several factors
may influence repair adhesion, including type of material, Aging Procedures
repair protocol, aging conditions, and type of RC.19 In addi- Half of the blocks of each material were submitted to aging
tion, since repairs are usually performed in restorations that prior to repair (storage in distilled water for 6 months at
have been in clinical use for months or years, aging proto- 37ºC) in order to simulate the degradation that occurs in
cols for the substrates are required to simulate clinical situ- the oral environment. The other half were stored in distilled
ations. However, studies using such protocols are few.15,39 water for 24 h at 37ºC. Then, the blocks were randomly di-
Since an effective intraoral repair protocol has yet to be vided into eight groups of n = 12, according to the following
defined for NCRs and the effect of storage is still controver-r factors: material (2 levels), surface conditioning method (2
sial, the objective of this study was to evaluate the influ- levels), and aging prior to repair (2 levels) (Fig 1, Table 2).
ence of different surface conditioning methods and aging
conditions on the repair bond strength between a conven- Surface Conditioning Methods and Repair Procedures
tional RC and NCR. The hypotheses of this study were that Substrate surfaces were conditioned using a chairside air-
1. the repair bond strength would not be affected by the abrasion device (Microjato Standard, Bioart; São Paulo, Bra-
restorative material; 2. silicatization would promote higher zil) attached to metal holder to standardize the distance
bond strengths; 3. aging prior to repair of restorative mater-r and angulation of the nozzle during air abrasion.11 Surfaces
ials would reduce repair bond strength. were air abraded (CJ: air abrasion with 30-μm CoJet; or AB:

276 The Journal of Adhesive Dentistry

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Table 1 Brands, material types, chemical compositions, batch numbers, and manufacturers of the materials used in
this study

Brand Material type Chemical composition Batch No. Manufacturer

Lava Ultimate Nanoceramic 80 wt% nanoceramic, 20 wt% resin N552776 3M Oral Care;
composite resin St Paul, MN,
USA
Filtek Z350 Resin composite Bis-GMA, UDMA, TEG-DMA, bis-EMA, nanoparticles (silica: 20 nm, NT23089
zirconia: 4-11 nm, agglomerate of 0.6-1 μm)
Shade: translucent
Scotch Bond Universal bonding Bis-GMA, HEMA, decamethylene dimethacrylate, ethanol, water, 577056 3M Oral Care
Universal agent silane treated silica, 2-propenoic acid, methacrylated phosphoric
acid, copolymer of acrylic and itaconic acid, ethyl-4-
dimethylaminobenzoate, camphorquinone, (dimethylamino)ethyl
methacrylate, methyl ethyl ketone
CoJet System Alumina particles 30-μm Al2O3, synthetic amorphous silica, and fumed, crystalline- –
coated with silica free titanium dioxide
Aluminum Alumina particles 50-μm Al2O3 –
oxide

Table 2 Mean shear bond strength (MPa) and standard deviations (SD) of the experimental groups according to the
factors “material”, “surface conditioning” and “aging prior to repair”

Material Surface conditioning Aging Groups Mean ± SD (MPa)

NCR CoJet (CJ) 24 h NCR24hCJ 20.88 ± 5.74BC
Al2O3 (AB) NCR24hAB 28.16 ± 7.44AB
CoJet (CJ) 6 months NCR6mCJ 29.37 ± 5.41A
Al2O3 (AB) NCR6mAB 23.47 ± 5.33ABC
RC CoJet (CJ) 24 h RC24hCJ 19.71 ± 4.21C
Al2O3 (AB) RC24hAB 17.61 ± 5.52C

CoJet (CJ) 6 months RC6mCJ 20.92 ± 7.29BC

Al2O3 (AB) RC6mAB 18.18 ± 5.6C
Different letters in the same column indicate statistical difference (Tukey’s test; p < 0.05). For group descriptions, see text.

Table 3 Three-way ANOVA and Tukey’s test results for shear bond strength of the experimental groups

Source DF TSS MSS F p

Material 1 972.69 972.688 27.76 0.000*
Aging prior to repair (aging) 1 46.75 46.75 1.33 0.251
Surface conditioning 1 18.05 18.05 0.52 0.475
Material x aging 1 6.16 6.16 0.18 0.676
Material x surface conditioning 1 57.83 57.82 1.65 0.202
Aging x surface conditioning 1 286.94 286.93 8.19 0.005*
Material x aging x surface conditioning 1 235.97 235.96 6.74 0.011*
Error 88 3082.99 35.034
Total 95 4707.38
*Statistical significance (p˂0.05), DF: degrees of freedom; TSS: total sum of squares, MSS: mean sum of squares; F: F statistics.

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Do different surface conditioning methods and aging prior to repair affect the repair bond
Research question strength of resin composite to nanoceramic resin?

1. The repair bond strength would not be affected by the restorative material
Hypothesis 2. Silicatization would promote higher bond strengths
3. Aging prior to repair of restorative materials would reduce repair bond strength

NCR specimens (12x5x10 mm3) (n = 24)

Fabrication of test
specimens and arranging
test groups RC specimens (12x5x10 mm3) (n = 24)

Storage in distilled water for 24 hours at 37°C (control group)

Aging prior to repair Storage in distilled water for 6 months at 37°C

Surface conditioning 50 μm AI2O2 + Adhesive resin

for repair 30 μm CoJet + Adhesive resin

Evaluation of surfaces Thermocycling Shear bond strength SEM evaluation of surfaces

under SEM (x 10.000, 5–55°C) (50 KgF, 0.5 mm/min) after debonding

Fig 1 Flowchart of the study protocol (NCR: Lava Ultimate; RC: Filtek Z350).

air abrasion with 50-μm Al2O3) according to the following Shear Bond Strength Test
parameters: 20 s duration; 2.5 bar pressure; 90-degree The specimens were subjected to shear bond testing (50
nozzle angle; 10 mm distance. Afterwards, the surfaces kgf, 0.5 mm/min) in a universal testing machine (DL-1000,
were ultrasonically cleaned in distilled water for 2 min and EMIC; São José dos Campos, Sao Paolo, Brazil), in which a
air dried. Subsequently, the area to receive the adhesive metal device was used to fix the specimen to maintain the
was limited to 3 mm using a piece of adhesive tape with a NCR-RC interface perpendicular to the horizontal plane. The
perforation. One coat of adhesive resin (Scotchbond Univer- r load was applied to the adhesive interface using an orth-
sal, 3M Oral Care) was applied with a microbrush under odontic wire (diameter: 0.2 mm) until debonding.33 Adhesive
active friction for 20 s to the limited adhesion area, air strength was calculated using the following formula: R = F/A,
dried for 5 s for solvent evaporation, and photopolymerized where R = adhesive strength (MPa); F = force (N); A = interfa-
for 20 s (Radii Cal, 1200 mW/cm2). cial area (mm). The adhesive area of each ceramic block was
After surface conditioning, to simulate repair on the sub- defined by the area of a circle, A = /r2, where / = 3.14 and
strate materials, RC (Z350) was applied on the substrates r = 1 mm, resulting in a cross-sectional area of 3.14 mm2.
using a Teflon matrix (∅ = 2 mm; h = 2 mm) (Ultradent Jig,
Ultradent; South Jordan, UT, USA) which allowed standard- Failure Analysis
ization of the adhesive area and height of the cylinder. After The surfaces of the debonded specimens were examined
adapting the matrix, it was filled with a single increment of using an optical stereomicroscope (20X, Stereo Discovery
RC and photopolymerized for 20 s (Radii Cal, 1200 mW/ V20, Zeiss; Göttingen, Germany). Failure modes were clas-
cm2). The matrices were removed and the cylinders were sified as: adhesive at the NCR-RC interface; mixed adhesive
again photopolymerized for 20 s. Afterwards, all bonded as- failure at the NCR-RC plus cohesive in the NCR; mixed ad-
semblies (NCR-RC) were submitted to thermocycling hesive failure at the NCR-RC interface and cohesive failure
(10,000 cycles, 5°C to 55°C, dwell time in each bath: 30 s) in the RC; cohesive failure in the RC.
(Nova Ethics; São Paulo, Brazil). After gold-sputter coating (30 nm) in vacuum for 180 s at
40 mA, the surface topography and failure modes of repre-
sentative specimens were analyzed using SEM for (Inspect

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 Moura et al

Fig 2 Distribution of failure types per

group. 12
10
8
6
4 Mixed failure (Type B)

Mixed failure (Type C)

2
0

S50, FEI; Brno, Czech Republic) at 20 KV and a magnifica- RC surfaces seemed to be deeper and wider than on NRC.
tion of 1500X. Moreover, the factor “aging prior to repair” did not influence
surface morphology, regardless of the material tested.
Statistical Analysis
After verifying the normality of the data, the data were ana-
lyzed using 3-way ANOVA and Tukey’s test (STATISTIX soft- DISCUSSION
ware v. 8, Analytical Software; Tallahassee, FL, USA). A
sample power of 99.9% was calculated based on the OpenEpi Using the shear bond strength test, this study investigated
website considering a 95% confidence interval. p-values the effect of different surface conditioning and aging proto-
less than 0.05 were considered statistically significant in cols on the repair bond strength of a conventional resin
all tests. composite to a nanoceramic resin CAD/CAM material.
Other methods are also available for for testing adhe-
sion, such as microtensile and microshear bond strength-
RESULTS tests. Although widely used in bond strength testing, the
microtensile test presents methodological difficulties and
Bond strength results (MPa) were significantly affected by requires cutting procedures that may cause pre-test fail-
the material type (p = 0.00) but not by surface conditioning ures. On the other hand, adequate microshear bond
method (p = 0.475) or aging prior to repair (p = 0.251) strength testing must include proper application of the ad-
(3-way ANOVA) (Table 3). hesive and resin cement on the small bonding area, which
When only the factor “material” was analyzed, NCR is about 1 mm2.34 Bearing that in mind, the macroshear
(25.47) presented significantly higher mean bond strengths bond strength test has some advantages, as it does not
did than RC (19.1) (p < 0.05). Within the NCR groups, require sectioning procedures and therefore is widely used
NCR6mCJ (29.37 ± 5.41) showed significantly higher mean in adhesion studies.34 Furthermore, shear tests could be
bond strengths compared to NCR24hCJ (20.88 ± 5.74) considered clinically more relevant, since they are related
(Table 3). For the RC groups, lower bond strengths were to less incorporation of defects during specimen prepar- r
observed with no significant differences between the ation and less damage compared to tensile tests. In order
groups. When all experimental groups were compared, the to overcome nonuniform stress distribution in a shear
mean bond strength of RC6mCJ (20.92 ± 7.29) was statis- test,34 a smaller adhesive area of 2 mm2 was used in this
tically similar to all the other groups, except for NCR6mCJ study.33 The bonding surface area (∅: 2 mm) was delimited
(29.37 ± 5.41). by adhesive tape with a perforation the size of the external
The failure analysis (Fig 2) revealed predominantly mixed diameter (∅: 3 mm) of the Teflon mold, which has an inter- r
failures of adhesive+cohesive in the substrate material nal diameter of 2 mm. In addition, an orthodontic wire was
(Fig 3), except for the groups NCR24hCJ and NCR6mAB, used to perform the test, which gives more reliable results
where mainly mixed failures of adhesive+cohesive at the due to more uniform force distribution than does a conven-
RC were observed (Fig 4). tional shear-test knife, as the wire encircles a larger area of
SEM images showed that surface morphologies varied the composite cylinder.33
according to the air abrasion protocols. Air abrasion with The first null hypothesis, that bond strength would not be
Al2O3 particles created deeper grooves than did CoJet on influenced by the restorative material, was rejected, as NCR
the material surfaces (Fig 5). However, the grooves on the presented bond strengths higher than the RC tested. The

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a b c d

e f g h

Fig 3 SEM images of surface morphology. a) NCR24hCJ; b) NCR6mCJ; c) NCR24hAB; d) NCR6mAB; e) RC24hCJ; f) RC6mCJ; g) RC24hAB;
h) RC6mAB. Note that AB resulted in deeper grooves than did CJ on the materials surface, the grooves on the RC surfaces are deeper and
wider than NRC, and that aging did not influence surface morphology of the materials tested. Original magnification: 1500X.

differences found may be related to the microstructural com- polymer surface, improving adhesion.13 Moreover, the
position of the materials. Although both are considered res- nanoparticles of this CAD/CAM material are treated with a
inous materials,12 NCR is based on CAD/CAM nanotechnol- silane coupling agent according to the manufacturer’s rec-
ogy and has a higher filler content (nanoceramic particles of ommendation.36 In contrast to the findings of this study,
80%, embedded in a highly polymerized resin matrix of some authors reported higher results for conventional resin
20%)12 when compared to RC (high-density composite resin composites.42 Since NCR contains UDMA monomer, which
material containing 72 wt% filler particles).1 As it is polymer-
r is polymerized industrially and has a higher degree of con-
ized under high pressure and temperature, NCR has a higher version than that of bis-GMA,42 low levels of residual mono-
degree of conversion than do conventionally polymerized res- mers and free radicals hinder additional copolymerization of
ins, limiting the number of available unreacted C-C bonds. In the NCR after repair.15,42 NCR resins have few carbon-car- r
addition, the nanoparticles are treated with a silane coupling bon double bonds on the surface due to the industrial poly-y
agent. The functionalized silane chemically bonds to both merization procedure, and therefore the interaction between
the nanoceramic and the resin matrix. This suggests that the substrate material and the resin composites makes
besides the micromechanical retention promoted by the sur- r repair difficult.36
face treatment, there was also chemical adhesion to the Based on our results, the second null hypothesis that
repair composite resin as well as to the universal adhesive. silication promotes better bond strengths was not ac-
The latter also contains silane and methacrylates, contribut- cepted. Although this study showed higher mean values for
ing to the adhesion of the silane monomers to NCR. This 30-μm CoJet for both materials, the bond strengths were
may explain the present results for this material.36 statically similar to the those obtained using air abrasion
Similar results have been found in some in vitro studies. with Al2O3. Similar results were reported previously.19,30
Loomans et al19 compared two resin materials, Lava Ulti- According to those authors, although both techniques pro-
mate (3M Oral Care) and a polymer-based resin (Clearfil moted an increase in surface roughness, the additional
Estenia, Kuraray; Tokyo, Japan), after different surface con- chemical action of the silica did not significantly increase
ditioning and thermocycling (10,000 cycles). In that study, the bond strength. However, they reported that the effect of
Lava Ultimate presented higher bond strength after repair air abrasion also depends on the microstructure and com-
and thermocycling,19 suggesting that this might be related position of the material.19,30
to different filler compositions which react differently during The adhesion between the aged substrate and the new
surface conditioning17,24 to improve adhesion even after composite for repair takes place through three mechan-
aging.19,36 The high filler content of Lava Ultimate favors isms: chemical bonding with the organic matrix, chemical
chemical interaction between primers and the silica on the bonding with the exposed filler particles, and micromechan-

280 The Journal of Adhesive Dentistry

 Moura et al

ical retention on the conditioned surface.7 The CoJet sys- a b

tem enables mechanical and chemical bonding compared
to air abrasion with pure alumina particles, including in-
creased surface energy through the deposition of silica on
the surface and chemical bonding through silane.24 Similar
to our study, other authors used different surface condition-
ing methods for the repair of six materials.42 They found
that the NCR (Lava Ultimate) presented higher bond
strengths, which were, however, statistically similar to the
air-abraded groups (CoJet+silane and Al2O3) vs groups
Fig 4 Representative stereomicroscopic images of failure analysis
roughened by a bur or without conditioning.42 (20X). a) Mixed failure type B in NCR; b) mixed failure type B in RC.
In addition to air abrasion methods, other methods such * substrate NCR; ( adhesive failure; & cohesive failure in the
as roughening with diamond burs, acid etching (9% hydro- substrate; star: cohesive failure in the adherent (RC).
fluoric acid or 37% phosphoric acid), or application of bond-
ing agents (silane or adhesives) have been tested, all with
varying results.15,36,39 Studies evaluating adhesion be- a b
tween CAD/CAM and resin materials showed that in addi-
tion to surface conditioning, the application of an adhesive
was essential.15,36,42 The silane used in this study con-
tains methacrylic silane and phosphate monomers, allowing
their concomitant interaction with different materials.36 This
silane was recommended for NCR repair, since in addition
to a silane coupling agent, it also has an MDP component
that chemically reacts with the inorganic component of the
NCR and zirconia fillers in the NCR.26,39,41 Özcan and Vol-
pato26 reported that silanization significantly improved the
long-term bond resistance of Lava Ultimate. Fig 5 Representative stereomicroscopic images of failure analysis
The third hypothesis, that aging of the restorative mater-r (20X). a) mixed failure type C in NCR; b) mixed failure type C in RC.
ials decreases the repair bond strength, was not accepted. ( adhesive failure in the substrate (NCR); & cohesive failure in
In this study, the materials aged were stored in water for the RC.
6 months at 37°C prior to the repair procedures. After-
wards, the surfaces were subjected to 10,000 thermal cy- y
cles to simulate 1 year of clinical use.14 Although the aging
factor was not significant, the interaction between material
type and aging showed a significant effect on the bond
strength. In the NCR group aged for 6 months, treatment
with CoJet resulted in significantly higher shear bond still unclear; this could be attributed to the use of different
strengths compared to the group aged for 24 h and to all thermocycling protocols, study parameters, conditioning
the RC groups. Aging might cause changes in restorative methods, and bond tests employed.36,39,42
materials, such as surface and volumetric changes.39 De- Microstructural characteristics and the effect of surface
spite the highly polymerized and reticulated structure of conditioning on the wear of materials have been described
NCR, storage in water may have induced degradation, in- previously.22 In this study, RC generally showed lower bond
creasing superficial roughness and microretentions, thus strength after air abrasion, especially using Al2O3 particles,
amplifying the air abrasion effect and optimizing the adhe- compared to NCR. This might be due to the reaction of RC
sion to the CR.5 This micromechanical retention on the sur- r nanofillers to the Al2O3 particles with substrate wear and
face of aged resinous materials has already been reported disintegration of the clusters.22 The loss of inorganic fillers
as one of the main mechanisms to obtain a reliable repair can reduce the interaction with the silane, reducing bond
bond,5,35 which may explain the findings of this study. strength after repair.30 SEM images also show a greater
These findings also corroborate those of a previous impact of these techniques on the RC than NCR surfaces.
study,39 in which even in aged NCR specimens, the air- Since RCs have a high percentage of organic matrix, they
abraded and silica-coated groups showed higher bond are more susceptible to air abrasion compared to CAD/CAM
strengths than groups that did not receive surface condi- composites, which might explain the results.19 In clinical
tioning, reinforcing the fundamental role of these tech- repair, the substrate surfaces are cleaned with air-water
niques for the repair of NCR restorations. Studies on the spray. In this study, substrates were cleaned using an ultra-
effect of aging on bond strength of CAD/CAM resinous ma- sonic device for the sake of standardization and to elimi-
terials showed that thermocycling did not affect the bond nate possible contamination as a confounding factor. Fu-
strength to the composite resin in repair procedures.15 ture studies should also look at clinical cleaning protocols
However, according to other studies, the effect of aging is and their effect on the adhesion protocols studied.

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The prevalence of mixed failures, with predominance of 11. Dal Piva AMO, Carvalho RLA, Lima AL, Bottino MA, Melo RM, Valandro LF.
Silica coating followed by heat-treatment of MDP-primer for resin bond
cohesive failures in the substrate material, can also be ex- stability toyttria-stabilized zirconia polycrystals. J Biomed Mater Res Part
plained by the filler content of the materials. In conven- B 2018:00B:000–000.
tional composites, the inorganic particles are incorporated 12. de Jesus Tavarez RR, Almeida Júnior LJDS, Guará TCG, Ribeiro IS, Maia
Filho EM, Firoozmand LM. Shear bond strength of different surface treat-
into a polymer matrix without interconnections,8 which may ments in bulk fill, microhybrid, and nanoparticle repair resins. Clin Cos-
favor the penetration of water during storage or thermocy- y met Investig Dent 2017;9:61–66.
cling, altering the surface and decreasing bond strength.9 13. Gajewski VE, Pfeifer CS, Froes-Salgado NR, Boaro LC, Braga RR. Mono-
mers used in resin composites: degree of conversion, mechanical proper-
r
Only for the NCR24hCJ and NCR6m Al2O3 groups were ties and water sorption/solubility. Braz Dent J 2012; 23:508–514.
mixed failures (adhesive+cohesive in the RC) more fre- 14. Gale MS, Darvell BW. Thermal cycling procedures for laboratory testing of
quent, although the bond strengths showed no statistically dental restorations. J Dent 1999;27:89–99.
significant difference. 15. Güngör MB, Nemli SK, Bal BT, Ünver S, Doğan A. Effect of surface treat-
ments on shear bond strength of resin composite bonded to CAD/CAM
In a clinical situation, several substrates (enamel, den- resin-ceramic hybrid materials. J Adv Prosthodont 2016;8:259–266.
tin, and restorative materials) can be affected by the repair 16. Kimmich M, Stappert C. Intraoral treatment of veneering porcelain chip-
procedures. Thus, further studies should investigate the ping of fixed dental restorations: A review and clinical application. J Am
influence of repair procedures on the bond strength to dif-f Dent Assoc 2013;144:31–44.
17. Loomans BA, Cardoso MV, Opdam NJ, Roeters FJ, De Munck J, Huys-
ferent substrates. In addition, long-term studies should be mans MC, Van Meerbeek B. Surface roughness of etched composite
performed to determine the procedure durability. resin in light of composite repair, J Dent 2011;39:499–505.
18. Loomans BA, Cardoso MV, Roeters FJ, Opdam NJ, de Munck J, Huys-
mans MC, van Meerbeek B. Is there one optimal repair technique for all
composites. Dent Mater 2011;27:701–709.
CONCLUSIONS 19. Loomans B, Mesko M, Moraes RR, Ruben J, Bronkhorst EM, Pereira-
Cenci T, Huysmans MC. Effect of different surface treatment techniques
Air abrasion with 50-μm Al2O3 or silicatization with 30-μm on the repair strength of indirect composites. J Dent 2017;59:18–25.
silica-coated alumina particles followed by adhesive applica- 20. Lucena-Martín C, González-López S, Navajas-Rodríguez DE, Mondelo JE.
The effect of various surface treatments and bonding agents on the re-
tion resulted in durable repair strength of the resin compos- paired strength of heat-treated composites. J Prosthet Dent 2001;86:
ite. Repair bond strength to nanoceramic CAD/CAM resin 481–488.
was higher than to the conventional resin composite tested. 21. Mesko ME, Sarkis-Onofre R, Cenci MS, Opdam NJ, Loomans B, Pereira-
Cenci T. Rehabilitation of severely worn teeth: a systematic review. J
Dent 2016;48:9–15.
22. Mitra SB, Wu D, Holmes BN. An application of nanotechnology in ad-
ACKNOWLEDGMENTS vanced dental materials. J Am Dent Assoc 2003;134:1382–1290.
23. Opdam NJ, Van de Sande FH, Bronkhorst E, Cenci MS, Bottenberg P, Pal-
This study was partly financed by the Coordenação de Aperfeiçoa- lesen U, Gaengler P, Lindberg A, Huysmans MC, Van Dijken JW. Longevity
mento de Pessoal de Nível Superior, Brasil (CAPES) – Finance Code of posterior composite restorations: a systematic review and meta-analy-
y
001. The authors would like to acknowledge 3M Oral Care for pro- sis. J Dent Res 2014;93:943–949.
viding the materials used for the experiments. 24. Özcan M, Barbosa SH, Melo RM, Galhano GAP, Botino MA. Effect of sur-
r
face conditioning methods on the microtensile bond strength of resin
composite to composite after aging conditions. Dent Mater 2007;23:
1276–1282
REFERENCES 25. Özcan M, Pekkan G. Effect of different adhesion strategies on bond
strength of composite resin to composite-dentin complex. Oper Dent 2013;
1. Acar O, Yilmaz B, Altintas SH, Chandrasekaran I, Johnston WM. Color 38:63–72.
stainability of CAD/CAM and nanocomposite resin materials. J Prosthet
Dent 2016;115:71–75. 26. Özcan M, Volpato CÂ. Surface conditioning and bonding protocol for
nanocomposite indirect restorations: how and why? J Adhes Dent
2. Awada A, Nathanson D. Mechanical properties of resin-ceramic CAD/CAM 2016;18:82.
restorative materials. J Prosthet Dent 2015;114:587–593.
27. Özlem U, Buyukhatipoglu IK, Seçilmis A. Shear bond strength of repair
3. Batista GR, Kamozaki MB, Gutierrez NC, Caneppele TM, Torres CR. Ef- f
systems to new CAD/CAM restorative materials. J Prosthodont 2018;27:
fects of different surface treatments on composite repairs. J Ades Dent
748-754.
2015;17:421–426.
28. Quinn JB, Quinn GD. Material properties and fractography of an indirect
4. Baur V, Ilie N. Repair of dental resin-based composites. Clin Oral Invest
dental resin composite Dent Mater 2010;26:589–599.
2013;17:601–608.
5. Bonstein T, Garlapo D, Donarummo J, Bush PJ. Evaluation of varied repair 29. Rekow ED, Silva NRFA, Coelho PG, Zhang Y, Guess P, Thompson VP. Per-
r
protocols applied to aged composite resin. J Adhes Dent 2005;7:41–49. formance of dental ceramics: challenges for improvements. J Dent Res
2011;90:937–952.
6. Brentel AS, Özcan M, Valandro LF, Alarca LG, Amaral R, Bottino MA. Mi-
crotensile bond strength of a resin cement to feldspathic ceramic after 30. Rodrigues SA Jr, Ferracane JL, Della Bona A. Influence of surface treat-
different etching and silanization regimens in dry and aged conditions. ments on the bond strength of repaired resin composite restorative ma-
Dent Mater 2013;23:1323–1331. terials. Dent Mater 2009;25:442–451.
7. Brosh T, Bichacho N, Blutstein R. Effect of combinations of surface treat- 31. Rossato DM, Bandeca MC, Saade EG, Lizarelli RFZ, Bagnato VS, Saad
ments and bonding agents on the bond strength of repaired composites. JRC. Influence of Er.YAG laser on surface treatment of aged composite
J Prosthet Dent 1997;77:122–126. resin to repair restoration. Laser Physics 2009;19:2144–2149.
8. Cekic-Nagas I, Ergun G, Egilmez F, Vallittu PK, Lassila LV. Micro-shear 32. Secilmis A, Ozlem U, Buyukhatipoglu IK. Evaluation of the shear bond
bond strength of different resin cements to ceramic/glass-polymer CAD- strength of two resin cements on different CAD/CAM materials. J Adhes
CAM block materials. J Prosthodont Res 2016;60:265–273. Sci Technol 2016;30: 983–993.
9. Coldea A, Swain MV, Thiel N. Mechanical properties of polymer-infiltrated- 33. Sinhoreti MA, Consani S, De Goes MF, Sobrinho LC, Knowles JC. Influ-
ceramic-network materials. Dent Mater 2013;29:419-426. ence of loading types on the shear strength of the dentin-resin interface
10. Curran P, Cattani-Lorente M, Wiskott HWA, Durual S, Scherrer SS. Grinding bonding. J Mater Sci Mater Med 2001;12:39–44.
damage assessment for CAD-CAM restorative materials. Dent Mater 34. Sirisha K, Rambabu T, Ravishankar Y, Ravikumar P. Validity of bond
2017;33:294–308. strength tests: A critical review-Part II. J Conserv Dent 2014;17:420–426.

282 The Journal of Adhesive Dentistry

 Moura et al

35. Souza MO, Leitune VC, Rodrigues SB, Samuel SM, Collares FM. One-year 41. Wahsh MM, Ghallab OH. Influence of different surfasse treatments on
aging effects on microtensile bond strengths of composite and repairs microshear bond strength of repair resin composite to two CAD/CAM es-
with different surface treatments. Braz Oral Res 2017;5:31–34. thetic restorative materials. Tanta Dent J 2015;12:178–184.
36. Stawarczyk B, Krawczuk A, Ilie N. Tensile bond strength of resin compos- 42. Wiegand A, Stucki L, Hoffmann R, Attin T, Stawarczyk B. Repairability of
ite repair in vitro using different surface preparation conditionings to an CAD/CAM high-density PMMA- and composite-based polymers. Clin Oral
aged CAD/CAM resin nanoceramic. Clin Oral Investig 2015;19:299–308. Investig 2015;19:2007–2013.
37. Stawarczyk B, Özcan M, Roos M, Schmutz F, Trottmann A, Hämmerle
CHF. Two-body wear rate of CAD/CAM resin blocks and their enamel an-
tagonists. J Prosthet Dent 2013;109:325–332.
38. Stawarczyk B, Sener B, Trottmann A, RoosM, ÖzcanM, Hämmerle CH.
Discoloration of manually fabricated resins and industrially fabricated
CAD/CAM blocks versus glass-ceramic: effect of storage media, duration Clinical relevance: Air abrasion with Al2O3 particles or
and subsequent polishing. Dent Mater J 2012;31:377–383. tribochemical silica coating followed by adhesive
39. Subaşı MG, Alp G. Repair bond strengths of non-aged and aged resin resin application are effective surface conditioning
nanoceramics. J Adv Prosthodont 2017;9:364–370.
methods for the repair of nanoceramic CAD/CAM resin
40. Van de Sande FH, Opdam NJ, Rodolpho PA, Correa MB, Demarco FF,
Cenci MS. Patient risk factors influence on survival of posterior compos- with the tested resin composite.
ites. J Dent Res 2013;92: 78S–83S.

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