d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230

Available online at www.sciencedirect.com

journal homepage: www.intl.elsevierhealth.com/journals/dema

Bonding effectiveness of self-adhesive composites to dentin

and enamel

Andr Poitevin a , Jan De Munck a , Annelies Van Ende a , Yuji Suyama a,b , Atsushi Mine a,c ,
Marleen Peumans a,d , Bart Van Meerbeek a,d,
a KU Leuven BIOMAT, Department of Oral Health Sciences, KU Leuven (University of Leuven), Leuven, Belgium
b Toranomon Hospital, Tokyo, Japan
c Department of Oral and Maxillofacial Rehabilitation, Okayama University Graduate School of Medicine, Dentistry and Pharmaceutical

Science, Okayama, Japan

d Department of Dentistry, University Hospital Leuven, Leuven, Belgium

a r t i c l e i n f o a b s t r a c t

Article history: Self-adhesive composites (SACs) are claimed to bond to tooth substrate without a separate
Received 1 March 2012 adhesive. Bonding effectiveness data are however still limited.
Received in revised form Objectives. In SubProject 1, the hypothesis was tested that the micro-tensile bond strength
2 October 2012 (TBS) to dentin of two owable SACs was alike that of a one-step self-etch adhesive (1-SEa)
Accepted 2 October 2012 combined with a owable composite (owC). In SubProject 2, the hypothesis was tested that
the nature of the smear layer did not affect the TBS of the SACs to dentin/enamel.
Methods. SubProject 1: The TBS to bur-cut dentin of two SACs (Fusio Liquid Dentin, Pentron;
Keywords: Vertise Flow, Kerr) was measured and compared to that of four 1-SEa/owC combinations
Self-adhesive (AdheSe One/Tetric EvoFlow, Ivoclar Vivadent; Adper Prompt L-Pop/Filtek Supreme XT Flow-
Composite able, 3M ESPE; iBond/Venus ow, Heraeus Kulzer; Xeno V/X-ow, Dentsply) and of one 3-step
Micro-tensile bond strength etch-and-rinse adhesive (3-E&Ra: OptiBond FL, Kerr) combined with Premise Flowable (Kerr).
Dentin The effect of pre-etching dentin with phosphoric acid on the TBS of the SAC Vertise Flow
Enamel (Kerr) was measured as well. SubProject 2: The TBS of the two SACs and one 1-SEa/owC
Smear layer combination (Adper Prompt L-Pop/Filtek Supreme XT Flowable, 3M ESPE) to either bur-cut
or SiC-paper ground dentin/enamel was measured. The effect of pre-etching enamel with
phosphoric acid on the TBS of the SAC Vertise Flow (Kerr) was also measured.
Results. SubProject 1: The TBS to dentin of both SACs was signicantly lower than that of the
1-SEa/owC and the 3-E&Ra/owC combinations, of which the latter performed best. The
SAC Fusio Liquid Dentin (Pentron) bonded signicantly better to dentin than Vertise Flow
(Kerr), except when dentin had additionally been pre-etched with phosphoric acid. SubPro-
ject 2: Surface smear did not interfere with bonding of the SACs to dentin/enamel, while
their TBS remained signicantly lower than that of the 1-SEa/owC combination. Prior
phosphoric-acid etching of dentin/enamel signicantly ameliorated the bonding effective-
ness of Vertise Flow (Kerr).
Signicance. The bonding effectiveness of owable SACs underscores that of 1-SEas and one
gold-standard 3-E&Ra when combined with their proprietary owable composite. Conse-
quently, routine clinical application of SACs should be carefully considered.
2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Corresponding author at: KU Leuven BIOMAT, Department of Oral Health Sciences, KU Leuven (University of Leuven), Kapucijnenvoer 7,
blok a bus 7001, BE-3000 Leuven, Belgium. Tel.: +32 16 337587; fax: +32 16 332752.
E-mail address: bart.vanmeerbeek@med.kuleuven.be (B. Van Meerbeek).
0109-5641/$ see front matter 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.dental.2012.10.001
222 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230

buccal enamel was attened using the above-mentioned BUR-

1. Introduction CUT or SiC-GROUND procedure. The teeth were randomly
divided in groups according to the SubProject and the specic
As todays adhesives are often regarded as technique-sensitive
adhesive material tested (Table 1): In SubProject 1, the TBS to
[15], combining the benets of adhesive and composite tech-
BUR-CUT dentin of the two SACs, Fusio Liquid Dentin (Pentron
nology into a self-adhesive restorative composite was the next
Clinical, Orange, CA, USA) and Vertise Flow (Kerr, Orange, CA,
step clinicians have been waiting for [6,7]. Especially simpli-
USA) was measured and compared to that of four 1-SEa/owC
cation in clinical adhesive procedures is a major drive for
combinations (AdheSe One/Tetric EvoFlow, Ivoclar Vivadent,
current research-and-development efforts at dental indus-
Schaan, Liechtenstein; Adper Prompt L-Pop/Filtek Supreme
try [6,7]. However, the hydrophobichydrophilic mismatch
XT Flowable, 3M ESPE, Seefeld, Germany; iBond/Venus ow,
between dental composite and tooth substrate needs to be
Heraeus Kulzer, Hanau, Germany; Xeno V/X-ow, Dentsply,
overcome in order to achieve a long-term lasting bond. The
Konstanz, Germany) and of one 3-step etch-and-rinse adhe-
introduction of self-adhesive composite cements [812] has
sive (3-E&Ra: OptiBond FL, Kerr) combined with Premise
led to the development of a new class of self-adhesive (restor-
Flowable (Kerr). The effect of pre-etching BUR-CUT dentin with
ative) composites (SACs) that are bonded to tooth enamel and
phosphoric acid (Kerr, Orange, CA, USA) on the TBS of the
dentin without a separate adhesive.
SAC Vertise Flow (Kerr) was measured as well. In SubProject 2,
Since their introduction, data regarding physical proper-
the TBS of the two SACs and one 1-SEa/owC combination
ties of SACs [1315], their shear bond strength and marginal
(Adper Prompt L-Pop/Filtek Supreme XT Flowable, 3M ESPE) to
sealing potential (micro-leakage studies) [1618] were pub-
either BUR-CUT or SiC-GROUND dentin and enamel was mea-
lished. Even more, SACs have been tested for orthodontic and
sured. The effect of pre-etching BUR-CUT and SiC-GROUND
endodontic purposes [19,20]. However, so far no micro-tensile
enamel with phosphoric acid (Kerr, Orange, CA, USA) on the
bond strength (TBS) data are available in literature. Of high
TBS of the SAC Vertise Flow (Kerr) was also measured. All
interest is for instance to know if the smear layer, typically
bonding and restorative procedures were performed strictly
prepared by bur clinically, may potentially interfere with the
according to the manufacturers instructions (Table 1). After
bonding effectiveness of this new group of composites. In
adhesive treatment, the surfaces were built up to a height
addition, all publications have dealt with only one commercial
of 5 mm with the respective owC (shade A2). Each layer of
SAC, namely Vertise Flow (Kerr).
1.5 mm was light-cured for 40 s using an Optilux 500 light-
Therefore, the aim of this study was to test in SubProject
curing unit (Demetron/Kerr, Danbury, CT, USA) with a light
1 hypothesis 1 that the TBS to bur-cut dentin of two (com-
output of not less than 600 mW/cm2 . After storage of the teeth
mercial) owable SACs was alike that of a one-step self-etch
for 1 week in 0.5% chloramine at 37 C, they were sectioned
adhesive (1-SEa) when combined with a owable composite
perpendicular to the bonding surface into square specimens of
(owC), and in SubProject 2 hypothesis 2 that the smear layer
1 mm 1 mm using a fully automated precision water-cooled
did not affect the TBS of the two SACs to dentin and enamel.
diamond saw (Accutom-50, Struers A/S, Ballerup, Denmark).
In addition, the effect of pre-etching tooth enamel/dentin with
For each tooth, only the 4 to 9 central sticks were used, result-
phosphoric acid on the TBS of the SAC Vertise Flow (Kerr) was
ing in 24 to 35 sticks per group. Specic measures were taken
tested as well, having hypothesized that pre-etching did not
to reduce the incidence of pre-testing failures (ptf) by suppor-
increase the TBS (hypothesis 3).
ting the slices with alginate (Alginot, Kerr, Orange, CA, USA)
during sectioning. The width and thickness of each specimen
were measured to the nearest 0.01 mm using a digital calliper
2. Materials and methods (Mitutoyo, Tokyo, Japan). For each micro-specimen, a bonding
surface of about 1 mm2 was obtained.
2.1. Micro-specimen preparation
2.2. TBS
The experimental set-up is schematically presented in Fig. 1.
Non-carious and non-restored human third molars (gathered The micro-specimens were xed with cyanoacrylate glue
following informed consent approved by the Commission for (Model Repair II Blue, Dentsply-Sankin, Ohtawara, Japan) onto
Medical Ethics of KU Leuven) were stored in 0.5% chloramine a notched BIOMAT jig [21]. The TBS of each micro-specimen
in water at 4 C and used within 1 month after extraction. was determined in a universal testing machine (Instron 5848
Ninety-ve teeth, 5 teeth per group, were mounted in gypsum Micro Tester, High Wycombe, Bucks, UK) using a load cell of
blocks in order to facilitate manipulation. For the dentin spec- 500 N and a crosshead speed of 1 mm/min. The TBS of each
imens, the occlusal third of the molar crowns was removed specimen was calculated in MPa, by dividing the imposed force
by means of a water-cooled slow-speed diamond saw (Isomet (in N) at the time of fracture by its cross-sectional bond area
1000, Buehler, Lake Bluff, IL, USA). A standard smear layer was (in mm2 ). All specimens were maintained moist throughout
produced by removing a thin layer of the surface using a water- the whole preparation and test procedure.
cooled, high-speed medium-grit diamond bur (842, Komet,
Lemgo, Germany) mounted in a custom-adapted MicroSpec- 2.3. Failure analysis and Feg-SEM examination
imen Former (BUR-CUT; thick and compact smear layer)
or using 600-grit silicon-carbide paper under running water All specimens tested were semi-quantitatively analyzed for
(SiC-GROUND; thin smear layer; solely in SubProject 2). For the mode of failure using a stereomicroscope at a magni-
the enamel specimens (solely in SubProject 2), lingual and cation of 50 (Wild M5A, Heerbrug, Switzerland). Failures
Table 1 Materials used in this study.
Material
Self-adhesive Fusio Dentin Liquid
owable composite (Pentron Clinical, Orange,
CA, USA)
Vertise Flow (Kerr, Orange,
CA, USA)
One-step self-etch AdheSe One (Ivoclar
adhesive Vivadent, Schaan,
Liechtenstein)
Adper Prompt L-Pop (3M
ESPE, Seefeld, Germany)
iBond (Heraeus Kulzer,
Hanau, Germany)
Xeno V (Dentsply,
Konstanz, Germany)
Three-step OptiBond FL (Kerr, Orange,
etch-and-rinse CA, USA)
adhesive
Flowable composite Filtek Supreme XT Flowable
(3M ESPE, St. Paul, MN, USA)
Premise Flowable (Kerr,
Orange, CA, USA)
Tetric EvoFlow (Ivoclar
Vivadent, Schaan,
Liechtenstein)
Venus ow (Heraeus-Kulzer,
Hanau, Germany)
X-ow (Dentsply, Konstanz,
Germany)
a
Composition as provided by respective manufacturer: bis-EMA, ethoxylated bisphenol A glycol dimethacrylate; bis-GMA, bisphenol-glycidyl methacrylate; DGDMA, diethylene glycol dimethacry-
late; GPDM, glycerol phosphate dimethacrylate; HEMA, hydroxyethylmethacrylate; PAMM, phthalic acid monoethyl methacrylate; TEGDMA, triethylene glycol dimethacrylate; UDMA, urethane
dimethacrylate; 4-MET, 4-methacryloxyethyltrimetellitic acid.
Compositiona [lot number]
UDMA, TEGDMA, HEMA, 4-MET, nano-sized amorphous silica, silane
treated barium glass, minor additives, photo curing system [3479986]
GPDM, HEMA, prepolymerized ller, nano-sized ytterbium uoride, 1-m
barium glass ller, nano-sized colloidal silica [3435242]
Derivatives of bis-acrylamide, water, bis-methacrylamide dihydrogen
phosphate, amino acid acrylamide, hydroxyalkyl-methacrylamide, highly
dispersed silicon dioxide, catalysts, stabilizers [L49718]
First blister: methacrylic phosphates, bis-GMA photo initiator [412924]
Second blister: water, HEMA, polyalkenoic acid polymer [412924]
UDMA, 4-meta, glutaraldehyde, acetone, water, photoinitiators, stabilizer
[010075]
Bifunctional acrylic amides, acryloamido alkylsulfonic acid, functionalized
phosphoric acid ester, acrylic acid, camphorquinone, butylated
benzenediol, water, tert-butanol, photoinitiators, stabilizer [0908001751]
Etching: 37.5% phosphoric acid, silica thickener [3034827]
Primer: HEMA, GPDM, PAMM, ethanol, water, photo-initiator [3457744]
Adhesive: TEGDMA, UDMA, GPDM, HEMA, bis-GMA, ller, photo initiator
[3461592]
Bis-GMA, TEGDMA, bis-EMA, functionalized dimethacrylate polymer,
silane treated ceramic, silane treated silica, silane treated zirconium oxide
[N110837]
Bis-EMA, TEGDMA, silica nanoller [3044072]
Bis-GMA, UDMA, decamethylene dimethacrylate, barium glass, ytterbium
triuoride, highly dispersed silicon dioxide, mixed oxide and copolymer
[L36209]
Bis-GMA, TEGDMA, barium glass [010122]
DGDMA, di- and multifunctional acrylate and methacrylate resins,
strontium alumino sodium uoro phosphor silicate glass, highly dispersed
silicon dioxide, UV stabilizer, ethyl-4-dimethylaminobenzoate,
camphorquinone, butylated hydroxyl toluene, iron pigments, titanium
oxide [0808001149]
Application
Dispense a 1 mm increment and agitate to condition the
tooth for 20 s prior to light curing for 10 s; syringe
additional material in increments of 1.52 mm and light
cure each increment for 10 s.
Dispense a thin layer (<0.5 mm) on a forcefully dried
surface; use a provided applicator with a brushing motion
for 1520 s; light cure for 20 s; syringe additional material
in increments of less than 2 mm and light cure each
increment for 20 s.
Brush onto the surface for >30 s; disperse excess with a
strong stream of air; light cure for 10 s.
Brush onto the surface; massage for 15 s applying
d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
pressure; gentle stream of air to thoroughly dry to a thin
lm; apply a second coat without massage; gentle stream
of air to thoroughly dry to a thin lm; light cure for 10 s.
Application for 20 s with agitation; start with gentle air
blow, followed by a strong air blow for at least 5 s; light
cure for 20 s.
Apply adhesive twice; gently agitate for 20 s; carefully air
blow for 5 s; light cure for 20 s.
Etch for 15 s; rinse thoroughly for 15 s; gently air dry for
3 s; apply primer with light brushing motion for 15 s; air
dry for 5 s; apply adhesive with light brushing motion for
15 s; air thin for 3 s; light cure for 20 s.
Apply in layers of max 2 mm and light cure for 20 s.
Apply in layers of max 2 mm and polymerize for 20 s.
Apply in layers of max 2 mm and light cure for 20 s
(>500 mW/cm2 ) or 10 s (>1000 mW/cm2 ).
Apply in thin layers (max 2 mm, baseliner max 1 mm);
apply a gentle stream of air and light cure for 20 s.
Incremental placement in 2 mm layers or less;
polymerization for at least 20 s.
223
224 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230

Fig. 1 Schematic illustrating the study design.

were recorded as either cohesive in dentin, adhesive at the
interface with the self-adhesive owable composite or adhe-
sive, cohesive in the adhesive, adhesive at the interface
between the adhesive and owable composite, and cohe-
sive in the (self-adhesive) owable composite. Representative
specimens were selected for fractographic examination by
Feg-SEM (Philips XL30, Eindhoven, The Netherlands), and
processed appropriately, including xation in glutaraldehyde,
dehydration in ascending concentrations of ethanol, and
chemical drying following the protocol described in detail by
Perdigo et al. [22].
2.4. Statistical analysis
One-way analysis of variance (ANOVA) in SubProject 1 and
two-way ANOVA in SubProject 2, and Tukey HSD multiple
comparisons test (both subprojects) were used to determine
statistical differences in TBS. All data were analyzed at a
signicance level of 0.05 using a software package (R2.12, R
Foundation for Statistical Computing, Vienna, Austria).
dentin with phosphoric acid signicantly increased the TBS
of the SAC Vertise Flow (Kerr; p < 0.001).
Failure analysis in SubProject 1 predominantly revealed
adhesive failures at the interface of both the SACs when
they were bonded to BUR-CUT dentin, and even for Vertise
Flow (Kerr) when dentin was pre-etched with phosphoric acid
(Table 2). A clearly more non-adhesive failure pattern was
recorded for the 1-SEa/owC and 3-E&Ra/owC combinations.
The bonding effectiveness data of SubProject 2, in which
potential interference of a thick versus thin smear layer on
the bonding effectiveness to dentin and enamel was tested,
are shown in Tables 3 and 4, and Figs. 3 and 4 for dentin and
enamel, respectively.
When bonded to dentin (Table 3 and Fig. 3), the nature of
the smear layer had no effect on the bonding effectiveness

3. Results

The bonding effectiveness data of SubProject 1 are shown

in Table 2 and Fig. 2. A signicantly lower TBS to BUR-
CUT dentin was recorded for both SACs Fusio Liquid Dentin
(Pentron) and Vertise Flow (Kerr) than for the 1-SEa/owC
combinations Adper Prompt L-Pop/Filtek Supreme XT Flow-
able (3M ESPE; p = 0.04923 and p < 0.001, respectively) and Xeno
V/X-ow (Dentsply; p < 0.001), and the 3-E&Ra/owC combina-
tion OptiBond FL/Premise Flowable (Kerr; p < 0.001). The SAC
Fusio Liquid Dentin (Pentron) did not perform signicantly dif-
ferent from the 1-SEa/owC combination iBond/Venus ow
(Heraeus Kulzer; p = 0.20392) and scored signicantly bet-
ter than the 1-SEa/owC combination AdheSe One/Tetric
EvoFlow (Ivoclar Vivadent; p = 0.00583). The SAC Vertise Flow
(Kerr) revealed a signicantly lower TBS to BUR-CUT dentin
than the SAC Fusio Liquid Dentin (Pentron; p < 0.001) and all Fig. 2 Bonding effectiveness to BUR-CUT dentin. Means
other 1-SEa/owC combinations except for AdheSe One/Tetric with the same letter are not signicantly different (one-way
EvoFlow (Ivoclar Vivadent; p = 0.34286). Pre-etching BUR-CUT ANOVA and Tukey HSD multiple comparisons test, p < 0.05).
Table 2 Micro-tensile bond strength (TBS) and failure analysis for the adhesive materials bonded to (BUR-CUT) dentin (SubProject 1).
Adhesive material TBS (SD) ptf/n TBS (excl. ptf) Failure
(ptf = 0 MPa) mode

Cohesive Adhesive at interface Cohesive Adhesive at Cohesive in

in dentin with self-adhesive in adhesive interface between (self-adhesive)
owable composite or adhesive and owable
adhesive owable composite composite
SAC Fusio Liquid Dentin 17.7 (8.6) 0/30 17.7 1 88 11
Vertise Flow 1.8 (2.7) 16/24 5.4 0 94 6
H3 PO4 + Vertise Flow 18.7 (11.0) 2/30 20.0 1 71 28

1-SEa/owC AdheSe One/Tetric 7.9 (5.7) 3/26 9.0 2 0 85 9 4

EvoFlow
Adper Prompt 25.4 (10.0) 0/30 25.4 0 3 41 0 56
L-Pop/Filtek Supreme

d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
XT Flowable
iBond/Venus ow 23.9 (10.3) 1/31 24.7 4 29 0 33 34
Xeno V/X-Flow 29.4 (11.7) 0/30 29.4 6 2 0 2 90

3-E&Ra/owC OptiBond FL/Premise 44.8 (13.6) 0/20 44.8 33 7 12 0 48

Flowable
SD, standard deviation; ptf, pre-testing failures; n, number of specimens.

Table 3 Micro-tensile bond strength (TBS) and failure analysis for the adhesive materials bonded to BUR-CUT versus SiC-GROUND dentin (SubProject 2).
Adhesive material TBS (SD) ptf/n TBS (excl. Failure mode
(ptf = 0 MPa) ptf)

Cohesive Adhesive at interface Cohesive Adhesive at Cohesive in

in dentin with self-adhesive in adhesive interface between (self-adhesive)
owable composite or adhesive and owable
adhesive owable composite composite
BUR-CUT Fusio Liquid Dentin 17.7 (8.6) 0/30 17.7 1 88 11
Vertise Flow 1.8 (2.7) 16/24 5.4 0 94 6
Adper Prompt 25.4 (10.0) 0/30 25.4 0 3 41 0 56
L-Pop/Filtek Supreme
XT Flowable

SiC-GROUND Fusio Liquid Dentin 17.1 (9.5) 0/30 17.1 0 98 2

Vertise Flow 5.3 (6.7) 14/31 9.7 0 38 62
Adper Prompt 34.9 (13.4) 0/30 34.9 6 15 31 1 47
L-Pop/Filtek Supreme
XT Flowable
SD, standard deviation; ptf, pre-testing failures; n, number of specimens.

225
226 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230

(self-adhesive)
Cohesive in

composite
owable

0
13
27
17

3
20
15
4
Table 4 Micro-tensile bond strength (TBS) and failure analysis for the adhesive materials bonded to BUR-CUT versus SiC-GROUND enamel (SubProject 2).

owable composite
interface between
adhesive and
Adhesive at

0
Failure mode

in adhesive
Cohesive

0
Cohesive Adhesive at interface

Fig. 3 Bonding effectiveness to BUR-CUT versus

owable composite or
with self-adhesive

SiC-GROUND dentin. Means with the same letter are not

signicantly different (two-way ANOVA and Tukey HSD
adhesive

multiple comparisons test, p < 0.05).

96
87
31
38

97
80
6
74

of both SACs Fusio Liquid Dentin (Pentron) and Vertise Flow

(Kerr) (p = 0.99990 and p = 0.71722, respectively), while the 1-
SEa/owC (control) combination Adper Prompt L-Pop/Filtek
in dentin

Supreme XT Flowable (3M ESPE) bonded signicantly better

4
0
42
33

0
0
79
22

to SiC-GROUND dentin (p = 0.00134). The SAC Fusio Liquid

Dentin (Pentron) performed signicantly better to BUR-CUT
and SiC-GROUND dentin than Vertise Flow (p < 0.001 for both
TBS (excl.

conditions). Both SACs revealed a signicantly lower TBS to

ptf)

BUR-CUT (p = 0.01783 for Fusio Liquid Dentin; p < 0.001 for Ver-
13.0
11.0
23.1
28.0

10.8
15.3
22.6
25.5

tise Flow) and SiC-GROUND (p < 0.001 for both SACs) dentin
ptf/n

SD, standard deviation; ptf, pre-testing failures; n, number of specimens.

0/26
0/32
0/35
0/34

0/33
0/29
0/35
0/25
(ptf = 0 MPa)
TBS (SD)

13.0 (4.3)
11.0 (4.2)
23.1 (7.1)
28.0 (9.8)

10.8 (5.8)
15.3 (6.0)
22.6 (7.6)
25.5 (8.2)
Adhesive material

L-Pop/Filtek Supreme

L-Pop/Filtek Supreme
H3 PO4 + Vertise Flow

H3 PO4 + Vertise Flow

Fusio Liquid Dentin

Fusio Liquid Dentin

Adper Prompt

Adper Prompt
Vertise Flow

Vertise Flow
XT Flowable

XT Flowable
SiC-GROUND

Fig. 4 Bonding effectiveness to BUR-CUT versus

BUR-CUT

SiC-GROUND enamel. Means with the same letter are not

signicantly different (two-way ANOVA and Tukey HSD
multiple comparisons test, p < 0.05).
 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230 227

Fig. 5 Feg-SEM photomicrographs of fractured micro-specimens. (a) Feg-SEM of the fractured BUR-CUT dentin side of a
representative specimen prepared with Fusio Liquid Dentin (Pentron); I, interface. Arrow, osmosis droplets. (b) Feg-SEM of
the fractured BUR-CUT dentin side of a representative specimen prepared with Vertise Flow (Kerr). (c) Feg-SEM of the
fractured BUR-CUT dentin side of a representative specimen prepared with Adper Prompt L-Pop/Filtek Supreme XT
Flowable; Ar, adhesive resin; C, composite. (d) Feg-SEM of the fractured BUR-CUT dentin side of a representative specimen
prepared with Xeno V/X-ow (Dentsply).

than the 1-SEa/owC (control) combination Adper Prompt
L-Pop/Filtek Supreme XT Flowable (3M ESPE).
When bonded to enamel (Table 4 and Fig. 4), the nature of
the smear layer had no effect on the bonding effectiveness
for any of the adhesive materials tested. Both SACs did not
bond statistically different, irrespective of the nature of the
smear layer (p = 0.9312 for Fusio Liquid Dentin; p = 0.2312 for
Vertise Flow). Pre-etching enamel with phosphoric acid sig-
nicantly increased the TBS of the SAC Vertise Flow (Kerr)
to both BUR-CUT (p < 0.01) and SiC-GROUND enamel (p < 0.01),
of which the TBS was no longer signicantly different from
the respective bond of the 1-SEa/owC (control) combination
Adper Prompt L-Pop/Filtek Supreme XT Flowable (3M ESPE) to
BUR-CUT (p = 0.0665) and SiC-GROUND enamel (p = 0.7614).
Failure analysis in SubProject 2 predominantly revealed
adhesive failures at the interface of both the SACs when
they were bonded to both BUR-CUT and SiC-GROUND dentin
(Table 3). A clearly more non-adhesive failure pattern was
recorded for the 1-SEa/owC combination Adper Prompt L-
Pop/Filtek Supreme XT Flowable (3M ESPE), when bonded to
both BUR-CUT and SiC-GROUND dentin. When bonded to
BUR-CUT and SiC-GROUND enamel (Table 4), the predominant
failure pattern was adhesive at the interface for both SACs,
except when enamel was pre-etched with phosphoric acid.
A clearly more non-adhesive failure pattern was recorded
for the 1-SEa/owC combination Adper Prompt L-Pop/Filtek
Supreme XT Flowable (3M ESPE).
In general, Feg-SEM of the most representative failures
in each experimental group conrmed the failure patterns
observed using the optical microscope. Specic fracture char-
acteristics were observed and are illustrated in Fig. 5, namely
both the SACs failed predominantly at the interface and were
unable to remove the smear plugs out of the tubules.
4. Discussion
So far, no independent data are available regarding the TBS
of the recently developed composite technology claiming to
self-adhere to tooth tissue. With this study, we have tested
the bonding effectiveness of the today only two commercially
available self-adhesive owable composites.
Hypothesis 1, as tested in SubProject 1, that the TBS to
BUR-CUT dentin of the two owable SACs was alike that of
the 1-SEa/owC combinations, should be rejected. One could
expect, and even accept, that the very simple-to-use SACs,
228 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
applied without a separate adhesive, would bond less effec-
tively to dentin than when a owC would be bonded to dentin
using the multi-step gold-standard 3-E&Ra (OptiBond FL,
Kerr) [1,21]. However, in light of a potentially universal use as
a restorative material, one could argue that the bonding effec-
tiveness of a SAC should minimally meet that of a 1-SEa/owC
combination; this is the reason why we selected four such 1-
SEa/owC combinations in this study as references/controls.
While the SAC Vertise Flow (Kerr) underperformed three out
of the four 1-SEa/owC combinations, the other SAC Fusio Liq-
uid Dentin (Pentron) only underperformed two 1-SEa/owC
combinations, and was equally effective and even signicantly
more effective than the other two 1-SEa/owC combinations.
Self-evidently, for comparison we combined the 1-SEas with
the owable composite produced by the same manufacturer,
as the kind of composite (and the actual brand) is known to
signicantly inuence the TBS [23].
Differences in bonding effectiveness between the two
SACs tested can in principle be ascribed to many factors,
among which probably the actual composition and the kind
of functional monomer contained in the material formula-
tion might be most determining (Table 1). The SAC Fusio
Liquid Dentin (Pentron) contains the functional monomer
4-methacryloxyethyltrimetellitic acid (4-MET) that has been
attributed chemical bonding potential to hydroxyapatite (HAp)
and tooth tissue [24], the latter however signicantly less
strong than for instance 10-methacryloyloxydecyl dihydrogen
phosphate (10-MDP). The functional monomer used in Ver-
tise Flow (Kerr) is glycerol phosphate dimethacrylate (GPDM).
This monomer is also used in the 3-step etch-and-rinse adhe-
sive OptiBond FL (Kerr) that in laboratory as well as clinical
research has proven to belong among the currently top-
performing adhesives [21,23]. To our knowledge, no data on
chemical analytic data on the bonding potential of GPDM are
available. Recent interfacial analysis of its two-step successor
OptiBond XTR (Kerr) that also contains GPDM, nevertheless
revealed a 2-m deep hybrid layer free of HAp (unpublished
observations); following the AD-concept [25,26], this most
likely indicates that GPDM etches rather than bonds to
HAp. To achieve self-adhesiveness, we believe that a relatively
viscous (owable) composite should contain a functional
monomer that rather possesses an effective chemical bonding
potential, as it cannot penetrate deeply. To fully elucidate the
bonding mechanisms of both the SACs tested, further in-depth
chemical interfacial analysis is denitely needed to comple-
ment some interfacial ultra-structure data already available
(see below).
Besides compositional differences, the rheological proper-
ties of the two SACs tested differed completely, with Fusio
Liquid Dentin (Pentron) being signicantly more uid than
Vertise Flow (Kerr). This should in part be ascribed to the lower
ller content in range of 65 wt% for Fusio Liquid Dentin (Pen-
tron) versus 70 wt% for Vertise Flow (Kerr). In this respect,
Fusio Liquid Dentin (Pentron) was found to be placed more
easily onto the tooth surface; it showed less stickiness to the
application instrument, and wetted better both dentin and
enamel. Such apparent easier handling may at least in part
have contributed to the better bonding effectiveness of Fusio
Liquid Dentin (Pentron) versus that of Vertise Flow (Kerr).
This signicant difference in bonding effectiveness between
the two SACs tested appeared also from the number of pre-
testing failures recorded (see also below), being respectively
67% and 45% when Vertise Flow was bonded to BUR-CUT and
SiC-GROUND dentin, versus no pre-testing failures for Fusio
Liquid Dentin (Pentron). In this respect, it is also noteworthy
that no pre-testing failures were recorded for any of the SACs
when bonded to enamel (SubProject 2).
SubProject 2 conrmed the results obtained in SubPro-
ject 1. Hypothesis 2, as tested in SubProject 2, that the
nature of the smear layer did not affect the TBS of the SACs
to dentin and enamel, was accepted. Indeed, no difference
in bonding effectiveness to BUR-CUT versus SiC-GROUND
enamel and dentin was recorded, though one could have
expected that the SACs would have bonded better to the
latter thinner, more regular and less compact smear-layer
covered tooth substrates. Preliminary research characteriz-
ing the interface of the SAC Vertise Flow (Kerr) with enamel
and dentin using TEM revealed an interface with tiny micro-
tags formed at bur-cut enamel [27]. In addition, also a rather
supercial interaction was observed at dentin, where Vertise
Flow (Kerr) was observed not to have removed smear plugs
out of the tubules for BUR-CUT, nor for SiC-GROUND dentin
[27]. The predominantly adhesive failures at the interface
of the SAC with the tooth substrate conrm the relatively
supercial interaction achieved. This kind of supercial inter-
action should be regarded as very alike that documented
for self-adhesive luting composites [812], as well as that
reported for another experimental self-adhesive lling mate-
rial [28].
Pre-etching enamel and dentin signicantly improved the
bonding effectiveness of the SAC Vertise Flow (Kerr), by which
hypothesis 3 was rejected. This was expected when bond-
ing to enamel, since phosphoric acid signicantly enhances
the surface energy of enamel and thus provides signicantly
more micro-retention [1]. The nature of the smear layer did
of course not play a role, since phosphoric acid is strong
enough to dissolve and, upon rinsing, remove both the thicker
BUR-CUT as well as the thinner SiC-GROUND smear layer.
A similar improved bonding effectiveness following before-
hand phosphoric-acid etching was previously found when
a self-adhesive luting composite was bonded to enamel [8].
In addition, Rengo et al. [17] found that pre-etching enamel
had no inuence on micro-leakage. A benecial effect of
pre-etching dentin with phosphoric acid on the bonding
effectiveness of Vertise Flow (Kerr) was not so expected, as
previous bond-strength tests for the same above-mentioned
self-adhesive luting composite revealed the opposite and thus
detrimental effect [8]. In that study, TEM revealed that phos-
phoric acid clearly exposed collagen up to a few micrometers
depth. The relatively viscous luting composite could not ade-
quately hybridize the collagen mesh, the reason why the
signicant reduction in bonding effectiveness was measured
[8]. Likewise, Rengo et al. reported that pre-etching dentin sig-
nicantly affected the marginal sealing potential of Vertise
Flow (Kerr) [17]. Eventually, it remains to assess how good the
bond of SACs to enamel and dentin, even when beforehand
etched with phosphoric acid, will resist biodegradation on the
long term. One study evaluating Vertise Flow (Kerr) recently
revealed a remarkable decline in shear bond strength upon
aging [20].
 d e n t a l m a t e r i a l s 2 9 ( 2 0 1 3 ) 221230
Special measures were taken to reduce the incidence of
pre-testing failures (ptf). Using alginate, we provided support
to the thin slices after the rst cut (and before the second cut
perpendicular to the rst one). Nevertheless, a relatively high
proportion of the Vertise Flow (Kerr) specimens failed prior
to testing when bonded to dentin. Therefore, the respective
TBS-values should be interpreted with care (Tables 2 and 3).
In case of a pre-testing failure, a bond-strength value of 0 MPa
was assigned to the specimen. This actually penalized the SAC
too severely, as there was always a certain bond strength above
0 MPa. If the specimens that failed prior to testing would have
been excluded from the TBS calculation (rather than being
considered as 0 MPa), self-evidently a higher TBS would have
been recorded. However, statistically no new signicances
were revealed, as was also found before by Mine et al. [29].
Eventually, a high occurrence of ptfs in one experimental
group generally goes together with relatively low TBS values
for the remaining specimens that did not fail prior to testing.
Until now, only few in vitro studies on other mate-
rial parameters of self-adhesive composites were published.
Salerno et al. [13] concluded that Vertise Flow (Kerr) showed a
remarkably high elastic modulus and hardness, whereas Wei
et al. [14,15] revealed that Vertise Flow (Kerr) exhibited signif-
icant hygroscopic expansion and shrinkage during water ab-
and desorption. The higher matrix content of self-adhesive
owable composites, as compared to conventional restorative
composites, may contribute to this increased water-sorption,
and thus may possibly affect their long-term performance
[23]. As many studies have reported relationships between
ller/matrix content and major physico-mechanical proper-
ties of dental lling materials [3033], denitely more basic
material characterization of SACs is also needed.
Class-V clinical trials remain the ultimate test to evalu-
ate adhesives, and are especially useful for in vitro versus
in vivo comparison [34]. Regarding clinical performance of
self-adhesive composites, only one short-term clinical trial
was found in literature [35], while the paper was not listed
within PubMed. In this study, Class-I restorations placed using
Vertise Flow (Kerr) were followed up. As macro-retention can-
not be excluded to retain the SAC in a Class-I cavity, one can
however not claim to have clinically assessed the actual bond-
ing effectiveness. The authors concluded that Vertise Flow
(Kerr) remained clinically acceptable over the 6-month follow-
up period. As in that study besides a longer follow-up, also a
proper control (or gold standard) was missing and a paired-
tooth study design was not applied, more clinical trials are
to be run before conclusions on the clinical performance of
self-adhesive composites can be drawn [3638].
5. Conclusion
Self-adhesive composites are clinically attractive as they
would further simplify the way teeth can be adhesively
and thus minimal-invasively restored. This laboratory
bond-strength study revealed that so far currently only two
commercial SACs underperform. Consequently, routine clin-
ical application of SACs should be very carefully considered,
in particular in case no macro-retention is provided.
229
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