Odontology

https://doi.org/10.1007/s10266-017-0324-3

ORIGINAL ARTICLE

Bonding performance of self‑adhesive flowable composites to enamel,

dentin and a nano‑hybrid composite
Jana Peterson1 · Marta Rizk1 · Monika Hoch1 · Annette Wiegand1

Received: 6 February 2017 / Accepted: 6 September 2017

© The Society of The Nippon Dental University 2017

Abstract
This study aimed to analyze bond strengths of self-adhesive flowable composites on enamel, dentin and nano-hybrid com-
posite. Enamel, dentin and nano-hybrid composite (Venus Diamond, Heraeus Kulzer, Germany) specimens were prepared.
Three self-adhesive composites (Constic, DMG, Germany; Fusio Liquid Dentin, Pentron Clinical, USA; Vertise Flow,
Kerr Dental, Italy) or a conventional flowable composite (Venus Diamond Flow, Heraeus Kulzer, Germany, etch&rinse
technique) were applied to enamel and dentin. Nano-hybrid composite specimens were initially aged by thermal cycling
(5000 cycles, 5–55 °C). Surfaces were left untreated or pretreated by mechanical roughening, ­Al2O3 air abrasion or silica
coating/silanization. In half of the composite specimens, an adhesive (Optibond FL, Kerr Dental, Italy) was used prior to
the application of the flowable composites. Following thermal cycling (5000 cycles, 5–55 °C) of all specimens, shear bond
strengths (SBS) and failure modes were analyzed (each subgroup n = 16). Statistical analysis was performed by ANOVAs/
Bonferroni post hoc tests, Weibull statistics and χ2-tests (p < 0.05). SBS (MPa) of the self-adhesive composites on enamel
and dentin were significantly lower (enamel: < 5, dentin: < 3) than those of the conventional flowable composite (enamel:
13.0 ± 5.1, dentin: 11.2 ± 6.3), and merely adhesive failures could be observed. On the nano-hybrid composite, SBS were
significantly related to the pretreatment. Adhesive application improved SBS of the conventional, but not of the self-adhesive
composites. The self-adhesive composite groups showed less cohesive failures than the reference group; the occurence of
cohesive failures increased after surface pretreatment. Bonding of self-adhesive flowable composites to enamel and dentin
is lower than bonding to a nano-hybrid composite.

Keywords  Self-adhesive flowable composite · Composite repair · Self-adhering composite · Bond strength · Repair
restoration

Introduction or self-adhesive monomers that are able to etch enamel and

Dental composites usually require a separate conditioning
step with an adhesive system to allow for bonding on dental
hard tissues. As this conditioning step might be time-con-
suming and technique-sensitive [1–4], not only self-adhesive
composite cements as luting materials for indirect restora-
tions and post systems, but also self-adhesive composites
for direct filling techniques have been developed over the
past years [5, 6]. These materials contain self-etching and/
* Jana Peterson
jana.peterson@med.uni‑goettingen.de
1
Department of Preventive Dentistry, Periodontology
and Cariology, University of Goettingen, Robert‑Koch‑Str.
40, 37075 Göttingen, Germany
dentin surfaces or chemically bond to hydroxyapatite [7].
Although several manufacturers already offer self-adhe-
sive composites for clinical use, only few studies on their
bond strengths are available. Immediately after applica-
tion, self-adhesive composites already show lower bond
strengths than conventional composites that were applied
with a bonding system in etch&rinse- or self-etch-technique
[8–11]. So far, there are limited data available on how aging
processes and degradation in the oral cavity may affect bond
strengths of self-adhesive composites over time [6]. Further-
more, no information can be found about the application of
self-adhesive composites as a repair material for defective
restorations.
Regarding minimally invasive dentistry, the repair of
dental restorations rather than their total replacement has
gained acceptance on a broad basis [12]. This approach

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 Odontology
leads to less removal of sound tooth structure, and might be
more cost-effective than performing a total replacement of a
merely partially defective restoration [13–15]. Nevertheless,
repairing defective direct or indirect restorations also makes
a conditioning of the repair surface (e.g., roughening or sil-
ica coating, silanization and/or the application of a bonding
system) necessary [16]. This leads to the question whether
self-adhesive composites accomplish a more simplified and
less technique sensitive repair procedure.
Therefore, the objective of this study was to analyze the
bonding performance of different self-adhesive flowable
composites to enamel, dentin and a nano-hybrid composite
after aging. The null hypothesis tested is that shear bond
strengths of self-adhesive flowable composites to enamel,
dentin and a nano-hybrid composite do not differ signifi-
cantly from a bonded conventional flowable composite.
Materials and methods
Three self-adhesive flowable composites and one conven-
tional flowable composite were examined in this study.
Table 1 lists their brand and manufacturer’s names, compo-
sition, and application instructions.
Tooth specimen preparation
The crowns of extracted caries-free human permanent
molars (collection of human teeth approved by local ethic
committee, No: 27/8/13) were embedded in resin and ground
parallel to the buccal surface under water-cooling (silicon
carbide paper P500, Hermes Schleifmittel GmbH, Ger-
many; cutting wheel Roto-Pol34, Struers, Germany) until
a flat enamel or dentin surface, respectively, was obtained.
In total, N = 64 enamel specimens and N = 64 dentin speci-
mens were prepared (each subgroup: n = 16). A customized
holding device was used to fix a transparent acrylic cylinder
(inner diameter: 3 mm; height: 4 mm) vertically on the flat
surface. Following manufacturers’ instructions (Table 1),
the self-adhesive composites were applied into the cylin-
der, not exceeding a maximum filling level of 2 mm. Light
curing (BA OPTIMA 10, B.A. International, Germany,
intensity > 800 mW/cm2, LED curing light) of the flow-
able composites was performed according to the manufac-
turers’ recommendations (Table 1) at 4 mm distance from
the surface of the flowables. The acrylic cylinders were not
removed.
Prior to the fixation and placement of the flowable com-
posite, an etch&rinse adhesive (Optibond FL, Kerr Dental,
Italy) was applied to either enamel or dentin surfaces in
the reference group. Application followed manufacturer’s
instructions: 30 s enamel etching with 35% ­H3PO4 (Ultra-
Etch, Ultradent Products Inc., USA), 15 s dentin etching
13
with 35% ­H3PO4 (Ultra-Etch, Ultradent Products Inc., USA),
primer application for 15 s, air drying for 5 s; adhesive appli-
cation for 15 s, air drying for 3 s, and light curing for 20 s.
All specimens were submitted to thermal cycling (5000
cycles, 5–55 °C, WILLYTEC THERMOCYCLER V 2.9,
Gebrüder Haake GmbH, Germany) as an artificial aging
procedure and subsequently stored in water for about 1 h
before shear bond strength was tested and fracture modes
were analyzed.
Nano‑hybrid composite specimen preparation
Increments of the nano-hybrid composite (Venus Diamond
A3, Heraeus Kulzer, Germany) were placed into a metal
ring (inner diameter: 6 mm, height 3 mm) positioned on a
glass plate. The composite was applied in increment tech-
nique; each increment was light cured at a distance of 10 mm
for 20 s. Then, the specimens’ surfaces were polished with
water-cooled silicon carbide paper (P800–P1200–P4000,
Hermes Schleifmittel GmbH, Germany; cutting wheel Roto-
Pol34, Struers, Germany) to achieve a flat surface. All speci-
mens (N = 512) were submitted to an initial thermal cycling
(5000 cycles, 5–55 °C) as an artificial aging procedure. Sim-
ulating various surface treatments prior to restoration repair,
the specimens were randomly assigned to four groups:
1. Mechanical roughening simulating bur abrasion. Speci-
mens were ground under water-cooling (silicon carbide
paper P500), rinsed with water and then air dried.
2. Al 2O 3 (Airsonic Aluminium-Oxyd Pulver 50  µm,
HAGER WERKEN, Germany) air abrasion using a
sandblasting unit (CoJet™Prep, 3M Espe, Germany;
15 s, 2.8 bar) at a distance of 10 mm in an angle of 45°.
­Al2O3 remnants were air blown.
3. Silica coating/silanization. The surfaces were silica
coated (CoJet™Sand Blast Coating Agent 30 µm, 3M
Espe, Germany; 15 s, 2.8 bar) using a sandblasting unit
at a 10 mm distance in an angle of 45°. Particle remnants
were air blown. The silane coupling agent (Espe™ Sil,
3M Espe, Germany) was applied following manufac-
turer’s instructions and then air dried.
4. After air drying of the specimens no further treatment
was performed.
Prior to the application of the flowable composites,
the surfaces of half of the specimens were treated with an
etch&rinse adhesive (Optibond FL, Prime and Adhesive,
Kerr Dental, Italy) or left untreated. A customized holding
device was used to fix a transparent acrylic cylinder (inner
diameter: 3 mm; height 4 mm) vertically on the flat surface.
The flowable composites were filled into the acrylic cylinder
up to a maximum level of 2 mm. Light curing was performed
as recommended by the manufacturer at a distance of 4 mm
 Odontology

Table 1  Composition and application of the flowable composites following manufacturer’s instructions

Material and manufacturer Matrix components Filler type and -diameter Filler load Application

Self-adhesive flowable com-
posite
Flowable composite
Nano-hybrid composite
Constic, DMG Bis-GMA, EBADMA, UDMA,
HEMA, TEGDMA, HDMA,
MDP
Fusio Liquid Dentin, Pentron UDMA, TEGDMA, HEMA,
Clinical 4-META
Vertise Flow, Kerr Dental GPDM, HEMA, MeHQ
Venus Diamond Flow, Heraeus Bis-GMA, TEGDMA, UDMA,
Kulzer EBADMA
Venus Diamond, Heraeus Kulzer TCD-Di-HEA, UDMA
Ba-glass
0.02–2.3 µm
amorphous silicon nanosized,
silanized Ba-glass, 1.2 µm
particle size in average
prepolymerized particles, Ba-
glass, ­SiO2, ­YbF3, ZnO
1 µm particle size in average
Ba–Al-Fl-Si-glass, ­YbF3, ­SiO2
20 nm–5 µm
Ba–Al-F-glass, ­YbF3, ­SiO2
1.8 µm particle size in average
38% by volume Brush in a thin layer (< 0.5 mm)
65% by weight of Constic for 20 s and light cure
for 20 s. Then apply Constic
with a Luerlock-Tip in layers not
exceeding 2 mm. Light cure each
layer for 20 s
52% by volume Brush in a thin layer (< 0.5 mm)
65% by weight of Fusio Liquid Dentin for 20 s
and light cure for 10 s. Then
apply Fusio Liquid Dentin with
a Luerlock-Tip in layers not
exceeding 2 mm. Light cure
each layer for 10 s, the final layer
for 20 s.
70% by weight Brush in a thin layer (< 0.5 mm)
of Vertise Flow for 20 s and light
cure for 20 s. Then apply Vertise
Flow with a Luerlock-Tip in lay-
ers not exceeding 2 mm. Light
cure each layer for 20 s
41% by volume Apply Venus Diamond Flow in
65% by weight layers not exceeding 2 mm and
light cure each layer for 20 s.
64% by volume Apply and adapt thoroughly in
82% by weight increments not exceeding 2 mm.
Light cure each increment for
20 s

Functional monomers of the self-adhesive composites are highlighted

Bis-GMA bisphenol A dimethacrylate, EBADMA ethoxylated bisphenol A dimethacrylate, GPDM glycerol phosphate dimethacrylate, HDMA 1,6-hexanediol dimethacrylate, HEMA hydrox-
yethyl methacrylate, MDP 10-methacryloyloxydecyl dihydrogen phosphate, MeHQ hydrochinon monoethyl ether, TCD-Di-HEA 2-propen acid, (octahydro-4,7 methano-1h indene-5-diyl)
bis(methylene minocarbonyloxy-2,1-ethanediyl)ester; TEGDMA triethylen glycol dimethacrylate, UDMA urethane dimethacrylate, 4-META 4-methacryloxyethyl trimellitic acid

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 Odontology
from the surface of the flowable composites. The acrylic
cylinders were not removed. For all subgroups, n = 16 speci-
mens were obtained.
All specimens were aged with an additional thermal
cycling procedure (5000 cycles, 5–55 °C) and subsequently
stored in water for about 1 h before shear bond strength was
tested and fracture modes were analyzed (Fig. 1).
Shear bond strength and failure mode analysis
Shear bond strength was tested with a universal testing
machine (Materialprüfmaschine 1446, Zwick GmbH & Co.
KG, Germany). A chisel-shaped loading device applied
shear force vertically to the adhesive interface at a speed of
1 mm/min. Force applied at debonding was recorded (Soft-
ware: testXpert V12.1, Zwick GmbH & Co. KG, Germany)
and shear bond strength was determined.
For failure mode analysis, all debonded surfaces were
microscopically examined with a stereomicroscope (Stemi
SV 11, Zeiss, Germany) at 1.6× magnification. Failures
were assessed as cohesive (failure occurred solely within
the specimen’s base: enamel, dentin, or nano-hybrid com-
posite; or within one of the flowable composites), as adhe-
sive (fracture occurred at the interface between base and
Fig. 1  Preparation of the nano-
hybrid composite specimen
Mechan.
roughening
Etch&Rinse adhesive Optibond FL
Constic
n = 16
13
flowable composite) or mixed (shares of cohesive as well as
adhesive failures).
Statistical analysis
Shear bond strength data were tested for normal distribu-
tion using Quantil–Quantil plots. 80% of the subgroups were
found to be normally distributed; thus for further statistical
evaluation, normal distribution was assumed for all data.
Shear bond strengths on enamel and dentin were each
statistically analyzed with one-way ANOVAs followed by
Bonferroni post hoc tests (p < 0.05). Shear bond strengths
on the nano-hybrid composite were analyzed using three-
way ANOVA (factors: surface pretreatment, adhesive and
flowable composite) followed by Bonferroni post hoc tests
(p < 0.05). Significant differences between the surface pre-
treatments, the surface conditioning with or without adhe-
sive and the flowable composites were separately analyzed
by one-way ANOVAs. Additionally, Weibull distribution
parameters (Weibull modulus m, characteristic strength o′0 )
were calculated using the maximum likelihood estimation
method at 95% confidence level.
Differences in the distribution of failure modes between
the subgroups were evaluated using χ2-test (p < 0.05).
Nano-hybrid composite Venus Diamond
N = 512
Thermal cycling (5000 cycles, 5-55°C)
Al2O3 Silica coating/
-
Sandblasting Silanization
-
Fusio Liquid Venus Diamond
Vertise Flow Flow
Dentin
n = 16 (reference group)
n = 16
n = 16
Thermal cycling (5000 cycles, 5-55°C)
Shear bond strength analysis
Fracture mode analysis
Odontology

The statistical analysis was performed with Statistica presented in Table  2. The self-adhesive composites all
(version 12, StatSoft, USA). obtained a similar Weibull modulus on enamel and den-
tin. Their characteristic strengths ranged between 1.4 and
3.9 MPa on enamel and 0.3 and 2.4 MPa on dentin. Com-
Results pared to the self-adhesive composites, the reference group
reached higher Weibull moduli (enamel: 2.8; dentin: 1.9)
Shear bond strength (MPa) of the self-adhesive compos- and characteristic strengths (enamel: 14.6  MPa; dentin
ites on enamel and dentin was significantly lower than 12.6 MPa).
that of Venus Diamond Flow (enamel: 13.0 ± 5.1, dentin: Bond strength to the nano-hybrid composite (Table 3) was
11.2  ±  6.3), whereas no significant difference between significantly related to the kind of pretreatment, the use of
enamel and dentin was detected (Fig. 2). an adhesive and the kind of flowable composite. All interac-
The Weibull parameters and their 95% confidence inter- tions were also found to be significant (three-way ANOVA).
vals of the flowable composites on enamel and dentin are One-way ANOVAs revealed significant differences between

Fig. 2  Shear bond strengths Constic Fusio Liquid Dentin Vertise Flow Venus Diamond Flow (reference group)
20
of the flowable composites on
enamel and dentin. Significant
b
differences between the differ- b
Shear bond strength (MPa)

ent flowable composites within 15

one substrate are marked by
different small letters

10

a a

5 a
a

a
a
0
enamel dentin

Table 2  Weibull parameters Weibull modulus m (95% CI) characteristic strength o′0 (95% CI)
(95% confidence intervals) of
the flowable composites on Enamel Dentin Enamel Dentin
enamel and dentin
Constic 0.8 (0.5; 1.2) 0.7 (0.5; 1.0) 3.9 (2.0; 7.5) 0.3 (0.2; 0.7)
Fusio Liquid Dentin 0.7 (0.5; 1.0) 0.8 (0.5; 1.2) 2.5 (1.2; 5.1) 2.4 (1.3; 4.6)
Vertise Flow 0.7 (0.5; 1.0) 0.7 (0.5; 1.0) 1.4 (0.7; 3.1) 0.7 (0.3; 1.5)
Venus Diamond Flow 2.8 (1.9; 4.2) 1.9 (1.3; 2.8) 14.6 (12.2; 17.5) 12.6 (9.6; 16.6)
(reference group)

Table 3  Shear bond strengths (MPa, mean ± standard deviation) of the flowable composites on nano-hybrid composite depending on the differ-
ent surface treatments and the application of the bonding system Optibond FL
Mechanical roughening Al2O3 air abrasion Silica coating/silanization No treatment

Optibond FL No bonding Optibond FL no bonding Optibond FL No bonding Optibond FL No bonding

Constic 12.7 ± 2.7a/B 10.9 ± 3.9ab/AB 11.7 ± 3.0a/AB 10.4 ± 2.1ab/AB 10.3 ± 3.8a/AB 13.5 ± 3.6a/B 10.0 ± 4.3ab/AB 5.6 ± 3.4a/A

Fusio Liquid 19.9 ± 6.4b/BC 14.7 ± 6.2b/B 15.1 ± 2.7a/B 18.8 ± 5.2c/BC 19.8 ± 5.3bc/BC 21.7 ± 7.4b/C 15.9 ± 5.5b/BC 6.4 ± 4.1a/A
Dentin
Vertise Flow 12.0 ± 3.0a/AB 6.5 ± 6.2ab/AB 14.2 ± 3.3a/B 10.0 ± 3.3a/AB 14.4 ± 4.1ab/B 12.2 ± 3.9a/AB 9.1 ± 2.4a/AB 6.5 ± 4.0a/A
ab/CD a/AB a/CD bc/CD b/CDE b/E ab/BC
Venus Diamond 16.4 ± 7.4 5.9 ± 3.3 17.3 ± 5.1 16.6 ± 4.5 21.3 ± 3.1 24.4 ± 2.8 11.0 ± 5.7 0.3 ± 0.6a/A
Flow (reference
group)

Within one column, significant differences between the flowable composites are marked with different small letters. Within one line, significant
differences between the different pretreatments are marked with different capital letters

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the kind of pretreatment (silica coating/silanization > Al2O3
air abrasion = mechanical roughening > no treatment), the
use of an adhesive (Optibond FL > no adhesive) and the
kind of flowable composite (Fusio Liquid Dentin > Venus
Diamond Flow > Constic = Vertise Flow). Considering
the results of the Bonferroni post hoc tests, the shear bond
strength of the conventional composite but not of the self-
adhesive flowable composites was improved by application
of the adhesive system.
Table 4 presents the Weibull parameters and their 95%
confidence intervals of the flowable composites on nano-
hybrid composite. The Weibull modulus ranged from 1.3
to 5.9 for the self-adhesive composites and up to 9.7 for the
reference group. All flowable composites reached a higher
characteristic strength when a mechanical pretreatment of
the repair surface was performed compared to an untreated
repair surface. The self-adhesive composites reached char-
acteristic repair strengths from 6.3 to 24.3 MPa, whereas
Venus Diamond Flow was able to attain characteristic repair
strengths values up to 25.7 MPa.
On both tooth- and composite specimens, the distribu-
tion of failure modes differed significantly. For enamel and
dentin, cohesive failure modes could merely be observed
for the conventional flowable composite, but not in any of
the self-adhesive composite groups (Table 5). Considering
the nano-hybrid composite, the majority of cohesive failure
modes were detected for the conventional flowable compos-
ite. For all groups, less adhesive failures were found when
surface pretreatment was conducted or an adhesive system
was applied prior to the application of the flowable com-
posite (Table 6).
Discussion
For this study, we analyzed shear bond strengths of all self-
adhesive composites that are currently commercially avail-
able as direct filling materials. Interpreting our results, the
null hypothesis that shear bond strengths of self-adhesive
flowable composites to enamel, dentin and a nano-hybrid
composite do not differ significantly from a conventional
flowable composite has to be rejected.
Self-adhesive flowable composites differ concerning
their composition and feature varying functional monomers.
Fusio Liquid Dentin chemically bonds to hydroxyapatite
using 4-methacryloxyethyl trimetellitic acid (4-META)
which is able to partially demineralize dentin and to form
ionic bonds between its carboxylate groups and the calcium

Table 4  Weibull parameters (95% confidence intervals): Weibull modulus m and characteristic strength o′0 (MPa) of the flowable composites on
nano-hybrid composite
Mechanical roughening Al2O3 air abrasion Silica coating/silanization No treatment
Optibond FL No bonding Optibond FL No bonding Optibond FL No bonding Optibond FL No bonding

Constic
 m 5.0 (3.5; 7.3) 3.1 (2.1; 4.5) 4.5 (3.0; 6.8) 5.8 (4.0; 8.5) 2.9 (2.0; 4.1) 4.1 (2.8; 5.9) 2.5 (1.7; 3.7) 1.8 (1.2; 2.5)
 o′0 13.8 (12.5; 15.3) 12.2 (10.3; 14.5) 12.9 (11.4; 14.5) 11.2 (10.2; 12.2) 11.5 (9.6; 13.9) 14.9 (13.1; 16.9) 11.3 (9.2; 13.9) 6.3 (4.7; 8.4)
Fusio Liquid Dentin
 m 3.4 (2.3; 5.0) 1.3 (0.8; 2.1) 5.9 (4.1; 8.6) 3.8 (2.6; 5.3) 4.2 (2.8; 6.2) 3.2 (2.2; 4.8) 3.2 (2.2; 4.6) 1.7 (1.2; 2.4)
 o′0 22.2 (19.1; 28.8) 15.2 (20.4; 22.1) 16.2 (14.8; 17.8) 20.8 (18.1; 23.9) 21.8 (19.3; 24.7) 24.3 (20.6; 28.7) 17.8 (15.1; 21.0) 7.3 (5.4; 9.8)
Vertise Flow
 m 4.2 (2.9; 6.1) 2.3 (1.6; 3.2) 4.9 (3.3; 7.3) 3.3 (2.2; 4.9) 3.8 (2.6; 5.5) 3.1 (2.2; 4.4) 4.3 (3.0; 6.3) 1.7 (1.1; 2.5)
 o′0 13.2 (11.6; 14.9) 13.0 (10.3; 16.3) 15.5 (13.9; 17.2) 11.0 (9.5; 12.9) 15.9 (13.9; 18.3) 13.6 (11.5; 16.0) 10.0 (8.9; 11.3) 7.3 (5.4; 9.9)
Venus Diamond Flow (reference group)
 m 2.3 (1.6; 3.6) 1.9 (1.3; 2.8) 4.2 (2.8; 6.3) 4.7 (3.1; 7.1) 7.3 (5.0; 10.6) 9.7 (6.6; 14.3) 2.0 (1.4; 3.0) 0.8 (0.6; 1.2)
′ 18.6 (15.0; 22.9) 6.7 (5.1; 8.8) 19.0 (16.8; 21.5) 18.2 (16.3; 20.3) 22.5 (21.0; 24.2) 25.7 (24.3; 27.1) 12.5 (9.7; 16.1) 0.3 (9.7; 16.1)
 o0

Table 5  Failure modes (%) of Enamel Dentin

the flowable composites on
tooth surface Cohesive Adhesive Mixed Cohesive Adhesive Mixed

Constic 0 81 19 0 81 19
Fusio Liquid Dentin 0 38 62 0 100 0
Vertise Flow 0 69 31 0 69 31
Venus Diamond Flow 31 6 63 6 19 75
(reference group)

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Odontology

Table 6  Failure modes (%) Surface treatment Bonding Failure mode

of the flowable composites
on nano-hybrid composite Cohesive Adhesive Mixed
depending on the different
surface treatments and the Constic Mechanical roughening + 0 13 88
application of the bonding − 0 69 31
system Optibond FL Al2O3 air abrasion + 27 0 73
− 6 13 81
Silica coating/silanization + 19 0 81
− 25 0 75
– + 6 19 75
− 0 94 6
Fusio Liquid Dentin Mechanical roughening + 44 0 56
− 0 38 63
Al2O3 air abrasion + 75 0 25
− 56 0 44
Silica coating/silanization + 75 0 25
− 73 0 27
– + 6 13 81
− 0 94 6
Vertise Flow Mechanical roughening + 0 0 100
− 0 31 69
Al2O3 air abrasion + 47 0 53
− 0 6 94
Silica coating/silanization + 31 0 69
− 13 0 88
– + 0 44 56
− 0 56 44
Venus Diamond Flow Mechanical roughening + 31 19 50
(reference group) − 0 100 0
Al2O3 air abrasion + 88 0 13
13 44 44
Silica coating/silanization + 63 0 38
− 56 6 38
– + 44 6 50
− 0 100 0

in hydroxyapatite [17]. Vertise Flow contains glycerol phos-
phate dimethacrylate (GPDM) monomers which are well
known from the adhesive system Optibond FL. GPDM fea-
tures a rather short spacer chain and a high hydrophilic-
ity that results in a strong etching effect and a better den-
tin wettability but also a relatively low chemical bonding
potential to hydroxyapatite compared to other self-adhesive
monomers [18]. Constic contains 10-methacryloyloxydecyl
dihydrogen phosphate (MDP) monomer that holds longer
and more hydrophobic spacer chains compared to the GPDM
monomer. MDP was found to form stable 10-MDP-Ca salts
which lead to a strong chemical bonding with hydroxyapatite
[18]. Probably due to the different compositions and differ-
ent functional monomers, the dental hard tissue interaction
of self-adhesive composites was found to be significantly
different [6]. In enamel, adhesive tags were verifiable with
an experimental self-adhesive composite (DMG) and Vertise
Flow, but irregularly with Fusio Liquid Dentin. In dentin,
tags were detectable with all systems, but Fusio Liquid Den-
tin and Vertise Flow resulted in thin and sparse tags com-
pared to the experimental material, where tags were partially
branched [6]. Not only when measured immediately after
application [7, 8, 10, 19, 20], but especially after aging [6,
9, 11], self-adhesive composites present significantly lower
bond strengths than conventional composites that were
applied with a bonding system in etch&rinse- or self-etch-
technique. In particular, the dental hard tissue interaction
is limited, when aprismatic enamel or dentin covered with
smear layer is present [21].
Interestingly, bond strengths of the different self-adhesive
systems after thermal cycling were not different in the pre-
sent study and in the study by Brueckner et al. [6], although

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 Odontology
the interaction with dental hard tissues varied distinctly.
Generally, flowable materials present higher water absorp-
tion than materials containing a higher filler load. Compared
to conventional composites, the hydrophilic monomers of
the self-adhesive materials have an even higher tendency of
water absorption, which leads to swelling of the matrix and
breaking of polymer chains [22]. Those interactions might
weaken the mechanical properties of the self-adhesive com-
posites, resulting in significantly reduced bond strength after
thermal cycling [6]. Wei et al. [23] noted visible cracks in
their Vertise Flow specimens after only 24 h of water expo-
sure and assumed that Vertise Flow presents a weaker bond
between filler and monomers in the composite matrix. As a
consequence, an increased filler loss and degradation when
exposed to water might be observed. Potential differences
among the materials regarding immediate bond strength
might, therefore, be covered by the distinct effects of aging.
Clinically, already 66% of class V restorations from a self-
adhesive flowable composite were unacceptable or lost after
only 6 months [24].
Considering the low bond strengths to enamel and dentin,
repair bond strength data were significantly higher, depend-
ing on the kind of surface pretreatment. As found in other
studies [25, 26], silica coating followed by silanization led
to the highest repair bond strength values. Silica coating
not only increases the repair surface area but also provides
additional retention by deposition of silica particles [27].
Silane application increases wettability and forms covalent
bonds with the hydroxyl groups of the silica particles on the
repair surface as well as with the methacrylate groups of the
repair composite [27]. The specimens that were sandblasted
with ­Al2O3 reached similar repair bond strengths than the
group in which diamond bur abrasion was simulated. Pre-
vious studies showed conflicting results with either simu-
lated diamond bur abrasion [28] or A ­ l2O3 sandblasting [25]
presenting higher repair bond strength. After sandblasting,
some alumina particles might remain attached to the surface
even after air blowing, which might affect adhesion between
different materials [29, 30]. However, several studies found
that sandblasting with ­Al2O3 is highly beneficial for repair
restorations, since it was shown to remove surface contami-
nation, exposes filler particles available for silanization and
increases surface roughness for mechanical retention [25,
27, 31].
Confirming previous studies [16, 31], mechanical con-
ditioning of the composite surfaces and the application of
adhesive improved repair bond strengths of Venus Diamond
Flow. While any kind of mechanical surface conditioning
was able to improve the bond strengths of the self-adhesive
flowables, additional application of Optibond FL showed
no further effect. The self-adhesive flowable composites
possibly were able to reach a higher wetting degree of the
mechanically pretreated composite surface than Venus
13
Diamond Flow. Therefore, the reference group profits from
the application of a low viscosity bonding system to obtain
improved shear bond strengths. Overall, repair bond strength
values of Fusio Liquid Dentin were higher than in all other
groups. During application, Fusio Liquid Dentin showed a
lower viscosity and consequently a better wettability than
the other self-adhesive composites.
As for all materials that rely on light polymerization,
shear bond strengths of both tooth and composite speci-
mens may have been affected by the curing light. The irra-
diance of light curing units can be highly inhomogeneous
leading to uneven polymerization within the composite and,
thus, reduced mechanical properties [32]. Therefore, in the
present study, light curing conditions were standardized to
minimize this effect.
So far only limited independent data on self-adhesive
composites are available. Mostly, in vitro studies with bond
strength testing immediately after composite application
were performed. Our study is one of the few [6, 9, 11] that
considers aging processes in the testing procedure. Never-
theless, transferring the results to clinical application should
be done with care [33]. A multitude of factors such as the
chemical and physical interactions in the oral cavity is not
considered. Nevertheless, some authors state a correlation
between bonding results in vitro with bonding effectiveness
in vivo [34, 35].
Weibull parameters were included in the statistical
analysis as they provide information about the variability
of results. A low Weibull modulus reflects a high variabil-
ity of bond strengths and, therefore, a low reliability on the
characteristic bond strength. Materials that obtain a higher
Weibull modulus should be favored over those with a low
Weibull modulus because they are likely to be less technique
sensitive [36].
Considering the low bonding results on enamel and
dentin in vitro [6–11, 19, 20], it is questionable whether
further clinical studies will lead to more promising results.
However, the approach of using self-adhesive composites
as repair material for small composite repairs should be
investigated further. Next to their bond strengths, also the
evaluation of the sealing ability of self-adhesive composites
on repair surfaces is important. A closer examination of the
interface between self-adhesive composite and repair surface
could lead to a better understanding of physical, chemical
and mechanical interactions and might help to improve the
bonding ability of those materials. Also the repairing poten-
tial of self-adhesive composites on different materials, such
as metal or ceramic, could be interesting.
In conclusion, it can be stated that within the limitations
of this in vitro study, self-adhesive composites presented
low bond strengths on enamel and dentin and, therefore,
cannot be recommended as direct filling material. As self-
adhesive composites showed better bonding performance
Odontology
on nano-hybrid composite than on hard tooth tissue, they
may possibly be used for small repairs within a composite
restoration.
Acknowledgements  The authors thank DMG, Heraeus Kulzer, Kerr
Dental and Pentron Clinical for providing the composite materials.
Statistical analysis was reviewed by Dr. Andreas Leha, Department of
Medical Statistics, University Goettingen.
Compliance with ethical standards  hydroxyapatite using XPS. Dent Mater J. 2006;25:645–9.
Conflict of interest  The authors declare that they have no conflict of
interest.
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