Dental Materials Journal 2018; 37(5): 717–724

Surface properties and color stability of dental flowable composites influenced

by simulated toothbrushing
Guangyun LAI1,2, Liya ZHAO3, Jun WANG1,2 and Karl-Heinz KUNZELMANN3

1
Department of Pediatric Dentistry, Ninth People’s Hospital, Shanghai Jiao Tong University School of Medicine, 639 Zhizaoju Road, Shanghai
200011, China
2
Shanghai Key Laboratory of Stomatology & Shanghai Research Institute of Stomatology; National Clinical Research Center of Stomatology, 639
Zhizaoju Road, Shanghai 200011, China
3
Department of Operative Dentistry, Periodontology and Pedodontics, Ludwig-Maximilians-University of Munich, Goethestr. 70, 80336, Munich,
Germany
Corresponding author, Jun WANG; E-mail: junwang0203@[Link]

This study evaluated surface gloss, roughness and color change of six current flowable composites after simulated toothbrushing,
including four traditional flowable composites (i.e. GrandioSO Flow, Arabesk Flow, Kerr Revolution Formula 2 and Gradia Direct
LoFlo), one self-adhering flowable composite (Kerr Vertise Flow) and one universal injectable composite (G-ænial Universal Flo).
Forty-eight dimensionally standardized specimens (n=8/group) were made from six composites. Before and after 1 h toothbrushing
simulation, surface gloss was measured with a glossmeter, and surface roughness was evaluated with a profilometer, and color
was measured with a spectrophotometer. In this study, G-ænial Universal Flo, termed as universal injectable composite by the
manufacturer, presented excellent surface properties after toothbrush abrasion; Gradia Direct LoFlo showed excellent color stablity
after toothbrush abrasion; color alteration of composites caused by toothbrush abrasion was acceptable on the premise that 3.3∆E
units were considered as acceptable threshold values.

Keywords: Toothbrush, Gloss, Roughness, Composite, Color

as well8,15). The color of an object depends on its surface

INTRODUCTION
spectral reflectance, which is a sensitive function of
Resin composites are now the most preferred its roughness16,17). It is reported that the rougher of
materials for both anterior and posterior direct dental composite resin surface, the higher chance of staining
restorations1,2). Since the introduction of dental and discoloration, which can affect the restoration’s
composites in the early 1960s, various changes, including aesthetics18).
the developments and advances in the field of filler For any restoration placed on a tooth, the surface
technology, have been made3). Reduction of filler volume should maintain smooth and shiny, and should have
realized the invention of flowable composites with lower color constancy during a long time use. In the oral cavity,
viscosity4). Despite being developed for class V cavities however, composite restorations may deteriorate due to
initally, flowable composites are widely accepted for a several factors. Toothbrush abrasion is an especially
variety of clinical applications for the better handling undesirable phenomenon, since it causes aesthetic and
properties compared with packable composites5). biological disadvantages including decreased gloss,
As aesthetic material, the optical appearance of a discoloration and accumulation of dental plaque19).
composite restoration is of paramount importance6). It is, therefore, clinically important to evaluate the
Among the important factors that influence the optical effect of toothbrush abrasion on the attributes of visual
appearance, gloss, surface roughness and color stability appearance of composite materials.
are particularly essential6-8). Gloss originates from The purpose of this investigation was to evaluate
an uneven geometrical light distribution reflected the surface roughness, the surface gloss and the color
by the surface and the gloss of composite materials is stability of six commercial flowable composites including
reported to be significantly influenced by the surface one universal injectable composite (G-ænial Universal
roughness9,10). Roughness, consisting of the finer Flo), one self-adhering flowable composite (Kerr
irregularities in the surface texture that are inherent Vertise Flow) and four traditional flowable composites
in the materials or the production process, has been (i.e. GrandioSO Flow, Arabesk Flow, Kerr Revolution
reported to play a prominent role in dental plaque Formula 2 and Gradia Direct LoFlo) after in vitro
accumulation11,12). A mean roughness of 0.2 μm has been toothbrush abrasion. The null hypotheses were: 1) there
stated as the critical threshold value for bacterial plaque woud be no differences among the tested materials in
retention13). Moreover, roughness is a determining factor the surface gloss, or the roughness, or the color stability;
for staining14). Any aesthetic restorative material must 2) there would be no correlation between the surface
not only simulate the natural tooth in color but also roughness and the gloss before and after the simulated
maintain the color stability over long periods of time toothbrushing; 3) there would be no correlation between

Received Jul 12, 2017: Accepted Nov 28, 2017

doi:10.4012/dmj.2017-233 JOI [Link]/dmj/2017-233
718 Dent Mater J 2018; 37(5): 717–724

the surface roughness and the color change after the before the simulated toothbrushing.
simulated toothbrushing.
Simulated toothbrusing
MATERIALS AND METHODS The in vitro toothbrush abrasion was conducted using a
toothbrushing simulator (Willytec, Munich, Germany).
Specimen preparation An electrical toothbrush (Oral-B Professional, Braun,
All the tested materials are listed in Table 1. Eight Frankfurt, Germany) was fixed on a holder. Each
rectangular samples (25 mm length×13 mm width×2 specimen was fixed on the sample holder that was kept
mm depth) were made of each composite. The surface in a plastic container filled with a slurry consisting of
of each specimen was covered with a transparent mylar dentifrice RDA 70 (Colgate Total, Colgate-Palmolive,
strip and gently pressed by a microscope glass slide Hamburg, Germany) and distilled water (using a
to extrude the excess materials. Each specimen was paste-to-water ratio of 1:1). All of the specimens were
polymerized for 180 s in a xenon stroboscopic light subjected to 60 min of brushing with a standardized
curing oven (Dentacolor XS, Heraeus Kulzer, Wehrheim, force of 2 N21).
Germany) at a light intensity of 400 mW/cm2, assuring After each toothbrushing test, the slurry was
the the surface was cured at the same time20). renewed and specimens were thoroughly ultrasonically
After light curing, the surface of each specimen was cleaned by distilled water for 10 min and gently air
polished with 180-, 320-, 600-, 800-, 1000-, 2500-, and dried.
4000-grit silicon carbide papers under running water
using a polishing machine (EXAKT, Apparatebau, Surface roughness measurement
Norderstedt, Germany). A new piece of abrasive paper The average surface roughness (Ra, µm) before and
was used for each specimen. after the toothbrush abrasion was determined with a
All of the polished specimens were ultrasonically surface profilometer (Pethometer S3p, Mahr, Gottigen,
cleaned by distilled water for 10 min to remove any Germany) using a tracing length of 5.6 mm and cut-off
debris and then stored in distilled water at 37°C for 24 h value of 0.8 mm at a speed of 0.5 mm/s. Ten-line traces

Table 1 The composites evaluated in the study

Inorganic
Composite
Code Type Matrix Filler filler content Manufacturer
shade
(wt%/vol%)

Bis-GMA, VOCO,
GrandioSO Silicon dioxide (20–40 nm)
GF Nanohybrid TEGDMA, 81/65 Cuxhaven,
Flow A3 Glass ceramic (1 μm)
HEDMA Germany

Bis-GMA, Barium/strontium
Arabesk
AF Microhybrid UDMA, borosilicate (mean 0.7 μm, 64/50.3 VOCO
Flow A3
TEGDMA 0.05–1.3 μm)

Prepolymerized fillers (20 μm)

GPDM, Nano-sized yetterbrium
Kerr Vertise Kerr, Orange,
KVF NA HEDMA, fluoride (40 nm) 70/48
Flow A3 CA, USA
Bis-GMA Barium glass filler (0.7–1.0 μm)
Colloidal nanosillica (10–40 nm)

Kerr Revolution Glass filler

KRF Hybrid Bis-GMA 60/41 Kerr
Formula 2 A3 (mean size 0.6 μm)

G-ænial UDMA,
Silicon dioxide (16 nm) GC, Tokyo,
Universal GUF Nanohybrid TEGDMA, 69/50
Strontium glass (200 nm) Japan
Flo A3 Bis-MEPP

HDR prepolymerized fillers

Multifunctional
(20 μm)
Gradia Direct Microfilled methacrylate
GDL Fluoro-alumino silicate glass 69/50 GC
LoFlo A3 hybrid monomers,
(1.7 μm)
UDMA
Nano-silica fillers (7 nm)

Bis-GMA: bis-phenol-A-diglycidyl methacrylate; UDMA: urethane dimethacrylate; TEGDMA: triethyleneglycol

dimethacrylate; HEDMA: hexanediol dimethacrylate glycol; GPDM: glycerol dimethacrylate dihydrogen phosphate; Bis-
MEPP: 2,2-bis (4-methacryloxy ethoxy phenyl) propane
 Dent Mater J 2018; 37(5): 717–724 719

around the center were recorded from each specimen: five at an accelerating voltage of 10 kV and a magnification
in the horizontal direction and five in the perpendicular of 5,000×.
direction. The mean Ra value was calculated for each
specimen. Calibration was done periodically to assure Statistical analysis
reliable readings. The statistical software R 3.3.1 for windows was
applied for the statistical evaluation of the data. As
Gloss measurement the distribution of all of the data was not normal and
The surface gloss was measured using a glossmeter variances among samples were unequal, nonparametric
(Micro-TRI-gloss, BYK-Gardner, Geretsried, Germany) analysis was used. A Wilcoxon signed-rank test was run
with a measurement area of 9×15 mm and a 60º to detect the effect of the simulated toothbrushing on
geometry. The measurements were expressed as gloss the surface gloss, the roughness and the color stability.
units (GU). Each time before a new test series, the device A Kruskal-Wallis test was used to evaluate whether the
was calibrated by means of calibration plate provided results were materials dependent, followed by a Steel-
by the manufacturer. For each specimen, three readings Dwass post hoc test performing multi-comparisons
were recorded followed by another three readings after between different composites. The significance level was
turning the specimen 90°20,22). set at ɑ=0.05.

Color measurement RESULTS

The color measurement was done before and after the
simulated toothbrushing test using a spectrophometer The gloss values before and after the simulated
(ColorEye 7000A, GretagMacbeth Instruments, NY, toothbrushing are shown in Table 2. The median gloss
USA) with CIEL*a*b* system. The standard illuminant values ranged from 78.4 to 91.4 GU before toothbrush
D50 in this study was chosen based on ISO 3664:2000. abrasion and from 12.6 to 61.0 GU after toothbrush
The spectrophotometer settings were selected as small abrasion. Before the toothbrush abrasion, KRF and
aperture size (SAV), specular component excluded GUF showed the highest gloss value, followed by KVF,
(SCE), diffuse/8°geometry and 100% UV included. while GF and GDL exhibited the lowest gloss value.
Before each measurement session the spectrophotometer After the toothbrush abrasion, GUF yielded the highest
was calibrated by using a white tile supplied by the gloss value, while GF as well as KVF showed the lowest
manufacturer and black light trap. gloss values.
The color measurement of each specimen was The surface roughness results are shown in Table
repeated three times by a single operator, and the mean 3. GF and KVF showed the highest Ra values before
of the three readings was taken. The color differences the toothbrush abrasion. After the 60 min simulated
∆E were calculated from the ∆L*, ∆a*, ∆b* value from toothbrushing KVF and GDL exhibited the highest Ra
each specimen using the following formula: values, followed by KRF and GF. GUF showed the lowest
∆E=[(∆L*)2+(∆a*)2+(∆b*)2]1/2 Ra value of 0.11 μm among all of the tested materials.
The clinically acceptable value for the color change Simple regression analysis showed no correlation
in dental composites in this study is assumed to be between the surface roughness and the gloss before and
∆E≤3.323). after the simulated toothbrushing.
The color changes of all the composites (ΔE), as well
SEM observation as ΔL*, Δa*, and Δb* are presented in Table 4. ΔE values
Two samples from each group were gold coated in were significantly different among all the composites
a sputter-coater (Polaron Range SC7620, Quorum after the simulated toothbrushing. Multi-comparisons
Technologies, West Sussex, UK) and observed with an showed ΔE for GDL was the lowest among all of the
FE-SEM (SUPRA 55VP, Zeiss, Oberkochen, Germany) tested materials. On the other hand, KVF showed the

Table 2 Statistical results of gloss values (GU) before and after toothbrushing simulation

Group Gloss before Gloss after

GF 78.4 [77.3–80.2]a 19.7 [18.2–21.6]a

AF 83.8 [83.5–84.3]b 44.5 [40.9–45.7]b

KVF 88.1 [87.7–88.8]c 12.6 [12.0–13.3]a

KRF 91.4 [90.8–92.1]d 39.6 [35.0–41.8]b

GUF 89.1 [88.3–90.2]c‚d 61.0 [60.2–62.4]d

GDL 78.6 [78.2–79.6]a 43.8 [40.6–45.4]b

The values of groups with same superscript letter showed no significantly different within the columns (ɑ=0.05).
720 Dent Mater J 2018; 37(5): 717–724

Table 3 Statistical results of surface roughness (Ra, μm) before and after toothbrushing simulation

Group Ra before Ra after

GF 0.06 [0.06–0.08] a
0.17 [0.14–0.18]a

AF 0.05 [0.05–0.06]b,d 0.14 [0.12–0.15]b

KVF 0.06 [0.06–0.06]a 0.21 [0.20–0.23]c

KRF 0.06 [0.05–0.06]b,c 0.17 [0.14–0.18]a

GUF 0.05 [0.05–0.06]c,d 0.11 [0.09–0.12]d

GDL 0.06 [0.05–0.06]b 0.20 [0.17–0.24]c

The values of groups with same superscript letter showed no significantly different within the columns (ɑ=0.05).

Table 4 ΔL*, Δa*, Δb* and ΔE (color change) values after toothbrushing simulation

Group ΔL* Δa* Δb* ΔE

GF 2.22 [1.62–2.40] a
−0.01 [−0.05–(0.06)] a
−0.53 [−0.79–(−0.29)] a,d
2.27 [1.98–2.47]a

AF 1.88 [1.68–1.99]a,d −0.11 [−0.15–(−0.08)]b −1.05 [−1.11–(−1.01)]b,c 2.15 [2.01–2.22]a

KVF 2.93 [2.77–3.02]b −1.04 [−1.09–(−1.01)]c −0.95 [−1.05–(−0.91)]b 3.23 [3.09–3.35]b

KRF 1.96 [1.69–2.46]a −0.12 [−0.16–(−0.12)]b −0.85 [−1.03–(−0.67)]b,d 2.16 [1.86–2.65]a

GUF 1.43 [1.27–1.80]c,d −0.18 [−0.20–(−0.15)]b,c −1.33 [−1.61–(−1.09)]c 2.07 [1.87–2.19]a

GDL 1.26 [0.96–1.59]c −0.04 [−0.06–(−0.02)]a −0.51 [−0.68–(−0.41)]a 1.40 [1.10–1.61]c

The values of groups with same superscript letter showed no significantly different within the columns (ɑ=0.05).

highest ΔE after the simulated toothbrushing. of 2 years21). Besides, the technical guidance ISO/TR
The SEM images of each composite before and after 14569-1 on wear testing by toothbrushing recommends
the simulated toothbrushing test are shown in Fig. 1. that the surface of a specimen exposed to the toothbrush
Although all of the composites showed a smooth surface should be flat and well grounded with grade 1000 silicon
after the polishing procedure, they demonstrated surface carbide paper24). In contrast, 4000 grit was used in this
irregularities, surface filler dislodgement and protrusion study to produce a polished surface that has a comparable
after the 60 min toothbrush abrasion. initial roughness and gloss. Cook and Thomas25) reported
that with a 60° measurement angle, the gloss of poor
DISCUSSION finish is generally considered to be below 60 GU, an
acceptable finish between 60 and 70 GU, a good finish
Once a composite restoration is placed in a mouth, a between 70 and 80 GU, and an excellent finish above 80
complex sequence of events will take place, leading to GU. Thus each composite in this study was well polished,
the deterioration of the restoration. Toothbrush abrasion as the mean gloss values were above 70 GU. In addition,
is one of the most common factors influencing surface according to a report released by Ivoclar Vivadent, a
properties and color stability of composites in vivo. This material with a gloss value of 70 GU to an observer does
in vitro study evaluated surface gloss, surface roughness not look less shiny than a material that achieves 90 GU.
and color stability of six commercial flowable composites Based on this theory, all of the investigated materials
influenced by simulated toothbrushing. In terms of can achieve favorable gloss with optimal finishing and
parameters for the toothbrush abrasion in vitro, a force polishing approach clinically.
of 200 g and 1 h strokes of circular movements were Until now, there is no agreement on the geometry
chosen referring to a previous study21). The force of 200 of gloss measurement. Some scientists26) claimed that
g is in line with the technical guidance ISO/TR 14569-1 a 20° angle allows for better differentiation than a 60°
on wear testing by toothbrushing, which requires a load angle, while others27) demonstrated that a 45° angle
that presses the brush against the specimen between differentiates materials better. In this study, a geometry
0.5 and 2.5 N24). If it is assumed that the ideal brushing of 60°, close to the observation angle of the surface by
time is 120 s three times a day, which equates to a tooth the average person, was chosen, which also confirms
surface brushing of 6 s a day, one hour brushing time with the standards established in the technical report of
may amount to a clinically simulated toothbrushing ISO 2813-201428).
 Dent Mater J 2018; 37(5): 717–724 721

Fig. 1 SEM images (5,000×) of specimens before (left column) and after simulated toothbrushing
(right column): GrandioSO Flow (a, b); Arabesk Flow (c, d); Kerr Vertise Flow (e, f); Kerr
Revolution Formula 2 (g, h); G-ænial Universal Flo (i, j); Gradia Direct LoFlo (k, l).
722 Dent Mater J 2018; 37(5): 717–724

Previous study described a significant relationship of composite may be related to the wear of resin
between gloss and surface roughness9). In this study, matrix and fillers, and the weakening of matrix-filler
however, no correlation between the gloss and the bonding. The decrease of gloss and increase of surface
surface roughness was found before and after the roughness, as reported in previous study, are material-
simulated toothbrushing. Furthermore, after polishing dependent29). This could explain why GF did not show
the surface roughness values were similar among some good surface properties. KVF has been introduced as a
materials such AF, KRF and GDL while their GU were first product of self-adhering flowable composites, which
statistically different. The same situation also happened includes a glycerophosphate dimethacrylate (GPDM)
after the toothbrushing simulation when compared GF adhesive monomer that acts like a coupling agent. KVF
and KRF. These may because in addition to surface eliminates the need for a separate adhesive application,
roughness, gloss is also influenced by other factors saving chair time and minimizing handling errors for
such as the difference between refractive indices of the dentists. It showed a high luster and smooth surface
resin matrix and filler29). And it may also confirm that after polishing, however, it remarkably deteriorated
compared to surface roughness, surface gloss is more after the simulated toothbrushing, resulting in obvious
sensitive for measuring the surface quality of composite surface filler dislodgement and protrusion.
materials30). Color plays an important role in obtaining
Aesthetic materials should not only show a high optimum aesthetics. The color stability is related to
luster after polishing, but also maintain their appearance the resin matrix, dimensions of filler particles, depth
after months and years of service31). After the toothbrush of polymerization and coloring agents36,37). Surface
abrasion, all the evaluated materials exhibited a roughness of a specimen influences the instrumental
significant reduction of the surface gloss. The decrease color coordinates, resin composites with a rough
in the surface gloss after the toothbrush abrasion could surface appeared lighter and less chromatic than those
be due to the increased roughness and changes in the with a smooth surface under the condition that the
surface topography resulting from abrasion of the resin diffuse reflection measured by spectrophotometer38).
matrix and loss of surface filler particles32). Until now A spectrophotometer with an integrating sphere can
the smoothness of composites materials has no agreed operate using two different types of measurement
threshold for unacceptable values. It was reported that geometry. Specular reflected light at the specimen is
an Ra value above 0.2 µm would be susceptible to an included in the SCI geometry and is excluded in the SCE
increase in plaque accumulation and higher risk for geometry. The surface roughness of resin composites
caries and periodontal inflammation13). In contrast, influences color differently by the measurement
Chung reported that restorations with roughness values geometry. In general, the SCE geometry, which reflects
below 1 µm could still be seen as smooth and glossy in the surface conditions of specimens, is suggested as
vitro33). After the polishing procedure, all the composites the correct geometry for the color measurement of
obtained very smooth surface with mean Ra values composites39).
between 0.05 and 0.07 µm. However, after the simulated The present results demonstrated that the simulated
toothbrushing, all the materials exhibited significant toothbrushing itself influenced the color stability of
increase of mean Ra values. KVF and GDL showed composites. To date, no agreement has been achieved
mean Ra values above 0.2 µm but below 1 µm after regarding the threshold levels for the color differences
the toothbrushing simulation, while other materials (∆E) that can be visually perceptible or clinically
exhibited mean Ra values below 0.2 µm. acceptable. One ∆E units has been cited frequently as a
Nanocomposites are claimed to have favorable standard for the perceptibility of small color differences40).
mechanical properties, higher surface quality, better However their study tested non-dental materials. Seghi
polish and gloss, as well as increased wear resistance34). et al. suggested 2 ∆E units as threshold values for color
GUF, one of the two evaluated nanohybrid composites, differences in porcelain disks41), while Da Silva et al.
showed excellent wear resistance with highest gloss reported that the acceptability thresholds were 2.7 ∆E
values and lowest roughness values both after the units for metal ceramic crowns42). Regarding composite
simulated toothbrushing. An explanation could be that restorations, Johnston and Kao43) defined 3.7 ∆E units as
apart from a homogenous dispersion of filler particles threshold values for color differences, and Ragain and
in GUF, a revolutionary new silane treatment method Johnston44) suggested average acceptability thresholds of
was used on the surface of the nano-sized glass fillers 2.72 ∆E units. In addition, 3.3 ∆E units were considered
to enhance the adhesion between glass particles and as acceptable threshold values for color differences by
resin matrix, which was stated by the manufacturer35). Ruyter et al.23). As it was used commonly in publications
Fillers were not easily worn when specimens were about in vitro color measurement of dental composites,
subjected to toothbrush abrasion, resulting in much 3.3 ∆E units were employed as acceptable threshold
less filler dislodgement and protrusion on the surface of values in this study. Therefore, the color changes of all of
GUF as shown by the SEM images (Fig. 1). The other the materials in this study could be acceptable. Surface
nanohybrid composite, GF, however, did not present roughness, as mentioned above, affected the color stability
good properties as GUF did. GF even showed the worst a lot. An increasingly roughened surface will reflect
surface gloss although it has the highest filler load (81 the individual segments of specular beam at slightly
wt%/65 vol%) in this study. The surface degradation different angles45). Along with the increased roughness,
 Dent Mater J 2018; 37(5): 717–724 723

the lightness of each material after toothbrush abrasion Key R&D Program of China (2017YFC0840100,2017YF
was higher than before. Except surface roughness, C0840110).
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