Article

The Effect of Dental Bleaching on Nanohybrid Composite

Surface Roughness: A Comparative In Vitro Study of SEM
and Profilometry
Dalia Abou Saad 1, *, Rania Shatila 2 , Gina Khazaal 3 , Marie Abboud 4 , Naji Kharouf 5,6, *
and Carina Mehanna Zogheib 7, *

1 Department of Esthetic and Prosthetic Dentistry, Faculty of Dental Medicine, Saint Joseph University of Beirut,
Beirut 1104 2020, Lebanon
2 Kamal A. Shair Central Research Science Laboratory, Faculty of Arts and Sciences, American University of
Beirut, P.O. Box 11-0236, Beirut 1107 2020, Lebanon; [email protected]
3 Department of Removable Prosthodontics, Faculty of Dental Medicine, Saint Joseph University of Beirut,
Beirut 1104 2020, Lebanon; [email protected]
4 Department of Physics, Faculty of Science, Saint Joseph University of Beirut, B.P. 11-514-Riad El Solh,
Beirut 1107 2050, Lebanon; [email protected]
5 Department of Biomaterials and Bioengineering, INSERM UMR_S 1121, University of Strasbourg,
67000 Strasbourg, France
6 Department of Endodontics and Conservative Dentistry, Faculty of Dental Medicine, University of Strasbourg,
67000 Strasbourg, France
7 Postgraduate Program in Restorative and Esthetic Dentistry, Dental Faculty, Saint Joseph University of Beirut,
Beirut 1104 2020, Lebanon
* Correspondence: [email protected] or [email protected] (D.A.S.);
[email protected] (N.K.); [email protected] (C.M.Z.);
Tel.: +961-76557543 (D.A.S.); +961-03579432 (C.M.Z.)

Abstract: Background: This study aimed to evaluate the effect of in-office bleaching
with 38% hydrogen peroxide (HP) on the surface roughness of a nanohybrid composite
resin by comparing two measurement techniques: Scanning Electron Microscopy (SEM)
and profilometry. Methods: Sixty composite specimens of identical shade and thickness
were prepared, light-cured, and polished following the manufacturer’s guidelines. These
samples were divided into six groups based on the applied surface treatments: group 1:
Academic Editor: Chensong Dong fresh composite (the control group), group 2: old composite, group 3: bleached fresh com-
Received: 21 May 2025 posite, group 4: bleached old composite, group 5: old repolished composite, and group 6:
Revised: 10 June 2025 old repolished bleached composite. Surface roughness was measured using profilometry
Accepted: 13 June 2025
and SEM. Results: Pearson correlation analysis revealed a moderately significant linear
Published: 19 June 2025
relationship (r = 0.548, p < 0.001) between the surface roughness measurements obtained
Citation: Saad, D.A.; Shatila, R.;
using SEM and the profilometer, indicating that both methods provide comparable results.
Khazaal, G.; Abboud, M.; Kharouf, N.;
A comparison of most groups showed significant differences (p < 0.001), highlighting
Zogheib, C.M. The Effect of Dental
Bleaching on Nanohybrid Composite
the increased surface roughness observed after bleaching both fresh and aged compos-
Surface Roughness: A Comparative In ites. Conclusions: Bleaching increased the surface roughness of nanohybrid composites.
Vitro Study of SEM and Profilometry. J. It might be better to use SEM and a profilometer together to obtain a more comprehensive
Compos. Sci. 2025, 9, 313. https:// understanding of the surface characteristics.
doi.org/10.3390/jcs9060313

Copyright: © 2025 by the authors. Keywords: composite resins; materials testing; microscopy; surface properties; tooth bleaching
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons 1. Introduction
Attribution (CC BY) license
(https://creativecommons.org/
Studies on a variety of adult populations have revealed that 19.6% to 65.9% of people
licenses/by/4.0/). are not satisfied with their tooth color, and 20.4% to 50% are not pleased with the appearance

J. Compos. Sci. 2025, 9, 313 https://doi.org/10.3390/jcs9060313

J. Compos. Sci. 2025, 9, 313 2 of 13

of their teeth [1]. Overall, this discontent with both tooth appearance and color is linked
to a heightened inclination for seeking treatments that enhance dental aesthetics, such as
tooth whitening [2]. A prior study that examined how tooth color affected social judgments
found that whiter teeth were associated with a more positive perception [3].
The integration of nanotechnology into conservative dentistry has given rise to the
formulation of nanofilled and nanohybrid composites. Nano-sized fillers enable superior
surface finishes and a smooth texture, contributing to a more natural appearance in dental
restorations [4]. Neo SpectraTM ST Effects (Dentsply, Konstanz, Germany), previously cited
in the literature as Ceram.x, is a nanohybrid composite characterized by the inclusion of
pre-polymerized SphereTEC® fillers, which are spherical particles with an average size of
approximately 15 µm. Moreover, the resin matrix includes finely dispersed methacrylic
polysiloxane nanoparticles, which share chemical similarities with glass materials and
ceramics [5]. According to the manufacturer, Neo Spectra ST was introduced as a rebranded
version of Ceram.x Spectra ST, with identical composition and performance characteristics.
Neo Spectra™ ST and Ceram.x™ Spectra ST are essentially the same nanohybrid composite
material developed by Dentsply Sirona, both utilizing the proprietary SphereTEC® filler
technology [6,7].
In the oral cavity, composite restorations endure various cyclic fatigue loads and are
exposed to diverse aging conditions throughout their service life. These conditions can lead
to matrix or filler degradation, interfacial debonding, or fracturing of filler particles due
to mechanical or environmental stresses. Over time, the combined effects of mechanical
and environmental aging contribute to the gradual deterioration of the material, crack
development, and eventual failure of the restoration. Water aging appears to facilitate
the dislodgement of filler particles from the fractured surface, which is caused by the
degradation of the silane bond connecting the filler particle to the resin [8].
The bleaching procedure is a widely debated topic in contemporary dentistry due
to its simplicity and conservative nature. While it has proven effective in enhancing the
color of natural teeth, it has sparked numerous conflicting discussions about its impact
on dental restoration materials, particularly composite resins [9]. To assess their effect on
the surface of resin composite materials, different approaches, including both qualitative
and quantitative techniques, have been employed [10]. Quantitative assessments are
typically performed with profilometers, which measure surface roughness assigned using
the Ra parameter [11]. SEM is commonly used for qualitative analysis, offering detailed
visual insights into surface topography and microscopic defects. SEM images can be
further analyzed quantitatively using specialized image processing software [12,13]. Image
analysis has gained recognition as a reliable method for material characterization across
various material science fields [14]. In dentistry, Van Pham and Vo [12] used ImageJ® 1.52,
an open-source software, combined with a Field Emission Scanning Electronic Microscope
(FE-SEM) to measure the surface roughness of endodontic instruments. Furthermore,
Balderrama et al. studied the surface roughness of different implants by analyzing SEM
images using ImageJ® software [15].
This study aimed to evaluate the impact of in-office bleaching on the surface roughness
of fresh and aged nanohybrid composites, employing two distinct methods, SEM and
profilometry, to analyze and compare their results. The integration of image quantification
from SEM data represents a significant advancement, providing precise, objective, and
detailed evaluations of surface modifications. Recognizing that alterations induced by
bleaching agents may have clinical significance, potentially compromising the integrity
of restorations and requiring replacement, it becomes imperative to determine whether
surface polishing alone can restore the composite to its original condition. Additionally,
J. Compos. Sci. 2025, 9, 313 3 of 13

this study explored the effect of post-bleaching polishing in restoring the initial surface
roughness of the composite.
The null hypotheses were as follows: There is no significant difference between pro-
filometry results and SEM-ImageJ® results, bleaching will not change the surface roughness
of the fresh and aged nanohybrid composites, and post-bleaching polishing has no effect
on the surface roughness.

2. Materials and Methods

This study protocol was reviewed and approved by the Ethics Committee of Saint
Joseph University of Beirut under the reference number USJ-2024-120.

2.1. Sample Size Calculation

To determine the sample size, a power analysis for 2 × 2 × 2 ANOVA (fixed effects,
special, main effects, and interactions) was conducted using G*Power software 3.1.9.7
for Windows (Heinrich Heine, Universitat Düsseldorf, Düsseldorf, Germany). A power
of 0.8, an alpha level of 0.05, 6 groups, and a numerator degree of freedom of 1 were
considered, and a large conventional effect size of 0.4 was estimated. The minimum sample
size required is 52 specimens in total. However, we selected a total of 60 specimens to
enhance the statistical power of our analysis.

2.2. Specimen Preparation

Sixty rectangular samples were fabricated using enamel shade E1 of the nanohybrid
composite Neo SpectraTM ST Effects (Dentsply, Konstanz, Germany), whose composition is
summarized in Table 1. These samples were prepared by filling a customized plexi mold
measuring 8 mm in length, 3 mm in width, and 2 mm in depth. The molds were slightly
overfilled with resin material, covered on both sides with a Mylar strip, and compressed
between two microscope glass slides to ensure uniformity and remove excess material. Each
specimen was polymerized for 20 s using an LED light with a wavelength of 380–515 nm
and a light intensity of 2300 mW/cm2 (Eighteeth Medical Curing Pen, Light Cure Unit), as
recommended by the manufacturer.

Table 1. Composition of the composite resin used in this study.

Filler Content
Material Type Composition
(w/w)
Neo
Matrix: Methacrylate modified
SpectraTM ST
polysiloxane dimethacrylates,
Effects E1 Nano- Weight: 78–80 wt.%
ethyl-4 (dimethylamino) benzoate,
(Dentsply, hybrid Volume: 60–62 vol.%
and bis(4-methyl-phenyl) iodonium
Konstanz,
hexafluorophosphate.
Germany)
Filler:
Barium glass, Ytterbium fluoride,
Inorganic fillers (0.1–3.0 µm),
SphereTEC® fillers (d3, 50 ≈ 15 µm)

All specimens were finished and polished by a single operator for consistency. Fin-
ishing was performed using Enhance® finishing points (Dentsply Caulk, Milford, DE,
USA) for 20 s, followed by polishing with Enhance® polishing cups and Prisma® Gloss™
Composite Polishing Paste (Dentsply Caulk, Milford, DE, USA) for another 20 s using a
low-speed micro-motor (10K RPM). The specimens were then rinsed with distilled water
for 10 s and air-dried for 5 s to remove any remaining debris.
J. Compos. Sci. 2025, 9, 313 4 of 13

The sixty specimens were evenly distributed into six groups, with 10 specimens assigned
to each group. The groups were categorized based on the type of surface treatment applied to
the specimens, including bleaching, staining, and repolishing procedures, as follows:
Group 1: fresh composite (unstained, unbleached); this was the control group.
Group 2: old composite (aged and stained, unbleached).
Group 3: bleached fresh composite (unstained, bleached).
Group 4: bleached old composite (aged and stained, bleached).
Group 5: old repolished composite (aged and stained, unbleached, repolished).
Group 6: old repolished bleached composite (aged and stained, bleached, repolished).

2.3. Simulated Staining and Aging Procedures

Following ISO 7491:2000 for dental materials, forty specimens (groups 2, 4, 5, and 6)
were aged via thermocycling and light exposure. The specimens were subjected to 20,000 cy-
cles in the SD Mechatronik Thermocycler (SD Mechatronik GmbH, Feldkirchen-Westerham,
Germany), alternating between 5 ◦ C and 55 ◦ C water baths with 20 s dwell time and a 10 s
rest time. This procedure was conducted to simulate two years of in vivo exposure to the
oral environment [16].
Given that the composite restoration may be subjected to a staining agent like coffee for
around 15 min daily in vivo (equivalent to consuming 1 or 2 cups per day) [16], these forty
specimens (groups 2, 4, 5, and 6) were then exposed to 200 cycles in the SD Mechatronik
Thermocycler alternating between a 5 ◦ C water bath and 55 ◦ C coffee bath with 20 s
dwell time and a 10 s rest time. Coffee is among the most widely consumed beverages
globally [17,18]. In Lebanon, Turkish coffee dominates, accounting for 65% of total coffee
consumption, while instant coffee makes up 35% [17]. Therefore, Café Najjar (Beirut,
Lebanon) was selected as the staining solution.

2.4. Bleaching Procedure

Thirty specimens (groups 3, 4, and 6) underwent bleaching with 38% HP (fläsh;
WHITEsmile, GmbH, Mannheim, Germany) following the manufacturer’s protocol.
Two sessions were conducted one week apart, with the agent applied twice for 15 min per
session. Specimens were rinsed with distilled water and air-dried with an air spray for
one minute between applications.

2.5. Repolishing
After undergoing surface treatments, the specimens in groups 5 and 6 were finally
repolished using the same polishing technique initially applied.

2.6. Surface Roughness Measurement

The average surface roughness (Ra) of all the specimens was first measured using a
Bruker Dektak XT surface profilometer (Dektak, Bruker, Billerica, MA, USA) equipped
with Vision64 software, followed by imaging with a Tescan MIRA3 scanning electron
microscope (SEM).
Profiling Procedure:
For the profilometric measurements, the mean Ra value for each sample was reported
as a result of three determinations at different regions near the center. The cut-off value
was 0.25 mm with a transverse length of 0.2 mm, a stylus speed of 0.02 mm/s, and a stylus
tip of 2 µm.
SEM Evaluation:
Following profilometric evaluation, all specimens were gold-coated using a sputter
coater (Quorum Q150T ES, Laughton, East Sussex, United Kingdom) and mounted onto
J. Compos. Sci. 2025, 9, 313 5 of 13

SEM stubs. Surface topography was then captured using secondary electron (SE) detector
at 8000× magnification and a 5 kV operating voltage (Figures 1–3). Morphometric analyses
of the digital SEM images were conducted by two blind and calibrated examiners. Three
SEM images near the center were taken for each specimen.

(a) (b)
Figure 1. (a) SEM image from a sample taken from group 1; (b) SEM image from a sample taken from
group 2 (magnification: 8000; scale: 5 µm).

(a) (b)
Figure 2. (a) SEM image from a sample taken from group 3; (b) SEM image from a sample taken from
group 4 (magnification: 8000; scale: 5 µm).

The surface roughness was quantified using open-source software, ImageJ® (NIH,
Bethesda, MD, USA), using the roughness calculation plugin, which measures roughness
parameters according to ISO 21920-2:2021; Geometrical product specifications (GPS)—
Surface texture: Profile—Part 2: Terms, definitions and surface texture parameters. Inter-
national Organization for Standardization: Geneva, Switzerland, 2021.: Ra (arithmetical
mean deviation), Rq (root mean square deviation), Rv (lowest valley), Rp (highest peak),
and Rt (total height). To relate the Ra value to the image’s pixel dimensions, the Ra value
was divided by the distance measured along the diagonal line. This calculation yields the
roughness of the surface expressed in micrometers per pixel (µm/pixel). The Ra value for
each specimen was calculated as the average of the Ra measurements obtained from three
SEM images of the same specimen.
J. Compos. Sci. 2025, 9, 313 6 of 13

(a) (b)
Figure 3. (a) SEM image from a sample taken from group 5; (b) SEM image from a sample taken from
group 6 (magnification: 8000; scale: 5 µm).

Ra, the arithmetic mean deviation of the surface profile, was chosen as the primary
measure of surface roughness due to its widespread use and standardization under ISO
21920-2:2022, forming the basis for statistical analysis in this study [19].

2.7. Statistical Methods

Data were analyzed using IBM SPSS Statistics (Version 26), with a significance level
set at 5%. Normality of the Ra distribution was tested using the Kolmogorov–Smirnov and
Shapiro–Wilk tests. Pearson correlation analysis was used to examine the relationship be-
tween profilometer and SEM measurements. One-way ANOVA was conducted to evaluate
differences in mean surface roughness across the treatment groups for each measurement
method. To account for the interactions between aging, bleaching, and repolishing, a
three-way ANOVA was performed to assess both main effects and interactions. Finally,
independent t-tests were used to compare roughness between bleaching conditions.

3. Results
3.1. SEM Observations
Representative SEM images from each group are presented in Figures 1–3. When
comparing the SEM images of the different groups, the fresh nanohybrid composite
(Figure 1a) presented the smoothest surface with no visible exposed filler particles. In
contrast, pores and irregular filler particles were found on the surface of the composite
after aging (Figure 1b).

3.2. Descriptive Statistics

The descriptive statistics presented in Tables 2 and 3 were used to evaluate the central
tendency, variability, and distribution of surface roughness within each group.

Table 2. Surface roughness summary in nanometers (profilometry).

Group N Mean Std. Error Std. Deviation Variance

1 10 141.57 0.09 0.29 0.09
2 10 222.72 1.58 4.98 24.81
3 10 212.40 1.22 3.87 14.98
4 10 254.90 0.61 1.93 3.73
5 10 167.33 1.64 5.18 26.80
6 10 159.81 2.18 6.91 47.70
J. Compos. Sci. 2025, 9, 313 7 of 13

Table 3. Surface roughness summary in micrometers per pixel (SEM).

Group N Mean Std. Error Std. Deviation Variance

1 10 0.09 0.00 0.00 0.00
2 10 19.59 1.58 0.94 0.89
3 10 19.63 1.22 0.89 0.79
4 10 21.39 0.61 0.63 0.40
5 10 19.75 1.64 0.54 0.29
6 10 22.61 2.18 0.43 0.19

3.3. Comparing Methods of Surface Roughness Measurement

Surface roughness was measured using two methods: the profilometer (in nanometers)
and the SEM (in micrometers per pixel) (Figures 1–4). These methods measure different
aspects of surface texture and use different units. A Pearson correlation analysis showed a
moderate correlation of 0.548, which was statistically significant (p < 0.001). This means
there is a relationship between the two methods, but it is not very strong.

(a) (b)
Figure 4. (a) A crack running diagonally across the surface of a specimen from group 6 (magni-
fication: 5; scale: 10 µm); (b) SEM image from a sample taken from group 1 with high contrast
(magnification: 4000; scale: 10 µm).

Because the correlation is moderate, the two methods cannot be directly compared
or used interchangeably. To fully understand the surface roughness, it was necessary to
analyze the results from each method separately, as each method captures unique details.

3.4. Surface Roughness Comparison Across Treatment Groups: ANOVA Results

Figure 5 presents the distribution of surface roughness in nanometers across the six
composite treatment groups. The boxplot clearly shows variations in surface roughness
between the groups. Group 1 (fresh composite) demonstrated the lowest median surface
roughness (mean = 141.57 nm, SD = 0.29 nm), indicating a smoother surface compared to all
other groups. In contrast, group 4 (bleached old composite) exhibited the highest median
surface roughness (mean = 254.90 nm, SD = 1.93 nm), suggesting that the combination of aging
and bleaching led to a significantly rougher surface than all the other groups. This overall
trend highlights the impact of different treatments on the roughness of dental composites.
Similarly, Figure 6 displays surface roughness measured using SEM in micrometers per
pixel across the same treatment groups. In this case, group 1 (fresh composite) again showed
the lowest surface roughness (mean = 0.0922 µm/pixel, SD = 0.0029 µm/pixel), while group 6
(old bleached repolished composite) exhibited the highest roughness (mean = 22.61 µm/pixel,
SD = 0.63 µm/pixel), followed by group 4 (mean = 21.39 µm/pixel, SD = 0.63 µm/pixel).
Interestingly, while group 4 had the highest roughness in nanometers, group 6 showed the
highest roughness when measured in micrometers per pixel, highlighting the importance
of examining results from both measurement methods to gain a complete understanding of
surface roughness.
J. Compos. Sci. 2025, 9, 313 8 of 13

Figure 5. Boxplots showing the surface roughness in nanometers across composite treatment groups
(measured using a profilometer).

Figure 6. Boxplots showing the surface roughness in micrometers per pixel across composite treat-
ment groups (measured using image analysis/SEM).

3.5. Three-Way ANOVA Analysis

The three-way ANOVA results for both nanometers and micrometers per pixel revealed
that aging, bleaching, and repolishing significantly affect the surface roughness of dental
composites. The interactions between these factors were also significant (p-value < 0.001),
indicating complex relationships that should be considered when evaluating the surface
characteristics of composites after various treatments.

3.6. Independent Samples T-Test Analysis

The table below (Table 4) summarizes the surface roughness measurements from
the study, comparing different treatment protocols across composite groups based on the
independent t-test.
J. Compos. Sci. 2025, 9, 313 9 of 13

Table 4. Comparison across the groups.

Surface Roughness (Nanometers) Surface Roughness (Micrometers per Pixel)

Mean ± Standard Mean ± Standard
Group Comparison p-Value p-Value
Deviation Deviation
−81.16 (141.57 ± 0.29 vs. −19.50 (0.09 ± 0.003
Group 1 vs. Group 2 <0.001 <0.001
222.72 ± 4.98) vs. 19.59 ± 0.94)
−70.83 (141.57 ± 0.29 vs. −19.53 (0.09 ± 0.003
Group 1 vs. Group 3 <0.001 <0.001
212.40 ± 3.87) vs. 19.63 ± 0.89)
−113.34 (141.57 ± 0.29 vs. −21.30 (0.09 ± 0.003
Group 1 vs. Group 4 <0.001 <0.001
254.90 ± 1.93) vs. 21.39 ± 0.63)
−25.76 (141.57 ± 0.29 vs. −19.65 (0.09 ± 0.003
Group 1 vs. Group 5 <0.001 <0.001
167.33 ± 5.18) vs. 19.75 ± 0.54)
−18.24 (141.57 ± 0.29 vs. −22.52 (0.09 ± 0.003
Group 1 vs. Group 6 <0.001 <0.001
159.81 ± 6.91) vs. 22.61 ± 0.43)
10.32 (222.72 ± 4.98 vs. −0.03 (19.59 ± 0.94
Group 2 vs. Group 3 <0.001 0.939 *
212.40 ± 3.87) vs. 19.63 ± 0.89)
−32.18 (222.72 ± 4.98 vs. −1.79 (19.59 ± 0.94
Group 2 vs. Group 4 <0.001 <0.001
254.90 ± 1.93) vs. 21.39 ± 0.63)
55.39 (222.72 ± 4.98 vs. −0.15 (19.59 ± 0.94
Group 2 vs. Group 5 <0.001 0.67 *
167.33 ± 5.18) vs. 19.75 ± 0.54)
62.91 (222.72 ± 4.98 vs. −3.02 (19.59 ± 0.94
Group 2 vs. Group 6 <0.001 <0.001 *
159.81 ± 6.91) vs. 22.61 ± 0.43)
−42.50 (212.40 ± 3.87 vs. −1.76 (19.63 ± 0.89
Group 3 vs. Group 4 <0.001 <0.001
254.90 ± 1.93) vs. 21.39 ± 0.63)
45.07 (212.40 ± 3.87 vs. −0.12 (19.63 ± 0.89
Group 3 vs. Group 5 <0.001 0.722 *
167.33 ± 5.18) vs. 19.75 ± 0.54)
52.59 (212.40 ± 3.87 vs. 2.99 (19.63 ± 0.89 vs.
Group 3 vs. Group 6 <0.001 <0.001 *
159.81 ± 6.91) 22.61 ± 0.43)
87.57 (254.90 ± 1.93 vs. 1.64 (21.39 ± 0.63 vs.
Group 4 vs. Group 5 <0.001 <0.001
167.33 ± 5.18) 19.75 ± 0.54)
95.09 (254.90 ± 1.93 vs. −1.22 (21.39 ± 0.63
Group 4 vs. Group 6 <0.001 <0.001 *
159.81 ± 6.91) vs. 22.61 ± 0.43)
7.52 (167.33 ± 5.18 vs. −2.87 (19.75 ± 0.54
Group 5 vs. Group 6 0.013 <0.001 *
159.81 ± 6.91) vs. 22.61 ± 0.43)
* indicate differences between the two measurement methods.

4. Discussion
To achieve the main goal of this study, the average surface roughness Ra was measured
using the profilometer device and SEM-ImageJ® software. Ra is the most commonly used
measurement unit in the majority of studies assessing the surface roughness of composite
resins [20].
Both the SEM (Figure 1a) and profilometer analyses of the control group, which con-
sisted of a fresh Neo SpectraTM ST Effects composite polished with the Enhance system,
revealed the lowest surface roughness at 141.57 nm (0.141 µm), as shown in Figures 4b and 5.
These findings are consistent with those of Yaldav et al., who reported a similar profilo-
metric value of 0.1457 µm and comparable SEM images for the fresh Ceram.x composite
polished using the Enhance system [21]. However, when studying the effects of bleaching
and repolishing, SEM and profilometer yielded different results, thereby rejecting the
first hypothesis.
J. Compos. Sci. 2025, 9, 313 10 of 13

The results of the present study indicate that bleaching fresh and old nanohybrid
composites significantly increases surface roughness according to both methods used
(Figures 1b, 2 and 3 and Table 4). Thus, this finding rejects the second null hypothesis. The
active bleaching agent, HP, often induces oxidation, promoting free radical formation [22,23].
After the dissociation of H2 O2 molecules, reactive free radicals can be generated, such as
superoxide ions (O2 − ), hydroxyl ions (OH− ), perhydroxyl ions (HOO− ), hydroxyl radicals
(HO•), and hydroperoxy radicals (HOO•). These species can interact with single and
double C–C bonds, as well as ester bonds within the polymer network at the surface of the
polymerized composite, potentially leading to the oxidation of these bonds (oxidative ester
cleavage) and promoting hydrolytic degradation at the resin–filler interface. The oxidation
of chemical bonds in the composite leads to its degradation and softening. This process
may create cracks in the matrix, facilitating the release of unreacted monomers from the
material. Furthermore, the oxidative stress at the resin–filler interface disrupts the silane
coupling agent, which is responsible for anchoring filler particles to the organic matrix.
This disruption contributes to filler–matrix debonding, matrix erosion, and the formation
of microscopic surface defects, all of which collectively contribute to a significant increase
in surface roughness and deterioration of the material’s physical properties [24].
Several studies have shown that bleaching agents increase the surface roughness of
composite materials. Popescu et al. found that 40% HP caused the greatest roughness, par-
ticularly in microhybrid composites, which were rougher than nanohybrid composites [19].
Similarly, Wongpraparatana et al. noted that both 10% CP and 40% HP significantly
increased surface roughness in composite materials and resin-modified glass ionomer ce-
ment [25]. In contrast, a study by Chakraborty et al. did not show any significant difference
in the surface roughness of the nanohybrid composite (Ceram.x ® SphereTEC™ one) after
bleaching with 35% HP [26]. This difference can be attributed to several reasons. Firstly, the
profilometer was used to assess the surface roughness; however, specific details regarding
the size of the stylus tip were not provided. Secondly, the composite samples were tested
in their fresh state, without any prior aging or staining processes.
To mitigate the increase in surface roughness, some authors suggested repolishing
the composite material after the bleaching process [19,27–29]. The findings of the present
study collectively suggest that the effectiveness of repolishing may vary depending on
the method of surface roughness measurement. Repolishing the composite material after
it has been subjected to bleaching, aging, and staining can significantly reduce surface
roughness, as shown by profilometer measurements. However, this process does not
completely return the composite to the original smoothness of its fresh, untouched state.
Polishing after bleaching can remove the residual monomers released by bleaching, which
positively affects the physical properties of the composite material [30]. However, the SEM
data (Figure 3a,b) indicated that repolishing might not fully mitigate the surface roughness
induced by bleaching, especially when considering the broader surface texture.
The stylus profilometer, utilized in this study, characterizes surface features at a scale
corresponding to the size of the stylus. The profilometer, with its 2 µm diamond stylus,
is less precise compared to the SEM. Due to its larger size, the profilometer cannot access
certain micro-irregularities and fails to capture surface features smaller than the stylus,
potentially leading to an underestimation of surface roughness [11,31].
A profilometer is designed to measure surface roughness by physically tracing the
surface with a stylus. The stylus tip’s size determines the smallest feature that can be
detected; in our case, a 2-micron tip would mean that the profilometer can detect surface
features down to around 2 microns in size or larger. This is significantly less sensitive than
SEM, which is why it operates effectively at the micron scale but cannot resolve nanoscale
features [31,32].
J. Compos. Sci. 2025, 9, 313 11 of 13

SEM is capable of detecting surface features at the nanoscale due to its high reso-
lution [33]. This is because SEM uses a focused beam of electrons to scan the surface
of a sample, providing very detailed images that can reveal fine surface details, such as
microcracks, nanostructures, or very small surface textures [34]. Scratches observed on the
surface can be mostly attributed to the grinding effect of the dislodged fillers [11,35].
The difference in Ra values between the two methods may also be attributed to the
fact that the measurement of surface parameters is influenced by the size of the area
under examination. Additionally, while the profilometer measures line roughness in either
horizontal or vertical directions, SEM assesses area roughness across the entire surface [11].
Both methods provide valuable but different insights into the effects of bleaching and
repolishing on composite surfaces.
The SEM results showed that repolishing after bleaching increased the surface rough-
ness. Repolishing a bleached composite may initially be intended to smooth the surface, but
if the bleaching process has already caused significant deterioration, additional polishing
can exacerbate surface roughness. The polishing process can create new scratches or reveal
subsurface defects that were hidden before bleaching (Figure 4a). The SEM images may
show more scratches and grinding marks after repolishing because the combination of
bleaching-induced degradation and mechanical abrasion from polishing tools can make
the surface appear rougher and less uniform. Pala et al. conducted a study to evaluate the
surface roughness of resin composites following various finishing and polishing techniques.
Their findings indicated that the most noticeable scratches and irregularities (deep pits and
undulating surfaces) were present on composites treated with the Enhance system [36].
When interpreting the results of the present study, it is important to acknowledge its
limitations. This study was conducted in vitro, limiting its representation of real-world
clinical conditions, particularly factors like saliva’s role in moderating bleaching effects [37,38].
While the findings provide valuable insights into material aging and degradation, further
research is needed to explore the influence of varying HP concentrations on the surface
roughness, particularly considering the guidelines of the European Scientific Committee on
Consumer Safety (SCCS) limiting HP levels in dental whitening products to a maximum of
6% [35]. Additionally, studies should focus on newer materials, nanocomposites, and different
polishing techniques. Integrating SEM imaging with profilometric analysis to determine the
surface roughness threshold for bacterial adhesion could also provide a more comprehensive
understanding of the interplay between surface characteristics and material performance.

5. Conclusions
Bleaching with 38% HP increased the surface roughness of both freshly treated and
aged nanohybrid composites measured using a profilometer and SEM.
From a clinical perspective, while repolishing may reduce surface roughness at a
finer scale (as measured in nanometers), it does not effectively smooth the broader surface
texture, particularly when observed with SEM. This limitation underscores the potential
need to replace restorations to maintain both aesthetic and functional outcomes. These
findings emphasize the importance of monitoring restorative materials post-bleaching and
considering replacement to ensure optimal clinical results and patient satisfaction.
SEM and profilometry are both recognized techniques for evaluating surface roughness
in materials, but their combined use is not universally standard practice in all studies.
While they offer complementary advantages—SEM providing detailed topography at the
microscopic level and profilometry offering quantitative roughness data—many studies
typically use one or the other depending on the research goals. Therefore, it might be better
to use these techniques together to obtain a more comprehensive understanding of surface
characteristics, especially in studies focusing on material properties at different scales.
J. Compos. Sci. 2025, 9, 313 12 of 13

Author Contributions: Conceptualization, D.A.S., C.M.Z. and G.K.; methodology, D.A.S. and C.M.Z.;
software, M.A., R.S. and D.A.S.; validation, C.M.Z. and D.A.S.; formal analysis, D.A.S., M.A. and
C.M.Z.; investigation, R.S., D.A.S. and M.A.; resources, C.M.Z.; data curation, D.A.S. and M.A.;
writing—original draft preparation, D.A.S.; writing—review and editing, N.K. and C.M.Z.; visual-
ization, D.A.S.; supervision, C.M.Z. and D.A.S.; project administration, D.A.S. and C.M.Z.; funding
acquisition, D.A.S. All authors have read and agreed to the published version of the manuscript.

Funding: This research received no external funding.

Data Availability Statement: The raw data supporting the conclusions of this article will be made
available by the authors on request.

Acknowledgments: The authors are grateful to Dentsply Sirona and WhiteSmile for their help
in providing materials for this research. Sincere gratitude is also extended to the Kamal A. Shair
Central Research Science Laboratory (CRSL) at the American University of Beirut for facilitating the
profilometry and SEM analyses. The thermocycling work was carried out at the Biomaterials unit at
the Cranio-Facial Research Laboratory at the Faculty of Dental Medicine at Saint Joseph University of
Beirut, Lebanon. All authors approved and validated the study.

Conflicts of Interest: The authors declare no conflicts of interest.

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