Original Article

Oxygen inhibition layer: A dilemma to be solved

Aarti C. Panchal, Geeta Asthana
Department of Conservative Dentistry and Endodontics, Government Dental College and Hospital, Ahmedabad, Gujarat, India

Abstract
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Objective: This study aimed to evaluate the thickness of oxygen inhibition layer (OIL), produced on various composite materials,
and to compare their interlayer shear bond strength (SBS), by treating the OIL with various agents.
Materials and Methods: The thickness of OIL of three different composite materials (120 specimens divided into three groups)
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Group 1 – Ivoclar Tetric N‑Ceram (nanohybrid composite), Group 2 – Ivoclar Te Econom Plus (microhybrid composite), and
Group 3 – GC EverX Posterior (a short glass fiber‑reinforced composite) was evaluated. Each group was divided into four
subgroups (A, B, C, and D) depending on the surface treatment given – no surface treatment (control group), ethanol, water
spray, and grinding with SiC paper. This was followed by interlayer SBS testing.
Statistical Analysis: The data were statistically analyzed using ANOVA at a significance level of P < 0.05. Tukey’s post hoc
analysis was performed following ANOVA to determine differences among the groups.
Results: The control group showed higher SBS irrespective of the type of composite material. The group treated with SiC paper
resulted in the lowest interlayer SBS among all groups. Glass fiber composite showed higher interlayer SBS compared to both
nanohybrid and microhybrid composites, irrespective of the surface treatment given.
Conclusion: The OIL, which acts as an intermediate layer, is retained on the surface of the composite even after treatment with
ethanol and water spray. The presence of an OIL improved the interlayer SBS of two adjacent composite layers and led to more
durable adhesion. Rather, the absence of an OIL adversely affected the bond strength and led to adhesive interfacial failures.
Keywords: Failure mode; oxygen inhibition layer; shear bond strength; surface treatment

INTRODUCTION hence also known as an unpolymerized (uncured) layer

of resin.[3,4] The thickness of the OIL could influence the
The composite resin material has become an integral interlayer bond strengths of the composite resins, as OIL is
part of modern restorative dentistry. Oxygen inhibition known to (i) impair the interfacial homogeneity;[2] (ii) permit
layer (OIL) is a sticky, resin‑rich uncured layer and always complete interdiffusion of the freshly overlaid composite
present when a composite or bonding resin is polymerized through the oxygen inhibition zone (if OIL is thin);[1] and (iii)
in air.[1] During the light‑curing procedure, oxygen in the compromise the mechanical strength (if OIL is thick).[5]
air interferes with the polymerization reaction (due to Hence, the thickness of the OIL is crucial for the integrity
higher reactivity of oxygen with a radical as compared to
of the layer itself and the quality of the interlayer bonding.
reactivity of monomer with the radical). This results in the
formation of an OIL on the surface of the composite. The
When a new increment of the composite is added, OIL
OIL is similar in composition to that of an uncured resin
with consumed or reduced amounts of photoinitiator,[1,2] formed on the previous layer readily adapts the overlying
material. It, thereby, increases the contact area and allows
Address for correspondence: increments of composite on both sides of OIL to cross the
Dr. Aarti C. Panchal, 5370, Viththalwadi, Tarsadi, Kosamba, interface and blend, to form an interdiffused zone, where
Surat ‑ 394 120, Gujarat, India.
E‑mail: draartipanchal@[Link] copolymerization can take place to produce a chemical bond.
All these actions will tend to fortify layer–layer interaction.[3]
Date of submission : 29.06.2019
Review completed : 17.07.2020 This is an open access journal, and articles are distributed under the terms
Date of acceptance : 21.08.2020
of the Creative Commons Attribution‑NonCommercial‑ShareAlike 4.0
Published: 04.12.2020
License, which allows others to remix, tweak, and build upon the work
Access this article online non‑commercially, as long as appropriate credit is given and the new
Quick Response Code: creations are licensed under the identical terms.
Website:
[Link] For reprints contact: WKHLRPMedknow_reprints@[Link]

How to cite this article: Panchal AC, Asthana G. Oxygen

DOI: inhibition layer: A dilemma to be solved. J Conserv Dent
10.4103/JCD.JCD_325_19
2020;23:254-8.

254 © 2020 Journal of Conservative Dentistry | Published by Wolters Kluwer - Medknow

 Panchal and Asthana: Effects of oxygen inhibition layer on shear bond strength

b
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a b
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c d
Figure 1: Stereomicroscopic (×40) photographs of the
thickness of the oxygen inhibition layer with various surface
treatments in the nanohybrid composite specimen. (a)
Control, (b) ethanol‑treated specimen, (c) water spray‑treated
specimen, (d) SiC paper‑treated specimen a d
Figure 2: Illustration of shear bond strength testing and
Composites are becoming more durable with advances in stereomicroscopic (×40) photographs of different failure
the filler particles, monomer matrices, improved adhesive modes. (a) Sample setup for shear bond strength testing, (b)
systems, and polymerization devices.[2,4,6‑8] Differences in adhesive failure, (c) cohesive failure, (d) mixed failure
the thickness of OIL have been observed among various
dimethacrylate‑based composites. This could be due to another microscope slide as a coverslip. The specimens
the filler content and its type and also network density were polymerized through the coverslip for 40 s using a
of the resin composite. The amount of diluent (TEGDMA) light‑emitting diode light‑curing unit. This method secured
also affects the oxygen inhibition depth (in this study, the formation of the OIL only at the outer sides of the
as in microhybrid and short glass fiber-reinforced specimens because air–resin contact was possible only at
(SGFR) composite). When a composite is reinforced with the resin boundary between the polymerized composite
fibers, the fibers and their orientation may also influence material and the spacers.
the oxygen inhibition depth.[9‑12] For years, the dental
The depth of the OIL was measured along the periphery of
community has held a common perception that an OIL is
each specimen using a stereomicroscope at a magnification
required before adding more layers of bonded composite.
of ×40, with a calibrated disk. Micrographs were taken of
Reports on how the OIL affects bond strength have been
each specimen using the computer imaging program, to
inconsistent, despite many efforts dedicated to the subject.
[13,14]
provide a visual record of the inhibition layer as shown in
Figure 1.
The present study was conducted to evaluate OIL, produced
Preparation of the specimen for interlayer
on different composite material, and to compare their
shear bond strength
interlayer shear bond strength (SBS), by treating the OIL
A total number of 120 specimens were prepared for this
with various agents.
study, which were divided into three groups of 40 specimens
each (Group‑1 nanohybrid, Group‑2 microhybrid, and
MATERIALS AND METHODS Group‑3 short glass fiber-reinforced) [Table 1].

Evaluation of the thickness of oxygen Each of the three groups was further subdivided into
inhibition layer four subgroups A, B, C, and D according to the surface
An equal amount of each type of composite resin (Ivoclar treatments given to the OIL.
Tetric N‑Ceram [nanohybrid composite], Ivoclar Te Econom A. Control group – No surface treatment was given to OIL
Plus [microhybrid composite], and GC EverX Posterior [a B. Ethanol group – OIL was treated by wiping it from the
short glass fiber‑reinforced composite]) was applied onto surface of the cured specimen using alcohol sponges
the middle of a horizontally placed glass microscope slides. soaked in 99 wt% ethanol for 20 s and then gently air
A constant sample thickness of 0.1 mm was ensured by dried for another 20 s
placing two glass plates (20 mm × 20 mm), as spacers, on C. Water spray group – OIL was treated with water applied
each side of the composite resin, which was covered by as a water spray for 20 s from a distance of ~5 mm

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 Panchal and Asthana: Effects of oxygen inhibition layer on shear bond strength

Table 1: Materials used in the study and their basic composition

Brand Manufacturer Type Composition
Tetric N Ceram Ivoclar Vivadent Nanohybrid Bis-GMA. Bis-EMA
UDMA
yttrium trifluoride
Barium glass 63.5 wt%, prepolymer 17 wt%
EverX Posterior GC, Tokyo, Japan Short glass Bis-GMA, PMMA, TEGDMA, E-glass fiber, barium borosilicate
Short glass fiber- fiber- Barium glass 74.2 wt% 53.6 vol%
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reinforced composite reinforced

composite
Te-Econom Plus Ivoclar Vivadent Microhybrid Bis-GMA, Bis-EMA, UDMA, TEGDMA Barium glass, yttrium trifluoride, silicon dioxide
(76 wt %53 vol%)
Bis-EMA: Bisphenol-A-dyethoxy dimethacrylate, Bis-GMA: Bisphenol A-glycidyl dimethacrylate, PMMA: Polymethylmethacrylate, TEGDMA: Triethylene-glycol
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dimethacrylate, UDMA: Urethane dimethacrylate

perpendicular to the specimen surface and then gently To analyze and to determine the fracture type, all fractured
air dried for another 20 s surfaces were visually examined under light microscopy at
D. SiC paper – OIL was treated by grinding the surface a magnification of ×40.
with 1000‑grit SiC paper.
RESULTS
OIL thickness was again measured in all the four
subgroups – A, B, C, and D after the surface treatments were Oxygen inhibition layer thickness
given to the OIL, and for the SBS testing, the specimens The optically measurable thickness of the OIL was
were further prepared. evaluated for different composites used in the study. The
results are presented in Table 2. SGFR composite (Group 3)
For specimen preparation, acrylic resin blocks were made, showed a maximum thickness of OIL, as compared to other
in which round retentive cavity of 5 mm diameter and 3 composites (Group 1 and Group 2).
mm depth was made. The same restorative material was
used as the substrate and the adherent material. Two‑way ANOVA showed that both the type of material and
the surface treatment had significant effects (P < 0.001) on
Following polymerization, surface treatment with various the thickness of the OIL.
agents was done. The adherent material was applied onto
the substrate in an increment of 2 mm using a translucent Interlayer shear bond strength
polyethylene mold with an inner diameter of 3.5 mm and The results of the SBS investigation between incrementally
polymerized for 40 s. placed composite layers are presented in Graph 1.

Storage and thermocycling of specimens A Three‑way ANOVA (material type, surface treatment, and
Half the specimens were stored dry at 37°C for 7 days and storage condition) revealed that both, type of composite
then tested for interlayer SBS. material and the surface treatment given, had significant
effects on the interlayer SBS (P < 0.001).
The other half were stored in distilled water for
48 h at room temperature (23 ± 1°C) and then The difference between the dry and the thermocycled
thermocycled (alternating immersion of the samples specimens was not statistically significant (P > 0.001).
in distilled water of a temperature of 5° and 55°C) for
6000 cycles, with a dwell time of the 30 s and a transfer DISCUSSION
time of 5 s. The specimens were then tested for interlayer
SBS. Dental composites get cured by free‑radical‑induced
polymerization reaction which is strongly inhibited by
Testing of interlayer shear bond strength free‑radical scavengers such as oxygen in the air. This
The SBS test was performed using a universal free oxygen in contact with composite resin diffuses and
testing machine at room temperature (23 ± 1°C). inhibits polymerization reaction forming peroxide radicals
The specimens were mounted in a mounting jig and that have low reactivity toward monomers.[1] This free
a circular edge blade created the shear type load monomer layer remaining on the surface after curing is
positioned over the interface between the substrate known as the oxygen‑inhibited layer.
and the adherent material at a crosshead speed of 1.0
mm/min until fracture. The shear load at failure was
recorded as shown in Figure 2. R + O2 → R – OO (stable radicals).[15]

256 Journal of Conservative Dentistry | Volume 23 | Issue 3 | May-June 2020

 Panchal and Asthana: Effects of oxygen inhibition layer on shear bond strength

The present study shows results in accordance with the

study of Koga et al.,[18] which showed that both the physical
and chemical surface properties of the OIL depend on
its thickness if relatively thin, the OIL allows diffusion of
the photoinitiator into the overlaying composite, thus
improving the bond strength.
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Water spray and ethanol treatments used in this present

study are clinically more practical methods. They were
applied for a controlled time of 20 s, and adverse bonding
effects were not observed following either surface
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Graph 1: Effects of surface treatments on the thickness of the treatment.[19]

oxygen inhibition layer on composites (three‑way ANOVA)
The OIL thickness of SiC paper‑treated groups was assumed
Table 2: Oxygen inhibition layer thickness value of all to be zero, as the grinding procedure removed the OIL
materials seen by stereomicroscope as confirmed microscopically. The mechanical polishing
Group 1 – Nanohybrid composite process not only removes the original surface of the
Thickness of oxygen inhibition layer (micron) composites but also removes the silane layer on the filler
Subgroup 1A (untreated surface) - 19.8 (5.5)*
Subgroup 1B (ethanol-treated surface) - 19.0 (5.7)* surface of composites which reduces the bond strength
Subgroup 1C (water spray-treated surface) - 19.4 (4.7)* between increments due to inadequate wetting of resin to
Subgroup 1D (SiC treated) - Nil the fillers as discussed by Vankerckhoven et al.[20]
Group 2 – Microhybrid composite
Thickness of oxygen inhibition layer (micron) The composite material and the surface layer treatment,
Subgroup 2A (untreated surface) - 17.78 (5.5)*
Subgroup 2B (ethanol-treated surface) - 17.19 (5.7)* both, affected the interlayer SBSs. The outcome for
Subgroup 2C (water spray-treated surface) -17.4 (4.7)* both dimethacrylate‑based composites (nanohybrid and
Subgroup 2D (SiC treated) - Nil microhybrid) was improved interlayer SBS when the OIL
Group 3 – Short glass fiber composite was present. This finding supports the influence of the
Thickness of oxygen inhibition layer (micron) physical surface properties of the OIL on the bond strength
Subgroup 3A (untreated surface) - 20.8 (5.5)*
Subgroup 3B (ethanol-treated surface) - 20.3 (5.7)* between incrementally placed composite layers and also
Subgroup 3C (water spray-treated surface) - 20.5 (4.7)* its influence on the failure mode. Therefore, it can be
Subgroup 3D (SiC treated) - Nil suggested that the surface wettability provided by the OIL
Values are given as mean (SD). The superscript symbols (*) within a value
is crucial for the adhesion of the adherent surface. Factors
represent a homogenous subset (P>0.05) among the groups for each material
individually. SD: Standard deviation such as the surface free energy of the solid and the surface
tension of the liquid influence wettability.[18]
As multilayer techniques are recommended to minimize
polymerization shrinkage as well as to increase the Among the three groups, Group 3 showed a higher
degree of conversion of dental composites, therefore, the interlayer bond compared to both nanohybrid and
interlayer bond strength achieved becomes an important microhybrid composites irrespective of any surface
consideration. Some studies on how the OIL affects bond treatment and storage condition. The above result can be
strength described a positive correlation, indicating explained in the context of the chemical composition of
that the OIL increased bond strength.[16] Kim et al. in each composite [Table 1].
2006 concluded that when the OIL was missing or too thin,
the absence or shortage of the unreacted monomers could The type of composite material and surface treatment
have failed to connect both sides chemically and also failed given had significant effects on failure mode too. Surface
to resist the shrinkage stress.[17] treatment of OIL with ethanol and water spray may have
extracted some unpolymerized monomers, which, in turn,
Among the three groups, SGFR composite (Group 3) showed influence the bond strength, which is evident as cohesive
a maximum thickness of OIL, followed by nanohybrid and breaks, observed among all groups. Predominantly,
least thickness of OIL in microhybrid. The plausible reason is, cohesive fractures were observed in SGFR composites,
composites impregnated with glass fiber may contain some where surface treatment was done with SiC, possibly due
voids between the fibers due to their orientation, and these to micromechanical interlock between monomer from
voids between the single fibers are assumed to be oxygen overlaying composite and fibers of underlying composite
reservoir which allows oxygen to inhibit polymerization exposed during the grinding procedure. The SiC treated all
deeper in the structure of the SGFR composite.[9‑12] groups resulted in the lowest interlayer bond strengths.

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 Panchal and Asthana: Effects of oxygen inhibition layer on shear bond strength

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258 Journal of Conservative Dentistry | Volume 23 | Issue 3 | May-June 2020