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In situ observation on the failure behavior of ZrO2-resin-dentin bonding

interface with prefabricated indentation defects
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 Mater. Res. Express 7 (2020) 085401 https://doi.org/10.1088/2053-1591/aba9f5

PAPER

In situ observation on the failure behavior of ZrO2-resin-dentin

OPEN ACCESS
bonding interface with prefabricated indentation defects
RECEIVED
14 May 2020
Zhichao Ma1,2,3, Hongzhao Zhang1,2, Dongni Liu1, Hongwei Zhao1,3,4,6 , Yan Feng5,6 and Luquan Ren3,4
REVISED 1
16 July 2020
School of Mechanical and Aerospace Engineering, Jilin University, Changchun, 130025, People’s Republic of China
2
Key Laboratory of CNC Equipment Reliability, Ministry of Education, Jilin University, Changchun, 130025, People’s Republic of China
ACCEPTED FOR PUBLICATION 3
Weihai Institute for Bionics-Jilin University, Weihai, 264207, People’s Republic of China
28 July 2020 4
Key Laboratory of Bionic Engineering Ministry of Education, Jilin University, Changchun, 130025, People’s Republic of China
PUBLISHED 5
Dental Center, 964th Hospital of PLA, Changchun, 130021, People’s Republic of China
7 August 2020 6
Authors to whom any correspondence should be addressed.
E-mail: [email protected] and [email protected]
Original content from this
work may be used under Keywords: dental restoration, in situ test, bonding failure, interfacial cracking, dentin
the terms of the Creative
Commons Attribution 4.0
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Any further distribution of
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Abstract
attribution to the Interfacial cracking and fracture of restorative materials are major obstacles to realize effective dental
author(s) and the title of
the work, journal citation restoration. Especially, the bonding failure of compound interfaces consisting of dentin, resin and
and DOI.
zirconium dioxide (ZrO2) ceramic, exhibit complexity, variability and unpredictability due to the
complicated loading type and oral environment. By using a self-developed miniaturized horizontal
device integrating with thermostatic artificial saliva, an approximate oral environment was established
to investigate the failure mechanism of ZrO2-resin-dentin compound interfaces. Through real-time
in situ observation of shearing deformation behaviors of the dentin-resin and resin-ZrO2 interfaces,
the continuous propagation processes of cracks nucleating from the interfacial intersection line or
dentin’s interior were analyzed in detail. The discontinuous cracking behaviors revealed the prior
crack of resin-ZrO2 interface, which attributed to the acid etching of dentin and significant gradients
in Young’s modulus and hardness compared with the corresponding parameters of dentin-resin
interface. The significant interfacial differences in mechanical properties promoted the crack
nucleation and induced the bonding failure. A widest crack with a width of 1.4 μm inside the dentin
was also observed from the fractured ZrO2-resin-dentin specimen. This paper focused on the
discontinuous interfacial cracking behaviors and bonding failure mechanisms of ZrO2-resin-dentin
specimen, which would be beneficial to the research of novel composite resins and the improvement
of bonding processes.

1. Introduction

Dental bonding restoration is an effective therapeutic method to directly cure tooth fractures, dental caries and
tooth erosion. Although a series of dental restorative materials, including metals [1] (Ni–Cr Alloy, Co–Cr Alloy
and Ti Alloy, etc), composite resins [2–4] and ceramic materials [5, 6] (feldspar ceramics, Al2O3 ceramics and
ZrO2 ceramic, etc), have been widely used, the strength and reliability of bonding interface need to be further
improved. Regarding the dentin restoration, although the demineralization process by acid etching [7] and
wettability enhancement could promote the infiltration of resin and produce cured mixed layer with thickness
with range from 2 μm to 10 μm [8], the interfacial cracking is still a major problem far away from mature
solution. The continuous interfacial cracking behavior and critical failure mechanism need to be taken into
account. Meanwhile, the dentin restoration in clinical scenario based on ZrO2 ceramic and resin exhibited
advantages in strength, manufacturability, appearance, wear resistance [9] and thermal stability [6], due to the
stable chemical properties, high strength, excellent crack resistance and biocompatibility of ZrO2 ceramics. The
infiltration effect of resin into the microporous structure of dentin could also realize the enhancement of
bonding strength [10].

© 2020 The Author(s). Published by IOP Publishing Ltd

Mater. Res. Express 7 (2020) 085401 Z Ma et al

Considering the variability of oral environment, service temperature, multi-oriented and static-dynamic
coupling characteristics of chewing forces [11, 12], the bonding cracking failure of ZrO2-resin-dentin
compound interfaces exhibited the diversity of failure behaviors [13, 14]. Meanwhile, as a typical brittle material,
ZrO2 ceramic might suffer from fracture risk due to the internal defects and variable loading types, including
hard particle scratch, interfacial shearing, surface friction and compressive cyclic loading [15]. The observation
of crack nucleation and propagation behaviors of compound interfaces was particularly important for
understanding the failure mechanisms [9, 16]. Especially, the real-time observation of crack evolution [17–19]
could reveal the discontinuous behaviors of compound interfaces and confirm the critical stress or strain
conditions leading to the nucleation of microcracks, which was beneficial to the researches of novel composite
resins development and the improvement of bonding processes [20]. Regarding the testing of bonding behavior
and failure mechanism of interfaces, etching steps and mechanical loads were important factors determining the
bonding strength [21]. Frankenberger et al systematically investigated the marginal integrity of dentin adhesives
subjected to thermo-mechanical loading, through the transmission electron microscopy analysis of a large
number of fracture morphologies, a two-step self-etch adhesives was proved as optimal adaptation to dentin
[22]. Luong et al revealed that low-viscosity resin improved the bonding strength of dentin, their tensile tests also
verified that the bonding strength of dentin and resin composite significantly decreased after 104 thermocycles
[23]. Meanwhile, considering the actual service condition of compound interfaces, in situ shearing tests could
equivalently investigate the continuous interfacial shearing behaviors and bonding failure mechanisms [17, 24].
Furthermore, according to our previous studies, prefabricated defects with large stress concentration coefficient
could be benefit to confirm the crack nucleation and facilitate the real-time observation of crack
propagation [25].
Regarding the ZrO2-resin-dentin compound interfaces, effective experimental methods are needed to
directly observe the continuous micro deformation behaviors and reveal the bonding failure mechanisms. In
this study, through the establishment of an experimental system integrating with approximate oral
environment, miniaturized in situ testing device and constant temperature control unit, the real-time
observations of evolution processes of the dentin-resin interface and resin-ZrO2 interface, the crack nucleation
and propagation behaviors and interfacial bonding failure mechanisms were experimentally investigated in
detail. The interfacial difference in mechanical properties was considered as the main influencing factor to
induce the bonding failure. The discontinuous fracture behavior of compound interfaces attributed to the
interface differences and prefabrication of indentation defects was also regarded as a research hypothesis.

2. Materials and methods

2.1. Specimen preparation

Taking the crown section of premolars from 18 to 60 years-old adults as experimental materials, which were
stored in deionized water at 4 °C [26] and subsequently immersed in normal saline solution containing
900 mg l−1 NaCl buffered with 57.5 mg l−1 CaCl2. The immersion treatment in deionized water would prevent
dehydration during the reservation process. Meanwhile, compared with artificial saliva, the immersion
treatment in normal saline would prevent subsequent potential spoilage and performance degradation. As stated
by Gustafson et al, the immersion in normal saline for a long time (6 days) will weaken the Young’s modulus
[27], therefore, the immersion lasted for 2 h to weaken the influences and maintain the equilibrium of Ca ion.
Symmetrical double L-shape specimens were prepared as shown in figure 1. Ethical approval for the collection of
premolars were obtained from institutional ethics review boards. Regarding the preparation procedures,
clinically collected dentin with L-shape was adhered with ZrO2 ceramic after etching by using light cured
composite resin (3M-resin-250, mainly consisted of silanized zirconia, ethylene dimethacrylate, silica and
2-Hydroxy-4-methoxybenzophenone, producer: 3 M ESPE, Germany) and bonding agent (mainly consisted of
2-methyl-2-acrylic acid 1, 2-hydroxyethyl methacrylic acid, photoinitiator, 3 M AdperTM, producer: 3 M ESPE,
Germany). Each ZrO2-resin-dentin adhesive specimen was prepared through bonding a couple of L-shape
dentin and ZrO2 ceramic. Figure 1(a) illustrates the sampling direction of clinically collected dentin, which was
cut from the direction perpendicular to occlusal surface. The enamel layer was removed through cutting and
subsequent mechanical polishing. Precise dental saw (AUTOFOR, YC22) with thickness of 0.2 mm and external
diameter of 22 mm was used to prepare rectangular dentin specimen. The rotation speed was set as
1000 r min−1. Then, with the aid of two degrees of freedom precision positioning platform (Supereyes, Z007)
integrated with digital microscope, the clinically collected extracted dentin (supplied by Dental Center, 964
Hospital of PLA) was firstly sliced into stepped L-shape with height difference of 1.5 mm, the inner side of the
specimen’s thinner part was the adhesive surface, which was cleaned ultrasonically for 10 s [28] and polished by
using diamond abrasive pastes with decreasing particle sizes ranging from 5 μm to 0.5 μm. By using an optical
microscope (Olympus DSX500) with a high depth of field and three-dimensional imaging function, the surface

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Mater. Res. Express 7 (2020) 085401 Z Ma et al

Figure 1. (a) Illustration of the sampling direction and method of L-shape ZrO2-resin-dentin adhesive specimen and (b) Indentation
preparation procedures of adhesive specimen with prefabricated indentation defects.

profile of polished dentin side was captured as shown in figure 1(b), and an average surface roughness was
measured as approximate 0.96±0.24 μm through line profile analysis, the mean value of roughness was
calculated based on 10 polished ZrO2-resin-dentin specimens and 50 randomly selected paths. Meanwhile,
ZrO2 ceramic with the same L-shape was fabricated by following a sequence of steps involving design of L-shape
3D model, stereolithography and high temperature sintering. The adhesive surface of dentin specimen was acid
etched before applying bonding agent by using phosphoric acid with concentration of 37% ± 2% (Gluma
Comfort Bond, producer: Heraeus Kulzer, Germany), the acid-etch time lasted for 30 s, then dentin specimen
was rinsed by distilled water. Then the bonding agent was brushed on the inner side of previously prepared
L-shape dentin twice using with uniform brushing time of 15 s and interval time of 20 s followed by 20 s light
curing. Then the resin was uniformly coated on both bonding surfaces followed by ultraviolet light curing lasting
for 30 s [29]. As a matter of fact, as the ZrO2-resin-dentin specimens were placed on the 2D precision positioning
platform, the tip of the light-cure lamp was right above the specimen’s surface with a constant height distance of
10 mm. With the aid of linear motion function of the platform, the relative motion trajectory of
ZrO2-resin-dentin specimens was along the direction of the composite interface. The thickness of resin between
dentin and ZrO2 was controlled by applying equivalent chewing force. A pre-compressive load of 100 N lasting
for 5 min was directly applied on the compound interface through a compressive device integrated with S-type
load sensor (BBS, Transcell), considering the natural chewing force with range from 30 N to 200 N [30]. As
shown in figure 1(b), the average interface thickness was measured as 316.2±36.7 μm.
In order to confirm the crack nucleation location and facilitate the observation of crack propagation, a series
of prefabricated Vickers indentation defects were prepared on the dentin-resin interface (defined as Interface I)
and resin-ZrO2 interface (Interface II), respectively. The prefabrication of Vickers indentation complied with
the requirement of International standard: ISO 6507-1-2018 [31]. The prefabricated indentation defects would
contribute to the analysis of the differential crack evolution behaviors at both interfaces. Based on identical
indentation loads of 10 N and dwell time of 15 s, the residual indentation imprints exhibited different
morphologies due to the differences in hardness and Young’s modulus of dentin and ZrO2 ceramic. Specifically,
the residual morphology on Interface I manifested as a regular rectangle imprint. However, compared with
Interface I, the differences in mechanical properties between ZrO2 ceramic and resin significantly affect the
indentation morphology on Interface II, and the overall dimension of residual indentation was relatively
smaller. Obvious plastic deformation accumulation was observed on the resin’s side. Meanwhile, the relatively
smaller and sharper morphology on the ZrO2 ceramic’s side was attributed to the continuous sliding behavior of
the Vickers indenter on the ZrO2 ceramic’s surface during the quasi-static indentation process.

2.2. Mechanical properties

Since the difference in mechanical properties affected the residual indentation morphologies, the critical
condition leading to the crack nucleation could be definitely related to the surface mechanical properties. By
using nanoindentation techniques (Agilent 200), a set of continuous testing locations along with a virtual path

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Mater. Res. Express 7 (2020) 085401 Z Ma et al

Figure 2. (a) Indentation load-depth responses of ZrO2-resin-dentin specimens on basis of constant indentation load of 200 mN, and
(b) illustrates corresponding Young’s modulus and hardness obtained from the load-depth curves to verify the significant differences
in mechanical properties.

passing through and perpendicular to the two parallel adhesive interfaces were selected to obtain the Young’s
modulus and hardness of various locations. Seen from figure 2(a), on basis of constant indentation load of 200
mN and dwell time of 20 s, significant differences in indentation responses were obtained, as the indentation
load-depth curves exhibited different maximum depths hm and residual depths hf dependent with the testing
locations. Regarding the ZrO2 and dentin sides, the average hm obtained from the curves were calculated as 0.83
μm and 1.85 μm, respectively. The indentation responses of resin side exhibited an average hm of 5.64 μm.
Considering that the slope of unloading curve could determine the hardness and Young’s modulus [32], the
gradient effect adjacent to the dentin-resin interface and resin-ZrO2 interface might cause asynchrony of
interfacial cracking behaviors. Specifically, 20 sets of indentation experiments were carried out in order to
reduce the experimental error. As shown in figure 2(b), with regard to the ZrO2, resin and dentin sides, the
calculated Young’s modulus and hardness were 190.66±23.62 GPa, 9.71±2.12 GPa, 86.55±13.28 GPa and
10.05±2.2 GPa, 0.29±0.27 GPa and 4.07±1.12 GPa, respectively. The average modulus ratios of ZrO2 to
resin and dentin to resin were 19.63 and 8.91, respectively. The corresponding hardness ratios were 34.66 and
14.03, respectively. The significant gradients in Young’s modulus and hardness of resin-ZrO2 interface might
promote the crack nucleation and affect the bonding cracking failure [33].

2.3. In situ testing device

A modified miniature horizontal device integrating with tensile/compressive loading function [34] was used to
carry out the equivalent shearing tests of ZrO2-resin-dentin specimens. According to our previous study [35], a
water bath integrated with a couple of heating rods and thermocouple was mounted at the specimen clamping
region between a couple of symmetrical columns with flat steps. Seen from figure 3, a medium container filled
with artificial saliva was placed inside the water bath. The thermostatic medium environment was achieved
based on closed loop control of water temperature. Therefore, through integrating with the container filled with
thermostatic artificial saliva, combined with the real-time observation of surface microstructure evolution by

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Figure 3. In situ testing device integrating with 3D imaging function and thermostatic artificial saliva.

using an optical microscope (Olympus DSX500) with a high depth of field and three-dimensional imaging
function, an in situ testing system under approximately thermostatic oral environment was established. When
subjected to a quasi-static compressive load, considering the orientations of compound interfaces were parallel
to the loading direction, the symmetrical double L-shape specimens sustained equivalent interface shear stress.
During the tests, constant temperature of 36.8 °C and quasi-static strain rate of 10−4/s were set. The prepared
double L-shape ZrO2-resin-dentin specimen was clamped between a couple of support columns, and a pair of
symmetrical flat steps on the columns were fabricated to weaken the misalignment during uniaxial testing. On
basis of a driving unit consisting of a high-power servo motor, two-stage worm gears and a ball screw with left-
and right-hand thread at the left and right ends, respectively, a maximum load of 2335 N, a uniaxial stroke of
8 mm and minimum loading speed of 10 nm s−1 were achieved. During the imaging process, due to the self-
locking function of worm gears, the imaging with high resolution could be obtained as the device could
momentarily stop before imaging [36]. Meanwhile, the left-and right-hand thread of ball screw could also
guarantee the relative stationary of indentation defects (as the observation target) during the shearing tests and
imaging process.

3. Results and discussions

3.1. Discontinuous deformation behaviors

By using the established in situ testing system under approximate oral environment, the crack evolution
behaviors nearby the prefabricated Vickers indentations defects on dentin-resin interface (Interface I) and
resin-ZrO2 interface (Interface II) were obtained through the real-time observation. When subjected to an
equivalent interfacial shearing load, the compound interfaces exhibited different crack propagation and
bonding failures behaviors [37]. As shown in figure 4(a), the load response showed segmented linear monotonic
increasing trends. From initial loading to 160.8 N, the ZrO2-resin-dentin specimen elongated linearly with a
relatively large slope. From 160.8 N to ultimate fracture, the equivalent shearing load gradually increased with a
relatively lower slope as a function of time, which indicated a discontinuous fracture process of the compound
interfaces [38]. Combined with the optical morphologies of a couple of a group of parallel compound interfaces,
the indentation microregions exhibited diversified deformation behaviors as illustrated in figure 4(b). On basis
of external load of 93.9 N, regarding Interface I, plenty of multi-oriented microcracks nucleating inside the
indentation imprint and a group of microcracks converging towards the Vickers indentation edge perpendicular
to Interface I were observed on the sides of dentin and resin, respectively. The orientation difference was
probably mainly attributed to the porous structure of dentin after acid etching treatment and isotropy and
amorphous properties of resin. The porous structure of dentin effectively restrained the crack propagation due
to the anti-cracking effect, and the stress concentration effect adjacent to the indentation edge at resin side
facilitated the convergence of microcracks. Meanwhile, the microcracks nucleation adjacent to the interface
exhibited approximately parallel orientations attributed to the significant differences in interface mechanical
properties. The main crack continuously propagated until a significant main crack formed along Interface I
inside the Vickers indentation when the load increased to 227.2 N. Until the final fracture occurred when
subjected to a shearing load of 247.9 N, no obvious interfacial cracking was visible. As a matter of fact, the

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Mater. Res. Express 7 (2020) 085401 Z Ma et al

Figure 4. (a) Shearing load response of ZrO2-resin-dentin specimen as a function of time and (b) discontinuous cracking processes of
dentin-resin (I) and resin-ZrO2 (II) interfaces.

microcracks nucleation locations were widely observed at dentin side, resin side and the interface, and the
microcracks located at interface I could be considered as the sources to induce the continuous crack propagation
and formation of main crack. Regarding Interface II, the resin inside the indentation imprint experienced
extrusion cracking, extrusion release, planarization of extrusion deformation and generation of residual crack
after fracture, successively. When subjected to a shearing load of 93.9 N, crack nucleation was also observed on
the ZrO2 side. Initial interfacial cracking and indentation edge cracking were also observed when the load further
increased to 160.8 N. On basis of 227.2 N, simultaneous interfacial cracking on both sides of indentation were
observed, but the surficial rather than internal cracking was confirmed as the indentation bottom did not crack
completely. Meanwhile, a circular arc crack profile inside the indentation imprint was observed, which
demonstrated the brittle cracking of ZrO2 ceramic contributed to the bonding failure of resin-ZrO2 interface.
Furthermore, when subjected to an equivalent shearing load of 247.9 N, the resin-ZrO2 interface completely
cracked, accompanied with the falling of previously formed ZrO2 fragment. Therefore, the actual fracture
process of ZrO2-resin-dentin specimen consisted of three processes, including initial interface cracking with
mainly elastic extension, crack propagation with remarkable plastic flow [39] and interfacial separation failure.
Regarding the dentin-resin interface, although the prefabricated Vickers indentation defects with edge length of
tens of microns has leaded to significant stress concentration effect, and plenty of multi-oriented microcracks
nucleating inside the indentation imprint were visible, the interfacial cracking failure appeared at the resin-ZrO2
interface. Seen from the ultimate cracked interface, the competition between the Young’s modulus or hardness
gradient of resin-ZrO2 interface and the stress concentration factor induced by Vickers indentation determined
the crack propagation process and location of complete fracture failure.
Regarding the resin-ZrO2 adhesive interface, the interface separation process was quantitatively described by
analyzing the crack width and depth evolutions as a function of shearing load. Seen from the shearing load
responses of ZrO2-resin-dentin specimen as shown in figure 4(a), based on a shearing load of 93.9 N, multi-
oriented microcracks were observed at various regions, the crack propagation behaviors under relatively larger
shearing loads with range from 93.9 N to 200.5 N were taken into account. The crack width and depth evolution
analyses were based on 10 double L-shape specimens with identical preparation process and loading conditions.
As illustrated in figure 5(a), approximate linear increasing trend of crack width was obtained. The combined
effects of prefabricated Vickers indentation and interfacial shearing load induced significant bonding cracking
with crack width of 4.09 μm under a relatively lower shearing load of 93.9 N. As shown in figure 5(b), with
increasing load ranging from 120.6 N to 200.5 N, the corresponding crack width presented a monotonic
increasing trend with range from 6.04 μm to 11.69 μm. Through linear fitting, the linear correlation coefficient
R2 of width-load curve was calculated as 0.9953. With the aid of an optical microscope (Olympus DSX500) with
three-dimensional imaging function and z-axis resolution of 0.01 μm, typical dimple-like crack region was
selected to equivalently calculate the crack depth. Similarly, the approximate linear increasing of crack depth was
described as shown in figure 5(c) with linear correlation coefficient R2 of 0.9912. Meanwhile, although the
observed microregions exhibited height difference with specific gradient, the crack depth was determined as the
height difference between the average height of neighboring microregions along the interface and the lowest
point of dimple-like crack. As shown in figure 5(d), with increasing load ranging from 93.9 N to 200.5 N, the
corresponding crack depth also presented a monotonic trend with range from 3.72 μm to 10.33 μm.

3.2. Interfacial cracking width

Since the discontinuous fracture processes of compound interfaces were directly observed through in situ
shearing tests under microscope, and the resin-ZrO2 interface has already completely fractured prior to the

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Mater. Res. Express 7 (2020) 085401 Z Ma et al

Figure 5. (a) Crack width evolution as a function of shearing load and corresponding (b) separation process of the resin-ZrO2 adhesive
interface, (c) and (d) illustrate corresponding depth evolution as a function of shearing load and crack depths of dimple-like crack
regions.

Figure 6. SEM images of dentin-resin interface to confirm the location and width of cracks.

dentin-resin interface, the ultimate morphology of not yet completely fractured dentin-resin interface was
characterized as illustrated in figure 6. As a matter of fact, although macroscopic cracks were not directly
observed at the interface, the scanning electron microscopy images also indicated intermittent interfacial cracks
[40]. The width of the widest microcrack was measured as 1.4 μm. Meanwhile, the location of the surface crack
initiation did not originate from the dentin-resin interface but dentin’s interior. The minimum spacing between
the dentin-resin interface and intermittent cracks, which were approximatively parallel to the interface, was
calculated as 2 μm. Furthermore, although the Vickers indentation with edge length of tens of microns has
induced significant stress concentration effect, the crack propagation path intersected the indentation edge at a
clear point and stopped continuous extension inside the indentation imprint, which demonstrated that the
cracks nucleated from the dentin’s interior under quasi-static shearing stress. The complete fracture of
resin-ZrO2 interface prior to the dentin-resin interface was attributed to the acid etching of dentin [41–43] and
significant gradients of interfacial mechanical properties, as a 2.2 times modulus ratio and 2.4 times hardness
ratio of resin-ZrO2 to dentin-resin interfaces have been experimentally confirmed.

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Figure 7. Microstructures of complete fractured resin-ZrO2 interface with residual (a) resin and (b) ZrO2 morphologies to illustrate
the low stress cracking behaviors.

3.3. Interfacial morphologies

The microstructures of complete fractured resin-ZrO2 interface were also analyzed to indirectly verify the effect
of acid etching on the interfacial bonding strengthening effect. As shown in figure 7, because the bonding process
of resin-ZrO2 interface did not involve an acid etching treatment, both the resin and ZrO2 surfaces manifested as
approximately flat and smooth features, which weakened the interfacial bonding strength. The resin layer
manifested as a general smooth shear surface under quasi-static interfacial shearing stress intersected with stripe
shaped residual resin due to the locally inhomogeneous plastic flow of resin. Meanwhile, discrete residual resins
were observed distributing on the ZrO2 surface unevenly. Residual resins were mostly round or elliptical in
shape with maximum single residual area of approximate 700 μm2 (diameter of 30 μm). With the aid of machine
vision technology, through the chromatic aberration analysis and image recognition [44], the actual residual
area of resin on ZrO2 ceramic surface was less than 5%, which directly caused the low stress cracking of
resin-ZrO2 interface. According to the previous research hypothesis, the researches above indicated that the
in situ experimental study was useful to investigate the problematic dentin interface restorations, and the
interfacial difference in mechanical properties was verified to induce the bonding failure and discontinuous
fracture behavior ZrO2-resin-dentin compound interfaces. However, this study was unable to achieve the in situ
testing under actual oral environment. Meanwhile, considering that the cyclic loading caused by repeated
chewing force would lead to interface fatigue failure, the in situ fatigue testing of ZrO2-resin-dentin specimen
would be benefit to reveal the micro failure mechanism and comply with the requirements of clinical scenario.

4. Conclusions

Discontinuous fracture behaviors of ZrO2-resin-dentin bonding interfaces were experimentally revealed

through equivalent in situ interfacial shearing tests. Controllable shearing load and thermostatic medium

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environment filled with artificial saliva were realized to carry out the in situ tests under approximate oral
environment. Interfacial difference in mechanical properties induced the low stress fracture (from the external
to internal) of resin-ZrO2 interface. With regard to the dentin-resin interface, the acid etching treatment and
relatively closer modulus or hardness differences between dentin and resin effectively restrained the interface
cracking. Compared with bonding strengthening effect by acid etching of dentin, the low stress fracture and
adhesion weakening of resin-ZrO2 interface were mainly attributed to the significant differences in modulus
ratio (19.63) and hardness ratio (34.66) of ZrO2 to resin, which promoted the crack nucleation and contributed
to the interfacial separation and ultimate bonding failure.

Acknowledgments

This work is funded by the National Natural Science Foundation of China (51875241, U1601203), National Key
R&D Program of China (2018YFF010124, YS2018YFA070002) and Jilin Province Science and Technology
Development Plan (20190302078GX, 20180201126GX).

ORCID iDs

Hongwei Zhao https://orcid.org/0000-0003-4746-389X

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