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Shear bond strength, finite element analysis, flexural strength and accuracy analysis
of additively manufactured bio-inspired 3Y-TZP for dental applications
Zengqi Ye, Li Zhu, Tianhong Zhou, Xian Tong, Zhaoping Chen, Xin Zhou, Shengbin
Huang, Yuncang Li, Jixing Lin, Cuie Wen, Jianfeng Ma
PII: S2238-7854(24)00458-7
DOI: https://doi.org/10.1016/j.jmrt.2024.02.164
Reference: JMRTEC 10090
Please cite this article as: Ye Z, Zhu L, Zhou T, Tong X, Chen Z, Zhou X, Huang S, Li Y, Lin J, Wen
C, Ma J, Shear bond strength, finite element analysis, flexural strength and accuracy analysis of
additively manufactured bio-inspired 3Y-TZP for dental applications, Journal of Materials Research and
Technology (2024), doi: https://doi.org/10.1016/j.jmrt.2024.02.164.
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dental applications
Zengqi Ye a, Li Zhu a, Tianhong Zhou a, Xian Tong a, Zhaoping Chen a, Xin Zhou a,
Shengbin Huang a, Yuncang Li b, Jixing Lin a*, Cuie Wen b*, and Jianfeng Ma a*
a
Institute of Stomatology, School and Hospital of Stomatology, Wenzhou Medical
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University, Wenzhou 325027, China
b
School of Engineering, RMIT University, Melbourne, Victoria 3001, Australia
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Abstract
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Weak shear bond strength (SBS) has always been a challenge for clinical bonding of
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zirconia to form precise complex structures and achieve bionic structure molding based
microstructure, and mechanical behavior. As report goes, the toe structure of tree frog
can effectively achieve friction enhancement on humid and flooded surfaces. In this
paper, we present a new type of 3Y-TZP material loaded with tree-frog bionic structures
via VPP additive manufacturing to improve SBS between resin cement and 3Y-TZP for
Corresponding authors.
E-mail addresses: jixing.lin@wmu.edu.cn (J. Lin), cuie.wen@rmit.edu.au (C. Wen), mjf@wmu.edu.cn (J.
Ma)
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clinical requirements. And flexural strength, finite element analysis and accuracy
application. The SBS of the bio-inspired group with 250 μm width and 250 μm height
reached a maximum of 22.7±1.3 MPa before hydrothermal aging, the flexural strength
of the bio-inspired group with 250 μm width and 150 μm height decreased the least,
reaching 825±30 MPa, and the accuracy analysis of the central-incisor veneer
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restoration loaded with the bionic structures showed that the average deviation value
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was 0.033±0.036 mm. This study has found that these bionic structures can effectively
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improve the SBS of the interface between zirconia and resin cement, while flexural
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strength and accuracy can also meet requirements of clinical dental application.
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1. Introduction
materials have been the mainstream choice for inlays, single crowns, and partial fixed
dentures due to their excellent mechanical properties [1]. However, a common reason
for the failure of clinical treatments using 3Y-TZP is retention loss [2], which indicates
that the shear bond strength (SBS) between the internal tissue surfaces of the zirconia
and the abutment has not yet fully met the requirement of clinical application, especially
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micro-mechanical structure to promote the bonding effect by means of hydrofluoric acid
etching as in glass ceramics [3]. Therefore, many scholars have investigated the
hot-acid etching [6], sol–gel silicon coating [7], and so on. But those pretreatment
methods are relatively complex which also makes them unsuitable for wide use in
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clinical applications.
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Multi-scale concave–convex textures are widely found on the interfaces of biological
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tissues in nature. For example, amorphous calcium carbonate grows to form a plate-like
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mineral phase in the nacreous interlocking structure to form the micro-morphology of
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bricks and mortar in order to achieve better flexural strength [8-10]. This type of
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interlocking structure of similar matrixes can also be found in the human skull to ensure
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the stable deposition of calcium salts during bone growth and development [11]. In
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recent years, scholars have conducted in-depth research on the anti-adverse sliding
phenomenon of the tree frog's feet. This multi-scale layered columnar structure gives
the tree frog a strong natural adhesion capability, greatly improving the viscous bonding
of the interfaces [12-14]. However, due to the limitations of the manufacture technology,
the effect of these textures on the bonding performance of dental ceramics has not yet
been reported.
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has been continuously optimized and applied in various fields. This technology provides
promising dental application by virtue of its control of complex shapes and internally
precise structures [15, 16]. In terms of accuracy, our research group has found that a
excellent fitting accuracy similar to that of a single crown via subtractive milling
method [17].
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Therefore, inspired by the natural biological texture of the feet of tree frogs, this study
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prepared 3Y-TZP veneers with bionic tree-frog structures using VPP to enhance the
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SBS. At the same time, the effect of the load on the mechanical properties of the
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structure is verified.
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The 3mol% yttrium oxide stabilized zirconia powder (3Y-7, Guangdong Orient Zirconic
Ind. Sci. Tech. Co., Ltd., China), pre-mixed resin solution (GTC-1, Kunshan Porimy Co.,
Ltd., China), and photoinitiator (TPO, Kunshan Porimy Co., Ltd., China) were mixed
according to the proportions given in Table 1. 3Y-TZP slurry with a solid content of
46.5 vol.% was obtained by fully grinding the mixture in a planetary ball mill for 10 h,
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Table 1. Components of 3Y-TZP Slurry
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diphenyl (2,4,6-trimethylbenzoyl) phosphine oxide.
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2.2 Digital model construction
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Materialise Magics 24.1 3D printing modeling software was used to design a printing
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model. As shown in Fig.1, the prism span (W) and height (H) was designed to be 250
μm, 350 μm or 450 μm and 150 μm, 250 μm, 500 μm, or 750 μm, which defined the
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as a 1.5 mm×4 mm×25 mm rectangular block for the three-point bending-strength test
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and as a 3 mm×10 mm×10 mm rectangular block for the SBS test. A turbine and
diamond bur are used to evenly grind the labial surface of the central incisor on dental
model for nearly 0.5mm. After preparation of teeth on dental model and scanning by the
intraoral scanner, a digital veneer restoration model of central incisor was obtained
using 3Shape Dental System CAD software, which was then loaded with the bionic
tree-frog structure at Materialise Magics 24.1.
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Fig.1. Structure diagram of bionic tree frog veneer. “a” refers to the length ofthe
prismatic side of the structural unit , “w” refers to the span betweenstructural units, “H”
refers to the prism height of the structural unit
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2.3 VPP printing and sintering
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The model was imported into a ceramic VPP printing device (GTC-1, Kunshan Porimy
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Co., Ltd., China). The printing used appropriate printing parameters: the thickness of
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each layer was 25 μm and the laser power was 1.138 W/cm2. The debinding and
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sintering process is shown in Fig. 2 using muffle furnace (1700X, Shenyang Kejing
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2.4 Compositional and microstructural analysis
The specimens were scanned using X-ray diffraction (XRD; SmartLab 9kW, Rigku,
Japan) with Cu–Kα radiation at RT. The recording of the XRD mode was applied in the
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2.5 SBS testing before and after hydrothermal aging
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The control group, sandblasting group and the experimental groups were prepared for
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SBS testing. The specimens were ultrasonically cleaned in distilled water for 10 min,
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then in alcohol for 5 min, finally dried at 80 °C in a drying cabinet. After cooling, their
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surfaces were coated with Z-prime plus (B-6002P, BISCO, USA), and rested for 6 min
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at RT. The sandblasting group was sandblasted with alumina particles at a pressure of
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0.3 MPa and a distance of 2 mm at a 45° angle for 20 s to simulate clinical surface
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treatment, and the same cleaning and pretreatment were performed. Resin cement
(Duo-Link, BISCO, USA) was injected into the mold (inner diameter 3 mm, outer
diameter 5 mm, height 3 mm) onto the specimens and then light-cured using an LED
light-curing lamp (LED-F, woodpecker, China) for 40 s under 1000 mW/cm2 light
Ten specimens from each group were placed in a constant-temperature water bath at
37 °C for 24 h while the other 10 specimens were placed in a hot and cold circulator to
run through a total of 5000 cycles where a cycle included two dwell stages in
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temperatures of 5 °C and 55 °C for 30 s each. The SBS testing was then carried out
according to ISO/TS 11405:2015 [18] and the SBS was measured using a universal
mechanical testing machine (Instron-3369, USA). The loading speed of the shear head
was 0.5 mm/min and the maximum load F was recorded when the specimen broke. The
F
P= (1)
S
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where P refers to shear bond strength (MPa); F denotes maximum load at fracture (N);
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and S refers to shear specimen interface cross-sectional area (mm2).
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2.6 Finite Element Analysis (FEA)
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The effect of tree frog bionic structure on the SBS of 3Y-TZP and resin cement
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interface was discussed theoretically by FEA. The bionic structure was digitally
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modeled in advance, and then imported to ansys2022R2 to perform the FEA. As shown
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in Fig. 3, zirconia phase files were combined with the corresponding resin phase. After
applying a unidirectional 200 N stress along the shear interface between zirconia and
resin, the simulation began. Since the specific fracture behavior is not only affected by
the mechanical behavior, but also by the interlayer bonding force, friction force, surface
chemical bonding force, etc. In order to eliminate the interference of other factors, we
cancel the friction coefficient between the zirconia phase and the resin phase, and
reduce the degree of deformation in the simulation. The deformation behavior and
fracture behavior after larger stress loading are also not further discussed.
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Fig.3. Schematic diagram of finite element analysis, a 200N stress was applied to the
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resin interface to simulate the force application process of SBS test.
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The flexural strength was measured on a universal mechanical testing machine with 10
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samples from each group according to ISO 6872:2015 [19]. The diameter of the
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indenter of the testing machine was 2 mm, the span of the specimens was 30 mm, the
loading speed was 1 mm/min, and the loading direction was parallel to the thickness of
the specimen. The three point bending strength formula can be given as follows:
3pl
σ= (2)
2wb2
where σ refers to three point bending strength (MPa); p denotes maximum load at
fracture (N); l refers to span (mm); w refers to width (mm); and b refers to thickness
(mm).
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2.8 Accuracy analysis of veneer restoration loaded with bionic structure
Micro-CT (Xradia Context MicroCT1, ZEISS, Germany) was used to scan and
construct the 3D models, which were then quantified against the initial model in
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The SBS and flexural strength were statistically analyzed using SPSS 16.0 software
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(SPSS Inc., USA). The average SBS and three point bending strength of each group
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were calculated and the experimental results are expressed as mean ± standard deviation
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(SD). Two-way ANOVA analysis of variance and the least significant difference method
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were used in SBS tests for comparative analysis between the two groups, setting the
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geometric variation and hydrothermal aging as the processing factors. And One-way
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ANOVA analysis of variance and the least significant difference method were used in
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flexural strength tests. When the significance level was α = 0.05, P < 0.05, the statistical
difference was considered significant (*) and when the significance level was α = 0.01,
P < 0.01, the statistical difference was considered very significant (**).
Fig. 4 shows XRD patterns of the VPP additively manufactured 3Y-TZP samples after
sintering at 1550 °C for 2 h. The phases were mainly composed of tetragonal zirconia
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(t-ZrO2) and small amounts of cubic zirconia (c-ZrO2) and yttrium oxide (Y2O3) were
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Fig.4. XRD patterns of VPP additively manufactured 3Y-TZP sintering at 1550 ℃.
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Fig. 5 shows SEM images of the different experimental groups. It can be seen that the
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structure size obtained via printing is basically consistent with the digital model.
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However, the boundaries of the printing are relatively rough, which may be related to
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the cleaning process. In addition, previous studies have shown that overall accuracy of
VPP-printed 3Y-TZP crowns are lower than those of CAD/CAM milled 3Y-TZP and
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Fig.5. Digital model and SEM images of VPP additively manufactured 3Y-TZP with
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different geometric dimensions.
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3.2 SBS of VPP-printed 3Y-TZP samples before and after hydrothermal aging
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Fig. 6a shows the SBS results for the different height groups, the control groups, and the
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sandblasting groups before hydrothermal aging. The SBS of the control group before
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the hydrothermal aging cycle was 8.9±2.1 MPa and increased to 10.3±1.5 MPa after
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250W+750H groups were 18.2±1.4 MPa, 22.7±1.3 MPa, 22.9±2.4 MPa and
19.9±2.1 MPa, respectively, and there were significant statistical differences (P < 0.01)
when compared with the control group and the sandblasting group. Overall, the SBS of
the groups with different height structures increased first and then decreased. Fig. 6b
shows the SBS values of the different width groups before hydrothermal aging. Similar
to the height groups, the SBS increased significantly with the addition of the structures
and was the highest at 22.7±1.3 MPa in the 250W+250H group, followed by the
350W+250H group, which was related to the poorer structural strength of the zirconia
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phase due to the increase in the resin phase. Fig. 6(c-d) showed that after 5000 cycles of
hydrothermal aging, the SBS of all groups decreased. The SBS of the control group and
the sandblasting group decreased significantly, at 29.6% and 43.9% of the pre-aging
SBS, respectively, while the declining ratio of the structural group was relatively small.
The best anti-aging group was the 250W+150H group and its SBS after hydrothermal
aging was 94.4% compared with pre-aging. The SBS of the 250W+500H group was still
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the highest after aging, at 17.5±0.8 MPa. Fig. 6 (e-f) shows the fracture results of
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samples without structure and with structure after SBS test.
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Fig. 6. SBS of VPP-printed 3Y-TZP samples: (a–b) before hydrothermal cycle aging;
(c–d) after hydrothermal cycle aging; * p <0.05, ** p <0.01, n = 10; (e-f) samples
without bionic structure and with structure after SBS test showed different patterns of
breakage.
The SBS between the polished zirconia surface and the resin cement was weak, but
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improved after sandblasting treatment [24, 25]. Previous research pointed out that the
SBS between different resin cements and dentin is about 16~23 MPa [26, 27], which
causes the frequent failure of bonding at the interfaces of zirconia–resin cement, defined
posterior teeth, various zirconia inlays, and zirconia-based veneer restorations. The SBS
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tests of the different structural groups loaded with bionic tree-frog structures before and
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after hydrothermal cycling showed that the heights from 150 μm to 500 μm achieved
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better bonding performance. After hydrothermal aging, the SBS of the 150 μm structure
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group showed the smallest decline, at 93.5% of the SBS at pre-aging, and the SBS of
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the 250 μm structure was at 76.8%. Therefore, the structural height of 150~250 μm has
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been found to be the best in our study. For the width group, the larger 350W and 450W
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structural groups compared with the 250W group did not show better SBS behavior, in
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keeping with the initial hypothesis when the model was established.
The fracture mode behavior after 1 year of hydrothermal environment simulation aging
changed significantly and the proportion of mixed fracture modes decreased clearly,
while the incidence of the interface fracture mode increased continuously or even
exceeded the proportion of the mixed fracture mode [28]. This indicates that the
aging. After the water-storage aging process, water may diffuse through the entire
interfaces through the microleakage of the resin–zirconia bonded interfaces and when
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the specimen area is smaller, and the leakage effect is greater [29]. Therefore, the
decrease in interface SBS is the main reason for the decrease in SBS after hydrothermal
aging. Secondly, the mechanical behavior of resin cement under long-term aging will
also be affected to a certain extent, becoming a secondary factor in the decrease in SBS.
The successful clinical application of zirconia requires a long-term stable bonding effect
and in order to achieve this goal, in addition to excellent short-term SBS, it also requires
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less damage to bonding performance after long-term aging. Aboushelib et al. proposed
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to achieve a stronger SBS effect through chemical bonding after coating a pretreatment
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agent on the surface of zirconia; however, after 90 days of water-storage aging the
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interface fracture mode was still the main one, which means the hydrolysis fracturing of
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chemical bonds occurs under hydrothermal aging leading to the failure of effective
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long-term bonding performance [30]. In this study, the experimental group showed a
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good anti-aging effect, which is mainly due to the enhancement effect of SBS brought
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about by the macroscopic mechanical locking structure, which can greatly reduce the
In order to analyze the stress of the geometric structure under the shear stress, the static
mechanical finite element analysis simulation is used to evaluate the stress distribution
of the bionic structure during the shear process, the stress concentration and the
maximum stress of different structures are explored. The Von-Mises stress distribution
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of each group of structures is shown in Fig. 7 (a-f). On the whole, the maximum stress
of all structural groups is distributed at the bottom of the structural column, which
means that the interface position of resin fracture is more inclined to be far away from
the force plane. The maximum stress of different structural groups is shown in Fig. 7
(g-h), and when the height of the structure is 250μm, the force at the maximum stress is
the lowest. With the increase of the height of the structure, the maximum stress
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decreases first and then increases, reaching the maximum at 750μm. Similarly, the
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maximum stress of different structural groups increases with the increase of width. In
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the process of SBS experiment, some groups with higher or wider structure size are
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prone to cause fracture of zirconia pillar. This result is affected by many factors, the
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most important of which is the interlayer fracture caused by the alignment of the
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printing direction and the force direction. The stress applied to the interface in the FEA
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is 200 N, which is similar to the force in the SBS test. According to the stress
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distribution in the FEA, the stress of the 250W + 150H group is concentrated on the
surface of the structure and the bottom of the structure, showing a relatively uniform
stress distribution while maximum stress is concentrated at the bottom of the structure.
The maximum stress of the 250W + 250H group is the lowest, only about 397.3 MPa,
and the stress distribution is more uniform, which is due to the increase in the size of the
structure along with the area of stress distribution, ultimately leading to a decrease in
the maximum stress. The structure height of 150 μm is too low, making the stress
increase slightly, and if the structure height is further reduced, the maximum stress may
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increase significantly under the same load until it is consistent with the plane, while the
SBS may decrease accordingly as well. As the height of the structure is greater than 250
μm, the maximum point stress value increases rapidly and concentrates at the bottom of
the structure. Excessive stress concentration will lead to obvious fracture of the zirconia
structure, followed by the occurrence of bond failure behavior. This can also explain the
actual situation in SBS test that when the structure height meets 250 μm, the maximum
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strength at the concentration is similar to fracture limitation of zirconia structure. When
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the structural strength is further improved, the structure fracture occurs during the SBS
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process, which has a certain correlation with the printing direction of the structure.
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When the printing direction is perpendicular to the structural direction, it is easier to
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cause interlayer separation at the bottom of such structures. The stress trend (Fig.7 (g-h))
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Fig.7. Finite element analysis simulates the stress distribution at the shear interface of
zirconia-resin cement under 200N stress: (a) structure groups with 150μm height and
250μm width (b) structure groups with 250μm height and 250μm width (c) structure
groups with 500μm height and 250μm width (d) structure groups with 750μm height
and 250μm width (e) structure groups with 250μm height and 350μm width (f) structure
groups with 250μm height and 450μm width; (g-h) maximum stress under different
structural heights and widths in finite element analysis.
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As the gap between the pillars increases, the stress concentration on the surface of
bionic structure increases slightly. As the width of the structure increases, the SBS
decreases slightly due to greater stress concentration. The simulation experiment in this
study follows the mechanical rules of Saint-Venant 's principle[31], which indicates the
stress farther away from the force position weakens or disappears accordingly, and the
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stress distribution on the initial contact surface is the most concentrated. Deeper fracture
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occurs at one end near the force position, while a fracture at the far force position is
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shallower, and even the residue of the resin at the top of the zirconia can be seen. This
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result suggests that the crack is generated at the bottom of the structure near the force
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position and then diffuses rapidly, and first transmits along the top interface of the
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zirconia structure, then it completely breaks in the resin phase, resulting in an overall
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fracture rather than a slow fracture. It means that the magnitude of the SBS is more
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related to the stress near the force. However, the laboratory simulation is not the specific
force situation in the clinic, the actual veneer restoration receives the shear stress so that
the distribution of the force is more evenly dispersed, and there is less concentrated
force in a certain direction. Therefore, theoretically the anti-shear force of the bionic
structure in practical application will be greater than that under the unilateral stress in
the laboratory.
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Fig. 8 shows the three point bending strength of the control group and the bionic
structure groups of different sizes. The flexural strength of the control group was the
highest at 892±40 MPa, followed by 250W+150H at 825±30 MPa. The flexural strength
347±26 MPa, and 285±14 MPa, respectively. With the increase in the height of the
structure, the flexural strength showed a downward trend and there were significant
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statistical differences between different height groups (P < 0.01). Compared with the
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control group, different widths including 350W and 450W produced significant
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statistical differences (P < 0.01) and their flexural strength was 578±42 MPa and
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566±46 MPa, respectively. With the increase in the width of the structure, the
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Fig. 8. Three-point bending strength of control group and different structural size
groups;** p < 0.01, n=10.
All structural groups meet the basic requirements of the restoration material for the
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anterior teeth, but the increase in structural height may have a certain impact on the
esthetic effect of the anterior teeth, such as low transmittance and color invariance of
According to the operating process shown in Fig. 9, a VPP based veneer restoration of a
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central incisor loaded with the bionic structure was successfully prepared. It can be seen
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that the veneer has a good shape, with a clear and complete structure, and it also shows
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a good transmission effect of restoration against the white light background.
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In order to quantify the fabrication accuracy of the VPP-based restoration loaded with
the bionic structures, micro-CT was used to construct a 3D model which was then
imported into software for accuracy analysis. In Fig. 10(a), the red part represents the
greater thickness of the restoration while the blue part represents the lesser thickness.
The minimum value of the overall thickness is in the range of 0.1~0.2 mm, located at
the bottom of the middle third of the structure (Fig. 10b). The maximum thickness is in
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the range 1.5~1.6 mm, mainly concentrated in the top third of the structure. The
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reconstructed 3D model was fitted with the original model, and Fig. 10(c-d) represent
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the fitting of the buccal surface and the lingual surface, respectively, of the veneer
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restoration loaded with the bionic structures. The positive deviation (red part) shown in
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the figure indicates that the bionic structure veneer model is larger than the
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STereolithography Language(STL) file and the negative deviation (blue part) is smaller.
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The results show that a total of 98.20% of the deviation points are lower than the
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clinically required 0.12 mm tolerance range and the average overall deviation is
0.033±0.036 mm, meeting the deviation range requirements of the current clinical
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Fig. 10. (a) Micro-CT 3D morphology and 3D thickness of veneer loaded with bionic
structures; (b) micro-CT cross-section image; (c) precision analysis of buccal surface
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The thickness of the vertical distance could be seen after the construction of the 3D
model and the application of this technology could achieve 0.1–0.2 mm ultra-thin
thickness with accuracy deviation of less than 0.12 mm, meeting the clinical sealing
requirements. Different types of support have greater impact on the accuracy of crowns,
so for veneers we need to study further which type of support can minimize the impact
on its clinical application. Although it was designed in advance, it was still impossible
to achieve completely uniform structural height ranging from 150–300 μm. However,
this height range is what has been fully discussed in the different height groups above,
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indicating that this height range can meet the needs for flexural strength and bonding
properties and processing accuracy of 3Y-TZP restorations loaded with bionic structures
clinical practice of dental restorations. In addition, how to ensure that the surface
accuracy is within the requirements of clinical application while not collapsing during
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the printing process is a direction that needs to be followed.
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Conclusion
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In this paper, 3Y-TZP loaded with tree-frog bionic structures were prepared by VPP to
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enhance the SBS at the zirconia-resin interface and the three-point bending strength test
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was used to compare the effects of different structures on the flexural strength.
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Furthermore, the FEA was used to explain the role of structural scale optimization in
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improving the SBS from the geometric factor mechanism, and the accuracy of the dental
restoration loaded with bionic structures was further discussed. The main conclusions
are as follows:
1. It has been validated that the bionic structures effectively promote the SBS of the
3Y-TZP. With the increase of structure height, the SBS increased first and then
decreased and when the pillar span was greater than 250μm, the SBS was weakened.
2. 250W + 150H group and 250W + 250H group have the minimum stress distribution,
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3. The flexural strength of the 3Y-TZP loaded with the bionic structures was weaken
4. The average deviation value in the accuracy of veneer restorations loaded with the
bionic structures was 0.033±0.036 mm, which met the deviation range requirements
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Zengqi Ye: Conceptualization, Methodology, Formal analysis, Investigation, Data
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curation, Writing-original draft; Li Zhu: Software, Validation, Data curation; Tianhong
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Zhou: Investigation, Data curation; Xian Tong: Investigation, Data curation; Zhaoping
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Chen: Investigation, Data curation; Xin Zhou: Data curation, Software; Shengbin
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Writing - review & editing; Cuie Wen: Resources, Supervision, Writing - review &
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The authors declared no potential conflicts of interest with respect to the research,
Acknowledgments
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This work was supported by the National Natural Science Foundation of China
(ZY2023008).
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Declaration of interests
☒ The authors declare that they have no known competing financial interests or personal relationships
that could have appeared to influence the work reported in this paper.
☐ The authors declare the following financial interests/personal relationships which may be considered
as potential competing interests:
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