Acta Biomaterialia 91 (2019) 24–34

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Acta Biomaterialia
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Full length article

Trade-off between fracture resistance and translucency of zirconia and

lithium-disilicate glass ceramics for monolithic restorations
Fei Zhang a, Helen Reveron a, Benedikt C. Spies b, Bart Van Meerbeek c, Jérôme Chevalier a,⇑
a
Université de Lyon, INSA-Lyon, MATEIS UMR CNRS 5510, 7 Avenue Jean Capelle, 69621 Villeurbanne Cedex, France
b
Charité – Universitätsmedizin Berlin, Freie Universität Berlin, Humboldt-Universität zu Berlin, and Berlin Institute of Health, Department of Prosthodontics, Geriatric Dentistry
and Craniomandibular Disorders, Aßmannshauser Str. 4-6, Berlin, Germany
c
KU Leuven (University of Leuven), Department of Oral Health Sciences, BIOMAT –Biomaterials Research Group & UZ Leuven (University Hospitals Leuven), Dentistry,
Kapucijnenvoer 7 blok a, B-3000 Leuven, Belgium

a r t i c l e i n f o a b s t r a c t

Article history: High strength and translucency are generally not coincident in one restorative material and there is still a
Received 27 January 2019 continuous development for a better balance between these two properties. Zirconia and lithium-
Received in revised form 7 April 2019 disilicate glass-ceramics are currently the most popular alternatives for monolithic restorations. In this
Accepted 22 April 2019
work, the mechanical properties and more important, the slow crack growth (SCG) resistance, which
Available online 26 April 2019
rules long-term durability, were thoroughly studied for three zirconia ceramics stabilized by 3, 4 and
5 mol% yttria in comparison to lithium-disilicate glass-ceramic. Translucency versus strength maps
Keywords:
revealed that the more translucent zirconia compositions (i.e. with higher yttria contents) fill the gap
Yttria-stabilized zirconia
Monolithic restorations
between the standard 3 mol% yttria stabilized zirconia (3Y-TZP) and lithium-disilicate. Moreover,
Slow crack growth increasing yttria content did not always result in lower strength, as values for 3 mol% and 4 mol% yttria
Mechanical properties were the same. Independent on the yttria contents, all zirconia showed similar relative susceptibility to
Translucency SCG under static and cyclic conditions and were significantly more SCG-resistant than lithium-disilicate
glass ceramic. A concern with higher yttria contents (5 and 4 mol%) however could lie in the higher sen-
sitivity to defects, resulting in a larger scatter in strength.

Statement of Significance

In addition to the common investigations on the generally reported strength, toughness and translucency,
V-KI diagrams (crack velocity versus stress-intensity factor) from fast fracture to threshold for three
newly developed zirconia were directly measured by double torsion methods under static and cyclic
loading conditions. The crack-growth mechanisms were analyzed in depth. Results were compared with
another popular dental ceramic, namely lithium-disilicate glass-ceramic, revealing the pros and cons of
polycrystalline and glass-ceramics in terms of long-term durability. This is the first time that V-KI curves
are compared for the major ceramic and glass-ceramic used for dental restorations. Strength versus
translucency maps for different CAD/CAM dental restorative materials were described, showing the cur-
rent indication range for zirconia ceramics.
Ó 2019 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

1. Introduction vulnerable to crack propagation, which may limit their indication.

Zirconia ceramics, in particular 3 mol% yttria stabilized tetragonal
All-ceramic restorations are popularly applied in dentistry, zirconia (3Y-TZP), can however exhibit high strength
thanks to their excellent biocompatibility and natural appearance (
1000 MPa), which allows the fabrication of long-span fixed den-
as compared to conventional porcelain-fused-to-metal (PFM) tal prosthesis (FDP) in load-bearing areas [1,2]. On the other side,
crowns and bridges, this together with the benefit of CAD/CAM most 3Y-TZP are insufficiently translucent and need to be veneered
for faster fabrication. Ceramic materials are inherently brittle and by a quite thick layer of feldspatic porcelain in order to meet the
patient’s individual tooth characteristics [3]. More recently, there
is a clear trend toward monolithic ceramic restorations, avoiding
⇑ Corresponding author.
difficulties with the veneering ceramics, i.e. the clinically rather
E-mail address: [email protected] (J. Chevalier).

https://doi.org/10.1016/j.actbio.2019.04.043
1742-7061/Ó 2019 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
 F. Zhang et al. / Acta Biomaterialia 91 (2019) 24–34 25

regularly encountered chipping of bi-layered zirconia ceramics, combination with a thorough investigation of their strength,
and enabling a less invasive tooth preparation. Monolithic restora- mechanical reliability (i.e. scatter in strength values), translucency
tions were reported to have become the first choice for posterior and microstructures. The results are compared to those of lithium-
teeth in the US since their introduction in 2014 [4]. In order to disilicate glass-ceramic, being another type of popularly used den-
use ceramics as monolithic restorations with or without a glaze tal ceramics for monolithic restorations. The results are then dis-
layer, the optical properties of the material itself have to approach cussed in the context of the search towards the best compromise
that of natural teeth with high translucency being emphasized as between crack resistance and translucency.
one of the primary parameters in controlling optical appearance
[5].
2. Materials and methods
3Y-TZP ceramics in general allow less light transmission than
glasses or glass-ceramics. Initially, they were even considered as
2.1. Materials
an opaque material [6]. Zirconia doped with 3 mol% yttria is poly-
crystalline and mostly in the tetragonal crystallography (which
Three high-translucent zirconia ceramics were processed from
explains the denomination often used of 3Y-TZP for 3 mol%
commercially available powders (Zpex, Zpex4 and ZpexSmile, all
Yttria-doped Tetragonal Zirconia Polycrystal). Thus, light scattering
from Tosoh, Tokyo, Japan). All these powders contain a low per-
occurs at grain boundaries due to birefringence, as well as at resid-
centage (0.05 wt%) of Al2O3. The yttria stabilizer content in Zpex,
ual pores even if present in low percentage. After years of develop-
Zpex4 and ZpexSmile was 3, 4 and 5 mol%, respectively. The result-
ment, many methods have been proposed to improve their
ing zirconia ceramics were referred to as ‘3Y’, ‘4Y’ and ‘5Y’ through-
translucency, including reduction of porosity acting as light scat-
out the text. Powders were compacted by uniaxial pressing at
tering defects or the alumina content, using nanostructured zirco-
40 bar applied on the piston for 40 s (Nannetti SSN/EA, Faenza
nia, and very recently increasing the yttria content [7,8]. A huge
(RA), Italy) to disks of 18 mm in diameter and rectangular plates
amount of different zirconia ceramics (tetragonal zirconia or TZPs,
with surface areas of 30  80 mm2, followed by cold isostatically
and partially stabilized zirconia or PSZs) are thus introduced in the
pressing at 300 MPa for 3 min. Pressed green bodies were debinded
dental field and numerous studies report the properties of various
following the thermal cycle suggested by the powder supplier, pre-
high-translucent zirconia ceramics (Table S1 in supplementary
sintered at 1000 °C for 1 h and finally pressure-less sintered in air
document). Increasing yttria content effectively enhances the
at 1450 °C for 2 h using the same sintering cycles for all zirconia
translucency of yttria-stabilized zirconia but lowers the strength
samples. All materials reached full density of 6.07 ± 0.01 (SD),
(less or no phase transformation toughening) [9,10], by which zir-
6.06 ± 0.01, and 6.06 ± 0.00 g/cm3 for 3Y, 4Y and 5Y, respectively.
conia with a high yttria content can only be used in low stress-
Sintered disks were used for translucency, microstructural and
bearing areas. However, the current positioning of the newest
phase characterizations. Bars for testing 4-point bending strength
monolithic zirconia generations in terms of mechanical and optical
were cut (Servocut 301-AA, Metkon, Rotterdam, Netherlands) from
properties is not clearly and fully defined.
sintered plates of approx. 22  60  5 mm3 to a size of
Moreover, few studies have been focused on slow crack-growth
5  4  45 mm3 and subsequently machined parallel to their final
behavior and fatigue [11–13], while it is especially important to
dimensions of 4  3  45 mm3. The specimens for slow crack
assess the long-term load-bearing capacity of crack-sensitive
growth tests were cut from sintered zirconia plates of approx.
ceramics [14]. Standards, solely requiring minimum mechanical
22  60  3 mm3 down to 20  40  3 mm3 and parallel ground
properties that are measured under fast fracture conditions
to 2 mm in thickness.
(referred to as the inert or initial mechanical strength of the mate-
Lithium-disilicate glass ceramic (referred to as ‘LS02 ) samples
rials [15–17]) should not be considered sufficient for safe use in
were machined from IPS e.max CAD blocks (IPS e.max CAD HT
patients, since the humid environment and cyclic loading in the
A2, Ivoclar Vivadent, Schaan, Liechtenstein; ‘HT’ = high translu-
oral environment can degrade the restoration’s load-bearing
cency). Plate-shaped specimens were cut from as-delivered blocks
capacity over time. Chemically-assisted slow crack growth (SCG)
of partially crystallized lithium metasilicate precursory phase
occurs due to the presence of water molecules (or other corrosive
using a low-speed diamond saw (Accutom-50, Struers, Ballerup,
species, like ammonia or polar solvents), which promote breakage
Denmark), followed by crystallization heat treatment according
of the strained ionic-covalent bonds at the crack tip, i.e. stress-
to the manufacturer’s instructions in a Programat P300 (Ivoclar
corrosion reaction, and initiate crack propagation at stress intensi-
Vivadent) vacuum ceramic oven.
ties (KI) below the material’s fracture toughness (KIC) [18–20]. Cyc-
lic loading induces fatigue in ceramics due to degradation of
extrinsic toughening effects [14]. Clinic and lab reports show that 2.2. Material characterization
dental restorations fail either due to chipping or fracture of the
whole structure; such failures often occur at a load far below the X-Ray Diffraction (XRD; 3003-TT, Seifert, Ahrensburg, Germany)
initial strength owing to SCG and cyclic fatigue [12,21]. In particu- was used to characterize the phase composition of sintered ceram-
lar, in case radial cracks appear at the cementation surface, SCG ics. XRD patterns were collected on as-sintered surfaces using Cu-
would very likely reduce the restoration’s loading-bearing capabil- Ka radiation at 40 kV and 40 mA from 20 to 90° (2h) with a step
ity over time [22]. When there is occlusal contact damage at the size of 0.01 for 3 s. Rietveld analysis of XRD patterns was per-
restoration’s surface, cracks can be initiated by cyclic loading and formed with Topas academic software (Bruker AXS, Karlsruhe, Ger-
propagate downwards and outwards driven by water-assisted many) to quantify phase contents and lattice parameters. Yttria
SCG (hydraulic pumping), resulting in bulk fractures [21]. There- content in the tetragonal zirconia phase was calculated based on
fore, investigating the fatigue behavior of these new high- the a and c unit cell parameters and the formula previously
translucent zirconia is highly demanded, in particular to determine reported [10,23,24].
the threshold stress intensity factor below which no slow crack The microstructures were analyzed by Scanning Electron Micro-
growth is expected. The threshold parameter was also suggested scopy (SEM; Supra 40, Carl Zeiss AG, Oberkochen, Germany) of as-
to be a better predictor than the SCG n parameter for the fatigue polished ceramic surfaces. Additional surface treatments (thermal
and clinical performance of dental ceramics [13]. and chemical etching, and coating of conductive layer) were
The aim of this work was to study the crack-growth properties avoided in order to observe the intrinsic microstructures of all
(static and cyclic fatigue) of newly developed zirconia ceramics in phases present (crystalline as well as glass phase). The grain size
26 F. Zhang et al. / Acta Biomaterialia 91 (2019) 24–34

distributions on >1000 grains were measured on SEM micrographs To obtain lower crack rates till near threshold crack rates (1012
according to the linear intercept method without applying any cor- m/s), constant loading tests were used. The specimens were sub-
rection factor. jected to different loads for a prescribed duration to induce crack
Four-point bending strength was measured at a loading rate of extension. The crack length was measured via optical microscopy
0.5 mm/min with 40 mm outer span and 20 mm inner span. Bend- with a precision of 2 mm. The crack velocity (V) was calculated as
ing bars (n = 20) were sequentially polished with 7, 3, and 1 mm the ratio of the crack increment (Da) to the duration (Dt):
diamond pastes prior to the tests. Fracture surfaces obtained by
Da
four-point bending testing were examined by SEM. V¼ ð3Þ
Dt
Translucency was measured on polished specimens (0.5-mm
and 1.0-mm thick; n = 6 per group) using a spectrophotometer Crack propagation tests under cyclic conditions were performed
(SpectroShadeTMMICRO, MHT OpticResearch, Niederhasli, under load control using a sine waveform between minimum and
Switzerland). CIELAB coordinates (L*, a* and b*) were recorded maximum load at a ‘R’ (R = Pmin/Pmax = KI,min/KI,max) ratio of 0.1 and
against white and black calibrated background boards with a thin a frequency of 10 Hz. The maximum load, i.e. the maximum
layer of vaseline applied in between. Contrast ratio (CR) was calcu- applied stress intensity factor, ‘KI,max’ (and also ‘KI,min’ to keep
lated, which is 0.0 for a transparent material and 1.0 for a totally R = 0.1) was lowered until the crack propagation was no longer
opaque material. observed even after loading for 6 days. The crack rate was again
determined using Eq. (3) and V-KI,max diagrams were obtained for
cyclic fatigue. The maximum load used in this work for cyclic fati-
2.3. Slow crack growth gue tests was in the range of 95–40 N, bringing Pmin of less
than 10 N with a negligible effect on the crack velocity.
The double-torsion (DT) method was used to measure crack- Known that the V-KI diagram of oxide ceramics generally pre-
growth velocity (V) versus applied stress-intensity factor (KI) sents three typical stages in air, attributed to three distinct mech-
curves under static and cyclic conditions at room temperature anisms; each stage (Stage I, II, III) of the V-KI diagram can be fitted
(
20 ± 2 °C) in ambient air (
50% RH). A wide range of crack- separately by the form of V = A (KI or KI,max)n, with ‘A’ and ‘n’ being
growth velocities from 1012 to 103 m/s were followed; the frac- constants that correspond to each stage. Since stage I has a primor-
ture toughness (KIC) associated with fast fracture and threshold dial practical importance of ruling the device longevity at the low
(KI0) below which no crack growth was observed, were deter- crack rate, the stress corrosion coefficient/fatigue parameter (n)
mined. Details of the DT loading configuration together with the value from stage I was determined as the slope in the plot of ln
double-torsion specimens (dimensions of 40  20  2 mm3 for zir- (KI) vs. ln (V).
conia and 40  18  2 mm3 for LS2) can be found in more details In the end, the crack-propagation features were observed by
elsewhere [25,26]. The tensile surface of the specimens was pol- SEM at the crack tip of the surface of DT specimens.
ished to facilitate crack observation. A notch of length ‘a00
(10 mm) was machined using a 0.3-mm thick diamond sawing 2.4. Statistical analyses
blade (ATM GmbH, Mammelzen, Germany). Two 10 kg Vickers
indentations were made at the tip of notch to initiate a small crack One-way analysis of variance (ANOVA) followed by Tukey’s post
on the tensile side of the sample. Subsequent pre-cracking was hoc was used to investigate statistical differences in the mean val-
performed by slowly loading the specimens at a rate of 10 mm/ ues between different materials at a significance level of a = 0.05
min, so to induce a real sharp crack with an initial length ‘ai’ (MinitabÒ16.2.1, Minitab Inc, Pennsylvania, USA). The bending
(12-13 mm) and stable crack front geometry [25]. strength results were also analyzed by Weibull statistics with con-
The KI in the double-torsion technique was calculated according fidence bounds (a = 0.05; 95% confidence interval).
to the following expression [18,26]:
 1=2  6=32 3. Results
Wm 3ð1 þ mÞ a
KI ¼ 2
P ð1Þ
T Ww a0
3.1. Phase characterization
where ‘P’ is the load, ‘a’ the total crack length, ‘a0’ the notch length,
‘Wm’ the span width, ‘T’ the thickness of the sample, ‘W’ the width XRD patterns (Fig. 1) showed that all 3Y, 4Y and 5Y zirconia
of the sample, ‘m’ the Poisson ratio, and ‘w’ a calibration factor [27]. ceramics were composed of mixed tetragonal (t-ZrO2) and cubic
Note that (a/a0)6/32 was the correction factor to conventional (c-ZrO2) phases. As expected from the ZrO2-Y2O3 phase diagram
expression of KI, because KI was demonstrated to slightly depend and previous results [29,30], increased yttria content led to higher
on the crack length due to the fact that the crack front was not cubic content at the expense of tetragonal phase. The XRD peaks
straight and longer on the tensile side [25]. corresponding to cubic phases in 4Y and 5Y can be clearly observed
To obtain the crack-growth curve in full range from threshold to in between the doublet peaks of tetragonal phases (Fig. 1b). Quan-
fast fracture, two methods were complementarily used, namely the tification of the XRD patterns by Rietveld analysis (Table 1)
relaxation and constant test. In the relaxation test that enables revealed the formation of about 40 and 60% c-ZrO2 in 4Y and 5Y,
measuring the velocity range of 107-102 m/s, pre-cracked speci- respectively, as compared to about 10% c-ZrO2 in 3Y. In addition,
mens were loaded at the rate of 0.3 mm/min to a certain load with the remaining tetragonal phase in 4Y and 5Y contained higher
the function of load versus time being recorded. The crack velocity yttria content together with a smaller tetragonality (lower c/a
(V) for the relaxation test was calculated using the following equa- ratio), consistent with current literature [29].
tion [26,28]:
3.2. Microstructure
  
Pf D dP
V ¼ af þ ð2Þ The microstructure of the zirconia ceramics revealed polycrys-
P2 B dt
talline and dense structures with only occasionally very few pores
with ‘af’ the final crack length, ‘Pf’ the final load, ‘dP/dt’ the slope of (Fig. 2a). Grain-size distributions were all unimodal (Fig. 2b). The
relaxation at a given time, and ‘D/B’ the constant from the compli- three zirconia ceramics significantly differed in microstructure
ance calibration [25]. for grain size (Table 2). On the other side, LS2 consisted of Li2Si2O5
 F. Zhang et al. / Acta Biomaterialia 91 (2019) 24–34 27

Fig. 1. (a) XRD patterns of as-sintered samples. The characteristic peaks of cubic zirconia and tetragonal zirconia are indexed in the pattern of 5Y and 3Y, respectively. (b)
Expanded view of 28–32, 33–38 and 70–78 diffraction 2h degrees.

Table 1
Phase composition and lattice parameters using XRD and Rietveld analysis.

3Y 4Y 5Y
XRD Tetragonal fraction (%) 87 ± 2 63 ± 4 42 ± 4
c/a 1.0151 ± 0.0002 1.0147 ± 0.0000 1.0126 ± 0.0007
Y2O3 (mol%) 2.7 ± 0.06 2.9 ± 0.01 3.7 ± 0.30
Cubic fraction (%) 13 ± 2 37 ± 4 58 ± 4
c (Å) 5.1379 ± 0.0005 5.1360 ± 0.0007 5.1348 ± 0.0001

Fig. 2. Microstructures: (a) SEM images of zirconia (3Y, 4Y, 5Y) ceramics and the reference LS2 glass ceramic. All SEM images were obtained following as-polished conditions
without any etching (neither thermal for zirconia ceramics, nor chemical for LS2). (b) Grain size distribution of 3Y, 4Y and 5Y zirconia.

crystals (confirmed by XRD) embedded in a glass matrix. The the translucency (lower CR) of zirconia ceramics (Table 2). Reduc-
length of the crystals was in the range of 2 mm (Table 2) with an ing thickness also increased the translucency of the three zirconia
aspect ratio of about 4 in respect of their diameter. Small pores ceramics. Nevertheless, at the same thickness, LS2 HT’s translu-
could be clearly observed in the crystalline and glass phases of cency remained significantly higher than that of all zirconia ceram-
the LS2 specimens. ics investigated (Fig. 3).

3.3. Translucency 3.4. Strength

At the thickness of 0.5- and 1.0-mm, the translucency of The average bending strength of 3Y, 4Y and 5Y was 908, 928
5Y > 4Y > 3Y and increasing yttria content significantly enhanced and 524 MPa, respectively (Table 2). Weibull analysis (Fig. 4a)
28 F. Zhang et al. / Acta Biomaterialia 91 (2019) 24–34

Table 2
Grain size, translucency and strength of all ceramics investigated. Mean values are reported with (±) 95% confidence interval.

Grain size (mm) Translucency (CR) 4-point bending strength

1.0 mm 0.5 mm Average (MPa) Weibull modulus
3Y 0.30 ± 0.01 a 0.65 ± 0.02 a 0.54 ± 0.02c 908 ± 44 a 9.2
4Y 0.36 ± 0.02b 0.59 ± 0.01b 0.47 ± 0.01 d 928 ± 82 a 6.3
5Y 0.53 ± 0.03c 0.45 ± 0.00 d 0.36 ± 0.01 e 534 ± 56b 4.9
LS2 1.72 ± 0.12 (L) – 0.28 ± 0.01f* 462 ± 15 # 10.0#
4.06 ± 0.36 (aspect ratio)

Different superscripts (for each variable) indicate statistically different results (significance level a = 0.05); *LS2 is HT, high translucency grade; # Value reported by Wendler
et al. (2017) using the same 4-point bending test [31].

Fig. 3. Translucency of zirconia ceramics and Lithium disilicate (LS2, high translu-
cency grade) in 0.5-mm thickness (low CR representing high translucency and vice
versa). Different superscripts indicate significantly different results (a = 0.05).

revealed their characteristic strength (r0) [95% C.I.] was 951 [901–
1002], 998 [925–1070] and 581 [532–631] MPa, respectively.
There was no statistical difference in bending strength between
3Y and 4Y (Table 2). However, a lower Weibull modulus was
obtained for 4Y samples. 5Y had an even lower strength and Wei-
bull modulus than 3Y and 4Y. Fractography of the bending bars
(Fig. 4b) were examined in the area close to the fracture origin
within the mirror region, since the crack initiated and rapidly
accelerated in this region. 3Y and 4Y exhibited similar fracture pat-
terns consisting of mixed intergranular and transgranular fractures
with fine zirconia-grain sizes, whereas the fracture surface of 5Y
was different with almost only transgranular fractures through
much larger zirconia grains.
Regarding the strength of LS2, the size of available LS2 blocks
(max. 40 mm in length) did not allow performing the 4-point
bending test in this work using 40 mm outer span and also the cor-
responding statistical analysis. The flexural strength of LS2 in
Table 2 was thus referred to the value reported by Wendler et al.
[31] using the same methodology and the same type of LS2 speci-
mens but smaller dimension. Considering also the previous report
showing that the biaxial strength of 5Y and LS2 were not statisti-
cally different [32], the 4-point bending strength of LS2 and 5Y
shown here in Table 2 should be similar or marginally different.
Fig. 4. Four-point bending strength of the zirconia ceramics investigated: (a)
Weibull plot with 95% confidence bands. Weibull characteristic strength (failure
3.5. Crack-growth resistance probability of 63.2%) is marked. (b) Fracture surfaces of bending bars imaged by
SEM. The image on the top left (the fractography of a 4Y specimen) is the
Under static loading (Fig. 5a), V-KI diagrams were recorded representative image of examining area close to the fracture origin.
from fast fracture (KIC) down to threshold (KI0) for all ceramics
investigated, including for the reference LS2 glass ceramic. The
toughness (KIC) was estimated at a high crack velocity of and a stress corrosion coefficient (n) of
30 were thus observed
103 m/s and the threshold (KI0) was determined from the points for all zirconia ceramics, which revealed a similar relative suscep-
below which there was an abrupt drop to a crack velocity of about tibility to SCG. When compared to LS2, 5Y and LS2 showed a similar
1012 m/s (see Table 3). Increasing yttria content clearly shifted the fracture toughness, but the KI0 of LS2 (1.1 MPam1/2) was lower
V-KI curve towards lower KI values. However, the V-KI curves than that of 5Y. Although the difference was only 0.4 MPam1/2, it
remained parallel in a log-log scale. Similar KI0/KIC values (
0.5) represented about 30% of relative difference. This finding indicated
 F. Zhang et al. / Acta Biomaterialia 91 (2019) 24–34 29

Fig. 5. Slow crack growth: (a) V-KI curves under static loading in air for the four ceramics investigated. The different crack-velocity regions (stage III, stage II, stage I and stage
0, i.e. threshold KI0) are marked in the curve of 3Y. (b) Effect of cyclic loading (10 Hz, R = 0.1) on V-KI curves for the three zirconia ceramics, presented as V-KImax. The dashed
line represents the estimated V-KImax curve if there would not be cyclic degradation in 3Y. (c) Comparison of V-KI/KImax curves for 5Y zirconia and LS2 glass ceramic under
static and cyclic fatigue.

Table 3
SCG parameter values.

KIC (MPam1/2) SCG Static SCG cyclic (10 Hz, R = 0.1)

KI0 (MPam1/2) KI0/KIC n, stage I KI0 (MPam1/2) KI0/KIC n, stage I
3Y 5.0 ± 0.3 2.7 ± 0.1 0.54 30.8 ± 7.2 2.5 0.49 20.9
4Y 4.0 ± 0.2 2.2 ± 0.1 0.55 27.7 ± 5.5 2.1 0.52 17.9
5Y 3.3 ± 0.2 1.5 ± 0.1 0.46 27.2 ± 3.2 1.4 0.43 23.7
LS2 3.1 ± 0.2 1.1 ± 0.1 0.35 15.8 ± 5.5 1.0 0.32 10.5

that LS2 was more sensitive to SCG than zirconia ceramics. The n cyclic loading than Pmax, the crack-growth rate would be lower
value of the V-KI curve corresponding to LS2 was indeed lower than at a constant maximum load, if no cyclic degradation was pre-
(
16) and a smaller KI0/KIC value (
0.35) was recorded. sent. The real effect of cyclic fatigue degradation is therefore appre-
With respect to the effect of cyclic loading, the cyclic V-KImax ciated from the difference between the calculated V-KImax curve
curves of zirconia ceramics are shown in Fig. 5b and the compar- (dashed lines in Fig. 5b for 3Y-TZP) and the experimental one.
ison to reference LS2 is shown in Fig. 5c. For the three zirconia Therefore, cyclic loading significantly degraded the crack resis-
ceramics, the crack-growth rates under cyclic loading were clearly tance of the three zirconia ceramics. Regarding the reference LS2
accelerated compared to static crack growth at equivalent stress glass ceramic (Fig. 5c), similar to the zirconia ceramics, cyclic
intensities. One should also note that cyclic crack-growth rate degradation was also observed for LS2: cyclic crack growth
was presented as a function of KImax and that the determination occurred at stress intensities below that for static crack growth;
of the exact cyclic degradation from the direct comparison of static KI0 was shifted to a lower value and the V-KI,max curve had a lower
V-KI and cyclic V-KI,max would not be correct. The crack velocity per slope (Table 3).
cycle (da/dN-KImax) if there was no cyclic fatigue degradation can Fig. 6 shows SEM images in the vicinity of the crack tips at the
be estimated, as previously reported [18], by an integration of surfaces of the DT samples. Unlike metals [14] and because of no
the V-KI (da/dt-KI) curve over a cycle. Crack-growth rate per cycle (or very localized and limited) plasticity, the crack-propagation
(da/dN-KImax) would have been lower than for static da/dt-KI, as modes and microstructures of cyclically and statically loaded spec-
indicated by the dash line for 3Y in Fig. 5b. Indeed, since the aver- imens did not show differences, so only images obtained from stat-
age integrated load (varying between Pmin and Pmax) is lower under ically loaded specimens were representatively shown. Along the
30 F. Zhang et al. / Acta Biomaterialia 91 (2019) 24–34

Fig. 6. Microstructures imaged by SEM in the vicinity of the crack tip at the surfaces of DT specimens and a schematic illustration of the phase transformation upon crack
growth in 3Y and 4Y zirconia ceramics.

crack path in 3Y, grains at a depth of 1–2 grains were transformed 3Y to 4Y and 5Y (Fig. 6) obviously resulted in the shifts of the V-KI
and a twining morphology of monoclinic grains were clearly curve to lower KI values with lower KIC and KI0 (Table 3). In 4Y and
observed to have arrested the crack opening (as illustrated in the 5Y, not only more non-transformable cubic phase was formed, the
schematic). 4Y revealed a similar behavior as 3Y, but less grains remaining tetragonal phase was also less transformable with lower
were transformed along the crack path. 5Y, on the other hand, tetragonality (Table 1). 4Y thus had less toughening effect from
exhibited no transformed grains. Crack bridging at the level of zir- phase transformation than 3Y, whereas 5Y did not show any evi-
conia grains can be found in all zirconia ceramics with however dence of phase transformation toughening. Although grain bridg-
relative straight crack propagation, if we compare with polycrys- ing that generally exists in polycrystalline ceramics was present
talline ceramics with larger or more elongated grains [33–35]. in all zirconia ceramics including 5Y (Fig. 6), this mechanism from
Crack deflection and bridging were more pronounced for LS2 with fine (0.3–0.5 mm, Table 2 and Fig. 6) and equiaxed grains should
clearly meandered crack paths (note also the different scale bar in merely be effective on small dimensions in a limited extent, unlike
LS2). in the case of coarse-grained Al2O3 or grain-elongated Si3N4
[14,33–35,38,39]. Due to the relative large and elongated Li2Si2O5
crystals (Fig. 2a) [40,41], crack deflection and crack bridging was
4. Discussion effective in LS2 (Fig. 6).
On the other side, different from the general expectation, 4Y,
4.1. Toughening and mechanical properties that are measured at fast although being less tough than 3Y, did not show a lower bending
fractures strength (Table 2). The high strength of 4Y should be related to
the small processing defects and the fine microstructure (Fig. 2).
The toughening mechanisms of the materials in general consist Based on the strength distribution (Table 2) and toughness values
of intrinsic (K0) and extrinsic toughening (DKc), and the extrinsic (Table 3), the size of critical flaws in 4Y was calculated to be in the
toughening mechanism working in the wake of the crack (i.e. range of 13–9 mm, using linear-elastic fracture mechanics and the
crack-shielding) is known to be the primary toughening sources Griffith equation (Y = 1.3) [42]. The critical flaw in 3Y and 5Y was
for brittle ceramic materials [36], by which transformation tough- in the range of 20–17 mm and 26–17 mm, respectively. The grain
ening, crack bridging, crack deflection and/or combinations thereof sizes/distributions (Fig. 2) and facture patterns (Fig. 4b) of 4Y
are relevant toughening mechanism in the four materials investi- and 3Y were also very close. Another work reported a biaxial
gated [36,37]. Reduction of phase-transformation toughening from strength of higher than 1100 MPa for 4Y, similar to that of 3Y,
 F. Zhang et al. / Acta Biomaterialia 91 (2019) 24–34 31

when using the same sintering cycles [43]. In the work reporting a with the same Zr-O-Zr bonds, presenting the same stress corrosion
lower strength of 4Y [32], the grain size of 4Y however was much at the crack tip, which has also been observed before for 3Y-TZP
larger than that of 3Y. Nevertheless, despite the similar strength of with different grain sizes and for zirconia stabilized by different
4Y and 3Y, the strength scatter of 4Y (m = 6) was higher than for 3Y stabilizers [51]. LS2 consists of 70 vol% Li2Si2O5 crystals and
(m = 10), followed by an even higher one for 5Y (m = 5) (Fig. 4). 30 vol% silicate glass phase. It is difficult to quantitatively compare
Decreased mechanical reliability when increasing yttria content the water affinity of Zr-O and Li-O/Si-O bonds, but (silicate) glass
should be attributed to the reduced crack-growth resistance and materials are known to be more susceptible to hydrolysis and
thus higher sensitivity to cracks/defects. At the same time, lower stress-corrosion than polycrystalline materials [12,13,52]. The dif-
crack resistance raises another concern in terms of surface treat- ferent SCG susceptibility recorded between zirconia and LS2
ment. Clinically conducted surface treatments, such as sandblast- (Fig. 5c) is reflected in stage I, confirming the effect of the stress-
ing, are able to enhance the strength of 3Y-TZP thanks to the corrosion reaction.
generated compressive stresses [44], but this effect might be com- Regarding the cyclic SCG, all studied ceramics showed cyclic
promised/lost [45] in PSZ (4Y and 5Y). degradation with decreased KI0,cyclic and lower slope of V-KI,max.
When comparing to LS2 glass ceramic, 4Y and 3Y showed better Cyclic fatigue accelerates the crack growth in brittle ceramics by
mechanical properties, but 5Y revealed only a marginally higher degrading the extent of extrinsic crack-tip shielding toughening
fracture toughness (Table 3) and flexural strength (Table 2) [32]. [14] that again involves transformation toughening, bridging,
Importantly, a lower strength scatter, i.e. higher mechanical relia- deflection and/or combinations thereof (Fig. 6) [14,36]. Since the
bility (m
10 [31,46–48]) was recorded for LS2 than 5Y. The find- extent of extrinsic toughening was not the same for the four stud-
ing that LS2 and 5Y have a similar fracture toughness (KIC) but ied materials, materials undergoing higher extrinsic toughening
different reliability, should probably be attributed to the different (i.e. 3Y) were expected to be more vulnerable to cyclic degradation.
proportions of intrinsic toughness (K0) and extrinsic toughening However, surprisingly, the extent of cyclic degradation (
5% loss in
(DKc). As explained at the beginning of the discussion, the KIC of KI0) was rather similar between the different samples. This similar
brittle materials and more specifically the crack growth resistance susceptibility to cyclic fatigue in the three zirconia ceramics points
(KR) commonly consists of K0 and DKc, and DKc can lead to a stably out that the transformation toughening (in 3Y and 4Y) is not
rising crack resistance, i.e. R-curve behavior [36,37]. K0 of LS2 is degraded by cyclic fatigue, since transformation toughening acts
reported to be about 1.2 MPam1/2 [40], whereas K0 of zirconia is as inelastic zones surrounding the crack tip but not behind the
around 2 MPam1/2 [36,49]. It can then be figured that DKc for crack tip like bridging [38]. The observed cyclic degradation can
LS2 is higher than for 5Y, resulting in a stronger R-curve for LS2 be attributed to the grain bridging mechanism, i.e. elastic or fric-
with better tolerance to cracks/defects. Indeed, the most potent tional bridging of contact shielding that can be degraded by load-
extrinsic toughening mechanism (i.e. phase transformation) for ing/unloading [14,38,39,53]. Even though, as discussed above
zirconia ceramics was absent in 5Y zirconia, while LS2 had obvi- that grain bridging for the studied zirconia ceramics is only effec-
ously effective extrinsic toughening effect from crack deflection tive in a limited extent and thus cyclic effects solely contribute to a
and crack bridging (Fig. 6), contributing to the higher mechanical very small proportion of overall degradation as compared to
reliability of LS2. Another similar lithium-disilicate glass-ceramic chemically-assisted SCG. From the aspect of threshold,
with elongated LS2 crystals (Empress 2, Ivoclar Vivadent AG) even chemically-assisted SCG presented about 50% reduction of the frac-
showed higher Weibull modulus than a 3Y-TZP ceramic [17]. The ture toughness for zirconia ceramics (KI0,static/KIC
0.5), but the
microstructure of LS2 investigated here (Fig. 2a) also showed more cyclic loading gave rise to 5% degradation of KI (KI0,cyclic was 5%
defects (porosities and heterogeneous structures) than that of 5Y, smaller than for KI0,static). The LS2 glass-ceramic, having elongated
despite they revealed a similar or marginally different strength. crystals in the order of 2 mm, suffers more from the cyclic fatigue
effect due to the higher dependence of its bridging mechanism
4.2. Long-term durability: SCG and cyclic fatigue on the friction effect at also a larger scale (Fig. 6). Furthermore,
the volume fraction of these elongated crystals together with their
Independent on KIC and the yttria content, 3Y, 4Y and 5Y size, aspect ratio, orientation are critical for the fracture resistance
showed a similar relative susceptibility to SCG under static loading of the LS2 glass-ceramic [41,54], raising the question about the
(parallel shift of V-KI curves in a log-log scale; KI0,static/KIC
0.5; influences of these factors on the SCG and cyclic fatigue of LS2
similar stage-I n value of
30), yet having a significant higher glass-ceramic for further investigations as well.
SCG resistance than LS2 (n of
16, KI0,static/KIC
0.4) (see Fig. 5a Above all, the three zirconia ceramics showed a similar SCG rel-
and Table 3). It is necessary to first clarify that the V-KI curves ative susceptibility under both static and cyclic loadings, but were
obtained in this work by DT should not be influenced by the more resistant to SCG than LS2 due to the higher susceptibility of
R-curve behavior. Although the extrinsic toughening effects and the glass phase to the water-assisted stress-corrosion reaction. Pre-
the resulting R-curve behavior were different for the four materials vious studies using indirect methods (dynamic and cyclic fatigue
investigated, the steady state conditions of the R-curve should be tests) also showed that LS2 glass ceramic would degrade faster over
reached in the crack-size domain of the DT tests. The transforma- time with smaller n values than zirconia [13,55] as well as in aque-
tion zone (h) in the studied 3Y was found to be about 1 mm (1–2 ous environment [11]. In fact, glass-containing ceramics, including
grains in Fig. 6), revealing that 3Y should reach the R-curve steady glass-infiltrated ceramics, generally exhibited a higher susceptibil-
status at a crack length of about 5 mm (about 5 times the transfor- ity to SCG than polycrystalline ceramics (zirconia, alumina)
mation zone [50]). Although the R-curve of LS2 is estimated to be [13,55–57]. One exception was reported for a leucite-reinforced
stronger than that of 5Y, a steep raise over the first micrometers glass ceramic that contained even 50–60% aluminosilicate glass
or tens of micrometers was also reported because of the fine (IPS Empress, Ivoclar Vivadent) [13]. Different from LS2 glass cera-
dimensions of Li2Si2O5 crystals [13,41]. In addition, the rising part mic, the enhanced SCG resistance in IPS Empress was attributed to
of R-curve would result in a higher slope of the V-KI curve [33], the compressive residual stress developed around the leucite crys-
which is the opposite as observed for LS2. Therefore, the differences tals [13,40].
in observed SCG susceptibility should not be attributed to the It is necessary to point out that the current work was performed
R-curve but to the material’s intrinsic susceptibility to water- in ambient air conditions (
50% RH) but not in water or body fluid,
assisted stress-corrosion reactions, namely chemically assisted because water molecules in air were enough for SCG to proceed
SCG. For the three zirconia ceramics, they are free of glass phase and only one stage (stage I) would be present in water with the
32 F. Zhang et al. / Acta Biomaterialia 91 (2019) 24–34

same stress-corrosion coefficient (i.e. the same SCG susceptibility) sion and test method are dominantly used. The influence of surface
and with the same threshold stress intensity factor KI0 (only differ- treatments especially for zirconia ceramics is also a topic of ongo-
ent crack growth rate) [20,58]. Nevertheless, the oral cavity is a ing investigation [60]. Therefore, in addition to the property of
complex environment with a fluctuating temperature, high acidic materials themselves, all above mentioned experimental and sam-
environment (low pH), bacteria and so on. This environment can pling uncertainties could contribute to increase the scatter of
especially be important for LS2, because LS2 shows a relatively high strength data.
dissolution in an acidic environment (Fig. S3 in the supplementary Zirconia, both TZP and PSZ, remain in general less translucent
document) and the V-KI diagram in an environment where the than lithium-(di)silicate glass ceramic. TZP here refers to 3Y-TZP
materials undergo some dissolution, could be substantially differ- in order to be consistent with the commonly used terminology
ent [59]. Although zirconia ceramics (3Y, 4Y and 5Y) are quite and PSZ refers to zirconia containing yttria contents higher than
resistant to acid etching (Fig. S3 in Supplementary documents), 3Y. In fact, it should be kept in mind, and this is again shown in
considering the hydrothermal aging behavior, it is also paramount the experimental results provided that all yttria-doped zirconia
to study the crack-growth behavior of zirconia ceramics in a more polycrystalline ceramics, with 3–6 mol% yttria are in fact a mixture
hostile environment more closely resembling the oral cavity, or of t- and c-ZrO2 (Table 1) [29], thus are all PSZ materials. The evo-
after a prolonged duration in such media. lution of the different zirconia generations from various ‘TZPs’ to
so-called ‘PSZ’ (sometimes even called not correctly ‘cubic zirco-
4.3. Material selection based on strength and translucency nia’) clearly shows the significant improvement in zirconia’s
translucency (Fig. S2).
Considering the numerous zirconia ceramics introduced in the In spite of the reflection at the surfaces, the main factor limiting
dental field and the fact that the mechanical and optical properties the light transmission of polycrystalline ceramics is scattering by
of different zirconia ceramics are highly variable, as discussed birefringence at the grain boundary and by pores or second phases
above, it is interesting to plot a flexural strength versus translu- [8]. The first generation of dental 3Y-TZP in general contains
cency map (the main parameters commonly employed as guidance 0.25 wt% alumina, allowing some light transmission but as previ-
to select the proper material to design and fabricate FDPs). Fig. 7 ously introduced, the formation of alumina particles limits their
displays a scatter plot of flexural strength versus translucency for translucency [10]. Then, lower alumina additions (up to as low as
various materials that can be processed by CAD-CAM. More detail 0.05 wt%) to zirconia have been suggested. The alumina addition
of the material classification and consulted data sources can be of less than 0.2 wt% is within the solubility limit of alumina in zir-
found in the supplementary Fig. S1 and Table S1. Admittedly, the conia and can thus be fully dissolved and segregated as Al3+ at the
strength is influenced by process conditions (pressing, pre- and zirconia grain boundaries [62,63]. In this way, the zirconia ceram-
sintering) with different flaw sizes and distributions, surface treat- ics can still be easily fully-dense sintered with the aid of Al3+ [64]
ments (ground, polished or as-sintered) [60], specimen dimensions while the formation of secondary alumina particles is avoided
and methodologies of bending tests with different effective (Fig. 2). Furthermore, as shown in Fig. S2b and by previous works
stressed volume [61]. Size limitations of many commercial CAD/ [10], decreasing alumina does not significantly compromise
CAM materials also lead to the fact that no single sample dimen- strength, but slightly lowers hydrothermal aging resistance
[9,10]. More recently, zirconia is being stabilized with higher yttria
contents to obtain even higher translucency (Fig. 3) by decreasing
the grain boundary birefringence (higher content of optically iso-
tropic cubic phase and lower birefringence of the remaining tetrag-
onal phase with smaller c/a tetragonality, Table 1) [9,10,65]. Some
of the new so-called ‘high-translucent’ PSZ already present light
transmission similar to that of LS2 with a low translucency (‘LT’)
or medium opacity (‘MO’). A part of the window in the map is
indeed also filled by these new zirconia ceramics (Fig. 7, Fig. S2
and Fig. S1). Therefore, with the development of high-translucent
zirconia, more indications in fixed prosthodontics can be covered
by monolithic restorations.

5. Conclusions

Despite the common understanding that increasing yttria con-

tent decreases toughening in yttria-stabilized zirconia ceramics
and thus reduces KIC and KI0, 5Y and 4Y PSZs with a higher translu-
cency are promising materials to be used for monolithic restora-
tions. In view of strength versus translucency map, these new
Fig. 7. Scatter plot of flexural strength versus translucency for various CAD-CAM translucent zirconia ceramics can fill a part of the material’s win-
restorative materials, along with the 95% confidence ellipse for each material group. dow between conventional 3Y-TZP and LS2 glass ceramic, even if
Note that zirconia group includes the results of 3Y, 4Y and 5Y materials obtained in the lower Weibull moduli measured require attention in terms of
this work and marked with red star symbols; the glass-infiltrated ceramics include
reliability issues.
a zirconia (the two materials/dots with a strength of about 600 MPa), alumina and
spinel (the two materials/dots with higher translucency) version; the ellipse for this All investigated zirconia ceramics showed a similar relative sus-
group is an illustration, but does not represent the 95% confidence ellipse because of ceptibility to static and cyclic SCG with a parallel shift of V-KI
the highly scattered data. In order to limit bias due to the different measurement curves. Cyclic fatigue degradation was significant, but modest for
methodologies employed, mainly bending strength was included, while the the four ceramics investigated and was not influenced by the trans-
translucency values were normalized to the light transmission through IPS e.max
CAD (Ivoclar Vivadent). More detail of the data sources consulted can be found in
formation toughening effect. LS2 glass-ceramic was less SCG-
the supplementary Table S1 and Fig. S1. (For interpretation of the references to resistant than zirconia ceramics, due to its susceptibility to
colour in this figure legend, the reader is referred to the web version of this article.) chemically-assisted stress corrosion. However, LS2 with pro-
 F. Zhang et al. / Acta Biomaterialia 91 (2019) 24–34 33

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