Dental Materials 39 (2023) 463–468

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Dental Materials
journal homepage: www.elsevier.com/locate/dental

Microstructure, composition, and flexural strength of different layers within

zirconia materials with strength gradient ]]
]]]]]]
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Thomas Strassera, , Markus Wertzb, Andreas Koenigb, Torsten Koetzschc, Martin Rosentritta
⁎

a
Department of Prosthetic Dentistry, University Hospital of Regensburg, 93053 Regensburg, Germany
b
Department of Prosthodontics and Material Sciences, Leipzig University, 04103 Leipzig, Germany
c
Institute of Mineralogy, Crystallography and Materials Science, Leipzig University, 04275 Leipzig, Germany

A R T I C L E I N F O A B S T R A C T

Keywords: Objectives: The aim of this study was to compare composition, microstructure, and mechanical strength of
Multilayer current multilayer zirconia blanks.
Zirconia Methods: Bar shaped specimens were made from several layers of multilayer zirconia blanks (Cercon ht ML,
3Y-TZP Dentsply Sirona, US; Katana Zirconia YML, Kuraray, J;SHOFU Disk ZR Lucent Supra, Shofu, J; priti multidisc
4Y-TZP
ZrO2 Multi Translucent, Pritidenta, D; IPS e.max ZirCAD Prime, Ivoclar Vivadent, FL). Flexural strength was
5Y-TZP
determined in a three-point bending test on extra-thin bars. X-ray diffraction (XRD) with Rietveld refinement
XRD
X-ray diffraction was used to assess crystal structure and scanning electron microscopy (SEM) imaging to visualize the micro­
Flexural strength structure of each material and layer.
SEM Results: Mean flexural strength varied between 467.5 ± 97.5 MPa (top layer, IPS e.max ZirCAD Prime) and
898.0 ± 188.5 MPa (bottom layer, Cercon ht ML) with significant (p ≤ 0.055) differences between the in­
dividual layers. XRD indicated 5Y-TZP for enamel-layers, 3Y-TZP for dentine-layers, individual mixtures of 3Y-
TZP, 4Y-TZP, or 5 Y-TZP for intermediate layers. SEM analysis showed grain sizes between approx. 0.15 and
4 µm. Grain size tended to decrease from top to bottom layers.
Significance: The investigated blanks differ predominantly in the intermediate layers. In addition to di­
mensioning of restorations, the milling position in the blanks must also be taken into account when using
multilayer zirconia as restorative material.

1. Introduction % Y2O3 as high strength, opaque zirconia features a high proportion of

At present, it appears that - in terms of technical complications -
monolithic restorations have a better clinical performance than ve­
neered restorations [1,2]. In this context, there is a need for restorative
materials that provide sufficient mechanical strength for wide-span
restorations and sufficient translucency for adequate esthetic design.
Zirconia materials with increasing translucency have been developed
for this purpose [3]. The factors that determine the translucency of
zirconia materials are complex and include the admixture of dopants,
blank fabrication, and the sintering process. These factors affect the
microstructure in terms of crystal structure and the occurrence of
porosities which, in turn, define light scattering and macroscopic opa­
city/translucency of the materials [4–7]. Varying the proportion of
Y2O3 added for stabilization is an essential aspect for increasing the
translucency of zirconia materials. "3Y-TZP" with an admixture of 3 mol
85–90 % tetragonal phase, which produces a stabilizing effect due to a
local volume increase resulting from the transformation of the tetra­
gonal into the monoclinic phase. "3Y-TZP" include two formulations,
either with an alumina concentration of 0.25 % by weight or the later
developed "3Y-TZP-LA/NA" (LA: low aluminum, NA: no aluminum)
with lower alumina concentrations down to 0.05 % and improved
mechanical properties and translucency [8,9]. In addition to “3Y-TZP”,
there are “4Y-TZPs” and “5Y-TZPs” with a respective share of 4 mol% or
5 mol% Y2O3 and an increased translucency, that feature an increased
cubic proportion of the crystal structure (5Y-TZP: approx. 50 %).
However, the increased translucency of these materials coincides with
less mechanical strength [10–14].
In order to profit from the individual advantages of different zir­
conia materials, multilayer blanks have been introduced. These multi­
layer blanks include several vertical layers with an individual

⁎
Correspondence to: Franz-Josef-Strauß-Allee 11, 93053 Regensburg, Germany.
E-mail address: thomas.strasser@ukr.de (T. Strasser).

https://doi.org/10.1016/j.dental.2023.03.012
Received 15 September 2022; Received in revised form 1 February 2023; Accepted 3 March 2023
0109-5641/© 2023 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.
T. Strasser, M. Wertz, A. Koenig et al. Dental Materials 39 (2023) 463–468

composition of 3Y-, 4Y- and/or 5Y-TZP and feature a translucency and
color gradient. At the top of the blanks, there are translucent portions
for incisal edges and cusps. At the bottom of the blanks, there are
opaque high strength portions for dentin and cervical parts. These
materials are intended for the fabrication of monolithic restorations
that feature both high strength and aesthetic appearance. Such strength
gradient multilayer blanks must be distinguished from multicolor
blanks, which consist entirely of a single zirconia type and merely
feature a color gradient. The rapid and continuous development of new
products leads to a confusing variety of materials on the dental market
and makes an optimal material selection challenging. Currently, there
are no long-term clinical data concerning restorations fabricated from
the respective materials. However, previous studies have shown that
the positioning of restorations within multilayer blanks may affect the
fracture force of the final restoration [15,16]. Against this background,
the aim of this study was to compare the phase composition, micro­
structure, and individual mechanical strength of current multilayer
zirconia blanks. The investigated hypothesis was that specimens milled
from different vertical positions within multilayer zirconia blanks
would not exhibit individual flexural strength in a three point bending
test. Further study aims were to investigate whether specimens milled
from individual positions within multilayer blanks exhibit individual
crystal structure and microstructure.
determined in a three point bending test (v = 1 mm/min, support
distance: 12 mm, radius of the support cylinders: 2 mm, radius of the
cylindrical loading piston: 2 mm; Z010, Zwick, D). Mean values and
standard deviations were determined and ANOVA and Bonferroni post-
hoc test were performed using a level of significance α 0.055.
2.2. Phase composition by X-ray diffraction (XRD)
For the analysis of phase compositions, a D8 Discover (Bruker AXS
Advanced X-ray Solutions GmbH, Karlsruhe, Germany) with a VÅNTEC-
500 (Vantec Thermal Technologies, Fremont CA, USA) area detector
and CuKα radiation (λ = 1.5418 Å; 40 kV / 40 mA) was used.
Data were gathered on the fracture edges of the specimens that had
previously been subjected to the three point bending test using the
measurement setup described by Wertz et al. [17]. Integration was
carried out using the software DIFFRAC.EVA (Version 3.1; Bruker AXS
Advanced X-ray Solutions GmbH, D).
For indication of the reflections, a Rietveld refined phase model
which included monoclinic (M), tetragonal (T, T’’), and cubic (C) phases
was used [17]. Texture effects and irregularities on the surface resulting
from the break-up were taken into account using a preferred orientation
approach according to March-Dollase [18,19] and a surface roughness
correction [20].

2. Materials and methods 2.3. Microstructure imaging by scanning electron microscopy (SEM)

2.1. Flexural strength
Bar shaped specimens (1 mm × 4 mm x 15 mm; n = 10 per in­
vestigated material and position) were milled from individual layers
within multilayer zirconia blanks. The milling positions were arranged
to represent the individual layers as provided by the manufacturers. For
the materials Cercon ht ML, Katana Zirconia YML, SHOFU Disk ZR
Lucent Supra four layers and for priti multidisc ZrO2 Multi Translucent
as well as IPS e.max ZirCAD Prime three layers were tested (Table 1). In
order to ensure that the bars were entirely located in the corresponding
zirconia layer, the bars were constructed with a reduced thickness in
comparison to standardized ISO specimens. Specimens were sintered
according to the manufacturers’ instructions (inFire HTC, Sirona, D).
Specimens were used as milled and not further processed. In order to
guarantee essential consistent conditions for the test, the specimens
were measured at three locations (Holex digital 150, Hoffmann group,
D) and controlled for constant geometry. Flexural strength was
SEM imaging (Quanta FEG 400, FEI, USA) was used to visualize the
individual microstructure of each material and layer. The specimens
were examined at magnifications between 10,000x and 30,000x (Low
vacuum; WD: 9.4 – 10.7 mm; HV: 15 keV).
3. Results
3.1. Flexural strength
ANOVA and Bonferroni post-hoc test showed significant (p ≤ 0.05)
differences in the mean flexural strength of individual layers of each in­
vestigated material (Table 2). Mean flexural strength (in MPa) ranged
between 521.7 ± 61.6 and 898.0 ± 188.5 (Cercon ht ML), 475.1 ± 85.9
and 765.0 ± 153.8 (Katana Zirconia YML), 491.0 ± 177.5 and
737.4 ± 122.9 (SHOFU Disk ZR Lucent Supra), 481.9 ± 111.7 and
707.2 ± 162.0 (priti multidisc ZrO2 Multi Translucent), and 467.5 ± 97.5
and 695.8 ± 71.8 (IPS e.max ZirCAD Prime).

Table 1
Groups; materials, manufacturers; milling positions (E: enamel; I1 / I2: intermediate 1 / 2; C: cervical).

Code Material Manufacturer Milling position (top to Layering

bottom) (manufacturer‘s information)

Material Position Thickness mm Nomenclature

C E Cercon ht ML Dentsply Sirona, USA 1 1.3 Incisal and transition areas

I1 2 1.3
I2 3 1.3
C 4 14.0 Dentin area
K E Katana Zirconia YML Kuraray, J 1 6.3 Enamel
I1 2 2.7 Body 1
I2 3 2.7 Body 2
C 4 6.3 Body 3
S E SHOFU Disk ZR Lucent Supra Shofu, J 1 4.2 Enamel
I1 2 4.9 Dentin (1st, 2nd, 3rd
I2 3 Layer)
C 4 4.9 Cervical
P E priti multidisc ZrO2 Multi Pritidenta, D 1 3.0 5Y-TZP
I Translucent 2 5.0 5Y-TZP / 3Y-TZP
C 3 12.0 3Y-TZP
E E IPS e.max ZirCAD Prime Ivoclar Vivadent, FL 1 3.2 Incisal
I 2 3.2 Transition
C 3 9.6 Dentin

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T. Strasser, M. Wertz, A. Koenig et al. Dental Materials 39 (2023) 463–468

Table 2 grain sizes. The layer structures of Cercon ht ML and priti multidisc
Flexural strength: superscript letters indicate significant differences in flexural ZrO2 Multi Translucent showed several changes between areas with
strength of individual layers of the respective material; structural analysis: larger (Fig. 2: blue arrows) and smaller grain size (Fig. 2: red arrows) in
major components of each layer according to XRD (3Y-TZP consisted mainly of the vertical direction. In the intermediate layers of SHOFU Disk ZR
the tetragonal phase T, small amounts of the tetragonal phase T’’, and the
Lucent Supra, coarse-grained areas were identified (Fig. 2: green ar­
monoclinic phase M; 4Y: T/T’’, small amounts of M, C; 5Y: T’’/C, small amounts
rows), which were embedded in a fine-grained base structure.
of M, T, C); 1 Consisted of a mixture of 3Y-/4Y-/5Y- PSZ, with a yttria content
between 3Y and 5Y.
4. Discussion
Code Flexural strength / MPa Phase
composition
Material Position Mean SD (XRD)
4.1. Flexural strength

C E 521.7a 61.6 5Y The investigated hypothesis, suggesting that specimens milled from
I1 667.1b 124.5 Mixture1 different vertical positions within multilayer zirconia blanks would not
I2 663.5c 238.5 Mixture1
C 898.0a, b, c 188.5 3Y
exhibit individual flexural strength in a three point bending test, was
K E 475.1a, b 85.9 5Y rejected. For all investigated materials, significant differences in flex­
I1 583.5c 72.1 Mixture1 ural strength were identified for specimens fabricated from individual
I2 765.0a, c 153.8 Mixture1 or several layers. As expected, the flexural strength gradually increased
C 712.5b 152.2 3Y + probable 4Y
from the incisal to the cervical blank areas. These observations are in
S E 491.0a 177.5 5Y
I1 593.3 118.6 Mixture1 line with data from recent publications on multilayer zirconia materials
I2 587.3 98.1 Mixture1 [15,21,22]. The flexural strength that were measured in this study seem
C 737.4a 122.9 3Y comparatively low for the respective zirconia types [23]. This phe­
P E 481.9a 111.7 5Y nomenon might be explained by the test setup of the current study as
I 652.7 171.2 3Y + little 5Y
C 707.2a 162.0 3Y
the edges of the specimens were not refinished. Compared with ISO
E E 467.5a 97.5 5Y tests, the specimens used in the present study have a reduced height and
I 535.2b 78.7 Mixture1 cross-sectional area, which could have affected the results. The small
C 695.8a, b 71.8 3Y cross-sectional area reduces the number of defects per sample, but vo­
lumetric flaws are much more likely positioned critically in a smaller
cross-section [24,25]. This probably leads to lower strength values for
3.2. Phase composition by X-ray diffraction (XRD)
the thinner specimens. Thus, although comparable in principle, test
geometry definitely plays a role in the evaluation of strength results.
XRD confirmed that all manufacturers use 5Y-TZP for their enamel
The measured values should primarily be used for comparison within
layers, while the dentine layers consisted of 3Y-TZP (Table 2). The in­
this investigation rather than comparisons with other studies. In three-
termediate layers included individual mixtures of 3Y-TZP, 4Y-TZP, or
point bending tests, bar-shaped specimens are loaded centrally in such a
5Y-TZP, featuring an increasing yttria content from dentine to enamel
way that the maximal tensile stress is located on the bottom of the bars
layers (Fig. 1).
and between the edges. These areas frequently feature flaws, which
may occur during the manufacturing of the specimens. Such flaws can
3.3. SEM microstructure analysis promote the formation of cracks and may finally cause failure of the
specimen [26]. The results of the current study indicated that there are
Fig. 2 shows SEM images of the sintered sample surfaces that re­ large differences in mechanical strength of the respective layers de­
present the vertical blank positions. Grain sizes varied between ap­ pending on the zirconia type. With regard to flexural strength, 5Y-TZP
proximately .15 µm and 4 µm and there was a tendency towards a de­ featured an intermediate position between lithium disilicate and 3Y-
crease from the top to the bottom layers in all investigated materials. TZP [27,28].
Highest overall grain sizes were identified for Katana Zirconia YML,
with only minor differences between the individual layers. Lowest grain 4.2. Phase composition by X-ray diffraction (XRD)
sizes were detected in the bottom layers of priti multidisc ZrO2 Multi
Translucent and IPS e.max ZirCAD Prime. Within the top and bottom Concerning the study aim to investigate whether specimens milled
layers of each material, the grain size varied only slightly. In contrast, from individual positions within multilayer blanks exhibit individual
the intermediate layers contained areas with considerably differing crystal structure, XRD confirmed this assumption. As far as indicated,

Fig. 1. Sample comparison of the observed curves of the layers from IPS e.max ZirCAD Prime (cervical, intermediate, enamel) around 35° (a), 60° (b), and 74° (c) in
2Θ with their phase indication (T, T’’, C).

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T. Strasser, M. Wertz, A. Koenig et al. Dental Materials 39 (2023) 463–468

Fig. 2. SEM (magn. 20,000x) of sintered sample surfaces, arranged by materials (C, K, S, P, E) and layers (E: enamel; I1 / I2: intermediate 1 / 2; C: cervical). (For
interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)

the found layer structures and compositions of the respective layers
largely support the information provided by the manufacturers. The
bottom layer consisted of 3Y-TZP in all blanks examined and 5Y-TZP
was always used for the top layer. Yet, some of the blanks differed
considerably with regard to the number and composition of the inter­
mediate layers. Individual compositions with proportions of 3Y-TZP,
4Y-TZP, or 5Y-TZP were identified here. It is therefore clear that the
terms "multilayer" and "monolithic" zirconia, which are sometimes used
as synonyms, should rather be understood as generic terms and that
more precise information, especially with regard to the individual yttria
content of the respective layers, is required to assess the actual material
properties of an individual blank [29].
Fig. 3 displays a sample comparison of the three different layers of
IPS e.max ZirCAD Prime (groups E-E, E-I, E-C) with the observed and
refined diffractograms of enamel, intermediate, and cervical layers. The
diffractograms show a disappearance of the monoclinic phase fraction

466
T. Strasser, M. Wertz, A. Koenig et al.
Fig. 3. Sample exemplary diffractograms for groups E-E (above), E-I (middle), E-C (below) with measured (Yobs) and, calculated (Ycalc), differences between Yobs
and Ycalc (Ydiff) and monoclinic (M), tetragonal (T, T’’), and cubic (C) phases.
(28° and 32°) and a decrease in the reflection splitting at 35°, 60°, and
74°, indicating a decrease in the tetragonal phase T and an increase in
the higher symmetric phase fractions (T'', C). Rietveld refinement
confirmed an increase from 3Y- to 5Y-TZP from dentine to enamel
layers. This method has been successfully used in previous studies to
assess the crystal structure of zirconia materials [17,30]. For most
samples, interpretation was unambiguous, though impurities or minor
components with low concentration are possible. Nevertheless, inter­
pretation of some samples was possibly subject to errors as several
mixtures may be possible or other conceivable interpretations exist (e.g.
3Y + 5Y vs. 4Y). Intermediate layers feature an yttria content that is
between incisal and the dentin layers. Sample preparation with sawing
and machining might affect phase fractions at the sample surfaces
[17,31].
4.3. Microstructure analysis by SEM
Regarding the study aim to investigate if specimens milled from
individual positions within multilayer zirconia blanks show individual
microstructure, SEM analysis confirmed this assumption. The SEM
images in Fig. 2 showed the typical appearance of sintered, poly­
crystalline oxide ceramics with grains closely packed together at the
grain boundaries. All images were taken at the same magnification
(20,000x). In a direct comparison of images from different materials, it
is noticeable that there is a general trend from larger to smaller grain
sizes in the direction from the top / enamel layers to the bottom /
cervical layers. For all investigated materials, the grain size of the top
and bottom layers was rather homogeneous. The intermediate layers
predominantly showed a grain size similar to that of the bottom layers.
However, accumulations of larger grains were embedded here or the
layers seemed to be traversed by interconnected zones with larger grain
size. This tendency was most evident in Cercon ht ML (groups C-E – C-
C) and less distinct in Katana Zirconia YML (groups K-E – K-C), which
featured a comparatively high overall grain size throughout its layers.
In groups C-I1 and C-I2, a transition between two similar grain sizes in
both layers was observed. Smaller grains were identified in the upper
part of the layer and larger grains in the lower part, so that layers with
larger and smaller grains alternate over the entire blank. The S-I1 and S-
I2 layers as well as the P-I layer were similar. Coarse-grained layers
seemed to alternate with fine-grained layers in the vertical direction,
too. Nevertheless, it should be taken into consideration that SEM ima­
ging only displays individual positions and does not provide a complete
overview of the entire specimen.
4.4. Synopsis
Comparing the properties investigated in this study, it is noticeable
that the flexural strength is related to the particular type of zirconia
detected in the respective layers. XRD analysis consistently detected 5Y-
467
Dental Materials 39 (2023) 463–468
TZP in the top/enamel layers. This observation is associated with the
lowest flexural strength measured for the respective blanks and larger
grain sizes than in the layers below. In the bottom layers, XRD analyses
showed only phases typical of 3Y-TZP. Highest flexural strength for
each blank except for Katana Zirconia YML was identified in the bottom
layers. Corresponding characteristics could be visualized in SEM ana­
lysis. Top and bottom layers showed a homogeneous distribution of
small (bottom) / coarse (top) grains.
Varying flexural strength in the intermediate layers may also be
attributed to less homogenous microstructures. In these layers, different
grain sizes are assembled next to each other along large areas. Data of
the current study indicate that increasing yttria content is accompanied
by an increase in grain size and reduced mechanical strength [32].
The maximal force that can be absorbed by a ceramic restoration is
defined by its “weakest link”. With regard to this aspect, occlusal
contacts are critical areas that are exposed to high stress [33]. In crowns
fabricated from multilayer blanks, the positioning of the occlusal / in­
cisal parts in one of the upper or intermediate layers defines the max­
imal force that can be absorbed by the final restoration (Badr et al.,
2022). Compared with the 3Y-TZP layers at the bottom of the blanks,
these layers are mechanically less resilient, and the occlusal / incisal
parts of the restorations are exposed to strong loads from the mastica­
tory forces. Thus, these parts represent the “weakest link” of the a re­
storation, the part from which cracks may originate, propagate further
towards the edges, and finally cause failure of the whole restoration.
Ceramics can withstand compressive loads better than tensile loads. In
the clinical application of all-ceramic fixed partial dentures, a high risk
of failure is to be expected if tensile stresses act in a weaker portion of
the restoration. In the occlusal / incisal region, compressive stresses are
more prevalent. Nevertheless, tensile stress might occur especially in
accentuated fissure areas. The bottom of the connectors are critical
areas where highest tensile stress is to be expected [34]. Thus, it might
be advantageous to avoid the positioning of connectors in the upper­
most layers. Users should be aware of the fact that the layer structure of
the blanks from different manufacturers is extremely different
(Table 1). While the high-strength bottom layer of Cercon ht ML ac­
counts for more than 75 % of the blank height, it is approx. 35 % for
Katana. This results in individual positioning specifications of the
manufacturers, which must be taken into account in the design of the
restorations. In order to ensure an appropriate application, dentists and
dental technicians need to understand the individual properties of these
multilayer materials. 3Y-TZP should be preferred over multilayer ma­
terials for restorations subjected to high forces, such as cantilever fixed
partial dentures.
5. Conclusion
All investigated blanks feature a layered structure. The composition
of the individual layers varied within the blanks. 5Y-TZP zirconia was
T. Strasser, M. Wertz, A. Koenig et al. Dental Materials 39 (2023) 463–468

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