RESEARCH AND EDUCATION

Fracture toughness of two lithium disilicate dental glass

ceramics
Lubna Alkadi, DDS, MSca and N. Dorin Ruse, MSc, PhD, MCIC, FADMb

Because of their natural appear- ABSTRACT

ance, translucency, biocompati- Statement of problem. IPS e.max CAD and IPS e.max Press (Ivoclar Vivadent AG) are lithium
bility, and optical properties, disilicate glass ceramics marketed as interchangeable materials indicated for the same clinical uses.
ceramics have become increas- However, different crystal sizes of lithium disilicate are formed during the processing of each of
ingly popular in dentistry.1-3 these materials, a factor that could lead to signicantly different mechanical properties. As me-
High demand motivates manu- chanical failure is always associated with a crack-initiation/crack-propagation process, fracture
facturers to introduce new and toughness (KIC) values could be useful in comparing different ceramics and possibly predicting
clinical performance.
improved ceramics, each claim-
ing superior esthetic, physical, Purpose. The purpose of this in vitro study was to determine and compare the KIC of IPS e.max CAD
and mechanical properties. In and IPS e.max Press.
addition, the fully digitized pro- Material and methods. The notchless triangular prism (NTP) specimen KIC test was used to
duction of dental restorations determine and compare the KIC of IPS e.max Press and IPS e.max CAD. Twenty 66612-mm NTP
involving digitized impression specimens of each material were prepared. IPS e.max CAD blocks were cut, ground, and then
making and computer-aided crystallized, while IPS e.max Press specimens were prepared by pressing IPS e.max Press ingots
design and computer-aided into molds obtained from 66612-mm wax prisms, using the lost wax technique. Each
specimen was mounted into a specimen holder, and custom grips were used to attach the
manufacturing (CAD/CAM) has
specimen holder assembly to a computerized universal testing machine (model 4301; Instron
led to the introduction of a new Canada, Inc). The assembly was loaded in tension at a crosshead speed of 0.1 mm/min, and the
category of machinable ce- KIC value was calculated based on the recorded maximum load at fracture. Fractured surfaces
ramics.4-7 were characterized using scanning electron microscopy (SEM). Results were statistically analyzed
Despite their favorable char- using Weibull statistics and the Student t test (a=.05).
acteristics, considerable con- Results. Signicantly (P<.05) higher KIC value was determined for IPS e.max Press than for IPS e.max
cerns remain regarding the CAD and, based on the Weibull modulus (m), IPS e.max Press was also more reliable. Fractured
mechanical properties of ce- surfaces, characterized by SEM, showed a marked difference between the 2 materials, suggesting a
ramics.8 The brittle ceramic more complete crystallization in IPS e.max Press, which was most likely responsible for the higher
materials may exhibit cata- KIC determined.
strophic fractures, particularly Conclusion. Within the limitations of this in vitro study, the results suggest that IPS e.max Press is
when exposed to tensile superior to IPS e.max CAD with regard to the KIC and characteristic Weibull parameters. (J Prosthet
stresses,9 which remains the Dent 2016;-:---)
main cause of their failure.10
IPS e.max is the name given by Ivoclar Vivadent AG ZirPress, and IPS e.max ZirCAD) and a veneering ma-
to a range of ceramic products that include 4 core ma- terial (IPS e.max Ceram). The products of interest in this
terials (IPS e.max Press, IPS e.max CAD, IPS e.max study, IPS e.max Press and IPS e.max CAD, are both

Presented as a poster at the 91st General Session of the International Association for Dental Research, Seattle, Wash, March 2013.
a
Assistant Professor, Division of Prosthodontics and Restorative Dentistry, Faculty of Dentistry, King Saud bin Abdulaziz University for Health Sciences, Riyadh, Saudi Arabia.
b
Professor, Division of Biomaterials, Faculty of Dentistry, The University of British Columbia, British Columbia, Vancouver, Canada.

THE JOURNAL OF PROSTHETIC DENTISTRY 1

2 Volume
Clinical Implications
Short- and long-term in vivo performance of
ceramics may be governed by, among other factors,
their resistance to crack propagation as determined
by their KIC values. Based solely on the KIC, the
clinical performance of IPS e.max Press may be
better than that of IPS e.max CAD.
lithium disilicate glass ceramics designed to have 2
different processing pathways for the fabrication of
ceramic restorations. Both of the materials can be used to
produce cores that can be veneered with feldspathic
ceramic (IPS e.max Ceram). They can also be used as
monolithic materials in the fabrication of anatomic con-
tour restorations (Ivoclar Vivadent AG; http://www.
ivoclarvivadent.com/en/p/all/products/all-ceramics/ips-emax-
technicians/download-center-ips-emax; 2016). In addition
to the monolithic block category, the IPS e.max CAD
system was recently expanded to include a second
category of blocks intended for veneering zirconia
substructures and a third category used to fabricate
implant-supported abutments for single teeth, where the
lithium disilicate milled components are bonded to a
titanium base. All are available in a wide variety of shades
and opacities.
IPS e.max CAD is a lithium disilicate glass ceramic
designed to be used with CAD/CAM technology. A
process called pressure casting leads to the production
of partially crystallized IPS e.max CAD blue blocks.
These blocks are composed of 40% lithium metasilicate
crystals ranging in size from 0.2 to 1.0 mm, embedded in
a glassy matrix. The partially crystallized state facilitates
a faster milling process. After restorations are milled to
the desired shape and contour, they are tempered at
850 C in furnaces developed by the manufacturer for
this material (Programat P300/P500; Ivoclar Vivadent
AG). In this process, lithium metasilicate crystals are
transformed into lithium disilicate crystals (70% volume
fraction), which are responsible for the high strength of
the material.11 The coloring ions responsible for the blue
color in the partially crystallized stage change the
oxidation state when tempered, leading to the desired
tooth color.
IPS e.max Press is supplied as ingots of lithium dis-
ilicate glass-ceramic in several monochromatic shades, 4
translucencies, and 2 sizes. Currently, new polychromatic
ingots (IPS e.max Press Multi; Ivoclar Vivadent AG)
provide a gradient of shades and translucencies
mimicking those of a natural tooth. These are supplied in
10 shades and a single size. The microstructure of IPS
e.max Press consists of approximately 70% lithium dis-
ilicate crystals measuring 3 to 6 mm in length. This
THE JOURNAL OF PROSTHETIC DENTISTRY
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12 mm
6 mm 6 mm
6 mm
Figure 1. Notchless triangular prism specimen.
product is processed with the lost wax technique, which
involves waxing the restorations to the desired contours,
sprueing, and investing the wax patterns, melting the
wax to create a mold within the investment, and then
heat pressing the molten ingot into the mold in a furnace
developed specically for this product. Restorations are
then divested, polished, characterized, and glazed before
delivery.
Clinical evidence shows that IPS e.max Press has a
survival rate of 96.6% over 3 years for single crown res-
torations.12 A study that evaluated xed partial dentures
fabricated from monolithic IPS e.max Press and observed
them for a mean period of 121 months found the survival
rate to be 100% after 5 years and 87.9% after 10 years.
The success rate was 91.1% after 5 years and 69.8% after
10 years.13 A clinical evaluation of single IPS e.max CAD
crowns showed 100% success after 2 years.14 However,
long- or short-term controlled clinical trials comparing
both materials are lacking.
Fracture toughness (KIC) is an intrinsic material
property, which describes the materials ability to with-
stand unstable crack propagation and which correlates
with clinical performance (fracture and wear).3,15 As
mechanical failure is always associated with a crack-
initiation/crack-propagation process, KIC values are use-
ful in comparing different ceramics and, possibly, in
predicting clinical performance. Many methods are
available for assessing KIC, among which the most
commonly used are the single-edge notched beam
(SENB), the chevron notched short rod (CNSR), and the
indentation fracture (IF) methods.16 To ensure repro-
ducibility, the international standardization of testing
procedures has been accomplished through detailed de-
scriptions of specimen congurations and dimensions, as
well as test protocols and is summarized in the American
Society for Testing and Materials (ASTM) standard
E1820-15.17 Most specimen congurations require pre-
crack initiation, which can lead to unstable crack growth.
The SENB method, although it does yield a stable crack,
is technique-sensitive.18 The CNSR specimen KIC test
developed by Barker19 is accepted by the ASTM.20
However, the specimen preparation involves cutting a
Alkadi and Ruse
- 2016
Figure 2. NTP specimen in holder, in mounting block, with spacer in
place. NTP, notchless triangular prism.
chevron-shaped notch into a cylindrical specimen, a
process that is difcult to achieve, particularly with brittle
materials such as ceramics. The notchless triangular
prism (NTP) specimen KIC test was developed to over-
come the difculties associated with the preparation of
CNSR specimens.21 The NTP specimen (Fig. 1) achieves
a nal conguration similar to that of the CNSR spec-
imen when tted into the specimen holder (Fig. 2),
thereby eliminating the difcult notching procedure.21
The NTP test was validated through nite element
analysis, and a calibration study was done in which
materials of known KIC were tested using the NTP and
the standard CNSR methods, leading to comparable re-
sults.21 The NTP test is a suitable method for determining
both material and adhesive interfacial KIC.21-25 The NTP
test was described as superior because of the simplicity of
specimen preparation.26
Two studies were found that report the KIC values for
IPS Empress 2 (Ivoclar Vivadent AG), a lithium disilicate
pressable glass-ceramic and predecessor of IPS e.max
Press. These studies reported the KIC of IPS Empress 2 to
be 3.4 MPa$m1/2 27 and 3.14 MPa$m1/2.28
IPS e.max Press and IPS e.max CAD are marketed as
clinically identical materials indicated for the same clin-
ical uses. However, different crystal sizes of lithium dis-
ilicate are formed during the manufacturing/processing of
each of these materials. Moreover, the different pro-
cessing methods involved in the processing of the ma-
terials may lead to signicantly different mechanical
properties. It would therefore be of interest, from both a
materials science point of view and a clinical usage point
of view, to characterize the materials in vitro, as a step
toward recommending one over the other in clinical
applications. The purpose of the current study was to
determine the KIC of IPS e.max Press and IPS e.max CAD
to test the null hypothesis that there is no signicant
difference in the KIC of the 2 materials.
Alkadi and Ruse
3
Figure 3. Custom-built grinder.
MATERIAL AND METHODS
The NTP specimen KIC test was used to determine and
compare the KIC values of IPS e.max Press and IPS
e.max CAD. A power analysis was used to calculate the
sample size (n) needed to detect a difference of 20%
among the groups, with an a value of .05 and power of
80%, using Lehrs basic formula29: n=D162 , where the
standard difference (D) is given by D = d/s, and d is the
target difference, and s is the standard deviation (SD).
The calculation was based on the results of a pilot
study that yielded a mean of 2 MPa$m1/2 and an SD of
0.3 MPa$m1/2. Based on the above, n was calculated to
be 9.
However, for materials susceptible to brittle fractures,
such as ceramics, Weibull statistics are recommended. In
Weibull statistical analysis, the probability of failure, Pf, is
related to the fracture stress by the following exponential
relationship30:
h  m i
s su
s0
Pf =1 e
In order analyze the results with Weibull statistics, 20
specimens were prepared for each group.31
IPS e.max CAD blocks were supplied by the
manufacturer (Ivoclar Vivadent AG). Twenty NTP
specimens were prepared by cutting and grinding.
Each IPS e.max CAD block was cut into 4 equal
rectangular blocks with diamond-impregnated slicing
wheels (UKAM) mounted on a low-speed saw
(Isomet; Buehler) and under continuous water irriga-
tion. Again under continuous water irrigation and
using a custom-built holder (Fig. 3), each of these
smaller blocks was then ground on consecutively ner
grit SiC paper (Buehler) up to 600 grit, mounted on a
grinding machine (Buehler) until 66612-mm NTP
specimens were obtained. The prisms were crystalized
in a furnace (Programat P500; Ivoclar Vivadent AG) at
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4 Volume - Issue -

Table 1. Results of mean SD fracture toughness (KIC) and statistical

analyses
Characteristic
Weibull Weibull KIC
Material KIC (in MPa$m 1/2
) Modulus (m) (in MPa$m1/2)
IPS e.max CAD 1.79 (0.26) 8.41 1.90
IPS e.max Press 2.50 (0.31)* 9.74 2.64
*Signicantly higher KIC value (Student t test; P<.05).

IPS e.max Press and IPS e.max CAD

3.000
y = 8.4088x 5.3585 y = 9.7448x 9.4073
2.000 R2 = 0.95788 R2 = 0.95813

1.000

In(In[1/(1-Pf)])
Figure 4. Custom grips attaching NTP specimen holder to testing
machine. NTP, notchless triangular prism. 0.000
0.200 0.400 0.600 0.800 1.000 1.200 1.400
1.000

840 C, following the protocol recommended by the 2.000

manufacturer.
IPS e.max Press ingots were supplied by the manu-
facturer (Ivoclar Vivadent AG). Twenty 66612-mm
NTP specimens were prepared by waxing, investing,
and pressing. To wax these prisms, a slightly oversized
(by w0.1-mm) polymethyl methacrylate (PMMA [Plex-
iglass]) prism was impressed using medium-body poly-
vinylsiloxane impression material (Aquasil; Dentsply
Intl). The prism was then retrieved, leaving a mold into
which melted dipping wax (Whip Mix Corp) was
repeatedly poured to produce 20 wax prisms. These wax
prisms were invested using the lost wax technique, and
IPS e.max Press was pressed into the molds at the Ivoclar
Vivadent headquarters in Amherst, NY. The prisms were
then polished to nal dimensions, with 600 SiC paper
under continuous water irrigation.
To determine KIC, 20 NTP specimens of each material
were tested. In each specimen, a defect (w0.1 mm) was
initiated with a sharp diamond disk secured between 2
PMMA blocks at a point midway along one of its edges
and aligned with the split line created by the spacer
placed between the 2 halves of the specimen holder
(Fig. 2). The specimen-holder assembly was then loaded
in tension at 0.1 mm/min with custom-designed grips
(Fig. 4) attached to a computerized universal testing
machine (Instron model 4301; Instron Canada, Inc)
equipped with a 1-kN Instron load cell (accuracy of
0.25% of the indicated load). The maximum load, Pmax,
recorded before fracture was used to calculate the KIC
value from the following equation21,32:
Pmax

KIC =Ymin ; modulus (m) and characteristic Weibull KIC than IPS
DW 1=2
where D is the specimen diameter (12 mm), W is the
specimen length (10.5 mm), and Y*min is the dimen-
sionless stress intensity factor coefcient minimum, of
3.000
e.max press
4.000 e.max CAD
5.000
In(KIC)
Figure 5. Weibull plot of KIC results.
28, as proposed by Ruse et al.21 Selected fractured
specimens were gold coated and characterized using
scanning electron microscopy (SEM; model S-3000N;
Hitachi).
Weibull statistical analysis was used to evaluate the
characteristic KIC and the reliability of each material.30
The Weibull modulus (m), represented by the slope of
the curves, indicates the reliability of each material (the
steeper the curve, the more reliable the material). Char-
acteristic Weibull KIC value was obtained from the plot at
the 63.2 percentile point.
An independent Student t test (a=.05) was also per-
formed to compare the results.
RESULTS
Results are summarized in Table 1 and in the Weibull
plot in Figure 5. The Student t test results showed that
IPS e.max Press (2.50 0.31 MPa$m1/2) had signicantly
(P<.05) higher KIC than IPS e.max CAD (1.79 0.26
MPa$m1/2). Results of the Weibull analysis revealed that
IPS e.max Press had higher values of both the Weibull
e.max CAD.
Figure 6 shows typical examples of a fractured IPS
e.max CAD surface (Fig. 6A1-A3) and IPS e.max Press
surface (Fig. 6B1-B3). At 50 magnication (Fig. 6, A1, B1),

THE JOURNAL OF PROSTHETIC DENTISTRY Alkadi and Ruse

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Figure 6. Scanning electron micrographs of fractured surfaces of IPS e.max CAD (A1) and IPS e.max Press (B1) specimens at 50 (A1, B1), 5000 (A2, B2)
and 10 000 (A3, B3) magnication.

one half of the fractured prism is shown, with the defect- propagation through the glassy matrix, whereas the IPS
induced zone at the tip of each prism. At higher mag- e.max Press surface looks rough and irregular, with
nications of 5000 and 10 000, the IPS e.max CAD minimal glassy matrix visible and an almost entirely
surface looks smooth (Fig. 6A2, A3), indicating a crack crystallized surface (Fig. 6B2, B3).

Alkadi and Ruse THE JOURNAL OF PROSTHETIC DENTISTRY

6 Volume
DISCUSSION
Analysis of the KIC results showed that IPS e.max Press
had signicantly (P<.05) higher KIC values than IPS
e.max CAD and that it also had higher values of both
Weibull m and characteristic Weibull KIC; therefore, the
null hypothesis was rejected. The KIC values determined
in this study (Table 1) were in agreement with the
manufacturers in-house testing reported values, which
were 2.5 to 3 MPa$m1/2 for IPS e.max Press and 2.0 to 2.5
MPa$m1/2 for IPS e.max CAD. Although manufacturers
in-house testing is considered the initial source of sci-
entic documentation for their products before release,
these results would have more value if conrmed by an
independent investigation to eliminate bias. No studies
were found comparing the KIC of the 2 materials or
reporting on the individual KIC values of either material.
Studies of IPS Empress 2, which is IPS e.max Presss
predecessor, showed a higher KIC value than that found
for IPS e.max Press in the current study.24-26 However,
IPS Empress 2 was not compared to any machinable
lithium disilicate in those studies, and therefore, the re-
sults cannot be related to those found in the current
study.
The difference identied between the KIC values for
IPS e.max Press and CAD can be attributed to the higher
amount of glassy matrix and reduced crystal phase and to
the smaller crystal size of the IPS e.max CAD. When the
SEM images of fractured surfaces were examined, IPS
e.max CAD showed a relatively smoother surface, and
the crack seemed to propagate within the glassy matrix
(Fig. 6, A2, A3), while IPS e.max Press appeared to have a
rougher surface with visible multiple crystals embedded
within the glassy matrix (Fig. 6, B2, B3). This suggests
that in the case of IPS e.max Press the presence of
crystals impeded crack propagation and was responsible
for its higher KIC. The higher Weibull modulus (Table 1)
determined for IPS e.max Press in this study suggests
that it is more reliable than IPS e.max CAD.
Based on the results of this study and the SEM
characterization of fractured surfaces, the crystallization
cycle recommended by the manufacturer for IPS e.max
CAD should perhaps be revised, as the fractured surfaces
did not appear to be fully crystallized. Furthermore, the
KIC values determined in this study suggest that IPS
e.max Press is a better material than IPS e.max CAD. This
information may help clinicians make decisions regarding
material selection. However, only long-term clinical trials
can conrm the in vivo superiority of one material over
the other.
CONCLUSIONS
Within the limitations of this in vitro study, the results
suggest that IPS e.max Press is better than IPS e.max
THE JOURNAL OF PROSTHETIC DENTISTRY
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CAD with regard to KIC and characteristic Weibull
parameters.
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Alkadi and Ruse THE JOURNAL OF PROSTHETIC DENTISTRY