REPORT No 17 | June 2006

Research and Development Ivoclar Vivadent AG

FL-9494 Schaan / Liechtenstein

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TA B L E O F C O N T E N T S

Dr Thomas Völkel

4 Editorial

Dr Harald Bürke

6 IPS e.max Press and IPS e.max CAD

Two state-of-the-art glass ceramics

Frank Rothbrust

17 IPS e.max ZirCAD

Zirconium oxide – ”White gold“

Marcel Schweiger

26 IPS e.max Ceram

The universal veneering ceramic – One for 4

Marcel Schweiger

34 IPS e.max ZirPress

The pressable veneering ceramic

Harald Kerschbaumer

37 IPS e.max
The development in terms of dental technology and shading

Dr Alexander Stiefenhofer | Harald Kerschbaumer

41 IPS e.max
Two clinical cases

3
 EDITORIAL

With the launch of IPS Empress in 1991, Ivoclar Vivadent achieved a

breakthrough in the development of all-ceramic dental restorations.
IPS Empress is a glass-ceramic, which is composed of a glass matrix and rein-
forcing crystalline contents. The crystals in IPS Empress are made of leucite. The
ceramic exhibits sufficient strength for the fabrication of crowns, inlays, onlays
and veneers. Within these indications, IPS Empress has been replacing metals
and alloys. Consequently, the biocompatibility and aesthetics of dental restora-
Dr Thomas Völkel tions has been considerably improved. IPS Empress restorations are fabricated
by means of an efficient heat-pressing technique, which endows the restora-
tions with a high accuracy of fit. This processing technique has proven itself for
all-ceramic restorations. Although IPS Empress continues to be the market
leader in this segment, 25 competitive systems have been developed in the
meantime.

In the further development of all-ceramics, particular attention has been

paid to increasing the strength and perfecting processing methods for the
fabrication of restorations. A stronger material has been achieved in the form
of the lithium disilicate glass-ceramic IPS Empress 2. The strength of this
ceramic enables the fabrication of three-unit anterior bridges if the stipulated
layering thicknesses and connector dimensions are observed.

Even higher strength values are achieved with oxide ceramics. The
strength of yttrium-stabilized zirconium oxide comes close to that of metals. It
is already recognized as a fully-fledged metal replacement. Clinical data
covering longer observation periods are still rare but look promising.

In recent years, CAD/CAM procedures have continuously gained in

popularity. New systems that allow the shape of teeth to be scanned accurately
and modified are gaining in importance on the market. ProCAD from Ivoclar
Vivadent is a leucite ceramic which is milled in CEREC units. The advantage of
this method is that the restorations can be fabricated chair-side. Thus, the
treatment time is considerably reduced. The use of oxide ceramics, such as
zirconium oxide, is only advisable if they are machined.

The new IPS e.max all-ceramic system allows the user to cover the
entire range of indications with only one system. The frameworks are
fabricated using either materials for the press or the CAM techniques.

4
REPORT
 EDITORIAL

– IPS e.max Press is a lithium disilicate glass-ceramic for the press

technique. Due to its fracture strength of 400 MPa, the material is suitable
for the fabrication of 3-unit bridge frameworks up to the second premolar
as a distal abutment.

– IPS e.max CAD is also based on lithium disilicate glass-ceramics. The

blocks are in a pre-crystallized metasilicate phase. The blocks appear blue
in colour, are soft and can thus be quickly milled to crown copings. In
addition, they prolong the service life of the tools used. The subsequent
crystallization firing endows the blocks with the final lithium disilicate
form. In this crystallization process, the blocks acquire their strength of
360 MPa.

– IPS e.max ZirCAD is a pre-sintered zirconium oxide block that contains

small quantities of yttrium oxide to stabilize the meta-stable tetragonal
phase. In the pre-sintered state, the block features a porous, chalk-like
morphology. After milling the framework, the zirconium oxide is densely
sintered in a process with temperatures up to 1500 °C. The resulting
material has now acquired its final strength of more than 900 MPa.
During the sintering process, the volume shrinks by approx. 20%. This
reduction in volume is already taken into account in the milling program.

– Zirconium oxide is only used for the framework. The white-opaque surface
has to be covered with a more translucent ceramic to achieve aesthetic
restorations. Such a build-up is possible with IPS e.max ZirPress. The
IPS e.max ZirPress ingots are pressed on the zirconium oxide frameworks
in the proven IPS Empress technique.

– IPS e.max Ceram is the layering material that is suitable for sintering on
all the IPS e.max materials.

The present Report No 17 is an addition to a series of issues about all-

ceramics. Number 6 described "IPS Empress – A new ceramic technology”.
Number 10 covered “IPS Empress: Material and clinical science”. “IPS Empress
2: The all-ceramic bridge and more…” was the title of No 12. While a collection
of general articles on all-ceramics was published in the previous issue
No 16, Report No 17 is devoted to the material properties and processing of the
entire IPS e.max system.

The Head of Ceramic Development, Marcel Schweiger, and his co-

workers Frank Rothbrust and Dr Harald Bürke describe the properties of
ceramics, the theoretical background and the procedures during the fabrica-
tion and preparation of restorations. Harald Kerschbaumer, Master Dental
Technician, focuses on dental technical aspects, particularly in the aesthetic per-
fection of restorations. Finally, Dr med dent Alexander Stiefenhofer presents
two clinical cases which he has documented with photos.

The articles, however, can only convey a few aspects of the materials and
their compatibility with each other. For further information, please refer to the
cited literature. It goes without saying that issue No 17 will not be the last report
about all-ceramics.

Dr Thomas Völkel
Scientific Services

REPORT 5
 Dr
IPS e.max Press and IPS e.max CAD Harald Bürke

Two state-of-the-art glass ceramics

1 Introduction Table 1:

IPS e.max Press and IPS e.max CAD are Possible classification of ceramic materials according to different
characteristics (examples)
the two framework materials from the IPS e.max
range that offer medium strength and maximum
aesthetics.
Manufacturing technique: Sintering
IPS e.max Press ingots are particularly Reaction sintering
suitable for single tooth restorations in the
Hot isostatic pressing
anterior and posterior region as well as anterior
bridges with a maximum of 3 units up to the Infiltration
second premolar as the abutment tooth. The
Melting
current range of indications for IPS e.max CAD
includes the fabrication of anterior crown Crystallization
copings. The results of currently conducted
Structure: Crystalline
clinical studies will show whether the range of
indications can be further extended. Both Glassy-amorphous
materials belong to the same group of
Multiple-phase partially crystalline
materials. Depending on the facilities available
in the dental laboratory or the preferences of Composition: Oxide ceramic
the dental technician, either the well-known
IPS Empress press technique or the CAD/CAM Non-oxide ceramic
technique can be chosen. Nitride ceramic
The results after veneering are very similar,
Silicate glass
so that it is even possible to combine both
techniques in one patient. Phosphate glass

Borosilicate glass
After a section with general informa-
tion, the present article will provide a more Alumosilicate glass ceramic
detailed description of the two materials.
Lithium silicate glass ceramic
Special emphasis will not only be placed on the
possibilities of glass ceramics, but also on their Function: Consumer good
limitations. Their potential can be fully tapped
Heat exchanger
only when the preparation guidelines are
strictly observed. Heating conductor

Electroceramic

Optoceramic

Dental ceramic

2 The building blocks of all- Property: Strength

ceramics: Ceramic – glass Resistance to temperature changes

– glass ceramic Electrical conductivity

Chemical resistance
Apart from acrylics, composites and
metal alloys, all-ceramic materials are increa- Thermal conductivity
singly used in dental prosthetics today. By defi-
Shade
nition, ceramic is an inorganic, non-metallic
material which is solidified by means of a firing Translucency
process and has a crystalline content of at least
30 % [1]. In the English language, the term has
an even broader meaning as there is no limita-
tion with regard to the crystalline content.

6
REPORT
 Various criteria are applied to differen- 2.1.3 Reaction sintering
tiate between the different materials in this We speak of reaction sintering if new
large group. The criteria may be eg production components are formed during the sintering
method, composition or function (Table 1). process. This is useful if, for example, the
desired ceramic shows little sintering activity.
Some-times, the changes in volume that occur
2.1 Ceramics as a result of the reaction are used in a
targeted fashion to counteract the shrinkage.
Ceramics in the narrower sense are
predominantly crystalline products which are
2.1.4 Porcelain
produced with the help of a sintering pro-
cedure. For this purpose, the ceramic powders The porcelain firing process represents
are mixed with a bonding agent and the a special case. The crystal phases (quartz,
required, slightly larger moulds are produced. mullite, feldspar, aluminium oxide) are
Various moulding procedures are available, eg surrounded by a large amount of glass phase.
uniaxial pressing, extrusion moulding, slip Apart from solution and precipitation, different
casting, injection casting or cold/hot isostatic chemical reactions occur. The high viscosity of
pressing. The pre-formed materials are fired at the liquid phase prevents deformation of the
high temperatures. During this "sintering" fired material.
process, diffusional mass transport occurs in
the course of which porosity is eliminated. The
driving force for this process is a reduction in 2.2 Glass
surface energy. Each system strives to reach
In the traditional sense, glass is an in-
the lowest possible energy level. The finer the
organic non-metallic, non-crystalline melt pro-
initial powder, the smaller the gaps that have
duct. In this context, the picture of the
to be closed, the larger the surface area that
“frozen super-cooled liquid” is helpful.
needs to be decreased and the higher the
Condensed material has a higher chemical
driving force for the sintering process. Finer
order than glass. Crystals are characterised by
powders show more sintering activity. The
a particularly high order. There is a fixed
grain boundaries also show a higher energy
spatial relationship between all of their atoms,
level than the crystal, eventually leading to
be it the nearest neighbours or more remote
crystal growth in the final stage of sintering.
atoms. A chemical short-range and long-range
Large crystals grow at the cost of small ones.
order exists. In the case of glasses and liquids,
the long-range order is completely annihilated.
2.1.1 Solid-state sintering
However, a short-range order exists, since the
In pure solid-state sintering, the distance from an atom to its nearest neighbour
sintering temperatures are lower than the is predetermined. The glass formation is linked
lowest melting temperature of the compo- to the kinetics of crystallization. Even though
nents involved. Diffusion occurs at the surface the crystals strive to reach the higher order if
of the powder particles and is brought about the temperature falls below the melting point,
by rearrangement within the crystal lattice as crystallization is prevented due to the limited
well as through the gas phase by evaporation mobility of the structural units at lower
and condensation. temperatures.

2.1.2 Liquid-phase sintering 2.2.1 Glass structure

A liquid phase is often used to accele- The prevailing models relating to the
rate the sintering process. A component, of structure of glass are based on the micro-
which the mixture usually only contains a small crystallite hypothesis and the network hypo-
amount, melts at the sintering temperature thesis. According to the microcrystallite hypo-
and wets the solid particles. This enables grain thesis, glass is composed of small, ordered
rearrangement in the initial stage. As sintering structural units of the size of a unit cell, which
proceeds, mass transport occurs through solu- are separated from each other by un-ordered
tion and precipitation, which considerably areas. The network hypothesis is based on the
accelerates the kinetics of sintering. assumption that the structural elements are
randomly connected (Fig 1). Depending on the
glass composition, both hypotheses are
justified. [4].

REPORT 7
 2.2.3 Bulk glass technology
As raw materials, individual oxides,
hydroxides or carbonates are used. They are
thoroughly mixed and jointly melted at high
temperatures. Initially, the chemicals react with
each other, hydroxide groups are segregated
and carbon dioxide is released. Eutectic
mixtures help to decrease the melting
temperature. After initial melting, the melt
must be mixed and homogenized. Trapped air
or gas should be able to escape. This procedure
is called purification. For this purpose, the melt
must have a very fluid consistency. Once the
glass melt is homogeneous and free of air
Fig 1: Amorphous silica structure (b) compared to crystal structure (a) [4] bubbles, the temperature is reduced, so that
the glass becomes more viscous. Depending
on the moulding process used, a clearly defined
viscosity must be achieved. The glass, which
demonstrates a viscosity similar to that of
honey, is poured into eg a separable steel
mould. The material is left to cool in this mould
until it has reached a temperature which
ensures that no deformation occurs during
removal. The corresponding temperature range
is called the transformation temperature range.

The glass is then frozen to a degree

that macroscopic deformation cannot take
place. However, the elements of the glass
structure are still sufficiently flexible to relax
Fig 2: Left: Glass network with sodium (Na) as network modifier the thermal stress. In a cooling furnace which,
Right: Schematic representation of the replacement of SiO2 by Al2O3 in a depending on the glass type, is operated at a
sodium silicate glass [2]
temperature of between approx 400–600 °C,
this stress is relieved before the glass is finally
cooled down to room temperature.
2.2.2 Composition of glasses
Standard glass is composed of network 2.2.4 Sinter glass technology
formers and at least one network modifier.
When coating steel (enamel) or ceramic
(glaze), glass powder is sintered onto a
Usually, silicon dioxide is used as the
substrate. When producing the glass powder,
network former. SiO4 tetrahedrons which are
the raw materials are melted at high tempera-
connected via their corners thus form the glass
tures as usual. However, the glass melt is not
network. Further commonly used network
poured into a mould but quenched in water.
formers are B2O3 or P2O5, either alone or in
Due to the thermal shock, the glass fractures.
combination with SiO2.
The resulting granulate is milled into a fine
powder. In the case of glass, the sintering
The network modifiers serve as fluxing
process is particularly simple. A reduction of
agents. By breaking the Si-O-Si bonds, they
the surface area is achieved by viscous flow
ensure that the glass melts more easily. Alkali
processes. The open porosity found initially is
as well as alkaline-earth oxides are used for
thus quickly eliminated. Further densification is
this purpose (Fig 2).
dependent on whether or not gas is contained
in the remaining closed pores. The rate of
Depending on the composition of the
diffusion of the gases determines the speed of
glass, some bivalent and trivalent oxides can
the final densification.
either be incorporated into the network or
produce gaps. These oxides are called inter-
mediate oxides. By means of the composition,
the properties of glasses can be varied within
broad limits.

8
REPORT
2.2.5 The characteristics of glass The crystal size and number can best
A typical characteristic of glass is a large- be controlled by clearly separating the tempe-
scale homogeneity which is characterized by rature ranges of maximum nucleation and
the absence of grain or phase boundaries. maximum crystal growth (Fig 3). The end pro-
Furthermore, glass is spatially isotropic, which duct is a ceramic whose properties are deter-
means that its properties are the same in all mined by the type, morphology, size, content
directions of space. and degree of cross-linking of the precipitated
crystal phase(s) as well as the remaining glass
The absence of grain boundaries is the phase. The objective of this crystallization pro-
reason for the disastrous fracture behaviour of cess is eg an increase in mechanical strength,
glass. As long as the surface is intact, glass can resistance to temperature changes or the
exhibit extremely high strength. Virgin glass targeted adjustment of thermal expansion and
fibres, for example, have a tensile strength optical or electrical characteristics.
under vacuum of 12,000 to 16,000 MPa.
However, as soon as a crack is initiated, it may The difference between the structure
spread unhindered. The typical shell-shaped of glass ceramics and conventional ceramics is
fracture pattern results. In order to increase the that glass ceramics are exclusively created by a
strength of glass, it is thus particularly important crystallization of the glass phase, so that a
to improve its scratch resistance. This prevents particularly fine-grained and homogenous
the surface of glass products from becoming structure is achieved. Their high crystalline
damaged prematurely and the products from content distinguishes glass ceramics from glasses.
being weakened.
2.3.1 Volume nucleation
Other properties, such as chemical In order to manufacture glass ceramics,
resistance, light refraction and thermal expan- specific glass compositions are often melted in
sion are significantly influenced by the chemical conjunction with special oxides as nucleating
composition. agents, processed like glass and moulded into
a transparent glass block. The additives
dramatically accelerate the nucleation that
2.3 Glass ceramics occurs within the glass in various ways. The
difficult thing in developing a glass ceramic is
In general, crystallization phenomena to find a suitable nucleating agent for the
represent defects in glassy products. However, crystal phase. Frequently, oxides are melted
in the production of glass ceramics, one or together with the glass which show only
more crystalline phases are deliberately limited solubility in the corresponding glass. At
precipitated. Glass ceramics are polycrystalline a low temperature, many nanocrystals of this
solids produced by means of a controlled phase form initially. These nanocrystals then
crystallization of glass [3]. A typical characteristic constitute the substrate on which the actual
of glass ceramics is that the crystals do not crystals are grown. This process is called
grow sporadically, randomly or accidentally heterogeneous nucleation.
within the glass matrix. This would lead to
uncontrolled crystal growth and result in an
inhomogeneous structure with inferior
properties.
Melting temperature

Initially, a glass of suitable composition

is melted and moulded into a still glassy ingot Crystal growth
using the conventional moulding procedure.
For the subsequent two-stage temperature
Temperature

treatment, the temperatures are chosen in

such a way that first the temperature range of
maximum nucleation is passed and then that Nucleation
of maximum crystallization.

Fig 3: Dependence of nucleation and crystal growth on temperature

REPORT 9
 The fact that amorphous phase The best-known and most widely used
separation is of particular importance for the glass ceramics are those based on the Li2O-
nucleation process has been pointed out by Al2O3-SiO2 system, which possess high thermal
Vogel, for example [4]. According to him, shock resistance due to their low thermal
crystallization is initiated within the micro- expansion. They are used for eg hot plates,
drops and initiates bulk crystallization which furnace windows or telescope mirrors [5].
leads to the formation of crystallites of uniform
size.

2.3.2 Surface nucleation

Many crystal phases are difficult to 3 The materials of the
produce in a controlled way using bulk nuclea-
IPS e.max System
tion procedures. Even if nucleation-supporting
additives are used, the nucleation rate of The IPS e.max System offers dental
species such as leucite or anorthite is so low technicians unique freedom. With only one
that the nucleation process is uneconomical veneering ceramic, consistently aesthetic
because of the long processing times. In this results can be achieved on different frame-
specific case, crystal growth is initiated at the work materials. The dental technician is free to
surface, so that the use of mechanically milled choose between resistant lithium disilicate
powder particles eventually leads to the glass ceramics and high-strength zirconium
formation of a glass ceramic. In the process, oxide. While the oxide-ceramic zirconium oxide
particular attention is paid to generating can only be shaped using a milling procedure,
crystal nuclei on the surface of the powder. resistant glass ceramics can either be processed
using the well-known IPS Empress hot pressing
In some systems, it is advantageous to procedure or milling techniques.
densely sinter the glass powder first and then
increase the temperature to a level that
ensures the desired crystal growth – in par- 3.1 Requirements placed upon frame-
ticular if the crystal phase shows little sintering
work materials
activity. In other systems, the sintering and
crystal growth processes overlap, and in some The requirements are based on the
systems crystallization of the powder particles product profile and ISO 6872. Central issues
is initiated first, while the sintering process is are mechanical strength, chemical resistance
conducted subsequently. as well as aesthetic properties. These desired
characteristics are listed in Table 2.
2.3.3 Classification of glass ceramics
Glass ceramics can be classified
according to their chemical composition, for
example, or according to their field of applica-
tion. Beall suggests classifying commercial
silicate glass ceramics into three groups based
on the mainly crystallizing mineral phase [12]:
Table 2:
– Silicates such as lithium metasilicate, Requirements placed upon framework materials
lithium disilicate, enstatite (MgSiO3),
diopside (CaMgSi2O6) or wollastonite
Biaxial strength > 360 MPa
(CaSiO3).
– Aluminium silicates with the main phases Fracture toughness > 2,5 MPm0,5
cordierite, beta-quartz, beta-spodumene, Low chemical solubility
< 100 µg/cm2
beta-eucryptite and anorthite acc. to ISO 6872
– Fluorosilicates; these include fluor- Pressability in EP 500, EP 600
containing mica glass ceramics based on 900 °C – 940 °C
and selected competitor furnaces
fluor-phlogopite (K,Na Mg3AlSi3O10F2)
and tetra silicate mica (KMg2,5Si4O10F2), as Machinability in widely used Edge stability, tool wear,
well as fluor-containing chain silicates CAD/CAM units milling times
such as canasite and fluor-richterite. Coefficient of thermal expansion:
Compatibility with IPS e.max veneering 10.0–10.8 *10-6 K-1
ceramic, which can also be used
for ZrO2
Shading of the final product according
to aesthetic requirements

10
REPORT
 However, it should be kept in mind that
due the enlargement of the diameter, the press
pressure has been reduced by 15 %. This may
lead to longer pressing times, particularly in
conjunction with furnaces of other manu-
3.2 IPS e.max Press facturers. However, it would be wrong to
increase the temperature so that it exceeds the
In the production of IPS e.max Press prescribed temperature, as this could lead to
ingots, new process technology is employed. the formation of a thicker reaction layer in the
The ingots are no longer manufactured via a area of contact with the investment material.
powder stage as in the case of IPS Empress and In extreme cases, exposure to excessively high
IPS Empress 2, but by bulk casting. As a result, temperatures could even damage the structure
a product can be manufactured that is entirely of the glass ceramic which would lead to a
porefree. reduction in strength. If problems occur, the
calibration of the furnace should be checked
3.2.1 Ion colouring and opaquing first. Similarly, it should be checked whether
mechanism sufficient pressing force is applied.
This new production procedure does
not involve the addition of colour pigments, as For restorations with thinly tapered
these would melt at the melting temperature. margins, thick and short sprues should be used
The product thus shows less defects, which at as a lot of press force is lost in conjunction with
the same time enables higher strength and long sprues. This loss of force is proportional to
higher translucency to be produced than with the length of the sprue, while the diameter
conventional sintering technology. affects the pressing speed to the fourth power.
If required, the diameter of the sprue may be
The colour is achieved with polyvalent slightly reduced at the point of contact with
ions which are atomically dissolved in the the object to reduce the time required for
glass. The colour centres interact with each grinding. The following sketch illustrates how
other and with the glass matrix through redox sprueing influences the press behaviour (Fig 4).
processes. In this context, the right combina-
tion and concentration of the colouring ions is After careful divesting, investment
essential. Also, the melting conditions must be residue needs to be removed with IPS e.max
precisely defined. Press Invex Liquid - a procedure commonly
used in conjunction with lithium disilicate
The desired opacity of the medium- materials. The indicated time should be strictly
opacity ingots is adjusted by means of a phase observed, as compared to IPS Empress 2, the
separation process which occurs within the new product features an improved chemical
remaining glassy phase during slow cooling in resistance which also affects the treatment
the press mould. The same effect originally led with Invex Liquid. It is recommended to place
to a formation of strong, undesired opalescence the restorations in a small, suitable container
in translucent glass ceramics. and cover them with fresh liquid each time.
Subsequently, the solution can be neutralized
3.2.2 Processing as indicated and discarded.
Processing in the dental laboratory is
done using the well-known IPS Empress
technology. This is characterised by high Flow of a fluid in a pipe (Hagen Poiseuille)
precision of fit.
• dV/dt = π r4 Δρ / 8ηl
The new press ingots are offered in 3-g r = radius
and 6-g sizes. In contrast to the IPS Empress ρ = pressure (press force: - 15% in 6-g ingots)
and IPS Empress 2 ingots, which feature a η = dynamic viscosity
diameter of 11.8 mm, the diameter of the new
Sprues: Diameter Length Pressing speed
ingots has been enlarged to 12.8 mm.
2.0 mm 8.0 mm 1.00
Correspondingly, the press system, ring base 2.0 mm 6.0 mm 1.33
and press plunger have been enlarged to 13 mm. 2.5 mm 4.0 mm 4.88
3.0 mm 6.0 mm 6.75

Fig 4: Repercussions of the sprue dimensions on the pressing force, sprues with a diameter
of 2.0 mm and a length of 8.0 mm correspond to standard 1.00

REPORT 11
 solved and the lithium disilicate crystallizes. As
virtually no shrinkage occurs during this con-
version process, the fit of the restoration can
be previously adjusted. In the course of the
conversion process, the material acquires a
3.3 IPS e.max CAD high strength of more than 300 MPa and a
fracture toughness of 2.0–2.5 MPa m0.5. The
CAD/CAM techniques are increasingly blue shade of the metasilicate glass ceramic
employed in the fabrication of dental restora- disappears and the desired tooth shade is
tions. Systems such as CEREC 3, inLab, Kavo achieved. This colour change is attributable to
Everst and others are technically mature and a change in the coordination number of the
enable economical, high-quality restorative colouring ions (Fig 7).
results. The intention was to offer a machinable
high-strength glass ceramic in addition to the 3.3.4 Complex crystallization of
high-strength glass ceramic IPS e.max Press. IPS e.max CAD

3.3.1 The task The following section will provide more

details about the re-crystallization process and
In the development of a suitable glass- related solidification.
ceramic version for computer-aided manufac-
turing, one general problem had to be solved. The development is based on glass
The higher the strength a material demonstra- ceramic material created from a lithium di-
tes, the more difficult it is to machine it. The silicate system. In Table 3, the composition of
biaxial flexural strength of the new pressable the material is shown. SiO2 and Li2O represent
ceramic IPS e.max Press, which is manufactured the crystal-forming components, while P2O5 is
using bulk casting technology, is above added as a nucleating agent. The remaining
400 MPa, while its fracture toughness is oxides are used to control the properties of the
2.5–3.0 MPa m0.5. Tests have shown that this residual glassy phase. They serve to adjust the
material cannot be machined in most units. In shade and translucency. Figure 5 shows the
general, the first set of tools is already worn binary phase diagram for the SiO2-Li2O system.
after the first restoration has been milled. In Within the system, three stable binary oxides
addition, machining times are long, which ren- occur: lithium orthosilicate (Li4SiO4), lithium
ders the procedure uneconomical. The task metasilicate (Li2SiO3) and lithium disilicate
was to develop a material that would enable (Li2Si2O5). The two latter oxides play a role in
quick, easy and precise machining, while a the crystallization of IPS e.max CAD. When
short, subsequent tempering process would relating it to the binary system SiO2-Li2O, the
impart the material with the required high composition of the material is close to that of
strength [8-10].

3.3.2 The approach

Material system
The mechanical properties of a glass
ceramic material are closely linked to its micro-
structure. A low content of isolated, preferably lithium orthosilicate
plate-shaped crystals dispersed in the glassy
matrix represent predetermined fracture lithium metasilicate
points. Wear of the material occurs tangentially
to the force acting on it. Uncontrolled crack
propagation is halted by the crystals [11]. A
high fraction of needle-shaped, close-knit solid
crystals generally makes crack propagation lithium disilicate
difficult. A large amount of new surface area
has to be created - a process which consumes
considerable energy. Consequently, such
structures show a high fracture toughness.

3.3.3 The solution

By two-stage crystallization using a
controlled double nucleation process and a
special composition of glasses, lithium meta-
silicate crystals are precipitated in a first step.
The resulting glass ceramic demonstrates
excellent processing properties. In a second
step, the metasilicate phase is completely dis- Fig 5: Phase diagram Li2O – SiO2

12
REPORT
disilicate. However, it is well-known that in position of the base glass corresponds to
materials containing between 5 and 30 mol % that of lithium disilicate, all metasilicate
of Li2O, a miscibility gap occurs [cfr 6, p 75; 7, crystals are consumed in this process. The
p 76]. This means that when the melt is desired lithium disilicate glass ceramic
cooled, areas rich in Li2O and SiO2 form. This forms.
phase separation is a prerequisite for the
simultaneous nucleation of lithium metasilicate Expressed in the form of a chemical
and lithium disilicate. In conjunction with reaction, lithium disilicate is created from
certain compositions, it is possible to adjust the the glassy phase of lithium metasilicate and
duration and temperature of nucleation in SiO2: Li2SiO3 + SiO2 = Li2Si2O5.
such a way as to achieve a defined nucleation
density and a defined ratio of crystal nuclei. Expressed in terms of volume, a glass
The subsequent crystallization process ceramic material containing 60–70 % of
comprises two stages. During the first stage, disilicate crystal phase and 30–40 % of glass
lithium metasilicate crystallizes almost phase is created from a glass ceramic
exclusively, while the lithium disilicate crystal material containing 30–40 % of metasilicate
nuclei remain in the glassy matrix in a latent crystal phase and 60–70 % of glass phase.
state (Figs 6 and 7).

During the second crystallization stage,

the lithium disilicate nuclei finally grow into
crystals at higher temperatures. As the com-

Table 3:

Chemical composition of the IPS e.max CAD Ostwald ripening:

Temperature

Crystal size is a
glass ceramic in % mass Dissolution of
LS and growth function of
Crystal
of LS2 crystals temperature
growth of LS
Simultaneous
SiO2 57 – 80
nucleation of
Li2O 11 – 19 two crystal
species
K2O 0 – 13.5
ZnO 0–8 Processing

P2O5 0 – 11
ZrO2 0–8
Zeit
Additional components 0 – 12
Colouring oxides Fig 6: Crystallization pattern of IPS e.max CAD; the first temperature treatment is carried out industrially, while the
final crystallization takes place in the dental laboratory (LS = lithium metasilicate, LS2 = lithium disilicate)

Nuclei from various crystal species Isolated LS nuclei after the first Cross-linked LS2 crystals result in In the Ostwald ripening stage, a
develop independently crystallization stage enable simple, high fracture strength and further temperature increase
precise machining toughness produces crystal growth

Transparent glass block after Glass ceramic block after the first CAD/CAM-manufactured restoration Restoration after conversion into LS2
nucleation of LS and LS2 crystallization stage made of LS glass ceramic glass ceramic at 850 °C

Fig 7: Complex crystallization of IPS e.max CAD (LS = lithium metasilicate, LS2 = lithium disilicate)

REPORT 13
 3.3.5 Processing objects should only be sand-
The nucleation and initial crytallization blasted in case of absolute
process establishes the basis for the final lithium necessity. IPS e.max CAD does
disilicate glass ceramic product. Nevertheless, not need to be sandblasted
the temperature and crystallization regime prior to further processing,
must be strictly observed. Excessively high tem- layering or glazing. It is
peratures may lead to a plastic deformation of sufficient to clean the surface
the restoration. To counteract this, with eg a steam blaster. After
supporting paste or zirconium oxide spheres immersion in Invex Liquid,
are used. Rounded edges and severe vitrifica- restorations fabricated with
tion of the surface are an indication of too high IPS e.max Press should be
firing temperatures. If the firing times are too blasted with glass beads at
short or the furnace temperature is too low, maximum 2 bar pressure to
the shades may not be precisely matched. In completely remove the reac-
tion layer. To minimize the Fig 8: Etched IPS e.max CAD surface - a retentive pattern has
contrast, the firing parameters have hardly any been created by etching with hydrofluoric acid (IPS Ceramic
impact on the strength. impact of the abrasive medium, Etching Gel, Ivoclar Vivadent)
the surface should not be
The special Ivoclar Vivadent firing tray positioned vertically, but at an
made of SiN ceramics is capable of balancing angle. After sandblasting, the
the temperature profile due to its good thermal surface needs to be cleaned
conductivity and relatively high thermal mass, with steam again or in the
independent of the number of objects placed ultrasonic unit.
in the furnace. The use of this firing tray in
conjunction with a calibrated ceramic furnace After finishing, the
is both essential and sufficient to successfully restoration should not be
conduct the final crystallization of IPS e.max sandblasted (Figs 9 and 10).
CAD. The retentive surfaces required
for cementation or adhesive
3.3.6 Sandblasting luting are created by etching
with hydrofluoric acid (Fig 8).
A whole section will be dedicated to
Investigations have revealed
this issue, as very different views exist. Many Fig 9: IPS e.max CAD surface after sandblasting – deep damage
that hydrofluoric acid etching of the glass ceramic is noticeable
dental technicians are used to sandblasting
hardly affects the strength of
their work patterns to create clean and rough
glass-ceramics (Table 4). It is
surfaces for the subsequent working steps.
interesting to note that
(careful) grinding with high-
However, if glass and glass ceramic sur-
quality fine-grain diamond
faces are sandblasted, so-called median cracks
burs is even less critical than
are produced. These cracks are perpendicular
sandblasting. However, any
to the surface and weaken the restoration due
generation of heat during the
to the notch effect. In the case of glass, this
grinding procedure should be
leads to a tremendous reduction in strength,
strictly avoided.
but also glass ceramics can be weakened, even
though the resulting cracks are stopped by the
incorporated crystals. Therefore, glass ceramic

Fig 10: IPS e.max CAD surface after sandblasting and etching –
the damaged areas cannot be eliminated by etching - this is
reflected in the biaxial strength values (Table 4)

Table 4:

Biaxial strength of IPS e.max CAD after different surface treatments

Surface polished with Etched Sandblasted Sandblasted

SiC paper grade 1000 surface surface and etched surface

Biaxial strength [MPa] 554 +/- 78 520 +/- 98 232+/-18 235 +/-25

14
REPORT
3.3.7 Microstructure 3.4 Properties of framework materials
Figures 11 to 13 show SEM pictures of The properties and respective values
glass-ceramics in different processing stages. achieved by IPS e.max CAD and IPS e.max
Press are indicated in the table below. The
requirements stipulated in the product profile
as well as ISO 6872 could be met.

Table 5:

Properties of framework materials

IPS e.max CAD IPS e.max CAD IPS e.max Press

machinable crystallized

Biaxial strength [MPa] 100–160 300–420 400–480

Fracture toughness [ MPam0,5] 0.9–1.1 2.0–2.5 2.5–3.0

Elastic modulus [GPa] – 90–100 90–100

Fig 11: SEM picture of the glass ceramic after completion of the
first crystallization stage at 650 °C; approx 30 % of LS crystals in
Vickers hardness [MPa] 5300–5500 5700–5900 5700–5900
the residual glassy phase (crystals etched with HF)
Solubility acc to ISO 6872 [µg/cm2] – 30–50 30–50

Crystallization temperature / – 850 °C 920–925 °C

Press temperature

Manual processing with rotary with rotary with rotary

diamond diamond diamond
instruments instruments instruments

CTE 100–400 ° [10-6K-1] 9.75–10.55 9.75–10.55

CTE 100–500 °C [10-6K-1] 10.20–10.70 10.20–10.90

Thermal shock test > 160 °C > 160 °C

Shading of the final Blue-purple A–D and A–D and

product according to shade of shaded Chromascop Chromascop
aesthetic requirements versions shades in various shades in various
degrees of degrees of
translucency translucency
Fig 12: SEM picture of the glass ceramic after completion of the
second crystallization stage at 850 °C; approx 70 % of LS2
crystals in the residual glassy phase (glass phase etched with HF)

Fig 13: SEM picture of the glass ceramic pressed using the
IPS Empress technique at 920 °C; approx 70 % of LS2 crystals in
the residual glassy phase (glass phase etched with HF)

REPORT 15
 4. Literature

[1] Hennicke, H.W.; Zum Begriff Keramik und zur

Einteilung keramischer Werkstoffe. Ber. Dtsch. Keram.
Ges. 44 209-201(1967)

[2] Scholze H. Glas; Springer Verlag Berlin, 1988

[3] P. W. McMillan; Glass-Ceramics; Academic Press Inc.

London 1979

[4] W. Vogel; Glaschemie; Springer-Verlag Berlin 1992

[5] Hans Bach; Low Thermal Expansion Glass Ceramics;

Scott Series on Glass and Glass Ceramics, Springer
Verlag Berlin (1995)

[6] Wolfram Höland and George Beall; Glass-Ceramic

Technology; The Am. Ceram. Soc. Ohio (2002)

[7] Z. Strnad; Glass-Ceramic Materials, Glass Science and

Technology 8; Elsevier Amsterdam – Oxford – New
York – Tokyo (1986)

[8] H. Unuma, K. Miura, K. Kodaira; Improvement of

Mechanical Properties of Machinable Glass-Ceramics
through Postmachining Heat treatments; J. Am.
Ceram. Soc. 75 [8] 2300-2301 (1992)

[9] M. Reise; Untersuchungen zur Verfestigung und

Aushärtung maschinell bearbeitbarer Glaskeramiken;
Dissertation; Technische Universität Darmstadt (1999)

[10] H. Bürke; TEM-Grundlagenuntersuchungen zur

Gefügeentwicklung in aushärtbaren
Glimmerglaskeramiken; Dissertation, Universität
Würzburg (2004)

[11] D. G. Grossmann; The Formation of Chips in a

Machineable Glass Ceramic; Glass Technology Vol. 24
No. 1 11-13 (1983)

[12] G. H. Beall; Design and Properties of Glass-Ceramics;

Annu. Rev. Mater. Sci. 22 (1992) 91-119

16
REPORT
 Frank
IPS e.max ZirCAD Rothbrust

Zirconium oxide – ”White gold“

1 Introduction The characteristics of ZrO2 can best be

described on the basis of the mineral baddeleyite
Zirconium oxide has been used for (ZrO2). They are based on the mineralogical
more than 20 years as a high-performance structure and the different crystal lattices this
material in industries such as engineering, material can adopt. In nature, the monoclinic
sensor technology and medical engineering phase is found, which is present in a stable
due to its excellent properties. The reason why form at room temperature up to 1170 °C. If
it is used in a variety of application fields is due the temperature increases above this limit, the
to the crystal-chemical characteristics of tetragonal phase is formed and as of 2370 °C,
zirconium oxide. Based on these properties, the cubic modification takes place. When the
Garvie et al. has gone so far as to describe material cools down, the transformation is
zirconium oxide as “ceramic steel” [1]. In the reversible at slightly different temperatures
past few years, in which zirconium oxide has [2–6] (Fig 1).
been successfully employed in the dental field
as brackets, abutments, framework material It is particularly noteworthy that the
and implants, the term “white steel” has often volume increases by 3-5% during transforma-
appeared in publications. However, can the tion from the tetragonal modification into the
term be generally applied to all types of monoclinic phase, only because of the diffe-
zirconium oxide? And can IPS e.max ZirCAD be rences in density in both unit cells. The trans-
described as “ceramic steel”? formation takes place spontaneously in the
form of a martensitic transformation as is
known from steel (a-martensite) [2–6].

2 Mineralogical properties This specific characteristic of ZrO2 has

been used in technology to develop special
of ZrO2 materials with selectively controlled properties.
For this purpose, however, the mineral
Zirconium oxide is a chemical com-
baddeleyite could not be used. Instead,
pound of Zr4+ metal ions and the O2-oxide ion.
synthetic base materials had to be employed.
The result is an oxidic compound of an ionic
This synthetic ZrO2 is characterized by the fact
character, which – despite the Zr4+ metal ion –
that it contains stabilizers, such as Y2O3, CaO,
does not belong to metals but to the group of
MgO, CeO2, Sc2O3 etc. These doping agents
non-metallic inorganic substances. It is basically
fulfil different tasks depending on the added
wrong to talk about metal or steel in this con-
quantity [7–8]:
text because zirconium oxide is clearly an oxide
ceramic with a fine-grain, poly-crystalline 1. To avoid the transformation of the
structure. tetragonal phase into the monoclinic (t/m
transformation) up to room temperature
and to keep the tetragonal phase
metastable at room temperature.

1170°C 2370°C

950°C 2355°C
monoclinic (M) tetragonal (T) cubic (c)
p = 5.83 g cm-3 p = 6.10 g cm-3 p = 6.10 g cm-3

+ ΔV ~3–5%
martensitic transformation
Fig 1: Modification of zirconia at different temperatures

REPORT 17
 2. To shift the transformation of the tetrago-
nal phase to lower temperatures
3. To keep the cubic phase metastable up to
room temperature

Based on the example of the doping

additive Y2O3 one can see which phases are
maintained stable in which areas depending
on the added quantities [9, 10]. In the forma-
tion of a ceramic microstructure, the structural
conditions and the thermal process have to be
taken into account to enable the cubic or
tetragonal stabilization of the modification up
to room temperature (see Fig 2) [11, 12].

Fig 2: Phase diagram in the ZrO2-Y2O3 system according to Yashima et al. [9] 3 ZrO2 materials
In the course of the past 30 years, a
number of different high-performance
materials have been developed. Their func-
Fully Stabilized Partially
Zirconia (FSZ) Stabiliized tional, biocompatible and mechanical pro-
Zirconia I (PSZ) perties have been optimized over time [5, 7, 8].
Four of the main types of these materials are
shown below (Fig 3).

1. FSZ,CSZ: Fully Stabilized Zirconia

Tetragonal Partially 2. PSZ I: Partially Stabilized Zirconia I
Zirconia Stabilized 3. PSZ II: Partially Stabilized Zirconia II
Polycrystals TZP Zirconia II (PSZ)
4. TZP: Tetragonal Zirconia Polycrystals

The transformation-reinforced materials

PSZ I, PSZ II and TZP are particularly note-
worthy due to their mechanical properties. In
these materials, the above described t/m trans-
cubic c monoclinic m
formation was employed in such a manner
tetragonal t microcrack that the typical brittleness of ceramics was
reduced. A "pseudo-ductile" behaviour of the
FIg 3: Different types of microstructure for high-performance zirconium oxide ceramics
ceramic increases the fracture toughness in the
event of a fracture, similar to steel. Two rein-
forcement mechanisms can be distinguished
here [5, 7, 8]:

1. microcrack-induced transformation
reinforcement (MR)
2. stress-induced transformation
reinforcement (TR)
Frontal Zone Frontal Zone
Crack tip
The MR in PSZ I is produced when the
stabilization of the tetragonal particles in the
cubic matrix is not sufficient and the t/m trans-
Wake formation takes place. The resulting micro-
cracks can impair the propagation of cracks if
a macrocrack occurs in the structure, as the
energy is distributed among many small
tetragonal tetragonal
monoklin monoklin microcracks along the process zone. In PSZ II,
however, TR takes place: The tetragonal grains
Fig 4: Crack propagation and stress-induced transformation reinforcement within Y-TZP are not able to transform in the strained matrix
due to their crystallite size and the stabiliza-
tion. They remain metastable in the matrix. If a

18
REPORT
crack penetrates the structure, the tension in hydrothermal instability has
the matrix is released and the tetragonal become irrelevant for the appli-
particles can transform. Due to the ensuing cation [15]. IPS e.max ZirCAD
volume change, the crack cannot propagate. (Fig 5) has been doped with a
The fracture toughness of the material in- content of about 0.25 wt%
creases. Because of this “pseudo-plastic” Al2O3. The excellent mechanical
deformation, the material is also called properties are maintained
“ceramic steel” [1]. despite the additive. At the Fig 5 IPS e.max ZirCAD B40 and C15

same time, the ageing behaviour is improved

The following diagram (Fig 4) shows in such a way that there is no risk of strength
the transformation mechanism of Tetragonal loss after hydrothermal exposure.
Zirconia Polycrystals TZP. In this type of ZrO2
partially stabilized with 3 mol-% Y2O3, all
individual crystals in the structure are
maintained metastable up to room tempera-
ture to the tetragonal phase. However, the 4 ZrO2 in dental
crystallites exhibit the chemical driving power
to martensitically transform into the mono- applications – processing
clinic phase [5]. Given the surrounding matrix, strategies
the crystallites impair each others growth, ie a
microstructure that consists of virtually 100% Of all the different ZrO2 materials, 3Y-
tetragonal crystallites with a mean size of TZP has established itself for dental applica-
about 0.4 – 0.5 µm is the result. Clearly, the tions. The difference in the products is less
stress of the microstructure can be com- between the different material parameters of
pensated by the transformation of tetragonal the individual manufacturers than between
crystallites into the monoclinic phase at the the type of processing method used and the
edges of the crack, the "wake zone". Crack technology for fabricating a dental restoration
propagation is inhibited. The fracture toughness with a TZP framework. Basically, two different
is considerably increased. strategies are applied:

In addition to excellent mechanical 1. CAD/CAM processing of ZrO2 in a densely

properties, this material also exhibits bio- sintered state or
compatible and optically acceptable characte- 2. CAD/CAM processing of the ZrO2 white
ristics. Therefore, it is used in the dental industry body.
as a framework material in the anterior and
posterior region. Hence, it is possible to cover The major distinguishing features are shown in
the indication range of metal-ceramics with Table 1.
this material. In this context, the material can
be called "white steel". However, it has to be
noted that with regard to its hydrothermal
durability, the material features poorer pro-
perties than metals to some extent [13, 14]. 5 Properties, also compared
Various publications have shown that pure 3Y-
TZP is increasingly prone to t/m transformation to other dental ceramics
during ageing in a temperature range of Due to the above mentioned rein-
70–250 °C in moist surroundings. The result is forcing mechanisms, 3Y-TZP features improved
a loss of strength. A type of corrosion becomes mechanical properties compared to conven-
apparent, which is similar to that in metals. tional dental ceramics. Both the fracture
Consequently, ZrO2 also features metal-like strength and fracture toughness are signifi-
properties in this respect. cantly higher than in other dental ceramics as
is shown in the following diagram (Fig 6).
By adding further doping agents, such Therefore, the material can be used as a frame-
as Al2O3 or CeO2 in small quantities, these work material in the anterior and posterior
negative properties of 3Y-TZP have been region for single crowns as well as multi-unit
considerably improved. Consequently, the bridge frameworks. In addition, 3Y-TZP is bio-
compatible. Consequently, it can even be used
for orthopaedic applications. Moreover, the
white frameworks can be layered with, for
example, IPS e.max Ceram for the fabrication
of highly aesthetic restorations.

REPORT 19
 Table 1: 6 IPS e.max ZirCAD –
Comparison of the advantages and disadvantages of the individual the procedure
processing strategies for ZrO2 in dental applications
Below is a description of the process
steps for the manufacture of a dental restora-
Processing of white body Processing of HIP ZrO2 tion made of IPS e.max ZirCAD (Fig 7). Apart
Advantages Disadvantages Advantages Disadvantages from the fabrication itself, the further process-
ing by the user is highlighted in particular. The
Easy processing Detailed calculation Accuracy of fit, High processing dental technician is responsible for the com-
of shrinkage precise milling, no costs (tools and puter-aided design of the framework structure
required distortion machine)
and the veneer. He uses precise computer-
Short processing Risk of fracture in Excellent aesthetics, Complex reworking aided machining in a milling unit to create an
time, particularly white state high translucency procedure with accurately fitting framework.
with CAD/CAM effects on the
framework structure

No complex HIP No control of model Direct model fitting Long processing

technology fit after CAM times

Favourable price Low translucency Impeccable Stained base

structure material required

Post-staining Low strength High strength

M A N U FA C T U R E R

Raw material / Granulate

Dry pressing

Presintering
Fracture toughness, KIC / MPa1/2

Completion of IPS e.max

ZirCAD block

DENTAL TECHNICIAN

CAD/CAM process

Dense sintering

Strength, σ/MPa Layering technique

Fig 6: Comparison of mechanical properties of different dental ceramics Fig 7: Process diagram for fabricating an IPS e.max ZirCAD
restoration

20
REPORT
 The procedure for processing the white After shaping, the material is finally
body shows the following characteristics: A densified in a high-temperature furnace
block, which has not yet attained its final (Fig 9), which has been especially developed
properties, such as strength, fracture toughness, for oxide ceramics. The process of final
density etc, but is predensified, is machined. In hardening in which the individual crystallites
this presintered state, the block can very easily move closer together by diffusion processes
be machined with suitable grinding instru- due to thermal activation until virtually no
ments. Only after shaping (CAM process) is the pores are left in the structure is called sintering.
block finally densified. Densification means This process takes place at 1500 °C. What is
that the material shrinks by a certain degree. important in this process is that both heating
This shrinkage has to be taken into account in and cooling rates are exactly coordinated with
the CAD/CAM process. Therefore, an enlarged the actual sintering procedure. Consequently,
framework is milled from the block. The more the thermal process of the equipment has to
detailed the degree of shrinkage in a block is be accurately adjusted to the processes in the
determined, the more precise is the accuracy material. Hence, the entire firing process in the
of fit after final hardening of the framework in Sintramat furnace takes about 8 hours. The
the firing procedure. material shrinks in every direction by about
20% in relation to the original size.

6.1 Material properties The following table (Table 2) shows a

summary of the most important material
Below is a description of the most properties of IPS e.max ZirCAD in a presintered
important phases that IPS e.max runs through state.
in the manufacturing process on the basis of
the material properties. 6.1.2 IPS e.max ZirCAD block – sintered
to full density
6.1.1 IPS e.max ZirCAD block –
In the following image (Fig 10) a three-
presintered
unit bridge and a crown coping are shown
The base material of IPS e.max ZirCAD before and after firing in the sintering furnace.
is a block in a presintered state, i.e. the The densification process changes the colour
material has not been finally densified yet but of the framework and endows it with a slight
the individual crystallites - which later form the translucency compared to the original material.
dense structure - are only connected to each The fully densified structure shows how the
other by sinter necks. The result is a loose, individual tetragonal crystallites are sintered to
porous structure with 50-% densification a dense compound and form a homogeneous
(Fig 8). The strength of the material has been microstructure (Fig 11). The grain boundaries
optimized in such a way that machining is still can only be made visible by etching, in this
easy to conduct on the one hand, while on the case with thermal etching at 1420 °C. Residual
other hand, the block does not break in the porosity is very low. Thus, the number of errors
CAD/CAM process. However, careful handling in the structure is minimized. The material is
is required for the finishing process. densified to more than 99% of the theoretical

Fig 8: SEM image of a fracture surface of an IPS e.max ZirCAD Fig 9: High-temperature furnace Sintramat from Ivoclar Vivadent
block, 30,000x magnification AG for firing IPS e.max ZirCAD

REPORT 21
 Table 2: density. The combination of high densification,
low error rate in the structure and the small,
Properties of IPS e.max ZirCAD mean crystallite size of approx. 0.5 µm results
in
- the presintered state with chemical composition in the high fracture strength of the material. In
addition, the above mentioned possibility of
Density /g cm-3 3.09 – 3.21 transforming the tetragonal particles leads to
Porosity /% 47.3 – 49.3 a reinforcing mechanism and thus to a fracture
toughness of more than 5.5 MPa m1/2. Other
Strength of presintered body /MPa 50 – 90 properties are summarized in Table 3.
Crystallite size /µm 0.25 – 0.35
ZrO2 /wt.% 87.0 – 95.0
Y2O3 /wt.% 4.0-6.0 6.2 Sources of error: reasons and
HfO2 /wt.% 1.0 – 5.0 effects

Al2O3 /wt.% 0.1-1.0 Some rules have to be observed in the

fabrication of high-quality IPS e.max ZirCAD
restorations.
Table 3:
As already described above, the firing
Material properties of IPS e.max ZirCAD process is decisive for the result. It is important
after the firing process in the densely sintered state that parameters, such as strength, density etc.
are controlled by the temperature-time regime.
Density /g/cm-3 >6.0 Furthermore, the thermal process in the furnace
Porosity /% <0.5 also has a considerable effect on the accuracy
of fit. Consequently, a component with a com-
Flexural strength [ISO 6872] /MPa >900 plex geometry, as is the case with a dental fra-
Fracture toughness /MPa m1/2 5.5 mework, can distort during the shrinkage pro-
Hardness HV10 /MPA 13000 cess. This deformation has to be controlled in
such a way that neither distortion nor
Thermal expansion α (100–400°C) /10-6 K-1 10.75
torque takes place. Therefore, the framework
Thermal expansion α (100–500°C) /10-6 K-1 10.80 should have free possibility of movement
Mineralogical phase – tetragonal during the firing procedure so that it can move
Crystallite size /µm 0.50–0.65 equally into all directions. For this purpose,
ZrO2 beads are used (Fig 13). The beads
provide an even support for the framework
and allow it to move freely during the sintering
process (Fig 12). It is only in this way that the
ZrO2 framework sintered to full density acquires
its excellent accuracy of fit (Fig 14).

6.2.1 Surface finishing

CAM processing with diamond tools
produces a surface structure on the ZrO2 frame-
work, which is also maintained after the
sintering process. The image of the surface
Fig 10: Comparison of IPS e.max ZirCAD Fig 11: SEM image of the IPS e.max ZirCAD after milling and sintering shows even milling
frameworks before and after the firing process microstructure sintered to full density (thermally
etched at 1420 °C, 20 min)
traces that are produced by finishing the

Fig 12: 3-unit bridge framework on IPS e.max Fig 13: Firing aid for the sintering process: Sintramat Fig 14: Accuracy of fit of a 3-unit bridge framework after the
ZirCAD on ZrO2 beads after the sintering process ZrO2 beads firing process on the model

22
REPORT
surface with diamond tools. Although one
a)
might assume that this surface roughness
implies great defective areas or even cracks,
the magnification (Fig 15) clearly shows that
no sharp-edged scrapes are visible within the
milling pattern.

In contrast, the surface is severely

stressed if it is sandblasted with aluminium
oxide particles (Fig 16), producing precipitous
structures up to deep cracks (Fig 17). The
sharp-edged cracks and defects have a
disastrous effect on the fracture behaviour in
brittle ceramics and thus reduce the strength
of a material.
b)

Garvie et al. [1] and Kosmac̆ et al. [16],

however, have been reporting for some time
that sandblasting does not have a negative
effect on the strength of TZP materials. To the
contrary, they argue that the strength is even
increased. This reinforcement is achieved due
to the phase transformation in the surface
from the tetragonal to the monoclinic phase,
whereby a superficial compressive stress
strengthens the ceramic [16]. The XRD pattern
(Fig 18) shows the superficial t/m transforma-
tion. Moreover, examinations have proven that
apart from the phase transformation Al2O3 Fig 15: Surface of the ZrO2 framework milled in a CAD/CAM
particles penetrate into the surface. process a) with 200x and b) 5000x magnification, both in a
sintered state

What has to be noted here is that a

reinforcement by sandblasting is only possible
for the framework. Reinforcing the entire
restoration with veneering material is not
possible. To the contrary, sandblasting the
surface prior to veneering weakens the entire
framework. The framework ceramic must not
be sandblasted before layering, since the bond
between the framework ceramics and layering
ceramics is weakened. In principle, only the
recommended tools must be used for finishing
after the sintering process.

Fig 16: Aluminium oxide particles 100 µm for sandblasting

Fig 17: Surface sandblasted with 100-µm aluminium oxide

particles at 4 bar

REPORT 23
 6.2.2 Influence of thermal treatment
The thermal process is decisive for the
formation of the microstructure and thus the
properties of the material. If the firing process
is not accurately controlled, undesirable firing
results will be the outcome, which often
cannot be visually differentiated. The difference
only becomes apparent upon inspection of the
microstructure and the comprehensive
characterization regarding the dental applica-
tion. Grain growth processes and the forma-
tion of different phases are often not visible to
the user.

6.3 Applications / indications of

IPS e.max ZirCAD
Due to the excellent mechanical
properties, IPS e.max ZirCAD is ideal for
multiple-unit bridge frameworks. In combina-
tion with the IPS e.max Ceram layering
ceramic, highly aesthetic dental restorations IPS e.max ZirCAD, sintered, sandblasted with 100-µm Alox, 3 bar
with a lifelike appearance can be fabricated IPS e.max ZirCAD, sintered
(Fig 19). Apart from the conventional design of t – tetragonal
a bridge framework, inlay-retained bridges can m – monoclinic

be fabricated with the 3Y-TZP material.

Fig 18: XRD patterns of the surface of finished IPS e.max ZirCAD samples: the monoclinic phase in the surface
becomes detectable after sandblasting
Although there are no high demands
on the material regarding mechanical
properties for crown copings, particularly in
the anterior region, zirconium oxide exhibits a
big advantage over conventional materials in
certain situations. Given the high opacity
compared to glass-ceramics, severely dis-
coloured and dark preparations can be
covered with zirconium oxide. Hence, the
shade of the restoration can be matched to the
surrounding teeth. Consequently, the influence
of the dark preparation can be compensated.

6.3.1 Press-on technique in conjunction

with frameworks
In addition to layering the IPS e.max
ZirCAD framework with the IPS e.max Ceram
veneering material, IPS e.max ZirPress can be
used to press onto the framework. The press-
on technique unites the advantages of the
Fig 19: Three-unit IPS e.max ZirCAD bridge veneered with IPS e.max Ceram
CAD/CAM and press techniques. Layering a
ceramic shoulder can be facilitated by pressing
a suitable material on a reduced framework. A
time-consuming and technically complex
layering process is no longer required with the
press-on technique. At the same time, highly
aesthetic results can be achieved. The different
materials, such as framework, layering and
pressed ceramic are compatible at all times
(see article on IPS e.max ZirPress).

24
REPORT
7 Literature

[1] Garvie R.C., Hannink R.H., Pascoe R.T.; Ceramic

Steel?, Nature (London); 258, 703-704 (1975)

[2] Subbarao E.C., Mati H.S., Srivastava K.K.; Phase

Transformation in Zirconia; Phys. Status Solidi A 21
[1], 9-40 (1974)

[3] Wolten G.M.; Diffusionless Phase Transformations in

Zirconia and Hafnia; J. Am. Ceram. Soc., 46 [9],
418–422 (1963)

[4] Bansal G.K., Heuer A.H.; On a Martensitic Phase

Transformation in Zirconia (ZrO2): I, Metallographic
Evidence; Acta Metall. 20 [11], 1281-1289 (1972); II,
Crystallograpghic Aspects, Acta Metall., 22 [4],
409–417 (1974)

[5] Heuer A.H., Claussen N., Kriven W.H. and Rühle R.;
Stability of Tetragonal ZrO2-Particles in Ceramic
Matrices; J. Am. Ceram. Soc. 65, 642-650 (1982)

[6] Deville S., Guénin G., Chevalier J.; Martensitic

transformation in zirconia Part I. Nanometer scale
predicition and measurement of transformation
induced relief.; Acta Materialica 52, 5697–5707
(2004)

[7] Lange F.F.; Transformation Toughening; J. Mat. Sci,

17, 247–254 (1982)

[8] Lange F.F.; Transformation-Toughened ZrO2:

Correlations between Grain Size Control and
Composition in the System ZrO2-Y2O3; J. Am.
Ceram. Soc. 69 [3], 240-242 (1986)

[9] Yashima M., Kakihana M., Yoshimura M.; Metastable-

Stable Phase Diagrams in the Zirconia-Containing
Systems Utilized in Solid-Oxide Fuel Cell Application;
Solid States Ionics; 86–88 [2], 1131–1149 (1996)

[10] Scott, H.G.; Phase relationships in the zirconia-yttria

system; J. Mat. Sci. 10, 1527–1535 (1975)

[11] Becher P.F., Swain M.V.; Grain-Size-Dependent

Transformation Behavior in Polycrystalline Tetragonal
Zirconia; J. Am. Ceram. Soc., 75 [3], 493–502 (1992)

[12] Ruiz L, Readey M.J.; Effect of Heat Treatment on

Grain Size, Phase Assemblage, and Mechanical
Properties of 3 mol% Y-TZP; J. Am. Ceram. Soc., 79
[9], 2331–2340 (1996)

[13] Lange F.F., Dunlop G.L., Davis B.I.; Degradation During

Aging of Transformation-Toughened ZrO2-Y2O3
Materials at 250°C; J. Am. Ceram. Soc. 69, 237–240
(1986)

[14] Tsugio Sato, Masahiko Shimada; Transformation of

Yttria-Doped Tetragonal ZrO2-Polycrystals by
Annealing in Water; J. Am. Ceram. Soc. 68 [6],
356–359 (1985)

[15] Tsugio Sato, Shiro Ohtaki, Tadashi Endo, Masahiko

Shimada; Improvement of Thermal Stability of Yttria-
Doped Tetragonal Zirconia Polycrystals by Alloying
with Various Oxides; Int. J. High Technology Ceramics
2, 167–177 (1986)

[16] Kosmac̆ T., Oblak C., Jevnikar P., Funduk N., Marion L.;
The effect of surface grinding and sandblasting on
flexural strength and reliability of Y-TZP zirconia
ceramic; Dental Materials 15, 426–433 (1999)

[17] Schweiger M.; Zirkoniumoxid – Hochfeste und

bruchzähe Strukturkeramik; Ästhetische Zahnmedizin
5, 248–257 (2004)

REPORT 25
 IPS e.max Ceram Marcel Schweiger

The universal veneering ceramic – One for 4

1 Introduction any leucite crystals because of its composition.

The components of the mixture include glasses
In the development of the IPS e.max from the SiO2-Li2O-Na2O-K2O-ZnO-Al2O3 multi-
Ceram veneering ceramic, the main emphasis component system. The base glasses of fluor-
was placed on characteristics such as aesthetics apatite glass ceramics additionally contain
and universal application. In regard to aesthetics, CaO, P2O5 and F components. These three
excellent results had previously been achieved basic components are a pre-requisite for fluor-
in conjunction with veneering materials such apatite crystal formation Ca5(PO4)3F. Silicate
as IPS d.SIGN and IPS Eris for E2 [1–3] using glasses are homogeneously melted in special
fluorapatite glass ceramics as opaquing agents glass melting furnaces at temperatures bet-
– a successful strategy that has been continued ween 1300 and 1500 °C and subsequently
in IPS e.max Ceram. converted into the final IPS e.max Ceram
product through controlled and reproducible
IPS e.max Ceram is truly universal tempering, milling and mixing procedures.
because it is compatible with the IPS e.max Except for the Glazes, Shades and Essence
framework materials ZirCAD (zirconium oxide materials, all IPS e.max Ceram products con-
ceramics), CAD and Press (lithium disilicate tain varying concentrations of fluorapatite
glass ceramics) as well as the pressable dentin crystals. Table 1 shows the composition of the
component ZirPress (fluorapatite glass main products.
ceramics). Optimal adjustment of the thermal
expansion and firing temperature was an The main component in all product
essential pre-requisite to meeting these groups is SiO2 with a content of more than
demands. 50 %wt. The sintering behaviour and wetting
of the framework surface during ceramic firing
in the dental laboratory is influenced by
additives such as Li2O, B2O3 and F. Al2O3 and
ZrO2 improve the chemical resistance, tempe-
2 Composition rature stability and mechanical strength of the
ceramic material. The alkali metal oxides K2O
IPS e.max Ceram is composed of silicate and Na2O are extremely important when it
glasses and fluorapatite glass ceramics. The comes to adjusting the thermal expansion
only natural ingredient used in the fabrication coefficient and the processing temperature.
of silicate glasses is quartz sand. No feldspar Depending on the SiO2 and Al2O3 content, the
components are required to manufacture amount of alkali metal oxide must be modi-
IPS e.max Ceram. Additionally, it cannot form fied. CaO, P2O5 and F are mandatory in order

Table 1:

Chemical composition of the different IPS e.max Ceram products (in %wt)

Layering materials Add-On ZirLiner Shade, Essence, Glaze

SiO2 60.0-65.0 61.0-68.0 50.0-60.0 61.0-68.0
Li2O 1.0-2.0 1.0-2.5 --- 1.0-2.5
Na2O 6.0-9.0 5.0-8.0 6.0-11.0 5.0-8.0
K2O 6.0-8.0 5.0-8.0 4.0-8.0 5.0-8.0
CaO 1.0-3.0 1.0-3.0 1.5-4.0 1.0-3.0
ZnO 2.0-3.0 2.0-4.0 --- 2.0-4.0
Al2O3 8.0-12.0 5.0-8.0 16.0-22.0 5.0-8.0
ZrO2 1.0-1.5 0.5-1.5 1.5-3.0 0.5-1.5
P2O5 0.1-1.0 --- 0.8-2.0 ---
F 1.0-2.0 1.0-2.0 0.2-1.5 1.0-2.0
Additional components: SrO, B2O3, ZrO2, TiO2

26
REPORT
to precipitate the fluorapatite. Thus indirectly, By using different concentrations of
the content of apatite-forming components CaO, P2O5 and F and by varying the crystalliza-
has an impact on the opacity and aesthetics of tion temperature and time, different shapes of
the material. fluorapatite crystals can be produced in a
targeted fashion. These processes are con-
The milling technique used when ducted in a controlled, reproducible way during
processing glass granulates into glass powder production. The quantity and shape of the
plays a decisive role. By means of the grain size crystals will not change any more during the
distribution and final grain size of the powder, ceramic firing procedure in the dental labora-
the handling properties can be selectively tory, which is conducted at 750 °C. This is
adjusted. While the Dentin and Incisal ensured by the fact that during the production
materials feature a coarse grain structure with procedure, a crystallization temperature
average particles sizes ranging from 30 to between 850 °C and 1150 °C is maintained
36 µm, very fine powders with average particle during a tempering period of more than one
sizes of 5 to 10 µm are used for the Essence hour. All subsequent firing cycles in the dental
materials and Glazes. Stained Essence laboratory are conducted at processing para-
materials can be admixed, just like colour meters that are clearly below these tempe-
pigments, in order to individually and homo- ratures. Consequently, no crystal growth can
geneously enhance the chroma of the existing ensue. In the case of IPS e.max Ceram, nano-
coarse-grain materials. scale as well as oblong fluorapatite crystals are
present. The long prismatic crystals have a
length of 1–2 µm and a cross-sectional dia-
meter of less than 200 nm. With less than
200 nm, the nano-scale crystals are very short in
3 Microstructure length. Their cross-sectional diameter is less
than 100 nm. For sizes below 100 nm, the term
IPS e.max Ceram is a homogeneous “nano” is justified. Evidence of the crystalline
mixture of fluorapatite-containing glass content can be provided by means of XRD. In
ceramic and sintered glass powders. The Figure 3, the X-ray diffraction diagram of a
sintered glasses are single-phase glasses and fluorapatite glass ceramic from the IPS e.max
do not contain any crystalline phases. As a Ceram range is shown and contrasted with a
result, these glasses remain completely stable reference pattern from pure fluorapatite.
during the ceramic firing process and do not
form any crystals. The glass ceramics contain Apart from the fact that the structure
fluorapatite crystals Ca5(PO4)3F. Evidence of of fluorapatite crystals is very similar to that
crystalline phases is provided by means of X- of natural tooth enamel, the crystals are
ray diffraction (XRD) and scanning electron systematically employed to adjust the optical
microscopy (SEM). Figures 1 and 2 show the properties of the different materials. More
fluorapatite crystal shapes that typically occur details on this subject can be found in chapter 4.
in IPS e.max Ceram.

Fluorapatite forms
long prismatic crystals with a
hexagonal base. Longitudinal
cuts show an oblong rec-
tangular surface and lateral
cuts the corresponding hexa-
gonal surfaces. The crystalline
symmetry is thus hexagonal.
The main components are
PO43+ tetrahedrons laterally
cross-linked with Ca2+ ions. F-
ions are embedded in the
intermediate spaces. Fluor-
apatite has a refractive index
ranging from 1.629 to 1.667. Fig 1: Longish fluorapatite crystals (etched; 3 % HF, 10 s) Fig 2: Nano-fluorapatite crystals (etched; 3 % HF, 10 s)

REPORT 27
 4 Properties
4.1 Optical properties
Fluorapatite crystals have a significant
impact on the light dynamics of IPS e.max
Ceram. The light is mainly refracted along the
crystals. In this refraction process, the light
wave range, particle size (cross-sectional dia-
meter) as well as the refractive index of the
filler particles and matrix play a crucial role. In
IPS e.max Ceram, the opacity is established
with the help of fluorapatite crystals which are
embedded in the glass matrix as particles. The
refractive index of the crystals (particles) is
between 1.63 and 1.67, which is higher than
that of the glass matrix which features 1.50 to
1.55. In contrast to conventional opaquing
techniques using ceramic particles such as
ZrO2 (refractive index 2.1 to 2.2) or TiO2
(refractive index 2.5 to 2.6), the differences
between the refractive index of the particles
and that of the matrix is significantly smaller in
IPS e.max Ceram. Consequently, light
PU PZ-GM/Neptun EB-1000 b:E37518, Art:549239 - File: E37518-1.RAW - Type: PSD fast-scan - Start: 10.000 ° - End: 60.158 ° - Step: 0.014 ° - Step time: 1. s - Temp.: 25 °C (Room) - Time Started scattering conditions which are ideal for
Operations: Background 0.120,1.000 | Import
00-015-0876 (*) - Fluorapatite, syn - Ca5(PO4)3F - Y: 107.87 % - d x by: 1. - WL: 1.54056 - Hexagonal - a 9.36840 - b 9.36840 - c 6.88410 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - dental applications are created. Optical pro-
perties such as translucency and brightness
Fig 3: X-ray diffractogram of a fluorapatite glass ceramic which is used in IPS e.max Ceram
can be ideally adjusted. If the difference
between the two refractive indices is too high,
for example, high brightness may be achieved,
but hardly any translucent properties can be
created because of the strong scattering
effect.

Opalescent properties are also caused

by light scattering. The short-wave (blue) por-
tion of the incident light is scattered and
reflected by the small crystals and phase
separation areas whose size is in the range of
100 to 500 nm. The long-wave (reddish) por-
tion of the light is not affected by these small
particles and may pass practically unhindered.
In incident light, the material appears bluish, in
transmitted light reddish-orange. This creates
the typical opalescent effect which imparts a
natural aesthetic appearance to restorations
veneered with IPS e.max Ceram in the incisal
region (Fig 4).

In addition, phase separation effects,

which play a crucial role in the production of
glass ceramics, are selectively employed in the
Fig 4: Schematic illustration of the opalescence effect: Transmission of long-wave light and scattering of the short-wave
light
Effect materials, apart from the nano-scale
fluorapatite crystals. Phase separation processes
can be controlled and reproduced just like
crystallization processes. In the case of IPS e.max
Ceram, these are conducted at temperatures
between 900 and 1150 °C. As a result, the
particle size remains completely stable during
the ceramic firing cycles conducted at 750 °C in

28
REPORT
the dental laboratory. The opalescent effect is (ISO 6872) of >50 MPa. The fluorapatite
thus maintained even during multiple firings. crystals do not measurably strengthen the
The drop-shaped phase separation areas have a glass ceramic as, for example, leucite and
diameter of approx 300 nm (Fig 5). lithium disilicate crystals do. The precipitation
Consequently, the basic requirements for wave- density is too low and the difference in the
length related light scattering and thus thermal expansion coefficient compared to the
opalescent effects are met. glass matrix is too small to reinforce dispersion.
It should be pointed out that all the currently
available veneering ceramics for ZrO2 frame-
works exhibit similar strength values of bet-
ween 70 and 100 MPa (measurements Ivoclar
Vivadent AG, 2003–2005). Table 2 shows a
comparison of the biaxial strength value of
different veneering ceramics for ZrO2 frame-
works.

Thus it should be kept in mind that the

firing temperatures which are used in the
fabrication of test specimens are higher than
those indicated by the manufacturer because
the test specimens lie flat on the firing tray and
are therefore not evenly exposed to the heat
Fig 5: Drop-phase in the nano-scale range and fluorapatite radiation of the furnace on all surfaces. In
crystals to achieve a natural opalescent effect (etched with 3 %
HF; 10 s) order to compensate for this difference in
energy compared to a centrally positioned
tooth restoration, the firing temperature
needs to be increased. It can be easily judged
4.2 Mechanical properties from the firing result whether the specimens
In clinical use, veneering ceramics are are completely fired. Only completely fired test
exposed to high chemical, thermal and specimens provide representative strength
mechanical stress. The individual types of values. All the measured veneering ceramics
stress overlap and may even be mutually re- comply with the minimum value of 50 MPa.
inforcing. The initial measurable strength of a Due to the high glass content, no significantly
material cannot be considered a characteristic higher strength values have been attained in
value, as the preparation technique and conjunction with leucite-free veneering
homogeneity of the manufacturing process ceramics to date. The ceramic veneer still
greatly influence the data obtained. Glasses represents the weakest part of all-ceramic
and ceramics are brittle-rigid materials to restorations. Therefore, the framework
which the principles of linear-elastic fracture dimensions should be maximized. This applies
mechanics apply. They do not undergo any to the posterior region in particular, as function
plastic deformation until failure occurs and should be given priority over aesthetics in this
thus demonstrate purely elastic behaviour. In area. A cusp-supporting design of the frame-
brittle-rigid materials, common fracture points work can further improve the mechanical
are material defects such as porosities, entrap- reliability of the restoration.
ments or voids at the surface. SiO2 fibres with
perfect surface and homogeneous volume
may reach tensile strength values between
12,000 and 16,000 MPa under vacuum. A
prepared sample rod made of the same glass,
however, achieves only 45 MPa. If the surface
Table 2:
of such a rod is sandblasted, tensile strength
values drop to a mere 14 MPa [4]. The larger Biaxial strength values (acc. to ISO 6872) of different ZrO2
the material defect, the higher the intensity of veneering ceramics (Ivoclar Vivadent AG measurements,
the tension under similar stress or tension. 2003 – 2005)
Thus minimizing the number and size of defec-
tive areas is an essential objective in the fabri- IPS e.max Ceram 90 ± 10MPa
cation of component parts with brittle-rigid
ZrO2-Keramik A (Nobel Zr) 102 ± 18 MPa
materials. IPS e.max Ceram achieves biaxial
strength values of between 80 and 100 MPa ZrO2-Keramik B (Cercon S) 84 ± 13 MPa
and thus easily fulfils the standard requirement ZrO2-Keramik C (Vita VM9) 97 ± 8MPa

REPORT 29
 4.3 Thermal properties In the case of IPS e.max ZirCAD, the maximum
tensile stress calculated is 15 MPa, and in the
The linear coefficient of thermal expan-
case of the glass ceramics IPS e.max CAD and
sion (CTE) of both the framework and
Press, the maximum value is 7 MPa. These
veneering material need to be compatibilized
figures are clearly below the inherent strength
with each other. The CTE indicates the expan-
values of the framework materials and thus do
sion or contraction a rod of 1 m length under-
not present a problem. However, the fact that
goes if the temperature is changed by
this theoretical calculation is based on the
1 °C or 1 K (Kelvin). The change in absolute
assumption of a homogeneous cooling
length is indicated in µm (=0.000001 m).
process should be kept in mind. Quick cooling
Therefore, the unit of measurement is
and varying thickness of the restoration may
µm/m*K. The measuring unit may also be
lead to an increase in tensile stress and even
abbreviated to ppm/K. However, the letters
transfer critical tensile stresses to the
ppm stand for “parts per million” and
veneering ceramic.
correspond to 0.0001%. The CTE thus indi-
cates the change in relative length of a
When comparing CTE values, it is
material per K. To illustrate this relationship, a
important that the values relate to identical
calculation example is shown below. The
temperature intervals. The indicated or
change in absolute length Dl of an IPS e.max
calculated CTE value is dependent on the
ZirCAD bridge with a length of 30 mm (Lo) is
temperature. As the transformation
to be determined within the temperature
temperature of IPS e.max Ceram is in the
range DT of 25 to 400 °C (CTE ZirCAD a =
range of 470–490 °C, the CTE value cannot be
10.75 µm/m*K).
analysed up to 500 °C. The transformation
point represents a characteristic point in the
Dl = a • DT • L0 • 0.000001
transition between the glassy solid state and
Dl = 10.75 • (400–25) K•30mm•0.000001/K
the glass melt. The linear expansion changes at
= 0.121mm=121µm
the transformation temperature. In the
analysis, the upper temperature limit is thus set
The change in absolute length Dl of an
at 400 °C in order to ensure a stable linear
IPS e.max ZirCAD bridge with a length of
expansion range. Correspondingly, the CTE
30 mm in the range of 25 to 400 °C is 121 µm.
values for framework ceramics are indicated in
the temperature range between 100 and 400
As a rule of thumb, the veneering
°C, even though it would be perfectly possible
ceramics used for dental restorations tend to
to evaluate the CTE values of these materials
establish a stable bond to the framework if
up to a temperature of 500 °C.
their CTE is lower than that of the framework
material. The mechanically weaker surface of
the veneering ceramic is thus exposed to
compressive strain. Glasses and ceramics can
resist compressive forces much more easily
than tensile forces. This principle is applied in
both metal and all-ceramics.

Due to the carefully selected CTE of

IPS e.max Ceram, the material is compatible
with IPS e.max CAD, Press and ZirCAD. Figure 6
shows the CTE values of the IPS e.max
materials.

No matter which combination of system

components is chosen, the CTE of IPS e.max
Ceram is always below that of the framework
ceramic. As a result, the mechanically weaker
veneering ceramic is exposed to compressive
stress while the surface of the stronger frame-
work ceramic is exposed to tensile stress. The
two-layer model allows the theoretically
occurring surface tension to be calculated [5]. Fig 6: Gradation of CTE values within the IPS e.max System (Ivoclar Vivadent 2005

30
REPORT
5 Sintering process In order to illustrate the sintering
process, a firing cycle conducted in a
IPS e.max Ceram is a low fusing glass Programat P200 was interrupted at the
ceramic. The sintering point of the mixture is temperature stages of 600, 650, 700 and
below 800 °C. Sintering is a dynamic process. 750 °C to enable SEM analysis of the sinter
The most important factors that influence this structure. The progress of the sintering process
process are grain size distribution, the specific is shown in Figs 6 to 9.
surface texture, surface conditioning of the
powder, densification of the powder, heating At 600 °C, the individual glass and glass
rate, final temperature and holding time. ceramic grains can still be easily distinguished.
IPS e.max Ceram is a glass ceramic material Thermal microscopy shows that the sintering
with a high content of glassy phase. Glassy process starts at 550 °C. First sinter necks form
materials demonstrate a characteristic trans- at the direct contact points between individual
formation as well as subsequent softening grains. The sinter structure exhibits low
range. In the softening range, the viscosity is strength at this stage. In the temperature range
108–1013.5 Pas. At the points of contact, first between 600 and 650 °C, strong sintering
melting bridges form between the individual activity is observed (Fig 8). At 650 °C, the
powder particles. Further densification is sinter shrinkage is around 19.3 %
achieved by liquid-phase sintering [6, 7]. By (corresponds to a linear shrinkage of 6.9%).
selective melting of the IPS e.max Ceram glass The individual grains are connected with each
grains, which is accomplished as from the other through pronounced sinter necks. These
softening point of 540 °C, the open pores are sinter necks form through localized melting of
continuously closed as the temperature the grains. Large grains and components with
increases. higher melting temperatures impart the
material with the required resistance against
The sintering behaviour can be charac- deformation. Up to 650 °C, the material has
terized by means of thermal microscopy. In the an open-pored structure. Volatile organic
process, a cylindrical powder specimen is substances need to be disintegrated and
heated at a constant rate and the sintering decomposed when this temperature is
shrinkage is recorded digitally by means of reached. If this is not so, isolated sinter pores
shadow projection. The volumetric shrinkage in the structure remain which are filled with
of the standardized, non-densified test undesirable reaction products. Therefore, it is
specimens is 45.4 %. Provided that the of utmost importance to use only IPS e.max
sintering behaviour is isotropic (identical in all build-up liquids. The organic components
directions), this corresponds to a linear used in these materials easily decompose at
shrinkage of 18.3 %. To enable a comparison, these temperatures. From 700 °C, the sintering
several competitive ceramic materials were process is so far advanced that only closed
subjected to the same test procedure (Table 3). porosities (isolated spaces) are present (Fig 9).
The linear shrinkage of all the systems was In contrast to trapped gas, this type of porosity
limited to the relatively narrow range between is easily eliminated as the sintering process
43.2 and 46.5 (linear 17.2 –18.8 %), while the advances. In the final stages of sintering, at
linear shrinkage of IPS e.max ZirCAD was 20 % 750 °C, the remaining closed porosities are
on average. densely sintered. Depending on the pre-
compaction by the dental technician, the total
volumetric shrinkage ranges between 40 and
45 %. A dense, homogenous sinter structure
results as shown in Figure 10.

Table 3:

Comparison of ZrO2 veneering ceramics with regard to characteristic temperatures and

volumetric shrinkage

Product name SS SE HT Linear Volumetric

[°C] [°C] [°C] shrinkage [%] shrinkage [%]
IPS e.max Ceram 550 749 935 18.3 45,4
Product A (Nobel Rondo Zr) 654 882 1170 17.2 43,2
Product B (Cercon CeramS) 560 803 1011 17.4 43,7
Product C (Vita VM9) 670 905 1241 18.8 46,5
SS = start of sintering; SE = end of sintering; HKT = hemisphere temperature

REPORT 31
 6 Bonding properties
IPS e.max Ceram is sintered onto
different framework materials. The properties
of the veneering ceramic are optimally co-
ordinated with corresponding framework
materials as regards the CTE and firing
temperature. The resulting adhesive regions
are visible on the polished sections shown
below (Figs 11–14).

IPS e.max CAD, Press and Ceram are of

Fig 7: Sinter microstructure at 600 °C and 64.0 % of Fig 8: Sinter microstructure at 650 °C and 83.3 % of
silicatic nature. Due to this chemical similarity, theoretical density theoretical density
adhesion can also be achieved through
chemical bonds within the glass structures.

IPS e.max ZirCAD is an oxide-based

ceramic which does not have any bonding
groups that are chemically similar to those of
silicate glass. At the temperature at which
ZirLiner is sintered, reactions occur that lead to
a chemical bond between the oxide ceramic
(IPS e.max ZirCAD) and the glass ceramic
(IPS e.max Ceram ZirLiner). The subsequent
firing cycles (wash and main firings) again
involve bonding of silicatic materials. As a
result of the chemical similarity, adhesion is
established through the formation of chemical
bonds within the glass structure. Fig 9: Sinter microstructure at 700 °C and 93.3 % of Fig 10: Sinter microstructure at 750 °C and 100 % of
theoretical density theoretical density

Surface conditioning of IPS e.max

ZirCAD is of particular importance when trying
to establish a bond between IPS e.max ZirCAD /
ZirLiner and Ceram. As described in the article
“IPS e.max ZirCAD", the transformation of
zirconia from its tetragonal to its monoclinic
phase is induced by mechanical stress. In dental
technology procedures, this transformation
process can easily be triggered by sandblasting
with aluminium oxide abrasive medium. A
modified surface results which consists of a
monoclinic phase and possibly trapped alu-
minium oxide particles. Due to the subsequent
ceramic bakes, which are conducted at 750 °C,
the monoclinic phase is maintained. Both the
Fig 11, 12: Bonding region between IPS e.max Ceram and IPS e.max CAD/Press (50x and 100x magnification,
monoclinic phase and the aluminium oxide polished section, BDE Contrast)
demonstrate a considerably lower CTE (in the
range of 7 to 8) than the tetragonal ZrO2. The
bonding layer undergoes overcritical changes
of the CTE value, ranging from 10.75 (tetra-
gonal dimensions) to 7 to 8 and finally 9.5
(ZirLiner and Ceram). Uncontrolled stress
results which weakens the bond and may lead
to chipping. Sandblasting the veneered surface
with aluminium oxide abrasive medium is
strongly forbidden.

Fig 13, 14: Bonding region between IPS e.max Ceram, ZirLiner and IPS e.max ZirCAD (100x and 1000x
magnification, polished section, BDE Contrast)

32
REPORT
7 Summary 8 Literature
IPS e.max Ceram is a veneering ceramic [1] Höland W., Rheinberger V., Wegner S., Frank M.;
Needle-like apatite-leucite glass-ceramic as a base
for universal use which is suitable for both material for the veneering of metal restorations in
zirconium oxide frameworks (IPS e.max dentistry; J Mater Sci Mater Med. 11 (1),11–7 (2000)
ZirCAD) and lithium disilicate frameworks [2] Höland W., Rheinberger V., Frank M.; Mechanism of
(IPS e.max Press, CAD). Due to the use of fluor- nucleation and controlled crystallization of needlelike
apatite glass ceramics as opaquing agent, apatite in glass-ceramics in the SiO2-Al2O3-K2O-CaO-
P2O5 systems; J Non-Cryst. Solids 253, 170–177
natural-looking aesthetics are achieved. (1999)

[3] Schweiger M., Höland W., Rheinberger V.;Nanophase

formation in different glass-ceramic systems; 104th
ACerS Meeting, St. Louis (2002)

[4] Kelly J.R.; Perspectives on strength; Dent Mater 11,

103–110 (1995)

[5] Lenz J.; Über die Spannungsverteilung in metallkera-

mischen Verbund-Biegeproben und die Ausbildung
von Transversalrissen in der Keramikverblendung;
Ceramic forum international/Berichte der DKG 60,
237–243 (1983)

[6] Kingery W.D., Bowen H.K., Uhlmann D.R.;

Introduction to ceramics; 2nd edition (Wiley, New
York, 1976)

[7] Petzow G., Kaysser W.A., Amtenbrink M.; Materials

science monographs 14, Sintering theory and
practice“ edited by Kolar D., Pejovnik S., Ristic M.M.
(Elsevier, Amsterdam, Oxford, New York, 1982)

REPORT 33
 IPS e.max ZirPress Marcel Schweiger

The pressable veneering ceramic

1 Introduction glasses and glass-ceramics are identical to

those of IPS e.max Ceram. The glasses are
IPS e.max ZirPress allows a dentin- homogeneously melted in special glass
shaded layer to be pressed on a CAD/CAM- melting furnaces at temperatures of
fabricated IPS e.max ZirCAD framework. 1300–1500 °C. Subsequently, they are trans-
Therefore, IPS e.max ZirPress represents a link formed into the IPS e.max ZirPress ingots by
between the IPS Empress and the CAD/CAM means of complex tempering, grinding, mixing
processing technique. The composition is and sintering processes. Table 1 shows the
similar to that of IPS e.max Ceram Dentin composition range of the main components.
materials. The opacity concept is also realized
by using fluorapatite glass-ceramics. Due to The chemical composition of IPS e.max
the IPS Empress technique, a very good ZirPress and IPS e.max Ceram is very similar.
cervical fit with high aesthetics in the anterior Identical basic materials are used in the mixing
region is achieved. The fully anatomical press- processes. By suitably adjusting the mixing
on procedure with subsequent stains and glaze ratios, the pressing temperature was
firing in the posterior region is a fast and sound established in such a way that IPS e.max
method to fabricate accurately fitting homo- ZirPress remains resistant to firing in subsequent
geneous restorations. In addition, the material firing cycles at 750 °C.
is ideally suitable for the fabrication of ZrO2-
supported inlay-retained bridges in conjunction
with the fully anatomical press-on technique.

3 Structure
IPS e.max ZirPress is a homogeneous
2 Composition mixture of fluorapatite-containing glass-
ceramics and sinter glasses. The sinter glasses
IPS e.max ZirPress is composed of sili- are single-phased and do not contain any
cate glasses and apatite glass-ceramics. The crystalline phases. The glass-ceramics used
only natural raw material used is quartz sand. contain fluorapatite crystals Ca5(PO4)3F. The
IPS e.max ZirPress does not contain any feld- presence of a crystalline phase
spar components or leucite crystals. Glasses is confirmed by XRD measure-
from the SiO2-Li2O-Na2O-K2O-ZnO-Al2O3 system ment and scanning electron
are used for the mixing components. For the microscopy (SEM). Figure 1
glass-ceramics which contain fluorapatite, the and 2 show the crystal forms
base glasses additionally include CaO, P2O5 typical of IPS e.max ZirPress.
and F. These three basic components are the
prerequisite for the formation of the By using different con-
Ca5(PO4)3F fluorapatite crystals. The base centration ratios of CaO-P2O5-
F and coordinated crystalliza-
Table 1: tion temperatures and times,
various fluorapatite crystal
Composition of IPS e.max ZirPress ingots forms can be selectively pro-
(wt.%) Fig 1: Longish fluorapatite crystals
duced. These processes take
place in a controlled fashion
SiO2 57.0 – 62.0 on a production scale. The
crystal quantity and form no
Na2O 6.0 – 8.0
longer changes during the
K2O 2.0 – 4.0 firing process in the dental
CaO 2.0 – 4.0 laboratory. IPS e.max ZirPress
Al2O3 12.0 – 16.0
contains needle-like and
nanoscale fluorapatite crystals.
ZrO2 1.5 – 2.5 The needles measure 1–2 µm
P2O5 1.0 – 2.0 in length and less than 200 nm
F 0.5 – 1.0 in diameter. The nano-scale
crystals have grown along a
Additional components: SrO, B2O3, ZnO
Fig 2: Nano-fluorapatite crystals

34
REPORT
slight longitudinal axis and have a length of less The firing stability during subsequent
than 200 nm. Their diameter measures firing cycles with IPS e.max Ceram is ensured
less than 100 nm. The term nano-crystals is by the temperature difference of 150 °C
applicable to sizes below 100 nm. between pressing and layering. The accuracy
of pressed ceramic shoulders or margins in
Apart from the fact that fluorapatite inlay-retained bridges is maintained and thus
crystals are employed because their structure is they no longer have to be adjusted. Hence,
very similar to that of natural dental enamel, possible shortcomings in the accuracy of fit of
the crystals are selectively used to establish the sintered and reduced ZrO2 frameworks can be
optical properties as regards translucency and improved.
brightness of the different ingots. This topic is
explained in the chapter IPS e.max Ceram and The CTE is ideally coordinated to the
is also valid for IPS e.max ZirPress. IPS e.max ZirCAD framework ceramic and
IPS e.max Ceram. The CTE is the highest in
IPS e.max ZirPress and decreases continuously
(see Fig 3).

4 Properties The bond between IPS e.max ZirPress

and the ZirLiner is very homogeneous and
IPS e.max ZirPress is a pressable compact due to the similar chemical composi-
material version of IPS e.max Ceram. There- tion (fluorapatite glass-ceramic) and virtually
fore, the chemical and physical properties of identical processing temperatures. Given the
both are very similar (Table 2). large difference in processing temperature of
50 °C between the ZirLiner (950 °C) and
The industrial sintering process and the IPS e.max ZirPress (900 °C), the ZirLiner which
IPS Empress processing technique endows has been fired prior to the press procedure
IPS e.max ZirPress with a very homogeneous, remains dimensionally stable on the ZirCAD
dense structure. If a veneer is built up by surface during the press procedure. Before
means of conventional layering and sintering, IPS e.max Ceram is layered on the pressed
there is always a latent risk of unintentionally ZirPress surface, it is important that the sur-
including defective areas in the structure of the face is properly conditioned. Complete re-
veneering ceramic. This risk is averted if moval of the reaction layer with the Invex
IPS e.max ZirPress is used. In addition, the liquid and the subsequent wash firing with
measured biaxial strength is about 20% higher IPS e.max Ceram are the requisite for an
than if IPS e.max Ceram is applied according to impeccable bond. Figures 4 and 5 show the
the layering technique. respective bond zones in the ceramo-graphic
grinding pattern.

Table 2:

IPS e.max ZirPress

Biaxial strength [MPa] * 110 ± 10

CTE (100-400°C)
9.75 ± 0.25
[µm/m*K]
Glass point [°C] 530 ± 10
Chemical resistance
30 ± 10
[µg/cm2] *
Vickers hardness HV5 [MPa] 5400 ± 200
* ISO 6872

Fig 3: CTE gradation of IPS e.max ZirCAD – ZirPress – Ceram

REPORT 35
 IPS e.max ZirPress can be etched with 5 Conclusion
hydrofluoric acid to produce a retentive
pattern. The etching pattern enables a good IPS e.max ZirPress is a fluorapatite-
bond to adhesive luting systems, such as containing glass-ceramic, which can be pro-
Variolink II or Multilink. The retentive pattern cessed in the IPS Empress technique. IPS e.max
in microscopic and macroscopic magnification ZirPress is used to press onto CAD/CAM-
is visible in Figs 6 and 7. The apatite crystals fabricated ZirCAD frameworks and thus
that have been produced as a result of etching represents a link between the IPS Empress and
the glass matrix are apparent in Fig 6. Figure 7 CAD/CAM processing technique. The chemical
shows high-contrast surfaces of the and physical properties are ideally coordinated
individual glass and glass-ceramic grains with with the IPS e.max ZirCAD framework ceramic
different etching patterns. and the IPS e.max Ceram veneering ceramic.
By using the IPS Empress technique, repro-
ducible results exhibiting a high accuracy of fit
and good aesthetic properties can be achieved.

Fig 4: Bond between IPS e.max ZirCAD, ZirLiner and ZirPress Fig 5: Bond between IPS e.max ZirPress and Ceram (etched, 3%
(polished ground surface) HF, 10 s)

Fig 6: Etching pattern of IPS e.max ZirPress with fluorapatite Fig 7: Etching pattern of IPS e.max ZirPress with glass and glass-
crystals (4.5% ceramic etching gel (HF); 20 seconds of reaction ceramic particles (4.5% ceramic etching gel (HF); 20 seconds of
time) reaction time)

36
REPORT
IPS e.max
The development in terms of dental technology and shading
Harald Kerschbaumer

1 Introduction material is in the "blue", pre-crystalline

state and thus easier to process. It is only
Ivoclar Vivadent AG offers a complete after milling that the restorations are
all-ceramic system with IPS e.max. IPS e.max endowed with their final strength and
Ceram which can be fired on the different colour by means of heat treatment.
framework materials made of lithium disilicate The shade and opacity of IPS e.max CAD
and zirconium oxide represents the core of the and IPS e.max Press frameworks are
system. In addition, the framework materials coordinated. The blocks are available in
can be processed with different methods: levels of medium opacity (MO).
IPS e.max CAD and ZirCAD in the CAD/CAM
technique, IPS e.max Press and IPS e.max – IPS e.max ZirCAD is a Y-TZP zirconium
ZirPress in the press technique. oxide. It can only be used for the
veneering technique. In order to achieve a
In order to use a veneering ceramic on shade match to the IPS e.max Press and
the different framework materials (Fig 1), a IPS e.max CAD framework materials,
common basis has to be established. The basis ZirLiner powders in special shades have
consists of the framework shades MO 0 – been developed to apply on the zirconium
white, MO 1 – light yellow, MO 2 – reddish, oxide frameworks.
MO 3 – yellowish, MO 4 – reddish-grey.
– IPS e.max ZirPress is used to press on
The shades of IPS e.max CAD and zirconium oxide frameworks. The ingots
IPS e.max Press are identical. The white are available in two levels of opacity: The
zirconium oxide is adjusted to the same basic MO ingots feature a higher opacity and
shades by means of the ZirLiner. colour saturation. Thus, they are used for
the fabrication of partially layered
restorations. The LT ingot is used for
pressing fully anatomical restorations.
Slight shade adjustments are applied with
the IPS e.max Ceram Shades. Unlike the
MO ingot, the LT ingot features a higher
translucency in order to achieve good
adaptation to the natural tooth (inlays
and partial crowns) and an incisal-like
effect in fully anatomically pressed
restorations. The two ingot types are
shaded according to the Vita Lumin
Fig 1: Unveneered frameworks: IPS e.max CAD, IPS e.max Press and
IPS e.max ZirCAD
Classic shade guide. The ingots are
available in the eight most popular
shades.

2 Framework materials
– IPS e.max Press is a lithium disilicate
glass-ceramic, which is available as a Table 1:
framework material in a medium opacity
(MO). Therefore, the opacity and the Table of opacity
resulting brightness value is of particular
importance for this ingot. The ingots are Material CR*
coloured according to the five basic e.max CAD MO 2 85%
shades MO 0, MO 1, MO 2, MO 3 and
e.max Press MO 2 85%
MO 4.
e.max Press HO 95%
– IPS e.max CAD is a lithium disilicate e.max ZirPress A3 MO 85%
glass-ceramic that has been particularly e.max ZirPress A3 LT 75%
optimized for CAD processing. During the
milling process in the unit, the framework e.max ZirCAD 95%

REPORT 37
 3 Veneering material
Basically, the development of veneering
ceramics covers the entire range of desirable
optical properties, such as translucency, opacity,
opal effect, fluorescence etc.

3.1 Opacity and translucency

Since the development of IPS Empress 2
and IPS d.SIGN, the conventional opaquing
agents (Fig 2), such as SnO2 and ZrO2, are no Fig 2: Conventional opaquing with SnO2 as the Fig 3: Opacity achieved by distributed nano-apatite
opaquing agent; SEM image, 5000x magnification crystals; SEM image, 5000x magnification
longer used for achieving the opacity in highly
aesthetic ceramics.

A glass component which contains a

variety of nano-apatite crystals (Fig 3) is used
to produce the desired opacity in IPS e.max
Ceram. This procedure allows a brightness
value that is similar to that of natural teeth and
excellent light transmitting properties (Fig 4) to
be achieved. This effect is the result of a well
coordinated refraction index between apatite
crystals and the residual glass matrix. The
refraction index of the conventional opaquing
agents stannous oxide or zirconium oxide is
considerably higher than that of the residual Fig 4: IPS e.max Ceram basic materials for achieving
the desired opacities; on the left basic material
glass matrix. Therefore, materials that have “transpa”, on the right basic material “opaque”
been treated with these agents appear rather
opaque and dark by transmitted light (Figs 5
and 6).

3.2 Opalescence
The opalescence of the IPS e.max
Ceram Effect materials is created by a selective
precipitation of nano-apatite crystals in the
size of 300 to 500 nm. The opalescent effect is
maintained even after multiple firing cycles.

The IPS e.max Effect materials 1 to 4

exhibit an opalescence that comes close to
that of natural teeth (Fig 7). They are mainly
Fig 5: Veneered zirconium oxide crowns by incident light; in the center IPS e.max ZirCAD / IPS e.max Ceram; on
used to determine the individual tooth shade. the left and right crowns from competitors
For the reproduction of shades from the shade
guide, however, the stipulated Incisal materials
(Fig 8) have to be used.

Fig 6: Veneered zirconium oxide crowns by transmitted light; in the center IPS e.max ZirCAD / IPS e.max Ceram;
on the left and right crowns from competitors

38
REPORT
 3.2 Fluorescence 3.3 The liner
The fluorescence of the IPS e.max The IPS e.max Ceram ZirLiner has two
Ceram layering materials has been determined functions. It establishes a sound bond to the
according to the proven IPS d.SIGN metal- zirconium oxide framework. In addition, the
ceramic. Special emphasis has been placed on liner endows the frameworks with the same
the natural concentration of fluorescent shade as IPS e.max CAD and IPS e.max Press
agents. Like in the natural tooth, the highest frameworks. In order to properly adjust the
concentration of fluorescent agents is in the required shade intensity, a special IPS e.max
root dentin and the lowest in the materials Ceram ZirLiner shade guide is available (Figs 10
used for the incisal region (Fig 9). and 11).

The range of ZirLiners consists of four

Table 2: shades, which correspond to the shade groups
MO 1 to 4, as well as a ZirLiner clear and four
Table of opacity
Intensive ZirLiners (yellow, orange, brown,
incisal).
Material CR*
e.max Ceram Body A3 75% Unlike zirconium oxide that has been
e.max Ceram Deep Dentin A3 90% stained with colouring liquids, zirconium oxide
frameworks shaded with ZirLiners can be
e.max Ceram Margin A3 85%
individually characterized. In some cases, a
e.max Ceram Incisal 2 40% white substructure is advantageous. For this
e.max Ceram Transpa Clear 10% purpose, ZirLiner clear can be used.
e.max Ceram Transpa Neutral 20%

Fig 7: Test sample of an opal component Fig 8: Test sample with ready-mixed Fig 9: IPS e.max Ceram crown with the respective shade tabs under UV light; Shoulder,
by transmitted light Effect 1 material by transmitted light Dentin and Enamel materials to show the course of fluorescence

Fig 10: Fired ZirLiner on IPS e.max ZirCAD crown with IPS e.max Ceram ZirLiner shade Fig 11: IPS e.max Ceram ZirLiner materials shade guide
guide

REPORT 39
 The IPS e.max Ceram ZirLiners are
transparent. Thus, light is transmitted into the
tooth structure and gingiva (Figs 12 and 13).

The development of the ZirLiners also Fig 12: ZirLiner on IPS e.max ZirCAD; light Fig 13: Opaque liner from a competitor;
is transmitted into the framework light is not transmitted
fulfils the need for natural fluorescence.
Zirconium oxide frameworks do not have any
inherent fluorescent properties. By adding
fluorescent agents to the ZirLiners, a natural-
looking fluorescence is transferred to the
frameworks (Fig 14).

Fig 14: Zirconium oxide with ZirLiner (left) and without ZirLiner (right) under UV light

40
REPORT
IPS e.max
Two clinical cases

Harald Dr Alexander
Kerschbauer Stiefenhofer

The following two clinical cases were exposed, and the overall colour of the two
treated with all-ceramic crown and bridge crowns was grey compared to the contra-
restorations. The first case involved a single lateral natural incisors (Fig 1). The gingiva of
tooth restoration with IPS e.max CAD/IPS e.max teeth 21 and 22 was located symmetrically to
Ceram crowns. The second case was restored the gingiva of the contralateral teeth 11 and
with an inlay/crown-retained bridge made of 12. The endodontic and periodontal state did
IPS e.max ZirCAD/IPS e.max ZirPress. not give any cause for concern (Fig 2).

Planning
Case 1: 46-year-old patient: Before abutment teeth 21 and 22 were
single crowns with lithium restored, the existing metal root posts with
disilicate glass-ceramic copings composite build-up material had to be re-
moved first. The prepared teeth had to be
in the maxilla restored with tooth-shaded, metal-free post
and core build-ups. For the crown, it was
Preoperative situation planned to use IPS e.max CAD MO frame-
The endodontically treated teeth 21 works in connection with the IPS e.max Ceram
and 22 which had been reconstructed with veneering ceramic. IPS e.max CAD MO is indi-
post and core build-ups had to be replaced by cated for single crowns in the anterior and
new prosthodontic restorations 13 years after posterior region. Since the IPS e.max CAD
insertion due to aesthetic shortcomings. The framework materials feature a similar opacity
following aspects were particularly noteworthy: to that of IPS e.max Ceram Deep Dentin, the
the crown margins were located in the supra- framework can be designed more generously
gingival area with the dark root surfaces in order to achieve maximum strength.

Fig 1: Preoperative situation: 13-year-old crowns on teeth 21 and 22. The root surfaces Fig 2: X-ray of teeth 21, 22 in the preoperative state. Opacities according to the
were exposed, as the gums had receded. In addition, the ceramic showed a grey colour endodontic and prosthetic restoration of teeth 21 and 22 with composite post and core
compared to the contralateral natural teeth. build-ups and crowns.

A B

Fig 3: Abutment teeth 21 and 22 reconstructed and postprepared with post and core build-ups made of composite and glass fibre posts ready to accommodate all-ceramic crowns.
Picture A shows an overview, Picture B shows a close-up of abutments 21 and 22.

REPORT 41
 Pretreatment formed foil after the wax-up was prepared.
The crowns were inserted with the eugenol-
Once the crowns and composite build-
free temporary luting cement Systemp.cem
ups, as well as endodontic posts had been
(Fig 4).
removed, new post and core build-ups were
inserted after the preparation was revised and
After a non-inflamed gingival situation
an elastomeric impression taken. The post and
was achieved after 4 weeks, the location of the
core build-ups were made using the light-
preparation margins in relation to the course
curing composite Tetric EvoCeram in the incre-
of the gingival margin was checked and an
mental layering technique and the glass fibre
impression of the abutment teeth taken. The
reinforced root posts FRC Postec on mounted
sulcus management comprised a thorough
super hard stone models with detachable
display of the preparation margin by means of
segments. The restorations were inserted after
the double cord technique. An electrosurgical
retraction cords were applied in a relatively dry
extension of the sulcus was not required. Iron-
operating field. For the adhesive cementation
IIII-sulfate was used as an astringent.
technique, the chemically curing luting com-
posite Multilink was used and the restoration
conditioned with the chemically curing
Multilink Primer. Subsequently, excess cement Fabrication of the restoration
was immediately removed prior to polymeriza- The best starting point for the frame-
tion using foam pellets and brushes. Finally, work design is the fully anatomical model of
the teeth were prepared to accommodate the the restoration, which is selectively reduced for
new crowns. The margin was prepared in the the veneer. It is important that the veneering
intrasulcular area (Fig 3). ceramic does not account for more than 50%
of the entire restoration thickness to avoid a
Temporary restorations were provided weakening of the overall restoration. The
in the form of resin crowns made of crown copings were fabricated of lithium di-
Systemp.c&b plus, which were fabricated silicate glass-ceramic blocks (IPS e.max CAD
directly on the patient. The temporary crowns MO) in the laboratory using the inLab system
were fabricated using a polyethylene vacuum from Sirona (Fig 5).

After fitting and finishing, the frame-

work is fired in a ceramic furnace. The use of
the stipulated silicon nitride firing tray and
the IPS Object Fix firing paste is of utmost
importance (Fig 6).

Only in this way can the stipulated

temperature profile be achieved and thus the
accurate shade and opacity attained. Figure 7
shows the tempered crown copings. Different
firing programs are available, depending on
the ceramic furnace in use.

Fig 4: Temporary restoration of teeth 21 and 22 with composite materials. Situation

after 4 weeks of treatment.

Fig 5: IPS e.max CAD MO crown copings Fig 6: Application of the firing paste Fig 7: Tempered crowns on silicon nitride

42
REPORT
Fig 8: The restoration is cleaned with steam Fig 9: Application of the wash paste Fig 10: First firing with Deep Dentin and characterization

A B

Fig 11: Completed crowns 21 and 22 made of IPS e.max CAD/IPS e.max Ceram. Picture A: labial view, Picture B: palatal view

A B

Fig 12: Situation after insertion of crowns 21 and 22 using glass ionomer cement. The
crowns have been in situ for 1 week. Picture A: overview, Picture B: close-up,
Picture C: final X-ray examination

REPORT 43
 Before the IPS e.max Ceram materials Placement
are applied, the framework is cleaned with
The strength of IPS e.max CAD/IPS e.max
steam or in an ultrasonic bath (Fig 8). The
Ceram crowns enables conventional cementa-
IPS e.max CAD framework must not be blasted
tion with a retentive core preparation. The
with aluminium oxide.
crowns were seated using the glass ionomer
cement Vivaglass CEM PL. The fully veneered
Before Dentin and Incisal materials are
crowns on IPS e.max CAD frameworks that
generously layered, a thin wash layer must be
have been veneered with IPS e.max Ceram
applied with any layering material and fired
harmoniously blend into the natural surround-
(Fig. 9). Subsequently, the restoration can be
ings (Fig 12).
completed as usual (Figs 10 and 11).
Six-month recalls showed an un-
The restoration must not be sand-
changing result regarding the soft tissue and
blasted with aluminium oxide prior to seating.
the quality of the ceramic (Fig 13).
The inner aspects of the restoration are treated
with IPS Ceramic Etching Gel for 20 seconds.
This etching procedure is conducted both with
adhesive and conventional cementation.

Figure 11 shows the completed crowns

after the second firing with Incisal and Transpa
materials on the model from a labial (Picture A)
and palatal view (Picture B).

A B

Fig 13: Recall after 6 months (Picture A) and 12 months (Picture B) after placement. The wedge-shaped defects in the upper posterior region had been restored in the meantime.

44
REPORT
 Case 2: 44-year-old patient: After sulcus management, elastic
impression taking, facebow transfer and
posterior bridge with registration of the horizontal and vertical jaw
zirconium oxide framework relation in the intercuspation position, the
super hard stone models were mounted into a
Preoperative situation semi-adjustable articulator to fabricate the
After successful periodontal treatment, inlay/crown-retained bridge 15-17.
the interdental space between teeth 15 and 17
had to be closed. Both abutment teeth 15 and The zirconium oxide bridge framework
17 were vital. Tooth 15 was crowned; tooth 17 was milled from an IPS e.max ZirCAD zirconium
showed a two-surface mesio-occlusal restora- oxide block in the inLab system from Sirona.
tion (Fig 14). The sintered zirconium oxide was fitted to the
master model. Once the framework was
finished, the ZirLiner in the suitable shade was
applied and fired (Fig 16).
Planning
The interdental space between 15 and A translucent pressed ceramic was
17 was to be closed with an adhesively luted, used to press a circular shoulder to tooth 15
all-ceramic inlay/crown-retained bridge with a and the side walls of the inlay in tooth 17.
zirconium oxide framework on which the
veneering ceramic was pressed and layered in
some areas. From a technical point of view, the
easiest and best solution in this case was to Wax-up and preparation for the press
press IPS e.max ZirPress onto the zirconium procedure
oxide framework. On the one hand, this allows
the complex occlusal surface to be designed A modelling wax that burns out without
with a proven wax-up. On the other hand, the leaving residue has to be used for the wax-up.
inlay in tooth 17 is much easier to fabricate by The teeth are modelled fully anatomically. A
means of the press technique than with the small portion of Incisal material is applied only
layering method. The translucent LT ingot was in the buccal and lingual area (Fig 17).
used to ensure ideal adaptation of the restora-
tion to the residual tooth structure. If the pontics in the posterior region are
voluminous, it is recommended to apply a ring-
shaped sprue (Fig 18) to achieve a detailed
Preparation and fabrication of the reproduction of the pontic (Fig 19).
restoration
Abutments 15 and 17 were prepared
according to a crown preparation with a
pronounced chamfer on tooth 15 and an MO
inlay preparation with a proximal shoulder on
tooth 17 (Fig 15). In the occlusal area, 1.5 mm
were available for the bridge framework and
veneer.

Fig 14: Orthopantograph after the periodontal treatment was completed. Interdental Fig 15: Preparation of the abutments for
space 15-17 to be closed the inlay/crown-retained bridge 15–17.
Circular chamfer on 15, inlay cavity with
proximal shoulder and slightly divergent
cavity walls on tooth 17

REPORT 45
 Completion present case, the preparations were isolated by
means of electrosurgical sulcus management,
After the sprues had been removed
iron-IIII-sulphate application and the place-
and the restorations completely fitted on the
ment of retraction cords (Ultrapak, Ultradent).
master model, a little space was provided for
It was not possible to use a rubber dam to
the build-up in the incisal area (Fig 20).
establish a completely dry field. Therefore, the
bridge was inserted under stringent moisture
To complete the anatomical form, the
control. The retraction cords had to remain in
incisal area was built up according to the free
place in the sulcus as far as possible during
layering technique with IPS e.max Ceram
placement to avoid sulcus fluid from escaping
(Fig 21).
and to protect the sulcus from penetration of
adhesive and luting composite. In the present
Finally, the restoration was stained with
case, the chemically curing Multilink luting
IPS e.max Ceram Shades and Essence materials
composite system was used for the adhesive
and glazed (Fig 22).
technique. Before the bridge was seated, the
restoration was conditioned with 5% hydro-
The basal view shows the central white-
fluoric acid gel (IPS Ceramic Etching Gel) in the
opaque IPS e.max ZirCAD zirconium oxide
area of the etchable IPS e.max ZirPress ceramic
bridge framework which was entirely covered
and subsequently silanized (Monobond-S).
with the IPS e.max ZirPress veneering ceramic
Cement excess was removed with foam
in the occlusal area and in the area of the
pellets, brushes and dental floss immediately
preparation margins. IPS e.max ZirPress is suit-
after placement before the restoration was
able for the adhesive technique.
light cured. At the cementation joint a brush
should be preferred over a foam pellet to
An inlay-retained bridge or a combined
prevent the luting composite from being
version, such as an inlay/crown-retained
wiped out of the cement margin. Figure 23
bridge has to be adhesively seated in order to
shows occlusal and buccal aspects of the
achieve the clinically required retention and
restoration in situ. The fully veneered inlay/
strength of the construction. As the zirconium
crown-retained bridge seamlessly blends into
oxide bridge framework exhibits only a very
the natural environment. The surrounding soft
low translucency, a chemically or dual-curing
tissue looks vital.
adhesive and luting composite have to be used
to ensure complete polymerization. In the

Fig 16: Reduced zirconium oxide framework with fired Fig 17: Complete wax-up of the restoration Fig 18: Attaching the sprues (note the ring-shaped sprue
ZirLiner on the pontic

Fig 19: Complete and accurate reproduction of details Fig 20: Pressed restoration completely seated on the Fig 21: Build-up of the incisal areas
master model

46
REPORT
Conclusion
The IPS e.max system currently offers
ceramic materials for the fabrication of single
tooth restorations (crowns, partial crowns,
veneers) and 3 to maximum 4-unit bridges in
the press and CAD/CAM techniques. Dental
technicians can work with only one layering
ceramic on the different framework materials
and thus cover virtually all indications in all-
ceramics. Dental technicians will appreciate
the benefit of having to handle only one
veneering ceramic, which will enable them to
fabricate predictable restorations more
Dental-lab work was fabricated by
efficiently. Franz Perkon and Andreja Mezan.

B B

C C

Fig 22: Completed inlay/crown-retained bridge 15-17: Picture A, B: view on the model; Fig 23: Inserted inlay/crown-retained bridge tooth 15 to 17. Final clinical pictures;
Picture C: basal view. The white-opaque zirconium oxide framework is visible in the Picture A: occlusal view, Picture B and C: buccal view
center

REPORT 47
 REPORT

Previous issues of the

Ivoclar Vivadent “Report”

Report No 1 (March 1984) * Report No 12 (December 1998)

G Beham Prof Dr W Höland
Dentin adhesion of restorative materials Dr med dent SD Heintze
IPS Empress 2: All-ceramic bridges and
Report No 2 (May 1985) * more ...
Dr V Rheinberger and G Beham
Adhesive bridges – new prosthetic Report No 13 (June 2000)
possibilities A Kammann
K Hagenbuch
Report No 3 (May 1986) * M Reis
P Wollwage H P Foser
Veneering materials for crowns and bridges Removable Denture Prosthetics: Materials Science,
Aesthetics and Tooth Setup
Report No 4 (December 1987) *
Dr P Dorsch Report No 14 (January 2001)
A review of proposed standards for metal-ceramic Dr Dr med dent A Rathke
restorations Dr sc nat U Lendenmann
Dentin adhesives: Excite in context
Report No 5 (January 1990)
G Ott Report No 15 (August 2004)
Composition and development of dental Dr G Zappini
composites Ing HTL S Hopfauf
U Spirig
Report No 6 (September 1990) * Focus on SR Adoro: Indirect Composites –
G Beham Materials Science and Development
IPS Empress: A new ceramic technology
Report No 16 (February 2006)
Report No 7 (November 1992) Dr V. Rheinberger
Dr U Salz Prof Dr H Kappert
The restored tooth – a complex bonding system P Oehri
T Specht
Report No 8 (January 1993) Dr Dr A Rathke
G Zanghellini, D Voser Dr T Völkel
Properties of resin based veneering materials Dr SD Heintze
Prof Dr JF Roulet
Report No 9 (March 1993) * HP Foser
R Grünenfelder Dr A Stiefenhofer
Stratos 200: New possibilities in biogenic All-ceramic Report: All-ceramic Restorations –
prosthetics Materials Science and Development

Report No 10 (July 1994)

Prof Dr W Höland,
Dipl Ing M Frank,
Dr rer nat U Salz, * out of print
Dr med dent G Unterbrink
IPS Empress: Material and clinical science

Report No 11 (January 1997)

K Hagenbuch
HP Foser
Artificial teeth – a symbiosis of materials, anatomy
and science

Ivoclar Vivadent Report

Published by Ivoclar Vivadent AG, Schaan, Liechtenstein
Editor: T Völkel
© 2006 by Ivoclar Vivadent AG, Schaan
600718/0606/e/W

48