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Materials	
  modelling	
  and	
  3D	
  prin2ng	
  in	
  
the	
  future	
  of	
  den2stry
Antonio	
  Licciulli
University	
  of	
  SalentoUniversity	
  of	
  Modena
21 3
1 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Outline
Introduction: ceramics for
prosthetic dentistry

The innovative process of
glass infiltrated alumina
composites

Microstructure and
properties of infiltrated
alumina composites

Conclusions
2 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
The future of dentistry
3 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Full ceramic prosthetic dentistry
Metal ceramic systems in prosthetic
dentistry involve complex, tedious,
time consuming lost vax processes
they have potential immunologic and
esthetic concerns
All ceramic prosthetic and implant
solution are under investigation
The novel technologies must provide
the same success rates of metal
implants
4 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Dental core ceramic families
Leucite reinforced glass ceramics, fabricated by
hot pressing the molten glass into a mold
σMOR ∼ 95-180 MPa, K1c= 1,3 MPa m1/2
Lithium disilicate reinforced glass ceramics,
fabricated by hot pressing
σMOR ∼ 340-400 MPa, K1c= 2-3,5 MPa m1/2
Glass infiltrated alumina pressed or slip cast
σMOR ∼ 350-500 MPa, K1c= 4-5 MPa m1/2
Zirconia fabricated by CAD/CAM
σMOR ∼ 800-1000 MPa, K1c > 5 MPa m1/2
Lithium dislocate GC
Leucite GC
MI alumina
3Y TZP
5μm
5μm
2μm
2μm
5 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Our innovation:
ceramic cores from oxide/oxide composites
Chopped fibers
reinforced CMC
microstructure
Crown, veneers,
bridges partial
dentures can be
conveniently produced

The tooth replica is
immersed in to a
special ceramic slurry

(dip moulding)
6 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Prosthetic dentistry: The restoration or
replacement of teeth
CROWNS are placed when a
significant amount of tooth
structure is lost 

Biting forces: 

incisors 200-250N 

premolars 150-500N, 

Molars 400 - 600N with maximum
up to 1000N

lateral load application 20-60N

BRIDGES are placed when there
are one or more teeth missing
7 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Smile modelling
8 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Structural analysis on all ceramic dental
bridge
The dimensions of the connector
cross-sections depend on the
physical properties of the core
ceramics

Maximum stress above 300MPa
in small gingival region at the
connectors, 

Up to now only zirconia (TSZ)
fulfill requirements on strength
and Weibull modulus

Our glass infiltrated composite
may represent a reliable solution
thank to its high strength and
Weibull modulus
9 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Prosthetic dentistry: the restoration or
replacement of teeth
DENTURES: replacement of an entire
or partial arch of teeth with a fixed
appliance 

Load application on implant sustained
prosthesis 40 - 400N

Strength requirement 800MPa

An IMPLANT is typically a titanium
screw that is placed into the jaw
bone. It is left in the bone for a period
of approximately 3-4 months to let it
"fuse" with the adjacent bone. A
metal or ceramic abutment is placed
for the crown to emerge from.
10 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
All Zirconia Dental Implant
prototype obtained by CNC
lathe
Zirconia dental Implants
Modified Titanium implant with
zirconia transgingival collar
11 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Implant design and reliability analysis
Implant
modeling
by CAD
Results feedback
and optimization

CNC
manufacturing
FEM
analysis
Reliability
analysis

12 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC CAD-CAM process
In production, several roughing cuts are
usually taken on the part, followed by
one or two finishing cuts
• Roughing - removes large amounts of
material from starting work part
– Creates shape close to desired
geometry, but leaves some material
for finish cutting
– High feeds and depths, low speeds
• Finishing - completes part geometry
– Final dimensions, tolerances, and
finish
– Low feeds and depths, high cutting
speeds
13 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Area1
Area 2
Area 3
Area 4
Area 5
Area 6
	
   	
   m σ0 σpeak Vi σi Bi B A
Area	
  1 9,2 841
171
0,227 171 9,82E-­‐08
2,09E-­‐07
0,9999998
(prob.	
  of	
  failure
	
  1	
  on	
  1.000.000)
Area	
  2 9,2 841 0,364 110 2,71E-­‐09
Area	
  3 9,2 841 0,182 125 4,40E-­‐09
Area	
  4 9,2 841 0,455 110 3,39E-­‐09
Area	
  5
9,2 841
0,727 150 9,41E-­‐08
Area	
  6 9,2 841 1,364 105 6,63E-­‐09
Stress state distribution and reliability
calculation
Thin wall design
implant
Fillet radius 0,7mm
14 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC CNC MILLING
15
15 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC CAD-CAM approach(zirconia)
Study of design(CAD) Toolpath design(CAM)
Materials, Tools,
cut parameter,
etc….
16 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Questions(?) before to start
Can we make it?
How to make it?
(setup)
How to make it?
(Toolpath, NC code)
17 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Questions(?) before to start
➢ how to turn the workpiece?
➢ what are the supports of the
workpiece during machining?
➢ which tools should I use?
➢ how should I position the
workpiece on the chuck?
➢ Which parameters should I
use in roughing and
finishing????
➢ ????
Titatium screw
Zirconia component
18 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Fixture planning
Zirconia workpiece
One sacrifical support(red) –
fixture on workpiece
CAD
MODEL
40x15x15 mm
19 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Fixture Planning
Fragile materials: metallic support
is needed!
Metallic pin(fixture on
chuck)
20 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Fixture Planning
Metallic support Toolpath planning
21 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Machining step by step
22 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Machining step by step
23 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Toolpath Planning
➢ Layer based toolpaths
➢ Machine visible surfaces from approach direction
➢ It consist in several tool movements;
➢ A gouge-free approach, given flute and shank diameter are same (or shank <
flute)
➢ Can approach finish machining using very small depths of cut
➢ We assume that tool length, not diameter will be active constraint
➢ To avoid collision, tool length > maximum swept diameter of part (Same as
stock diameter)
➢ Tool diameter chosen as smallest available for required length (not conventional
tools)
24 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Toolpath Planning
Which is the goal?
➢ Generate the shortest
tool-path for machining
of a part
➢ Minor number of
movements tools means
high efficienty
Shorter production time
Decrease production cost
25 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC
%
O0000(STAMPOCOPERCHIO_PORTASONDA)
N102 G0 G17 G40 G49 G80 G90
N104 T1 M6
N106 G0 G90 G54 X185. Y4.8 A0. S6366 M3
N108 G43 H1 Z64.978
N110 Z44.978
N112 G1 Z39.978 F1018.6
N114 X184.638 F2037.1
N116 X183.936 Z39.805
Toolpath planning
Cad Model Toolpath design
SimulationNC Program
26 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Accelerated aging and fatigue test
Test conditions: saline
environment, 1.000.000
of cyclic bending stress
loading with peak stress of
320 MPa and frequency of
20 Hz.
ISO 13356:2008 “Implants
for surgery – ceramic
materials based on yttria
stabilized tetragonal
zirconia (Y-TZP)
Salentec ZirconiaCE
displays no break during
fatigue test 0"
200"
400"
600"
800"
1000"
before" a.er"1.000.000"of"
cyclic"loading"
σMOR%[MPa]%
941"±"136"
768"±"137"
27 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
3D scanning system Teeth design by CAD CAM software for mill
programming
Computer numerical
control machining
Components of a CAD CAM system
Sintering Presintered ceramic disk
28 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC
Ceramic CNC machining in
Dentistry application
29 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC Salentec ZrO2
Blocks, Blanks, and several
dimensions are available
Properties:
- Pure ZrO2 presintered;
- Bar code guarantees
material properties and
contraction
- 98 mm diameter and different
thicknesses (10-25 mm)
- Approximately 25 elements
per disk milled
- Even bridges 14 Merged
30 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
‹N›
SALENTEC
Computer assisted
design(CAD)
31 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Plaster replica of
tooth
Dip plaster replica on
“magics slurry”
Drying and presintering
Excess glass removal,
porcelain enamelling
Melt infiltration of alumina composite
Sintering Melt infiltration
32 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
The Alumina matrix
Fine and reactive grade Al2O3
powder (AES-23, Sumitomo
chemicals, Japan) and CT530
and CT1200 from Almatis have
been compared

Size of α crystal from 0,3-4μm

Bimodal distribution, fired density
3,77g/cm3

Green density 2,57 3,77g/cm3,
sintered density 3,77g/cm3
10μm
Presintered AES23
33 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
The fibrous preform
Chopped fibres from Saffil
were produced by ball milling
a fibrous mat

Alumina content  95-97 %

Median Diameter  3.0-3.5 μm

Median length 20-50 μm

Tensile Strength  1.5GPa

Melting Point  > 2000°C

Young's Modulus  300GPa

40μm
34 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
!
Main feature of CMC dental core
Instantly 0,5mm thick uncracked crown
are obtained

Net shape forming and sintering
❏35 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
!
With and without fibre reinforcement:
advantages in forming
The slurry without fibrous
reinforcement cannot withstand
the mechanical stresses due to
shrinkage on the convex mold

Thank to the fibre reinforcement
the green will not crack
36 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Net shape forming and sintering
The linear shrinkage in pre-sintered
blocks was 0.045 ± 0.019 % 

After glass infiltration the linear
shrinkage was 0.078 ± 0.015 %. 

The shrinkage was found to be
uniform in all three axes with no
warping or cracking of the samples

shrinkage was found be ∼4 times
less than than the lowest found in
literature (VITA In-ceram alumina
samples which showed 0.21%)
°under similar pre-sintering
conditions
Green
Sintered
37 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Total porosity approx.
20%
Bulk density 3.2 g/cm3
Fibre addition spreads
the pore size distribution
toward high dimensions,
reduces total porosity
increasing the volume of
big pores at a time
Porosity of alumina preform
38 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
11
Oxide are mixed and fused at
1300°C

Frits are obtained quenching
the molten oxide in water

La2O3 behaves like glass
modifier

B2O3 behaves like network
former but also reduces
melting temperature
Lantanide glass frits development
Oxide La-1 La-2 La-3
SiO2 16 % 14,5 % 13.89 %
Al2O3 16 % 16 % 12.22 %
B2O3 13 % 14,5 % 17.89 %
La2O3 45 % 45 % 47.43 %
CeO2 3 % 3 % 2.95 %
CaO 3 % 3 % 2.88 %
TiO2 4 % 4% 2,74 %
39 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
11
Lantanide based glass are
obtained in a full amorphous
structure

BO4- tetrahedrons form in
presence of alkaline, alkaline
earth cations

BO4- tetrahedrons, should lead
to a strengthening of the glass
Microstructure of lantanide glass frits
Silica tetrahedrals 

+ tetragonal planar BO3
BO4 tetrahedrons
40 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
!
Differential thermal analysis on glass frits
Tg glass transition temperature (650°C)

Tc crystallization temperature 

Tx onset of crystallization (863°C)

∆T = Tx-Tg stability interval (213°C)
Tg
Tx
Tc
41 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
!11
jlkl
Thermal evolution of lantanide glass frits
Sintering Softnening Sphere
Hemisphere Fusion
42 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Morphology and composition of infiltrated
composite
30μm
43 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
11
XRD analysis of La-3 infiltrated
samples revealed small
crystalline peaks of Lanthanum
silicate (La2Si2O7).

The calculations revealed that
~13 % of the glass phase has
crystallized
Microstructure of infiltrated CMC
44 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
!
Glass infiltration
300μm
45 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Melt infiltration vs
temperature and time
Penetration rate of glass into
alumina is limited by glass
viscosity

Temperature is the main element at
a fixed glass composition
influencing glass viscosity
1150°C
1200°C
1250°C
MeltinfiltratedLa3onAES23
46 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Melt infiltration vs porosity
Infiltration is driven by capillarity

Glass penetration increases with
increasing pore radious and
porosity
AES23 20% porosity
CT1200 36% porosity
CT530 32% porosity
MeltinfiltratedLa3at1250°C
47 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Strength increase after glass infiltration
Flexural	
  strength	
  (MPa)
0,0
150,0
300,0
450,0
600,0
VITA La-­‐1 La-­‐2 La-­‐3
The infiltrated glass greatly
increases the mechanical
strength

The La-2 glass infiltrated
sample is similar to the best
performing alumina
before
melt
infiltration
48 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Weibull plot of preform and glass infiltrated
composite
Melt infiltrated composites
display very high strength
and Weibull modulus (14)
The calculated value is
significantly higher than
conventionally sintered
alumina ∿ 5-10
49 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Conclusions
All ceramic prosthesis and implants are
the new frontier in dentistry. With respect
to metal/ceramic, they may become more
performing and affordable 

Ceramic scientists have to face important
challenges in terms of material innovation,
structural performances

Net shape forming process was
developed using an alumina based
composite suitable for crown, veneers
and bridges

The glass infiltrated composites showed
significant increase in strength combined
with a significant increase in the Weibull
modulus.
50 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
Thank you
for your kind attention

for your warm hospitality
51 Licciulli "Open lab" tribute 2 - 07 gennaio 2015

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Ldb OpenLab_Licciulli-prototipazione di materiali avanziati (parte 2)

  • 1. Materials  modelling  and  3D  prin2ng  in   the  future  of  den2stry Antonio  Licciulli University  of  SalentoUniversity  of  Modena 21 3 1 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 2. Outline Introduction: ceramics for prosthetic dentistry The innovative process of glass infiltrated alumina composites Microstructure and properties of infiltrated alumina composites Conclusions 2 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 3. The future of dentistry 3 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 4. Full ceramic prosthetic dentistry Metal ceramic systems in prosthetic dentistry involve complex, tedious, time consuming lost vax processes they have potential immunologic and esthetic concerns All ceramic prosthetic and implant solution are under investigation The novel technologies must provide the same success rates of metal implants 4 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 5. Dental core ceramic families Leucite reinforced glass ceramics, fabricated by hot pressing the molten glass into a mold σMOR ∼ 95-180 MPa, K1c= 1,3 MPa m1/2 Lithium disilicate reinforced glass ceramics, fabricated by hot pressing σMOR ∼ 340-400 MPa, K1c= 2-3,5 MPa m1/2 Glass infiltrated alumina pressed or slip cast σMOR ∼ 350-500 MPa, K1c= 4-5 MPa m1/2 Zirconia fabricated by CAD/CAM σMOR ∼ 800-1000 MPa, K1c > 5 MPa m1/2 Lithium dislocate GC Leucite GC MI alumina 3Y TZP 5μm 5μm 2μm 2μm 5 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 6. Our innovation: ceramic cores from oxide/oxide composites Chopped fibers reinforced CMC microstructure Crown, veneers, bridges partial dentures can be conveniently produced The tooth replica is immersed in to a special ceramic slurry (dip moulding) 6 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 7. Prosthetic dentistry: The restoration or replacement of teeth CROWNS are placed when a significant amount of tooth structure is lost Biting forces: incisors 200-250N premolars 150-500N, Molars 400 - 600N with maximum up to 1000N lateral load application 20-60N BRIDGES are placed when there are one or more teeth missing 7 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 8. Smile modelling 8 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 9. Structural analysis on all ceramic dental bridge The dimensions of the connector cross-sections depend on the physical properties of the core ceramics Maximum stress above 300MPa in small gingival region at the connectors, Up to now only zirconia (TSZ) fulfill requirements on strength and Weibull modulus Our glass infiltrated composite may represent a reliable solution thank to its high strength and Weibull modulus 9 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 10. Prosthetic dentistry: the restoration or replacement of teeth DENTURES: replacement of an entire or partial arch of teeth with a fixed appliance Load application on implant sustained prosthesis 40 - 400N Strength requirement 800MPa An IMPLANT is typically a titanium screw that is placed into the jaw bone. It is left in the bone for a period of approximately 3-4 months to let it "fuse" with the adjacent bone. A metal or ceramic abutment is placed for the crown to emerge from. 10 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 11. All Zirconia Dental Implant prototype obtained by CNC lathe Zirconia dental Implants Modified Titanium implant with zirconia transgingival collar 11 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 12. Implant design and reliability analysis Implant modeling by CAD Results feedback and optimization CNC manufacturing FEM analysis Reliability analysis 12 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 13. ‹N› SALENTEC CAD-CAM process In production, several roughing cuts are usually taken on the part, followed by one or two finishing cuts • Roughing - removes large amounts of material from starting work part – Creates shape close to desired geometry, but leaves some material for finish cutting – High feeds and depths, low speeds • Finishing - completes part geometry – Final dimensions, tolerances, and finish – Low feeds and depths, high cutting speeds 13 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 14. Area1 Area 2 Area 3 Area 4 Area 5 Area 6     m σ0 σpeak Vi σi Bi B A Area  1 9,2 841 171 0,227 171 9,82E-­‐08 2,09E-­‐07 0,9999998 (prob.  of  failure  1  on  1.000.000) Area  2 9,2 841 0,364 110 2,71E-­‐09 Area  3 9,2 841 0,182 125 4,40E-­‐09 Area  4 9,2 841 0,455 110 3,39E-­‐09 Area  5 9,2 841 0,727 150 9,41E-­‐08 Area  6 9,2 841 1,364 105 6,63E-­‐09 Stress state distribution and reliability calculation Thin wall design implant Fillet radius 0,7mm 14 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 15. ‹N› SALENTEC CNC MILLING 15 15 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 16. ‹N› SALENTEC CAD-CAM approach(zirconia) Study of design(CAD) Toolpath design(CAM) Materials, Tools, cut parameter, etc…. 16 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 17. ‹N› SALENTEC Questions(?) before to start Can we make it? How to make it? (setup) How to make it? (Toolpath, NC code) 17 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 18. ‹N› SALENTEC Questions(?) before to start ➢ how to turn the workpiece? ➢ what are the supports of the workpiece during machining? ➢ which tools should I use? ➢ how should I position the workpiece on the chuck? ➢ Which parameters should I use in roughing and finishing???? ➢ ???? Titatium screw Zirconia component 18 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 19. ‹N› SALENTEC Fixture planning Zirconia workpiece One sacrifical support(red) – fixture on workpiece CAD MODEL 40x15x15 mm 19 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 20. ‹N› SALENTEC Fixture Planning Fragile materials: metallic support is needed! Metallic pin(fixture on chuck) 20 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 21. ‹N› SALENTEC Fixture Planning Metallic support Toolpath planning 21 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 22. ‹N› SALENTEC Machining step by step 22 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 23. ‹N› SALENTEC Machining step by step 23 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 24. ‹N› SALENTEC Toolpath Planning ➢ Layer based toolpaths ➢ Machine visible surfaces from approach direction ➢ It consist in several tool movements; ➢ A gouge-free approach, given flute and shank diameter are same (or shank < flute) ➢ Can approach finish machining using very small depths of cut ➢ We assume that tool length, not diameter will be active constraint ➢ To avoid collision, tool length > maximum swept diameter of part (Same as stock diameter) ➢ Tool diameter chosen as smallest available for required length (not conventional tools) 24 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 25. ‹N› SALENTEC Toolpath Planning Which is the goal? ➢ Generate the shortest tool-path for machining of a part ➢ Minor number of movements tools means high efficienty Shorter production time Decrease production cost 25 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 26. ‹N› SALENTEC % O0000(STAMPOCOPERCHIO_PORTASONDA) N102 G0 G17 G40 G49 G80 G90 N104 T1 M6 N106 G0 G90 G54 X185. Y4.8 A0. S6366 M3 N108 G43 H1 Z64.978 N110 Z44.978 N112 G1 Z39.978 F1018.6 N114 X184.638 F2037.1 N116 X183.936 Z39.805 Toolpath planning Cad Model Toolpath design SimulationNC Program 26 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 27. Accelerated aging and fatigue test Test conditions: saline environment, 1.000.000 of cyclic bending stress loading with peak stress of 320 MPa and frequency of 20 Hz. ISO 13356:2008 “Implants for surgery – ceramic materials based on yttria stabilized tetragonal zirconia (Y-TZP) Salentec ZirconiaCE displays no break during fatigue test 0" 200" 400" 600" 800" 1000" before" a.er"1.000.000"of" cyclic"loading" σMOR%[MPa]% 941"±"136" 768"±"137" 27 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 28. 3D scanning system Teeth design by CAD CAM software for mill programming Computer numerical control machining Components of a CAD CAM system Sintering Presintered ceramic disk 28 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 29. ‹N› SALENTEC Ceramic CNC machining in Dentistry application 29 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 30. ‹N› SALENTEC Salentec ZrO2 Blocks, Blanks, and several dimensions are available Properties: - Pure ZrO2 presintered; - Bar code guarantees material properties and contraction - 98 mm diameter and different thicknesses (10-25 mm) - Approximately 25 elements per disk milled - Even bridges 14 Merged 30 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 31. ‹N› SALENTEC Computer assisted design(CAD) 31 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 32. Plaster replica of tooth Dip plaster replica on “magics slurry” Drying and presintering Excess glass removal, porcelain enamelling Melt infiltration of alumina composite Sintering Melt infiltration 32 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 33. The Alumina matrix Fine and reactive grade Al2O3 powder (AES-23, Sumitomo chemicals, Japan) and CT530 and CT1200 from Almatis have been compared Size of α crystal from 0,3-4μm Bimodal distribution, fired density 3,77g/cm3 Green density 2,57 3,77g/cm3, sintered density 3,77g/cm3 10μm Presintered AES23 33 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 34. The fibrous preform Chopped fibres from Saffil were produced by ball milling a fibrous mat Alumina content  95-97 % Median Diameter  3.0-3.5 μm Median length 20-50 μm Tensile Strength  1.5GPa Melting Point  > 2000°C Young's Modulus  300GPa 40μm 34 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 35. ! Main feature of CMC dental core Instantly 0,5mm thick uncracked crown are obtained Net shape forming and sintering ❏35 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 36. ! With and without fibre reinforcement: advantages in forming The slurry without fibrous reinforcement cannot withstand the mechanical stresses due to shrinkage on the convex mold Thank to the fibre reinforcement the green will not crack 36 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 37. Net shape forming and sintering The linear shrinkage in pre-sintered blocks was 0.045 ± 0.019 % After glass infiltration the linear shrinkage was 0.078 ± 0.015 %. The shrinkage was found to be uniform in all three axes with no warping or cracking of the samples shrinkage was found be ∼4 times less than than the lowest found in literature (VITA In-ceram alumina samples which showed 0.21%) °under similar pre-sintering conditions Green Sintered 37 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 38. Total porosity approx. 20% Bulk density 3.2 g/cm3 Fibre addition spreads the pore size distribution toward high dimensions, reduces total porosity increasing the volume of big pores at a time Porosity of alumina preform 38 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 39. 11 Oxide are mixed and fused at 1300°C Frits are obtained quenching the molten oxide in water La2O3 behaves like glass modifier B2O3 behaves like network former but also reduces melting temperature Lantanide glass frits development Oxide La-1 La-2 La-3 SiO2 16 % 14,5 % 13.89 % Al2O3 16 % 16 % 12.22 % B2O3 13 % 14,5 % 17.89 % La2O3 45 % 45 % 47.43 % CeO2 3 % 3 % 2.95 % CaO 3 % 3 % 2.88 % TiO2 4 % 4% 2,74 % 39 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 40. 11 Lantanide based glass are obtained in a full amorphous structure BO4- tetrahedrons form in presence of alkaline, alkaline earth cations BO4- tetrahedrons, should lead to a strengthening of the glass Microstructure of lantanide glass frits Silica tetrahedrals 
 + tetragonal planar BO3 BO4 tetrahedrons 40 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 41. ! Differential thermal analysis on glass frits Tg glass transition temperature (650°C) Tc crystallization temperature Tx onset of crystallization (863°C) ∆T = Tx-Tg stability interval (213°C) Tg Tx Tc 41 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 42. !11 jlkl Thermal evolution of lantanide glass frits Sintering Softnening Sphere Hemisphere Fusion 42 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 43. Morphology and composition of infiltrated composite 30μm 43 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 44. 11 XRD analysis of La-3 infiltrated samples revealed small crystalline peaks of Lanthanum silicate (La2Si2O7). The calculations revealed that ~13 % of the glass phase has crystallized Microstructure of infiltrated CMC 44 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 45. ! Glass infiltration 300μm 45 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 46. Melt infiltration vs temperature and time Penetration rate of glass into alumina is limited by glass viscosity Temperature is the main element at a fixed glass composition influencing glass viscosity 1150°C 1200°C 1250°C MeltinfiltratedLa3onAES23 46 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 47. Melt infiltration vs porosity Infiltration is driven by capillarity Glass penetration increases with increasing pore radious and porosity AES23 20% porosity CT1200 36% porosity CT530 32% porosity MeltinfiltratedLa3at1250°C 47 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 48. Strength increase after glass infiltration Flexural  strength  (MPa) 0,0 150,0 300,0 450,0 600,0 VITA La-­‐1 La-­‐2 La-­‐3 The infiltrated glass greatly increases the mechanical strength The La-2 glass infiltrated sample is similar to the best performing alumina before melt infiltration 48 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 49. Weibull plot of preform and glass infiltrated composite Melt infiltrated composites display very high strength and Weibull modulus (14) The calculated value is significantly higher than conventionally sintered alumina ∿ 5-10 49 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 50. Conclusions All ceramic prosthesis and implants are the new frontier in dentistry. With respect to metal/ceramic, they may become more performing and affordable Ceramic scientists have to face important challenges in terms of material innovation, structural performances Net shape forming process was developed using an alumina based composite suitable for crown, veneers and bridges The glass infiltrated composites showed significant increase in strength combined with a significant increase in the Weibull modulus. 50 Licciulli "Open lab" tribute 2 - 07 gennaio 2015
  • 51. Thank you for your kind attention for your warm hospitality 51 Licciulli "Open lab" tribute 2 - 07 gennaio 2015