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Introduction of the

Characteristics and Synthetic


method of Portland cement
derivatives(Silicate cement)




Date: 2014/06/03
Presenter: Kuan-Wei Lu
Supervisor: Yuan-Min Lin, PhD
Shue-Feng Yang, Ms

1
1
Advantage of Portland cement
derivatives as endodontic treatment
materials
2
Synthetic method of Portland cement
derivatives
3
Current Lab Step and Conclusion
2



3
1
Advantage of Portland cement
derivatives as endodontic treatment
materials
2
Synthetic method of Portland cement
derivatives
3
Current Lab Step
Advantage of Portland cement derivatives
as endodontic treatment materials
4
Pulp capping

Salako, Joseph et al. (2003)
Advantage of Portland cement derivatives
as endodontic treatment materials
Pulp capping
Ca(OH)2 MTA
5
TR Ford et al. ,1996
Advantage of Portland cement derivatives
as endodontic treatment materials
Root-end retrograde filling material

6
Author Method Disadvantage Advantage
Amalgam Nelson and
Mahler
(1990)

in vitro
air
pressure
test
Water-contaminated
Greater Micro-
leakage
Zinc contiained alloy
Delayed expansion
Low-copper alloy
Delayed
expansion
root fracture
risk
High copper
alloy
with better
sealing ability
Advantage of Portland cement derivatives
as endodontic treatment materials
Root-end retrograde filling material

7
Author Method Disadvantage Advantage
Adhesive
Resin
Composite
(Retroplast)
von Arx,
Hanni et
al. (2010)

1-year
Clinical S/S
Follow up
Radiographic
evaluation

91.3% healed
cases of MTA-
treated teeth >
79.5% healed cases
of Retroplast-
treated teeth
significantly higher
(P = .003)
Lower setting
time

8
1
Advantage of Portland cement
derivatives as endodontic treatment
materials
2
Synthetic method of Portland cement
derivatives
3
Current Lab Step

Background of Portland cement
derivatives

9
Mahmoud Torabinejad, DMD,
MSD, PhD
Professor of Endodontics
Department of Endodontics,
School of Dentistry, Loma Linda
University, Loma Linda, CA.
Introduce Portland cement derivatives to
dental application
GMTA/WMTA






GMTA(since 1995) WMTA(since 2002)
(image origin : http://www.dentsplymea.com/products/endodontics/retreatment-
repair/proroot-mta)
10
Portland cement
derivatives
Published Article
Calcium
oxide (CaO)
Silicon
Dioxide
(SiO2)
Aluminum
oxide
(Al2O3)
Others
GMTA
Torabinejad et al.,
US Patent Number:
5415547, 1995

65%

21% 4%
Fe2O3 5%
MgO 2%
N2O K2O
0.5%
SO3 2.5%

WMTA
(main particle)
G. VOICU et al. 2012
70.95%

26.78%

2.27%

Partial-Stabilized
Cement
Lin, Wang et al. 2003
69.4% 21.6% 5.8%
Fe2O3 3.2%
ZnO 0.5-3%

11
Composition of Portland Cement
Derivatives

12
Published Article Main Crystalline Structures
GMTA
Torabinejad et al.,
US Patent Number:
5415547, 1995
Tricalcium silicate (3CaOSiO2)
Dicalcium silicate (2CaOSiO2)
Tricalcium aluminate(3CaOAl2O3)
Tetracalcium aluminoferrite (4Ca0Al2O3Fe2O3)
WMTA
(main particle)
G. VOICU et al.
2012
Tricalcium silicate (3CaOSiO2),
Dicalcium silicate (2CaOSiO2),
Tricalcium aluminate(3CaOAl2O3)

Partial-Stabilized
Cement
Lin, Wang et al. 2003
Tricalcium silicate (3CaOSiO2),
Dicalcium silicate (2CaOSiO2),
Tricalcium aluminate(3CaOAl2O3)
Tetracalcium aluminoferrite (4Ca0Al2O3Fe2O3).

Synthesis
of Portland
Cement
Derivatives
13
Sol-gel technique

Melt-quenching
technique
Traditional Synthesis of Portland
Cement Derivatives
Melt-quenching technique
Making powder component mixed as a raw
material, placed at melting temperature,
then
quick quenched to the final crystalline
Laudisio and Branda (2001)
14
Traditional Synthesis of Portland
Cement Derivatives
Formation in the CaO-SiO2 system is limited
for
Lower CaO (<20% mol) content by the presence
of a liquid-liquid immiscibility
higher CaO (>20 % mol) content by high
liquidus temperature
Laudisio and Branda (2001)

15

16
SiO2(1723C)
3CaOSiO2
(>2100C)
CaO(2200C)
Sol-gel synthesis of Portland
Cement Derivatives
Sol
The Sol is made of solid particles (metal alkoxide, ex:
TEOS,(OC2H5)4 Si) of a diameter measuring few to
hundred nm suspended in a liquid phase
Gel (gelation phase)
Formed by means of hydrolysis and condensation
reactions of solid particles



17
C. J. Brinker and G. W. Scherer(1990)
Sol-gel synthesis of Portland
Cement Derivatives
Controlled factors
Concentration of monomer precursor(water to
alkoxide ratio)
Reaction temperatures
Catalyst
Time cost for gelation/maturation
Laudisio and Branda (2001)

18
Sol-gel synthesis of Portland
Cement Derivatives

19
Condensational reaction
Hydrolysis reaction
Si
RO
RO
RO
OR
HO
-

Si
OR
OR
RO OR
HO Si
OR
OR
OR
OR
-
-

OH
-
C. J. Brinker and G. W. Scherer(1990)
20
C. J. Brinker and G. W. Scherer(1990)
Sol-gel synthesis of Portland
Cement Derivatives
Gel (gelation phase)
Drying the Gel by means of low temperature treatments
(25-100 C), it is possible to obtain porous solid matrices
(XEROGELs).


21
C. J. Brinker and G. W. Scherer(1990)
22
C. J. Brinker and G. W. Scherer(1990)
Product analysis: X ray-
Diffraction Analysis (XRD)
23
XRD-Basic Theory
Wavelength of X-ray0.1-100


24
K1(1.392)
JG Brown et al., 1966
Family of Crystal Plane
25
JG Brown et al., 1966
Bragg Equation
26
2dsin = n
W.H Bragg et al., 1913
Comparison of Processing
Protocol
Torabinejad
et al.,1995
Lin, Wang et al.
2003
G. VOICU et al.
2012
Ndong,
Sadhasivam et al.
2012
Method Melt-
quenching
Melt-
quenching
Sol-gel Sol-gel
Product GMTA PSC WMTA PSC-Zn
Heat
treatment
Temperature
14001650
C
(?)
13001400
C
(?)
12501350
C
1400 C
Heat
treatment
Time
Not mentioned 2hrs 30 mins 2hrs
Total cost time Not mentioned 2hrs 22 days 4 days
Raw material Type I
Portland
cement
Gypsum
Bismuth oxide
CaO(lime)
SiO2(Powder)
ZnO/CrO/CoO

Ca(NO3)24H2O
Al(NO3)39H2O
TEOS

Ca(NO3)24H2O
Zn(NO3)26H2O
C12H27AlO3
Acetyl acetone
Ammonia
water(catalyst)

27
28
Lin, Wang et al. 2003
1400 C
G. VOICU et al. 2012
Melt-quenching technique vs.
Sol-gel technique

29
Advantage Disadvantage
Melt-quenching
technique

1. Time saving
2. Easier preparation of
raw material

1. Higher heat
treatment
temperature
2. Unsatisfied Phase
distribution

Sol-gel technique

1. Lower heat treatment
temperature
2. Uniform phase
distribution
3. Higher reactivity of
the product
4. Small particle size
availability
1. Cost time
2. More complicated
raw material



30
1
Advantage of Portland cement
derivatives as endodontic treatment
materials
2
Synthetic method of Portland cement
derivatives
3
Current Lab Step
Sol-gel synthesis of WMTA
2 Samples:
WMTA(Densply,Tusla)
Pilot study sample
Raw material:
Ca(NO3)24H2O
Al(NO3)39H2O
Tetraethyl-orthosilicate (TEOS,C6H16O3Si)
- G. VOICU et al. Digest Journal of Nanomaterials and
Biostructures, 2012

31
32
33
Sol-gel synthesis of WMTA
The powder was pressed in pellets and
thermally treated at 1250C or 1350C for
30 minutes
Grinded for two hours into a laboratory
planetary mill (v=150 rot/min)

34
-G. VOICU et al. Digest Journal of Nanomaterials and
Biostructures, 2012

WMTA(Proot MTA,Tusla)


Pilot study sample


X2
X1
Y1
Discussion
WMTA(Proot MTA) obtained from VGH
has high quality
Unknown peak of X1 X2 may be the
contaminated by the melting
crucible( Intolerable to 1200C)
Y1 peak(32-33) stands for the exist of the
triclinic Tricalcium silicate (3CaOSiO2),
but the intensity is not enough.
37
Lin, Wang et al. 2003
Conclusion
Portland cement derivatives may have more
favorable outcome as pulp capping/
retrograde root end sealing material
compared to other common dental
materials
X ray-Diffraction Analysis (XRD) can be a
high sensitive tool for detection of the
crystal structure and composition of the
38
Conclusion
Main component of WMTA could be
synthesized by sol-gel technique to achieve
uniform phase distribution, but it takes time
for gelation/maturation.
39
Questions
1)Which of the following compound is not
the main functional component of the
Portland cement derivatives?
1. Tricalcium silicate (3CaOSiO2)
2. MonoCalcium silicate(CaOSiO2)
3. Tricalcium aluminate(3CaOAl2O3)
4. Dicalcium silicate (2CaOSiO2)

40
Questions
2)Which of the following description is not
related to the Sol-Gel technique?
1. Higher heat treatment temperature
2. Uniform phase distribution
3. Higher reactivity of the product
4. Small particle size availability

41
Questions
Which one bellow is Mahmoud
Torabinejad, DMD, MSD, PhD?
1. 2. 3.

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Thank you for your attention!
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