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Mechanical properties and micro


structural analysis of a NiCr alloy cast
under different temperatures
Karina Andrea Novaes Olivieri
1
Maximiliano P. Neisser
2
Paulo C. R. de Souza
3
Marco Antnio Bottino
2
1
Graduate Dental Student, Department of
Dental Materials and Prosthodontics, School
of Dentistry of So Jos dos Campos
UNESP- Brazil.
2
Professor of the Department of Dental
Materials and Prosthodontics, School of
Dentistry of So Jos dos Campos UNESP-
Brazil
3
Engineer and Senior Instructor, School of
Chemistry , Araraquara, UNESP, Brazil.
Received for publication: January 8, 2004
Accepted: February:22, 2004
Correspondence to:
Karina Andrea Novaes Olivieri
UNESP School of Dentistry of So Jos dos
Campos
Rua: Engenheiro Francisco Jos Longo, 777
Bairro Jardim So Dimas
So Jos dos Campos S/P
12245-000
e-mail: kaolivieri@ig.com.br
Abstract
The purpose of this study was to evaluate the chemical and metallurgi-
cal aspects, mechanical properties and hardness of the NiCr dental
alloy when it was submitted to different castings temperatures. An
NiCr alloy was cast, with lost wax technique, 20 specimens, separated
in two groups of 10 each one, in two different casting temperatures: a)
in accordance with the manufactures instructions (T1); b) above manu-
factures instructions (T2). It was done chemical and metallographic
analysis witch scanning electron microscope in the alloy in these condi-
tions: no cast, T1 and T2. It was determined mechanical properties and
hardness, too. The microstructures were similar to no cast, T1 and T2.
There was no significant difference between chemical analysis and to
mechanical properties. The hardness of the T1 and T2 groups was
greater than no cast group. Clinically, it may predict that when elevated
temperatures were used, above manufactures recommendations (more
than 100C), there will be failures in the prosthesis, like porosities,
fissures or cracks.
Key Words:
NiCr alloy, casting temperatures, mechanical properties.
Braz J Oral Sci. January/March 2004 - Vol. 3 - Number 8
415
Introduction
The cast metal restorations have been used in Dentistry
since last decade. Nowadays, several resources are
available to obtain more precise castings due to the
introduction of new materials, more accurate techniques,
and especially to a more scientific approach of the casting
process
1
.
The choice of an alloy is based on several factors. Cost is
a serious consideration due to the high price of gold. Other
factors that shall be considered are biocompatibility and
corrosion resistance
2
. These factors in particular limit the
use of alloys for dental prostheses, and the choice of an
specific application is primarily determined by their
mechanical properties, such as hardness, mechanical
strength and ductility, as according to Van Noort
3
.
Due to the worsened economical situation and consequent
increase in the price of gold, the use of these alloys became
impractical and inaccessible for many practitioners
4-5
.
The non-nobl e met al al l oys are chemi cal l y and
metallurgical complex, with critical and more precise
laboratory procedures than gold-based alloys, especially
regarding fabricating and casting procedures. Hence, the
choice of a prosthetic laboratory and technician by the
dental practitioner is important for the casting quality. In
1972 the American Dental Association
6
(ADA) proposed
a Program for Acceptance of Metal Alloys in the EUA
aiming at evaluating all metal alloys for cast restorations,
including those not included in its specifications, all
alternative alloys to the gold-based alloys and those
whi ch apart from t hei r composi t i on, demonst rat ed
biological compatibility and adequate physical, chemical
and mechanical properties.
The inferior qualities of non-noble metal alloys when
compared to gold-based alloys led to the introduction of
quantitative and qualitative modifications in their chemical
composition, either in fabricating and casting procedures
or in laboratory techniques, all of which had the objective
of allowing their use as eventual substitutes for cast gold
restorations, at the same time that in vivo and in vitro
studies were performed with comparative purposes
4, 7
.
Due to the absence of literature research that may support
the influence of dental alloy casting temperature on their
microstructure and mechanical properties, it was the
purpose of this in vitro study to evaluate this influence
on a NiCr alloy used for fixed partial and single prostheses.
Material and Methods
The Wiron 99 alloy (BEGOWilcos-Brasil) is specifically
applied for dental use in Fixed Partial Prostheses. This
alloy has 65% of nickel (Ni), 22.5% of chromium (Cr), 9.5%
of molybdenum (Mo), besides other chemical elements,
such as C, Nb, Si, Fe and Ce , and has a specific mass of
8.2 according to data supplied by the manufacturer.
Twenty specimens were obtained by means of lost wax
casting technique and divided in two groups of ten, so
that each one was submitted to a different temperature:
T1 recommended by the manufacturer, and T2 above
t he recommended t emperat ure. Tabl e 1 shows t he
temperatures used for alloy casting in the two studied
conditions.
The templates that originated the specimens in this study
were built in a laboratory specialized in dental prostheses
using blue wax for inlay casting using a usinated stainless
steel matrix, according to the International Standards
Organization (ISO) specification number 6871, as it can be
seen in Figure 1.
Wax templates were invested in a metal ring previously
underlain with amiantus. Then the phosphate-based
investment (Micro- Fine 1700- Talladium - USA) was
poured according to the manufacturers recommendations.
After the final investment setting, models were placed in
an EDG furnace (model EDGCON 3P 3000) for wax
elimination under temperatures between 600
O
and 900
O
C
for 90 minutes.
Casting was performed in a centrifuge by argon gas
induction (model DUCATRON Series 3 France) using
a digital optical infrared pyrometer (M-GULTAN- Pirograt-
IS-3D- Germany) for temperature control.
Upon cast i ng compl et i on, ri ngs were l eft at room
temperature for cooling. Specimens were separated from
Fig. 1 - Templates that originated the specimens in this study.
* in accordance with the manufactures instructions
Alloy
Wiron 99
Casting Temperature* (T1)
(C)
1420
Above of casting temperature (T2)
(C)
1520 20
Table 1 - Temperatures used for alloy casting in the two
studied conditions
Braz J Oral Sci. 3(8):414-419 Mechanical properties and micro structural analysis of a NiCr alloy cast under different temperatures
416
their investments and submitted to blasting with glass
micro balls and subsequently with aluminum oxide.
External machining using mounted tips and abrasive
rubbers was performed for final finishing.
The chemical composition analysis of the alloys in this
st udy was performed i n t he Cent er for Mat eri al s
Characterization and Development (CMCD at the Federal
University of So Carlos UFSCAR).
Samples with approximately 3mm of thickness were
obtained from the tensile strength test specimens and
embedded in transparent chemically activated acrylic
resin. They were then mechanically polished using 360,
400, 600, 1000 and 2000 mesh sandpaper followed by alumna
polishing with 1 and 0.3mm. This procedure aimed at
obtaining a flat and polished surface. After that, samples
were chemically etched using a 2:1 HCl and HNO
3
solution
for approximately 10 seconds. The etching was controlled
t o produce a correct observat i on of phases and
morphologies present in the microstructure.
Finally, they were submitted to metallographic examination
using Scanning Electron Microscopy (SEM) in a JEOL-
JSM microscope (T-330) coupled to a x-ray dispersive
energy analyzer (XDE) and a camera with similar origin.
The tensile and elongation tests were performed using a
Material Test System (MTS 810) equipment and data
analysis was made using a specialized computer software
(Test Star II) coupled to the system. Load cells of 100kN
with 1,0mm/mim speed were used. Hardness measurements
were obtained using a Micromet 2003 Buehler device
under 500gf or 4903 mN strength
4,8-10
.
Two-way analysis of variance (ANOVA) was used to
detected significant differences among the conditions
studied.
Results
Table 2 shows the chemical analysis results under the
three studied conditions for the NiCr alloy (NC= no cast;
T1= temperature recommended by the manufacturer
(1420C) and T2= temperature above the recommended
(1520C)).
Figure 2 shows the SEM analysis of the NiCr alloy in the
no cast condition (NC).
Figure 3 shows the SEM analysis of the NiCr alloy under the
T1 condition. We verified a clumsier dendritic microstructure
and less quantity of particles than in the NC condition.
Figure 4 shows the SEM analysis of the NiCr alloy under the
T2 condition. We verified a clumsier dendritic brute fusion
microstructure with fewer amounts of precipitates than under
the NC and T1 conditions.
The results obtained in the tensile strength test and
respective statistical data can be observed in Figures 5,6
and 7. The results obtained with the Vickers hardness test
and respective statistical analysis can be verified in Figure 8.
Table 2 - Chemical analysis performed for the three studied
conditions using the NiCr alloy (% m/m)
Elements
C
Cr
Mo
Si
Nb
Ce
Fe
Ni
NC
0,0127 0,0005
24,4 0,07
9,08 0,02
0,482 0,08
0,742 0,05
0,347 0,03
0,10 0,03
BALANCE
T1
0,0161 0,002
22,5 0,15
8,99 0,10
0,232 0,007
0,606 0,01
<0,012
0,13 0,03
BALANCE
T2
0,0100 0,0003
22,3 0,42
9,29 0,25
0,222 0,02
0,603 0,05
< 0,012
0,17 0,01
BALANCE
Braz J Oral Sci. 3(8):414-419 Mechanical properties and micro structural analysis of a NiCr alloy cast under different temperatures
Fig. 3 Micrography of the NiCr alloy in the T1 condition, Attack:
gua rgia, 1000X
Precipitate
Fig. 2Micrography of the NiCr alloy in the NC condition,Attack:
gua rgia, 1000X .
Precipitate
Porosity
Fig.4 Micrography of the NiCr alloy in the T2 condition, Attack:
gua rgia, 1000X
Precipitate
Porosity
417
Fig.7 NiCr alloy in the T1 and T2 conditions statistical analysis of
creeping.
Fig. 6 NiCr alloy in the T1 and T2 conditions statistical analysis
of rupture tensile strength.
Fig.5 NiCr alloy in the T1 and T2 conditions statistical analysis
of elongation
Fig.8 NiCr alloy in the No Cast (NC), T1 and T2 conditions
statistical analysis of Vickers hardness.
Discussion
By observing the chemical analysis of the alloy in an no
cast condition, we verified that Table 2 is coherent with
the composition supplied by the manufacturer. The
chemical composition of Ni, Cr, Mo, C , Nb and Fe remained
practically constant under the three studied conditions.
For Si and Ce there was a slight reduction under the T1
and T2 conditions when compared to the NC condition.
This reduction may be due to an inefficient protection
provi ded by t he argon at mosphere duri ng cast i ng
procedures, as long as these elements are more reactive
with oxygen under high temperatures.
Lewis
11
found a composition of 69.30% Ni, 16.00% Cr;
5.40%Mo, 3.90% Mg; 2.89% Al, among other metals in
less quantity, in a chemical analysis using X-ray emission
spectrometry microscopy of a NiCr alloy. Baran
12
states
that the binary phase diagram for the NiCr system shows
extensive solid solubility of chromium in nickel, and as a
resul t bi nary al l oys are hardened by means of
precipitation. Approximately 37% of Cr in weight can
remain dissolved at room temperature in the gamma matrix.
This author found the following composition for the Wiron
S and Wiron 77 alloys: Wiron S: 69% Ni, 17% Cr, 5% Mo,
0,37% Fe, 0.42% Co, 0.04 C, 3% Mn and Wiron 77: 67% Ni,
20% Cr, 65 Mo, 1.5% Nb, 4% Si, 0.04%C. Mondelli
5
also
reported the chemical composition of some NiCr alloys:
Nicron G (70.0% Ni, !9.1% Cr; 4.20% Mo); Kromalit (62.5%
Ni, 20.4% Cr, 6.58% Mo) and Resistal P (62.5% Ni; 18.5%
Cr e 9.85% Mo). This results are similar to those obtained
in this study. We can verify in a Figure 2 a dendritic brute
fusion microstructure with precipitates dispersed in the
entire matrix
13-14
.
The SEM of the NiCr alloy in this study shows a dendritic
Braz J Oral Sci. 3(8):414-419 Mechanical properties and micro structural analysis of a NiCr alloy cast under different temperatures
418
brute fusion microstructure with porosities similar to those
found by Lewis
15
. When the alloy was cast above the
recommended temperature this microstructure was less
refined and presented more porosity.
Lewis
16
observed an interdendritic phase with a lamellar
structure and areas of micro porosity in an original ingot
of NiCr alloy. According to this author, the lamellar -shaped
morphology is considered as the normal shape produced
with the euthetic solidification. In a first casting he
observed l amel l ar st ruct ures wi t h i nt erdendri t i c
distribution. The overheated microstructure presented
three characteristics:
a) Absence of acicular phase;
b) Absence of interdendritic euthetic phase;
c) Absence of fine linear interdendritic phase.
Lewis
17
studied fusion patterns (ADA n 14) obtained from
a Ni-based alloy submitted to a tensile strength test and
observed under SEM. The Ni-based alloys exhibited a
strong tendency towards a dendritic crystallization, as it
was also evidenced in this study.
Lewis
18-19
showed that the solidification produced using
NiCr alloys initially involves the formation of a dendritic
skeleton followed by the filling of the process that occurs
interdendritically. The first formed solid is essentially the
NiCr solution, and in each case the two elements are
presented in strictly corresponding proportions to those
determined for alloys. It would be expected that this
composi t i on was mai nt ai ned duri ng t he subsequent
solidification, and the study demonstrated that this is
normally the situation that occurs inside the alloy. The
optical microscopy of the NiCr alloy shows a transitional
zone between the matrix and the interdendritic euthetic
formations, as it was evidenced in the present study.
The rupture tensile strength and creeping limit values for
the T1 and T2 conditions of the NiCr alloy are statistically
similar. The elongation presents higher values under the
T2 than the T1 condition. This can be explained by the
more homogeneous microstructure observed under the
T2 condition.
The elongation values obtained under the T1 and T2
condi t i ons are si mi l ar t o t hose found for Ul t rat ek,
Microbond NP/2 and Litecast alloys (24%, 27% and 28%,
respectively), as according to Baran
12
.
The Vickers hardness values for the NiCr alloy under T1
and T2 conditions are statistically similar, but higher than
those found under the NC condition. These results are in
agreement with Phillips
4
and Baran
12
for the Wiron alloy
submi t t ed t o t he t emperat ure recommended by t he
manufacturer.
Moffa et al .
20
compared t wo Ni Cr al l oys wi t h a
conventional gold-based alloy and concluded that the
Vickers hardness is 174 for the gold alloy and 270-310 for
the non-gold alloys. These values obtained for non-gold
alloys are superior to those found in this study.
Conclusion
This study evaluated the metallurgical and clinical aspects
of the different casting temperatures on a NiCr alloy. Within
the limitations of this work, it can conclude:
All the castings that were performed using manufactures
recommendations showed the best results.
Clinically, it may predict that when elevated temperatures
was used, above manufactures recommendations (more than
200C), there will be failures in the prosthesis, like porosities,
fissures or cracks.
Acknowledgements
The authors thank FAPESP (# 98/15302-0) for the financial
support and the Institute of Chemical of Araraquara-
UNESP.
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419
Braz J Oral Sci. 3(8):414-419 Mechanical properties and micro structural analysis of a NiCr alloy cast under different temperatures
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