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Relationship between microstructure and ductility of


investment cast ASTM F-75 implant alloy
M. Gomez, H. Mancha,* A. Salinas, J. L. Rodrguez, J. Escobedo, M. Castro, and M. Mendez
Centro de Investigacion y Estudios Avanzados del IPN-Unidad Saltillo, Carr. Saltillo-Monterrey Km. 13, Apartado
Postal 663, C.P. 25000, Saltillo, Coahuila, Mexico
Hip replacement implants fabricated using the ASTM F-75
alloy sometimes fail in a sudden catastrophic way. In general,
fractures start at microstructural defects subjected to stress
corrosion under chemical attack by body fluids. In this paper
the results of a study on the effect of casting parameters on the
microstructure of ASTM F-75 are presented. The preheating
mold temperature and the liquid temperature were varied
between 900 and 10008C, and 1410 and 14708C, respectively.
Optimum static strength and ductility were obtained when
shrinkage microporosity and the volume fraction of M23C6
eutectic carbides precipitated at grain boundaries were

minimized by increasing the preheating mold temperature


to 10008C and by using intermediate pouring temperatures
of 14558C. Under these casting conditions, however, the solidification rates are low, leading to large grain sizes, which, in
turn, reduce the strength of the material under dynamic
loading conditions. The volume fraction of the M23C6
blocky carbides appears to be independent of the casting
conditions; however, their size and spatial distributions determine the strength of the as-cast alloys. q 1997 John Wiley &

INTRODUCTION

researchers found that the presence or absence of continuous films of grain boundary carbides, discontinuous spherical carbides, and lamellar interdendritic carbides had a definite effect on the properties of the
alloy. When the microstructure showed a large-volume
fraction of grain boundary carbides, the measured
elongation to fracture values averaged 3.4%, with the
specimens showing globular and discontinuous intragranular carbides exhibiting larger ductilities. Some of
the specimens of the latter type showed as much as
12% elongation to fracture as well as a noticeable reduction in cross-sectional area. In this case it was also
observed that the grain size was particularly large,
with as few as two or three grains per cross-section.
Further work by Asgar and Peyton2 showed that
when the pouring temperature was increased, the ductility was improved without a severe effect on the yield
and tensile strengths in the as-cast condition. They
also suggested that the UTS was not affected by the
presence of microporosity, a result which disagrees
with the observations of Hollander and Wulff,3 who
reported that the UTS can be considerably improved
when the microvoids in an investment cast piece are
reduced by a hot isostatic pressing (HIP) treatment.
From the results of Asgar and Peyton,1,2 the following
observations arise: for tensile test pieces of the same
gauge length, higher casting temperatures result in
greater values of ductility; and for the same casting

ASTM F-75 cobalt-base alloy investment castings


have been used extensively for the manufacture of
orthopedic implants. The ASTM F-75 standard specification establishes the mechanical properties as follows:
yield strength, 450 MPa (min.); UTS, 650 Mpa (min.);
and minimum ductility of 8% elongation to fracture.
However, analysis of the open literature shows a great
deal of variation in mechanical properties data,
especially in the case of ductility. For example, %
elongation-to-fracture values range from as low as 3%
to as high as 12% in the as-cast condition,1,2 with no
clear explanation for such a wide range of variation.
However, analysis of these reports does provide that
information suggests the variation is associated with
a wide range of processing and testing conditions,
namely different pouring and preheating mold temperatures; small variations in carbon, chromium, and
molybdenum contents; and even the tensile test specimen size.
Asgar and Peyton1 studied the effect of the casting conditionsmetal pouring and mold temperatureson the mechanical properties of HS21 alloy,
which is essentially the same as ASTM F-75. These
*To whom correspondence should be addressed.

Sons, Inc.

Journal of Biomedical Materials Research, Vol. 34, 157163 (1997)


q 1997 John Wiley & Sons, Inc.

CCC 0021-9304/97/020157-07

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MEZ ET AL.
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158

conditions, the greatest values of ductility are measured from tensile tests performed on the specimens
with the smallest gauge lengths.
Riddighough4 reported that the grain size in Co26Cr-0.5C alloy (X-40) castings depended on the temperature of the liquid metal prior to casting and the
preheating temperature of the mold. They showed that
in an investment cast blade the grain size varied significantly with the blade depth. This result clearly demonstrated the cooling rate dependency of the as-cast
grain size. As in the work of Asgar and Petyon, Riddighough reported a strong correlation between carbide volume fraction and mold temperature for the X40 alloys.
Microporosity in as-cast ASTM F-75 alloys has severe detrimental effects on their mechanical properties,
especially on their ductility.1,3,5 Hollander and Wulf3
demonstrated that the elimination of microporosity by
hot isostatic pressing leads to a 50% increase in the
ductility with little effect on the yield strength and
good improvement of the tensile strength. However,
in their investigation,3 the authors did not report their
casting conditions, and therefore it is not possible to
establish a causeeffect relationship between microporosity and microstructure or tensile properties.
Georgette and Davison5 sintered cobalt powder
around tensile test specimens. This caused severe porosity at the base metal-coating interface, leading to a
decrease in the tensile strength and elongation to failure. The incorporation of a HIP cycle in the processing
of the coated tensile test specimen increased the tensile
strength, the yield strength, and the elongation to fracture as a result of the elimination of porosity.
In this article, we present microstructural evidence
showing that pouring and preheating mold temperatures affect the evolution of the microstructure during
solidification and that different microstructures result
in a wide range of mechanical properties in the alloy
ASTM F-75. An active patient with a hip replacement
prosthesis may easily subject the implant to tensile
stresses close to, or over, the UTS of the material. In a
separate publication,6 it is shown that the ASTM F-75
fails catastrophically right at the UTS, with no signs
of localized deformation. Thus, since a failed implant
complicates severely the revision arthroplasty, the
present results indicate that ductility, as measured by
the elongation to fracture in a standard tensile test,
may be used as a good acceptance test for ASTM F-75
orthopedic implants. However, in view of the wide
range of ductility values reported in the literature, we
will discuss the limitations of the standard methods
used to determine the ductility of this type of alloy.

four measurements on each sample. The results, expressed as mean values for all data with the corresponding standard deviation, were as follows: 27% Cr
6 0.19, 5.29% Mo 6 0.03, 0.25% C 6 0.006, 0.48% Si 6
0.007, 0.75% Mn 6 0.007, 0.43% Ni 6 0.02, 1.5% Fe 6
0.007, and Co (balance). An analysis of variance allowed
us to establish that the mean values of elements concentrated on the samples presented differences that were
not statistically significant at a 95% confidence level.
Chemical analysis was performed by the Leco fusion
technique to determine carbon content and by spark
emission spectroscopy to determine all other elements.
The alloy was melted in an electric vacuum induction
furnace and cast into a ceramic investment casting
mold placed inside the furnace chamber, which was
maintained under an Ar gas pressure of 0.65 atm. Several heats were fabricated that varied the metal pouring
temperature from 1410 to 14708C and the mold temperatures from 900 to 10008C. The liquid metal was cast
into 10-mm diameter bars, which were then machined
into standard ASTM E8 subsize tension test specimens
with a gauge length of 25.4 mm and a gauge diameter
of 6.3 mm. The tensile tests were performed in a computer-controlled electro-mechanical system using a
25.4-mm gauge length extensometer with a 50% span.
This extensometer is built so that it is capable of withstanding fracture of the specimen during the test. Thus,
since tensile samples did not exhibit necking right up
to the point of fracture, the reading from the extensometer at the point of fracture was a sensitive measure
of the % elongation to fracture. This method of estimation of the ductility of the specimens avoids the errors
introduced by joining the fracture surfaces together
and measuring the distance between two previously
established fiducial marks. As will be shown later,
when the gauge length of the test piece is small, the
standard method can introduce errors as large as 100%.
The tensile test specimens and the testing procedure
conformed to the ASTM E8 standard specifications. As
a function of casting parameters, grain size and the
volume fraction of carbides in the microstructure were
followed quantitatively, using a computer-controlled
image analyzer according to the Abrams procedure
(ASTM E-112). In all the specimens tested (three for
each experimental condition), the microstructure and
features of the fracture surfaces were examined using
optical and scanning electron microscopy. In each specimen, the entire fracture surface was observed.

MATERIALS AND METHODS

The as-cast microstructure of the various ASTM F-75


bars fabricated consisted of a strongly cored dendritic
matrix with a distribution of dispersed carbides that
presented three different morphologies. A eutectic

The chemical composition, in wt.%, of the ASTM F75 alloy was determined for each heat by performing

RESULTS

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MICROSTRUCTURE AND DUCTILITY OF ASTM F-75

carbide with a lamellar morphology was formed at


interdendritic regions or at grain boundaries. The overall composition of this carbide was evaluated semiquantitatively by EDS microanalysis and was found to
be similar to that of the dendritic matrix. The chemical
composition of individual lamellae was close to that
of the matrix and to that of the well known M23C6
(M 5 Co, Cr, Mo) carbide.7,8 The other two carbide
morphologies had blocky appearances and were
found to have precipitated at the interface between the
matrix and the eutectic carbide pools and also within
the interior of the dendritic matrix. EDS microanalysis
showed that these carbides also had a chemical composition similar to the M23C6 carbide although these were
richer in molybdenum. Qualitatively, the microstructure of the alloys prepared under the various casting
conditions did not show a great deal of variation (see
Fig. 1). However, the relative volume fractions of eutectic and blocky carbides and the grain size were,
indeed, strongly dependent on the casting conditions.
Figure 2 illustrates the effect of the preheating mold
temperature and the pouring temperature on the grain
size. As can be seen, the grain size increases faster with
pouring temperature when the mold temperature is
10008C, reaching average values as large as 0.8 mm at
Tpouring 5 1470 and Tmold 5 10008C. Figure 3(a) shows
the effect of pouring temperature on the volume fractions of eutectic and blocky carbides. As can be
seen, when the mold temperature is 9008C, the volume
fraction of carbides decreases linearly with increasing
pouring temperature, leading to a lower total carbide
volume fraction of about 14%. In contrast, when the
preheating mold temperature is increased to 10008C,
the volume fractions of eutectic and blocky carbides decrease rapidly with a pouring temperature that
increases beyond 14408C. After that, the volume fraction of eutectic carbides remains constant at values
smaller than 2%. Figure 3(b) shows the effect of the
pouring temperature on the ratio of the volume fraction of blocky carbides to that of eutectic carbides,
r(B/E). At a preheating mold temperature of 9008C,
the ratio r(B/E) is constant and, generally, slightly
lower than one. In contrast, when the molds are preheated at 10008C, the ratio r(B/E) is always greater
than one and shows a general tendency to increase
with increasing pouring temperature.
Figure 4 illustrates the effect of the casting conditions
on the mechanical properties of tensile strength (UTS),
yield strength (YS), and % elongation to fracture. The
results reported in Figure 4 are the average values
from three as-cast or heat-treated specimens. Typical
standard deviations were on the order of 6 0.51,
6 55, and 6 54 for elongation, UTS, and yield strength,
respectively. It can be seen that when the preheating
mold temperature is increased, the UTS [Fig. 4(a)] and
YS [Fig. 4(b)] slightly increase and comfortably exceed
the static strength requirements established by the

159

(b)
Figure 1. As-cast microstructures of the alloys studied
showing the dependency of the volume fraction of eutectic
and blocky carbides on the casting conditions: (a) preheating mold temperature 9008C, pouring temperature 14188C;
(b) preheating mold temperature 10008C, pouring temperature 14558C. Original magnification 3100.

ASTM F-75 standard specification for all casting conditions employed in the present work. However, in all
cases, the % elongation to fracture was below 4%,
which is about 50% lower than the minimum value
established by ASTM F-75. The analysis of variance
for all data at Tmold 5 9008C showed that the differences
of mean values were not statistically significant at a
95% confidence level. In contrast, because there is no
statistical evidence to say that the mean values are
equal, the same analysis for data at Tmold 5 10008C
shows small increasing tendency of ductility with the
increasing pouring temperature. It is noteworthy that
despite the minimum YS and UTS obtained with Tpouring

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160

mens cast at 14178C in a mold preheated at 10008C.


The mechanical properties data obtained from the tensile tests performed on these specimens are also plotted
in Figure 4. As can be seen, the mechanical properties
of the material cast at 14558C are superior to those
of the material cast at the lower temperature. The %
elongation to fracture is increased by nearly 300%, with
a 10% improvement in UTS and no significant effect
on the yield strength.

DISCUSSION

Figure 2. Effect of preheating mold temperature and pouring temperature on the grain size.

The experimental results presented establish a clear


relationship among the microstructure, mechanical
properties, and the processing parameters for the
ASTM F-75 alloy. The preheating mold temperature

5 14558C and Tmold 5 10008C, the maximum elongation


to fracture was only 3.12%. Specimens cast under these
conditions were subsequently given a standard solution heat treatment at 12208C for 4 h and then oil
quenched. A similar heat treatment was given to speci-

Figure 3. Effect of preheating mold temperature and pouring temperature on: (a) the volume fraction of eutectic and
blocky carbides; (b) the ratio of the volume fraction of
blocky carbides to that of eutectic carbides, r(B/E).

Figure 4. Effect of the casting conditions on the mechanical


properties: (a) tensile strength (UTS); (b) yield strength (YS);
(c) % elongation to fracture of as-cast ASTM F-75 alloy.

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MICROSTRUCTURE AND DUCTILITY OF ASTM F-75

was observed to affect the grain size, carbide volume


fractions, and amount and type of microporosity in the
as-cast microstructures. The effect of a higher pouring
temperature on the grain size is more pronounced
when the preheating mold temperature is higher. (Fig.
2). This effect can be explained in terms of the increase
in the number of nuclei activated by the larger undercoolings caused by larger differences between the
pouring and the preheating mold temperatures. This
argument is further substantiated by the results reported by Riddighough4 for X-40 alloys. Figure 3 shows
that for molds preheated at 10008C, the ratio r(B/E)
and the individual carbide volume fractions tend towards an approximately constant value at high pouring temperatures. This result may be associated with
the development of similar segregation patterns of C,
Mo, and Cr during the solidification process at the
higher pouring temperatures. In the case of material
cast into molds preheated at 9008C, the ratio r(B/E)
remains relatively constant over the whole range of
pouring temperatures. The individual volume fractions of carbides nevertheless decrease linearly as the
pouring temperature increases [Fig. 3(a)]. This implies
that the solute segregation pattern in this case may
be affected by the pouring temperature. The changes
observed in the carbide volume fraction and the grain
size affect the mechanical properties, as reported by
Asgar and Peyton.1 The results reported in Fig. 3 are
certainly affected by the variation of the microstructure
with casting parameters. In particular, the small increase in ductility observed when the mold was preheated to 10008C instead of 9008C is associated with
the elimination of microporosity, as shown in the SEM
photomicrographs of Figure 5, and the change of the
ratio of eutectic to blocky carbide volume fractions. As can be seen, for specimens poured into molds
preheated at 9008C (Fig. 5), the microporosity decreases
as the pouring temperature is increased from 14308C
to 14708C. Figure 5(c) shows that for the metal poured
at 14558 in a mold preheated at 10008C, the microporosity was completely eliminated.
The results reported by Asgar and Peyton2 are presented in graphical form in Figure 6. As can be seen,
the ductility was strongly affected by the casting temperature, with values as low as 3.5% when the mold
was preheated at 8718C and the metal was cast at
14268C. These authors suggested that these results
were associated with the presence of a considerable
amount of microporosity. This certainly can explain
their results at the lowest pouring temperature of
14268C. At higher casting temperatures, Asgar and
Peyton report2 values as large as 12% for their ASTM
F-75 alloys in the as-cast condition. These values are
at least 50% higher than those measured in the present
work and are similar to those obtained in the solutiontreated material. However, we attribute these large
values of ductility for as-cast ASTM F-75 to significant

161

Figure 5. Microporosity in as-cast ASTM F-75 using different casting conditions.

errors associated with estimating ductility in nonstandard gauge length specimens from measurements of
% elongation to fracture. Figure 7 shows graphically
the effect of the gauge length on the % elongation to
fracture values reported by Asgar and Peyton. The
usual method of placing the fracture surfaces of the
test specimen as close together as possible and measur-

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MEZ ET AL.
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Figure 6. Effect of pouring temperature on ultimate tensile


strength (UTS), yield strength (YS), and % elongation, as
reported by Asgar and Peyton.2

ing the distance between two previously inscribed fiducial marks can introduce considerable error when
the gauge length is small. In order to illustrate this,
Figure 8 shows a set of SEM micrographs showing the
mismatch produced when one attempts to join together
the two fracture surfaces of the tensile specimens tested
to failure. In the examples shown in Figure 8, the mismatch causes a separation distance of approximately
150 em. For a tensile test specimen with a gauge length
of approximately 3 mm, the mismatch distance represents an error greater than 50%. This problem is more
serious for alloys that are intrinsically brittle and have
a large grain size. In order to eliminate from the results
of a tension test this kind of experimental error in
the estimation of the ductility, the use of large-span
extensometers capable of withstanding the fracture of
the specimen is recommended. Figure 7 demonstrates
that for specimens with a gauge length greater than
about 25 mm, the measured elongation to fracture becomes independent of gauge length, and then, using
an axial extensometer, the results of Asgar and Peyton

Figure 7. Effect of gauge length on the % elongation to


fracture values, as reported by Asgar and Peyton.2

Figure 8. SEM micrograph showing the mismatch produced when attempting to join together the two fracture
surfaces of a tensile specimen tested to failure.

do indeed agree with the elongation to fracture measured in the present work.
The high ductility obtained in solution-treated
ASTM F-75 [Fig. 3(a,b)] is associated with a pouring
temperature of 14558C and a preheating mold temperature of 10008C. Under these conditions the microporosity was completely eliminated [Fig. 5(c)]. The lower
ductility values observed at the lowest pouring temperatures correspond to specimens cast into molds
preheated at lower temperatures. These specimens
showed also a large amount of microporosity. From
this result it can be concluded that the solution heat
treatment improves effectively the ductility of ASTM
F-75 alloys only when the microporosity has been eliminated completely. It is also noteworthy that the small
increase in tensile strength after the solution heat treatment is consistent with the reduction in the microporosity present in the alloy.

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MICROSTRUCTURE AND DUCTILITY OF ASTM F-75

CONCLUSIONS
The present article presents a clear correlation
between processing-microstructure and mechanical
properties for ASTM F-75 alloys. It was found that the
as-cast grain size is very sensitive to preheating mold
and metal pouring temperatures. Also, it was shown
that the formation of eutectic carbides can be minimized by increasing the preheating mold and metal
pouring temperatures. This microstructure control
through optimization of the processing parameters
leads to optimum mechanical properties.
It was demonstrated that the maximum tensile ductility attainable in as-cast ASTM F-75 is on the order
of 4% for the wide range of casting conditions testing
in the present work. In addition, an acceptable level
of ductility (according with the ASTM F-75) can be
achieved in this material by a subsequent solution
treatment if, and only if, the casting conditions are
such that the microporosity is completely eliminated
from the casting.
Finally, when the measured % elongation to fracture
is used to estimate the ductility of large grain size
and brittle metals, it is of paramount importance that
calibrated, large-span extensometers be used. The use
of subsize tensile test specimens and the traditional
method of measuring % elongation to fracture by joining together the fracture surfaces of a fractured specimen may lead to an important overestimation of the
ductility of the material being evaluated.

163

Technical support from Eruviel Cordova R. and Dora A.


Cortes H. is gratefully acknowledged. This work was supported by grants from CONACYT, projects PREAIN 933049
and DAIC 3074-A.

References
1. K. Asgar and F. Peyton, Effect of microstructure on the
physical properties of cobalt base alloys, J. Dent. Res.,
6372 (1961).
2. K. Asgar and F. Peyton, Effect of casting conditions on
some mechanical properties of cobalt base alloys, J.
Dent. Res., 40, 7386 (1961).
3. R. Hollander and J. Wulff, New technology for mechanical properties improvement of cast Co-Cr-Mo-C implants, J. Biomed. Mater. Res., 9, 367369 (1975).
4. M. Riddighough, Properties of cobalt-base investmentcast alloys, Foundry Trade J., 107, 421428 (1959).
5. F. S. Georgette and J. A. Davidson, The effect of HIPing
on fatigue and tensile strength of as-cast, porous-coated
Co-Cr-Mo alloy, J. Biomed. Mater. Res., 20, 12291248
(1986).
6. H. M. Mancha, A. R. Salinas, M. L. Gomez, M. R. Castro,
M. N. Mendez, and J. B. Escobedo, Effect of heat treatment on the mechanical properties of an as-cast ASTMF75 alloy, J. Mater. Synth. Process. (to appear).
7. Chester T. Sims, A contemporary view of cobalt-base
alloys, J. Metals, 21, 2742 (1969).
8. W. V. Youdelis and O. Kwon, Carbide phases in cobalt
base superalloy: Role of nucleation entropy in refinement, Metal Sci., 17, 379384 (1983).
Received August 16, 1995
Accepted February 26, 1996

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