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W.J. BOETTINGER, M.E. WILLIAMS, S.R. CORIELL, U.R. KATTNER, and B.A. MUELLER
The alpha case thickness at the surface of a Ti-6Al-4V (wt pct) step wedge investment casting has
been measured and successfully predicted. The prediction uses temperature-time results obtained from
a heat flow simulation of the casting. The temperature-time results were coupled to a simple model
for diffusion of oxygen into the beta phase during continuous cooling. Oxygen concentration and
microhardness profiles were measured from the surface in contact with the ZrO2 face coat of the
shell mold into the interior of the casting. The oxygen content in the metal at the shell mold interface
was between 5 and 9.5 wt pct in general agreement with a thermodynamic calculation for bcc Ti in
contact with ZrO2. At the limit of the alpha case region, as determined by standard metallographic
technique, the oxygen concentration was found to be no more than 0.02 wt pct above the level of
oxygen in the bulk alloy. Using this information and one particular literature value for the activation
energy for diffusion of oxygen, a nearly linear relationship was obtained between the measured and
predicted alpha case thicknesses at various positions on the casting surface. Reduction of the prefactor
of this diffusion coefficient by a factor of 7.5 produces excellent agreement between predicted and
measured alpha case thicknesses. Such a reduction is not inconsistent with the scatter of literature
values for the diffusion coefficient.
I. INTRODUCTION
alloy far from the casting surface. For ZrO2 particles in the
face coat, a composition of 70 wt pct Zr (30 at pct Zr) and
28 wt pct O (68 at pct O) was obtained with the other
elements totaling about 2 wt pct. For the bulk alloy, average
concentrations of 5.7 wt pct Al, 3.8 wt pct V, and 0.7 wt
pct O were obtained. The measurements have an estimated
standard uncertainty of 60.5 wt pct. The measured Al and
V contents are within specifications for this alloy. However,
the measured O content is too high. The actual level of
oxygen in the interior of the casting is 0.25 wt pct, as
measured by a combustion technique. The line scans also
showed the oxygen concentrations in the bulk to be systematically high by approximately 0.5 wt pct. Therefore, the profiles were corrected to give oxygen values close to 0.25 wt
pct in the bulk. The microhardness profiles across the alpha
case region were obtained using a Vickers indenter with a
100 g load.
III. EXPERIMENTAL RESULTS
A. Shell Mold Microstructure
The SEM and optical micrographs of the interface
between the shell mold material and the alloy in a gate
section (not shown in Figure 1) with a very thin alpha case
region are shown in Figure 2. In the shell mold, the bright
particles in close proximity to the alloy are ZrO2. The regions
between the ZrO2 particles appear to be porosity. No Si
signal from the binder was detected in this region.
B. Alpha Case Microstructure and Thickness
Fig. 1Geometry of step wedge test casting. Only a quarter section is
shown. The full widths (W ) of the arms are 7.5 cm (left) and 3.8 cm (right).
The bottom six steps were analyzed. Their widths (S) increase from 0.64
to 3.8 cm.
(a)
[1]
(b)
Fig. 2Micrograph of shell mold/metal interface. (a) Optical, vertical lines
indicate width of alpha case region; and (b) backscattered SEM. The arrow
indicates the thin single-phase alpha region found at the surface. The alpha
plate structure with residual beta phase (light) is seen further from the mold.
7.5-cm-Wide Arm
Step Thickness
(cm)
Inside
(cm)
Outside
(cm)
Inside
(cm)
Outside
(cm)
0.64
1.3
1.9
2.5
3.2
3.8
0.038
0.056
0.074
0.084
0.081
0.086
0.023
0.066
0.066
0.081
0.076
0.089
0.028
0.058
0.081
0.091
0.107
0.104
0.03
0.064
0.081
0.091
0.107
0.102
[2]
Fig. 3Plots of measured oxygen content (circles and solid lines) and microhardness (crosses and dashed lines) vs distance and corresponding micrographs
for three different step widths: (a) and (b) 0.6 cm, (c) and (d ) 1.3 cm, and (e) and ( f ) 3.2 cm. The solid lines are fits to the data using an error function.
The vertical lines indicate the extent of alpha case, as determined by optical metallography.
1 2
C
5
D
t
x
x
cm
cm
cm
cm
cm
cm
(exp)
(exp)
(exp)
(erf)
(erf)
(erf)
9.5
7.7
5.3
8.5
7.3
5.0
6
6
6
6
6
6
0.4
0.3
0.5
0.4
0.3
0.4
0.22
0.20
0.19
0.29
0.30
0.29
6
6
6
6
6
6
0.08
0.12
0.17
0.09
0.12
0.16
0.0036
0.0090
0.0197
0.0065
0.0156
0.0322
6.4
6.4
5.4
3.5
3.7
3.3
C*
0.24
0.21
0.21
0.29
0.30
0.29
Next, solidification begins at the mold wall with the formation of a layer of the beta phase according to the TiAl-V phase diagram. This layer quickly thickens at a rate
controlled by heat flow. The much slower oxygen penetration
is controlled by solid diffusion in the beta phase. As solidification is completed and the casting cools, an oxygen concentration profile will develop in the beta phase. The calculations shown subsequently reveal that the oxygen profile in
the beta phase is essentially fixed by the time the beta transus
temperature (b/a 1 b phase diagram boundary) is reached.
This is due to the strong temperature dependence of the
diffusion coefficient.
With continued cooling, the metal temperature will drop
below the beta transus temperature. Because oxygen is an
alpha stabilizer, the beta transus temperature increases with
increasing oxygen content. Thus, the alpha phase will first
nucleate near the mold surface and grow inward to form the
thin single-phase alpha layer seen in Figure 2(b). This kind
of growth requires diffusion through an ever thickening alpha
layer and is quite slow.[5]
As the temperature continues to fall, interior points will
drop below their local beta transus temperatures (i.e., become
supersaturated), and a microstructure of alpha platelets in a
beta matrix are observed. This type of alpha transition
requires only a local redistribution of the O, Al, and V and
retains beta between the alpha plates. Near the mold surface,
the plates grow at a higher temperature and produce a coarse
structure. Farther from the interface, where the local beta
transus temperature is lower, the alpha plate size is finer.
Thus, the alpha case microstructure is primarily governed
by the oxygen profile existing in the beta phase prior to
alpha formation.
Rather than treating these events in detail, we propose a
simple model that computes only the oxygen concentration
profile that is established near the mold surface in the beta
phase. The short-range diffusion of oxygen and other elements that is required to form the platelet structure of the
alpha phase from the beta phase is not modeled. Beta grain
boundary diffusion has also not been included. It does not
seem reasonable that grain boundary diffusion should be
significant compared to bulk diffusion for the high-temperature diffusion of an interstitial element.
V. DIFFUSION MODEL
We consider the one-dimensional penetration of oxygen
into the beta phase with a fixed concentration of oxygen at
the metal surface. We define a coordinate system such that
x 5 0 is the outer edge of the metal and x 5 ` is the interior
of the sample. The concentration of oxygen in the beta phase
is denoted by C(x, t) and satisfies the diffusion equation
METALLURGICAL AND MATERIALS TRANSACTIONS B
[3]
[4]
C(`, t) 5 C`
[5]
[6]
If the boundary concentrations and the diffusion coefficients are constant (e.g., isothermal diffusion), there is a
well-known similarity solution for which isoconcentrates
move with the square root of time. The solution satisfying
the boundary conditions is
C 5 C0 2 (C0 2 C`) erf (x/!4Dt)
[7]
t5
e D(T(t8))dt8
[8]
Here, we have neglected the spatial variation of the temperature, which should be small over the thickness of the alpha
case. If we assume the usual temperature dependence for
the diffusion coefficient,
D 5 D0 exp (2Q/RT )
[9]
then
t
t 5 D0
e exp (2Q/RT(t8))dt8
[10]
[11]
C* 2 C`
C0 2 C`
[12]
Source
[W13]
[R61]
[C33]
[R40b] (Ti-6Al-4V/Air)
1 RT 2
DGf
[13]
[14]
1.6
3.14 3 104
8.3 3 1022
388
Q (KJ/mole)
201.7
287.4
130
249
(a)
(b)
Fig. 6(a) Calculated temperature vs time curves in the metal at the
surface of the different steps from the 7.5-cm-wide section. The curves
were obtained from a ProCAST simulation. (b) Predicted alpha-case thicknesses vs time at the same positions using D0 5 388 cm2/s, Q 5 249 KJ/
mole, and l 5 1.567 and beginning the integration at the solidus temperature
of 1868 K. In (a) and (b), the curves for individual casting locations (nodes)
are in the same order from top to bottom.
growth of the alpha case thicknesses for the various positions from the 7.5 cm section using the diffusion value
for [R40b] and for l 5 1.57 are given in Figure 6(b). It
can be seen that the alpha case thickness changes little
after the temperature reaches about 1422 K. Thus, the
alpha case thickness is essentially determined at a temperature well above the beta transus temperature (,996 K)
of the bulk alloy composition.
VOLUME 31B, DECEMBER 20001425
(a)
(b)
Fig. 7(a) Plots of measured vs predicted alpha-case thickness using l
5 1.567 and the [W13] and [R40b] diffusion data. Linear fits are shown.
(b) Plot of measured vs predicted alpha-case thickness using l 5 1.567
and the [C33] diffusion data. A linear fit is shown.
VII. DISCUSSION
A. Comparison of Measured and Predicted Alpha
Case Thicknesses
A comparison of measured and predicted alpha case thicknesses using two different values for the diffusion coefficient
is shown in Figure 7(a). Shown are linear fits to the relationship between measured vs predicted thicknesses, which suggest significant credibility of the chosen alpha case model.
While the fits have intercepts near zero, use of the [W13]
diffusion data gives predictions that are too small by about
a factor of 1.6, and the predictions using the [R40b] diffusion
data are too large by about a factor of 2. We note no systematic difference for the quality of the fit for the data from the
3.8-cm-thick section vs the 7.5 cm thick section.
The other two sets of diffusion data, [C33] and [R61],
give poorer results. Figure 7(b) shows the results using the
diffusion data of [C33]. The intercept is far from zero and
the use of this diffusion data with this simple model appears
invalid. The [R61] data gives predicted alpha case thicknesses 5 times larger than the measured values. It is interesting to note that the effect of decreasing the value of Q is to
shift the y intercept to more negative numbers. These two
diffusion data sets, [C33] and [R61], will not be considered further.
Fitting the data of Figure 7(a) with the function, measured
5 constant * (predicted)n, gave exponents of 1.05 and 1.14
for the [R40b] and [W13] diffusion data, respectively. Thus,
it appears that the use of the [R40b] activation energy gives
1426VOLUME 31B, DECEMBER 2000