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Surface Tension and Viscosity of Industrial

Alloys from Parabolic Flight Experiments Results of the ThermoLab Project
ARTICLE in MICROGRAVITY - SCIENCE AND TECHNOLOGY FEBRUARY 2005
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R. Wunderlich, R. Aune, L. Battezati, R. Brooks et al: Surface Tension and Viscosity of Industrial Alloy - the ThermoLab Project

Ragnhild Aune1, Livio Battezzati2, Rob Brooks3, Ivan Egry4, Hans-Jrg Fecht5, Jean-Paul
Garandet6, Ken C. Mills7, Alberto Passerone8, Peter N. Quested3, Enrica Ricci8, Stephan
Schneider4, Seshadri Seetharaman1, Rainer K. Wunderlich5, Bernard Vinet6

Surface Tension and Viscosity of Industrial

Alloys from Parabolic Flight Experiments
Results of the ThermoLab Project
The surface tension and the viscosity of a series of industrial
alloys have been measured by the oscillating drop technique
with an electromagnetic levitation device under reduced gravity
conditions in several parabolic flights. It was demonstrated that
the 20 seconds of reduced gravity available in a parabola were
sufficient for melting, heating into the liquid phase, and cooling
to solidification of typically 7 mm diameter metallic specimen.
The surface tension and the viscosity were obtained from the frequency and the damping time constant of the oscillation which
were evaluated from the temperature signal of a highresolution
pyrometer. Alloys processed included steels, Ni-based superalloys, and Ti-alloys which were supplied by industrial partners to
the project. Three to four parabolas were sufficient to obtain the
surface tension and the viscosity over a large range in temperature.

Authors:
1

2
3

5
6
7
8

Department of Materials Science and Engineering,

Royal Institute of Technology, Stockholm, Sweden
Universit degli Studi di Torino, Torino, Italy
Materials Centre, National Physical Laboratory,
Teddington, United Kingdom
ZEUS (Zentrum fr Erstarrung Unterkhlter Schmelzen)
at DLR, Cologne, Germany
Materials Division, University of Ulm, Ulm, Germany
Department of Materials, Imperial College STM, London, United Kingdom
IENI-CNR Ge, Genoa, Italy
Dpartement des Technologies pour les Engergies Nouvelles,
CEA/DTEN, Grenoble, France

Mail Address:
Rainer K. Wunderlich, Materials Division, University of Ulm,
Albert-Einstein-Allee 47, 89081 Ulm, Germany

Z-Tec Publishing, Bremen Microgravity sci. technol. XVI

INTRODUCTION
The numerical simulation of casting and microstructure formation is used increasingly by industry [1] for the optimization of
casting and the improvement of product quality. Models
describing fluid and heat flow are combined with thermodynamic models of nucleation and growth kinetics, phase selection, and phase stability in the solid phase [2]. The increasing
sophistication of numerical simulation is, however, met by a
pronounced lack of thermophysical property data which is owed
to the high chemical reactivity of many metallic alloys in the
liquid phase. As a consequence, for many high-temperature
alloys conventional thermoanalytical techniques where the
specimen is in contact with a container are difficult to apply and
fraught with error. In order to overcome these limitations, containerless methods for thermophysical property measurements
have been developed and applied under reduced-gravity conditions [3, 4].
Knowledge of the surface tension is relevant for the prediction of defects such as gas porosity, the contribution of
Marangoni convection to fluid transport, and for an estimate of
the effect of liquid - mould interaction. The viscosity is relevant
for the calculation of the convective contribution to heat transfer, for simulations of mould filling and, in general, for all
processes involving moving fluid. The experiments to be
described were conducted within the framework of the
ThermoLab project which was initiated to provide thermophysical property values of industrial alloys by the application of
containerless processing under reduced gravity conditions and
in ground-based laboratory including also conventional techniques.
EXPERIMENTAL PROGRAMME
The alloy selection was mainly driven by the industrial user
group of the ThermoLab project. While for the Ni-based alloys
measurements of the surface tension and of the viscosity could
also be performed by the sessile drop and the oscillating cup
method in ground-based laboratory, this was not possible for the
11

R. Wunderlich, R. Aune, L. Battezati, R. Brooks et al: Surface Tension and Viscosity of Industrial Alloy - the ThermoLab Project

Alloy

T1 / C

Flight

Ti6Al4V

1655

Oct 2001

Ti 6242

1705

Oct. 2002

-TiAl

1566

June 2003

CMSX-4

1382

Oct. 2002

IN738LC

1345

June 2003

MM247LC

1368

June 2003

C263

1355

June 2003

low alloyed steel

1480

June 2003

cast iron

1367

June 2003

Table 1. Overview of the alloys processed on parabolic flights for the

measurement of the surface tension and the viscosity.

Ti-alloys because of their high melting temperatures and high

chemical reactivity in the liquid phase. In Table 1, an overview
of the specimen processed on the parabolic flights is shown. The
Ti6242 alloy is a variant of the Ti6Al4V alloy with an addition
of Zr and W in the few per cent range. In order to investigate the
influence of the oxygen concentration, a Ni-based superalloy
and a Ti-alloy with different oxygen concentrations were
processed.
EXPERIMENTAL SET-UP AND
SAMPLE PREPARATION
The parabolic flight experiments were performed on board an
Airbus A320. The experimental set-up on the parabolic flights
was similar to that of the containerless electromagnetic processing facility TEMPUS which has been used in the IML-2 and
MSL-1 Spacelab experiments for the measurement of thermophysical properties of liquid metals and alloys [3,4]. The specimen were contained in an ultra-high vacuum compatible vessel.
Positioning was by a radio-frequency quadrupole field and heating by a dipole field of frequencies 240 kHz and 340 kHz,

respectively. The temperature was measured by an optical

pyrometer in the top position which was calibrated at the liquidus temperature obtained from high temperature calorimetry,
for the Ti 6-4 and Ti 6-242 alloys values provided by the industrial partner have been used. The pyrometer had a sampling rate
of 100 Hz, and a temperature resolution of 0.02 K. The specimen shape was recorded by two 100 Hz video cameras in the
side and the top view position. The experimental chamber was
operated under flowing or static argon and a He-Ar mixture.
The 7 mm diameter specimen were contained either in an open
cage structure, or in a cup with observation slits from the side
on a SiN pedestal.
Specimen were polished and stored in a glove box with highpurity argon. The oxygen concentration of representative specimen and of the processed samples was analyzed with the LECO
hot gas extraction method. The influence of oxygen on the surface tension and the viscosity was investigated for a CMSX-4
Ni-based superalloy and a Ti6Al4V specimen. Specimen with
different oxygen concentrations were prepared by re-melting in
an arc melter either with or without using additional Ti-getter.
Typical oxygen concentrations of the low and high oxygen concentration specimen were 50 ppm and 350 ppm, and 1450 ppm
and 1720 ppm for the CMSX-4 and Ti6Al4V specimen, respectively.
PROCESSING
The parabolic flights provided approx. 20 seconds of reduced
gravity (-g). Specimen were preheated to approx. 1000C
under an atmosphere of 20 mbar argon. At the onset of the -g
phase when the specimen was freely suspended, the heating
field was turned on. After having reached maximum temperature, the chamber was flooded with about 300 mbar of high
purity helium to increase the cooling rate which was in the
range of 60Ks-1 to 25Ks-1. A typical processing sequence of a Ti6-4 alloy is shown in Figure 1 with melting (1), heating to maximum temperature (2), free cooling with application of surface
excitation pulses (3), and undercooling and recalescence (4). In
this way, the surface tension could be obtained over a large
range in temperature from a single parabola. Three to four
parabolas were sufficient to obtain the surface tension and viscosity values. All Ti-alloys processed on the parabolic flights
exhibited an undercooling of about 300K with the Ti6Al4V
alloys undercooling close to the hypercooling limit. For the Tialloys, the undercooling was independent of the oxygen content. The Ni-based superalloys undercooled typically by 90100K.
DATA EVALUATION

Fig.1. Temperature-time profile of a Ti6Al4V specimen shown on the

left hand ordinate, heater current shown on the right hand ordinate.

12

For a force free, spherical droplet of mass the surface tension,

, is obtained from the frequency, , of the l=2 mode of the surface oscillations by the Raleigh formula:
=

3/8

2
Microgravity sci. technol. XVI-1 (2005)

R. Wunderlich, R. Aune, L. Battezati, R. Brooks et al: Surface Tension and Viscosity of Industrial Alloy - the ThermoLab Project

Higher oscillation modes are usually not observed because of

their much stronger damping. The viscosity, , is obtained from
the damping time constant, , of the surface oscillations according to:

3/(20) (/R) 1

Two methods are available for the evaluation of the oscillation

frequency and damping time constant. In digital image analysis,
the video recordings of the specimen shape are analyzed. This
method requires a rather high software and digital processing
effort [5]. Alternatively, the surface oscillations can be evaluated from the high-frequency modulation of the temperature signal [6] originating from the variation of the surface normal with
respect to the optical axis of the pyrometer and from the variation of the surface position with respect to focal plane of the
pyrometer. This approach has the advantage of being fast and
easy to apply. It is, however, more susceptible to sample movements which result in an additional amplitude modulation of the
pyrometer signal appearing as sidebands in the Fourier spectrum and beat oscillations which can impede the evaluation of
the damping time constant. The results presented here have
been obtained with the temperature analysis method. In Figure
2a,b the high frequency oscillations of the temperature signal
extracted by Fourier filtering and the corresponding Fourier
spectrum are shown. The sidebands are symmetric, and split by
the frequency of the sample movements. A further splitting in
the main peak is not resolved because of the small sampling
time interval.

is observed with results obtained in ground-based laboratories

with the sessile drop method. In Figure 4, Arrhenius plots of the
viscosity of the high and low oxygen CMSX-4 alloys obtained
from the parabolic flight are shown. A significant increase in the
viscosity of the high-oxygen specimen is apparent. No comparable data have been found in the literature. For applications in
casting simulations, the lower viscosity data are recommended
because this oxygen concentration is closer to that of the industrial alloys. The results show that the oxygen concentration is a
critical parameter in viscosity measurements for these alloys.
(T1)/ Nm-1

d/dT

Source

IN738LC

1.85

-1.48 10-3

PF June 2003

MM247LC

1.86

-1.36 10-3

PF June 2003

C263

1.74

-0.69 10-3

PF June 2003

CMSX-4 low ox.

1.78

-1.28 10-3

PF Oct. 2002

CMSX-4 high ox.

1.75

-1.80 10

-3

PF Oct. 2002

CMSX-4

1.97

-1.38 10

-3

sessile drop 1-g

CMSX-4

1.83

-1.45 10

-3

sessile drop 1-g

Alloy

Table 2. Surface tension at Tl and temperature coefficient of Nibased superalloys. The two bottom rows show values obtained in the
ground-based programme.

RESULTS
Ni-based superalloys
As a typical result for the Ni-based superalloys, the surface tension as a function of temperature of the alloy MM247LC is
shown in Figure 5. The data exhibit low scatter and can be very
well fit by a linear regression. The results were compiled from
4 parabolas. In Table 2, a compilation of the surface tension of
the Ni-based superalloys obtained on the parabolic flights is
shown. For CMSX-4, very good agreement of (Tl) and d/dT

Fig.3. Surface tension as a function of temperature of the Ni-based

alloy MM247LC results from three parabolas indicated by , and .

Fig.2a. High frequency component of the temperature signal shown on the left hand side; 2b. Fourier spectrum of a 0.64 s time slice

Microgravity sci. technol. XVI-1 (2005)

13

R. Wunderlich, R. Aune, L. Battezati, R. Brooks et al: Surface Tension and Viscosity of Industrial Alloy - the ThermoLab Project

(T1)/ Nm-1

d/dT

Ti6Al4V

1.52

-5.52 10-4

PF Nov. 2001

Ti6Al4V

1.49

-4.10 10

-4

PF Oct. 2002

Ti6Al4V

1.52

-4.50 10

-3

PF Oct. 2002

Ti-6-242

1.51

-8.73 10

PF Oct. 2002

Ti6Al4V

1.52

n.a

pendant drop 1-g

Alloy

Source

-3

Table 3. Surface tension at Tl and temperature coefficient of Ni- ased

superalloys. The two bottom rows show values obtained in the
ground-based programme.
Alloy

T / C

h / mPa.s

Ti64

1824 +/- 100

3.92

Ti64

1670 +/- 80

4.82

Ti6242

1740 +/- 100

3.70

Ti6242

1626 +/- 80

4.76

Table 4. Viscosity of TiAlV alloys.

) and high

Fig.4. CMSX-4; Arrhenius plot of the viscosity of the low (

() oxygen alloy.

Fig.5. Ti6Al4V, surface tension as a function of temperature.

14

Ti-alloys
As an example of the quality of the data obtained in the parabolic flights for the Ti-alloys the surface tension as a function of
temperature of Ti6Al4V is shown in Figure 5. Very good agreement with a value obtained by the pendant drop technique at the
liquidus temperature, i.e., (Tl) = 1.52 Nm-1, was obtained giving support to the results of the parabolic flights where no comparison values over a large range in temperature are available
from other techniques. Moreover, a reproducibility of the surface tension at Tl of better 1 % was obtained in data obtained
from two different parabolic flights and with specimen of different diameter as shown in Table 3. Viscosity values for the TiAl-V alloys obtained on the parabolic flights are given in Table
4.
CONCLUSIONS
Parabolic flights were proved as a valuable tool for the measurement of the surface tension and the viscosity of high melting
point industrial alloys. Measurements are carried out almost
routinely and a large amount of property values has been
acquired. A very good reproducibility of surface tension values
for Ti-alloys were obtained on different parabolic flights. It
could be shown that electromagnetic processing conditions had
no effect on the surface tension values. Further improvements
may be expected from an optimization of the temperature-time
profiles for viscosity measurements which will, however,
require a larger number of parabolas to cover the same temperature range as for the surface tension measurements.
ACKNOWLEDGEMENTS
This work was supported by the European Space Agency (ESA)
Microgravity Applications Support Programme (MAP) under
contract number AO-99-022 (14306/01/NL/SH) and by the
German Aerospace Center (DLR) under contract number 50
WM 0041. The parabolic flight opportunities were provided by
DLR and ESA. Support from the facility developer EADS
Space Systems and the Microgravity User Support Center at
DLR Cologne is gratefully acknowledged.
REFERENCES
[1] Dantzig, J. A.: Solidification Modeling: Status and Outlook, JOM, vol. 52,
no. 12, p. 18 (2000).
[2] Saunders, N., in: Superalloys 1996. Kissenger, R. D. et al. (Eds.), TMS,
Warrendale, Pennsylvania, p. 101 (1996).
[3] Egry, I., Lohfer, G., Jacobs, G.: Surface Tension of Liquid Metals:
Results from Measurements on Ground and in Space, Phys. Rev. Letters,
vol. 75, p. 4043 (1995).
[4] Wunderlich, R. K., Fecht, H.-J.: Thermophysical Properties of Bulk
Metallic Glass Forming Alloys in the Stable and Undercooled Liquid
A Microgravity Investigation, J. Mat. Trans. JIM, vol. 42, no. 4, p. 565
(2001).
[5] Egry, I., Jacobs, G., Schwartz, E., Szekely, J.: Surface Tension
Measurements of Metallic Melts under Micro-Gravity, Int. J.
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[6] Rsner-Kuhn, M., Hofmeister, W. H., Kuppermann, G., Morton, C. W.,
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Warrendale, Pennsylvania, p. 33 (1999).

Microgravity sci. technol. XVI-1 (2005)