VISCOSITY OF MOLTEN AI-21.

5% Si
UDC 541.1:532.13:669.715

V. Z. Kisun'ko, A. I. Pogorelov,
A . V. Mazur, I. A. Novokhatskii,
and V. I. Mazur

The problem of structural changes in molten metals has recently come into controversy
[i-5].
This is connected mainly with procedural difficulties [6-11] and uncertainties of a
metrological character [12-14] in using nonstandard ways of measuring the structure-sensitive
properties of melts.
Of particular importance is determination of the possibility of structural transformations of the polymorphic type in aluminum and its alloys [5, 15-22].
The
aim of this work is a study of structural changes in liquid eutectic alloy AI-21.5% Si from the
results of its change in kinematic viscosity v.
Viscosity was calculated by the successive approximation method (to the sixth approximation including the zero approximation) using the equations of Shvidkovskii [6] for values of
parameters determined by experiment, i.e., the decrement of freely damped torsional vibrations
of a crucible with a melt A0/A n and the period of vibrations ~(m)" The number of parameters
Observed in this way was N l = 14...28 and N 2 = i0 for A0/A n and ~(m) respectively.

Vibration

amplitude was measured from a flat scale 500 mm long with a scale division of 1 mm, and the
vibration period was measured by a timer with an instrument error A~ = +_ 0.05 sec with the
number of vibrations for the series m = i0.
Experiments were carried out in a viscosimeter [23] in strict accordance with the recommendations given in [6-11, 23].
The viscosimeter included two supporting structures consisting of clamps, a tungsten wire (0.12 mm in diameter and about 500 mm long), a holder for
a mirror, a molybdenum rod 3 mm in diameter, and a titanium lid over the crucible.
Two types
of crucible were used, i.e., of aluminum oxide AI203 and beryllia BeO, 50 mm high of strictly
cylindrical shape with zero porosity, which corresponded to the specifications in [9]. Vibration period ~ for the supporting structure was specified as ~>9.4 sec with a BeO crucible
and T _>11.5 sec with an AI203 crucible (i.e., a limit of > 7 sec from [7] was observed).
The internal radius of crucible made of AI203 was R ~ 1.35 and R m 1.15 cm, respectively, which
with a specimen height of H = 30-35 mm corresponded to conditions 2~R2/Tv _> i00, H > 1.85 [6]
and R_> i.i cm [8].
The relative error in determining
1

Ao

-~-m~-~

depends

logarithmic decrements of torsional vibrations

6 =

[6] mainly on instrument error for determining the final amplitude A n and

ratio A0/A n . In order to obtain the minimum relative error observations were previously
collected for number of vibrations n in the series (for the supporting structure with a beryllium oxide crucible n = 7 and for aluminum oxide n = 6).
Before measurements the size of the isothermal zone in the device was determined. Special screens made it possible to obtain a working zone of length Z -~ 60 mm with a temperature
gradient over the height of the crucible not more than +_ 2.5C.
Temperature was measured by
a Chromel-Alumel thermocouple in a class 0.05 PP-63 instrument.
Parameters of the freely damped vibrations of the system without metal ("no load system")
were determined through 50-60C over the whole temperature range for viscosity measurements.
In this way the value t 0 was calculated (average for five parallel observations of the vibration period with number of vibrations in the series z = I00) and also 60 (average of ten
;

A 0

parallel observations of logarithmic decrement 6 o =-~-;n~-~

with a number of vibrations

Dnepropetrovsk Metallurgical Institute.

Translated from Metallovedenie
Obrabotka Metallov, No. 9, pp. 30-35, September, 1987.

0026-06'73/87/0910-0675512.50

in

i Termicheskaya

1988 Plenum Publishing Corporation

675

the series n = 23). The graphical dependences obtained t 0 = f(t) and 80 = f(t) made it possible to determine values of t 0 and 80 at each measurement temperature for entering these
values in the calculation equation, although it is assumed in [6] that accurate values of
them are not required since the term in the equation which contains them is normally small
compared with 8.
It is known [24] that at about 725C reaction of aluminum with oxygen proceeds with a
negligibly small partial pressure of oxygen po 2 = 4.4.10 -4 Pa, which within the viscosimeter
is almost impossible to maintain. A study was made in [25] of the thermodynamics of the reactions in the system AI-O taking account of the possibility of stable existence of readilyvolatile lower aluminum oxides (AI20, AIO). Also given was a diagram for the dependence of
log po 2 on temperature plotted from equations for log PO~ obtained from equations for formation reactions of the corresponding oxides. It was established that at a point with coordinates 2240K and log po 2 = -14.87 the system AI-O is invariant, Below 2240K, Al2Ogas is unstable, and equilibrium shifts in the directions of AI203 formation. Up to 2716.5K this is
also valid in relation to oxide AIO. Thus, close to tm = II00C it is possible to retain
in the gas phase of the working zone a limitingly low stable content of oxygen. Control of
gas phase purity, and also the flowing (3 liter/h) high purity gas used b~ us, i.e., helium
(supplied in a unit previously evacuated to I0-i00 Pa from above), provides an oxygen content in accordance with the recommendations in [i0, 26]. As special tests have shown in the
gas phase the viscosimeter working volume POe = 10-?-10-8 Pa is maintained. On one hand this
provides a low rate of oxidation for the bul~ of the metal, and on the other hand application of a solid and stable oxide film on the surface of the melt, serving as a second end to
the contact surface, which is taken into account in calculating viscosity by the equations
in [6]. Before determination the melt was overheated by 40-50C above the first required
temperature for observation and held for 1.5-2 h. Achievement of equilibrium in the oxide
(crucible)-melt-gas (oxygen of the gas phase) system was recorded by the absence of disturbances of the supporting device and cessation of displacements of the zero line. Vibration
amplitude and period were determined according to data in [i0, ii, 23] in a cooling regime
with fixed temperatures through each 7-120C after holding for 30-40 min.
Studies were carried out on specimens weighing 30-40 g of alloy AI-21.5% Si which was
obtained from specially pure aluminum grade A999 and single-crystal silicon. The results
of measuring A0/An, ~m, ~ and log ~ in the temperature range 725-I050C are presented in Fig.
i.
In accordance with data in [13, 14] an estimate was made by us of the random measurement error for torsional vibration decrement and period, viscosity and its logarithm in the
region of anomalies for their polytherms. Calculations were carried out for neighboring tem-

.4o/A5

~.1o~~/~,~

31

Z,35

T,o,c ,,~.

# ?,

_ .~r

'

0,,3.~

~ ?00 BOO 900 -1000t,C

%0
a

A&

r,o,c .~.

76,B5

~0

~O(l/t).so ~"

~.~o~, :/seo

'

zg(~.~o~)

0.4=3

?00 800 900 lO00t,C ' %0

~0

~O(#/t).~ ~

b:

Fig. i. Temperature dependence for liquid alloy AI - 21.5% Si

parameters in a crucible made of AI203 (a) and BeO (b): decrement of freely damped torsional vibrations A0/An, period of
torsional vibrations ~ 0 ; kinematic viscosity v and logarithm
of kinematic viscosity log v.

676

peratures which with graphical plotting of polytherms and their prior analysis on semilogarithmic coordinates relate to different temperature regions.
Given in Table 1 are values of
average square deviation for the results of observing S and two-way probabilities for the
ranges of random errors of measured results ( 5x) for A0/An, ~m, v and log v calculated by
equations in [13].
In addition, in accordance with data in [14] coefficients of variation were calculated:
W x is for an estimate of the random error of measuring A0/An, Zm, v and log v (with a corresponding number of observations for a given temperature) and W n is for estimating the error
of the observation method used by us for these values.
Values of W x and W n calculated for
ten limiting temperatures in the range of anomalies are also given in Table i. The average
value of W n may be taken as that characterizing the error for the oxidation methods used and
calculation of torsional vibration decrement, vibration period, viscosity and values of its
logarithm.
Normally the sensitivity of the device to changes in viscosity may be determined a priori from the equation K = 0.5 6 [6]. This does not take account of the effect upon instrument sensitivity of temperature changes for values of z, z0, and 60, and also the contribution to measurement errors of specimen height as a result of its volumetric expansion.
This
approach to estimating instrument sensitivity requires in each specific case experimental
verification and metrological analysis.
It follows from Table 1 that the error for the result of direct viscosity measurements according to the procedure recommended by us is g o v erned mainly by the error of torsional vibration determination for the crucible with the
melt.
The contribution of errors in determining z to the overall error of calculation v by
successive approximation according to equations in [6] is small, since the error of the observation method T(m ) is an order of magnitude less than the error for the observation method
for vibration amplitude (Table i). This will be all the more valid in relation to errors of
determining 60, t0, and H. Consequently, an estimate of viscosimeter sensitivity to temperature changes may in fact be carried out to a first approximation proceeding from errors
for determining the vibration amplitude for the crucible with the melt, which is quite small,
i.e., it is characterized by instrument error.
However, a stricter metrological estimate
of instrument sensitivity to viscosity changes is impossible without statistical treatment
of the observed results similar to that carried out by us (Table I). In addition, on the
TABLE 1

I
, "

XVx

~.V?t

Crucibl, of Ai203

Index
t, =C

Ao/A,

y'107, i
I
sec~'' lrn2/~ec}":
(v-lO,)

788
796
914
924
963
972,5
1008
1014

0,026
0,024
0,021
0,023
0,017
0,027
0,017
0,018

0,050
0,050
0,050
0,050
0,050
0,050
0,050

0,048
0,046
0,039
0,042
0,031
0,048
0,030

0,007
0,007
0,007
0,007
0,005
0,009
0,005
0,006

788
796
914
963
972,5
1008
1014

0,010
0,010
0,010
0,010
0,010
0,011
0,010
0,010

0,034
0,034
0,034
0,034
0,034
0,034
0,034
0,034

0,028
0,027
0,023
0,024
0,018
0,019
0,017
0,019

788
796
914
924
963
972,5
1008
1014

0,19
0,19
0,16
0,16
0,13
0,15
0,13
0,13

0,013
0,013
0,013
0,013
0,013
0,0t3
0,0t3
0,018

0,46
0,42
0,41
0,43
0.34
0,36
0,33

924

788
796
914
924
963
972,5
1008,0
1014,0

Average

0,75
0,69
0,64
0,68
0,53
0,83
0,52
0,55
0,65

0,050

0,04
0,04
0,04
0,04
0,04
0,04
0,04
0,04
0,04

0,032

AJA,

~,,sec

768,0
775,5
820,5
829,0
970,0
980,5
1005,0
I013,5

0,020
0,032
0,017
0,022
0,023
0,019
0,014
0,020

0,050
0,050
0,050
0,050
0,050
0,050
0,050
0,050

0,055
0,089
0,047
0.057
0,055
0,049
0,037
0,05~

0,007
0,011
0,007
0,008
0,011
0,006
0,006
0,009

0,0041
0,0041
0,0041
0,0041
0,0029
0,0035
O,O02g

768,0
775,5
870,5
879,0
970,0
980,5
1005,0
1013,5

0,012[
0,008 I
0,011 [
0,009[
0,013 I
0,010 I
O,Ol2
0,012

0,034
0,034
0,034
0,034
0,034
0,034
0,034
0,034

0,032
0.021
0,028
0,02]
0,034
0,027
0,035
0,032

0,0052
0,0035
0,0035
O,O04&
0,0048
0,0041
0,0043
0,0041

0,44
0,38
0,44
0,44
0,38
0,40
0,37

768,0
775,5
870,5
879,0
970,0
980,5
I005,0
I013,5

0,16
0,I9
0,16
0,19
0,15
0,16
0,13
0,19

0,016
0,016
0,016
0,016
0,016
0,010
0,016
0.016

0.40
0,49
0,40
0,49
0,35
0.44
0,35
0,48

0,33
0,40
0,35
0,41
0,44
0,35
0,34
0,50

768,0
0.61
775.5
1,01
870 5 0,57
879,0
0,70
970,0
0,78
980,5
0.63
1005,0
0,48
1013 5 0,65
I A v e r a g e i 0,68

0,050
0,050
0,050
0.050

],50
2,6C
t.50
1.77

0,0035

0,35

Cm:cibleof BeO

0,38

t,

I g (v. ! 07)

1,71
1,56
1,54
1,60
t,26
1,90
1,25
1.30
1,52

11,65
t 1,45
1,63
1,66
1,41
2,10
1,39
1,42
1,59

0,050
0,05
0,05
0,05

0,05

1,87
1,66
t.50

.l,SO

1 ,75

1,25

2,10
1,30
1.49
2.30
1,29

1,26
I ,8&

t,61

677

basis of data in Table 1 and Fig. 1 it is possible to conclude that with ~ > i0 sec the instrument error is 0.5 sec, the number of vibrations in the series m ~ i0, the number of parallel
observations N 2 ~ I0, results of measuring the vibration period for the crucible with the
melt may be used as an additional method for determining the temperature at which there are
structural changes in the melt.
An analysis was also carried out for the reliability of presenting polytherms A0/A n =
f(t), T = f(i), ~ = f(t) and log ~ = f(I/T) with disruption of functional relationships.
According to data in [13, 14[ the solution of this problem is reduced to clarifying the
fitting of boundary points in the region o ~ an anomaly to one or different collections of
parallel measurement results. Calculations carried out taking account of recommendations in
[13, 14] showed that with a confidence level x = 0.995...0.999 there is a jumpwise change in
torsional vibration decrement and period, and also viscosity and its logarithm. Reliability
ranges of boundary values A0/An, ~m, ~ and log v were referred to average values of temperature
obtained with two-way graphical linear extrapolation of function log v = f(i/T) into the region
of the anomaly (see Fig. i). Given in Table 2 are the temperatures of structural transformation (ts. t) in molten AI - 21.5% Si, and also values of preexponential constant multiple
A and activation energy for viscous flow E~ of the melt in temperature ranges in which viscosity changes in accordance with the equation v = A exp (Ev/RT).
Breaks and extremes in the polytherms for viscosity observed previously for aluminum and
AI-Si alloys [27-31] are a consequence of distortion of the true picture for development of
structural transformations due to marked temperature steps for measurements (20-30C), and
also disruption of system (melt-oxide film-crucible-gas phase) stability caused by work in
the heating schedule and not in the cooling schedule. The amount of these disturbances and
distortions increases as temperature increases, and with a changeover through each new structural transformation.
The results obtained in the present work (Table 2 and Fig. i) made it possible to detail
a picture [30] for development of structural transformations in hypereutectic silumin. Results of measuring viscosity with high sensitivity over a wide temperature range in a cooling
regime through small temperature intervals (not more than 12C) indicated that with the temperatures studied (from 700C and above), apart from a small general reduction in absolute
values for viscosity of liquid alloys, there are four structural transformations. For all
of these four transformations a jumpwise change in viscosity is typical, and for different
types of crucible the temperature of the first two transformations (from the cooling path
for the melt) coincide, but the other two differ by 20 and 40C.
Addition confirmation of the idea of jumpwise structural rebuilding in the melt studied
may be the jumpwise change in activation energy of their viscous flow E v at ts. t. With an
increase in ts. t the E~ increases (Table 2). This tendency can be followed particularly clearly
TABLE 2
C~cible
material

[S,t

Temperature range,
,of

795

725...795

0,48

3750
1

Al2Os

915

795...915

9,63

3300

970

915...970

0,45

4300

970...1010

0,45

4250

1010...1060

0,41

4600

725...775

2.85

450

775...875

1,15

2250

875

875...975

0,91

2900

975

975...I010

0,28

5950

IOlO

I010...I045

0,24

6400

1010

775

BeO

678

for a melt cooled in a BeO crucible which is recommended by the authors in [9] for most precise measurements.
The difference in temperature for structural transformations in molten AI-Si placed in
AI20 ~ and BeO crucibles may apparently be explained by the effect of exchange interphase
processes in the crucible-metal boundry. In favor of this suggestion is the existence of a
marked change in the wettability of substrates made of AI20 ~ and SiC by aluminum melts recorded in [32].
X-ray study of liquid silumins of hypereutectic composition [33] showed that at least
in the range 660-700C their structure is satisfactorily described by a model involving superposition of the following structural regions: a microregion with statistically random
distribution of aluminum and silicon atoms according to type of coordination SC (r I = 0.265
nm) and bcc (r I = 0.280 nm), and microregions with a distribution of atoms for components of
the AI3Si silicide type based on fcc packing (r I = 0.306 nm). These data are confirmed by the
results of tests for quenching alloys from the liquid condition: several intermediate phases
of the silicide type form on the basis of the last structural zone [33].
On the basis of structural analysis of results it is possible to conclude that values
of t s t and t s t (for melts in a BeO crucible) coincide with the temperature for structural
trar,sformation in h q u l d aluminum determzned by the methods of viscosimetry [15] and calorimetry [22]. Thus, ts.tz and ts.t2 may be identified with high probability as the transformation temperatures in allmninum clusters.

"

By comparing the results obtained with data given in [20, 30, 34, 35] for kinematic
viscosity of AI-Si alloys, and also taking account of the nature of change in activation energy for viscous flow in different temperature ranges, it is possible to suggest that at ts.t~
there is decomposition of clusters with fcc-like packing with silicide stoichiometry.
Taking account of data in [36], the temperature of the fourth structural transformation
may be treated as the start of formation of silicon clusters with a SC-like coordination
similar to those which are detected in hypereutectic AI-Si melts [37].
CONCLUSIONS
i. It is possible to detect structural transformations in molten metals with the use of
highly accurate procedures followed by metrological evaluation of the measured results
2. At certain temperatures in liquid hypereutectic silumin there are structural transformations connected with a change in close order prameters, and also with the occurrence and
decomposition of different types of less clusters.
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3.
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6.
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