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Characterisation of rheology and stability

of DMS milled grades of ferrosilicon


Fengnian Shi
The University of Queensland, Sustainable Minerals Institute, Julius Kruttschnitt Mineral
Research Centre, 40 Isles Road, Indooroopilly, Brisbane, Qld 4068, Australia
*Email address: f.shi@uq.edu.au; Telephone: +617 3365 5913; Fax: +617 3365 5999

ABSTRACT

Ferrosilicon (FeSi) slurry rheology and stability have a significant impact on dense medium
separation efficiency. Due to the fast-settling nature of the FeSi particles of very high solid
density, it is a challenge to acquire accurate measurement of the FeSi rheological
characteristics. A testing rig including a slurry circulating system was set up, which consists
of a sump, a pump, a pneumatic stirrer, a viscosity measuring chamber and a set of valves
controlling flow rate. A Mettler RM180 rheometer with a modified bobbin-cup system was
employed to measure slurry rheological flow curves of different milled FeSi grades provided
by DMS Powders. Slurry stability at various FeSi slurry densities was determined with a
250 ml measuring cylinder. The apparent viscosities were calculated at two shear rates: 10
and 150 s-1, which are assumed to cover a typical shear rate range in dense medium drum
and dense medium cyclone operation. Relationships of the apparent viscosity and stability
as a function of slurry density and FeSi grade were established and presented in graphical
form. These graphs can be used for dense media selection, given the required separation
density and viscosity.

Keywords: Dense medium separation; Rheology; Viscosity; Medium stability.

1. Introduction
In dense medium separation, medium rheology plays an important role in separation
efficiency. A high viscosity increases particle misplacement in dense medium cyclones and
baths. It decreases the separation density in cyclones due to a reduction in the medium
differential. It can change the separation density of bath separators as well (increasing or
decreasing separation density depends on the bath feeding location).
Medium stability is another operational parameter influencing dense medium separation
efficiency. All dense media solids are inherently unstable because they have a higher
density than the liquid (water) in which they are suspended. Stability is important in
determining the behaviour of the medium in the separator. In general it is desirable to have
a stable medium to prevent strong density gradients in the separator, which usually inhibits
an efficient separation.
In a review of the effects of dense medium viscosity on separation efficiency, Napier-Munn
(1990) reported that very few studies have been undertaken on the direct effects of the
rheological properties of the medium on the separation process. This is probably because of
the experimental difficulties involved in the measurement of rheology in the process
environment, and the problems of decoupling rheology from the other process variables.
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 2

In the past decades, much effort has been devoted to attempting to address the rheology
measurement, modelling and application in mineral processing research programs
conducted at the Julius Kruttschnitt Mineral Research Centre (JKMRC). This includes the
work of Castro (1990), Masinja (1992), Napier-Munn et al. (1994), Shi (1995), Dunglison and
Napier-Munn (1995), Shi and Napier-Munn (1996a, b; 1999, 2002), Shi and Zheng (2003), Li
et al (2015), etc. One major development was to set up a testing rig at the JKMRC pilot
plant for viscosity measurement of slurries containing fast-settling particles such as coarse
minerals and ferrosilicon (FeSi) powders.
FeSi powders have wide applications in dense medium separation, particularly for the
mineral industry. In order to provide the rheological characteristic data and medium stability
information to the FeSi users, the JKMRC was commissioned by DMS Powders, the major
FeSi supplier, to conduct measurements of a number of FeSi samples to determine
rheological property and stability. This paper presents the experimental details, data
reduction methods, and the measured rheological properties and stabilities of the DMS
milled grades of FeSi.

2. Experiment

2.1. Material

DMS Powders supplied six milled FeSi samples: 270D, 150D, 100D, 65D Granular, 65D
Thos Begbie (65D TB), and 65D Mixed. The samples were delivered to the JKMRC in two
batches: Grade 270D was tested first for viscometer bobbin-cup modification. After
completion of the first stage of work, the rest of the FeSi samples were tested in a separate
project.
For the milled grades of FeSi, quartz and steel scrap are melted in a furnace with a
reductant to produce molten ferrosilicon with a silicon content around 15%. The material is
then water granulated and subsequently dried, milled and air classified into the various
grades. The milled grades 270D, 150D and 100D were manufactured using the traditional
technique. 65D Granular was made on the submerged arc furnace with higher carbon and
trace elements, thus its relative density (RD) is slightly lower. Basically, it is the same grade
as the 65D using the traditional manufacturing technique. Grade 65D TB is a milled product
that was made on induction furnace and with lower carbon and trace element but higher RD.
Grade 65D Mixed is a mixture of 50% 65D Granular with 50% 65D TB. All the three 65D
grades were milled to the similar size but with different alloys and different RDs.
Sieving analysis on the six FeSi samples was performed to determine their size distributions.
Table 1 shows the cumulative 80% passing sizes (P80) and the percentage passing 75 m
for the six received samples. These two points represent the coarse end and the fine end of
size distribution curves, respectively. The table shows a trend of increased P80 in an order
from fine to coarse: 270D, 150D, 100D to 65D, which is as expected. However, the three
65D samples exhibit differences in size, contradictory to the expectation of a similar size.

Table 1: Product sizing results of the six milled FeSi samples

270D 150D 100D 65D 65D TB 65D


Granular Mixed
P80 (m) 37.0 68 72 81 91 100
Passing 75 m (%) 98.3 98.8 85.9 74.3 64.0 41.9
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 3

2.2. Measurement of medium rheology

Dense medium slurries are inherently unstable because they are composed of a high density
fine particles dispersed in a low density phase (water), and the high density solids tend to
settle by gravity. It is therefore important to keep the FeSi particles well suspended and to
maintain consistent slurry density during rheological measurements. A test rig was set up at
the JKMRC pilot plant especially for the rheological measurement of FeSi samples (Figure
1). This is similar to the Debex on-line slurry viscometer described by Reeves (1985) and
Napier-Munn et al. (1989). The rig comprises a pump, a sump with a pneumatic stirrer, a set
of valves, a viscosity measuring chamber, and the Mettler RM180 viscometer. The RM180
is a rotational viscometer with a concentric cylinder system. The commercial sets of bobbins
and cups were found not suitable for FeSi slurry measurement: The narrow-gap system was
often blocked by the slurry; and the wide-gap system was not able to produce a torque
reading larger than the viscometer reliable reading threshold. A set of modified bobbin-cup
measuring system was fabricated with a larger bobbin diameter and knolled bobbin surface
in a cup with wide gap. The viscometer was calibrated with special silicone fluids of known
viscosities. Figure 2 shows the flow diagram in the measuring chamber, and a picture with
FeSi slurry in the measuring chamber.

RM180
Viscometer

Stirrer
Measuring
Chamber

Bob6
Sump

Measuring
Pump
Cup
kknurlle

Figure 1: FeSi rheological measurement rig


Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 4

Figure 2: Measuring chamber flow diagram (the viscometer measuring cup being
removed to show the bobbin) and the picture with FeSi slurry in the chamber

It was found that the received FeSi samples contained a small amount of coarse particles
larger than 150 microns (top size 1.18-1.4 mm). During the rheology measurement, these
coarse particles, though only less than 0.5% of the total mass, had a tendency to jam the
bobbin-cup system, or to affect FeSi slurry to flow through the gap between the bobbin and
the cup. This causes unstable torques to be recorded. A procedure to scalp the FeSi solids
at a sieve of 150 micron was therefore adopted to remove the oversize particles prior to
mixing with water.
The experiment was started with only water in the system. After the pump was warmed up,
FeSi solids were gradually added into the sump, while the pneumatic stirrer was running in
the sump. Since the viscometer with the modified measuring system is not suitable for less
than 10 mPa.s viscosity measurement, the lowest FeSi slurry density was set at around
2700 kg/m3. Slurry density was measured by weighing the slurry in a one-litre measuring
cylinder.
When the slurry reached the required density, rheology measurement started. The
viscometer was controlled by the software ‘Orchestra’. The bobbin rotational speeds were
varied from 50 rpm, 100 rpm up to 1000 rpm in 100 rpm increments. At each rpm, 10 torque
readings were recorded. The data of rpm, torque and slurry temperature were imported to
an Excel spreadsheet for further analysis.
Various methods to adjust slurry density were tried. These included starting with the highest
density then reducing density by adding water, and starting with lowest slurry density then
increasing density by adding FeSi solids into the system. It was found that the slurry system
was disturbed whenever FeSi or water was added. Eventually, a third approach was
adopted by taking out water from the slurry to gradually increase slurry density. A small
amount of slurry was taken out to allow the FeSi particles to settle, water was decanted, then
the slurry was returned into the pump-sump system.
The 10 measurement data at each rpm were averaged to give a mean value and a standard
deviation. A constant named the Coefficient of Variation (CoV) is used to describe the
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 5

relative data variation in the repeat measurement. The CoV is defined as a percentage of
Standard Deviation (SD) divided by the mean torque reading at each rpm. A smaller CoV
indicates more stable measurement.

2.3. Measurement of medium stability

For efficient operation, a dense medium slurry is required to exhibit an adequate stability
(resistance to settling). The medium stability is defined as reciprocal of the rate at which the
medium solids settle down under gravity.
To measure FeSi medium stability, a 250 ml measuring cylinder was used (Figure 3). The
following procedure was followed:
1) Calculate the required FeSi mass and water mass to make up a desired slurry density.
2) Mix the FeSi solids and water thoroughly, and transfer 250 ml of the well mixed FeSi
slurry to a measuring cylinder.
3) Weigh the tared mass of the slurry. Record the real slurry RD.
4) Invert the measuring cylinder ten times.
5) Place the measuring cylinder on a flat bench top, and start stopwatch.
6) At every 10 seconds or 20 seconds interval, measure the fall of the mudline by
recording its position (against a ruler on the side of the measuring cylinder).
7) Repeat steps 4-6, and average the readings.

Mudline

Figure 3: FeSi slurry sedimentation rate measurement set-up

3. Data reduction

3.1. Flow curve data reduction

FeSi slurry flow curves (or rheograms) are used to describe slurry rheological behaviour.
The flow curve is a plot of shear stress versus shear rate. The apparent viscosity is the
slope of a line connecting the origin of coordinates and a point on the flow curve at a
specified shear rate. For Newtonian flow, the rheogram is a straight line through the origin
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 6

and the apparent viscosity is a constant, regardless of the shear rate. For non-Newtonian
flow, the apparent viscosity takes different values at different shear rates. The shear stress
and shear rate can be determined from the viscometer measurement data.
Shear stress is calculated at the bobbin surface by Eq. 1:

(1)

where Sb is shear stress at the bobbin surface (Pa)


Mb is the measured torque (N.m)
h is the effective height of bobbin (m)
Rb is the bobbin radius (m).

The effective height of the bobbin is estimated by calibration against the known viscosities of
silicone fluids.
The equation used to calculate shear rate for Newtonian flow cannot be used for FeSi slurry,
particularly in the case where a large gap between the bobbin and the cup was adopted to
allow free passage of the slurry, as is in this case. An equation for non-Newtonian flow (Eq.
2, Van Wazer et al., 1963) was used for the FeSi data processing:

( ) ( )
̇ [ ( )
] (2)

where ̇ is shear rate (s-1), is bobbin angular velocity (rad/sec), is the ratio of cup to
bobbin radii, Sb is shear stress at the bobbin surface (Pa), is yield stress (Pa), and m is
calculated by taking the first-order derivative of the plot:

( )
(3)

It is worth noting that the higher order derivative in Eq. 2 only adds a very minor difference
(<2%) in the calculated shear rate. For simplicity, the calculation of non-Newtonian shear
rate (Eq. 2) was terminated with the first-order derivative in the FeSi applications.
FeSi medium is a non-Newtonian flow with yield stress. The yield stress is involved in the
calculation of shear rate (Eqs. 2 and 3), and needs to be determined. However, it is not
practical to directly measure the yield stress using the Mettler RM180 viscometer with the
modified bobbin-cup system, since the measurements taken at less than 50 rpm are
associated with very large CoV (eg. >200%), and are not reliable (the torque readings were
often found smaller than 0.25 mN.m, the threshold for reliable torque measurement with the
RM180 viscometer). The vane method (Nguyen and Boger, 1983; Shi and Zheng, 2003)
was tried, but it was found that the torque readings were unstable in the measuring chamber
where strong FeSi slurry circulation takes place. Extrapolation of the plot of shear stress
versus angular velocity to a zero angular velocity was therefore adopted to estimate the
apparent yield stress.
In the current viscosity measurements, slurry temperature was not controlled. It was
observed that slurry temperature varied in the tests, particularly for 270D that was tested in
summer time, in which slurry temperature went up to 48.3oC. The effect of slurry
temperature on FeSi rheology has to be taken into account. Correction of temperature effect
is based on the viscosity of suspending phase (ie. water) in relation to temperature. Torque
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 7

readings at the measured temperature were corrected to a standard temperature of 25oC,


consistent with the reference temperature that the commercial calibration silicone liquids are
based on. The temperature correction takes the following form (Eq. 4):

( )
( ) (4)
( )

where T(25oC) is the torque reading at the reference temperature of 25oC, Tm is the torque
reading at the measurement temperature, w(25oC) is the water viscosity at 25oC, and
w(measured) is water viscosity at the temperature of measurement. For example, the water
viscosity is 0.894 mPa.s at 25oC and 0.565 mPa.s at 48.3oC respectively. For a torque of
10 mN.m measured at 48.3oC, the corrected torque at 25oC is 15.8 mN.m. In comparison,
the corrected torque at 25oC is 11.5 mN.m for a 10 mN.m torque measured at 31oC.
Flow curves were constructed by plotting the calculated shear stress against shear rate,
including the extrapolated yield stress at zero shear rate. The data of shear stress and
shear rate were fitted with various commonly used rheology models such as the Herschel-
Buckley model and the Casson model. It was found that majority of FeSi slurries exhibit a
dilatant nature with yield stress. The Herschel-Buckley model and the Casson model are
good for pseudoplastic flow curve, but do not fit the dilatant flow curve well. Polynomial
equations were used to get smoothed flow curves. By way of example, Figure 4 gives flow
curves of 150D grade at various slurry densities. It can be seen that the rheology switches
from dilatant to pseudoplastic nature between an RD of 3.17 and 3.35.

Figure 4: Flow curves of 150D grade at various slurry densities

3.2. Stability data reduction

The recorded mudline positions (cm from bottom) in relation to the time measured were
plotted for each slurry density. From the previous work, a linear trend was expected. The
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 8

gradient of the line represents the rate of descent of the mudline. Figure 5 shows an
example of the sedimentation lines for 150D FeSi at various slurry densities. It was
observed in some measurements that the sedimentation response was not linear towards
the end of the measurement, particularly for higher slurry densities.
17
150D
16
Distance from bottom (cm)

15

14

13

12

11

10
0 50 100 150 200 250 300 350

Time (Sec)

3.48 RD 3.35 RD 3.22 RD 2.93 RD 2.85 RD 2.64 RD

Figure 5: FeSi 150D sedimentation lines at various slurry densities

Linear regression was applied to generate a gradient for each sedimentation line. The non-
linear section of the sedimentation data was not included in the regression. The stability of
FeSi medium was calculated from the regressed gradients. The stability is defined as the
reciprocal of the gradient of the initial linear section of the sedimentation curves, in unit of
sec/cm. The physical meaning of the stability is the time required for FeSi particles in a
given density of slurry to settle a distance of 1 cm. A longer time indicates a more stable
slurry.

4. Result and discussion

4.1. Apparent viscosity as a function of FeSi slurry density

Apparent viscosities were determined from the fitted flow curve equations, calculated for two
nominal shear rates: 10 and 150 s-1. Since dense medium slurry is non-Newtonian, different
shear rates will give different apparent viscosities. The question is what shear rate should
be used to represent the prevailing shear rate in bath separator and in dense medium
cyclone. Literature reports estimation of shear rates in ball mills (Shi and Napier-Munn,
1999) and in a laboratory tumbling mill (Govender et al., 2010). The literature also contains
a number of reports estimating typical shear rates for dense medium separation (eg, Lilge et
al., 1958; Dunglison et al., 1999; Narasimha et al., 2007). Lilge et al. (1958) calculated
shear rates within a cyclone and estimated between 100 and 200 s-1. An average value of
150 s-1 was used as typical of cyclone separation, and 10 s-1 was typical of bath separation.
This is consistent to the previous work for Samancor FeSi rheology measurements
(Dunglison et al., 1999).
The summarised graphic presentation of the apparent viscosity in relation to slurry density at
the two shear rates are given in Figure 6, with detailed gridlines for easy interpolation at a
slurry density of interest. It is noticed that at a small shear rate (such as 10 s-1), the
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 9

apparent viscosity is much greater than that at a high shear rate. This is largely due to the
yield stress associated with the FeSi slurries.
Figure 6 demonstrates that 270D grade exhibits the highest apparent viscosity, and 65D the
lowest viscosity. The apparent viscosities appear in an order from high to low: 270D, 150D,
100D, 65D granular. The difference in apparent viscosity for various grades is more
pronounced at 10 s-1 shear rate, noting that the scales of viscosity in the two shear rate plots
are different. This trend is as expected. Since solid RD and particle shape of the milled
FeSi grades are similar, it is believed that the difference in apparent viscosity across the
whole shear rate range is attributable to the particle size factor. The P80 size of the milled
grades shown in Table 1 is found to be well correlated with the apparent viscosity presented
in Figure 6. The viscosity trend of the three 65D grades is more complex, since their alloy
composition, solids RD and particle size are different. In general, however, there is not
much difference in apparent viscosity for the three 65D samples at low slurry densities.
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 10

Figure 3: Apparent viscosities vs slurry density for the milled FeSi grades,
temperature corrected to 25oC

The graph of apparent viscosity versus slurry density is a characteristic curve for a given
FeSi grade. One application of such curves is to estimate the maximum slurry density
possible for a given separation requirement, hence to determine a suitable FeSi grade for
the required duty. For example, set a nominal maximum apparent viscosity of 500 mPa.s
(1 mPa.s = 1 cP) for an effective bath separation. The graphs of apparent viscosity at the
shear rate 10 s-1 are used to estimate the maximum slurry density that a specified FeSi
grade can reach for this nominal apparent viscosity. Table 2 gives the predicted slurry
densities for various FeSi grades to reach the nominal apparent viscosity of 500 mPa.s at a
shear rate 10 s-1 by using the graphs of the fitted trend lines presented in Figure 6. The
nominal maximum apparent viscosity of 500 mPa.s for bath dense medium separation is an
arbitrary number. More detailed research is required to establish the relationship between
the separation efficiency and the medium density.

Table 2: The predicted maximum slurry densities for various FeSi grades to reach a
nominal apparent viscosity of 500 mPa.s at 10 s-1 shear rate and 25oC temperature.

Grade Slurry density (kg/m3)


270D 3000
150D 2980
100D 3070
65D Granular 3180
65D TB 3240
65D Mixed 3250
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 11

4.2. Comparison of FeSi medium stability

Figure 7 presents the FeSi slurry stability in relation to slurry density for the milled FeSi
samples. Note that 270D does not appear in Figure 7. 270D was tested earlier than the
other FeSi grades and it was not required at that time to measure the stability in the initial
stage of the project. Figure 7 demonstrates that the stability of the six milled FeSi samples
is in an order from high to low: 150D, 100D, 65DGranular, 65D Mixed and 65D TB. As
expected, FeSi slurry appears more stable at a higher medium density (increased trend lines
with slurry density), yet the relationship is not linear.

a.

Figure 7: FeSi slurry stability vs slurry density for the milled grades.

High medium stability is usually associated with high slurry viscosity. Figure 8 shows the
medium stability in relation to apparent viscosity at a shear rate of 10 s-1 for a slurry density
of 3100 kg/m3 for the five milled grades. The data were back-calculated from the trend line
regression as presented in Figures 6 and 7. The linear fit shows an R-square of 0.97,
confirming that the stability is closely correlated with viscosity. Plotting the apparent
viscosity at other shear rates and for different slurry densities shows the similar correlation.
Dense medium separation requires a medium slurry with an adequate stability for
satisfactory medium handling and separation efficiency. Since high medium stability is
associated with high viscosity, which adversely affects medium handling and separation
efficiency, a trade-off between stability and viscosity should therefore be established. A high
medium stability can be achieved by increasing slurry volume concentration, fines content,
irregular particle shape, contamination of low RD material with FeSi, material oxidation, etc.
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 12

Figure 8: Medium stability in relation to apparent viscosity at a shear rate of 10 s-1 for
a slurry density of 3100 kg/m3 for the five milled FeSi grades.

There is no doubt that characterising medium rheology and stability for various grades of
FeSi will assist the selection of FeSi and determination of the trade-off operational point in a
dense medium separation process. However, it is worth noting that the characterisation
results presented in this paper are from clean FeSi material. In a dense medium separation
process, FeSi medium is recovered and re-used. Material degradation, oxidation and
contamination with ore cannot be avoided. Characteristics of medium stability and viscosity
would therefore be different from that using the clean FeSi material (Napier-Munn and Scott,
1990). It is therefore recommended that characterisation of medium viscosity and stability
for the DMS Powders product be conducted in an environment similar to the plant operation.

5. Conclusion
A specifically designed testing rig has been set up to keep the fast-settling FeSi particles
well suspended for dense medium rheology measurement. Six milled FeSi grades supplied
by DMS Powders were measured using this testing rig and the results are reported in this
paper. Medium stability of the FeSi samples was determined using a 250 ml transparent
measuring cylinder. Apparent viscosities at two shear rates in relation to slurry densities for
the six milled FeSi are reported. These graphs can be used for dense medium selection,
given the required separation density and viscosity. Medium stability and slurry viscosity are
found to be closely associated. To achieve an optimal separation efficiency, a trade-off
between stability and viscosity should be established. Characterisation of FeSi slurry
rheology and stability will assist in determining the optimal dense separation conditions.

6. Acknowledgement
The author gratefully acknowledges DMS Powders for funding the work and the permission
to publish the major results. The assistance provided by JKMRC Workshop in modifying the
bobbin-cup system, the JKMRC pilot plant in setting up the testing rig and Ph.D student
Weiran Zuo in conducting the tests is acknowledged. The valuable comments from Prof.
Tim Napier-Munn in reviewing this manuscript are sincerely appreciated.
Shi: Characterisation of rheology and stability of DMS milled grades of ferrosilicon 13

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