Lecture 8 & 9

VISCOSITY MEASUREMENTS
Table: Some dimensionless number
Name Abbreviation Definition
Fluid mechanics
g    0 L
Drag coefficient Cd v 2
g    0 L2
Eötvos number Eö 
2dP
Friction coefficient Nt
v 2 L

Froudes number Fr v 2
   0 gL
Mortons number Mo g 4
 3
Rel. roughness Rs
d'
d
Reynolds number Re vd vd

 v

Webers number We v 2 L

Mass transfer
 gTL3
Grashofs number Grm
v2
 Mass transfer
Grashofs number Grm gTL3
v2
C p D
Lewis number Le
k

Schmidts number C v
D

Sherwoods number Sh hm L
D
Heat transfer
Grashofs number Grh gL3 T
v2
Nussels number Nu hv L
k
Pranolts number Pr C p
k
 Shear stress to viscous flow

V1

V2

YX = . (dVx/dY) Newton’s Law

Shear stress = viscosity x velocity gradient
 Units of Viscosity
• a tangential force of 1 dyne per cm2 maintains
a difference in velocity of 1 cm per s. between
two parallel planes = dyne.s/cm2 = 1 Poise

• Centipoise ,(cP) = 0.01 poise.

• One poise = 0.1 Pa·s
• Pa.s = 1 N. s/m2.
Viscosity of water at 20oC = 0.01 poise
= 1 centipoise
 Kinematic viscosity
• Ratio of the viscosity to density:

ν=μ/ρ

where ν = kinematic viscosity, μ = absolute or

dynamic viscosity, ρ = density. In the SI-system
the unit is m2/s
Compare with diffusivity and thermal diffusivity!
 Some relationships
D = B.KB.T
Where, D = diffusion coeff.

B = mobility (mol. S-1. J-1)

KB = Boltzmann constant

T = Temperature, Kelvin
 Thermal activation
• Let us recall Diffusion coefficient: D = B.kB.T
Diffusion is a thermally activated process
- Activation energy is needed for movement of particles from
one position to another
- Thus fluidity ( = 1/ viscosity) is also a thermally activated
process

- Viscosity should be proportional to

+ ΔG‡ /RT
Viscosity should be decreasing with temperature
Activation Process
 Temperature Depence of Viscosities

 EA 
Arrhenius Relationship: η  A exp  
A  RT 
 

 EW 
Weymann Relationship: η  A Texp  
W  RT 
 

 BB 
Brostow Relationship: η  exp  A B   C BlogT 
 T 
 Viscosity Measurement Methods
Viscometer Measurement Range Comment
Pa.s
Rotating Torque measured on static bob- 101-10-2 Needs very accurate vertical
crucible alignment.
Rotating Torque measured on bob-several 100-102 Alignment problems
bob companies make viscometers overcome using flexible joint
Falling Time for bob to fall (or drag) through 100.5-105 Needs a long, uniform hot
Body known distance Zone
Oscillating Amplitude of plate in sample and air 10-1.5-101 Need melt density value
plate
Oscillating Measures log decrement of amplitude 10-4 -10-1 1.Need melt density value
Viscometer Of Twisting 2.Roscoe Eqn.
Recommended
Shiraishi Rotating plate-torque Parallel plate 102- 1011
sample height –time Indentation-rate of
penetration
SLS Damping of scattered waves on 10-5 - 0.5 Also measures surface
surface("ripplons") tension
Principle of the Rotating Cylinder
Method
Assumption: Laminar flow between the
concentric cylinders.

Viscosity, η = [M/(8 .π2. n. h)].((1/r12) – (1/r22))

Unit: dyne.s/cm2 = Poise
M= torque, dyne.cm
n = revolutions, s
h= height of the inner cylinder , cm
r1=radius of the inner cylinder
r2 = radius of the outer cylinder
Viscosity of liquid iron

T. Iida and R. I. L. Guthrie: The physical

properties of liquid metals, Clarendon
Press, Oxford, (1988).
 Ranges of viscosities
1. Iron-making slags:
ca 4- 6 poise at 1773 K

2. LD slags: ca 0.5 poise at 1873 K

22

20

18
Slag

3. Mould flux slags:

B
16
C
Viscosity [dPa s]

14
E
12
F
10 A
8

0
1300 1350 1400 1450 1500 1550 1600 1650 1700

Temperature [K]
 Choice of Materials
1. Choice depends upon the temperature range,
oxygen partial pressure requirement and
stability.
2. The melting point should be atleast 100 K
above the max. temperature of
measurement.
3. Chemically inert to the system studied.
4. The materials for the container as well as the
spindle need not necessarily be the same
 Choice of Materials (contd.)
Pt: chemically inert, can be used in oxidizing
atm., (consider the formation of PtOx at high
oxygen pressures)., soft, often breaks,
expensive (50 % of the cost can be recovered
by leaving back the scrap). Max. temp. ca
1673 K.
Pt-30 % Rh: Better mechanical strength; can be
used upto 1823 K. Very useful.
 Choice of Materials (contd.)
Carbon-free iron: ARMCO iron,
• quite advantageous for FeO-containing slags
(keeps the equilibrium at Fe-slag boundary).
• The atmosphere should be inert, pO2 > 10-13 Pa.
• Inexpensive material; can be discarded after
experiments.
• Shaping is easy
• Max. temperature is1723 K (safe limit).
 Choice of Materials (contd.)
Nickel/Inconel:
• Stands slightly higher oxygen pressures (pO2
~10-10 Pa.
• Fairly stable to chemical attack. In oxidizing
atm., it can form NiO which will dissolve in the
slag. aNiO decreases forming the driving force
for dissolution.
• Used with advantage in some kinetic studies.
 Choice of Materials (contd.)
Mo
• very good for steel temperatures,

• expensive,

• difficult to machine,

• brittle after one use.

Often there is no choice to Mo!

 Choice of Materials (contd.)
Graphite crucibles and spindles:

Not advisable due to:

Chemical reactions with slags and

Slipping of the slag on the surface of the crucible

and spindel (absence of friction)
 Choice of crucible materials
• In order to ensure the absence of crucible
effects:

• Calibration trials can be made with two

different crucible materials

• Confirm the reproducibility

 Viscosity measurement for molten slag

Choice of Crucible
and spindel material

Measurements Atmosphere
Viscosity of Ar, Air, N2, CO, CO2, SO2, H2 etc.
Mixing: possible
Molten Mould Flux for CC Flow rate: controllable
Molten Synthetic Slag etc. Gas cleaning system: available
Po2: controllable by mixing CO and CO2
at ~1600oC Min. Po2<10-21atm
 Viscometer

Rotating cylinder method

Viscometer:
Brookfield RVDV-II+
(Max. torque: 7.187×10-4Nm)

Material:
Armco iron(crucible, spindle)

Crucible diameter:
36 and 40mm

Rotation speed:
10, 20, 30, 40, 50rpm
(for checking the linearity)
Atmosphere: deoxidized Ar gas (using Cu and Mg
chip) Condition:
Temperature range: ~1723 K Steady state(Temp. Torque.)
 Gas atmosphere
1. Gas purification steps, already discussed.

2. The crucible materials like Fe or Mo have to

be protected.
3. The viscometer itself should be protected
from gas and condensates originating from
the measuring system.
 Some construction details
1. The hanging wire for the spindle should be
straight, stiff and aligned vertically without
touching the sides.

2. The coupling between the reaction tube and

the viscometer should be flexible (as for
example, the use of bellows) to protect from
gas leakage.
3. Separate gas stream to protect the
viscometer from corrosive gases and dust.
 Calibration of the unit
Calibration has to done both
at room temperature as well as
at high temperature.

Room Temperature: Standars oils can be obtained

from the instrument supplier.
High temperature calibration: EU standard; not
available. CaO-SiO2 melts checked against EU
standard in our group.
 Choice of High Temperature
Calibration liquid
1. The system should be completely molten in the
temperature range – atleast 100 K above the liquidus
temperature.

1. The system should be chemically stable:

a) With respect to gas phase (for example, vapour
losses)
b) With respect to container material

3. The viscosity of the liquid for calibration should be in

the same viscosity range as the measuring liquid.
CaO-SiO2 phase diagram
A typical calibration line (Voltage (Torque) vs. RPM)
cp (=centi-poise):
1 Unit of viscosity
0.9 49cp
0.8 98cp
484cp
0.7 980cp
0.6 4940cp
0.5
0.4
Voltage(Torque)/V
0.3
0.2
0.1
0

0 20 40 60 80 100
RPM

RPM: Revolutions Per Minute

A typical calibration line (Viscosity vs. Slope)

5000
y = 1.70665099.E+05x
4000 R2 = 9.99999362.E-01

3000

Viscosity/cp 2000

1000

0
0 0.01 0.02 0.03
Slope
Slope of Torque vs. RPM
 Systems experimentally studied
• Binary systems:
• Quarternary systems:
– CaO-SiO2
– Al2O3-CaO-MgO-SiO2
– FeO-SiO2
– CaO-FeO-MgO- SiO2
– MnO-SiO2
– CaO-FeO-MnO- SiO2
• Ternary systems:
– CaO-MgO-MnO- SiO2
– Al2O3-FeO-SiO2
– FeO-MgO-MnO- SiO2
– Al2O3-CaO-Cr2O3
– CaO-CaF2-FeO-SiO2
– CaO-FeO-SiO2
– CaO-MgO-SiO2
– CaO-MnO-SiO2 • Quinary system
– FeO-MgO-SiO2 – CaO-FeO-MgO-MnO- SiO2
– FeO-MnO-SiO2
– CaO-CaF2-SiO2 • Industial mold fluxes
– Al2O3-CaO-FeO • Cr2O3-containing systems
A typical results (Viscosity)

44%SiO2, 12%Al2O3, 41%CaO, 3%MgO slag.

Influence of CaF2 and temperature on the viscosity.
 Viscosity Measurement

2500

SSAB lu
Sandvik
2000 SSAB ox
Sandvik flux2
Viscosity [centipoise]

SSAB lu flux2
Avesta
1500
Start

1000

500

0
1000 1050 1100 1150 1200 1250 1300 1350 1400 1450
Temperarture [˚C]
Mould flux viscosities
Mould fluxes
 Factors in the measurements of
viscosities between liquidus and
solidus
1. Appearance of crystals

2. Annular space between the crucible and the

spindle
3. Latent heat affecting the viscosities
4. Composition changes during partial
solidification.
“The concept of Break point” is not just a system
property; but also the measurement technique.
 3.0 2900

Viscosity
2800
2.5 Q/R
2700
Viscosity (dPa·s)

2600

Q/R (K)
2.0

2500

1.5
2400

2300
1.0

2200
265 270 275 280 285 290

The viscosities and the activation energies

for viscous flow for H2O as a function of temperature.
 10 10
2
(d Q/dT)/R
0 0

-10 -10

(dQ/dT)/R
(dQ/dT)/R
(d2Q/dT)/R

-20 -20

-30 -30

-40 -40
263 268 273 278 283 288 293

T (K)

The first and second derivatives of the activation

energies for viscous flow for pure water
 Two Phase Viscosities

600
580
Measured Viscosities
560 Computed Viscosities by Taylor's Model Einstein:
540 Computed Viscosities by Einstein's Model eff =  (1+2.5 c)
520
Taylor:
Viscosity(mPa.s)

500
480 eff =  (1+ c{1 + 2.5/ 1 + })
460
440
420
400
380
360
340

0,00 0,05 0,10 0,15 0,20

Volume Fraction of Water by Volume

 Dynamic Viscosity Measurements
Oxidation of Fayalite slag in CO-CO2 atm.
Pco/PCO2 = 9.81
140

130 Experiment A, T=1673K

Experiment B, T=1673K
120
Experiment C, T=1623K
110
Viscosity (dPa·s)

100

90

80

70

60

50

40
0 500 1000 1500 2000

Time (min)
Dynamic Viscosity Measurements
Alumina Dissolution in slag
8

1757 K
7 1740 K
1714 K
6
Viscosity (dPa·s)

3
(40 % CaO,-5 % FeO-50 % SiO2-5 % CaF2 )

2
0 500 1000 1500 2000 2500 3000 3500

Time (min)
Shahbazian F., Du Sichen and Seetharaman S. ISIJ International, vol.42, 2002, pp.155-62
Viscosity changed under dynamic foaming

0,15

0,14

0,13
Viscosity (mPas)

0,12

0,11

0,10 Slag 1
Slag 2
0,09
Slag 3
Slag 4
0,08
Slag 5
Slag 6
0,07

-10 0 10 20 30 40 50 60 70 80 90 100 110 120

Time (min)
 Applications
80 l/min argon gas is injected into 100 ton of steel

Center of
the ladle

Jönsson P.G., L. Jonsson L. and Du Sichen ISIJ International, Japan, vol.37,1997, pp.484-91
 Microgravity experiments

Advantages:
- Avoid contamination
- Quick heating and quenching
- Avoid convection due to the gravity
(density variations in fluids)

etc.
Microgravity experiments –Drop shaft
Drop tower

Drop
Drop shaft
capsule
Free fall
zone
490m
Total depth
710m
Electro Magnetic Levitation Levitated drop = Contactless !!

Side view Top view

F3 F4
minus
F2
plus F1

F5

20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38
Overview Frequency, Hz
FFT-Spectra of a liquid Ni15Cu20Fe65 alloy (1733K).
Microgravity experiments
- Parabolic flights
Typical parabolic flight

www.dlr.de
Sounding rocket
Kiruna, Sweden
Electrostatic Levitator (ESL)
Camera Illumination lamp

Position laser
Heating laser

Position detector
Chamber
Pyrometer

Pyrometer Camera

Sample

Position laser
Position detector
Camera
High Voltage

Top Electrode Sample

Side Electrode

Small hole for aerodynamic levitation JAXA, Japan

Bottom Electrode
1cm
Launch pedestal
Latest image of ISS taken from Space Shuttle Discovery in July 2005
(Courtesy of NASA)

International Space Station

Microgravity experiments