Finger Printing Of Mould Powder

By Determining Phases, Viscosity,

Composition And Melting Rate

By
Anupam Sadhu (163110002)
Anushri Nag (163110005)
Sachin Sudhir Ambekar (163110011)

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 Problem
• To finger print a specific type of slag for
reproducing it by the determination of following
properties:
1. Chemical composition
2. Phases present
3. Melting rate
4. Viscosity

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 Role of mould flux powder
• In continues casting
process role of mould flux
powder is very important.
• Thermal insulation
• Prevention of reoxidation
• Inclusions entrapment
• Lubrication between the
solidified steel shell and
the mould
• Heat transfer control

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 Analysis of phases present
• Composition analysis of flux gives various minerals present in
the flux.

• Analysis of phases gives whether or not these minerals are

present in form various phases.

• The analysis for presence of phases for any mixture is best

done by XRD.

• Example of phases is given by phase diagram.

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5
 XRD Principle
• XRD is based on bragg’s law.
• Bragg’s principle relates interlayer spacing to diffraction
angle.

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 XRD Principle
• By XRD analysis we can
find out the type of
crystal structure as well
as the lattice parameter.
• Type of crystal structure
is found out due to
presence of structure
factor.

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 Experiment
• X- Rays are generated by hitting target material with high
energy electrons.
• These X-rays are then incident on the sample to study crystal
structure.

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 Experiment
• Some of the incident beam gets diffracted and then is collected
by detector.
• Intensity vs diffraction angle graph is plotted.

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 Analysis
• The graph obtained is
analysed for the phases
present.

• Combination of intensity
and bragg’s angle is unique
for every phase.

• Thus identification of
phases is possible.

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Analysis
• It is done by computer software by comparing the obtained
data with the existing data.
• It can be done manually with Hana Walt or Fink method.
• Manual work is easier with limited elements. Slags have
multiple complex systems, hence software analysis is
preferred.
• Results show that initial powder contains different phases
but after thermal treatment these phases react and new
phases are formed.

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XRD of powder XRD after thermal treatment

The composition of above powder is:

Phase % Phase %
SiO2 34.33 CaF2 15.39
CaO 29.63 Na2O 4.75
Al2O3 5.55 MgO 3.05
C-Total 4.11 CO2 3.22 12
Precaution
 Particle size of the specimen should not be too much fine otherwise peak
broadening can take place.

 Sample should be protected from moisture exposer.

 The powder should be dispersed uniformly to avoid any discrepancy in data.

 Caution should be taken for XRD exposer.

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Chemical Composition Determination
by XRF

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 Principle
 The band gap between
different energy gaps for
different materials are unique.
 High energy X-ray knocks out
the inner cell electrons
creating hole in the lower
energy states.
 Electron from the upper cell
jumps into the lower energy
state by the release of energy.

 That way we can get “characteristics emission” which act as a finger print of any
material.

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 Procedure

The sample is normally prepared

as a flat disc.

Step by step
procedure:

Sample is kept on
sample holder

X-ray is emitted from Collimator will

X-ray will hit the sample
the x-ray generator intensify the x-ray

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 Procedure
Detector will convert
Secondary x-ray will Collimator will
the x-ray energy into
be generated concentrate the x-ray
electric signal

Sample chemical composition of mould powder by XRF

technique

Mould Powder Amount Mould Powder Amount

Constituents Constituents
SiO2 33 K2O 0.1
CaO 34 Na2O 12.8
MgO 0.5 Li2O 0.4
Al2O3 2.8 F 7.9
Fe2O3 1.4 C 6
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 Limitation and Precaution

 This cannot be done for light-weight material as Boron (B) because high energy
X-ray will rupture the material.
 XRF analyses can not distinguish ions of the same element in different valence
states.
 Safety should be taken to avoid x-ray exposure.

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 Importance of Melting Rate
• Melting rate controls the thickness of the melted slag layer.

• Optimum slag layer thickness in 10-15 mm

 If the slag layer is too thin then

 Unmelt powder will create defect in surface.

 If the slag layer is too thick then

 Crystallized rim will emerge at the meniscus which will disturb

solidification process.

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 Principle
Melting procedure of mould
powder in the continuous casting
units:
 In case of continuous casting solid mould
powder is added to the system.

 Liquid steel comes in contact with the

mould powder.

 Heat is being transferred from liquid steel

to mould powder

 Powder melts to form a lubricating layer.

Here during the measurement of melting

rate we are trying to recreate the condition
like cast houses.
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 Principle
Experimental principle:

 Liquid pool of molten metal is produced below the mould powder bed.
 Some markers of platinum is kept above the mould powder bed.
 Due to heat transfer the mould powder will start to melt from the part of
immediate contact with liquid metal.
 Gradually the mould powder will get compacted due to melting and sintering of
the powder.
 As the compactness in the bottom part is increasing the platinum markers will
come down gradually.
 The rate of coming down will be proportional to the melting rate.

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 Melting Rate Calculation

Instrument required:
• X-Ray machine
• One specially designed Alumina tube.
• Induction coil and power supply.
• Alumina lid.

Experimental Procedure:

Addition Of Metal into Melting the metal with

the tube closed lid

Kipping the
Filling the tube with
temperature at 1600°
mould powder
C

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Continued:

Kipping the
Putting the Pt markers
temperature fixed at
at different levels
1600° C

Watching the
Mathematical movement of Pt
calculation using the markers by X-ray
movement data imaging

Movement of two platinum

4.5 markers
4
3.5
Distance

3
2.5
2
1.5
1
0.5
0
100 200 300 400 500 600 700 800 900 1000
Time (s)
Series 1 Series 2
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 Precautions:
 During melting of metal it should not come in contact with air.

 Heat supply from the coil should be constant.

 Temperature of the pool should be constant.

 During melting rate calculation heat flux should also be taken into account.

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 Viscosity
Measurement

By rotating cylinder method

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 Principle
 It is based on the principle that the fluid
whose viscosity is being measured is sheared
between two surfaces.
 In these viscometers one of the surfaces is
stationary and the other is rotated by an
external drive and the fluid fills the space in
between.
 The measurements are conducted by applying either a constant torque and
measuring the changes in the speed of rotation or applying a constant speed
and measuring the changes in the torque.
 Whole thing is carried out at a temperature higher than melting temperature of
the mould powder.
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 Procedure

Prerequisites:
• Crucible Selection: Iron Crucible • Viscometer needed to be
calibrated using some kind
• Melting temperature determination of oil 27
 Step by Step Procedure
Mount the Iron Crucible in high temperature furnace

The spindle was kept inside the furnace above the crucible

Rotating Spindle dipped into the molten liquid

Argon gas is supplied inside the furnace to get

inert atmosphere

Temperature of the furnace was increased to melt the

mould powder

Torque for rotation was calculated

Torque was compared with the standard chart to

get the viscosity value 28
 Example plot of viscosity vs. temperature

Break Point:
The solidification start or break point (Tbreak) is the temperature where a rapid
increase in viscosity with a decrease in temperature is observed.

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Change of Viscosity With Temperature

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 Precautions
 The distance between the spindle and the crucible should be
large enough.

 The spindle should not touch the crucible bottom.

 The crucible should be placed in even temperature zone.

 The wire attached to the spindle should be straight and stiff.

 The temperature of the furnace should not fluctuate.

 Atmosphere should be inert.

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 Conclusion
 From the all tests we performed we can understand the properties like phase,
composition, viscosity and melting rate of the mould powder.
 This tests will help us to understand the properties of the mould powder we are
going to finger print.
 But still these tests are not enough to duplicate the powder in a proper way.
 Many other things like grain size, processing method, raw materials also needed
be understood.

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