Title of Invention

DEVELOPMENT OF MICROALLOYED ULTRA HIGH STRENGTH STEEL

Abstract Conventional mode of production of high strength steel used lower carbon concentration, maintaining lower finish rolling temperatures. Reduction in carbon content during melting increased cost of melting operation of steel and lower finished rolling temperatures required high amount of rolling load and energy. The present invention aims at overcoming of above drawbacks by enhancing the carbon concentration of steel and using higher finish rolling temperatures. This invention provides a novel microalloyed ultra high strength steel having the composition - i) carbon 0.06 - 0.15% by wt.; ii) phosphorus - 0.01% max by wt.; iii) sulphur - 0.01% max by wt.; iv) silicon 0.2 - 0.7% by wt.; v) manganese 1.2 - 1.8% by wt.; vi) nickel 3.0 - 3.8% by wt.; vii) molybdenum 0.4 - l.0% by wt.; viii) copper - 1.5% max by wt.; ix) niobium 0.04 - 0.09% by wt.; x) titanium 0.02 - 0.08% by wt.; xi) aluminium 0.02 - 0.03% by wt.; xii) chromium - 1.5% max by wt. The subject invention also provides a process for preparing the aforesaid ultra high strength steel.
Full Text -2-
The present invention relates to development of ultra high
strength steel and is also concerned with a process for preparing
such steel. More particularly this invention pertains to the
production of ultra high strength steel (identified herein as
MICRO MSF-1700) using Mn, Ni, Mo, Cr and Cu along with Nb and Ti
as microalloy components, thereby achieving a 160 ksi yield
strength. Such low carbon ultra high strength steels using
mieroalloying additions when subjected to radial forging followed
by thermo-mechanical controlled processing (hereinafter referred
to in this specification in its abbreviated form "TMCP") at
various finish rolling temperatures (FRT) and accelerated cooling
resulted in products found useful in making gun barrels, crank-
shaft and for other structural purposes.
During the last three decades considerable efforts were
exerted towards development of micro-alloyed high strength steel
using.No, Ti and V singly or in combination to achieve a good
combination of mechanical properties. This Fe-C-Mn system alloyed
with micro alloying elements undergoes thermo mechanical controlled
processing (TMCP). New classes of high strength low alloy (HSLA)
steel emerged to achieve better strength and toughness, better
weldability and corrosion resistance. Two prime microstructures
of th€!se new classes of steels are ferrite martensite (dual
phase) and acicular ferrite. The basic objective of adding micro
alloying elements is to hinder the recrystallisation and grain
growth of austenite and by deforming the austenite, heavily pan-
caked shaped grains can be produced. Ultimately this austenite
when subjected to water quenching engenders fine acicular-ferrite
along with some polygonal ferrite, to achieve attractive set of
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mechanical properties i.e, strength and toughness simultaneously.
These fine ferrite grains are developed during controlled rolling
technique through repeated recrystallisation. Microalloying
elements not only help in developing fine ferrite grains, but
also act as precipitation hardener where Mn increases strength
properties through solid solution hardening. The strength
properties of the acicular ferritic HSLA steel is achieved not
only due to size of ferrite, but shape of ferrite also plays an
important role and these steel posseses YS-500-600 Mpa, UTS-600-
750 Mpa along with toughness value 70-80 J at ambient temperature.
One of the interesting properties of this kind of steel is low
impact transition temperature value ~50°C, besides good weldability
and corrosion resistance. These properties have led them for
their use in several structural purposes.
Microstructure and associated properties also vary depending
on post cooling conditions. The major processing route for
production of these categories of steels are thermomechanically
controlled processing Controlled rolling though forging route is
another viable technique to process these steels with better
structural homogeneity and soundness. All these developments
have opened a new era to produce strong and tough steel.
These kinds of steels were produced earlier with lower
carbon concentration and maintaining lower finish rolling
temperatures. Reduction in carbon content during melting increases
cost of melting operation of steel and maintaining lower finished
rolling temperatures also required higher amount of rolling load
and energy.
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The present invention aims at overcoming the drawbacks of
the prior art and provides a solution by enhancing the carbon
concentration of steel and using higher finish rolling temperature.
The principal object of the present invention is to provide
a novel microalloyed ultra high strength steel suited for structural
purposes.
A further object of this invention is to provide a process
for preparing microalloyed ultra high strength steel for structural
purposes.
A still further object of this invention is to provide a
microalloyed ultra high strength steel wherein acicular ferrite
and/or Bainite in the microstructure is produceed by adopting
controlled rolling operation followed by accelerated cooling.
Another object of this invention is to provide a process for
preparing microalloyed ultra high strength steel wherein products
of desired grade and characteristics are obtained by radial
forging and followed by controlled thermo mechanical processing.
The foregoing objects are achieved by this invention according
to which there is provided microalloyed ultra high strength steel
having the composition -
i) carbon - 0.06 - 0.15% by wt.;
ii) phosphorus - 0.01% max by wt.;
iii) sulphur - 0.01% max by wt.;
iv) silicon - 0.2 - 0.7% by wt.;
SRD/ns/FILE-1/PATENT

v) manganese - 1.2 - 1.8% by wt.;
vi) nickel - 3.0 - 3.8% by wt.;
vii) molybdenum - 0.4 - 1.0% by wt.;
viii) copper - 1.5% max by wt.;
ix) niobium - 0.04 - 0.09% by wt.;
x) titanium - 0.02 - 0.08% by wt.;
xi) aluminium - 0.02 - 0.03% by wt.;
xii) chromium - 1.5% max by wt.;
The present invention further provides a process for preparing
microalloyed ultra high strength steel as defined hereinabove,
which comprises -
a) introducing charge of raw materials in an electric arc
furnace maintained at lower tap of around 2 for 15 minutes,
using maximum tap voltage of 180 volts at tap 4 after
subsidence of arc till the complete melting of the charge
materials;
b) lowering the furnace tap at 3 to avoid high temperature
followed by addition of iron ore, mill scale and limestone
along with Fe-Mn alloy and then carrying out slagging after
around 40 minutes (slag out I);
c) adding to the charge substances selected from lime
stone, manganese and mill scale, followed by slag out (II)
after 40 minutes of refining;
d) adding after 20 minutes of slag out II in step(c), the
following materials lime stone, Fe-Mn and mill scale
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and after 10 minutes of addition, and thereafter
slagging out for the third time (III);
e) after slag out III/ carrying out addition of lime
stone, Fe-Si, manganese, Fe-Mo, pure nickel, metallic
aluminium as per requirement and continuing refining;
f) after 10 minutes of refining, adding Fe-Si and lime
stone followed by slag out IV;
g) carrying out complete slag out and making reducing slag
by adding coke podwer, calcium carbide, spar and limestone,
followed by addition of undernoted materials for higher
requirement :
Fe-Si, Fe-Mo, pure Ni-manganese, pure Cu, and covering
the melt with reducing slag and tapping in the ladle preheated
upto around 900°C;
h) adding the following for formation of a right slag :
lime - 10 kg/ton, spar - 3 kg/ton, pet coke - 0.3 kg/ton,
Fe-Si - 3 kg/ton, Al - 1.2 Kg/ton, ramming mass - 50 kg and
feeding 50 metres of Ca-Si and Al to the ladle as wire
injection;
i) adding to the ladle Fe-Nb and Fe-Ti for facilitating
formation of micro-alloy, and
j ) pouring the molten mass into moulds, followed by teeming,
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stripping of ingots, radial forging and thermo mechanical
processing to obtain the desired products.
The details of the experimental work are discussed below in
which melting of the starting materials was carried out in an
electric arc furnace of around 2.5 ton capacity. 10 inch square
ingots were cast in metal moulds and thereafter forged in radial
forging machine.
Plants and equipments used in carrying out the production of
microalloyed high strength steel are as given hereafter in numbered
paragraphs :
1. Electric Arc Furnace :
The present project work of "micro-alloyed steel MICRO MSF-
1700" has been planned to heat the charge and cast the ingots in
2T-EAF. It is a 2.5 ton capacity furnace and its details are
given below. The furnace proper looks more like a saucepan
covered from top with an inverted saucer. The electrodes are
inserted through the cover from the top.
The roof along with the electrodes swings clearly off the
body to facilitate charging from top.
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The roof is lifted a little and the furnace body moves to one
side clearly off the roof to facilitate charging.
The furnace unit consists of following parts:
i. Furnace body -i.e., the shell, the hearth, and the walls. The
spout the door,etc.
ii. Gears for furnace body movements,
iii. Roof arrangements,
iv. Electrodes, their holders and supports,
v. Electrical equipment -i.e., the transformer, the cables the
vi. Electrode control mechanism, etc.
2» The furnace body
The furnace shell. The furnace shell is a welded or riveted
steel plate construction and has a cylindrical saucepan like shape.
It has spherical bottom. The spout for tapping the metal is welded
to the bottom and the main door is situated directly opposite the
spout.
3. Refractory lining: -
The furnace shell in lined from inside with suitable refractory
to suit the refining operation. The details are given below.
4. The hearth: -
Next to the shell is a layer of firebricks at the bottom and is
followed by magnesite brickwork to form the brick sub-hearth.
Necessary gaps are left in the brickwork for its expansion on
heating. Ramming tarred dolomite or magnesite makes the working
hearth. Newly rammed hearth is slowly dried and brought to the
working temperature by placing coke on the bottom and striking an
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— 9 —
arc against it. A freshly rammed hearth is given a slag wash at the
working temperature.
5 The side wall.
Magnesite, dolomite or chrome-magnesite (preferably metal
encased) is used to line the sidewalk
6. The tap hole.
A round former is inserted and the space left around is
rammed to make the tap hole.
7. The door: -
Furnaces have only one door directly opposite the tap hole
and any additions during refining are made through this door. This
is the main door and is also used for slagging.
8. The qears for furnace body movements.
The furnace body needs to be tilted nearly through 45° on the
tapping side and 15° on the slagging side. The tilting gear is either
hydraulic or electrical. In electrical a motor actuates the rear of the
furnace. Guide rails are used to ensure true movements. Some
locking arrangement is necessary for the horizontal positioning of
the furnace. The furnace is tilted around its center of gravity so that
the spout also changes its positions. The ladle needs to be either
suitably located even for later position of the spout or it should be
adjusted during tapping.

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9. The roof: -
The roof is a domed construction and rises about one per cent
in span towards the center. The roof has three holes located
symmetrically to allow insertion of the electrodes. The holes are
made from ring-type bricks. The roof in an electric arc furnace is
subject to greater thermal fluctuations and hence basic roof cannot
be used. The current trend is to use high alumina, 70-80% AI2O3
bricks to make the roof.
10. The electrode and its support: -
The electrode. The electrodes are of graphite and are
capable of carrying current at high density. Their sizes of Electrodes
are 6 inches. These are circular in cross-section and each piece is
about l-3m long. The electrode pieces are joined, one to the other,
with the help of a nipple.
Electrode control. For efficient melting the arc must be
stabilized to supply uniformly a maximum amount of energy. This
necessitates keeping the distance between the electrode and the
charge constant. As melting occurs this distance increases and if
any solid piece collapses in, it may decrease. The electrode is
automatically adjusted to maintain a stable arc. The electrode
control systems either tries to maintain a constant current or
constant voltage across the gap. A third type of control tries to
maintain constant impedance in the individual electrode circuit.
Each electrode is provided with an independent Electro-mechanical
or electrode is hydraulic system of control.
The electrode support. The furnace is provided with a
vertical column or mast to which horizontal arms are attached and
the electrode is held by the arm in position. The mast itself rises

- 11 -
and falls; the electrode arm is rigidly attached to the mast. It allows
easy titling of the furnace. Electro-mechanical or Electro-hydraulic
drives are used for activation of the masts in effecting electrode
control. The electrode arm supporting the electrode clamp is
generally tubular and is water-cooled. It is insulated from the mast
as well as the clamp. The electrode is held in a vertical position in a
water-cooled copper clamp situated at the end of the electrode arm.
It is vital to have the contact of the clamp with the electrode as
clean as is possible, so as to keep the contact resistance to an
absolute minimum.
ii# The Transformer: -
The primary voltage may be 6 KV and the secondary with
series tappings from 1-4 i.e., from 90-180 volts. During meting
more power is required than during refining. The transformer
capacity is designed to suit melting requirements. The capacity is,
therefore, under-utilized during refining. The capacity of the
transformer is 3000 KVA.
12. Scrap yard: -
The scrap yard in 2TON-EAFis having varieties of scraps with
low sulphur and phosphor the following scraps are frequently used
for the production of different grades of steels,
i. Railway scraps i.e., railway wheels, railway type, axle etc.
ii. Rejected ingot scraps,
iii. Shell scraps,
iv. Strips
v. Return scraps i.e., dead head cutting tail and cuttings etc.

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Here scraps have been divided into 3 categories
i. HNCM i.e., high Nickel-chrome-molybdenum,
ii. LNCM i.e., low Nickel-chrome-molybdenum,
iii. Plain carbon steel scraps.
Characteristic need for scraps:
It is preferred to get the moisture free and grease/oil free scraps.
But unfortunately the same is not available at normal conditions.
M&S factory, Ichapur has no scraps-preheating facility for moisture
and oil-grease removal and also no facility of shot blasting to
remove the rust
13. Ladle heating system: -
Ladle in the EAF-2 Ton is being heated by hard coke while in
case of eaf-15ton ladle is heated by oil fired burner upto a
temperature of 900°- 1000°c.
14. Wire-feeding system: -
This consists of CaSi and Al wires. These both are fed to liquid
metal in automatic manner.
15• Teeming bay/ pit side with pouring mould
facility: -
There are different sizes of cast iron moulds ranges in sizes
from 10", 14" & 16" and also 23". The moulds are arranged in the
pit and liquid metal poured in moulds from the ladle with over head
crane.
Radial forging: -
The Technical Data of Radial Forging Section is given below.

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SPECIFICATIONS
INPUT DIMENSIONS :-
650 mm Diameter (ESR Ingot)
23"- Octagon (LFVD Ingot)
Max. Wt. = 7.05 Ton
OUT PUT DIMENSIONS: -
Min. Dia.= 75mm
Square = 80mm
Length Max. = 11000 mm
TUBE DIMENSIONS: -
Min. Bore = 60mm
Max. Bore = 250mm
Starting Length = 4300 mm Max.
FORGING FORCE / DIE = 12000KN
FORGING POWER = 1260KW
NO. OF STROKES / DIE = 200/min
ADJUSTMENT RANGE IN DIA = Upto 330mm
17. Furnaces: -
Radial forging section have the following furnaces, all made by
Stewart & Lloyds Ltd.
18. Batch type furnace: -
3 nos. each having 2 zones
Size 4.5x4.5x2 misters
Oil fired / and LPG fired
Capacity = 50 tons/ heat
Max. Temp=1250°C
Electrode load = 120 Kw
Rate of heating =150°C/hr.

- 14 -
19. Working hearth fumes: -
it is having 2 zones.
Size 13x2.5x2metres
Oil fired/and LPG fired
Capacity 36tons/heat
Electrode load = 110 Kw
Temp=1150°C max.
20. Zones of bogie hearth furnace: -
Size: - 11.00x2.00x2.00 meters
Zones = 7
Capacity = 50tons
Max temperature =1000°C
Electrically, hearted -load: 1800kw
Heating element: - 84nos/fce
H.E material = Nichronthal- 40 i.e., 80-20nicr
Size 1586x45x2.5 mm
Wt/ element = 15kg
Kw/element=21.6
Rate of heating = 200°C/hr
21. Pit furnace: -
Have one zone
Size: 2.0x3.0metres
Temp = 600°C
Electrically heated-load = 72kw
Heating element: Ni-Cr=80-20.

-15-
The invention will be further illustrated by means of the
following Examples which is given by way of illustration and not
by way of limitation.
(a) Charge planned :
It is found the furnace capacity is 2280 kg. Basing on the
furnace capacity the following charge materials were planned to
load/charge.
MSF CLASSIFICATION FORM OF SCRAP QTY (Kg)
IV/9 Strip 1600 kg
III/9 Ingot 570 kg
Mild steel Pressed Bundles 120 kg(l no)
Pure Nickel 75 kg
Fe-Mo 20 kg
Broken Electrodes 15 kg
Total 2390 kg
Considering the oxidation losses of alloy additions, higher
than the required level was added in the charge.
The chemical compositions of charges materials are given
below :

MSFCLAN C S P Si Mn Ni Cr Cu Al
IV/9 0.09 .025 .025 0.13 .30- 0.15 0.02 0.20 0.03
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0.13 MAX MAX MAX .50 MAX MAX MAX 0.09
III/9 0.150.25 .06max .06max .35max 1.00max
All the charge materials were placed in the furnace at a
time.
(b) Fettling: -
After tapping the previous heat, lining is inspected. The
slag-metal line, doorsill, tap hole, spout and damaged area of
hearth are all repaired manually with the ramming mass i.e.,
magnesite.
(c) Charging: -
Roof is opened and furnace is charged with bucket
charger. Initially 80Kg of the carbon steel pressed bundles are
charged. Upon, III/9 ingot was placed. Over that, IV/9 strips are
charged. Finally the remaining 40Kg of pressed bundles (C.S.) were
put.
(d) Power on: -
After completion of charge, roof is placed and power is
ON. Electrodes are lowered down and arc is struck. Furnace is kept
at lower tap i.e., 2 for 15 mins. And when the arc subsides inside
the scrap, maximum tap voltage is used i.e., 180 volts at tap 4. It
took 2 hours for complete melting of the charge materials.
(e) Refining: -

- 17 -
After ensuring the charge is melted, furnace tap is
lowered i.e., at 3 in order to avoid higher temperature. For
maintaining dephosphorisation favorable condition i.e., high
oxidizing atmosphere and high basicity (and low temperature also)
50kg of Iron ore and 15kg mill scale is added along with 50kg of
limestone. As the Mn requirement is above 1.5%, Fe-Mn of 10kg is
also added.
After 40mins slagging was done and sample 1 was
taken.
Keeping in view the reversible nature of phosphor and
still high requirement of Mn, the following additions done.
Lime stone-5okg-For basicity
Mn-metal-10kg-For higher requirement
Mill scale-10kg-For o2 potential
After 40 mins of refining, slag out - II was done and the
following additions were made after 20 mins of slag out- II.
Lime stone-50kg
Fe-Mn-5kg
Mill scale-5kg
After 10mins of additions slag out-Ill was done and again
the following additions were made
Lime stone-50kg-For basicity
Fe-si-12 kg-For still higher requirement
Mn-metal-35 kg-For still higher requirement
Fe-mo-6 kg-For still higher requirement
Pure nickel-5 kg-For still higher requirement
AI-5 kg-For the requirement
After lOmins of refining, sample -II was taken and To
achieve the final requirement, the following additions were made
after sample-II.
Fe-si-15kg-for still higher requirement

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Lime stone-50kg
Again slag out-IV was done and sample-Ill was taken
(f) Slag-off & reducing slag: -
After comparing the above analysis with the required one,
complete slag out (oxide slag) was done and the reducing slag was
made by adding
Coke powder-50kg
CaC2 -5kg} for the removal of 02 in slag
Spar & lime stone-for basicity
The following alloy additions also made for still higher
requirement
Fe-Si-6kg Fe-Mo-6kg pure Ni-8kg Mn-Metal-8kg pure Cu-10kg.
Higher tap position made for higher temperature, which is a
favorable condition for desulphurization along with high basicity and
low 02 potential.
Finishing and tapping the heat: -
Temperature measured and found as 1672°c which is
sufficient for tapping. The melt is covered with the reducing slag
and tapped in the already preheated (upto 900°c temperature)
ladle.
The following additions are made into the ladle for keeping a
right slag.
Lime - 10Kg/ton
Spar - 3Kg/ton
Pet coke -0.3Kg/ton
Fe-Si-3Kg/ton

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AI-1.2Kg/ton
Ramming mass-50Kg
Wire injection is also fed to the ladle as follows
CaSi -50mtrs.
AI-50mtrs.
The following important micro-allay addition are made to the
ladle
Fe-Nb-21/2Kg
Fe-Ti-21/2Kg
During refining the total additions made in the furnace are as
follows: -
Additions Qty (kg)
Lime stone 500
Iron ore 50
Flour spar 50
Coke power 50
Ca-carbide 50
Mill scale 30(shovels)
Fe-Si 33
Fe-Mn 15
Fe-Mo 12
Pure Ni 13
Pure Al 5
Mn metal 53
P Cu 10
(h) Pit practice & teeming: -
Ingot moulds were thoroughly cleaned by wire brush and
acetylene sheet is applied to gins smooth coating for smooth
removal of ingot. Corrugated card board or anti splashing disc or
clear steel borings were kept at the bottom position of moulds to
over come the problem of splashing during top pouring. Dead heads

- 20 -
were placed properly. The contact between mould and dead was
sealed with asbestos threads for leak proof of hot metal as well as
Casey removal of dead head.
(i) Teeming: -
Liquid steel tapped in ladle was taken to pitside with the help
of overhead crane for teeming in moulds of size 10". During this top
pouring ladle nozzle was centered over each hot top of each mould
and was cast one by one in sequence. Total 5nos of wide-end-up
10" square moulds are used.
After completion of teeming in every mould, the hot top was
covered with exothermic powder and oxygen lancing .
The total moulds filled are 41/2, and the total weight of metal
cast was 570x4=2280Kg + 200Kg(approx) = 2480Kg (approx).
(j) Sampling: -
After completion of Teeming, 2No.s of Samples were
collected. These were sent for chemical analysis and found as
follows:
(k) Stripping of ingots: -
Ingots cast in the ingot moulds were stripped off when
solidified.
Solidification time is generally as follows : -
{ingot size in inches (cross section)/2} 2- x mins.
The Tapping temperature calculated as per the Appendix- C
(1) RADIAL FORGING

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Heating was carried out to one of the 4 ingots for subsequent forging as
per the following HT cycle in the batch type furnace No-1, and the Time-
Temperature curve given above shows the result.
The loading and unloading of ingots into the furnace is done by the loader.
Radial forging is a fully automated plant. The 10" ingot has been reduced
to 95 mm Round Comer Square with the single heat. The finish forging Temperature
was foundto be 952°C. After forging, the ingot was water cooled to room temperature.
After breaking of scale, the temperature of ingot was found as 1111°C
Forging started at 10-38 hrs
Temperature found at 10-40 hrs = 1054ºC
Forging finished at 10-45 hrs was at the temperature of 952°C.
Time taken for completion of Forging =■ 07 mins.
Thanao Mechanical Controlled Prooassing
The ingots of 95 mm X 95 mm were reheated at various temperatures label
(1150 to 1300°C) and controlled rolled to 14 mm thick plates. Finished rolling
temperatures were 880°C, 850°C, 800°C and 750°C. Finally the rolled plates were
subjected to either air cooling or water quenching.
Table 1 : Chemical composition (WTPCT of the Steels)

E1e- C Si S P Mn Ni Mo Cu Cr Nb Ti Al
nents
0 0.06^ 0.2- 0.01 0.01 1 1.2- 3 .0- 0 .4- 2.1 1.5 3.04- 0. 02- 0.02
0 0.18 0.7 Max Max 1 1.8 3. 8 1. 0 Max Max 0.09 0. 06 Max
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Determation Ac1 and Ac3 tempereture of the steels
Specimens for dilatometric study were machined from the
forged bars. For low rates of cooling, specimens were 90 mm long
and 6 mm in diameter. Specimens, for high cooling rates were
85 mm long and 6.3 mm in diameter with a 3 mm diameter hole
through the sample centerline. Dilation curves were obtained by
heating the sample (in an argon atmosphere) at a rate of 10°C/s
from room temperature to 1200°C, austinitising at 1200°C for 240
seconds and then cooling at various controlled rates from
0.1°C/s in a Gleeble 1500 thermo mechanical simulator. Phase
transformation temperatures were ontained by radial contraction
measurements as a function of temperatures and samples
formetallography and hardness were removed from the sections at
switch temperature and dimensional changes were measured.
Microatructural Characterisation
Optical, SEM with EDS and TEM with EDS were used for
microstructural characterization and X-ray diffractometric study
was performed to determine the volume fraction of retained austenite
in the TMCP steel.
Evolution of Mechanical Properties
The mechanical properties of TMCP steels were determined by
hardness, Tensile, and Charpy Impact testing.
Results
Table below shows Ac1 and Ac3 temperatures of the steels from
the dilametric Study.
Table : Ac1 and Ac3 temperatures of the steel

Steel Ac1 Ac3
642-685 840-855
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Microstructure
The microstructure at various finished rolling temperatures
show predominantly lath martensite within pancaked grains and
comparatively finer lath size has been obtained for the steel
processed below 800°C finished rolling temperature (FRT).
Transmission Electron Microscopic (TEM) study shows
predominantly lath martensite structure at various FRTs. Formation
of fine twins in the lath is also observed. Selected Area Diffraction
Pattern shows reflection from TiN/TiCN and NbCN along with matrix.
TEM study also reveals fine precipitates interacting with
dislocation and copper particles distributed in the matrix.
Mechanical Properties
Tensile and impact values of the steels are given below :

Tensile properties Impact toughness(CVN)
Hardness UTS YS % Room Temp ~40°C
(VHN) (Mpa) (Mpa) Elongation (Joules) (Joules)
398-452 1680-1750 1375-1450 12 - 17.8 60 - 70 55 - 65
It is a notable feature of this invention that the mechanical
properties achieved in industrial heats in the course of production
of "MICRO MSF-1700" ultra high strength steel are closely similar
to those obtained in laboratory scale heats. In other words,
translation of laboratory scale production into industrial scale
production is quite successful and poses no procedural
difficulties.

-24-
The microstructure of steel produceed by following the
procedure described above has been found to contain a mixture of
bainite and martensite, and the volume fraction of martensite
varies with the rate of cooling. Air-cooled steel shows less
amount of mertensite. The steel thus produced contains higher
amount of carbon in comparison to HSLA-100 steel, whereby the
yield strength and ultimate tensile strength are increased by
~400 to 450 Mpa attended with moderate toughness. This product
possesses strength equivalent to ultra high strength steel.
The steel possesses yield strength to the ~ of 1400 Mpa and
UTS to the ~ of 1700 Mpa along with 15 to 17% elongation and
toughness of 60 to 70 Joules. The strength values are much higher
than those of HSLA-100 steel. In thermo mechanical controlled
processing finish rolling temperature can also be maintained at
a higher level.
The microalloyed high strength steel produced in accordance
with the present invention can be suitably used for making crank-
shaft, hull, structural purposes, and also for making barrels
such as gun barrels and small arms and ammunitions.
As the present invention may be embodied in several forms
without departing from the spirit or essential characteristics
thereof, it should be understood that the above-described example
is not limited by any of the details of the foregoing description,
unless otherwise specified, but rather should be construed broadly
within its spirit and scope as defined in the appended claims
and, therefore, all changes and modifications that fall within
the meets and bounds of the claims, or equivalents of such meets
and bounds, are therefore intended to be embraced by the claims
appended hereafter.

-25-
We claim :
1. Microalloyed ultra high strength steel having the composition-

i) carbon 0.06 - 0.15% by wt.;
ii) phosphorus - 0.01% max by wt.;
iii) sulphur - 0.01% max by wt.;
iv) silicon 0.2 - 0.7% by wt.;
v) manganese 1.2 - 1.8% by wt.;
vi) nickel 3.0 - 3.8% by wt.;
vii) molybdenum 0.4 - 1.0% by wt.;
viii) copper - 1.5% max by wt.;
ix) niobium 0.04 - 0.09% by wt.;
x) titanium 0.02 - 0.08% by wt.;
XX) aluminium 0.02 - 0.03% by wt.;
xii) chromium — 1.5% max by wt.;
. 2. Microalloyed steel as claimed in Claim l, wherein aluminium
and chromium are present in amounts of 0.02% and 1.0% by weight,
respectively.
3. Microalloyed steel as claimed in Claims 1 and 2, wherein
last traces of oxygen in the molten mass in the ladle are removed
by wire injection of CaSi and/or Al in amounts as described
hereinbefore.
4. Microalloyed ultra high strength steel, substantially as
hereinbefore described with particular reference to the
illustrative examples and graphical representations.
SRD/ns/FILE-1/PATENT

-26-
5. A process for preparing micro alloyed ultra high strength
steel as claimed in Claims 1-4, which comprises -
a) introducing charge of raw materials in an electric arc
furnace maintained at lower tap of around 2 for 15 minutes,
using maximum tap voltage of 180 volts at tap 4 after
subsidence of arc till the complete melting of the charge
materials;
b) lowering the furnace tap at 3 to avoid high temperature
followed by addition of iron ore, mill scale and limestone
along with Fe-Mn alloy and then carrying out slagging after
around 40 minutes (slag out I);
c) adding to the charge substances selected from lime
stone, manganese and mill scale, followed by slag out (II)
after 40 minutes of refining;
d) adding after 20 minutes of slag out II in step(c), the
following materials lime stone, Fe-Mn and mill scale are
added and after 10 minutes of addition, and thereafter
slagging out for the third time (III);
e) after slag out III, carrying out addition of lime
stone, Fe-Si, manganese, Fe-Mo, pure nickel, metallic
aluminium as per requirement and continuing refining;
f) after 10 minutes of refining, adding Fe-Si and lime
stone followed by slag out IV;

-27-
g) carrying out complete slag out and making reducing slag
by adding coke podwer, calcium carbide, spar and limestone,
followed by addition of undernoted materials for higher
requirement :
Fe-Si, Fe-Mo, pure Ni-manganese, pure Cu, and covering
the melt with reducing slag and tapping in the ladle preheated
upto around 900°C;
h) adding the following for formation of a right slag :
lime - 10 kg/ton, spar - 3 kg/ton, pet coke - 0.3 kg/ton,
Fe-Si - 3 kg/ton, Al - 1.2 Kg/ton, ramming mass - 50 kg and
feeding 50 metres of Ca-Si and Al to the ladle as wire
injection;
i) adding to the ladle Fe-Nb and Fe-Ti for facilitating
formation of micro-alloy, and
j) pouring the molten mass into moulds, followed by teeming,
stripping of ingots, radial forging and thermo mechanical
processing to obtain the desired products.
6. A process as claimed in Claim 5, wherein the ingots are
released from moulds, subjected to radial forging, cooled to room
temperature, reheated to various temperature levels varying between
1150° and 1300°C, rolled into 14 mm thick plates which were
finally subjected to either air cooling or water quenching.

-28-
7. A process as claimed in Claims 5 and 6, wherein initial
forging temperature employed was around 1054°C, finishing
temperature was around 952°C and time taken for completion of
forging was 7 minutes.
8. A process for preparing microalloyed ultra high strength
steel, substantially as hereinbefore described with particulars
reference to the illustrative Example given hereinbefore.

SHVRS/FJLE-J/JWOtT

Conventional mode of production of high strength steel used
lower carbon concentration, maintaining lower finish rolling
temperatures. Reduction in carbon content during melting increased
cost of melting operation of steel and lower finished rolling
temperatures required high amount of rolling load and energy.
The present invention aims at overcoming of above drawbacks
by enhancing the carbon concentration of steel and using higher
finish rolling temperatures.
This invention provides a novel microalloyed ultra high
strength steel having the composition -

i) carbon 0.06 - 0.15% by wt.;
ii) phosphorus - 0.01% max by wt.;
iii) sulphur - 0.01% max by wt.;
iv) silicon 0.2 - 0.7% by wt.;
v) manganese 1.2 - 1.8% by wt.;
vi) nickel 3.0 - 3.8% by wt.;
vii) molybdenum 0.4 - l.0% by wt.;
viii) copper - 1.5% max by wt.;
ix) niobium 0.04 - 0.09% by wt.;
x) titanium 0.02 - 0.08% by wt.;
xi) aluminium 0.02 - 0.03% by wt.;
xii) chromium - 1.5% max by wt.
The subject invention also provides a process for preparing
the aforesaid ultra high strength steel.

Documents:

00551-kol-2007-abstract.pdf

00551-kol-2007-claims.pdf

00551-kol-2007-correspondence others 1.1.pdf

00551-kol-2007-correspondence others 1.2.pdf

00551-kol-2007-correspondence others.pdf

00551-kol-2007-correspondence.pdf

00551-kol-2007-description complete.pdf

00551-kol-2007-form 1.pdf

00551-kol-2007-form 18.pdf

00551-kol-2007-form 2.pdf

00551-kol-2007-form 3.pdf

00551-kol-2007-form 9 1.1.pdf

00551-kol-2007-form-9.pdf

00551-kol-2007-gpa.pdf

551-KOL-2007-(26-03-2012)-CORRESPONDENCE.pdf

551-KOL-2007-(26-03-2012)-FORM-27.pdf

551-KOL-2007-CANCELLED DOCOMENT-1.1.pdf

551-KOL-2007-CANCELLED DOCUMENTS.pdf

551-KOL-2007-CLAIMS 1.1.pdf

551-KOL-2007-CLAIMS-1.2.pdf

551-KOL-2007-CORRESPONDENCE 1.3.pdf

551-KOL-2007-CORRESPONDENCE-1.4.pdf

551-KOL-2007-DESCRIPTION COMPLETE.pdf

551-KOL-2007-FORM 1.pdf

551-KOL-2007-FORM 2.pdf

551-KOL-2007-FORM 27.pdf

551-KOL-2007-OTHERS 1.1.pdf

551-KOL-2007-OTHERS-1.2.pdf

551-KOL-2007-REPLY TO EXAMINATION REPORT.pdf


Patent Number 235705
Indian Patent Application Number 551/KOL/2007
PG Journal Number 33/2009
Publication Date 14-Aug-2009
Grant Date 11-Aug-2009
Date of Filing 04-Apr-2007
Name of Patentee METAL & STEEL FACTORY
Applicant Address ISHAPORE, P.O. NAWABGANJ, DIST. 24-PARGANAS (NORTH)
Inventors:
# Inventor's Name Inventor's Address
1 CHATTERJEE PROF. DR. SUBRATA DEPARTMENT OF METALLURGY AND MATERIALS ENGINEERING, BENGAL ENGINEERING AND SCIENCE UNIVERSITY SHIBPUR, HOWRAH - 711103
2 CHANDER SUBHASH ISHAPORE, P.O. NAWABGANJ, DIST. 24-PARGANAS (NORTH), WEST BENGAL-743144
3 BANDYOPADHYAY PARTHA SARATHI ISHAPORE, P.O. NAWABGANJ, DIST. 24-PARGANAS (NORTH), WEST BENGAL-743144
PCT International Classification Number C22C38/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA