Steel Quality

Role of Secondary Refining and Continuous Casting

Dr. Santanu Kr Ray
Department of Mechanical Engineering
Indian Institute of Technology, Madras

Module - 01
Lecture - 04
Evaluation of Residuals and Inclusions

Yeah, let me recapitulate a bit what I had discussed in the earlier session I was covering
non metallic inclusions which are known as NMIs then I have talked about you know
there are 2 basic distinctions one is the micro inclusion whether size is less than 10
micron say more or less one to 10 micron range.

(Refer Slide Time: 00:30)

So, these are basically or essentially product of metallurgical processes for example, de-
oxidation, through de-oxidation what about inclusions I have generated we can call them
as indigenous non metallic inclusions and they are usually minor in sizes smaller in sizes
in the ranges of one to 10 micron these are basically oxides and from sulphur you know
sulphides can be form.

So, we can have sulphides also they are also normally very small in size in this range and
then there can be complex oxysulphides combination of sulphides and oxides there can
be occurs different types of oxides I am not only talking of only alumina, there may be
different oxides like TIF2; titanium oxide there may be combination of you know oxides

So, from the metallurgical processes what about inclusions are getting generated they are
finer in size normally in the range of one to 10 micron and then I talked about exogenous
entrapments which are relatively large in size much larger than 10 micron this ranged
one to 10 and those exogenous entrapments are usually larger in size basically where
from they are getting generated they getting generated from the slag entrapment slag may
be from ladle from tundish from the mould there can be re-oxidation products which are
also exogenous entrapment how de-oxidation products are getting generated when liquid
steel will getting expose to air there is re-oxidation

So, this re-oxidation products are also normally larger in size then there may be
refractory erosion products; that means, erosion products from the refractory lining from
the metallurgical vessels of say ladle or the tundish the there are refractory lining in all of
this metallurgical vessels. So, the refractory erosion products are also part of the
exogenous entrapments. So, these are the 3 broad you know geniuses of exogenous
entrapments which are relatively larger in size.

(Refer Slide Time: 02:59)

Then I talked about NMIs the basically encompass sulphides coming from the sulphur of
steel oxides which is coming from the oxygen content at the final stage normally if it is
beyond you know solubility limit they will be oxides if the sulphur is beyond the
solubility limit they will be sulphides precipitations formation of sulphides oxides

Now, I have also talked about the total oxygen in steel total oxygen has 2 components
one is the dissolved another is the oxygen present as oxides I have also mentioned that
where you are properly deoxidizing the steel killing the steel with aluminum for
example, then the. So, dissolved oxygen is very low less than 5 ppm. So, most of the
oxygen present in steel will be as oxide. So, the total oxygen content can gives an
indication of the oxygen present as oxide.

So, therefore, total oxygen content after refining is normally taken as a measure of oxide
cleanliness because the dissolved oxygen is low. So, what about total oxygen is present
we are assuming the majority of it is present as oxide inclusions.

(Refer Slide Time: 04:34)

So, this total oxygen can be taken as a measured of oxide cleanliness is steel then we had
also talked about what are the distribution of inclusion sizes this is very a important
concept when we call a clean steel it is not free from inclusions there are a numerable
inclusions, but fortunately most of the inclusions are smaller in sizes I had given an
example that 1 kg of you know reasonably clean steel I am talking of clean steel not
talking of you know dirty steel they contain as highest 10 to over 8 NMIs .
So, you can imagine how many non metallic inclusion are present in one kg of
reasonably clean steel fortunately most of them inclusions 99.99 percent or more of it are
of smaller size only about 400 are of the 80 to 130 micron size only about 10 are 130 to
200 micron size only the probability of having only one large inclusion in this you know
1 kg of steel of having size 200 to 270 micron size so; that means, most of the inclusions
are very small in size and hence they are benign; that means, they are less harmful. So,
we need not really bother about those very fine inclusions what we have to bother about
is a few large NMIs which are really harmful from the quality point of view by large I
am again repeating we are meaning more than 5 pmm; 50 micron size 5 0; that means,
inclusions which are larger than 50 micron, they are really harmful and we have to be
very careful about those, but incidentally we I must mention the detection of these few
rather very few macro inclusions in steel is that really difficult.

Now, today I will discuss how inclusions are detected in steel what are the different ways
how small you know miner small inclusions or micro inclusions can be detected how
macro inclusions can be detected which are very difficult I have told and how they can
be detected now let us go one by one to these aspects.

(Refer Slide Time: 06:55)

I am now talking about evaluation of residuals and NMIs first let me talk about what is
the process route how steel is produced in commercial you knows level or commercial
scale it can be 2 broad routes for the production normal grades of steel one is the blast
furnace basic oxygen furnace and then secondary refining and casting one is this route
another is DRI; that means, direct reduction iron electric arc furnace and then secondary
refining and continuous casting.

So, the when a before secondary refining which is actually the little metallurgy part of
the steel where you can do lot of refining lot of quality improvement in steel we have 2
broad categories either blast furnace BOF route or direct reduction iron which is also
known as sponge iron and electric arc furnace route finally, of course, we have to do
whether we had doing producing steel by BF BOF or DRI EAF the final processing has
to be secondary refining or little metallurgy and of course, the steel has to be final finally,
cast whether true in got route or through contentious casting route.

Now, when we are talking of quality of steel we have to put emphasis on secondary
refining and casting because most of the refining is possible only at this stages. So, let us
try to understand where from we will get the samples you know for quality evaluation;
obviously, we have to take the samples from the final stages of refining or during casting
if it is possible.

So, let us see what are the stages normally samples for evaluation of quality had taken
from liquid steel; that means, liquid steel in the ladle if it is done through continuous
casting it can be taken from tundish or in certain cases it can be taken from the mould
also if it is necessary to evaluate what is the quality level of liquid steel in mould it is
possible.

So, liquid steel evaluation if you are interested in we can take samples either from the
ladle from the tundish or from the mould how the liquid steel sample is taken we can
take a you know small cup of or a cylinder of steel using which we can take a liquid steel
sample it has to be must in the liquid bath we have to be careful does we take a
homogeneous part of the liquid steel. So, it has to be you know slight interior in the bath
not exactly at the top not at bottom somewhere in between we have to take the liquid
steel sample we can take solid steel sample also where from we have to take the sample
then we have to take from the cast slab or bloom or billet; that means, once the slab has
been cast or the bloom or the billet has been cast we can cut small pieces from the slab
bloom or billet again we have to be careful that is its sample have to be not from the top
not from the bottom of surface, but somewhere from in between. So, there is a process of
taking the sample again if you are interested in evaluating the quality of the final
product.

Then we can take sample solid sample; obviously, from the final product final product
means it can be hot role product it can be hot role plate it can be hot role coil it can be
you know forged product forging it can be even coal load steel we can take samples from
those products and evaluate. So, basically for evaluation of residuals and NMIs samples
can be taken either from the liquid stage; obviously, from the final stage of refining
because I mean that is the final stage where the quality has more or less come to a
particular level before that you know we cannot take sample before that because after
that many refining actions will be there. So, we will be interested in getting the quality at
the final stage of refining. So, we take samples either from the ladle or tundish or mould
basically the liquid steel sample I am talking of at this levels or we can take cast slab or
bloom or billet samples we can take samples from the final product as well.

(Refer Slide Time: 11:45)

Now, let us try to understand how do you evaluate this is very important we have taken
samples we have been careful the sample represent a homogeneous mass whether from
the liquid or from the solid or from the final product we have ensure the sample are not
from the surfaces it is from the interior whether it is liquid or solid now let us come to
the different aspects of quality which I have already covered for example, if you are
interested in knowing what are the sulphur and phosphors where from we get
information on these 2 elements these are part of the routine steel analysis you know
steel is analyzed at the stage of preparation of the sample from liquid steel; that means,
sample is taken from liquid steel sample is prepared very fast and then they are evaluated
by XRF or may be optical emission nowadays that is facility for online evaluation it is
very fast sample is taken it is just some surface is polished to get a good ready and
immediately analysis can be done.

So, as I was telling you sulphur and phosphors which are very 2 important residuals in
steel we can get information in these information about these 2 elements from routine
steel analysis which covered sulphur phosphors.

Now, I have told you the total oxygen is a very important parameter which normally we
do not measure in routine steel analysis, but from the quality point of view total oxygen
should be measured particularly for evaluating the oxide cleanliness of steel. So, how can
it be done using small machines samples what do I mean by this from the samples which
are taken for routine steel analysis we can cut small samples and then machine those say
the diameter may be you know 5 millimeter and the length may be 5 to 10 millimeter;
that means, cylindrical samples small cylindrical samples can be machined which can be
analyzed by oxygen nitrogen analyzer.

We can analyze both total oxygen and total nitrogen from this analysis. So, total oxygen
and total nitrogen can be analyzed using very small cylindrical samples which are
machined from samples we have collected either from the liquid steel or from the solid
steel these are this evaluations. That means, this determination of total oxygen and
nitrogen can be done through oxygen nitrogen analyzer it is a you know is a very
common analytical tool for evaluation of quality and we must use this for evaluation of
total oxygen and total nitrogen in steel one thing we have to keep in mind here we are
preparing machined samples we have to be careful the during machining the sample does
not get heated up.

Then what is going to happen is we are going to oxidize the steel samples small samples
oxidizing means we are unnecessary creating more oxygen in steel. So, if you analyze or
oxidize sample whatever you readings will get will be erroneous it will not reflect the
real total oxygen in the sample because we have additionally put some oxygen in the
steel. So, we have to be careful not to heat up the samples during machining in this
regard there is no change in nitrogen when sample is getting heated up we increase that
total oxygen in steel because of oxidation, but there is no nitrogenation of the steel.

So, nitrogen remains same. So, from nitrogen analysis also we can understand before and
after like if you if you machine it too much if the sample gets heated up we will find that
oxygen you know readings is going up, but nitrogen reading does not increase. So, that
gives an indication that you know there has been some increase in oxygen during
machining. So, we have to be careful about that. So, that we do not get an erroneous
result.

Now, how do evaluate inclusions I have talked about micro inclusions which are small in
size say about less than 10 micron in size; obviously, we cannot see this with normal eye
we have to use optical microscope. So, how do we see micro inclusions under optical
microscope we have to polish the surface? So, that there are no you know abbreviations
of the surface the surface is like mirror we call it a mirror finish. So, if you polish the
surface in this fashion we can really see micro inclusions in the sample.

Now, for looking at macro inclusion as I have told you micro inclusions are very few in
numbers. So, we can see numerable micro inclusions under microscope, but there will be
possibly very few or we may not even fined macro inclusions on the microscope. So,
what we do what is the way there is a technique called slime extraction; that means, the
steel sample whatever the machine steel sample whatever has been taken from the you
know either liquid steel or solid steel after machining it is slightly bigger than you know
samples for oxygen nitrogen. So, these samples can be electrolyzed which is called slime
extraction.

So, after electrolysis you know what will be electrolyzed the steel will be taken into the
solution in the electrolysis electrolytic solution and what will remain in the as slime are
the macro inclusions. So, those slime after extraction we can see those under you know
different evaluation techniques like under maybe we can use SEM; to find out what are
the constituents we can see those under at low magnification an microscope to find out
what are the sizes these are the techniques of using macro inclusions. So, we should
know what are the macro inclusions; that means, there are constituents chemical
chemistry chemical constituents and what are the size distributions likewise for micro
inclusions as well we should know what are the type of inclusions and what are the size
distributions.

Now, as I was talking about we should know the type of inclusions of the chemistry of
inclusions whether micro or macro how do you do that there is a technique called x ray
analysis using wavelength dispersion or energy dispersion there are attachment these are
attachments in SEM; SEM is scanning electron microscopes when you put the samples
under scanning electron microscope we can see the normal secondary electron images
we can also see are also rather evaluate what are the elements present we can always also
know what are the elements present in those inclusions by this attachments wavelength
dispersive and energy dispersive of x ray attachments basically what is the technique
whenever electronics falling on the samples in scanning electron micro scope x rays
elemental x rays are also getting generated.

So, depending on what are the elements presenting in the samples we have different
wavelengths for example, if we have calcium in the sample like you I have told you
calcium oxides is a very common you know NMI non metallic inclusion in steel like if
you have a slack sample you may have calcium oxide in it to certain extent. So, whether
that is calcium in the sample we can get from this attachment there will be a typical
wavelength of calcium either from the wave length or the energy of that whatever x ray
is getting generated if we catch those x ray. If we detect those x ray either we know as a
review identify the wave length or the energy of the x ray we know what are the
elements present because every element will have different wave length of x rays which
are getting generated.

So, this is very very important this technique has been used extensively in recent years to
identify the type of elements and from that we can find out what are the constituents like
if we you know the calcium is present oxygen is present we know it is calcium oxide if
you know fluorine is present calcium is present and we know to what extent they at
present we know it is calcium florid. Similarly all constituents can be evaluated we can
get an idea even quantitative idea if you have a standard samples like how much of
calcium oxide is present not only if the qualitative point of view from the qualitative
point of view quantitatively also we can identified how much of this constituents are
present in inclusions even in case of you know surface defects as I have told you the
defects when if the inclusions are more in number you know large in size they can show
up at the surface of the product as in defect either as a crack or there may be a you know
entrapment coming up to the surface.

So, we can know; what are the constituents present using this technique we have to make
a small sample from that preserving the constituents they should not get damaged and
then we analyze. So, under evaluation methods sulphur phosphorus can we can get from
routine steel analysis we know what is the phosphorus if it is less than 0 1 5 or 0 2 5
sulphur how much is it whether it is 0 0 5 0 0 8 0 1 0 if sulphur is low less than 0 0 5 we
know sulphur is will be less if phosphorus is low we know that the deleterious effect of
phosphors will be much less in the steel we know what is the total oxygen from oxygen
nitrogen analyzer we know what is the total nitrogen. So, we know how much of oxide
cleanliness actually we should get in the sample in the final product micro inclusions we
can observed on the optical microscope macro inclusions we can observe using slime
extraction; that means, through electrolysis process and we know what are the
constituents using WDX or EDX attachments of scanning electron microscope.

So, these are the different techniques by which we can evaluate the different quality
parameters in steel whether these are sulphur phosphorus; that means, the you know the
quantity of that quantity of that residuals or oxygen nitrogen how much total oxygen is
present whether it is the inclusions we know their sizes, we know what are the
inclusions, we know what are that size distributions, we know they are quantitative value
whether is the volume fraction is less than point one we call it clean steel or it is more
then we call it is a relatively dirty steel unclean steel.

So, what are these parameters we must evaluate this to understand quantitatively what is
the level of the quality in the steel we are talking about and then we decide whether this
is for the particular application or not now we should remember certain important issues
during this evaluation whatever data.
(Refer Slide Time: 24:26)

We are getting from this evaluations we have to be very careful about those we are
analyzing these data first I have talk to you that when you are evaluating micro
inclusions under optical microscope what any inclusion under optical microscope what
we are getting is basically a 2 d 2 dimensional image because basically we are looking at
a surface may be we are to look at hundred surfaces to get an average, but steel it is a
surface 2 dimensional surface. So, how do you know what is the distribution of
inclusions in a in the bulk of the sample in the volume of sample. So, it is necessary to
confer these 2 dimensional distribution to 3 dimensional distribution which is more
realistic we should be getting more information have would the 3 dimensional
distribution of inclusions in steel.

So, by a simple relationship this is the relationship we can convert the 2 dimensional
distribution which is normally obtained through optical microscopic observation 2 a
more realistic 3 dimensional yeah information like how is it done this n 2 d is basically
the number of inclusions per square millimeter of the sample we are looking at sample
surface we are looking at. So, if you want to know what is the 3 dimensional; that means,
what is the number of inclusions per cubic meter we can use this n 2 d value by dividing
it with the inclusion diameter which is by let us take an average inclusion diameter this d
p is the inclusion diameter in micron micrometer.
So, dividing this n 2 d by a d p and multiplying it 10 to the power twelve this is the
conversion factor we can get the 3 dimensional number of inclusions per cubic meter. So,
what is what I am trying to tell let us take a particular size of inclusion say 60 millimeter
some 60 to 65 millimeter range we have got a distribution in number in the 2
dimensional observations.

Now, what should is what should be these numbered in 3 dimension for this 60 to
seventy millimeter their size. So, let us take an average; that means, 60 to 70 average is
65 we divide the number of 2 d and 2 d divided by this and multiplied 10 to the power
twelve we get the number of inclusions of this average diameter in a you know in a in an
sample of one micrometer.

So, by this way we can get this is this is square micrometer this is not millimeter. So, by
this way we know; what are the 3 dimensional figures which is a more realistic figure.

(Refer Slide Time: 27:33)

Now let us try to go in to some other issues we are talked about how these inclusions
whether it is a micro and macro can be evaluated, but you know this observation of the
shapes shape is also very important I have talked about the number the sizes, but mostly
they are not necessary always spherical a liquid steel these are spherical of course,, but
we are when you are deforming the steel; that means, when you are using a role steel or a
forged steel we will get inclusions of different shapes even under you know liquid steel
all inclusions are not of spherical shape that is certain inclusions may there might be
having a different shape might be having a you know triangular shape trapezoid shape
and so on and so forth.

So, what is important to identify the shape also the content that was the volume fraction
size distribution what are the numbers for a particular sizes of this micro inclusion under
macroscope under the microscope of the macro by slime extraction, but if these
evaluation we have to keep in mind these are very very time consuming what do I mean
right we have taken the samples we have polish the samples we are putting in the
microscope may be we have to look at hundred different surfaces to get a realistic view
to get a statistical view this electrolysis for micro or macro and inclusions by slime
extraction technique takes lot of time.

So, all these techniques are useful, but they are time consuming these are essentially post
mortem analysis; that means, the steel has already been made it has been processed after
that only we are getting what is the level of quality is it really useful may be yes once the
steel has been made once the steel has performed in service may be you want to know if
the it has not performed well what was the problem then it is useful. So, it is basically
sort of post mortem analysis; that means, after the steel has been made it has been
process then it has been made into a product we are trying to get the information because
these are the time taking process we do not know when the steel is under preparation or
you know refining under casting under rolling we do not know we do not get this results.

So, these are time consuming, but in contrast analysis of sulphur as element or total
oxygen is very fast because as I told you earlier nowadays even online analysis is
possible for these elements; that means, when the steel is under processing; that means,
when the steel is even getting cast we can get this analysis.

So, we know from this fast analysis of sulphur and total oxygen what will be the
possibility of getting sulphide inclusion in that steel what will be the possibility of
getting oxide cleanliness in that steel. So, when the steel is cast by the time we have the
information casting will take may be say it can take from half an hour to may be one and
half hour. So, in during this casting itself by the time we had finish casting all this
information and sulphur and total oxygen will be available to the steel maker.

So, at that stage of steel casting the steel maker knows what is the possibility of quality
in that cast what will be the level of sulphide inclusion what is the level of total oxygen I
am talking of total oxygen here it does not matter in which form oxide is present it may
be alumina it may be CEO, it may be you know MNO it may be anything. So, total oxide
inclusion we can get an idea from total oxygen as I have told earlier.

So, this is a very fast and we can get this information by the time steel is getting cast. So,
if you find that total oxygen sulphur is beyond the ranges which has stipulated for the
particular product you know we can decide whether this slab or this bloom or this billet
whether at all we should process for the subsequent product because these are going to
give us very undesirable quality this elements analysis of this elements sulphur and total
oxygen give us indication what is the level of quality unlike you know this analysis of
inclusion or whether it is micro and macro which are time consuming which take lot of
time.

So, when the steel has been cast we do not know what is the level of inclusions real
inclusions we have not evaluated it is not possible to get the analysis by that time, but
this sulphur and total oxygen analysis we already have by the stem by the time the steel
is cast. So, we know whether the steel will be relatively clean or relatively unclean. So,
we will get we can take a decision at this stage we can take a disposition decision; that
means, whether this slab or this bloom or this billet should be process for this product or
should be process for some other inferior product quality of inferior steel like you know
in no steel is thrown away if the steel is relatively inferior quality it can be a process for a
particular quality requirement where a particular level of application is the level of
quality is tolerable, but that quality may not be tolerable for a very string in a apparition.

So, a disposition decision can be taken based on the analysis of sulphur and total oxygen
in the cast steel this aspect is very important and good steel makers nowadays a taking
this decisions on quality based on analysis of sulphur and total oxygen they are not
waiting for the analysis for the evaluation of the inclusions which will take a lot of time
that taking decision based on sulphur and total oxygen in the steel.

So, we can decide whether this steel which is steel in the cast steel which has not been
processed whether we process it because we know that this particular steel or the product
will not give rise to good quality. So, it will not fulfill the string and requirements. So,
what is the point it processing this cast steel rather we should process it for some inferior
quality of steel that is always a as I have told that is always a particular steel applications
depending on the quality.

So, we can take a decision on disposition of that particular you know steel cast
depending on how much of sulphur how much of total oxygen we have obtained
therefore, this sulphur and total oxygen are used for a quick decision on the level of
quality in the cast steel this is very very important we have to keep in mind that all
decision nowadays are taken based on this sulphur and total oxygen add the stage of cast
itself we do not wait for the steel to be processed and then we get a very bad quality on
the surface because we know if the sulphur is high or the total oxygen is high or even the
you know if the sulphur is low, but the total oxygen is high; that means, the oxide
cleanliness will be poor, if the sulphur is more total oxygen is less; that means, sulphide
inclusions will be poor.

So, we know from this data; what is going to be the quality. So, we take a decision at this
stage itself I am trying to (Refer Time: 35:41) on this because please remember at this
stage only we have to take a decision we should not allow expensive processing of the
steel and then come to the conclusion that is this steel this product does not have the
requisite quality we take a decision before that; before the steel has been rolled or
processed I think you should appreciate the important of this decision.