Clean Steel Assessment

Chad R. Cathcart1

1
Stelco Inc.
2330 Regional Road 3, Nanticoke, ON N0A 1L0
Phone: +1.519.587.4541
Email: chad.cathcart@stelco.com

Keywords: Clean Steel, Steel Cleanness, Alumina, Inclusions, SEM Analysis, Sliver

INTRODUCTION
Professor Kent Peaslee was a strong advocate of the steelmaking industry throughout his career but particularly once he
entered the academic world. This conviction lent itself to many of the projects he worked on, with the goal of improving the
long-term sustainability of our industry. One of his passions surrounded the attraction and retention of the highly skilled
talent that is required to keep the industry competitive, productive and technically competent.1,2 His focus on nurturing the
next generation of skilled talent was evident in his lectures and public presentations. The Association for Iron and Steel
Technology has chosen to celebrate the memory of Professor Peaslee with a volume on various aspects of clean steel
production, measurement and application. This paper is an introduction to clean steel production and measurement, aimed
primarily at the young Metallurgist beginning their career but is also applicable to the non-Metallurgist. The references
included provide an avenue for a more in-depth study into particular aspects of clean steel assessment.

WHAT IS CLEAN STEEL?

Clean steel, in its most literal interpretation, has low levels of both solute (e.g. sulphur, phosphorous and nitrogen) and
residual elements (e.g. copper, nickel and tin), along with a low level of non-metallic inclusions. To clarify the meaning of
clean steel, Cramb3 defined the former two items as “high purity” and “low residual” steels, thus leaving clean steel to refer
to the level of non-metallic inclusions. For our purposes, clean steel refers to the production of steel with sufficiently low
levels of non-metallic inclusions so as not to have a detrimental impact on either surface quality or final product mechanical
properties (e.g. strength, formability, ductility, fatigue life) for the desired application. From this definition, the exact nature
of clean steel will have a different meaning depending on the production route and more importantly, the expected in-service
characteristics of the product. To the casual observer, the concept of clean steel would refer to the reduction, or potentially
the absence, of non-metallic inclusions. However, this is not required, or sometimes even desired, for every application. As
an example, steel produced for a basic flat-roll product with limited forming requirements would have significantly different
expectations than steel produced for bearing applications. Thus, inclusions that would cause a significant issue for one
application may have no influence on another. For instance, MnS inclusions have a significant detrimental effect on
formability for sheet steels but are a desired inclusion phase in free-machining steels. There are many other examples of
“Inclusion Engineering” to produce a desired population of non-metallic inclusions in terms of their size, distribution and
composition. Clean steel is, therefore, dependent on the customer’s application and the likelihood of a given inclusion to
cause a product defect. Customer demands to reduce defect rates lead to stricter requirements for a given application. This
drives the need to develop methods for clean steel assessment with a view to controlling and ultimately tailoring the inclusion
population to the level required by the customer’s application.
The primary focus of clean steel production is to avoid the formation and promote the removal of macro-inclusions. These
inclusions are the most detrimental to final steel properties. Reducing the population of micro-inclusions is also important to
prevent the agglomeration of these micro-inclusions late in the process when they can no longer be removed and avoid the
creation of new macro-inclusions. The size of macro-inclusion that will cause a problem will vary by application. Several
publications3-6 have compiled summaries of the critical inclusion sizes that can be tolerated for various end uses as

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summarised in Table I. These inclusion sizes are a general guideline and are being challenged by continuing customer
demands for higher performing steels.

Table I: Critical Inclusion Sizes for Various Applications3-6

Steel Product Critical Size (µm)
Cold Rolled Sheet 240
UOE-Pipe 200
Heavy Plate 200 (cluster)
ERW-Pipe 100 – 140
Automotive & Deep Drawing Sheet 100
Cold Forgings 100
Draw and Ironed cans 20 – 50
Steel Cord 30
Wire 20
Ball Bearings 15
Tire Cord 10 – 20
Lead frame for LSI 5
Shadow Mask for CRT 5

This paper will review some of the available methods to determine the cleanness of a sample while providing information on
how this information can then be related back to the process. The focus of this paper is on those clean steel assessment
techniques that can be readily applied in a plant production environment.

STEEL CLEANNESS ASSESSMENT METHODS

There are many methods currently in use to evaluate steel cleanness. These range from direct quantitative measurements of
inclusion size, density, distribution, shape and composition to methods that, while using inclusion observations, can only
provide qualitative information. There are also indirect methods that rely on measurements of elements or compositional
changes that can be related to possible changes in steel cleanness. In addition, the use of a defined quality or process event
can be used as an indicator of steel cleanness. Direct methods provide the most accurate information, but are typically costly
and time consuming. Indirect methods and quality/process event indicators can provide useful information but normally as a
qualitative indicator only. Whatever method is chosen must produce reliable and repeatable results if it is to be used for
evaluation of the impact of process modifications on steel cleanness. Zhang and Thomas4,5 provided a comprehensive review
of over twenty techniques for assessment of steel cleanness. Table II is a modified and updated version of the one presented
in their review. This table provides a brief overview of the advantages and disadvantages of some of the more commonly
applied direct and indirect inclusion measurement techniques.
As indicated in Table II, there are numerous methods available to observe and measure steel cleanness. The question then
becomes: how do we use these methods to determine how clean our steel is, benchmark a given heat or process, evaluate
new operating equipment and practices, or for root cause analysis of an operational or quality issue?

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 Table II: Comparison of Methods for Evaluating Steel Cleanness4,5
Method
Optical Microscopy (OM)
OM with Automated Image Analysis
Sulphur Print / Macro-Etch
Scanning Electron Microscopy (SEM)
Automated SEM systems
Optical Emission Spectroscopy with
Pulse Discrimination Analysis (OES-
PDA)
Slab Step Milling
Electrolytic Extraction / Slime
Remelt Buttons (Electron-Beam Melting
/ Cold Crucible Melting)
Ultrasonic (Conventional, High
Frequency, MIDAS, LSHR, Scanning
Acoustic Microscope)
Cathodoluminescence Microscopy
Indirect - Total Oxygen Measurement
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Advantages
- Inclusion amount, size distribution
(mainly 5-30µm) & morphology
possible
- Similar to above
- Large area covered
- Inexpensive
- 3-dimensional morphology can be
revealed
- Composition measured (with
EDX/EPMA)
- Inclusion amount, size distribution (1-
30 µm)
- Composition measured
- Large quantity of inclusions measured
- Measures total oxygen, distribution and
composition
- Fast
- Inclusion distribution
- Large area covered
- Accurate inclusion amount measured
- Captures rare large inclusions
- With subsequent analysis, can get 3-D
size distribution and morphology
- Accurate inclusion amount measured
- Size distribution estimate
- Detects rare large inclusions
- Large areas can be measured
- Can be automated
- Relatively large area can be scanned
- Rapid identification of various phases
and distribution
- Quick
- Inexpensive
Disadvantages
- No composition data
- Two dimensional; difficulties in
interpreting complex 3-D inclusions
- Time consuming to obtain inclusion
size/distribution data
- No composition data
- Two dimensional; difficulties in
interpreting complex 3-D inclusions
- No amount, composition or size
distribution
- Macro-inclusions/segregation only
- Can be limited by steel chemistry
- Measures only individual inclusions
- Time consuming
- Small sample size precludes likelihood
of observing macro-inclusions
- Observations are typically two-
dimensional.
- No morphology data
- Only for inclusions < 12 µm
- Plant dependent
- Extremely Time consuming
- Time consuming to dissolve entire
large sample
- Manual inclusion observation/counting
- No morphology data
- Low melting point inclusions can
easily fuse and agglomerate
- Slow and expensive
- No morphology or composition data
- Only for macro-inclusions (> 40 µm)
- Both gas and inclusions counted
- Impact of surface quality and structural
homogeneity
- No morphology, size, or composition
data
- Qualitative phase information based on
reference colours
- No morphology, size or composition
data
- Highly dependent on sample quality
 Indirect – Process Based Measurements
Indirect – Mechanical Property Tests
(e.g. Formability, Fatigue testing)
Indirect – Downstream Inspection results
(e.g. Automated surface inspection
systems, ultrasonic testing)
- Inexpensive, data is typically readily - Can be time consuming to filter out
available process noise
- May lack sensitivity to accurately
measure cleanness
- Relevant to potential end user - Time Consuming
- Large areas can be tested - No morphology, size or composition
data
- Possibility to detect impact of rare
large inclusions - Influence of subsequent downstream
operations
- Relevant to potential end user - No morphology, size or composition
data
- Large areas can be tested
- Influence of subsequent downstream
operations
- Timeliness of feedback

Selection of the appropriate method for inclusion measurement will depend on the nature of the problem to be addressed, the
size and type of inclusions to be measured, the time available for feedback and access to the necessary equipment. Hénault7
has presented a visual representation of the detection limit of some of the more common measurement techniques relative to
the volume of steel evaluated as shown in Figure 1. One of these techniques may provide the required information, but
typically, a combination of techniques is used. Clean steel assessment can be undertaken through samples or process
observations during liquid steel refining and casting as well as through samples or inspection data on semi-finished or
finished product.

Figure 1: Detection limit according to the mass of steel analysed through different test methods7

INDIRECT ASSESSMENT METHODS

As the name implies, indirect assessment methods do not provide explicit quantitative information on the size, chemistry or
distribution of non-metallic inclusions. They are useful in providing a qualitative evaluation of the relative cleanness of a
heat or process. In addition, these techniques typically do not require special sampling or analysis methods.

Total Oxygen Measurement

Total oxygen (OT) measurement is perhaps the most widely used method for indirect assessment of steel cleanness.8-15 The
assumption behind this technique is that OT is the sum of the dissolved (free) oxygen and the oxygen combined as non-
metallic inclusions. As free oxygen in killed steels is typically on the order of 3-5 ppm, and does not vary significantly from
heat to heat, then any variance in OT is due to the variance in the level of oxide inclusions in the steel. Yang et al8,9 used OT

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measurements to determine the impact of various deoxidizers on inclusion levels and for comparison of various tundish and
SEN design modifications. While OT is a useful method for comparing relative cleanness, it provides no information on
inclusion chemistry, size, distribution or morphology. Due to the small sample size used for OT measurement, sample quality
is important, as a single large exogenous inclusion (e.g. slag or refractory) will dramatically alter results. This also extends to
indigenous inclusions, as the presence of an isolated macro-inclusion will result in an erroneously high reading. Despite
these issues, OT is still a widely used technique to provide relative determinations of oxide inclusion levels.

Process Measurements
Zhang and Thomas,4,5 in their comprehensive review of cleanness evaluation, referenced several indirect methods that could
be used including the measurement of nitrogen pick-up, aluminum loss and slag composition. Aluminum loss between the
secondary refining station and caster has been correlated with inclusion composition and to OT at the Caster.16,17 While these
techniques may still provide useful information, advancements in steel processing have reduced these indicators to levels
where they lack sufficient sensitivity for proper evaluation of steel cleanness. Readers interested in additional information on
these techniques are referred to the references noted above. An additional method reviewed by Zhang and Thomas4,5 was the
use of submerged entry nozzle (SEN) clogging as an indicator of cleanness. While clogging can be caused by other factors,
such as refractory failure or freezing, the most typical cause is the build-up of non-metallic inclusions due to poor steel
cleanness. Figure 2 compares mould level and stopper rod position for heats with various degrees of clogging from non-
metallic inclusion build-up in the SEN. Figure 2a shows the case for no clogging, and all process indicators (stopper rod
position, mould level and cast speed) are steady. Figure 2b demonstrates moderate clogging behaviour, with both mould
level and cast speed remaining steady. However, stopper rod position is continually opening over the course of the heat to
maintain throughput. Figure 2c exhibits a more severe clogging case and, as in 2b, the stopper rod position is opening to
maintain mould level but has become more erratic due to the build-up and release of clogging material that is now impacting
mould level control. In addition, it can be observed that cast speed was reduced to compensate for the clogging in this
example. Finally, Figure 2d is an example of rapid and catastrophic clogging behaviour. In this case, the stopper opening
rate has become extreme with significant events caused by the build-up and release of clogging material resulting in
significant mould level variations and erratic speed control.

Mould Level Rod Position Argon Flow Argon Pressure Cast Speed Mould Level Rod Position Argon Flow Argon Pressure Cast Speed

(a) No Clogging (b) Moderate Clogging

Mould Level Rod Position Argon Flow Argon Pressure Cast Speed Mould Level Rod Position Argon Flow Argon Pressure Cast Speed

(c) Severe Clogging (d) Catastrophic Clogging

Figure 2: Comparison of various degrees of Clogging
These figures indicate that a measurement of stopper/gate position or mould level fluctuation can provide an indication of the
degree of clogging present and, by extension, provide a relative measure of steel cleanness. The simplest method is to use a
measure of the mould level deviation as an indicator of problems due to clogging.18,19 But the influence of other factors on
mould level variation and the desire to better understand clogging behaviour has led to the development of a Clogging Index

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or Nozzle Clogging Factor20-23 to evaluate the degree of clogging experienced and relate it to either upstream steelmaking
factors or downstream quality issues. This type of index has been used by Story et al24 to correlate nozzle clogging to the
inclusion population present in the liquid steel. For steels that are calcium treated the degree of clogging can provide a useful
estimation of the degree of inclusion modification.19,20
As previously discussed, measuring the degree of nozzle clogging can provide an indication of the relative cleanness of the
steel. Furthermore, nozzle clogging can also provide information on the nature of inclusions present in the liquid steel
through direct observation of the clogged material.18,25-27 Tuttle et al22 used the analysis of clogged nozzles to evaluate
whether the permeability of the refractory components was a contributing factor in the observed clogging. Direct
observations of the nature of the clogging material, particularly when combined with in-process inclusion observations,
allows for a determination of the potential source of the clogging material. Fuhr et al28 and Rastogi and Cramb29 provided a
comprehensive overview of techniques to evaluate the clogging mass for identification of potential sources of the non-
metallic inclusions contained within. Similar work relating nozzle clogging observations to process parameters and direct or
indirect measurements has also been performed.30-33 Maddalena et al34 completed their analysis for Stainless Steels and
provided an overview of the various inclusions and some of the factors influencing their formation and deposition which is
reproduced below in Table III.

Table III: Solid Inclusions in SEN Build-up34

Downstream Product Assessment

Evaluation of failures during customer use or processing, while an indirect assessment method, provides the most direct
information regarding the actual impact of steel cleanness. Unfortunately, this is also the most undesirable method of clean
steel assessment from both a cost and reputational point of view. Similar information can be obtained through mechanical
property tests on the product (e.g. HIC tests for sour-service plate or fatigue tests on bearings) or by in-process inspections
(e.g. visual/automated surface inspection or ultrasonic testing). Additional information can be obtained by sampling the

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failures and directly examining the inclusions to determine the location, type and size of the inclusion causing the failure.
However, particularly for parts that have failed during customer processing or use, traceability of the failure back to its
original heat can be problematic. Timeliness of feedback may also be an issue. In many cases, this results in knowledge of
the failure mechanism based on defect analysis but little information for determining actual root cause. In the case of an
isolated failure, there is also the lack of statistical certainty regarding the potential process conditions that resulted in the
failure. The advent of automated inspection systems through subsequent downstream processes goes a significant way to
address these issues.
Automated inspections systems can inspect each piece of steel, thus providing a sample size that can now be statistically
correlated to upstream process parameters. Any defect found can be contained and dealt with in-house, avoiding costly
failures for the end customer. The comparison of overall reject levels back to various process parameters is the simplest
method of evaluation.35-39 This method becomes more useful if the defects can be classified into similar groups to avoid the
influence of defects unrelated to steelmaking operations. Historically, inspection was done manually, however, modern
automated surface inspection systems perform a similar task. This is most commonly done for sliver type defects and many
papers30, 40-43 have investigated the impact of items such as mould fluid flow or stopper rod movement on the “sliver index”.
This type of analysis can be very useful if the slivers observed have a common root cause. The trouble arises if there are
multiple potential root causes that lead to defects with a similar outward appearance. Taking slivers, for example, they could
just as easily be related to FeO based defects (whether from the caster or the rolling mill), alumina based defects (from
steelmaking inclusions), or due to entrapment of exogenous inclusions (e.g. slag or mould powder). This is effectively
illustrated by Figure 3, which compares the appearance (top image of each set) and optical metallographic analysis (bottom
image of each set) of three pairs of outwardly comparable defects. Each set of defects has the same macro appearance and
display similar characteristics when examined by optical microscopy but have different root causes. The defects on the left
(a, c and e) were determined to be FeO based defects from the hot rolling mill while those on the right (b, d and f) are
alumina based defects from the steelmaking process. The root causes for each set of defects are dramatically different and an
investigation based on the global sliver index without confirming root cause would result in erroneous conclusions or provide
results that were so sporadic as to be meaningless. The conclusion is that while indirect assessment methods are useful, they
lack specific information regarding the true nature of the defect and the ability to determine root cause. Therefore, when
using any type of indirect assessment method, and particularly when downstream product assessments are used, it is
necessary to combine the indirect observations with some type of direct observation to aid in determining the actual root
cause of the defect.

DIRECT ASSESSMENT METHODS

As outlined in Table II there are several methods that can be used to directly measure the cleanness of steel. Like the indirect
methods outlined above, direct assessments can be used on steel at any point during the production process. Historically, the
most common assessment was performed on the finished product. This was typically performed following a failure at a
downstream unit or end customer. Current trends have been increasingly focused on performing cleanness assessments
earlier in the process with a focus on prevention rather than detection of defects. The following sections will provide an
overview of those methods most commonly available to the Mill Metallurgist.

3a) FeO based Seam 3b) Al2O3 based Seam

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 3c) FeO based Sliver 3d) Al2O3 based Sliver

3e) Severe FeO based Sliver 3f) Severe Al2O3 based Sliver
Figure 3: Metallographic comparison of FeO and Al2O3 based Defects
(upper image in each figure is of the surface while the lower is a cross-section)

Final Product Assessment

Similar to the use of downstream inspection data or failure rates to evaluate cleanness, the use of direct metallographic
examination of the final product provides the most information with respect to the impact of steel cleanness on product
performance. Direct observations of the final steel product allow for the determination of the size, and potentially the
composition, of the inclusion responsible for the failure. Many papers have combined downstream investigations with
confirmation of defect source to refine their root cause analysis and determine effective actions to reduce defect
occurrence.26,38,44-48 The most common metallographic methods are Optical and SEM based microscopy combined with EDX
determination of inclusion composition. Once the size and composition of the inclusion causing the failure are known this
information can provide clues as to the potential source of the defect in the steelmaking operation. One of the more useful
tools available to assist in determining the potential origin of a defect is the “Unified Decision Tree for Surface Defects on
HR and CR Sheet” prepared by the AISI (now AIST) Technical Committee on Metallurgy – Steelmaking and Casting49
shown in Figure 4. While the Decision Tree is primarily focused on the source of FeO based defects, it also provides general
guidance for determining potential root causes of defects related to other non-metallic inclusions.
One of the key items to note from Figure 4 is the differentiation between exogenous and indigenous inclusions. Exogenous
inclusions are introduced into the steel by the steelmaking process itself and can be avoided through appropriate procedural

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modifications. Examples of easily identifiable exogenous inclusions would be those related to slag entrapment (whether
ladle, tundish or mould) or refractory breakdown. These inclusions typically have a specific composition that can be used to
trace potential root cause (e.g. Na or K for mould powder) or can be classified based on a combination of composition and
morphology. Indigenous inclusions are those that are inherent to the steelmaking process, with the most common being
oxides resulting from the deoxidation process and sulphide based inclusions. As most steels are killed with aluminum, the
most commonly encountered inclusion is alumina, which forms by the reaction of aluminum with dissolved oxygen per
Equation 1.

2[Al] + 3[O] → (Al2O3) (1)

One of the difficulties in evaluating product samples is classifying an inclusion, such as alumina, that can be either
indigenous (deoxidation source) or exogenous (reoxidation source). Numerous references in literature provide the
background on the development of alumina inclusion morphology.11,29,31,50-53 As shown in Figure 4, it was believed that the
source of the alumina inclusion could be determined based on general size classification. Recent work by Tiekink et al53
suggests that there is no difference in size between inclusions produced by deoxidation and reoxidation and any variations in
size are predominantly due to variations in the oxygen gradient at the time of formation. It should be noted, however, that
inclusions will tend to coarsen with time due to agglomeration,54-56 thus shifting the size distribution and causing the average
inclusion size to increase over time. This time impact can also explain some of the observed size differential.
Another issue that arises when evaluating inclusions in finished or semi-finished steel samples is the potential for
composition changes during solidification. It becomes difficult to relate the inclusion composition present in the solid steel
sample back to the composition that was present in the liquid steel. One example is exogenous inclusions initially high in
SiO2 (e.g. mould powder or tundish slag) will end up lower in SiO2 and higher in Al2O3 due to the reduction of the SiO2 by
dissolved Al per Equation 2.

3(SiO2) + 4[Al] → 2(Al2O3) + 3[Si] (2)

This modification of inclusion composition during solidification must also be considered when attempting to evaluate
calcium treated steels and relate inclusions present in the solid state with those originally present in the liquid. A review of
the principles of calcium treatment of steel is provided in detail elsewhere57,58 but in general terms, the goal is to modify solid

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 Figure 4: Consolidated Defect Decision Tree49

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alumina inclusions into liquid or semi-liquid calcium aluminates per Equation 3 while avoiding the formation of CaS per
Equation 4.

[Ca] + (x+⅓)Al2O3 → CaO·xAl2O3 + ⅔[Al] (3)

[Ca] + [S] → CaS (4)

The modification of calcium containing inclusions during solidification has been reviewed in literature.59-62 During casting,
the rate of solidification is slow causing inclusions to be pushed into the remaining liquid. At the same time, solute elements
such as aluminum and sulphur are rejected from the solidifying steel into the remaining liquid. Wang et al59 proposed that
this solute rejection, combined with lower temperatures during solidification, causes the reaction to proceed per Equation 5
where sat corresponds to the saturated Al2O3 composition in equilibrium with the solid CaAl2O4.

2/(1.5-3sat)(Al2O3)sat·(CaO)(1-sat) + ⅔[Al] + [S] ↔ (1+2sat)/(1.5-3sat)(Al2O3)0.5 + (CaO)0.5 + CaS (5)

For this reason, based on Equation 5, inclusions in the solid state will typically exhibit a higher proportion of Al and CaS rich
inclusions when compared to those present in the liquid state.

Semi-Finished Product Analysis

Despite the difficulties associated with evaluating inclusion compositions following solidification, there is still significant
information that can be obtained by examining the semi-finished product. Reviewing the semi-finished product provides key
insights into the degree of macro-segregation resulting from either solute segregation during solidification (Figure 5a) or due
to an external cause such as strand halfway cracking (Figure 5b). The causes of segregation and cracking in the as-cast
product are reviewed elsewhere,63-65 leaving our focus on detection and severity measurement.

Figure 5a) Schematic of Centreline Segregation Figure 5b) Example of Halfway Cracking
Even today, the most common method for evaluation is through acid macroetching or sulphur printing. The resulting etch or
print is compared to a set of standards with numerical ratings, the most commonly used being the Mannesmann rating
system.66 One benefit of this method is it is comparatively simple, however, the results produced are qualitative in nature and
highly subjective.67 Efforts to provide a more reproducible and quantitative evaluation focussed initially on image analysis of
either the macroetch or sulphur print68,69 as shown in Figure 6 or through direct analysis of chemistry segregation by
drilling.70

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 Figure 6: Image analysis of Centreline Segregation
There has been considerable effort over the last five years to develop a true quantitative measure for segregation and cracking
in the as-cast product using various methods, with Piccone et al71 providing an excellent review of the status of the various
techniques available for centreline evaluation. Sengupta et al72-74 have pioneered the use of X-ray Fluorescence as a method
to map segregation while also providing a quantitative measure of chemistry variation. Others have promoted the use of
microprobe analysis75 or ultrasonic methods.76 Recently, Abraham et al77 presented a refinement on the image analysis
technique to provide a more quantitative measure of segregation and halfway cracking. Although these methods are still in
development, a truly quantitative measure for evaluating segregation and halfway cracking is getting closer.
In addition to evaluating segregation and halfway cracking, macroetching and sulphur printing provide the opportunity to
assess steel cleanness with respect to alumina and other inclusions typically present in liquid steel. The Mannesmann rating
system provides standards for both spot and cloud shaped inclusions.66 Similar to the evaluation of finished steel products,
the ability to combine the evaluation of both the location and composition of inclusions within the semi-finished product can
provide insight into the potential source of the inclusions, as well as the inclusion distribution generated by liquid flow within
the caster mould. This type of analysis is very time consuming and involves taking multiple samples both across the width
and through the thickness of the semi-finished steel product.78-80 This idea has been fully utilised by Demmon et al81 who
presented the idea of slab step milling to map inclusion distribution across the width and through a portion of the thickness of
an entire slab. This technique attempts to bridge the gap between detecting and identifying the micro-inclusions (< 20 µm),
typically conducted by optical or SEM based metallography, and the macro-inclusions (> 20 µm), particularly those over 100
µm in size. It is these macro-inclusions that are most critical when related to product performance as reviewed in Table I.
Detecting and classifying macro-inclusions becomes a problem of looking for the proverbial “needle in a haystack”. This is
made evident by Figure 7, which illustrates the number of inclusions present in a specific volume of steel relative to size.
Typical microscopy samples consist of only a small volume of steel making the probability of finding an isolated large
inclusion exceedingly small. If a sufficiently large volume can be analysed, then the probability of detecting an isolated large
inclusion increases considerably.
Returning to Figure 1, the most common method for detecting isolated macro-inclusions is using Ultrasonic detection
techniques. The detection of isolated inclusions that exceed the critical size as outlined in Table 1 is of interest to those
manufacturers producing steel with very stringent quality requirements (e.g. bearing steel) where a single large inclusion can
cause catastrophic failure of the final product. The literature contains several papers that review the application of ultrasonic
testing methods to the detection of isolated large inclusions.7,82-85 Ruby-Meyer et al86 used ultrasonic inspection techniques to
locate the isolated macro-inclusions and then sectioned the test specimen for metallographic analysis to determine the
potential source of each inclusion. Another example of the application of ultrasonic testing was presented by Glaws et al,70,82
who described the use of a conical test section to allow for inspection through the thickness of a round bar. This technique
was used to evaluate the impact of electromagnetic stirring on the macro-inclusion distribution within the bar.

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 Number of Inclusions

Inclusion Size

Figure 7: Schematic of Number of inclusions per unit volume of steel

A variation on ultrasonic testing used for slab production is MIDAS (Mannesmann Inclusion Detection by Analysing
Surfboards) where a sample perpendicular to the casting direction is rolled to elongate the inclusions and enable detection by
ultrasonic methods and subsequent microscopic analysis.78,87-90

Process Analysis of Liquid Steel Samples

The analyses discussed in the previous sections can provide useful information relating to the overall cleanness of the steel
product (whether finished or semi-finished) and information on the suitability of the product for the intended application,
however, it can be difficult to correlate this information back to changes in liquid steel processing parameters. For this
reason, direct analysis of samples taken during liquid steel processing can provide invaluable information to guide
enhancements for improving steel cleanness. The most commonly used method for this type of evaluation has been
microscopic analysis (whether optical or SEM based) of standard lollipop samples. Due to their small size these samples can
be rapidly quenched thus providing an inclusion population more consistent with that in the liquid steel. Initially, this
analysis required the metallographer to manually review, count and classify the various inclusions found based on a set of
standards such as ASTM E45.91 Since a single sample contains hundreds, if not thousands, of inclusions this process
invariably resulted in an incomplete picture of the inclusions present in the steel. Nevertheless, there are many papers
outlining process improvements using just these manual techniques.10,25,50,92-94 The development of automated image analysis
was a step toward the ability to visually classify and determine sizes of inclusions.95 Optical image analysis relies on
inclusion morphology rather than an actual analysis for determination of composition and can therefore be misleading or
inconclusive.96 It was not until the advent of automated SEM based inclusion analysis that a more complete picture of the
inclusion population in liquid steel became available.60,97-99 Story et al100 provided an excellent overview of the system and
this is reproduced graphically in Figure 8. This technique takes advantage of the general inclusion population distribution as
shown in Figure 7. While the SEM will capture and analyse all inclusions in the desired scanning area, the data is analysed
based on a specific size range of inclusions, typically between 1 to 10 µm. Smaller inclusions are excluded due to issues with
processing the sheer quantity of inclusions, while larger inclusions are excluded due to the low probability of finding them
consistently. The assumption is that the population of micro-inclusions within this size range is representative of the
inclusion population within the heat and can therefore be correlated to the macro-inclusions that cause product defects.101
This same micro-inclusion population can then also be related back to steel processing to determine those specific variables
that influence inclusion formation.

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 Figure 8: Process of automated inclusion analysis and identification100
Per ASTM E214298 the inclusions can be classified in a manner similar to ASTM E4591 based on morphology alone.
However, the advantage of the SEM based system is that the addition of EDS analysis allows for classification by chemistry
rather than just morphology. ASTM E2142 also allows for the use of a user defined classification scheme. This provides
considerable flexibility in the analysis, with the typical output consisting of classifying the inclusions by size, frequency, area
fraction and composition. These classifications allow for direct comparisons either within or between heats to evaluate and
compare changes in steelmaking practices. Graphical outputs of items such as frequency or area fraction are used to compare
overall or individual inclusion compositions between heats or different process routes. One of the more common outputs of
these systems is to display the inclusions on a suitable ternary diagram. An example of a typical output for an automated
SEM based system is shown in Figure 9.102 This figure compares the area fraction and displays ternary diagrams for heats
exhibiting relative ratings for sulphide shape control. Plotting the inclusions on a ternary diagram is a useful tool for
comparing the inclusion population through a process to see how the composition changes during treatment or for comparing
the difference in inclusion populations based on specific processing parameters of interest.

Figure 9: Example outputs of Automated SEM inclusion analysis comparing heats rated for sulphide shape control102
This type of analysis allows for a rapid identification of the quantity of liquid and solid inclusions, particularly when
evaluating the inclusion composition for castability. Adding calcium to the steel will result in the modification of alumina
(Al2O3) to calcium aluminates or it will react with sulphur to form calcium sulphide (CaS) as discussed in detail
elsewhere.57,60,103 The initial Al (and by extension Al2O3), S and O level of the steel and the amount of Ca added will
determine what inclusion phase is formed. The desired outcome is to produce a liquid inclusion product and avoid the
formation of solid phases that can negatively impact both castability and product performance. Story et al99 used automated
SEM inclusion analysis to compare inclusion compositions and compared the results to casting performance. It was found
that conversion to 100% liquid inclusions was not required to improve castability and that good castability could still be
obtained when the inclusions were 50% liquid as shown in Figure 10.

AISTech 2018 Proceedings. © 2018 by AIST.

 Figure 10: Inclusion Composition of a heat with Stable Casting Performance from Story et al99
Casting performance was then compared to the inclusion composition and a modified Ca/Al ratio was proposed to account
for the CaS content in the inclusions. This ratio is reproduced as Equation 6 where the Ca, Al and S represent the atomic %
of each element within the inclusion. A value of 0.4 to 0.8 was determined to be optimum to avoid solid inclusion formation
when the ratio is too low and to avoid refractory erosion at higher ratios.

“Ca / Al” = [ Ca – (S – 2) ] / Al (6)

One item that has not been considered in the above discussion is the influence of Mg on the inclusions and its subsequent
impact on castability. Frank104 provided an overview of Mg-containing spinels, their impact on castability and background
on those factors that influenced their formation. More recent work by Pretorius et al6,105 has discussed the modification of
Mg-containing inclusions by Ca treatment.
Since its development, automated inclusion analysis by SEM has become the standard for evaluating steel cleanness and
there are many examples in the literature outlining its application for process improvement efforts.24,48,106-120 Despite the
quality of information that can be obtained using automated SEM based analysis it has one significant drawback, as does any
metallographic based technique, in that the results can only be obtained offline due to the requirements of sample preparation.
It would obviously be very desirable, particularly from a process control or evaluation standpoint, if information on the
inclusion population could be obtained in real time.
The development of OES based Pulse Discrimination Analysis (PDA)121 has provided a method to quickly detect inclusions
in a steel sample. PDA uses the relative intensities of the individual sparks, which are significantly higher when the spark is
on an inclusion than the intensity obtained for the dissolved element in steel as shown in Figure 11. Weerts et al122 provide a
more in-depth description on the background of PDA and some comparisons of PDA to SEM based analysis. Interpretation
of these sparks allows for an estimation of the relative quantity of the inclusions but does not provide information on the
shape or size. There are a number of examples from literature regarding the application of PDA to monitor various aspects of
steel production.16,123-126 Recently Pretorius et al6,127 reviewed the use of PDA to evaluate Ca-treatment effectiveness with the
goal of developing a technique for real-time analysis.

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 Al O
2 3
Inclusions
Intensity
Dissolved Al

Figure 11: Individual Spark Intensity during OES analysis

As previously mentioned, the high cooling rates achieved with the typical “lollipop” type sample provide an inclusion
population closer to that of the liquid steel. However, results obtained with any of the above techniques can be influenced by
artifacts of the sampling process that ultimately lead to erroneous results. The most obvious impact would be the entrainment
of slag during the sampling process. Hansén et al128 presented an overview of some of the aspects of a reliable sampling
routine to provide high quality samples suitable for inclusion analysis. Other authors have also reviewed the aspects of
sampling techniques and provided recommendations on obtaining high quality samples.129-131 Finally, Pitts et al,132 while not
specifically evaluating the impact of sample quality, outlined an innovative method for obtaining simultaneous steel samples
at varying depths in the ladle and found that the inclusion population varied at each location, further reinforcing the need for
consistency in sampling techniques.

STATISTICAL EVALUATION
Each of the direct assessment methods reviewed above can only determine the inclusion population in the sample that is
analysed. Some relevant questions then arise. Do the inclusions present in the sample adequately represent the inclusions
present in the heat? How do we determine the maximum inclusion size that will likely be encountered? How does the two-
dimensional observation of an inclusion in a metallographic sample relate to the actual three-dimensional shape and size?
The answer to these questions can be provided through the various statistical techniques that have been developed to
represent the inclusion size distribution within a heat based on the results obtained from an individual sample. It can be seen
from Figure 7 that the typical inclusion size distribution follows a log-normal pattern. The logarithm of the log-normal
distribution is normally distributed thus allowing for statistical analysis. Murakami133 first described the use of the Statistics
of Extreme Values (SEV) for calculating the maximum probable inclusion area based on a series of observations. Atkinson
et al134-136 reviewed the use of SEV as it relates to steel cleanness assessment and developed a method based on the
Generalized Pareto Distribution. A comparison of the general principles behind each of these techniques is reproduced in
Figure 12.136 The use of extreme value analysis of non-metallic inclusions in steel is also outlined in ASTM E2283.137
The methods described above are based on metallographic analysis of polished metal samples and therefore are based around
the 2-dimensional observations of the inclusions. The apparent size of a 3-dimensional inclusion will vary based on
polishing depth, and in the case of a dendritic or clustered inclusion, what is one large inclusion may appear as a series of
smaller inclusions. This is illustrated in detail in Figure 13 which compares how a three-dimensional inclusion population
would appear when sectioned and mounted on different two-dimensional planes. Zhou et al138 recognized this issue and
reviewed the impact of various inclusion types on the results obtained through a 2-D examination of samples by SEV and the
potential error generated. Several other authors139-146 also investigated this problem, including the direct comparison of 2-D
metallographic results to actual 3-D results obtained by techniques such as electrolytic extraction. Another example of the
application of the theories above was the work by Abraham et al147 in developing an inclusion rating system referred to as the
“Total Interparticle Spacing” (TIS). Other statistical techniques have been used including cluster analysis148 which simplifies
the analysis by grouping or clustering the inclusion data into sets with similar properties. The results of any of the above
analyses can be used to aid in predicting the impact of the inclusions on mechanical properties (e.g. fatigue life149) or other
product performance characteristic (e.g. surface quality).

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 Figure 12a) General Description of SEV method 12b) General Description of GPD method136

Figure 13: Impact of Sectioning on two-dimensional inclusion appearance101

CONCLUSION
This review outlined a few of the most commonly available methods used for steel cleanness assessment within the industry
and provides a reference to the information available for a more in-depth study on a specific technique or topic. The reader is
referred to the references that follow for further in-depth study but the following papers are suggested to start their study.
Zhang and Thomas, “State of the Art in Evaluation and Control of Steel Cleanliness – A Review”5
Pretorius et al, “An Overview of Steel Cleanliness from an Industry Perspective”6
Abraham et al, “Inclusion Engineering and the Metallurgy of Calcium Treatment”58
Piccone et al, “Quantitative Methods of Evaluating Centreline Segregation”71
Story et al, “Study of Casting Issues using Rapid Inclusion Identification and Analysis”.106
Kaushik et al, “Inclusion Characterization: A tool for Measurement of Steel Cleanliness and Process Control”108
Atkinson et al, “Characterization of Inclusions in Clean Steels: A Review Including the Statistics of Extreme Methods”136
Any assessment of steel cleanness must consider the final application and the ability of the product to meet the customer’s
requirements. Once these requirements are understood then the appropriate technique, or combination of techniques, can be
selected.

AISTech 2018 Proceedings. © 2018 by AIST.

 ACKNOWLEDGEMENTS
I would like to thank Stelco management for the permission to publish this paper as well as the members of the AIST
Subcommittee on Inclusion Engineering and Clean Steel (Sunday Abraham, Bill Jones, Sridhar Seetharamen and Pat
Philbin). I would also like to provide a special thanks to Scott Story for his advice and guidance.

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84. H. Nagayama, T. Nishikawa, I. Fujii and S. Kinoshita, “New Method of Evaluating Non-Metallic Inclusions and
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105. E.B. Pretorius, H.G. Oltmann and T. Cash, “The Effective modification of Spinel Inclusions by Ca-Treatment in LCAK
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126. I.R.C. Whiteside, R.T. Bryce, A. Clarke, J. Van Boggelen, L. Way, M. Hargest and I. Blake, “Exploitation of Spark-
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145. S.N. Lekakh, V. Thapliyal and K. Peaslee, “Use of an Inverse Algorithm for 2D to 3D Particle Size Conversion and Its
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