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Effects of Inclusions
Effects of Inclusions
2 0 1 9;8(2):2408–2422
www.jmrt.com.br
Review Article
a r t i c l e i n f o a b s t r a c t
Article history: Non-metallic inclusions (NMIs) occur typically in low or very low volume fractions (from
Received 5 May 2018 10−2 in a high oxygen weld deposit to 10−5 in very clean bearing steels) but play an impor-
Accepted 15 January 2019 tant role in many properties of steel. NMIs play a decisive role in processes involving ductile
Available online 22 February 2019 fracture, fatigue and corrosion, for instance. These are some of the properties more rele-
vant to the performance of steel in structural and mechanical applications. Furthermore,
Keywords: NMIs may influence nucleation during phase transformations of steel. In this work, the rela-
Non-metallic inclusions tion of these properties to NMIs is reviewed, highlighting progress and difficulties in each
Fracture area. Perhaps because of their very low volume fraction, NMIs are sometimes overlooked
Fatigue in the basic physical metallurgy education and their study is left to the realm of those
Ductility interested in steelmaking. In the last decades a dramatic evolution in the understanding
Steel of their relationship to properties, however, has led to significant improvements in many
Steelmaking steel products: the outstanding increase of fatigue life in automotive springs and in bear-
ings is one of many such examples. It is concluded that steel improvement in many cases
requires “inclusion engineering” and this can only be achieved through close collaboration
between physical metallurgy, process metallurgy and steelmaking. Those who realized this
have made significant progress in steel development in recent decades as highlighted in
this short review.
© 2019 The Authors. Published by Elsevier B.V. This is an open access article under the
CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
E-mail: andre.costaesilva@gmail.com
https://doi.org/10.1016/j.jmrt.2019.01.009
2238-7854/© 2019 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
j m a t e r r e s t e c h n o l . 2 0 1 9;8(2):2408–2422 2409
0.6
Before hot After
FeO working hot working
ν 0.4
Void
0.2 Mn in (Fe.Mn)O “hard’’
inclusion
ν 0.1 Ca-aluminates
0
1.0 MnS
Fig. 2 – Schematic illustration of the behavior of NMIs after
Me, X = Te X=Se thermomechanical treatment, depending on their relative
(Mn, Me)(S, X)
0.5 plasticity at the working temperatures.
800 1000 1200 1400 1600
Temperature (ºC)
48,5
μm
134 μm
a 1000
400
900
Upper shelf energy in charpy-V test (J)
200
800
60 600
0.2%C
SAE 4063
40
500 SAE 5150
SAE 4052
20 SAE 4140
400
SAE 4340
SAE 2340
10 300
0 0.2 0.4 0.6 0.8 1.0 20 30 40 50 60
Inclusion projected length per unit area (mm/mm2)
Hardness (HRC)
b
Short transverse or normal Fig. 11 – Relationship between hardness (HRC) and fatigue
limit (MPa).
1 Longitudinal
Adapted from Ref. [85].
2 Transverse
d1 d1
Normal 4.3. Influence on fatigue
plane
d2
The importance of inclusions on the fatigue of steel has been
d3 long recognized [75–77]. The effect of type, composition, shape
and size of NMIs on fatigue have been extensively discussed
in many publications without a firm conclusion, however. Cor-
relations between total oxygen content and rolling contact
Longitudinal
d3 plane fatigue in rails [78] and with L10 in bearings (the number of
d2 cycles at which 90% of fatigue samples fail) have been demon-
strated [79] but with limited quantitative success. A recent
Transverse
plane review dedicated to bearing steels addresses in detail many of
these issues [80]. The work of Murakami and co-workers has
Fig. 10 – (a) Effect of inclusion projected length on upper shed new light on understanding the effects of NMIs on fatigue
shelf energy in Charpy tests for steels with 0.1% and 0.2%C. both before [81,82], and after [83] the publication of his book
The symbols indicate individual steels used for the tests. [84]. His views can be summarized in the following statements:
(b) Orientations and dimensions used to determine The fatigue limit is correlated with the existence of non-
projected lengths. propagating cracks. It is not related to crack initiation. . .“the
Adapted from Ref. [65]. fatigue limit is a threshold stress for crack propagation and not
the critical stress for crack initiation”. Fatigue limit correlates
with hardness, up to around 400HV (e.g. Fig. 11, [85]). In this
region, “the fatigue limit is determined by a material property
important areas present challenges to further advances: (a) showing the average resistance to plastic deformation of the
the proper characterization of the properties of NMIs and their material”.
interfaces with steel; (b) an adequate metric for character- As one passes the 400 HV threshold, the ideal fatigue limit,
izing size, shape and distribution of the large multi-particle associated with the material properties cannot be reached, in
population and (c) the difficulties associated with compu- general, due to the presence of defects (such as inclusions).
tational methods considering the multi-particle population. “Defects smaller than a critical size are non-damaging (not-
When modeling fracture, detailed elastic-plastic calculations detrimental) to fatigue strength and the critical size is smaller
of void nucleation can be performed if constitutive equations for materials having a higher static strength, so that a defect
are defined for the matrix, inclusions and interface (e.g. [74]). of a given size is more detrimental to high strength steels than
Conversely, very interesting examples of how to deal with (a) to low strength metals.” Murakami demonstrated with several
and (b) can be found, for instance, in Refs. [36,50]. A relevant experimental examples that since the fatigue limit is a stress
example of advances in computational methods is presented at which crack propagation does not occur, small defects can
in Ref. [23]. and will have cracks starting from them that may or may not
j m a t e r r e s t e c h n o l . 2 0 1 9;8(2):2408–2422 2415
3 a
(HV + 120) 4
10% error
1 3 CaO-AI2O3
σ
Globular
Harmful index
10% error
TiN
2
σ = 1.43 (HV + 120) /( area ) 1/6 AI2O3
0.3
10 100 1000 (Ca,Mn)S
1
area μm
σ / σw
regarded as mechanically equivalent to a stress-free defect or
pore. Thus, tessellated stresses, for instance [32] could be less Oxides, ≤10 μm
0.5 Oxides, 10 μm < <20 μm
important than previously thought. Using this approach, he Oxides, ≤20 μm
was able to find adequate relationships to predict the fatigue Tin, ≤6 μm
: Average diameter
limit of high strength steels, reconciling the endurance limit
0
relationship with hardness by including a term related to
105 106 107 108
the cross-section area transverse to the loading, occupied by
Cycles to failure, Nf
inclusion. Depending on the loading, position of the inclu-
sions can be important, and this is accounted for. Thus, for
Fig. 13 – (a) Harmfulness index of different inclusions as a
inclusions close to the surface in rotation-bending Murakami
function of composition and size, assessed by Monnot and
and co-workers proposed an empirical relation between the
co-workers [77]. (b) Monnot’s data reanalyzed by Murakami
endurance limit and hardness given by Eq. (1), where the area
[84] shows that inclusion “harmfulness” is very similar for
of the inclusion is considered. Murakami has developed simi-
the various types of inclusions and the fatigue behavior
lar equations for inclusions in other positions.
follows Eq. (1) (ordinate normalized by estimated fatigue
limit).
√ 1
⁄6
w ∼
= 1.43 (Hv + 120) /( areas ) (1)
sufficiently large and play an important role. This relation- without hot/controlled working. Thus, weld metal composi-
ship between size and strength is consistent with Murakami’s tion is tailored to cause the precipitation of adequate nuclei
EB “clean steel” results reported above. The results of Pessard for acicular ferrite. Some of the factors considered relevant
and co-workers [96], who studied fatigue anisotropy in three for a NMI to act as a nucleus [105,106] for acicular ferrite
different steels, are also a good example: they did not observe are: crystal structure, differences in CTE and depletion in
any anisotropy in the fatigue behavior of a low strength C35 austenite-stabilizing elements such as Mn around the inclu-
steel ( U = 580 MPa, AISI 1035, where U is the tensile strength) sions [107,108]. The latter is the most favored explanation,
with reasonably normal sulfur content (0.045%). On the other followed by stresses generated by CTE differences between
hand, higher strength steels ( U = 1050–1150 MPa) with high inclusion and the austenite matrix [106]. This gains special
sulfur content (0.073–0.075%), presented fatigue anisotropy, relevance with the prospect of thin plate casting, where the
associated with NMI-related fatigue fracture. extent of hot/controlled working that can be performed to
The anisotropy of fatigue resistance is included in refine the austenite grain is very limited [109]. The impor-
√
Murakami’s formulation, since the term areas is calculated tance of this phenomenon in welding is well discussed in Refs.
using the projected area of the inclusion (or defect) onto a [106,110,111]. The control of NMIs for nucleation in thin foil
plane perpendicular to the maximum tensile stress [84]. This continuous casting is discussed by [109,112–114]. One of the
is confirmed by experimental results (e.g. [97,98]). first and clearer in situ observations of the nucleation pro-
Some recent results in rolling contact fatigue (RCF) seem to cess was done by Sugiyama and Shigesato [115] who discussed
contradict – at least partially – Murakami’s concepts regarding in detail their observations on the importance of manganese
the effects of NMIs on fatigue. Both Sada and co-workers [99] sulfide on ferrite nucleation. Li and co-workers have shown
and Hashimoto and co-workers [100] observed that hot iso- experimentally and using first principle calculations that Zr
static pressing (HIP) of SAE 52100 bearing steel improved RCF and Ti oxides promote Mn depleted zones in the NMI–matrix
life. They attributed the effect to the elimination of the cavi- interface, favoring ferrite nucleation [116,117]. Furthermore,
ties between NMIs and the steel matrix. As the inclusion size is they have shown that MnS can nucleate on Zr oxide. As a
not altered by HIP, these authors considered that the NMI–steel result, they have shown the beneficial effect of Zr-Ti deox-
interface condition also plays a role in fatigue life. On the other idation in HSLA steels, promoting finer and more uniform
hand, the NMI–matrix interface strength has been considered dispersions of MnS and acicular ferrite microstructures [118].
an important factor in the microscopy phenomena involved Grong and co-workers [119] reviewed the possibilities of pro-
in fatigue cracking. Spriestersbach and co-workers [101], for ducing “dispersoids”, inclusions with a sufficiently fine size
instance, noted that “classical” NMIs (oxides, complex oxides and compositions to affect nucleation in solidification as well
and sulfides) debond easily due to the low NMI–steel inter- as ferrite nucleation. In order to achieve this, these particles,
facial strength. Furthermore, differences in CTEs [32] may however, would be formed in a more complex way than just
promote NMIs-matrix separation. Thus, classical NMIs may be resulting from classical NMI formation reactions, which are
considered to behave as holes, as proposed by Murakami. Con- the focus here.
versely, TiN, for instance, has a strong bond to the matrix and
the TiN–steel interface shows no separation. When TiN is sub- 4.5. Influence on machinability
jected to high stresses it cracks, and the cracks propagate into
the matrix. Thus, the correlation between TiN size and fatigue Perhaps one of the properties most traditionally related to
behavior could be different from the one observed for “classi- NMIs is machinability [120]. The effects of sulfides [121] are
cal” NMIs [101]. Evidently, this is an important argument and well known and the design of these inclusions for machin-
further research is needed to clarify these phenomena. This ability has been quite successful [122]. A detailed review on
is a very important issue for RCF. However, the microstruc- the role of NMIs on machinability, covering many types of
tural changes observed during RCF [102] make investigating inclusions has been published recently [33]. Computational
the effects of the individual NMI very difficult, as experimental thermodynamics has been used to design steels with good
results (e.g. [103]) demonstrate. machinability by tailoring sulfides to substitute Pb “metallic
Furthermore, Murakami’s assumption [81] that the dimen- inclusions” [123]. Lead added steel presents important health
sion of NMIs parallel to the stress is not important has been hazards during steelmaking and significant environmental
questioned. Observations in steels with elongated NMIs larger impact. Presently the automotive industry is defining a min-
than those found in very clean steel (such as bearing steels) imum sulfur content for non-resulfurized steels to improve
suggest that these NMIs may have a larger than expected their machinability. This has posed an interesting challenge
influence, due to the long region of the material that will be to bar manufacturers who need to adjust their processes to
subjected to stress concentration [104]. prevent nozzle clogging by the use of calcium in presence of
sulfur in the range of 0.020% [124]. Stringent process control
4.4. Influence on the nucleation of ferrite is required, in this case.
NMIs may play an important role in phase transformations. 4.6. Influence on surface finish
Their influence on nucleation in continuous casting and ingot
casting was discussed in a previous publication [1]. NMIs also Albeit surface finish can be considered a machinability issue,
play a critical role in the nucleation of fine acicular ferrite in the case of tool steels for plastic molds, for instance, presents
weld metal. This microstructure is important to achieve satis- extraordinary requirements. Studies have shown that both
factory mechanical properties with low carbon compositions microstructure and cleanness play an important role. Simple
j m a t e r r e s t e c h n o l . 2 0 1 9;8(2):2408–2422 2417
forms of cleanness quantification, however, are not able, in steels. Banding was also shown to be critical to the hydro-
general, to correlate with polishing quality [125]. Inclusion gen induced failure of AISI 4140 bolts in sub-sea applications
type play a definite role in the process: in the case of ESR of subjected to cathodic protection [139]. Du and co-workers
P20 steel, for instance, it was demonstrated that the typical [140] have shown the beneficial effects of generating a fine
desulfurization of ESR is deleterious for surface finish and dispersion of oxide and sulfide NMIs through Zr + Ti deox-
inert atmosphere remelting must be used to prevent desul- idation on HIC resistance, when compared to conventional
furization and guarantee that sulfides will cover the oxide Al deoxidation. In a recent review, Ohaeri and co-workers
inclusions allowing a good surface finish [126]. The compared [141] confirmed that NMIs in general can be deleterious to
results of VAR and the so-called PESR (ESR under inert gas) in resistance to hydrogen degradation but confirmed that elon-
[125] can be explained in the light of this observation. gated inclusions apparently have a more negative effect. The
importance of elongated sulfides on the extent of hydro-
4.7. Influence on corrosion gen blistering has also been demonstrated [135]. Thus, NMIs
shape, amount and type play an important role in hydrogen
Two examples of the influence of NMIs on the corrosion perfor- cracking. The eventual clustering of NMIs, particularly regions
mance of steels are the importance of inclusions on hydrogen of microstructural banding, has a synergistic effect in pro-
related failures such as hydrogen-induced cracking (HIC) and moting problems associated with hydrogen and should be
on the formation of pits, as discussed in the next sections. carefully avoided.
Additionally, it should be noted that Murakami has demon-
4.7.1. NMIs and hydrogen related failures strated that hydrogen trapping at NMIs has a significant effect
The importance of inclusions as traps and nuclei for HIC has on super long life fatigue phenomena [142].
been recognized at least since the 1970s [127]. The importance It is evident from the above discussion that inclusion engi-
of the synergistic effect of segregation and NMIs, particularly neering will play an increasingly important role in the design
manganese sulfide was soon also recognized. Nakai and co- of hydrogen resistant steels.
workers [128] observed that shape control of sulfides had a
great influence on HIC. They showed that higher oxygen steel 4.7.2. Pitting
with type I sulfides (that do not have high plasticity) had better Wranglén [143] reported the importance of MnS as pitting
resistance to HIC than Al-killed steel with type II sulfides that initiation sites both in carbon and stainless steels. He pro-
elongated during rolling. However, they preferred either Ca or posed that in carbon steels, the attack starts in the matrix
Ce sulfide modification in order to guarantee good properties. close to the sulfide inclusion, which is nobler than the
It was also clear that simply reducing sulfur and controlling matrix while in stainless steels, the attack would start at
sulfide shape was not sufficient to guarantee excellent HIC the sulfide inclusion proper. With the development of char-
resistance [128] since crack propagation was controlled by seg- acterization techniques, Ryan and co-workers [144] measured
regation. Thus, lower C and lower Mn steels were developed, the presence of a chromium depleted region surrounding sul-
as well as accelerated cooling strategies [129] to promote less fide inclusions in stainless steels and proposed that these
segregation, particularly banding, and more uniform hard- would be the initiation sites. They did not, however, pro-
ness in the microstructure. The interaction of segregation pose a mechanism for the formation of these regions nor
and calcium modification was demonstrated by Matsumiya describe the thermal history of their sample. Their results
and others [130,131] who showed that in large segregates were contested by measurements performed by Meng and
usual calcium treatment could be ineffective to prevent the co-workers in various steels (including Ryan’s original sam-
formation of MnS. Thus, very low sulfur and avoidance of ple) [145] and by [146]. The observations of Ryan resemble
MnS has become the rule to guarantee good HIC resistance the composition profiles around chromium carbides in sen-
[132,133]. Nonetheless, inclusions continue to play an impor- sitized stainless steel. While a clear explanation exists for
tant role on HIC crack nucleation. In very clean steels, it has the formation of chromium depleted regions in the matrix
been shown that not only MnS promotes hydrogen cracking. around carbides in sensitization that is not the case for
When studying the resistance of API X120 HSLA steel, Huang the matrix surrounding sulfide inclusions. More recently,
and co-workers [134] related steel cleanness to reduced effect Williams and co-workers [147] observed a layer of Fe rich
of hydrogen, regardless of the inclusion type. They did not sulfide surrounding the sulfide inclusions in stainless steels.
give information on sulfur content of their steel, however. Jin This layer would preferentially dissolve and start the pit-
and co-workers [133] reported that in a Ca treated API X100 ting process. In their conclusions, they suggest that inclusion
steel with 50 ppm S, oxides were detrimental to hydrogen engineering could be used to control the composition of
resistance. Domizzi and co-workers [135] could not correlate the Mn-Fe-Cr-S sulfides and prevent this from happening.
sulfide length or sulfur content to HIC resistance in steels Park and Kang [148] recently reviewed the issue of NMIs
with sulfur in the 50–150 ppm range. They propose that sul- in stainless steels. They discussed the process of solid-
fur content and size influence resistance to hydrogen: “. . . a ification of the sulfides that could lead to the situation
small number of very elongated inclusions may reduce the HIC observed by Williams. It seems clear that subtle chemical
resistance in the same way as a greater number of shorter par- composition differences around NMIs can be of paramount
ticles.” They also emphasize the relevance of banding, which importance for the pitting of stainless steel. Results presently
in HSLA steels is normally associated with higher Mn con- available indicate that the composition variations caused
tents. The effects of banding were confirmed by [136] in SA during sulfide formation could play a very important role.
516 steels and by Dunne and co-workers [137,138] in API X70 Liu and co-workers recently [149] demonstrated the effect
2418 j m a t e r r e s t e c h n o l . 2 0 1 9;8(2):2408–2422
of alumina clusters on pitting of carbon steels. Ma and be the most adequate way to properly characterize NMIs in
co-workers [150] have shown the anisotropic behavior of pit- clean steel.
ting associated to manganese sulfide NMIs. Thus, it is clear
that NMIs, in particular sulfides, have a crucial role in pitting.
Park and Kang [148] remark that the presence of oxide inclu-
6. Conclusions
sions can also play an important role in pitting of stainless
Non-metallic inclusions influence many properties of steels
steels.
relevant to their performance in mechanical and struc-
tural applications. The understanding of how this happens
has evolved in the last decades. Significant progress in the
5. The importance of characterization and quantification of this understanding has been made. Some
quantification of NMIs important limitations persist, however: while the modeling
of ductile fracture has significantly evolved, there has been
little progress in measuring both NMI and NMI-steel interfa-
Based on the above discussion, it is evident that proper
cial properties, a knowledge that is essential to the progress
characterization and quantification of the amount, shape,
of modeling efforts. Furthermore, considering multi-particle
distribution and properties of NMIs is critical for steel charac-
populations and non-uniform distributions in models remains
terization and for the further development of improved steels.
a significant challenge. This is also a challenge for charac-
The importance of the new methods of inclusion characteriza-
terization and quantification of NMIs: while some clustering
tion in the 1990s that made possible proper fatigue predictions
of NMIs will be detected by enhanced non-destructive test-
was also briefly reviewed and discussed in a previous publica-
ing, current methods of quantification focus on the size
tion [1]. This gives an example of how important and dynamic
of particles of the average background NMI population and
the field is. An important challenge in characterization and
do not, in general, measure particle spacing or account for
quantification of NMIs in current clean steel [4] is being able
non-uniform distribution of particles. Combination of charac-
to detect and quantify the “cloud” (or background) of small
terization methods should be used if proper understanding
inclusions and the few large ones. If they occur in large enough
of NMI population is desired. Great progress has been made
sizes, they may be detected by non-destructive testing (NDT),
in the understanding of the importance of NMIs in high
as discussed in item 4.1 above. Characterization techniques
cycle fatigue. This has been accompanied by progress in
that sample large volumes of steel using NDT, such as MIDAS
specific NMI quantification methods and inclusion engineer-
[151,152] are limited by the detection limit of the technique
ing, resulting in significant improvements in materials for
used. Furthermore, in some applications, inclusions consid-
these applications. The use of NMIs for improved machin-
ered “large” are below the limits of reasonable NDT. Scanning
ability has greatly advanced with the understanding of NMI
a sample or the whole volume of steel using NDT becomes
genesis. Inclusion engineering has led to new compositions
useless in this case. Furthermore, clustering and concen-
with improved machinability and surface finish. Significant
tration of secondary NMIs associated with microsegregation
developments also happened in understanding the effect of
[1,29,131] may lead to NMIs behaving, effectively, as if they
NMIs on ferrite nucleation. These developments have reached
were larger [96,98]. Thus, intermediate size clusters or regions
industrial maturity. The understanding of the importance of
where NMIs are concentrated and will influence steel behavior
NMIs in pitting corrosion and hydrogen related fracture has
may not be detected with the current characterization tech-
made enormous progress. However, the interaction of NMIs
niques and may be too small for the current non-destructive
and segregation, inherent to casting processes, still poses a
examination technique. When these clusters are associated
significant challenge to the complete understanding of NMI
with production events (mainly in the casting process (e.g.
influence on the complex hydrogen related fracture phe-
[153]), stringent process control may limit their occurrence
nomenon.
or identify when they occur. However, some route to charac-
Progress in the understanding and control of the effects of
terize the non-uniform distribution of secondary inclusions,
NMIs on the properties of steels in mechanical and structural
caused by microsegregation, may require additional develop-
applications require the close collaboration between physical
ment efforts. With the presently available techniques, more
metallurgy, process metallurgy and steelmaking. Those who
efforts could be placed on evaluating neighbor spacing dis-
realized this have made dramatic progress in steel develop-
tribution by different techniques [4,154,155] which can rely
ment in recent decades and will probably continue to do so.
on usual quantitative metallography tools and are frequently
applied to composites. Present efforts at development new
techniques of three dimensional (3D) characterization such as
Conflicts of interest
X-ray Micro-CT [156] or other 3D reconstruction techniques
[157,158] may also become viable solutions in the future.
The author declares no conflicts of interest.
Presently, techniques such as automated SEM-EDS analysis
(frequently mentioned using the commercial name ASPEX® )
offer the possibility of sampling large areas. Combined with Acknowledgements
3D reconstruction (e.g. [153]) this may also give valuable infor-
mation on particle distribution and clustering. While different The author thanks all his former and present students for
methods will give different information about NMI population inspiration and important contributions to the work on non-
[3], most probably a combination of methods will continue to metallic inclusions in steels. The collaboration of colleagues
j m a t e r r e s t e c h n o l . 2 0 1 9;8(2):2408–2422 2419
in many steelmakers and research organizations is gratefully [22] Zhang L, Guo C, Yang W, Ren Y, Ling H. Deformability of
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