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MACROSCOPIC METHOD FOR ASSESSING THE CONTENT OF NON-METALLIC

INCLUSIONS - BLUE FRACTURE

Conference Paper · April 2018

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 12 th Scientific/Research Symposium with International Participation
„Metallic and Nonmetallic Materials“ B&H, 19-20. April 2018

MACROSCOPIC METHOD FOR ASSESSING THE CONTENT OF

NON-METALLIC INCLUSIONS - BLUE FRACTURE

Belma Fakić, scientific associate

Adisa Burić, B.Sc.
Edib Horoz B.Sc.
University of Zenica, Institute „Kemal Kapetanović“ of Zenica

Key words: bearing steel, macroscopic method, blue fracture, non metallic inclusion

SUMMARY
Non-metallic inclusions usually deteriorate mechanical properties and surface quality of steel
products. Presence of non metallic inclusions might have negative affected some of the mechanical
properties of steels like ductility, toughness, anisotropy, and formability. Macroscopic method for
assessing the content of non-metallic inclusions in forged or rolled steel products is used for
determination non-metallic inclusions visible to the naked eye or with aid of a magnifying with
magnification of not more than 10 times. Only inclusions equal to or greater than 1 mm long are
taken into consideration. In this paper is given procedure for blue fracture test method applied on bar
diameter φ 60mm bearing steel 100Cr6.

1. INTRODUCTION
Low alloy steel, 100Cr6 thanks to its high hardness, wear resistance, surface finishing and
dimensional precision, it is widely used to manufacture mechanical components, such as
precision bearings, automotive components (brakes, steering, line shaft), bicycle, agitators,
appliances, sliders, quick couplings, machine tool, lock mechanisms, conveyor belts, skates,
pens, pumps, castors, measurement instruments, valves. The presence of non-metal inclusions
in the steel 100Cr6 should be minimized due to the exploitation conditions of the specified
components.

2. ORIGIN AND PROPERTIES OF NON-METALLIC INCLUSIONS

During produce any type of steel, it is impossible to avoid the appearance of non-metallic
inclusions. Non-metallic inclusions can not be separated during the crystallization process
and in solid alloy act as a harmful side of the body.
Non-metallic inclusions in steels can be divided into two groups, those of indigenous and
those of exogenous origin. The former group contains inclusions occurring as a result of the
reactions taking place in the molten or solidifying steel, whereas the latter contains the
inclusions resulting from mechanical incorporation of slags, refractories or other materials
with which the molten steel comes into contact. Exogenous inclusions are usually larger than
the indigenous inclusions and, thus, non-metallic inclusions can also be divided into
microinclusions and macroinclusions. Macroinclusions are more detrimental when their
effects on the properties of steel, and especially fatigue properties, are considered [1].
Non metallic inclusions are chemical compounds of metals (e.g. iron, manganese, aluminium,
silicon and calcium) with non metals (e.g. oxygen, sulphur, carbon, hydrogen and nitrogen).
Non metallic inclusions form separate phases. The non metallic phases containing more than
one compound (e.g. different oxides, oxide + sulphide) are called complex non metallic
inclusions (spinels, silicates, oxy-sulphides, and carbonitrides).
Despite the presence of non metallic inclusions in steels in small percentage (0.01 % to 0.02
%), they have a significant effect on the properties of steels [2]. They are the cause for
dangerous and serious material defects such as brittleness and a wide variety of crack
formations. However, some of these inclusions can also have a beneficial effect on steels
properties by nucleating acicular ferrite during the austenite to ferrite phase transformation
especially in low carbon steels. The properties of steels generally affected by the
non metallic inclusions include tensile strength, deformability or ductility, toughness, fatigue
strength, corrosion resistance, weldability, polishability, and machinability [3].
Some inclusions found in bearing steels have incoherent interfaces with the steel and the
stress described is that tangential to the inclusion–matrix interface. All of the inclusions listed
melt at a temperature greater than that of the steel, and are less dense compared with the steel.
Some of inclusions which are listed in Table 1, are problematic in bearing steels for a variety
of reasons. They have different thermal expansion coefficients from the matrix, in most cases
less than that of austenite. As a consequence of cooling to ambient temperatures, tensile and
compressive residual stresses develop parallel and normal to the inclusion–matrix interface.
The inclusions may be brittle, and the resulting cracks concentrate stress and hence may
propagate into the steel. Even the simple presence of an uncracked inclusion introduces a
mechanical heterogeneity which locally changes the distribution of stress. Almost all of the
common non-metallic inclusions have weak interfaces with the steel. Strain incompatibilities
during deformation processing of the steel can then lead to the formation of cavities at the
localized at the inclusion interface along the direction of the principle plastic strain [4].

Table 1. Properties of non metallic inclusions [4]

Inclusion Shape Hardness (HV30) eΤ (10-6 K-1)

MnS, CaS Streaky 150-170 18,1

Al2O3 Aggregates ≈ 2200 8,0
Ca aluminates Globular 900-2500 6,5 – 10,0
MnO-SiO2 Oblong >1100 5,0
TiC Sharp cuboids ≈ 3000 9,4
TiN Sharp cuboids ≈ 2500 9,4

Debonding can occur during the course of fatigue. Alumina inclusions have been shown to
detach from the matrix during loading, thus concentrating stress in the surrounding matrix; in
contrast, titanium carbonnitride particles are apparently strongly connected to the matrix and
hence fracture by cleavage, leading to a different mechanism of crack initiation [4], Fig. 1.
 Figure 1. (a) Detachment of matrix from spherical alumina inclusion in a push–pull fatigue test with
The cusps on the cavity are assumed to be associated with the plane of hot-rolling. (b) Similar effect
but the cavity illustrated is empty (c) Cleaved Ti(C,N) particle which maintains a bond with the
matrix. Micrographs courtesy of H. Bomas [4].

2.1 Influence of non-metallic inclusions

The presence of non-metallic inclusions in a sense represents the crack or cavity in the steel
as a metal connection interruption basis weight and acts as the internal notch. Considering the
strength of the inclusions is small and that the bond between the inclusions and the metal
barely exists [3], this means that non-metallic inclusions can only transmit insignificant
strains.
Non-metallic inclusions are no coherent with metallic matrix, they prevent dislocation
migration and serve as stress concentrators. Due to this reason, 70...100 % primary
microcracks were initiated on non-metallic inclusions, inspite of only 0.1- 0.2 volume percent
of inclusions existing in steel. It was established that microcracks contours were often faithful
copies of inclusion contours, contributing greatly to crack formation in steel in process of
cyclic loading [5].
Since the latter are products of reactions within the steel, they are normal constituents of it.
Because ordinary manufacturing processes cannot entirely rid the steel of such inclusions, it
is desirable to control their kind and amount within such limits that the steel is relatively free
from those inclusions which are considered most injurious [6].

2.2 Techniques of Evaluating Macro Inclusions

Unlike micro inclusions that are dominant in steel, macro inclusions are very rare and their
detection requires more time and attention if using the conventional metallographic methods.
Very skilled SEM and LOM users waste more time on samples and in most cases these
inclusions are not even detected. With advancement in the ladle metallurgical processes, very
low oxygen contents can be achieved in steel and this has resulted to high cleanliness in steel
products. The index for macro inclusions has therefore been reduced to zero in recent years
by using both step down tests and blue fracture testing.It has becoming more and more
difficult to detect macro inclusions even though they exist in steel products. Reclamations
are received by clean steel companies each year and macro inclusions have been the
contributing factor for some failures [6].

There are few methods for determination macro non-metallic inclusions [7, 8]:
- Ultrasonic immersion test,
- Magnetic particles
- Blue fracture test,
- Step-mashined test,
- Hardness fracture test.
2.3 Makro inclusions
Operations such as deoxidation and desulfurization are done in order to obtain the correct
amounts of oxygen and sulphur in the steel. These elements contribute to the formation of
non-metallic inclusions in steel during solidification and the consequences of these inclusions
are catastrophic to the mechanical properties of the material during usage. Elements such as
Al, Si, Ca and the Rare Earth Metals (REM) are used to remove oxygen and sulphur from
steel. Micro inclusions (1-20µm) that may formed from the reactions of these elements often
coagulate to form clusters and inclusions of bigger sizes (>100µm) known as macro
inclusions [9].

3. BLUE FRACTURE TESTING

Blue fracture testing of macro non-metallic inclusions may be carried out quantitatively or
qualitatively. Quantitative examination is carried out by counting the inclusions and using
one or both of the following parameters of the inclusions: length and thickness.

The distribution of the inclusions based on length is given in table 2.

Table 2. Inclusion distribution based on length [7].

Symbol Length l (mm)
L0 No macroscopic inclusion
L1 1,0≤ l ≤ 2,5
L2 2,5≤ l ≤ 5
L3 5,0≤ l ≤ 10
L4 l >10

The distribution of the inclusions based on thickness is given in table 3.

Table 3. Inclusion distribution based on thickness [7].

Symbol Thickness e (mm)
T0 No macroscopic inclusion
T1 0,1≤ e ≤ 0,25
T2 0,25≤e ≤ 0,50
T3 0,5≤ e ≤ 1,0
T4 e >1,0

Qualitative examination is carried out by comparison with the series of ten reference
diagrams, figure 2. Account is taken of the positions of the inclusions within the section for
example core, surface or uniform distribution,
 Explanation of terms:
Very short stringers: 1 to 2,5 mm Few: ≤ 3
Short stringers: > 2,5 mm Several: > 3
Long stringers: > 5 mm Thick: > 0,5 mm

Figure 2. Standard diagrams for the blue fracture test method [7].

4. MATERIAL FOR TESTING

For this paper work, wrought bar diameter φ 60 mm bearing steel 100Cr6 was tested.
Chemical composition is given in table 4:

Table 4. Chemical composition of bar φ 60 mm

Chemical composition, %
Material
C Si Mn P S Cr

100Cr6 0,85 0,56 1,10 0,011 0,014 1,47

5. EXPERIMENTAL PART
Blue fracture testing was done at Metallographic and Mechanical laboratories of Institute
“Kemal Kapetanović” of Zenica.

5.1 Sampling of test piece

Test pieces are slices with thickness of 10 mm. The thickness being measured parallel to the
longitudinal direction. For this paper work three samples were tested. The test pieces for blue
fracture testing are given at figure 3.

Figure 3. Test pieces for blue fracture testing

5.2 Preparation of test piece

Both sides of the test piece is prepared to get plan-parallel surfaces. At the center of the
normal side of the longitudinal axis of the rod, a groove was formed. The purpose of this
groove is to facilitate the fracture of the test piece. The groove depth is up to 2 mm. Test
pieces were heated in laboratory furnace so that at moment of starting the test, the metal is at
blue brittleness temperature (350-400°C). After heating samples fractured with the testing
mashine AMSLER, 200kN in the Mechanical laboratory, (fig. 4a). Broken samples is shown
at fig 4b.

a) b)
Figure 4. AMSLER - Testing mashine and broken sample

5.3 Testing procedure

One of two broken parts of test piece is examined with magnification less then to X 10 using
stereo light microscope TECHNIVAL 2. Testing results are given in table 5. The broken
surface is compared to diagram chart given at figure 2.
Table 5. Blue fracture testing of bar φ 60 mm
Testing
Sample Thickness of non- Length of non-
area Total length of non-metallic
of metallic inclusion metallic inclusion
inclusion per testing area
100Cr6 (mm) (mm)
(dm2)
1 0,20 1,5 0,035
2 0,20 1,0 0,035 4,3 mm / 0,112 dm2
3 0,25 1,8 0,420
 In accordance to diagram chart given at figure 2 given in standard BAS ISO 3763:2009 the
assessment is: 1.
Macro non metallic inclusion observed on one of the test piece is given at figure 5 .

Non metallic
inclusion

a) X10 magnification b) X40 magnification

Figure 5. Macro non metallic inclusion in blue fracture

6. CONCLUSION
Based on the performed treatment heating at temperature of blue fracture and samples testing
at X10 magnification, macro non-metallic inclusion, very short stringer, was detected. By the
length and thickness of the macro nonmetallic inclusion were estimated at 1.
Blue fracture as a method of testing macro non-metallic inclusions is relatively simple and
reliable. The size of the detected non-metallic inclusions indicates the risk of application of
the test batch and indicates the need for further testing due to possible influence of the
presence of non-metallic inclusions on the mechanical properties of steel 100Cr6.

7. REFERENCE
[1] Juvonen P.: Effects of non-metallic inclusions on fatigue properties of calcium treated steels,
dissertation, Helsinki, 2004.
[2] http://ispatguru.com/non-metal-inclusions-in-steels/( seen 10.02.2018.)
[3] Šuman H.: Metalografija, Univerzitet u Beogradu, Zavod za izdavanje udžbenika SR Srbije,
Beograd, 1962. (str. 325 – 330)
[4] Bhadeshia H.K.D.H.: Steels for bearings, Progress in Materials Science 57 (2012), 268–435
[5] Volchok I.P., Vilniansky A.E.: Effect of non-metallic inclusions on crack propagation and fatigue
life of steel, (http://www.gruppofrattura.it/ocs/index.php/esis/ECF13/paper/viewFile/8452/4896,
29.11.2017.)
[6] Thornton P.A.: The influence of non-metallic inclusions on the mechanical properties of steel: a
review, Journal of materials science 6, 1971.
[7] Standard ISO 3763: 2009 – Wrought steels - Macroscopic methods for assessing the content of
non - metallic inclusions
[8] Standard: S130000:2010: Technical delivery conditions – Steel and Iron – Rolling bearing steel
100Cr6
[9] Asumadu T.K.: Macro inclusion research: Detection and evaluation of macro inclusions in special,
Stockholm, 2012.

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