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    <journal-meta />
    <article-meta>
      <title-group>
        <article-title>Fractographic analysis of fractures of graphitized cast iron using optical microscopy</article-title>
      </title-group>
      <contrib-group>
        <contrib contrib-type="author">
          <string-name>K.V. Makarenko</string-name>
          <xref ref-type="aff" rid="aff0">0</xref>
        </contrib>
        <contrib contrib-type="author">
          <string-name>A.A. Nikitin</string-name>
          <xref ref-type="aff" rid="aff0">0</xref>
        </contrib>
        <contrib contrib-type="author">
          <string-name>A.S. Parenko</string-name>
          <xref ref-type="aff" rid="aff0">0</xref>
        </contrib>
        <contrib contrib-type="author">
          <string-name>Bryansk</string-name>
          <xref ref-type="aff" rid="aff0">0</xref>
        </contrib>
        <contrib contrib-type="author">
          <string-name>Russian Federation</string-name>
          <xref ref-type="aff" rid="aff0">0</xref>
        </contrib>
        <aff id="aff0">
          <label>0</label>
          <institution>Makarenko Konstantin V., Doctor of Technical Sciences, Professor, Department of Engineering and Materials Science, Bryansk State Technical University</institution>
        </aff>
      </contrib-group>
      <abstract>
        <p>Fractography - methods for studying material fractures, the science of the structure of fracture surfaces. Fractography is widely used to determine the causes of destruction of materials and structures. In materials sciences, fractography is used to study crack propagation, microstructure studies, and quality control. When investigating the failure of structures, determining the type of crack (material fatigue, hydrogen embrittlement, stress corrosion cracking, exceeding the permissible load, etc.) makes it possible to determine the cause of the failure. Fractographic studies include the study of a fracture with the naked eye, using an optical and electron microscope. Other methods are also often used, such as measuring hardness or studying the distribution of chemical elements using Xray spectral microanalysis. Fractographic (or fracture) analysis is the first and obligatory stage of research that must be performed by an expert of the metallurgical examination laboratory when determining the causes of material destruction. Visual examination of the fracture (fracture) surface makes it possible to establish the location of the beginning of fracture, the nature of its further course, to make a judgment about the degree of plasticity of the material and about possible structural defects that led to the initiation and development of cracks. The use of fractographic analysis methods for reconstructing the fracture surface of graphitized cast iron is proposed. The influence of various inclusions in the structure of cast iron is considered. A study of the fracture surface of graphitized cast irons was carried out, and the causes affecting the fracture process were identified.</p>
      </abstract>
      <kwd-group>
        <kwd>cast iron</kwd>
        <kwd>graphite</kwd>
        <kwd>fracture</kwd>
        <kwd>fractographic analysis</kwd>
      </kwd-group>
    </article-meta>
  </front>
  <body>
    <sec id="sec-1">
      <title>1. Introduction</title>
      <p>
        Fractography as a method for learning fracture’s is
widely used in examinations to identify the causes of the
destruction of various parts of machines and objects.
Traditionally, scanning electron microscopy is used for
these purposes [
        <xref ref-type="bibr" rid="ref1">1-3</xref>
        ]. A distinctive feature of the imaging
 2 +
250
 
+

2 2
high strength
gray
 =
C
3,5
useful increase; А – lens aperture; n – refractive index; λ –
light wavelength. DOF becomes smaller as the numerical
aperture and microscope increase (for example, for white
light Т=54 μm at А=0,17, N=90 and Т=0,6 μm at А=1,25,
N=1080). These numbers characterize the height of those
structural details that can be examined with a single
microscope setup.
      </p>
      <p>
        Modern digital microscopes based on the use of
traditional optical systems using specialized software make
it possible to solve the problems of fractographic analysis
without the use of expensive electron microscopes [
        <xref ref-type="bibr" rid="ref4 ref5 ref6">6-8</xref>
        ].
      </p>
      <p>The aim of the article is to demonstrate the capabilities
of digital optical microscopy in conjunction
with the
developed image processing algorithms for obtaining
fractographic images of fractures of the surfaces of
graphitized cast irons.
2.</p>
    </sec>
    <sec id="sec-2">
      <title>Research methodology</title>
      <p>Test specimens were made from graphitized cast iron
smelted in induction furnaces. The melt was modified by
magnesium in an autoclave to obtain spherical graphite in
it. Gray cast iron modification was carried out in a ladle by
ferrosilicon. The chemical composition of graphitized cast
irons is presented in table 1.</p>
      <p>Content elements %
2,4
1,6</p>
      <p>Mn
1,0
1,3</p>
      <p>S
0,02
0,06</p>
      <p>P
0,04
0,4</p>
      <p>Cr
0,4
0,3</p>
      <p>Ni
1,3
0,4</p>
      <p>Mo
0,7
0,35
0,05</p>
      <p>After modification, cast irons were poured into dry
sand-clay molds to obtain solid sleeve castings ∅ 130 mm.</p>
      <p>From castings of high-strength and gray cast iron on a
lathe, blanks of rings with a section of 6×3,5 mm and 6×5
mm were cut. The castle was cut in the rings. In order to
reduce the influence of segregation phenomena, the rings
were subjected to heat treatment. Heat treatment for rings of
ductile and gray cast iron: austenitization temperature
850оС, holding time 60</p>
      <p>min; air cooling to room
temperatures; tempering 410оС for 60 min.</p>
      <p>After heat treatment, microstructural research and tests of
mechanical properties were carried out (table 2). Bending test
of heat-treated rings was carried out in accordance with the
scheme shown in the fig. 1.</p>
      <p>Copyright © 2020 for this paper by its authors. Use permitted under Creative Commons License Attribution 4.0 International (CC BY
Cast iron class
High-strength</p>
      <p>For 3-dimensional reconstruction of fracture surfaces,
a layer-by-layer microscopy method was used. The
method allows to obtain topographic reliefs of volumetric
objects based on information from partially sharp images.</p>
      <p>To do this, using a digital microscope, we recorded images
of the microstructure of the fracture surface with a certain
depth step. The study and registration of the microstructure
was carried out on an analytical computerized complex,
which was created on the basis of an inverted Leica DM
IRM metallographic microscope. A number of such
images are presented in Fig. 2.</p>
      <p>Fig. 2. The initial series of images of fracture of a sample of
high-strength cast iron with spherical graphite with a depth step</p>
      <p>of 8 μm, ×200</p>
      <p>Optical Reconstruction 3D (OptiRec3D – developer
Ph.D. Chmykhov D.V. (FSBEI BO BSTU)) software was
used to reconstruct the surface of cast iron fracture from
the initial series of previously obtained images. The
program performs volumetric reconstruction of the surface
by a set of photographs of one object photographed with a
given depth step. OptiRec3D has a good source data
processing speed and high accuracy of reconstructed
models. An example of the volume surface of a fracture of
a sample of High-strength cast iron with nodular graphite
is presented in Fig. 3.</p>
      <p>Fig. 3. The fracture surface of ductile iron obtained using the</p>
      <p>optical reconstruction program OptiRec3D</p>
      <p>To obtain a fracture image of the surface of graphitized
gray and ductile iron, a set of photographs of
microstructures was used. Image spacing 8 μm for
Highstrength cast iron and 12 μm for gray iron. The pixel size
in the images was determined by the increase in the lens,
in both cases it was 0.637 μm. The fracture surface of
High-strength cast iron with a surface image (Fig. 4) is
shown in Fig. 5.</p>
      <p>Fig. 4. The microstructure of the fracture surface of a sample of</p>
      <p>High-strength cast iron with spherical graphite, obtained by
summing up areas with high definition from various images of a
number of data (etching with 4% alcohol solution of nitric</p>
      <p>acid), × 200
Fig. 5. The fracture surface of a sample of high-strength cast
iron with spherical graphite with an overlaid image of its</p>
      <p>microstructure</p>
      <p>The fracture structure of gray cast iron with lamellar
graphite after various stages of the surface reconstruction
operation is shown in Fig. 6.</p>
      <p>Fig. 6. The fracture surface of gray cast iron with lamellar
graphite: a - surface microstructure × 200; b - volumetric
reconstruction of the surface with the applied microstructure; c
model of fracture surface obtained using OptiRec3D software</p>
      <p>The fracture surface of gray cast iron (Figure 6, b) is
characterized by a rougher structure and a pronounced
relationship with the location of the graphite phase than
that of a sample of high-strength cast iron. An analysis of
the image of the fracture surface shows that cracks in the
fracture process mainly formed along the planes of
graphite inclusions (Figure 6, a). The observed picture
indicates that the destruction passed through the centers of
the eutectic colonies, where the graphite inclusions have
the largest transverse dimensions. In these areas of cast
iron, the metal matrix is strongly fragmented by the
graphite phase.</p>
    </sec>
    <sec id="sec-3">
      <title>The discussion of the results</title>
      <p>Analysis of the fracture surface shows that nonmetalic
inclusions also contributed to the destruction of gray cast
iron. Greater pollution of cast iron by sulfur and additional
doping with phosphorus lead to the appearance of sulfide
inclusions and regions with phosphide eutectics in the
structure, which, like graphite, are stress concentrates.</p>
      <p>Phosphide eutectic and sulfide inclusions in the
structure of cast iron are usually concentrated on the
periphery of eutectic colonies. In these areas on the surface
model (Figure 6, b) peaks and troughs are observed,
indicating that the destruction occurred precisely on these
structural elements. The negative effect of phosphide
eutectic is explained by the fact that it, hardening at the last
stage of crystallization, isolates individual eutectic cells,
thereby creating interfaces in the structure. The interface,
as well as graphite plates, violate the continuity and
uniformity of the metal matrix. Cementite inclusions
present in phosphide eutectic increase its hardness and
contribute to brittle fracture. Thus, a crack in gray cast iron
can pass either through eutectic cells along the graphite
planes, or bypassing them and collapsing along sulfide
inclusions or regions of phosphide eutectic.</p>
      <p>Despite the fact that graphite inclusions in high-strength
cast iron have the shape of spheroids, and this, according to
numerous authors, significantly weakens their negative
impact on mechanical properties, the features of their
distribution, as shown above, affect the mechanism of cast
iron fracture. When studying the microstructure of the
fracture surface of high-strength cast iron (Figure 4), it is
noteworthy that the fracture surface passes along the chains
of graphite inclusions. Analysis of the fracture surface shows
that it is precisely along the cluster chains of eutectic cells that
cast iron is destroyed.</p>
      <p>The destruction of High-strength cast iron rings takes
place in several stages. At the initial stage, the nucleation
of cracks begins at the boundary “graphite - metal matrix”,
because, despite their compact form, graphite inclusions
separate the metal matrix of cast iron. Then, the process of
separation of the structure is localized by plastic
deformation of the metal matrix. At this stage, the
development of microcracks follows the paths of least
resistance along those sections of the metal matrix that are
between two adjacent graphite inclusions. The weakening
of the metal matrix occurs as a result of the occurrence in
the structure of isthmuses between adjacent graphite
inclusions combined into cluster chains. Figure 4 shows that
the graphite inclusions emerging on the fracture surface are
interconnected and form “strings” along which the crack
propagates during fracture. Moreover, in the process of
fracture, graphite inclusions often remain intact, which
indicates the existence of a gap between graphite and a
metal matrix. At the final stage, the fusion of microcracks
begins and the destruction of cast iron occurs.</p>
      <p>In high-strength cast iron, nonmetalic inclusions are
much smaller than in gray cast iron, so their effect on the
destruction processes is reduced. When studying the
surface structure of fracture of ductile iron (Figure 5),
there are practically no peaks and depressions, which, as
previously shown, for gray iron are parts of the structure
where nonmetallic inclusions are located. The reason of
this is that the contained in the ligature magnesium used to
modify cast iron is partially spent on desulfurization,
binding sulfur to a compound removed with slag</p>
      <p>Research of fracture surfaces of graphitized cast irons
prove that the destruction processes are influenced not
only by the shape, but also by the distribution of the
graphite phase.
4.</p>
    </sec>
    <sec id="sec-4">
      <title>Conclusion</title>
      <p>The results of using a modern digital optical
microscope in combination with specialized software
presented in the article made it possible to obtain
highquality fractograms of fractures of graphitized cast irons.
The results demonstrated a high degree of adequacy and
allowed us to assess the relationship between the structure
of the material and the processes of destruction The
potential inherent in this method will expand the
capabilities of traditional optical microscopy and is an
excellent alternative to expensive scanning electron
microscopy.</p>
    </sec>
    <sec id="sec-5">
      <title>References:</title>
      <p>[1] Stremel, M.A. Possibilities of fractography / M.A.</p>
      <p>Stremel / Metallurgy and heat treatment of metals.
2005. - No. 5 (599). - pp. 35-43.
[2] Stremel, M.A. On the analysis of images in
fractography (methodological notes) / M.A. Stremel /
Deformation and fracture of materials. - 2015. - No. 10.
- pp. 2-9.</p>
    </sec>
    <sec id="sec-6">
      <title>About the authors</title>
    </sec>
  </body>
  <back>
    <ref-list>
      <ref id="ref1">
        <mixed-citation>
          [3]
          <string-name>
            <surname>Strelnikov</surname>
            ,
            <given-names>I.V.</given-names>
          </string-name>
          <article-title>Quality issues of plasma spot welding: metallography</article-title>
          , fractography, statistics / I.V.
          <string-name>
            <surname>Strelnikov</surname>
            ,
            <given-names>A.V.</given-names>
          </string-name>
          <string-name>
            <surname>Konovalov</surname>
            ,
            <given-names>F.</given-names>
          </string-name>
          <article-title>Stempfer / Welding and diagnostics</article-title>
          . -
          <source>2010</source>
          . - No. 5. - pp.
          <fpage>47</fpage>
          -
          <lpage>50</lpage>
          .
        </mixed-citation>
      </ref>
      <ref id="ref2">
        <mixed-citation>
          [4]
          <string-name>
            <surname>Clarke</surname>
            ,
            <given-names>A.R.</given-names>
          </string-name>
          <string-name>
            <surname>Microscopy</surname>
          </string-name>
          <article-title>Techniques for Materials Science /</article-title>
          <string-name>
            <given-names>A.R.</given-names>
            <surname>Clarke</surname>
          </string-name>
          ,
          <string-name>
            <given-names>C.N.</given-names>
            <surname>Eberhardt</surname>
          </string-name>
          . - England, Cambridge: Woodhead Publishing Limited,
          <year>2002</year>
          . - 459 p.
        </mixed-citation>
      </ref>
      <ref id="ref3">
        <mixed-citation>
          [5]
          <string-name>
            <surname>Wu</surname>
            ,
            <given-names>Q Microscope</given-names>
          </string-name>
          <string-name>
            <surname>Image</surname>
            <given-names>Processing</given-names>
          </string-name>
          / Qiang Wu, Fatima A.
          <string-name>
            <surname>Merchant</surname>
          </string-name>
          ,
          <string-name>
            <surname>Kenneth</surname>
            <given-names>R.</given-names>
          </string-name>
          <string-name>
            <surname>Castleman</surname>
          </string-name>
          . - England, London: Elsevier,
          <year>2008</year>
          . - 548 p.
        </mixed-citation>
      </ref>
      <ref id="ref4">
        <mixed-citation>
          [6]
          <string-name>
            <surname>Makarenko</surname>
            ,
            <given-names>K.V.</given-names>
          </string-name>
          <article-title>Fractal Analysis of Morphological Parameters of the Structure Materials /</article-title>
          K.V.
          <string-name>
            <surname>Makarenko</surname>
            ,
            <given-names>A</given-names>
          </string-name>
          .A. Nikitin // CEUR Workshop Proceeding of the 9th
          <source>International Conference on Computer Graphics and Vision</source>
          (GraphiCon
          <year>2019</year>
          ). - Vol.
          <volume>2485</volume>
          . - pp.
          <fpage>240</fpage>
          -
          <lpage>243</lpage>
          .
        </mixed-citation>
      </ref>
      <ref id="ref5">
        <mixed-citation>
          [7]
          <string-name>
            <surname>Panteleev</surname>
            , V.G. Computer microscopy / V.G. Panteleev,
            <given-names>O.V.</given-names>
          </string-name>
          <string-name>
            <surname>Egorova</surname>
            ,
            <given-names>E.I.</given-names>
          </string-name>
          <string-name>
            <surname>Klykova</surname>
          </string-name>
          . - M: Technosphere,
          <year>2005</year>
          . - 304 p.
        </mixed-citation>
      </ref>
      <ref id="ref6">
        <mixed-citation>
          [8]
          <string-name>
            <surname>Zentsova</surname>
          </string-name>
          , EA Digital optical microscopy / E.A. Zentsova // In the collection:
          <article-title>Innovations, quality and service in engineering and technology Collection of scientific papers of the 5th International Scientific</article-title>
          and
          <string-name>
            <given-names>Practical</given-names>
            <surname>Conference</surname>
          </string-name>
          . - 2015 - pp.
          <fpage>150</fpage>
          -
          <lpage>153</lpage>
          .
        </mixed-citation>
      </ref>
    </ref-list>
  </back>
</article>