=Paper= {{Paper |id=Vol-2485/paper54 |storemode=property |title=Visualization of the Phase Volume Distribution in Alloys |pdfUrl=https://ceur-ws.org/Vol-2485/paper54.pdf |volume=Vol-2485 |authors=Konstantin Makarenko,Sergey Kuzovov,Alexander Nikitin }} ==Visualization of the Phase Volume Distribution in Alloys == https://ceur-ws.org/Vol-2485/paper54.pdf
                Visualization of the Phase Volume Distribution in Alloys
                                      Makarenko K.V., Kuzovov S.S., Nikitin A.A.
                              makkon1@yandex.ru| kss41188@inbox.ru|zzzalexzzz95@gmail.com
                                          BSTU, Bryansk, Russian Federation
    The method of obtaining the volume distribution of phases in structural materials is considered. The technique is based on the layer-
by-layer grinding of metallographic samples with photo fixation of microstructure images and the subsequent computer processing of
these images. An example of using the developed methodology to study the features of the volumetric distribution of graphite inclusions
in high-strength cast irons is presented. The classification of graphite inclusions depending on the shape, size and distribution features
is given. The study of the features of the distribution of graphite inclusions led to the conclusion about the patterns and mechanisms of
formation graphite phase in cast iron.
    Keywords: visualization, tomography, volume distribution, phase, materials, cast iron, graphite.

                                                                        investigated cast iron, % mass: 3.17 C; 3.3 S; 0.76 Mn, 0.06 P;
    1. Introduction                                                     0.03S; 0.05 Mg.
                                                                               Cast iron was cast into sand and loam moulds for making
         The methods of obtaining the idea about the volume
                                                                        the castings of different shapes and blanks in the form of the
    distribution of phases in different structural materials have
                                                                        block of size 500x500x1000. From the blanks were obtained the
    undergone considerable evolutionary development in recent
                                                                        specimens for metallographic investigations, in the castings were
    decades. Basic principles and approaches were laid down in
                                                                        investigated the microstructure of special boss specimens and
    the works by S.A.Saltykov [9]. The methods which were used
                                                                        elements of pouring gate systems.
    by stereometric metallography were characterized by high
                                                                               Subsequent investigations of the volume distribution of
    labor intensity and required from the researcher special
                                                                        graphite inclusions were carried out on one specimen cut out
    preparation and thorough execution of the developed methods.
                                                                        from the blank, with the use of methods of optical tomography
    However, the results which were obtained in the course of
                                                                        (fig.1)
    present investigation, widened considerably the idea
    (conception) about the processes going in the materials, and
    allowed to maintain important relations between their
    structure and properties. For example, the works by K.P.Bunin
    with his pupils [1], allowed to get the idea about morphology
    of graphite inclusions in grey cast irons.
                The wide introduction of computer methods of                     a)                     b)                   c)
    processing the images simplified considerably the methods                   Fig.1. Stages of processing the images of the
    and visualizations of phase volume distribution in alloys.            microstructure of the high-strength cast iron:
    However, the approaches remained the same.                                  a) – initial image of microstructure x80;
         At the present time an individual direction named as a                 b) – transformation to binary image of graphite
    three-dimensional one [5,12,6] is developing intensely in the         inclusions distribution in the plane of the metallographic
    material science. As follows from the name, with such an              specimen;
    approach the structures of the described materials have a 3-                c) – summation of binary images
    dimensional (volume) image. Undoubtedly, such an approach
    allows to obtain a more integral and realistic idea about the              As reference points served the imprints of introduction of
    structure of the materials and processes going in them              the hardness tester indenter TK-2M in the surface layers of the
    [11,3,4,2,8].                                                       metallographic specimen. For obtaining the idea about volume
         The main method which is used by the new direction in          location of the graphite phase the layered machining was made
    the material science is a computer computational tomography         on the grinding-and-polishing machine-tool TIME PG-1000.
    [7]. Tomography used in the material science, uses different        The calculation of the depth of grinding was determined by the
    physical processes and methods for investigation of internal        change of the diameter of the harness tester indenter imprint
    structure of materials: X-ray, magnetic-resonance, acoustic         (fig.2). The diameter of the imprint was determined by means of
    ones and a traditional one based on the mechanical layered          the special eyepiece with the scale, for the graduation of which a
    grinding the material with obtaining 2-dimensional images of        reference object (micrometer) was used.
    the structure and their subsequent summation and transition
    to the volume representation [9].
         In the present article the methods is presented based on the
    latter approach of computer tomography. The developed
    methods was used for the study of peculiarities of distribution
    of the graphite phase in high-strength cast irons.
                                                                                     a)                     b)                     c)
        2. Methods of Holding the Investigation                                 Fig. 2. Methods of determination of the grinding depth:
                                                                                a) – diagram of introduction of hardness tester
         For the study of volume distribution of graphite phase in        indenter and obtaining the imprint;
  cast irons the cast iron was made in the production conditions of             b) – photo of initial imprint of indenter on the surface
  the cast iron workshop of the CJSC «UK BMZ». The specimens
                                                                          of the investigated specimen;
  were investigated from the cast iron which was produced by
  means of induction melting in the furnace PVK-NK, based on                    c) – geometric diagram of determination of depth at
  the remelting of conversion pig iron PVK-NK and steel С245.             successive grinding of the specimen along the change of
  As a carburizer, the graphitized coke breeze was used.                  indenter imprint diameter.
  Inoculation was made in the ladle by the sandwich process, the
  inoculant FeSiMg-7. The average chemical composition of the




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         Distribution of graphite was studied on the non-etched          simultaneously and crystallized in the same conditions. In the cast
    metallographic specimen with the help of the inverted                iron structure the chains occur which are represented only by
    metallographic microscope Nikon ECLIPSE MA 200 with                  small inclusions, or small inclusions are at the beginning (at the
    magnification x80. The observed microstructure was fixed             end) of the chain. It is explained by the fact that on the
    with the help of the digital camera built into the microscope.       metallographic specimens at the layered grinding the complete
    The next processing of the obtained photos was made with the         inclusion is not present wholly, but only the projections of the cut
    help of program Above Photoshop and Image J. For obtaining           (section) corresponding to the upper or lower part of the graphite
    the image of volume distribution of graphite inclusions in the       spheroid, cut by the plane of the metallographic specimen during
    matrix of the cast iron was used the program module Image J,         investigation. The observed chains do not have any generalizing
    for rendering the volume images – the module Volume J.               regularities in structure. By topological structure they form nuclear
                                                                         complexes passing into each other which bifurcate and inosculate,
                                                                         or grow (swell) in layers. Under the cell in this case the eutectic
    3. Results of Investigations                                         cell is meant.
                                                                                     Besides the spheroidal graphite, in the cast iron
               The results of computer processing of the
                                                                         microstructure are present inclusions of irregular compact shape.
    microstructure are presented in fig.3. Unfortunately, such an
                                                                         They have comparatively big sizes. It means that in the process of
    image does not allow to evaluate fully the picture of volume
                                                                         growth they do not lack in carbon. Such graphite, as a rule, is not
    distribution of the graphite phase in cast irons, because
                                                                         included into chains and is located in the microstructure apart
    graphite inclusions on different levels obstruct each other.
                                                                         (fig.4, a and b).
                                                                                     Location and shape of graphite inclusions of non-
                                                                         spheroidal shape show that they appear at the final stage of
                                                                         hardening the cast iron, in the conditions not allowing their
                                                                         spheroidizing because of the lack of Mg.
                                                                                     Besides the above-mentioned graphite forms, in the cast
                                                                         iron microstructure the areas occur with especially big inclusions,
                                                                         fig. 4, a and b. The prevailing size shows that graphite spheroids
                                                                         are initial. The composition of the investigated cast iron is eutectic
                                                                         one , however, the elements of structure of hypereutectic cast iron
                                                                         are present. Formation of excessive, even for layers of eutectic
                                                                         composition, primary phases was also observed earlier, in
                                                                         particular, in systems Al-Si, Pb-Bi and Zn-Gd [10]. The arisen
                                                                         contradiction is explained by a considerable deviation in the
                                                                         processes of hardening of real production alloys from balanced
                                                                         conditions of crystallization of eutectic alloys. The main reason
                                                                         which results in appearing the primary crystals of phases is
                                                                         fluctuation of chemical composition. For cast irons the increase of
                                                                         stability of chemical composition fluctuations is conditioned by
    Fig.3. Volume distribution of graphite inclusions in high-           additional inoculation. Initially in the melt Fe-C-Si there are areas
    strength cast iron with spheroidal graphite                          with different content of carbon and silicon, hereby the areas
                                                                         enriched with silicon are depleted with carbon, and vice versa; this
                                                                         is connected with influence of silicon on thermodynamic activity
               The next analysis was carried out on separate levels      of carbon. At inoculation with silicon-containing spheroidizating
    with division of initial mass into 2 separate layers. The results    alloying compositions to which also refers the inoculant FeSiMg-
    of the analysis in the form of projections of isolines of graphite   7, the process of heterogenisation increases. In the areas with
    inclusions are presented in fig.4, a and b.                          increased concentration of carbon graphite inclusions start
                                                                         forming, as the concentration of carbon in these areas exceed
                                                                         ultimate solubility in the iron melt at this temperature. Fluctuations
                                                                         of the content result in arising not only individual inclusions of
                                                                         primary graphite (fig.4 , a), but also in formation of spheroidal
                                                                         cluster consisting of several primary inclusions (fig.4, b). The
                                                                         structure of the cluster presented by the chains of graphite
                                                                         inclusions, shows the unified mechanism of distribution of
                                                                         inclusions of primary and eutectic graphite.
                                                                                     Thus, graphite inclusions observed in the cast iron
                                                                         microstructure can be classified by the following kinds: I - cluster
                a)                               b)
                                                                         and individual inclusions of primary graphite of spheroidal shape;
      Fig.4. Layered distribution of graphite inclusions in high-
                                                                         II – spheroidal inclusions of eutectic graphite         and III –large
      strength cast iron:
                                                                         compact inclusions of non-spheroidal shape.
            a) – layer consists of 10 images;
                                                                                     Based on classification of graphite inclusions, the
            b) – layer consists of 8 images                              pattern of distribution of graphite phase in the high-strength cast
                                                                         iron is developed. Morphological peculiarities of the structure of
                                                                         graphite inclusions, observed on metallographic specimens, can be
                                                                         explained by the fact that graphite in the cast iron forms in several
    4. Discussion of Results                                             stages.
           During the analysis of images (fig.4) the fact draws                      At the initial stage of crystallization after inoculation
attention that the chains of inclusions are represented by graphite      occurs heterogenization of the melt by silicon and carbon.
spheroids of approximately the same size. Apparently, such               Heterogenization of the melt results in its separation into layers. In
graphite inclusions making the chain,              were nucleated        the areas with increased concentration of carbon the centres of
                                                                         crystallization of graphite start to arise. The subsequent
overcooling, which arises at the inoculation of the melt with                        The structures of chains of graphite inclusions, formed
magnesium-containing alloying compositions, stabilize the nuclei         in the process of crystallization of the high-strength cast iron, are,
of graphite inclusions. The nuclei of graphite phase grow with big       by themselves, fractal clusters, which can be described with the
speeds on account of accelerated diffusion of carbon and get big         help of the CCA pattern (Cluster-Cluster Aggregation). In this
sizes. Graphite inclusions arising in the melt volume, limited by        pattern the particles colliding with each other, form originally
fluctuation, during the contact which is caused by their growth and      simple clusters, which later unite in the clusters of big sizes. The
the size of fluctuation, form spherical cluster at the moment            clusters arising in the melt, consisting in eutectic nuclei, manifest
preceding formation of the austenite shells. In case when sizes          themselves most clearly in the flaws of shrink origin. In shrink
of arising fluctuation are comparatively small, a single inclusion       cavities, at the condition when the mother liquor, enriched with
of primary graphite forms in it. Hereby, in case of formation of         segregated materials and carbon, is removed in the process of
several centres of crystallization of graphite in a small area of the    shrinkage, the crystallized welded cluster chains of eutectic grains
melt, occurs their accretion into one big inclusion in accordance        are found in the shrink porosity. This is the proof of the suggested
with the mechanism of overcondensation.                                  cluster pattern of distribution of graphite inclusions in high-
           At the next stage in the areas of the melt with chemical      strength iron.
composition corresponding to eutectic content of the alloy                           Big graphite of irregular compact shape is crystallized at
components, eutectic cells start to form, which present by               the last stage from the mother melt, in the areas stuck by growing
themselves graphite of spheroidal shape covered with shells of           austenite-and-graphite eutectic aggregates. The proof of
crystallizing austenite. Graphite nuclei in the melt areas arise         crystallization of graphite from the mother liquor are the fringes
evenly, the process of coalescence, which aligns average sizes           of graphite observed in shrink cavities. Graphite crystallizing at
of centres of graphite crystallization, prevents them from               the last stage, is surrounded, as a rule, by the pearlite structure and
segregation.                                                             does not have any ferrite fringes of the “bull’s eye” type. The
           In case of arising, beside the growing graphite nucleus,      conditions of formation of graphite inclusions do not contribute to
of another smaller one, a gradual enlargement of the smaller one         spheroidization of graphite, and it degenerates into the compact,
is observed, on account of diffusion of carbon from small nuclei         close to vermicular, X-shape. Apparently, the last portions of
to big ones, which arose earlier. Graphite inclusions form at the        metal crystallize without concentration of residual magnesium,
big rates of overcooling and are covered with austenite shell earlier    required for spheroidization of graphite.
than primary graphite, which slows down their subsequent growth.
Chemical composition of austenite surrounding graphite                         5. Conclusion
inclusions, has the increased concentration of silicon, which
                                                                               Methods of visualization of phase volume distribution in
confirms the fact of formation of ferrite areas around graphite, the
                                                                           alloys is developed. The suggested method is used for the
so-called “ a bull’s eye “ structure. The growth and formation of
                                                                           analysis of peculiarities of graphite phase distribution in high-
graphite inclusions at this stage occurs in the areas of the melt with
                                                                           strength cast irons and for the study of crystallization process.
the increased content of silicon.
                                                                           The processes of primary structure formation of graphite phase
           The organization of the chains of eutectic graphite,
                                                                           in high-strength cast irons are investigated. At the use of
observed on the metallographic specimen is caused by weldability
                                                                           methods of stereology and digital metallography was obtained
of austenite shells and their subsequent joint growth during
crystallization. At this stage, due to the shortfall of carbon             3D-distribution of graphite inclusions in the cast iron. The
                                                                           classification of graphite inclusions dependent on the shape,
duffusing through austenite shells, the neighbouring (competitive)
                                                                           sizes and peculiarities of their distribution, is stated. The
graphite inclusions can get the shape of ellipsoids and form the
                                                                           hypothesis is proposed about the fact that structures of chains of
necks uniting them (fig.5).
                                                                           graphite inclusions forming in the process of crystallization of
                                                                           the high-strength cast iron, are actually fractal clusters which
                                                                           can be described with the help of the CCA pattern (Cluster-
                                                                           Cluster Aggregation).

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