Ciwt~on Vol. 29. No,. 4!5. pp. 547-555. 1991 oow-6223191 $3.110 + .

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THE FORMATION OF KISH GRAPHITE

SHENGLI Lru and CARL R. LOPER, JR.

Department of Materials Science and Engineering, The University of Wisconsin-Madison,
Madison, WI 53706

(Received 4 September 1990; accepted in revised form 2 October 1990)

Abstrac&-The formation mechanism of kish graphite has been studied by observing the morphology
developed under a number of experimental conditions. Kish graphite is formed on the free surface of
molten iron and grows in a foliated dendritic manner. However, this surface formation mode mty,be
suppressed in favor of graphite formation within the melt by increasing the cooling rate and avoiding
the presence of oxygen at the melt surface. Oxygen not only affects the graphite morphology by attacking
the growth front of kish graphite crystal, but promotes nucleation of graphite on the melt surface.
Increased cooling rates and exposure of the melt to oxygen favor the formation of a foliated dendritic
structure. On the other hand, slow cooling and avoidance of oxygen result in the formation of a graphite
ahcet over the melt surface. In addition, sulfur has been shown to play an important role in the formation
of kish graphite.
Key Words-Kish graphite, graphite morphology, foliated dendritic structure.

1. INTRODUCTION the formation of silicate substrates[ 17,191. Contin-

Kish graphite is typically a byproduct formed in the
manufacture of blast furnace hot metal or in cast
irons. Carbon in excess of the solubility limit sepa-
rates from the molten iron as graphite flakes as the
melt is cooled. A considerable tonnage of kish graph-
ite is produced daily in steel production. Kish graph-
ite has long been recognized as an example of
graphite having ideal, or near ideal, crystal struc-
tures[l]. X-ray diffraction analysis has shown that
the structure of kish graphite is almost identical with
that of natural graphite[2,3,4]. The electronic and
magnetic properties, electronic band structures, etc.
of kish graphite have been investigated in more re-
cent studies{59]. These properties were comparable
to that of Ticonderoga single graphite crystals and
highiy oriented pyrolytic graphite[lO]. Lately, kish
graphite crystals have been investigated as the host
material for graphite intercalation compounds[ 1l-
131. Regardless of these achievements, very little is
known about the formation process of kish graphite.
Because of limited high-quality natural graphite re-
sources and associated en~fironmenta1 concerns, the
synthesis of graphite as kish graphite or a similar
process has been proposed[l4-161 with the need for
improved understanding of the mechanism of kish
graphite formation.
Graphite, formed as the primary or eutectic phase
in commercial cast irons, has been extensively stud-
ied by cast iron metallurgists. It has been universally
accepted that the nucleation of primary graphite in
cast irons is a heterogeneous nucleation event in-
volving a disc-shaped nucleus (due to its highly
anisotropic structure) formed on a fiat substrate
or nucleant[ 17,181. Experimental data has demon-
strated that heterogeneous nucleation of graphite
occurs primarily by oxides, particularly silicates, in
a process complicated by difficulties associated with
ued growth may proceed via a two-dimensional nu-
cleation mechanism resulting in anisotropic growth
rates forming a flake-like shape which may be altered
by screw dislocations and/or rotational bounda-
ries[20,21). The instability of the faceted graphite
growth interface has been attributed to the effects
of undercooling and impu~ty elements[l7,22].
Kish graphite formed as a byproduct of iron smelt-
ing or similar processes, in which molten iron cools
relatively slowly and graphite accumulates on the
surface of the iron, has not been studied in detail.
This may be because the graphite crystals were con-
sidered too impure and imperfect to be of much
interest[5]. Recently, a number of theories have
been proposed to describe the formation of kish
graphitei23.241. Volume agglomeration refers to the
precipitation of kish graphite from the carbon sat-
urated melt, its growth and agglomeration within the
melt, and its subsequent flotation to the melt surface.
Surface agglomeration is based on the agglomeration
of microflakes of kish graphite on the surface of the
melt. It has also been proposed that kish graphite
may form directly on the melt surface[25,26]. These
theories. however, have not been supported by ex-
tensive experimental evidence.
The present studies were conducted to verify and
characterize the process of formation of kish graph-
ite and to evaluate factors involved (e.g., cooling
rate, atmosphere, melt composition, etc.). In addi-
tion, the morphology of industrially produced kish
graphite was examined, and the conditions involved
in its formation were studied experimentally.
2. EXPERIMENTAL
The morphology of kish graphite formed under
various conditions encountered in both steel-making
operations and in laboratory experiments (e.g., com-

547
548 S. LKJ and C. R. LOPER
position, cooling rate, atmosphere) was observed Table 1. Composion of raw materials and blast furnace
visually and with a scanning electronic micro- iron
scope (JEOL JSM-35C). All graphite samples were
c s1 M” s P Fe
mounted using conductive silver paint. Special at-
tention was paid to the morphological differences in Rg Imn 4.35 0.18 O.ocs 0.015 0.025 Rem
sample orientations and surfaces.
StllCOtJ 99.9 .- -- -- --
Two experimental procedures (referred to as open
Carbon 99.8 ._ .. .-
bath and closed bath) were designed to examine the
EIectrolytlc Iron -- .. .. -. -- 99.9
formation of kish graphite. The open bath procedure
Blast Furnace Iron * 0.4X 0.5 0.4 0.04 Rem
was adopted to reproduce the conditions of indus-
trial kish graphite formation in a 135 kg air melted
* The carbon content vaoes with llquldus temperature.
alumina crucible induction furnace. The melt was * Sulfur level prior to desullurlzatlon (0.02 after desulhrfxatton).

saturated with a high-purity carbon raiser at 1550°C.

Excess carbon raiser was removed, and the forma-
tion of kish graphite was observed as the melt was
cooled at about 900”Cih.
The closed bath procedure was designed to eval-
uate the effects of cooling rate, melt composition,
atmosphere, and so on on kish graphite formation.
This procedure required a smaller amount of melt
(about 4.5 kg) prepared in a graphite crucible (see
Fig. l), sealed so that different atmospheres (e.g.,
air, argon) could be introduced into the crucible.
The gas flow rate was controlled at about 0.5 m3/h
while the melt cooling rate was varied from lOOO”C/
h to 20”C/h. The melt was carbon saturated from
the crucible wall; otherwise the experimental tech-
nique for the closed bath procedure was similar to
that of the open bath procedure.
Melt charge materials used in these experiments
included select high-purity pig iron, pure silicon,
electrolytic iron, and a high-purity carbon raiser (see
Table 1). Most of the melts were prepared using pig
iron as the basic charge material with some addition
of silicon to yield about 0.4% Si. The sulfur content
was adjusted with iron sulfide (FeS). A few heats
were produced from a base of electrolytic iron.
Blast furnace kish graphite was collected from a
large hot metal transfer ladle and from surrounding
areas where it had settled from the atmosphere. The
temperature of the carbon-saturated molten iron
ranged from 1.500 to 1300°C. While in the transfer
car the melt cooling rate was estimated to be about
20”C/h, but during ladle transfer higher cooling rates
were achieved. The average composition of the car-
bon-saturated iron is presented in Table 1.
3. RESULTS
3.1 Industrial kish graphite
Generally, industrial kish graphite exhibits a plate-
like appearance, with the plate size ranging from
several centimeters across to fine mesh sizes; how-
ever, the coarse flakes predominate. The plate thick-
ness varies from 0.01 to 0.10 mm depending on the
size of the flake. The plates have a relatively flat
surface with irregularly rounded corners and exhibit
a dark, metallic luster. The shape of the kish graphite
is larger in size but not as thick as that found in most
natural flake graphite.
Industrial kish graphite was of two types. The first
is characterized by greater branching of a thin lay-
ered structure, appearing like several microflakes
joined to form a large flake (see Fig, 2). (This ap-
pearance may well have been the basis of the stated
agglomeration formation theory.) In subsequent dis-
cussion this type of kish graphite has been termed
“fast-cooled kish graphite.” The second type ex-
hibits a thicker plate structure with less branching
and smoother surfaces (see Fig. 3). This type has
been termed “slow-cooled kish graphite.”
The slow-cooled kish graphite was not as dense or
solid as expected and exhibited split edges (see Fig.
4) and a less well developed layered structure (de-
teriorated, degenerated) (see Fig. 5). Both the slow-
and fast-cooled types of kish graphite developed with
varying degrees of foliated dendritic structure. The
foliated dendrite is a particular case of a layered
dendrite in which some of the growth layers have
developed laterally to various degrees depending on
the availability of supersaturated carbon.

3.2 Kish graphite from open bath melts

Fig. 1. Schematic diagram illustrating the apparatus for the
closed bath kish graphite growth experiments.
Kish graphite produced in open bath melts is il-
lustrated in Fig. 6. The layered, or foliated, dendritic
structure is apparent in the edge view where the split,
but still interconnected, layers are evident. The
platelets lying on top of each other are approxi-
mately parallel, displaying well-defined hexagonal
corners and growth steps (these were not observed
in the industrial kish graphite).
 The formation of kish graphite 549

Fig. 2. (a) Fast-cooled kish graphite collected from a steel- Fig. 3. (a) A slow-cooled industrial kish graphite plate.
making operation. Scanning electron microscopy (SEM) SEM 60 x (b) Edge view of the kish graphite plate shown
60x. (b) Edge view of the kish graphite plate shown in in (a). SEM 60x.
(a). SEM 60 x

A difference was observed between the appear- graphite exhibits evidence of a more ideal crystal
ance of the kish graphite surface formed in contact structure.
with the melt and that formed in contact with air A large film of graphite was formed at slow cooling
(see Fig. 7). The surface formed in contact with air rates, less than 200”Cih (see Fig. 9). Both the top
was smoother and cleaner, attributed to not being and bottom surfaces exhibit features characteristic
in contact with the melt after the initial stages of its of single crystals rather than of a foliated dendritic
growth. The foliated dendritic growth of this plate structure.
resulted from the separation of the upper surface
from the melt during its edgewise growth, causing a
large increase in the volume of the kish flake. This
separation also resulted in some layers appearing to
have been bent. The lower surface (in contact with
the melt) displayed a rougher surface containing
growth steps, pits, and entrapped melt beads.

3.3 Graphite from closed bath melts

(argon atmosphere)
Primary graphite was observed to precipitate
within the bulk of the melt rather than on the melt
surface when held under an argon atmosphere and
cooled at rates in excess of 50OWh. Graphite crys-
tals grown within the melt were examined in the
fracture surface of a solidified melt block (see Fig.
Fig. 4. Edge view of slow-cooled kish graphite exhibiting
8). The graphite shows characteristic hexagonal split edges. The large, irregularly shaped particles are en-
growth features, a tubular appearance, and appears trapped slag while the small, round particles are iron. SEM
thicker than does kish graphite. Furthermore, the 1200x.
550 S. LIU and C. R. LOPER

Fig. 5. Slow-cooled kish graphite flake which had been

cleaved to reveal the foliated dendritic structure. SEM
12x.

The formation of graphite crystals was studied at

intermediate cooling rates (180,230,280, and 38o”C/
h) to evaluate the transition in morphology. In all
cases the top surface remained smooth but the bot-
tom (melt) surface was altered by the cooling rate.

Fig. 7. (a) Upper (air) side of laboratory-grown (open

bath) kish graphite showing a relatively smooth surface.
SEM 60 x (b) Lower (melt) side of the kish graphite crys-
tal shown in (a). Note the rough surface appearance and
the entrapment of iron beads. SEM 60 x

At slow cooling rates a pyramidal growth mode was

observed (see Fig. 10). With an increase in the cool-
ing rate, some of the plates were noted to tilt at a
small angle (see Fig. 11). This tilting was attributed
to a degradation of pyramidal growth. At still higher
cooling rates (see Fig. 12), substantial branching was
03 i

Fig. 6. (a) Kish graphite grown in an open bath melt show-

ing the foliated dendritic growth structure, and an agglom-
erate-like morphology with a hexagonal dendritic growth
front. SEM 60 x (b) Edge view of the kish graphite shown
in (a) exhibiting the split and interconnected leaves within
this plate. SEM 60 x
Fig. 8. Fracture surface of a sample of iron showing the
cleavage of graphite crystals which had grown in the melt.
SEM6Ox.
 The formation of kish graphite
Fig. 9. (a) The top surface of a graphite film developed at
slow cooling rates. SEM 60x (b) The bottom surface of
the graphite film shown in (a). SEM 60X.
noted at the tips of these platelets (with branching
occurring dendritically from {lOTO}crystal faces).
On the other hand, reducing the cooling rate to
about 5O”Cih resulted in the formation of a large
single crystal of graphite on the melt surface (see
Fig. 13). This crystal is larger, thicker, denser, and
Fig. 10. Kish graphite formed in the closed bath experi-
ments using an argon atmosphere. The bottom (melt) sur-
face is shown here, grown at a cooling rate of 23OWh.
The smooth surface has broken down into a pyramidal
growth mode[ 171. SEM 60 x
551
Fig. 11. The bottom surface of a thin crystal film grown
at 280”C/h exhibiting the tilting of platelets due to growth
interference. SEM 60 X
appears more c~stalIog~phicaliy perfect than in-
dustrial kish graphite.
3.4 Graphite from closed bath melts
(air atmosphere)
This set of experiments was conducted similarly
to those just described, except that the melts were
produced in air. At high cooling rates (9OOWh, the
kish exhibited a layered structure almost identical to
that obtained in the open bath experiments (see Fig.
14). A 50% increase in the air flow rate (0.75 m’i
h) resulted in a smaller flakes having a more open,
foliated structure, due to oxidation (see Fig. 15). In
addition, it is likely that this change could in part be
attributed to increased local cooling rates due to the
greater air flow rate. A more detailed view of kish
graphite formed under these circumstances is pre-
sented in Fig. 16, where the “etching” of the graphite
by oxygen is evident in the kish graphite structure.
At lower cooling rates, less than 20O”C/h, the for-
mation of graphite on the melt surface was com-
Fig. 12. The bottom surface of a thin crystal film grown
at 380”Cih showing a greater amount of branching. SEM
60x.
 S. LIU and C R. LOPER
Fig. 13a. Atmoshpere surface of a smooth crystal sheet
grown at low cooling rates, 50Wh. SEM 60 x .
pletely prevented as oxidation consumed carbon at
the melt surface.
4. DISCUSSION
Graphite as the primary phase in hypereutectic
melts of Fe-C alloys will precipitate when the melt
is cooled below the liquidus temperature. However,
it is evident from these experiments that primary
graphite can be formed by different modes under
different growth conditions. Kish graphite is char-
acterized by its foliated dendritic structure (to var-
ious degrees) and by the fact that this structure is
formed on the surface of the melt when exposed to
air. The evidence of contact with the melt on one
surface of the crystal but not the other and the round
corners exhibited in industrial kish graphite which
may be attributed to their impingement with slag
(oxides, etc.) during surface growth are consistent
with a surface formation mechanism. In contrast to
the formation of graphite crystals within the melt,
this is referred to as a surface formation mode.
Graphite as a faceted phase exhibits growth insta-
bilities both as a proeutectic phase and during solid-
Fig. 13b. Bottom surface of the crystal sheet shown in Fig.
13a showing steps on this surface. SEM 60 x
Fig. 13~. Edge view of the crystal shown in Figs. 13a and
13b showing a thicker, denser fracture surface than ob-
served in kish graphite. SEM 60 x .
ification of the eutectic and has thus attracted con-
siderable attention[l7]. The foliated dendritic
structure, however, is unique in that the degradation
of the growth front occurs not only in the a direction
of the graphite crystal but also in the c direction.
Branching typically occurs in the basal plane but also
develops with overlapping split layers approximately
parallel to the basal plane. This agglomerated char-
acter is demonstrated more clearly by the sketch
shown in Fig. 17[27]. This sketch presents the ap-
pearance of individua1 graphite particles which have
been agglomerated, although they have in fact de-
veloped as a single complex dendrite. It was ob-
served that the foliated dendritic structure is pro-
moted by higher cooling rates and by the exposure
of the melt surface to air.
When the effect of air was excluded by introducing
an argon atmosphere, graphite crystal films were
observed to form on the melt surface (also referred
to as surface formation mode) promoted by slow
cooling. While higher cooling rates suppressed the
surface formation mode, the primary graphite phase
was precipitated on crucible wails or within the body
Fig. 14. The foliated dendritic structure of kish graphite
grown in the closed bath technique with an air atmosphere.
SEM6Ox.
 The formation of kish graphite
Fig. 15. Kish graphite formed in the closed bath experi-
ments with higher air flow rates showing smaller flakes and
an open, foliated structure. SEM 60 x .
of the melt in a manner which is similar to that of
primary graphite formation in commercial cast irons.
It has been demonstrated that cooling rate is an in-
fluential factor in controlling the growth mode, at-
tributed to the effect of diffusion on the solute
redistribution for maintaining the interface stability
and the effect on the undercooling required for in-
itiating bulk graphite nucleation within the melt. In-
creased undercooling associated with faster cooling
rates results in the transition from surface growth to
volume growth. Fioatation, then, may or may not
occur depending on local conditions. In the gener-
ation of kish in commercial steel-making operations,
the cooling rates are typically slow, favoring the sur-
face formation mode.
The presence of air at the melt surface is also a
significant factor. The relative ease of graphite for-
mation associated with the exposure of the melt sur-
face to air may be attributed to the formation of
oxides on the melt surface serving as nuclei for
graphite crystals. Two observations support this pro-
posal: (a) that large quantities of kish graphite
formed at temperatures below 1400°C (below which
Fig. 16. Kish graphite grown in the air atmosphere showing
grooves on the surface due to the preferential oxidation.
SEM 480 x
s53
Fig. 17. Sketches illustrating a foliated dendritic struc-
ture[27]. (a) Top view of the dendritic structure. (b) Section
view, showing the same feature as shown in Fig. 6.
SiO, is stable), and (b) that much less kish graphite
was observed to form in a silicon-free melt (electro-
lytic iron charge). The foliated dendritic structure
was formed only when the graphite was grown on
the surface of the melt; graphite developed within
the melt exhibited a thicker, plate-like structure. It
is apparent that the presence of oxygen from the air
was a major factor assisting the growth of kish graph-
ite.
The effect of oxygen may be due to defects de-
veloped along the growth front. At the temperatures
involved, oxygen will attack the graphite crystal on
both basal and prism planes, resulting in the char-
acteristic claw defects shown in Fig. 18[1]. The claw
defects occur when foreign atoms (oxygen being the
principal example) are bonded at edge defects and/
or screw dislocations in the carbon hexagon net-
work, and when these broken bonds lead to holes
or reentrant ruptures in the hexagonal network of
carbon atoms. To accommodate the disparity in size
of these foreign atoms, the network must deviate
from being planar. The crystallographic defects
which result cause the carbon network to bulge or
buckle and are believed to be the cause of the fol-
iated dendritic structure. Evidence of oxygen attack
on the graphite surface is apparent in Fig. 16.
Three forms of foliated dendrites are depicted in
Fig. 19. Edge splitting is often observed in kish
Fig. 18. Out of plane buckling of a carbon hexagonal nct-
work at a claw defect due to repulsion between corner
atoms (marked with a dot). (After A R. Uhbeiohde et
Ui.[Il).
554 S. LIU and C. R. LOPER
a b c the graphite morphology by attacking the growth
Fig. 19. Model of foliated dendritic formation showing typ-
ical observations of foliated dendrites. Exposure to air dur-
ing growth increased from a to c. (a) Edge splitting. (b)
Plane branching. (c) Corner flipping.
graphite formed with a slight exposure to air, while
plane branching and corner flipping are more often
observed at greater exposure of the developing kish
to air. This occurrence is attributed to the effect of
air (oxygen) on the formation of claw defects[l].
Edge defects may be formed as a result of a single
(or a few) claw defect, whereas plane branching and
corner bending may be the result of multiple or con-
centrated claw defects. This occurance is also con-
sidered to be associated with the effect of instability
at the growth front caused by higher cooling rates
due to higher air flow rates, which is more likely for
the case of corner flipping.
Commercial kish graphite was of two types, char-
acterized according to the conditions under which it
formed. The thinner and more highly branched
graphite resulted from fast cooling and direct ex-
posure to air. These conditions would be expected
during the surface cleaning of blast furnace hot metal
or during melt transfer. The thicker and more plate-
like graphite would have formed during slower cool-
ing and less contact with air. These conditions would
be enhanced under a slag and/or kish layer in the
transfer car.
It is well known that the solidification of cast irons
is affected significantly by the sulfur content. At
lower levels, increased sulfur reduces chill formation
as a result of increased nucleation. On the other
hand, high sulfur contents restrict eutectic cell
growth and lead to chill formation[28-301. Further-
more, sulfur retards the dissolution of carbon in the
melt[31]. The role of sulfur was noted in the present
study, where it was observed that in the range of
0.10 to 0.40% sulfur surface formation of graphite
was enhanced with increasing sulfur content. This
effect may be because sulfur is highly surface active,
reducing the surface tension of liquid iron[32,33],
and because of the interfacial energy between the
liquid iron and graphite[34], which favors the for-
mation of graphite on the surface of the melt.
The interlayer spacing of the industrial kish graph-
ite was investigated using an x-ray diffractometer.
The resultant data appeared to be identical or very
close to that of the ideal graphite structure, about
3.3550 A. For more detail, see [35].
5. SUMMARY
Kish graphite as a proeutectic phase in hypereu-
tectic iron has been demonstrated to form on the
surface of the melt and to grow in a foliated dendritic
manner. The surface growth of graphite can be sup-
pressed in favor of a growth mode within the melt
by increasing the cooling rate and avoiding the pres-
ence of oxygen at the melt surface. It is apparent
that oxygen is important not only in that it affects
front of the kish graphite crystal, but that it provides
a means to nucleate graphite on the melt surface
(through the oxidation of silicon). Increased cooling
rates and exposure of the melt to oxygen favor the
formation of foliated dendritic structures. On the
other hand, slow cooling and avoidance of oxygen
result in the formation of a graphite sheet over the
melt surface. In addition, however sulfur contents
promote the surface formation mode.
Acknowledgment-The authors express their gratitude to
the Superior Graphite Company for the partial financial
support of this research program.
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