Article No : n05_n02
Carbon, 3. Graphite
WILHELM FROHS, SGL Carbon GmbH, Meitingen, Germany
FERDINAND VON STURM, former SIGRI GmbH, Meitingen, Germany
ERHARD WEGE, former SIGRI GmbH, Meitingen, Germany
GABRIELE NUTSCH, former Technische Universit€at Ilmenau, Germany
WERNER HANDL, H.C. Carbon GmbH, Germany
1. Graphite Single Crystal . . . . . . . . . . . . . . . . . 721
2. Natural Graphite . . . . . . . . . . . . . . . . . . . . . 724
As early as 800 B.C. the Celts extracted graphite
and produced fire-proof ceramics, as proven by
finding places near Passau (Germany) and Cesky
Krumlov (Czech Republic).
Graphite has been used for the production
of refractory crucibles since at least the 15th
century, and for pencils since about 1550. It was
frequently mixed with optically similar minerals
such as galena, molybdenite, and even lead. As
chemical knowledge was very limited in those
days, graphite was called plumbago, meaning
‘‘which acts (writes) like lead’’. The name ‘‘pen-
cil lead’’ originates from this mistake. It was not
until 1779 when the German – Swedish pharma-
cist and chemist C. W. SCHEELE (1742 – 1786)
analyzed plumbago and proved that it was a form
of carbon, not of lead.
ABRAHAM GOTTLOB WERNER (1750 – 1817)
named graphite after the Greek word ‘‘g r a j
e i n’’ (to write). Since then, the history of
graphite has been closely associated with the
development of electricity. Sir HUMPHRY DAVY,
in 1800, was probably the first to use carbon
electrodes for his studies on the electric arc. The
increasing demand for electric arc light carbons
since about 1870 gave rise to several processes
for the manufacture of artificial carbon CARRÉ,
BRUSH, SIEMENS). At the beginning of the 20th
century, important electrolytic and electrothermic
processes using carbon or graphite electrodes
became available, e.g., aluminum electrolysis
(HALL, H
E ROULT), alkali – chlorine electrolysis
(CASTNER et al.), calcium carbide (WILLSON),
electric steel (HÉROULT), and silicon carbide

2012 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
DOI: 10.1002/14356007.n05_n02
Article with Color Figures
3. Synthetic Graphite . . . . . . . . . . . . . . . . . . . . 725
References . . . . . . . . . . . . . . . . . . . . . . . . . . . 729
(ACHESON). Progress has been made in customizing
the carbon and graphite grades and increasing
their usefulness for new and more rigorous
applications.
1. Graphite Single Crystal
The ideal crystal lattice of hexagonal graphite is
shown in Figure 1. As consequence of the sp2
hybridization each carbon atom has three nearest
neighbors within the same layer plane. The dis-
tancebetweenin-planecarbonatomsis0.1421 nm
in graphite (sp2 hybridization), compared to
0.1544 nmindiamond (sp3 hybridization)[1]. The
in-plane bonding energy of graphite is
430 kJ/
mol, thus 80 kJ/mol higher than that of diamond,
and one of the highest bonding energies known.
The bonding angle between the carbon atoms is
120 . The overlapping p-orbitals perpendicular to
the C-atom planes are filled with delocalized elec-
trons forming the weak p-bonds with a distance of
0.354 nm between the planes. The bonding energy
between the basal planes (graphene layers) is in the
range of van der Waals forces only.
This layer structure results in an extreme
anisotropy of the physical properties of graphite
(Table 1) [2–6].
Remarkable is the negative coefficient of
thermal expansion (CTE) within the plane.
Thus, below 670 K graphite contracts in a di-
rection whereas it expands in c direction. Paral-
lel to the basic planes graphite is a metallic
conductor, whose electrical resistivity increases
722 Carbon, 3. Graphite Vol. 6

Figure 1. A. Lattice of the cubic diamond and the hexagonal graphite crystal; B. sp3 hybridization in the diamond lattice; C. sp2
hybridization in the graphite lattice

with temperature. Perpendicular to the planes
graphite behaves like a semiconductor. The
thermal conductivity decreases with tempera-
ture. At room temperature the in-plane thermal
conductivity is higher then that of copper. The
high Young’s modulus of 1060 GPa within the
plane should allow a theoretical strength of
100 000 MPa. This unique potential in mechan-
ical properties is exploited in carbon fibers
which are used to reinforce different matrices
(see ! Fibers, 15. Carbon Fibers).
The basic planes can easily be shifted against
each other. This gives graphite its lubrication
properties which are widely used in industrial
and private applications (locks). Two modifica-
tions of graphite are known. The energetically
preferred stacking sequence is ABAB. (hexago-
nal modification) . Formation of the rhombohe-
dral modification ABCABC. can be achieved
to a certain degree by strong mechanical
impact and shearing during milling. In some
cases natural graphite can contain 30% of the

Table 1. Properties of diamond and graphite (single crystals) and synthetic graphite at various temperatures

Diamond Graphite Synthetic graphite

c- a- with across with across with across with across

direction direction grain grain grain grain grain grain grain grain
room room 1000 K 1500 K 2000 K
temperature temperature

Density, g/cm3 3.515 2.266 1.80 1.80 1.79 1.79

Coefficient of 0.8 28.3
1.5 0.1 1.5 1 2.4 1.5 2.9 1.80 3.20
thermal expansion
(15–150  C), 10
6 K
1
Thermal conductivity 20 0.04–0.06 10 to 15 350 180 150 75 110 55 85.00 45.00
[43], W cm
1 K
1
Electrical resistivity, 1020 1 50  3.5  7.0  3.2  6.4  3.3  6.6  4.0  8.0 
W cm 10
6 10
4 10
4 10
4 10
4 10
4 10
4 10
4 10
4
Magnetic susceptibility
21
0.3
[44], 10
6 cm3 g
Elastic modulus [43], 1000 36 1060 20 6 22 6.5 24 7.5 26.0 8.0
GPa
Mohs hardness [45] 10 9 0.5
Vol. 6 Carbon, 3. Graphite 723

rhombohedral modification. The rhombohedral

modification can be re-transferred into the hex-
agonal modification by annealing. This change in
modification has not yet found any industrial
application.
Neither natural graphite nor artificially pro-
duced synthetic graphitic carbons are perfect in
structure. Lattice defects in planes, defect in the
stacking sequence and bending of planes lead to
deviations from the ideal crystal lattice. The most
frequently applied structure analysis for carbon
materials is X-ray diffraction. Only materials
which show in their X-ray spectra the modulation
of the three-dimensional (112)-interference
should be named graphitic carbon. It has become
common to use the easily measurable mean
interlayer spacing c/2 instead of the three-dimen-
sional (112)-interference. With the limits for
ideal graphite c/2 ¼ 0.3354 (100%) and for non-
graphitic carbon c/2 ¼ 0.344 nm the degree of
graphitization can be calculated [7, 8]. Materials
within these limits should be termed graphitic
carbons independent of the degree of graphitiza-
tion. All other carbons are nongraphitic carbons.
In nongraphitic carbons the stacking of the gra- Figure 2. A. High resolution transmission electron micros-
phene layers is totally random (turbostratic) [9]. copy (HRTEM) bright-field image of graphitized coal tar
The above applied terms follow the IUPAC pitch coke; B. Electron diffraction pattern of a highly oriented
pyrolytic graphite (HOPG)
Nomenclature which should be consequently
applied [10].
Along with the disorder goes the width of the treme structural order in this synthetic graphite
X-ray diffraction lines. Whereas the mean crys- (Fig. 2) [12].
tallite size in c direction Lc (stacking height) can In 2003 scientists of the University of Augs-
be calculated from the width of the (002) inter- burg were able to visualize for the first time the
ference, the width of the (100) or (110) interfer- completely hexagonal carbon rings in a HOPG
ence can be taken to calculate the mean crystallite material by atomic force microscopy (AFM)
size in a direction La [7–9, 11]. (Fig. 3.) [13].
It is evident that the material properties of
graphitic and nongraphitic carbon materials
strongly alter with the degree of structural disor-
der. This broad variety in the crystallographic
structure opens manifold areas of application
which are multiplied by the morphological plu-
rality of different forms of carbon.
Closest to the ideal graphite lattice are natural
graphites and artificially produced highly orient-
ed pyrolytic graphite (HOPG). The parallel ar-
rangement of graphene layers can be visualized
by High Resolution Transmission Electron Mi-
croscopy (HRTEM). Figure 2A shows a HRTEM
color
bright-field image of a graphitized coke derived fig
from coal tar pitch [12]. The high symmetry in Figure 3. AFM image of graphite. The hexagonal carbon
the electron diffraction pattern of a highly or- rings are visible and the complete lattice surface is imaged
dered pyrolytic graphite (HOPG) shows the ex- [13]
 724 Carbon, 3. Graphite Vol. 6

graphite deposits (see Fig. 4) develop synerge-

color
fig
Figure 4. SEM picture of a flake natural graphite
2. Natural Graphite
Occurrence and Properties. Numerous
hypotheses on the genesis of natural graphite
existed, but today most of them are outdated. It
is currently supposed that organic matter was the
origin of most natural graphites with the probable
exception of the Sri Lanka (vein type) deposits.
The origin of vein graphite deposits is still not
certain. In regionally metamorphosed (granulit-
ic, charnockitic) rocks, graphite is thought to
form epigenetically from carbon-rich hydrother-
mal or pneumatolytic solutions as interlocking
aggregates of coarse graphite crystals in veins
containing 75–100% carbon. Disseminated flake
tically from carbonaceous material in sedimen-
tary rocks that have been subjected to garnet
grade or higher regional metamorphism. Con-
current large-scale folding of the metasedimen-
tary sequences is common and fold limbs often
host deposits. Deposits are usually stratabound
and consist of individual beds or lenses in
gneisses, schists, and marbles that are richer in
graphite than associated beds [14]. Single flakes
may range from 0.5 to 25 mm. The decomposi-
tion of compounds, e.g., carbide, carbonates,
carbonyl, and cyano compounds, is less impor-
tant for the genesis of graphite deposits.
Natural graphite is divided into vein type,
flake type, and microcrystalline type, often in-
correctly called amorphous graphite. Crystallin-
ity, refractoriness, and other properties of natural
graphite from different deposits may vary sub-
stantially because of differences in the precursor
materials and the conditions of metamorphosis.
In general, natural graphite is a ductile soft
mineral which easily cleaves parallel to the basic
layer. The flaky and vein grades show a typical
metallic luster; the microcrystalline ‘‘amor-
phous’’ grades have a duller black appearance.
Table 2 shows a classification [15, 16]. The host
rocks consist of quartz, mica, gneiss, feldspars
associated with pegmatite aplite, granite magne-
tite, and calcite.

Table 2. Classification of natural graphite

Average crystallite
Deposit Carbon content, % diameter, mm Origin

Macrocrystalline Brazil < 60 < 0.1 syngenetic cata- and mesozonal

flakes Germany (Kropfm€uhl) metamorphism of sapropelites
China
Canada
Malagasy Republic
Norway
India
Zimbabwe
Russia
Mozambique
Tanzania
Macrocrystalline epigenetic, probably
lumps Sri Lanka < 100 < 0.01 pneumatolytic

Mesocrystalline Austria 30–90 < 0.001 syngenetic metamorphism

Czech Republic of sapropelites
Microcrystalline China 30–90 < 0.001 syngenetic, epizonal
Korea metamorphism of coals
Russia
Mexico Austria
Vol. 6
Figure 5. Classification of different forms of carbon according IUPAC nomenclature. Approved IUPAC terms are printed in
italics [10]
3. Synthetic Graphite
According to IUPAC nomenclature [10] the term
‘‘synthetic graphite’’ should be used instead of
‘‘artificial graphite’’. The IUPAC describes
‘‘synthetic graphite’’ as follows: Synthetic
graphite is a material consisting of graphitic
carbon which has been obtained by graphitiza-
tion of non-graphitic carbon, by chemical vapor
deposition (CVD) from hydrocarbons at a tem-
perature above 2500 K, by decomposition of
thermally unstable carbides or by crystallizing
from metal melts supersaturated with carbon.
Figure 5 provides an overview on the recom-
mended IUPAC nomenclature, together with
examples for visualization.
In principal all carbon containing materials
are suited as raw materials for the production of
nongraphitic or graphitic solid carbon materials
as long as sufficient carbon remains after the first
thermal degradation, the so-called pyrolysis.
Whether the product of pyrolysis is a nongraphi-
tizable or graphitizable carbon depends in gen-
eral on the mobility of the molecules during
pyrolysis. This means the capability to arrange
the necessary microstructural pre-order for the
subsequent solid-state healing process under
Carbon, 3. Graphite 725
graphitization conditions (> 2500 K). The prin-
ciple is illustrated in Figure 6.
Carbon containing materials passing through
a liquid or gaseous form during pyrolysis give
graphitizable carbons. Materials which remain
solid under pyrolysis conditions maintain their
microstructural arrangement under graphitiza-
tion treatment. Transitions between solid-, liq-
uid-, and gas-phase pyrolysis do exist and can
result in partially graphitic regions after graph-
itization treatment.
Examples for a solid-phase pyrolysis are chars
and glass-like carbon. Due to the structural dis-
order and impossibility of molecular arrange-
ment during pyrolysis these materials do not
graphitize.
Another industrially important example are
carbon fibers from polyacrylonitrile (PAN) pre-
cursors. Polyacrylonitrile precursor fibers are
stabilized in air. The stabilized fibers do not melt
during subsequent pyrolysis. Further treatment at
graphitization temperatures (high-modulus car-
bon fibers) does not result in a graphitic carbon
fiber.
In case of the liquid-phase pyrolysis the for-
mation of optically anisotropic spherulites (car-
bonaceous mesophase) is essential for the later
 726 Carbon, 3. Graphite
Figure 6. Gaseous, liquid, and solid pyrolysis and their products
structural order of the final graphitic carbon.
Figure 7 shows an optical micrograph of meso-
phase spherulites. The changing color under
polarized light shows the anisotropy of the spher-
ulites [17]. BROOKS and TAYLOR were the first to
discover the formation of these spherules during
the pyrolysis of petroleum pitch and coal-tar
pitch as well as during the softening of coal
[18]. During heat treatment, pitch gradually
forms an isotropic melt and develops small (few
microns in size) spherulites with increasing tem-
perature. The diameter of the spherulites in-
creases with temperature, to a lesser extend with
the residence time. The spherules are nematic
liquid crystals composed of large parallel stacked
aromatic molecules.
color
fig
Figure 7. Optical micrograph of carbonaceous mesophase
from heated anthracene oil [17]
Vol. 6
After the formation of a sufficient number of
spherulites, so-called secondary QI’s, they touch
each other and coalesce under the formation of
bigger spherules. With ongoing growth the
spherulitic mesophase is transferred into the bulk
mesophase, viscosity increases and the carbona-
ceous material becomes solid (Fig. 8). Formation
and structure of the mesophase are essentially
governed by three limiting conditions:
1. The shape of the polyaromatic molecules
must favor the formation of liquid crystals
(i.e., highly aromatic, few heteroatoms and
few aliphatic side chains)
2. The fluidity of the system
3. The reaction or condensation rate must be
smaller than the ordering rate
Other factors influencing the structure of the
mesophase – which eminently affect structure
and properties of the coke or of the synthetic
graphite after graphitization, respectively – are
the amount of nonmelting constituents and/or the
amount and size of impurities [19, 20]. Impuri-
ties are the so-called primary QI’s, which are
solid particles like ash, soot, refractory particles,
cenospheres (porous to hollow carbonaceous
sphere-like particles), and others, which are not
soluble in quinoline. These particles tend to settle
on the surface of the mesophase spherulites and
hinder the coalescence of the mesophase (Fig. 8)
[21–23].
Vol. 6
Figure 8. Carbonaceous mesophase structure and mechanism of growth by coalescence of spherulites [21–23]
The chemistry of the pyrolytic conversion of
hydrocarbons to solid carbon involves numerous
chemical reactions. Generalized schemes have
been developed by studying simpler models [24,
25]. The major reactions involved are:
. Bond cleavage and formation of free radicals
. Molecular rearrangement
. Thermal polymerization/polycondensation
. Aromatization
. Elimination of aliphatic side-chains and
dehydrogenation
A generalized scheme is shown in Figure 9
with structural models of the chemical reaction
products. The pyrolysis is accompanied by the
release of volatile reaction products. This release
of volatiles induces the development of pores.
Shrinkage reactions during the subsequent solid
state degradation contribute to the porosity with
cracks and slit pores. The pore sizes reach from
micropores (< 2 nm) over mesopores (2–
50 nm) to macropores (> 50 nm). The highest
Carbon, 3. Graphite 727
porosity is achieved at heat treatment tempera-
tures of around 870 K. Micropores were postu-
lated in the 1950s to buffer the thermal expansion
and thus being responsible for the low thermal
expansion behavior of polygranular carbon ma-
terials [26]. This postulate was experimentally
proven later [27].
After pyrolysis further heat treatment to above
2500 K is necessary to obtain synthetic graphite.
Industrially most important is the heat treatment
of graphitizable carbon compounds above
2500 K by means of electrically heated furnaces
known as Acheson [28] and Castner furnaces
[29] (see ! Carbon, 4. Industrial Carbons). For
granular forms of carbon or powders electrically
heated shaft furnaces or fluidized-bed reactors
are used [26, 27, 30]. The thermal graphitization
process can be accelerated by catalysts. Although
catalytic graphitization had already been studied
by ACHESON it remained of minor importance.
Other methods for the production of synthetic
graphite are vapor deposition of volatile carbon
compounds or the condensation of carbon vapor
728 Carbon, 3. Graphite Vol. 6

Figure 9. Reaction scheme for carbonization and graphitization

(pyrolytic graphite) [31]. The crystallization of
carbon melts at pressures above 15 MPa [32], the
precipitation from oversaturated metal melts
(Kish graphite) [33], the decomposition of car-
bide crystals and nitrogenation of calcium car-
bide [34], and the electrolytic decomposition of
carbonate melts [35] have been applied.
Crucial during the heat treatment to graphiti-
zation temperatures is the release of the incorpo-
rated heteroatoms sulfur and nitrogen. The re-
lease of nitrogen starts at around 1670 K fol-
lowed by the release of sulfur at around 1870 K
[36, 37]. Both volatiles lead to an irreversible
expansion with the potential to destroy the poly-
granular body. This behavior is known as puffing
[38, 39].
During further heat treatment to graphitiza-
tion temperatures above 2500 K lattice defects

Figure 10. Structural development of a graphitizable carbon during heat treatment up to graphitization temperatures [42]
Vol. 6
are eliminated, combined with the growth of the
graphene layers in a and c direction (La ¼ ap-
parent crystallite size, Lc ¼ mean stacking
height) and the narrowing of the interlayer dis-
tance towards the value of the ideal graphite
crystal. The development of the graphite crystal
under graphitization temperatures was investi-
gated in situ by X-ray diffraction up to 2870 K
[40]. This investigation showed that prior to the
interlayer distance shrinkage defects in the layers
must be healed enabling the necessary parallel
arrangement.
Above temperatures of about 2770 K the
lattice order can be improved by mechanical
impact like high pressure or tension [41]. The
most illustrative description of the graphite lat-
tice formation during high temperature treatment
was given by MARSH in 1982 (Fig. 10) [42].
Gas-phase pyrolysis is characterized by ther-
mal cracking of gaseous hydrocarbon com-
pounds and deposition of carbon on a substrate.
Traditional industrial examples are carbon black
and pyrolytic carbon. But also vapor-grown car-
bon fibers (VGCF) and carbon nanoparticles
(fullerenes, nanotubes, nanocaps) are generated
by gas-phase pyrolysis.
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Further Reading
P. Delhaes (ed.): Graphite and Precursors, vol. 1, Gordon
and Breach, Amsterdam 2001.
M. Inagaki (ed.): New Carbons, 1st ed., Elsevier, Amsterdam
2000.
H. O. Pierson: Handbook of Carbon, Graphite, Diamond and
Fullerenes, Noyes Publ., Park Ridge, NJ 1993.