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DOI: 10.1002/adma.200600715
Synthesis of WC Nanotubes**
By Swati Vilas Pol, Vilas Ganpat Pol, and Aharon Gedanken*
Over the last 15 years, nanotubes have become the symbol
of the new and fast-developing research area of nanotechnol-
ogy. The particular physical and chemical properties of quasi
one- and two-dimensional solids promise new inventions,
innovative products, and fresh contributions to human knowl-
edge. In addition to the size effects, the geometry of low-di-
mensional materials is an important conceptual novelty in ma-
terials research.[1] The first reports on carbon nanotubes in
1991 by Iijima[2] and on inorganic (WS2) nanotubes by Tenne
et al.[3] in 1992 have been followed by intense experimental
and theoretical research on hollow cylindrical structures. A
list of inorganic nanotubes, fabricated by different synthetic
routes, has been compiled by Rao et al.[4] This present com-
munication is confined to inorganic tungsten carbide nano-
tubes, which have not yet been reported in the literature, to
the best of our knowledge.
Tungsten carbide in particular might find potential applica-
tions owing to its unusual properties, such as high melting
point, superior hardness, low friction coefficient, high oxida-
tion resistance, and superior electrical conductivity.[5] Arie
et al. prepared a nanometer-sized WC needle on a tungsten
tip using catalytic deposition.[6] WC was shown to have a plati-
num-like behavior for the chemisorption of hydrogen and
oxygen, and its applicability as an alternative electrocatalyst
of Pt was demonstrated. The early studies showed that this
combination of an early transition metal with carbon yielded
materials with attractive catalytic activity, stability, selectivity,
and resistance to poisoning.[7] There are several routes to pre-
pare tungsten carbide, including the direct carburization of
tungsten powder, solid-state metathesis, reduction carburiza-
tion, mechanical milling, and polymeric precursor routes using
metal alkoxides.[8,9] WC production generally proceeds as a
two-step process. First, the oxide is reduced to high-purity
tungsten in a hydrogen atmosphere. The tungsten metal is
then mixed with the required amount of carbon and reacts at
a temperature of 1400–1600 °C to produce tungsten car-
bide.[10,11] The most important tungsten carbides are WC and
– Sample
[*] Prof. A. Gedanken, S. V. Pol, Dr. V. G. Pol
Department of Chemistry and Kanbar Laboratory for Nanomaterials
at the Bar-Ilan University Center for Advanced Materials and
Nanotechnology, Bar-Ilan University
Ramat-Gan 52900 (Israel)
E-mail: gedanken@mail.biu.ac.il
[**] V. G. Pol and S. V. Pol are thankful to Bar-Ilan University, Israel, for
financial assistance.
Adv. Mater. 2006, 18, 2023–2027 © 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
W2C. W2C is thermodynamically unstable at low tempera-
tures, while WC is stable, as confirmed by its electrochemical
stability in acidic solutions.[12]
Herein, we report, for the first time, on a solvent- and tem-
plate-free, competent, and straightforward approach for the
synthesis of inorganic WC nanotubes. The low-temperature
(900 °C) thermal decomposition of W(CO)6 in the presence of
Mg powder is carried out under its autogenic pressure in a
closed Swagelok cell to fabricate nanotubes of WC. The diam-
eter of the WC nanotubes ranges from 30 to 70 nm, and the
length varies from 1 to 10 lm. The thermal decomposition of
bare W(CO)6 yields a mixture of WO2, WC, W2C, and C, ex-
hibiting the growth tendency of any one of the products. The
replacement of Mg powder by Na yielded Na2WO4, which
was converted to H2WO4 after treatment in dilute HCl, keep-
ing its flakelike morphology. The suggested mechanism is sup-
ported by experimental data resulting from a series of control
reactions. This is, to our knowledge, the first report on the
preparation of nanotubes of WC.
The phase purity of the obtained samples was characterized
on a Bruker AXS D* Advance X-ray powder diffractometer
with Cu Ka radiation (k = 1.5418 Å). As shown in Figure 1a,
the diffraction patterns of the W–CO/Mg sample (the as-pre-
pared sample) can be indexed to face-centered cubic (fcc,
space group Fm-3m) MgO (marked with M), and matches
well with the PDF No. 45-946 (PDF: powder diffraction file).
In addition, the small diffraction peaks are assigned to WC,
and W2C (marked with *). The acid-treated W–CO/Mg sam-
ple confirms the removal of MgO impurities (Fig. 1b), and the
product can be indexed to that of the hexagonal phase (space
group P6m2) with lattice constants a = 2.90, c = 2.83 Å of WC
(peak intensities and positions are shown and confirmed from
PDF No. 51-939). The additional, small diffraction peaks are
obtained for hexagonal a-W2C (space group P3m1) (marked
with *), and the graphitic carbon peak appeared at 26.6°.
The diffraction patterns of the W–CO/Na sample (Table 1)
could be completely indexed to that of fcc (space group
Table 1. Reactant(s), reaction conditions, obtained morphology, and the
achieved products.
Reactant(s) Temperature/ Morphology Products
name atmosphere/time TEM
W– W(CO)6+Mg 900 °C/N2/3h tubes+particles WC+MgO
CO/Mg +W2C+C
W– W(CO)6+Na 900 °C/N2/3h flakes Na2WO4+WC
CO/Na +W2C+C
W–CO W(CO)6 900 °C/N2/3h wires+particles WO2
+WC+W2C+C
2023
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Figure 1. The powder XRD patterns of a) the W–CO/Mg sample and
b) acid-treated (30 % dilute HCl) W–CO/Mg sample [M = MgO, C = car-
bon, line pattern = WC, and * = W2C].
Fd-3m) Na2WO4 (peak intensities and positions are matched
with PDF No. 12-772). The Na ions are replaced during dilute
HCl treatment, resulting in the formation of a monoclinic
phase (space group P2/m) of hydrotungstite, H2WO4·H2O
(PDF No. 16-166). The catalytic growth in the presence of Na
resulted in the formation of filaments of Na2WO4 (see below,
Fig. 2b). The diameter of the filaments ranges between 100
and 200 nm, with a length of several micrometers. The Na
ions are found to be replaced during the dilute HCl treatment
a for the fcc lattice of the MgO. The nanotubes have a diameter
c area, which provides further evidence for the identification of
d the product as WC. It illustrates the perfect arrangement of
Figure 2. SEM images of a) acid-treated W–CO/Mg sample, b) the
W–CO/Na sample, and c) the W–CO sample. d) Bulk EDX spectrum of
the W–CO/Mg sample.
to form hydrotungstite acid, without a change in the morphol-
ogy of the filaments. The diffraction patterns of the W–CO
sample could be indexed to a mixture of hexagonal WC,
monoclinic WO2 (PDF No. 32-1393), and hexagonal a-W2C
(PDF No. 35-776).
2024 www.advmat.de © 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Figure 2a shows a scanning electron microscopy (SEM,
JEOL-JSM 840) image of acid-treated WC nanotubes that
were prepared by the thermal decomposition of W(CO)6 in
the presence of Mg powder. They have diameters of 30 to
70 nm and lengths of several micrometers. The formed tubes
are straight, coiled, or zigzag in shape. The single coil-like WC
nanotube shown at high resolution in the inset image has a di-
ameter of ca. 50 nm and a length of 1 lm. The thermal disso-
ciation of only W(CO)6, without Mg or Na, in a closed Swage-
lok cell at 900 °C resulted in the formation of 200 nm particles
and others with a short, wirelike morphology with 100 nm di-
ameters (Fig. 2c). Only a few of the wires are grown to more
than a micrometer. The X-ray diffraction (XRD) analysis of
the W–CO sample illustrates the presence of WO2, W2C, and
WC. The bulk energy-dispersive X-ray analysis carried out on
the WC nanotubes depicted in Figure 2a shows a 1:1.12 molar
ratio for W/C (Fig. 2d). A small percentage of oxygen is also
detected and the Au signal originates from the sample being
gold-coated for better conductivity while imaging.
The crystalline nature of the WC nanotubes is confirmed
using transmission electron microscopy (TEM) measure-
ments. The TEM (Fig. 3a) image of the as-prepared
W–CO/Mg sample contains tubes and nanoparticles. Selec-
tive-area energy-dispersive X-ray (SAEDX) analysis con-
firmed that the dark black particle (marked by an arrow) con-
tains Mg and O with a 1:1 atomic ratio. Furthermore, it
illustrates the perfect arrangement of the atomic layers with
an interlayer spacing of 0.215 nm between the (200) lattice
planes, which is very close to the literature value (0.21 nm)
ranging from 30 to 70 nm and a length varying from 1 to
5 lm. The MgO particles are dissolved during the acid treat-
ment and pure WC tubes remain (Fig. 3b). The inset image
shows a typical WC nanotube coil with a diameter of 70 nm
and a length of more than a micrometer. Figure 3c demon-
strates the high-resolution TEM (HRTEM) (JEOL-3010 op-
erated at 200 kV) image of the edge of the marked circular
the atomic layers and the lack of defects. The measured dis-
tance between these (001) lattice planes is 0.273 nm, which is
very close to the literature value (0.28 nm) for the hexagonal
lattice of WC. The selected-area electron diffraction (SAED)
pattern of the WC nanotube (inset image) and the diffraction
rings can be indexed to the reflections of the tungsten carbide
planes, (001) and (100). The HRTEM of a single nanotube is
depicted in Figure 3d. The inner diameter of a typical tube is
20 nm with a wall thickness of 25 nm. The WC tube is defect
free and highly crystalline. The SAEDX analysis of this tube
showed a tungsten to carbon ratio of 1:1 and a small amount
of oxygen (Fig. 3e). The oxygen contamination in WC nano-
tubes (washed W–CO/Mg sample) is also measured using an
oxygen analyzer (Eager 200) and found to be 0.7 at %.
When we checked the TEM grid carefully, a few bamboo-
shaped tubes (periodic formation of compartment layers)
were observed, although rarely (Fig. 3f) in the acid-treated
Adv. Mater. 2006, 18, 2023–2027

a the morphology or in the structure of the W–CO/
0.5 µm 0.2 µm
e several experiments at different temperatures in
Figure 3. TEM images of a) the W–CO/Mg sample, b) the acid-treated W–CO/Mg
sample, c) the acid-treated W–CO/Mg sample at high resolution and its ED pattern,
d) a single WC tube shown at high resolution. e) SAEDX spectrum of the tubes pre-
sented in (d), and f) bamboo-shaped carbon nanotubes. Upper inset: SAEDX on the
carbon nanotubes; lower inset: HRTEM image of a graphitic tube.
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inside the Swagelok reactor. No change in either
Mg sample before or after washing with 30 % HCl
was obtained. This confirms that the Swagelok
body has no catalytic role. In addition, the bulk
EDX or SAEDX analysis did not detect any trace
amount of impurities from the Swagelok body in
the WC nanotubes when the reaction was carried
out in the Swagelok reactor.
A surface-area analyzer [Micromeritics (Gemi-
ni 2375)] was used to measure the surface area of
the as-prepared sample, W–CO/Mg, and the acid-
treated sample, W–CO/Mg. Brunauer–Emmett–
Teller surface areas of 10.9 m2 g–1 and 9.2 m2 g–1
were measured for both samples.
To confirm the precise contents of the WC nano-
tubes, we used a wave dispersive X-ray (WDX) an-
alyzer, which was much more sensitive to lower
elemental concentrations than the EDX technique,
which is usually attached to a scanning electron mi-
croscope. In Figure 4, the left-hand picture is the
SEM image of the WC nanotubes, the middle im-
age verifies the presence of tungsten, while the
right image provides the carbon content.
The thermal decomposition of bare W(CO)6 in a
closed Swagelok cell at 900 °C under a nitrogen at-
mosphere yields WO2 + WC + W2C + C. In an at-
tempt to remove the O from WO2, we performed
the 800 to 950 °C range. It is evident from XRD
analysis that WO2 is the predominant product at
800 °C, 900 °C, and even at 950 °C. In addition, the
morphology of the product remains a mixture of
particles and short wires. With a longer reaction
time (8 h) at 900 °C the length of the wires could
increase up to 1 lm, maintaining analogous reac-
tion products such as WO2, WC, W2C, and C. The
reason for the addition of Mg is to use its reactivity
with oxygen, thereby avoiding the formation of
WO2. Indeed, the reaction products are
WC + MgO + W2C + C. Based on previous findings
and the control reactions described in Table 2, we
suggest the following mechanism for the formation
of WC.

–CO/Mg sample. These coiled tubes possess a 35 nm diameter W(CO)6 → W + 6 CO (1)

and a length of several micrometers. The interlayer spacing
(0.33 nm) determined from the HRTEM and SAEDX mea- W + 2CO > WO2 + 2C (2)
surements confirms that these tubes are formed from graphit-
WO2 + 2 Mg → W + 2 MgO (3)
ic carbon. This means that in addition to WC nanotubes,
ca. 7 % carbon nanotubes (seen in XRD, Fig. 1b) are formed 2 CO → C + CO2 (Boudard reaction) (4)
owing to the influence of the surface geometry[13] of the cata-
lytic MgO particles. To eliminate the possibility that the reac- W + C → WC + W2C (5)
tion is catalyzed by Fe, Co, Ni, or Cr (Swagelok body compo- The final products, WC and W2C, are obtained in reaction 5,
nents), a control experiment was carried out in which a quartz and carbon is obtained in reactions 2 and 4. Whether MgO
tube was filled with the reactants. The quartz tube was placed catalyzes reaction 5 is not clear.

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To explore the role of MgO in leading towards the final
product, additional control reactions were carried out (Ta-
ble 2). The thermal decomposition of tungstic acid (H2WO4)
at 900 °C under inert atmosphere forms WO3 (sample 1). We
intentionally added bare Mg powder to tungstic acid to react
at 900 °C, thinking that tungsten would be obtained in addi-
tion to MgO. The results convinced us that tungsten (sam-
ple 2) can indeed form at 900 °C under autogenic pressure.
The reaction between bare tungsten, carbon, and MgO at
900 °C under autogenic pressure leads to the formation of
WC + W2C + C + W (sample 3). This proves that bare tungsten
and carbon in the presence of MgO would form tungsten car-
bide. Here, some of the tungsten and carbon remained un-
reacted because of the micrometer dimensions that might
need a higher temperature to react and achieve tungsten car-
bide as the sole product, while in our reaction the nanometer-
sized particles are essential for a complete reaction at 900 °C.
The thermal solid-state reaction between WO3 + Mg + C at
900 °C yielded WC + W2C + MgO + W (sample 5). The ther-
mal decomposition of W(CO)6 in the presence of MgO also
led to the formation of WC + MgO + C + W (sample 4). The
above reactions 1 to 3 facilitate our claim regarding the for-
mation of either W or WC at 900 °C under autogenic pressure.
The MgO sample (W–CO/Mg) was washed with dilute HCl,
and the product was a mixture of around 90 % WC, 3 % W2C,
and 7 % carbon (wt %, approximated from XRD measure-
ments, area under the peaks). Another approximation was
made using HRTEM measurements and SAED spectra. Out
of twelve nanotubes one was found to be of carbon, while the
rest were WC. A slight excess of carbon was also observed in
CHNS analysis. It is difficult to obtain 100 % WC as the sole
product, even after changing the reaction time and tempera-
ture. To get rid of additional carbon nanotubes in order to
achieve 100 % WC nanotubes and also to confirm the stability
Table 2. Reactant(s), reaction conditions, and the achieved products of the control ex-
periments.
Sample Reactant(s) Temperture/atmosphere/time
name
1 H2WO4 900°C/N2/3h
2 H2WO4+Mg 900°C/N2/3h
3 W(10 lm)+C+MgO 900°C/N2/3h
4 W(CO)6+MgO 900°C/N2/3h
5 WO3+Mg+C 900°C/N2/3h
2026 www.advmat.de © 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Figure 4. X-ray mapping of tungsten and car-
bon for the SEM image of the acid-treated
W–CO/Mg sample (WC nanotubes).
of the WC nanotubes, we carried out thermogravimetric anal-
ysis (TGA) of an acid-treated W–CO/Mg sample in an air at-
mosphere. We observed very little (ca. 1.5 wt %) weight loss
in the sample above 500 °C with the same material yield
(WC + W2C + C, confirmed by XRD). This gives direct evi-
dence for the thermal stability of the formed products.
Recently, Shanmugam[5] et al. proposed that the precursors
(12-phosphotungstic acid and hexadecyltrimethylammonium
bromide) are converted to WO2 and free carbon at low tem-
peratures (800 °C) in a reaction under autogenic pressure at
elevated temperature (RAPET); the free carbon reduces the
WO2 to metallic tungsten at 900 °C. The tungsten produced in
the reaction can further react with carbon, giving rise to tung-
sten carbide nanorods at 1000 °C. (Mg powder might have fa-
vored our present reaction at a lower temperature.) Nanome-
ter-sized tungsten carbide needles (1 lm × 50 nm) were
synthesized on a tungsten tip by the chemical vapor deposi-
tion of benzene with a nickel catalyst at 750 °C.[14] The present
reaction is more complex because CO might undergo dispro-
portion (Boudard reaction) to produce CO2 and carbon (reac-
tion 4). It is likely that Mg can promote the CO dissociation
reaction in a similar manner, as in the case of the alkali-pro-
moted Fischer–Tropsch catalysis.[15] Carbon nanotubes[16] and
nested fullerenes are also prepared from supercritical CO2 by
a chemical reaction of carbon dioxide with Mg in a closed cell
for 3 h at 1000 °C, yielding MgO and carbon. Rana and Ge-
danken presented a detailed description of the formation of
MgO and the catalytic growth of carbon nanoflasks during the
thermal decomposition of Co(CO)3NO in the presence of Mg
at 900 °C.[17] They proposed that the Co particles lying on the
MgO surface grow graphitic carbon at 900 °C during the 3 h
reaction. In the present case, the formed tungsten particles lie
on the MgO nuclei surface and react with the carbon formed
from the dispropotionation reaction to further grow WC tubes
at 900 °C. The formation of WC nanotubes by the
thermal decomposition of W(CO)6 in the presence
of Mg powder is a potential route for the produc-
tion of novel WC nanotubes. The effect of tungsten
Products on the synthesis of multiwalled carbon nanotubes
using cobalt as a catalyst is also reported by Ishika-
WO3 wa et al.[18]
W+MgO There are two possibilities for the rolling mecha-
WC+W2C+W+MgO nism for the formation of WC nanotubes. The first
WC+MgO+C+W is the directed growth of hexagonal WC unit cells
WC+W2C+W+MgO
in a very specific direction in the presence of MgO.
Adv. Mater. 2006, 18, 2023–2027

The second possibility, which explains the formation of the in- –
[1]
organic fullerenes discovered by Tenne et al.,[3] is related to
[2]
the layered structures, where, at high temperature, the un- [3]
paired electrons at the edge form chemical bonds with parallel [4]
edges. Since WC is not a layered structure, the first possibility
is the one which occurs for WC. [5]
In conclusion, a competent route is reported herein for the
[6]
first time for the synthesis of WC nanotubes. The low-temper-
[7]
ature (900 °C) thermal decompositions of W(CO)6 and Mg
powder are carried out under autogenic pressure in a closed
Swagelok cell to capitulate the nanotubes of WC. The thermal [8]
decomposition of bare W(CO)6 with Na and Mg yields totally
[9]
different morphological and crystallographic products. The
probable mechanism is supported by the obtained data from a [10]
series of control reactions and previous publications.
[11]
[12]
Experimental [13]
[14]
[15]
In a typical synthesis of WC nanotubes 820 mg of W(CO)6 and
[16]
410 mg of pure Mg powder (99.9 %, Acros Chem.) were introduced
into a 3 mL stainless-steel reactor at room temperature under nitro-
gen (glove box). The filled cell was closed tightly with the other plug [17]
[19] and kept inside the quartz tube under a flow of nitrogen to avoid [18]
surface oxidation of the Swagelok during the heat treatment. The
temperature of the tube furnace was raised to 900 °C at a rate of [19]
20 °C min–1 and the temperature was maintained at 900 °C for 3 h. [20]
The Swagelok reactor heated at 900 °C was gradually cooled (ca. 5 h)
to room temperature, opened, and 0.842 g of black powder was ob-
tained. The black mixture was treated with a 30 % diluted HCl solu-
tion to remove MgO contamination. The product was centrifuged
(9000 rpm), washed three times with anhydrous ethanol, and vacuum-
dried for 12 h. The weight of the dried WC nanotubes was 0.490 g.
For the acid-treated sample, the content of carbon was found to be [21]
7.1 % with a negligible amount of hydrogen (0.3 %), as obtained from
CHNS analysis (Eager 200). Analogous reactions were carried out for
W(CO)6 as well by using a Na reactant. The significant reactions are
summarized in Table 1 with the reaction parameters and the achieved
products. Such a one-stage, efficient, simple economic RAPET tech-
nique has been previously employed for the fabrication of various in-
[22]
teresting nanostructures [20–22].
Received: April 4, 2006
Final version: May 12, 2006
Published online: July 4, 2006
______________________
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