Carbon 43 (2005) 22092214

www.elsevier.com/locate/carbon

Hydrogen adsorption in dierent carbon nanostructures

Barbara Panella

a,*

, Michael Hirscher a, Siegmar Roth b

Max-Planck-Institut fu r Metallforschung, Heisenbergstr. 3, D-70569Stuttgart, Germany

Max-Planck-Institut fu r Festko rperforschung, Heisenbergstr. 1, D-70569Stuttgart, Germany
Received 23 July 2004; accepted 29 March 2005
Available online 10 May 2005

Abstract
Hydrogen adsorption in dierent carbonaceous materials with optimized structure was investigated at room temperature and
77 K. Activated carbon, amorphous carbon nanotubes, SWCNTs and porous carbon samples all show the same adsorption properties. The fast kinetics and complete reversibility of the process indicate that the interaction between hydrogen molecules and the
carbon nanostructure is due to physisorption. At 77 K the adsorption isotherm of all samples can be explained with the Langmuir
model, while at room temperature the storage capacity is a linear function of the pressure. The surface area and pore size of the
carbon materials were characterized by N2 adsorption at 77 K and correlated to their hydrogen storage capacity. A linear relation
between hydrogen uptake and specic surface area (SSA) is obtained for all samples independent of the nature of the carbon material. The best material with a SSA of 2560m2/g shows a storage capacity of 4.5 wt% at 77 K.
2005 Elsevier Ltd. All rights reserved.
Keywords: Activated carbon; Carbon nanotubes; adsorption; Adsorption properties; Surface area

1. Introduction
Hydrogen
storage isasthe
bottleneck
for
the breakthrough
of hydrogen
energy
carrierstorage
in automotive
applications.
Ininvestigated
the last years
dito
erent
technologies
have
been
[1,2]
develop
a
secure
and
cheap
way to liquefaction,
save hydrogen.
Storage
by gas
compression,
hydrogen
or
in
the
form
of
metal
hydrides,induced
possessthesevere
disadvantages.
These
drawbacks
have
study
of
new
storage
concepts
as
physical
adsorption
on
nanomaterials.
Especially
novel
carbon
materials,
such
as
carbon
nanotubes,
activated
carbon
and
carbon
attracted a storage
lot of
interest,
however,
the nanobers
values orders
for have
their
capacity
scatter
over
several
of hydrogen
magnitude
[3]. At
present,
the
independently
conrmed
and
repeatable
storage capacities in carbon materials at room tempera*
Corresponding author. Tel.: +49 711 6891810; fax: +49 711
6891952.
E-mail address: bpanella@mf.mpg.de (B. Panella).

0008-6223/$
- see front matter 2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.carbon.2005.03.037

ture
are less
1 wt% [4,5],
however,
higher values
can be
reached
bythan
lowering
the
temperature.
The materials
process
responsible
for
hydrogenis
adsorption
in carbon
at
moderate
temperature
physisorption
[610],
which
is
based
on weak van
der Waals
forces between
adsorbate
and
adsorbent.
At room
temperature
the magnitude
of
this
interaction
can
be
of
the
same
order
as
the
thermal
motion
energy
of gas
molecules
onbetheachieved
surface, [11,12].
therefore
only
low
storage
capacities
can
If
the
system
isthe
cooled
down, the
interaction
be- tween
the
surface
and
gas
molecule
becomes
stronger
than the
thermal
motion
energy
of
the
adsorbate,
which
is
proportional to the temperature.
In characterized
this work, diand
erentinvestigated
carbon nanostructures
have
been
in pressures
view of both
their
hydrogen
adsorption
capacity
up77to K.
high
at
room
temperature
and
at
These
materials
possess
which
havespeci
been
forand
the
hydrogenstructures
uptake,
e.g.,
high
c optimized
surface
micropore
density.
In order
to understand
the area
nature
of
the adsorption
process,
the hydrogen
storage capacity

221
0

B. B.
Panella
Panella
et et
al. al.
/ Carbon
/ Carbon
4343
(2005)
(2005)
22092214
22092214

221
0

Table 1
Carbon nanomaterials investigated for hydrogen storage and their structural properties
Sample (country)

BET SSA

Average pore

Pore volume for pores with

Helium density

221
1

B. B.
Panella
Panella
et et
al. al.
/ Carbon
/ Carbon
4343
(2005)
(2005)
22092214
22092214
[m2/g]
diameter [A ]
radius <6.5 A [cm3/g]

[g/cm3]

Activated carbon I (Canada)

Porous carbon I (Mexico)
Activated carbon II (Germany)
Puried SWCNT I (USA/Germany)
Porous carbon II (Mexico)
Puried SWCNT II (USA)
Amorphous CNT (China)
SWCNTs (Russia)
Ros 1 (Cyprus)
Ros 3 (Cyprus)

2564
1646
1065
1024
946
854
369
124
34
22

2.0
2.2
2.0
2.0
2.1
2.1
2.2
1.7
2.1
2.0

11.75
11.08
18.23
15.37
10.60
17.09
14.48
15.52
11.46
11.32

is
correlated to the structural properties of the carbon
samples.
2. Experimental
2.1. Carbon nanostructures
carbon worldwide
materials for
havethis
been
obtained
from
di
Various
erent
suppliers
study.
Firstly,
different
types
of been
carbon
nanotubes
(CNTs)
with
speci
c
structures
have
selected.
Amorphous
carbon
nanotubes
have
been
produced
by
DC
arc
discharge
in
atmosphere of hydrogen gas at temperatures above an
300
C [13].
Thesefrom
nanotubes
hollow
pipes
with
diameter
ranging
10nm toare
15 nm,
and
the walls
show
no
long-range
ordered
structure.
Single-walled
carbon
nanotubes
(SWCNTs),
which
have
been
produced
with
the
HiPco
(High from
pressure
CO
conversion)
method,
have
been
purchased
CNI.
This
synthesis
produces
a
high
yield
of
well
ordered
SWCNTs
with
a
narrow
diametermetal
distribution
around 1Therefore,
nm, however,
still
containing
catalyst
particles.
this
material
has
been
puri

ed
by
either
selective
oxidation
and
subsequent
HCl
treatment
(sample
I) of
[14]SWCNTs
or standard
purica1 tion
procedures
giving
98 wt%
(sample
Additionally,
we
received
SWCNTs
prepared byII).
graphite
arc discharge
evaporation
in helium
atmosphere
and
collecting
the
soot
from
the
cold
walls
of
theareaction
chamber
[15].
These samples
contain
typically
high
fraction
of
amorphous
carbon
and
catalyst
particles.
Otherhydrocarbons
samples have in
been low
produced
byarc
cracking
of liquid
voltage
discharge
or
resistive
heating.
Thisa and
method
results
in
a
mixture
of
MWCNTs,
SWCNTs
polyhedral
nanoparticles
of
di

erent
compositions
and
are
called
Ros
1
and
Ros
3
by
the
producer
[16].
Secondly,
activated
carbon
fromcarbon
dierent
have
been[17],
investigated.samples
Activated
I issuppliers
similar to
AX-21
1

Vajo J. Private communication.

0.75
0.46
0.49
0.39
0.25
0.36
0.13
0.05
0.01
0.0065

221
1

which
is obtained
from
thea reaction
of coke
with
KOH,
giving
a to
product
with
doubled
speci
c Porous
surface
area
compared
regular
grade
porous
carbon.
carbon
samples
1
and
2
are
carbon
structures
with
ordered
pores of
which have
been prepared
by
the pyrolysis
ofuniform
sucrose size
embedded
in mesoporous
sil- ica
[18].
The
surface
area
and
the
pore
dimension
of
the
samples
have been
measured
quantachrome
autosorb
gas
sorption
system
using with
nitrogen
gas at
K surface
and
applying
the
multipoint
BET method
for 77
theof
area,
and
the
MP-method
which
is
an
extension
the
de
Boer
s t-method
for the micropore
volume.
The
di2 er-areas
ent
carbon
nanostructures
possess
speci
c 2560m
surface
2
ranging
from
approximately
20m
/g
to
/g,
and
high
pore densities,
Table 1. The
highest
surface
very
the see
maximum
theoretical
surfacearea
of is
a
2
doubleclose
sidedtographite
sheet of 2630m
/g.
2.2. Hydrogen storage measurement
The hydrogen
adsorption
has been which
measured
by of
a
manually
controlled
Sieverts
apparatus,
consists
two
volumes
connected
through
a valve,
i.e.,Owing
sample
holder
and
gas
inlet
chamber
of
constant
volume.
to
the
design
witheven
smallsmall
volumes,
the apparatus
can
be used
investigate
quantities
of carbon
material. to
A
schematic
diagram
of
the apparatus
is
shown
in Fig.
1.
The
apparatus
was
previously
tested
for
leak
absence
and
for
accuracy
through
calibration
with
the
empty
sample
holderhydrogen
and with gas
wellhas
known
drides.
Ultra pure
beenmetal
usedhy-for
the
experiments.
Typically
the
mass
of
the
carbon
samples
used
for
hydrogen
storage
measurements
is
100300
mg.
Prior
to
measurement,
the samples 2are
degassed
and heated
at
200 C for
approximately
h until
a pressure
of
6
1

10
mbar
is
reached.
Then
the
desired
hydrogen
pressure
is introduced
inisthe
thermostated
chamber
and
after
thermal
reached,
the gas is
per-pressure
mitted
to
expand
inequilibrium
the
sample
holder.
The
drop
is caused
by the
gas expansion
in a measured
bigger

Pump

after each
adsorption
the
sample
is heated
and degassed.
This
means
that each
storage
is obtained
independently
from
previous
step.value
The
ideal
gas
equation
withthe
acalculate
compressibility
factorcorrected
up
to the
second
order
is
used
to
the
amount
of
adsorbed
hydrogen
from
the
pressure
drop.
For
some
samples
hydrogen storage capacity in the pressure range from the
0.2
bar
toa0.9
barmicrobalance.
and at 77 K Here
is measured
gravimetriwith
the mass
change as
acally
function
ofCahn
hydrogen
pressure is recorded.
The con-

techniques
is a further
proof for the accuracy of our volumetric measuring
system.

Manometer

reservoir

H2

He

waterbath

Sample holder

Fig.
1. Schematic
diagram
of the
SievertsForapparatus
used toatmeasure
hydrogen
storage
in and
carbon
samples,
temperature
reservoir
holder
are measurements
immersed
the room
water
bath. For
measurements
atsample
77 K the
sample
holder
is in
immersed
in
liquid
nitrogen.

3. Results and discussion

volume
hydrogen
adsorption
in thewesample.
After
no
moreand
pressure
change
issure
observed,
wait equilibfor
an
additional
1015 min
to be
thatadsorption
the thermal
rium
is
reached.
After
hydrogen
at
room
temperature,
the
sample
holder
is
cooled
in
liquid
nitrogen
until
the decrease
new equilibrium
conditionpressure
is reached.
In
this
case
the
ofand
the due
hydrogen
is due
to
the
cooling
of sample
the gas
to the enhancement
of
adsorption
in
the
at
low
temperature.
To
evaluate
the
storageis capacity
of the
carbonconditions
materials
the
experiment
repeatedsample
under
the
same
with
a
non-adsorbing
(Seasand)
having
the
same
volume
theblind
carbon
material.
volume
sample is as
measured
volumetrically
withThe
helium
gas. of the
Each adsorption cycle is repeated at dierent hydrogen pressures from 2 bar to approximately 60bar and

Similar
adsorption
isotherms
have been obtained
for
all
investigated
carbon
nanostructures.
Furthermore,
they
show
aeach
complete
reversibility
ofa the
hydrogen
uptake.
After
adsorption
cycle
at
given
pressure
the
hydrogen
removedforfrom
and thehydromeasurement
isisrepeated
dithe
erentsample
pressure.
gen
storage
capacity
is aindependent
of the The
number
of
adsorption
cycles
which
proves
that
hydrogen
is
stored
reversibly
in
these
carbonholder,
materials.
If hydrogen pressure
gas was
expanded
in
the
sample
the
equilibrium
is
reached
within apressure
few seconds.
During
waiting indicating
for 1015
min
no
further
change
is observed,
thatcharacteristic
thermal
equilibrium
is reached.
These fast kinetics
are
for physisorption.
Fig. 2 carbon
shows the
hydrogen
adsorption
isotherms
of
activated
I and
ofEven
puri
ed SWCNTs
at 77als
K
and
at room
temperature.
though
the two II
materipossess
a
completely
di

erent
n
anostructure,
the
shape
of the isotherms is very similar. This shape is

Fig.
2. Hydrogen
adsorption
isotherms at room temperature and at 77 K tted with a Henry type and a Langmuir type equation, respectively (a) for activated
carbon,
(b) for puri
ed SWCNTs.

characteristic for all investigated carbon materials. At

298 K the hydrogen uptake is a linear function of the
pressure, which can be explained with Henry s law. At
room temperature no saturation occurs in the investigated pressure range and the adsorbed hydrogen layer
on the carbon surface is very diluted.
At low temperature the isotherms can be tted with a
Langmuir-type equation (type I isotherm) indicating
that saturation takes place with a hydrogen monolayer
formation, as usual for microporous surfaces. In fact,
the pore dimensions limit the hydrogen adsorption to
one molecular layer in structures with micropores
[19,20].
Additionally, an average value of the adsorption enthalpy at 77 K can be estimated by applying the Langmuir equation [2123]:
h

1
1 exp

e
kT

Fig.
3. Relation
storage
capacity
of the
diof
erent
carbon
samples atbetween
77 K andhydrogen
their speci
c surface
area. The
slope
the
t is 1.91 10 3 wt% m 2 g.

where
e is constant,
the adsorption
potential of hthe
k the
Boltzmann
Tchemical
the temperature,
thesolid,
coverage,
and
lgas.the
potential
of
aafractional
hydrogen
molecule
in
the
The
chemical
potential
as
function
of
thevalues
hydrogen
pressure
is calculated
using the
lated
of the
enthalpy
and
the entropy
at tabu77enK
[24].
This
evaluation
yields
an
average
adsorption
thalpy
of
(56

10)
meV
for
activated
carbon
I,
which
is
with
a
storage
capacity
of
about
4.5
wt%
at
77
K,
the
best
material
analyzed.
This
adsorption
potential
has depento be
considered
as
an
approximate
value
since
any
dence
between
the adsorption
potential
and
has
been
neglected.
Nevertheless,
the low
valuecoverage
clearly
indicates
that
hydrogen
is material.
physically
adsorbed
in this
carbonaceous
nanoporous
Chemisorption
of
hydrogen
would
require
more
than
ten
times
higher
enthalpy of adsorption [25,26].
The
hydrogen
uptake
of
the
di

erent
carbon
nanostructures
at An
77 Kalmost
is correlated
to their
specicthesurface
area
(Fig. 3).
linear the
relation
between
age
capacity,
evaluated
from
saturation
value
ofstorthe
Langmuir

t,
and
the
speci

c
surface
area
is obtained
for
all
materials
investigated.
In
contrast,
the
storage
capacity
seems
to
be
independent
of
the
nature
of
the
carbon
nanomaterial,
as long-range
order
or curvature
of
the
graphene
sheets.scattering
In
accordance,
similar
have
ndingsbeen
by
inelastic
investigations
reported inneutron
Refs. [8,9].
An upper
limit
of thebyhydrogen
adsorbed
inthe
a
monolayer
can be
estimated
assuming the
density
of
liquid
[10]. Accordingly,
the
maximum
hydrogenadsorbate
storage capacity
per specic surface
area of3
carbon can
be theoretically calculated to 2.28 10
mass% m 2 g.
The experimental results yield a slope of 1.91
10 3 mass% m 2 g, which is smaller than the theoretical

value,
because
at density
77 K the
of the monolayer
is
smaller
thancorresponds
the
of density
liquid hydrogen.
The measured value
to
2 an occupancy of one hydro
gen molecule per 17.5 A of carbon surface. Assuming a
closely packed distribution of hydrogen molecules on
the
surface
of thedistance
adsorbent,
occupancy
corresponds
to a on
reticular
of 4.5this
A Further
between
hydrogen
molecules
the carbon surface.
considering
the
2 area of a carbon hexagon of the graphene sheet (5.2

A
), approximately
six hydrogen
molecules would
occupy
the area of 20carbon
hexagons.
On the other hand, under the assumption that the
closely
packed
hydrogen
monolayer
has an
intermolecular

distance
equal value
to
thatat
of 77
liquid
(4.1
A
experimental
K hydrogen
corresponds
to ),athe
surface
coverage of 84%.
Similarand
results
linear relationof between
hydrogen
uptake
speciof
cbyasurface
materials
have been
obtained
Nijkamparea
et al. [27]carbon
with a slope
of
1.5 10 3 mass% m 2 g at a pressure of 1 bar and
77 K.
Theoretical calculations [28,12] indicate, that hydrogen adsorption is favoured in small micropores. Therefore, the hydrogen adsorption capacity is correlated to
the pore volume of pores possessing diameter less than
1.3 nm (Fig. 4). The linear relation between the pore volume and the storage capacity demonstrates that carbon
materials ideal for hydrogen storage should possess a
high microporosity with a small pore dimension.
Fig. 5 shows that at room temperature as well the
storage capacity of the carbon samples at a pressure of
65 bar depends almost linearly to their surface area. In
this case the slope of the curve is only 0.23
10 3 mass% m 2 g, which corresponds to a surface coverage of only 10% assuming the density of the liquid
adsorbate. Similar low hydrogen storage capacities at

dered
arraysmaterials
of the graphene
sheets. Asadsorption
a consequence
promising
for surface
hydrogen
are
nanostructures
with high
area and micropore
density.
While at room
temperature
the highest
measured
storage
1 wt%toeven
atuphigh
hydrogen
pressure,value
atAmong
77isK less
it all
isthan
possible
store
to 4.5
wt% of
hydrogen.
investigated
materials
activated
carbon
with
high
grade
of
porosity
is
the
best
nanostructure
for
hydrogen kinetics
adsorption.
Owing
tocarbon
the fast
adsorption
and
desorption
and
the
reversibility,
physisorption
is a very
promising Future
conceptinvesfor hydrogen
storage
at moderate
tigations
should
concentrate
onconditions.
new carbon,
materialsinwith
sur-toface
area,
even
higher
than
activated
order
achieve
successful
storage
capacities
not
only
at
low
temperature but also at ambient conditions.
Acknowledgments

Fig.
Correlation
between
hydrogen
pore4.volume
for pores
with the
diameter
<1.3storage
nm. capacity at 77 K and the

The
authors du
areQuebec,
thankful Canada,
to Richard
Chahine
from
the
Universite
forVajo
the
synthesis
of
the
activated carbon
sampleforI, John
from
HRL
Laboratories,
California,
purifying
the
CNI
SWCNTs
andus
Channing
Ahn
fromWe
CalTech,
California,
for
providing
with
the
samples.
are
also
grateful
to
Mauricio
Terrones,
Humberto
Terrones,
Eduardo
Terres
Manuel
Dominguez
from IPICyT,
ico,
forand
the Jose
synthesis
of the
porous
carbon
samplesMexand
Ursula
Dettla-Wegliskowska
from
the
Max-PlanckInstitut
fu r ofFestko
rperforschung
inI. Stuttgart
forgoes
the
puri

cation
the
SWCNTs
sample
Our
thank
also
to Alexander
Okotrup
and Lyubov
Bulsheva
from
the
Institute
of
Inorganic
Chemistry
SB
RAS,
Russia,
for
the
SWCNTs Freiberg,
sample, toGermany,
W. Heschel
from the TU
Bergakademie
for providing
the
activated
Carbon
II sample,
to Maria
XenophontosIoannou
from
Rosseter
Holdings
Ltd,
Cyprus,
the
Ros1
and
Ros3
samples,
and
to
Yongning
Liuforfrom
the
Department
of
Material
Science
and
Engineering
at
the
Xi CNT
an Jiatong
University,
China
for the
amorphous
sample.
We
are
also
thankful
to
Annette
Fuchs for the N2 sorption measurements.
References
[1] Zu ttel A. Materials for hydrogen storage. Mater Today 2003;
6(9):2433.
[2] Schlapbach L, editor. Hydrogen storage special issue. MRS Bull
2002; 27(2).
[3] Hirscher M, Becher M. Hydrogen storage in carbon nanotubes. J
Nanosci Nanotech 2003;3(12):317.
[4] Ritschel M, Uhlemann M, Guteisch O, Leonhardt A, Gra A,
Taeschner C, et al. Hydrogen storage in dierent carbon nanostructures. Appl Phys Lett 2002;80(16):29857.

Fig.
5. Hydrogen
storage
capacity
in wt% samples.
at 298 K and 66 bar as a
function
of the surface
area
of the carbon

RT have been found by NMR investigations in

SWCNTs [2931].
4. Conclusion
Dioptimized
erent carbon
materials
been investigated
with
structures
for have
hydrogen
adsorption.
The
fast kinetics
and
complete
reversibility
clear
evidence
that
the
process
responsible
for give
hydrogen
adsorption
in
carbon
nanostructures
is
physisorption.
The
amount
of
hydrogen
physisorbed
depends
almost
linearly
on at
theroom
speci
c surface area,
both
at low temperature
and
temperature,
and
is independent
of
the
type
of carbon
nanostructure.
Therefore
the
hydrogen
adsorption
process
is
based
on
the
local
interaction
between
the hydrogen
moleculeorder,
and curvature
the surface,
however,
independent
of long-range
or or-

[5] Chen
Haluska
M, Res
Dettla
-WegliProc
skowka
U, Hirscher M,
Becher X,
M, Roth
S. Mater
SocSymp
2002;706:Z9.11.16.
[6] Haluska
M,
Hirscher
M, Becher
M, Dettla
-Wegliskowka
U,
Chen
X,
Roth
S.
Interaction
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