Journal of Power Sources 195 (2010) 1463–1471
Contents lists available at ScienceDirect
Journal of Power Sources
journal homepage: www.elsevier.com/locate/jpowsour
Chemical vapor synthesis and characterization of aluminum nanopowder
Jin Won Choi, Hong Yong Sohn
∗
, Young Joon Choi, Zhigang Zak Fang
Department of Metallurgical Engineering, University of Utah, 135 South 1460 East, Room 412, Salt Lake City, UT 84112-0114, USA
article info
Article history:
Received 23 July 2009
Received in revised form 1 September 2009
Accepted 2 September 2009
Available online 11 September 2009
Keywords:
Hydrogen storage
Chemical vapor synthesis
Aluminum nanopowder
Nanocrystalline materials
abstract
Aluminum is a component in many promising hydrogen storage materials such as aluminum hydride and
complex aluminum hydrides. In this research, Al and TiAl
3
-containing Al nanopowders were prepared by
a chemical vapor synthesis (CVS) process using Mg as the reducing agent. XRD and EDS results indicated
that the produced powder was composed of Al or Al with TiAl
3
. The shape of the powder was spherical
with the average size in the range of 10–50 nm measured by SEM, TEM, BET and ZetaPALS compared with
the typically larger than 100 nm for commercially available fine Al powders. In addition, the effects of the
operating conditions such as Ar flow rate, precursor feed rate and reaction temperature on the properties
of the product powder were investigated.
© 2009 Elsevier B.V. All rights reserved.
1. Introduction
Hydrogen is one of the most promising alternative energy car-
riers [1,2]. Currently, the simplest and most common method
of hydrogen storage uses thick-walled pressurized tanks. Other
methods such as liquid hydrogen in a cryogenic tank, physisorp-
tion of hydrogen, metal hydrides and complex hydrides, many of
them containing aluminum, as well as the use of hydrocarbons
have been studied [1–6]. Metal hydrides and complex hydrides
offer a safe way to store hydrogen. However, the kinetics of
dehydrogenation is too slow in a near-ambient temperature and
the reactions are not readily reversible under reasonable condi-
tions [3,6]. To overcome these barriers, nanoparticles and doping
elements are considered. Recent studies have shown that the dehy-
drogenation temperature can be lowered and the reversibility
of hydrides such as sodium alanate can be increased by doping
the compounds with Ti [7–9]. In addition, nanoscaled materials
offer many advantages. The small size of these materials strongly
enhances the kinetics of hydrogenation and dehydrogenation by
increasing the reaction and diffusion rates. In other words, the
reactivity per unit mass of nanostructured materials due to the
large surface area is significantly higher and the diffusion path
from surface to bulk is shorter than that of the larger sized materi-
als.
The synthesis techniques for nanosized materials include gas
condensation, plasma processing, chemical vapor synthesis (CVS),
sol–gel, rapid quenching, crystallization of amorphous solids and
∗
Corresponding author. Tel.: +1 801 581 5491; fax: +1 801 581 4937.
E-mail address: h.y.sohn@utah.edu (H.Y. Sohn).
mechanical milling/alloying [10,11]. Most methods require an
extensive effort to control the size of the particles in the nanome-
ter range to prevent agglomeration and oxidation due to the highly
reactive nature of the particle surface. Chemical vapor synthesis
is a method to prepare solid powders by vapor phase reactions. It
was developed from the chemical vapor deposition technique to
form particles instead of a film. CVS has considerable flexibility in
producing nanomaterials by the use of a wide variety of precur-
sors. The CVS process, which has been successfully developed at
the University of Utah, involves reducing a vapor phase mixture of
volatile precursors of the constituent metals by magnesium vapor
or hydrogen, depending on the thermodynamics of the synthesis
reactions. The key advantages of this process are the small size of
produced particles, the ability to produce powders of many differ-
ent compositions, the homogeneity of powder composition, and
the ease of doping element addition in one-step synthesis. Sohn et
al. [12–15] applied the basic concepts of the hydrogen reduction of
metal chlorides to the CVS of intermetallic and metal alloy pow-
ders. When hydrogen is used, these chemical vapor reactions can
generally be written as follows:
mMCl
x
(g) + nNCl
y
(g) + 0.5(mx + ny)H
2
= M
m
N
n
(s) + (mn + ny)HCl(g) (1)
where M and N represent two different metals with x and y being
the valences and M
m
N
n
being the intermetallic compound formed.
Another key feature of chemical vapor synthesis is that it allows the
formation of doped or multi-component nanoparticles through the
use of multiple precursors. Sohn et al. [16] synthesized WC–Co com-
posite powder by reducing WCl
6
and CoCl
2
precursors. Choi et al.
[17] prepared Mg nanoparticles doped with Ti in a vapor phase reac-
tion, which showed superior hydrogen storage properties. Ehrman
0378-7753/$ – see front matter © 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.jpowsour.2009.09.007