Effect of Electron Beam on Nanoparticle Dynamics in Solution during in situ TEM
Observation
Jingyu Lu
1,2,3,4
, Zainul Aabdin
1,2,3,4
, Utkarsh Anand
3
, and Utkur Mirsaidov
1,2,3,4
1.
Department of Physics, National University of Singapore, 2 Science Drive 3, Singapore, 117551.
2.
Centre for Advanced 2D Materials and Graphene Research Centre, National University of Singapore,
6 Science Drive 2, Singapore 117546.
3.
Centre for BioImaging Sciences, Department of Biological Sciences, National University of
Singapore, Science Drive 4, Singapore, 117543.
4.
Nanocore, 4 Engineering Drive 3, National University of Singapore, Singapore 117576.
The recent development in in situ TEM enabled to visualize the nucleation, growth, coalescence and
shape evolution of nanoparticles [1-4]. Some of these processes are driven by electron beam effects [5].
In this study we found that under intense electron beam nanoparticles aggregate together and form a
large cluster that relaxes into a large spherical nanoparticle. While under low electron beam different
attachment of nanoparticles results in nanorod structures.
The observation was performed with the TEM JEOL 2010F operated at 200 kV, and dynamics were
captured at 10 frames per second. The sample was made of 1 mM HAuCl
4
and CTAB solution
entrapped between two ~20 nm thick SiN
x
membranes in a liquid cell, more details can be found
elsewhere[6]. Attachment of nanoparticles, observed in these liquid cells with TEM for low electron
beam condition, is a common way to form nanorod structures as shown in Figure 1. When electron dose
is less than 200 e/(A
2
.s), only small nanoparticles (radius<3 nm) exhibit evident motion (Figure 1(a)-
(b)). As the dose rate increases, larger nanoparticles start moving (Figure 1(c)-(f)). Note that the
nanoparticles encircled in red ellipses in each frame merged together. Two large elongated
nanoparticles, formed from individual particles, attach at their endpoints and new longer rod-like
nanoparticle is formed. Once these rod-like structures were formed, the attachment of new nanoparticles
takes place at the rod tips, thus the nanorod grows even longer, as shown in Figure 1(d)-(f). Similar
phenomena are found in the synthesis of Pt
3
Fe nanorods [7] as well.
At high electron doses, the consecutive attachment of 5 nanoparticles forms a big spherical nanoparticle
(~11 nm in diameter) instead of a nanorods structure as shown in Figure 2. In each attachment case here,
the smaller nanoparticle is fused into the larger nanoparticle; our observations reveal that the larger the
two attaching nanoparticles, the longer it takes to form a spherical nanoparticle after the coalescence,
(Figure 2(a)-(c) vs Figure 2(f)-(g)). Figure 2(i) shows the evolution of projected area of these
nanoparticles. The projected area of each new nanoparticle formed by the attachment of two
nanoparticles decreases steadily as they tend to become spherical in shape. On the whole, the total
projected area was decreased by ~43% at the end of the process, indicating that the surface energy
minimization contributes greatly to this shape relaxation [3]. Further study is on the way to uncover
more details.
Paper No. 0129
257
doi:10.1017/S1431927615002081 © Microscopy Society of America 2015
Microsc. Microanal. 21 (Suppl 3), 2015