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Article

Thermal Effect and Rayleigh Instability of


Ultrathin 4H Hexagonal Gold Nanoribbons
Peifeng Li, Ying Han, Xiao
Zhou, ..., Jun Song, Hua Zhang,
Yang Lu
jun.song2@mcgill.ca (J.S.)
hua.zhang@cityu.edu.hk (H.Z.)
yanglu@cityu.edu.hk (Y.L.)

HIGHLIGHTS
Thermal effect of ultrathin 4H Au
NRBs was studied by in situ
electron microscopy

The 4H hexagonal phase of Au


NRBs remains quite stable upon
being heated up to 400 K

Under moderate heating,


Rayleigh instability occurred in 4H
Au NRBs with size effect

Phase transition from 4H to FCC


occurred when the heating
temperature approached 800 K

Thermal responses in terms of geometry and crystalline phase evolution of


ultrathin hexagonal gold nanoribbons (4H Au NRBs) were studied by in situ TEM.
Under moderate electron beam-induced heating below 400 K, ‘‘Rayleigh
instability’’ occurred with an obvious geometric effect, but the 4H phase remained
stable. However, phase transition from 4H to face-centered cubic phase occurred
when heating temperature approached 800 K by a dedicated MEMS chip, which
agrees well with the molecular dynamics simulation results.

Li et al., Matter 2, 1–8


March 4, 2020 ª 2019 Elsevier Inc.
https://doi.org/10.1016/j.matt.2019.10.003
Please cite this article in press as: Li et al., Thermal Effect and Rayleigh Instability of Ultrathin 4H Hexagonal Gold Nanoribbons, Matter (2019),
https://doi.org/10.1016/j.matt.2019.10.003

Article
Thermal Effect and Rayleigh Instability
of Ultrathin 4H Hexagonal Gold Nanoribbons
Peifeng Li,1,2,7 Ying Han,1,7 Xiao Zhou,3,7 Zhanxi Fan,4 Shang Xu,1 Ke Cao,1 Fanling Meng,1 Libo Gao,1
Jun Song,3,* Hua Zhang,4,5,6,8,* and Yang Lu1,5,*

SUMMARY Progress and Potential


Recently, gold nanoribbons (Au NRBs) with hexagonal (4H) phase have emerged Thermal stability of ultrathin
as a new kind of ultrathin Au nanostructure with unusual metastable crystal metallic nanostructures has been
phase, which could possess unique physiochemical properties and various a critical issue for their practical
promising applications. However, its geometric structure and phase stability un- applications. The emerging
der realistic service conditions, like Joule heating or external thermal loading, hexagonal (4H) gold nanoribbons
have not been well studied. Here, we systematically investigated the thermal re- (Au NRBs) possess promising
sponses in geometries and crystalline phases of ultrathin 4H Au NRBs under nanoelectronic, plasmonic, and
controlled in situ heating. It is found that upon moderate electron beam irradi- catalytic applications; however,
ation heating below 400 K, ‘‘Rayleigh instability’’ can be gradually observed, their thermal stability at elevated
showing an obvious geometric effect, but the 4H phase remains stable. How- temperatures has not been well
ever, phase transition from 4H to face-centered cubic phases occurs when understood. Here, we report a
heating temperature approaches 800 K by using a dedicated microelectrome- systematic study on the thermal
chanical system heating chip, which agrees well with the result obtained by mo- effect of ultrathin 4H Au NRBs by
lecular dynamics simulations. using in situ transmission electron
microscopy characterization.
INTRODUCTION Despite Rayleigh instability upon
moderate electron beam-induced
In the past decade, various ultrathin metallic nanowires with a diameter of less than
heating below 400 K, there was
10 nm have been synthesized as a new kind of one-dimensional (1D) nanomaterial,
no obvious phase transition
which have shown unique physical and chemical properties with various promising
observed in ultrathin 4H Au NRBs.
applications.1–9 In particular, ultrathin gold (Au) nanostructures are considered
However, phase transition from
one of the most promising candidates for future nanoelectronics applications10–14
4H to face-centered cubic phases
owing to their excellent thermal stability, electrical and mechanical properties,
did occur when heating
and chemical inertness. Recently, ultrathin Au nanoribbons (NRBs) with an unusual
temperature reached 800 K,
metastable hexagonal (4H) phase,15 unlike normal Au with face-centered cubic
which agrees well with the
(FCC) phase,1–4 have been synthesized and possess promising plasmonic and cata-
molecular dynamics simulations.
lytic applications such as electrocatalytic hydrogen evolution reaction.16–19 Of note,
This work provides key insights
4H and FCC phases distinguish each other in terms of characteristic stacking se-
into the thermal stability of
quences (i.e., ‘‘ABCB’’ for 4H and ‘‘ABC’’ for FCC) along their close-packed direc-
ultrathin 4H Au nanostructures
tions. However, their thermal stability at elevated temperatures, which should be
and may facilitate their future
of critical importance for their future practical applications, has not been well stud-
practical application in
ied.20–23 In this work, we systematically investigate the thermal responses of 4H Au
nanoelectronics, plasmonics, and
NRBs under the moderate- and high-temperature heating, and characterize their
catalysis.
geometric and atomic structural evolutions under the different thermal loading
mechanisms.

RESULTS AND DISCUSSION


Figure 1A shows a typical transmission electron microscopy (TEM) image of the syn-
thesized ultrathin Au NRBs synthesized by using our previous synthetic method.15
The folding part of Au NRB (inset of Figure 1A) proves its ribbon shape with a

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https://doi.org/10.1016/j.matt.2019.10.003

Figure 1. TEM Analysis of 4H Au NRBs and Two In Situ TEM Heating Modes
(A and B) High-magnification TEM image (A) and HRTEM image (B) of ultrathin 4H Au NRBs. Insets:
(A)TEM image of a typical folded Au NRB; (B) the corresponding FFT pattern.
(C) Schematic diagram of ultrathin 4H Au NRB under E-beam irradiation-induced heating.
(D) Schematic diagram of ultrathin 4H Au NRBs under MEMS chip-induced heating.

thickness of around 2 nm. The high-resolution TEM (HRTEM) image and the corre-
sponding fast Fourier transform (FFT) pattern confirm the 4H hexagonal phase of
Au NRBs (Figure 1B). The unit cell of the 4H Au NRB and its close-packed planes
along the [001]4H direction with a characteristic stacking sequence of ‘‘ABCB’’ can
be observed in Figure 4A. To study the thermal effect on the ultrathin Au NRBs,
we used two heating mechanisms, i.e., a controlled electron beam (E-beam) irradi-
ation-induced moderate heating and a dedicated microelectromechanical system
(MEMS) chip-induced high-temperature heating, which are schematically illustrated
in Figures 1C and 1D, respectively. The E-beam irradiation was carefully controlled 1Department of Mechanical Engineering, City
with a current density of 50 pA/cm2 as a moderate local heating mechanism, University of Hong Kong, Kowloon 999077, Hong
Kong, China
providing temperature from tens to hundreds degrees Kelvin (<400 K),24–26 2Collegeof Materials Science and Engineering,
while the MEMS chip provided a quick and controllable global heating up to 800– Shenzhen University, Shenzhen 518060, China
1,600 K.27,28 3Department of Mining and Materials
Engineering, McGill University, Montréal, QC
H3A 0C5, Canada
First, the geometric evolution of the ultrathin Au NRBs was studied upon moderate
4Center for Programmable Materials, School of
E-beam irradiation heating. As shown in Figures 2A and 2B, an ultrathin Au NRB with Materials Science and Engineering, Nanyang
average width (w) of 13.4 nm showed a significant geometry change after 15 min of Technological University, 50 Nanyang Avenue,
Singapore 639798, Singapore
E-beam irradiation. Its smooth shape changed into a sinusoidal shape (Figure 2B).
5Hong Kong Branch of National Precious Metals
This phenomenon is recognized as ‘‘Rayleigh instability,’’29,30 which was originally
Material Engineering Research Center (NPMM),
found in fluid but has been recently discovered in some metallic nanostruc- 83 Tat Chee Avenue, Kowloon, Hong Kong,
tures.31–37 The driving force of Rayleigh instability is that liquids, or nanoscale solids China
6Department of Chemistry, City University of
with active diffusing atoms and high surface energy, by virtue of their surface ten-
Hong Kong, Kowloon, Hong Kong, China
sion, tend to minimize their surface areas.38 It is worth mentioning that unlike Ray- 7These authors contributed equally
leigh instability that occurs in cylindrical nanowires,31–37 both the necking width, 8Lead Contact
w1 = 10.1 nm, and the bulging width, w2 = 12.9 nm, of the Au NRB after E-beam irra-
*Correspondence: jun.song2@mcgill.ca (J.S.),
diation (Figures 2B and 2C) become smaller than the initial width, w = 13.4 nm (Fig- hua.zhang@cityu.edu.hk (H.Z.),
ure 2A), which could be attributed to its ribbon shape possessing a general tendency yanglu@cityu.edu.hk (Y.L.)
to become a cylindrical shape upon heating, so as to reduce the surface area while https://doi.org/10.1016/j.matt.2019.10.003

2 Matter 2, 1–8, March 4, 2020


Please cite this article in press as: Li et al., Thermal Effect and Rayleigh Instability of Ultrathin 4H Hexagonal Gold Nanoribbons, Matter (2019),
https://doi.org/10.1016/j.matt.2019.10.003

Figure 2. Rayleigh Instability and Phase Stabilization of Ultrathin 4H Au NRBs at Moderate Temperature
(A and B) Ultrathin 4H Au NRB before E-beam irradiation (A) and after 15-min E-beam irradiation (B).
(C) Schematic diagrams of the shape evolution of Au NRBs before and after E-beam irradiation.
(D–F) Geometric shape and crystal phase evolutions of another ultrathin 4H Au NRB before (D) and after E-beam irradiation for 15 min (E) and 45 min (F).
Insets in (D) to (F) show the corresponding FFT patterns.

the constant total volume is maintained (like liquid behavior). The geometric evolu-
tion of ultrathin 4H Au NRB after E-beam irradiation is schematically shown in Fig-
ure 2C. As reported previously, surface atom diffusion is the dominant mechanism
for the geometric evolution of Rayleigh instability.37 Considering the decreasing
overall width, it can be speculated that the surface Au atoms would also migrate to-
ward the thickness direction to minimize the surface area during the Rayleigh insta-
bility process. Therefore, the thicknesses, i.e., both the necking part (t1) and bulging
part (t2), of the Au NRB increase after E-beam irradiation (Figure 2C). Figure S1
shows similar geometric evolution of another ultrathin 4H Au NRB under E-beam
irradiation. Figure S1A shows its average width of 13.2 nm, and the 40 -tilted
TEM image in Figure S1B confirms its ribbon shape. After 20 min of irradiation, Ray-
leigh instability obviously occurs with an overall decreased width (Figure S1C) but
increased thickness (Figure S1D), consistent with the aforementioned results (Fig-
ures 2A–2C).

HRTEM was used to analyze the phase stability and atomic-structure evolution of ul-
trathin 4H Au NRB under E-beam irradiation heating. In Figure 2D, the initial ultrathin
Au NRB with 4H phase was confirmed by the HRTEM image and corresponding FFT
pattern. After 15 min of irradiation, Rayleigh instability gradually occurred with
obvious necking appearing, but no phase transition occurred (Figure 2E). When
the irradiation time reached 45 min, the Rayleigh instability became more significant
(Figure 2F). The necking and bulging widths are both considerably smaller than the

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Figure 3. Phase Transition of Ultrathin 4H Au NRB from 4H to FCC at High Temperature


(A) TEM image of the ultrathin 4H Au NRB before MEMS chip-induced heating.
(B–D) Crystal phase evolutions of the ultrathin 4H Au NRB under MEMS chip-induced heating at 800
K for 2 min (B), 4 min (C), and 5 min (D). Insets: (A) Zoom-in HRTEM image of the initial Au NRB in the
dashed white area; (D) high-magnification HRTEM image of the Au NRB in the dashed white area
after 5-min heating (top) and the corresponding FFT pattern from the dashed red area (bottom).

initial width of the Au NRB. Importantly, the 4H phase of Au NRB is still maintained,
as verified by its HRTEM image and the corresponding FFT pattern (Figure 2F).
Video S1 shows the aforementioned evolution process in detail. To confirm the
observed phenomena, we investigated more ultrathin 4H Au NRBs in terms of their
phase stability. Figure S2 shows the results of another two Au NRBs irradiated by
E-beam for 15 min and 30 min, respectively. Similar to the aforementioned results
shown in Figure 2, no phase transition occurred. Therefore, under moderate
E-beam irradiation heating, despite the Rayleigh instability, the ultrathin 4H Au
NRBs do show high phase stability at moderate temperature (<400 K) even over
an extended time period.24–26

We further studied the phase stability of 4H Au NRBs at higher temperature using


MEMS chip-induced heating (Figure 1D). Under the heating rate of 1 K/s, the ultra-
thin 4H Au NRB was quickly heated from 300 to 800 K without E-beam. After the
temperature reached 800 K and stayed constant, the E-beam was turned on to
investigate the evolution of geometric shape and crystal phase of 4H Au NRBs
in TEM. In the beginning the 4H phase of Au NRBs was maintained, which can
be seen from the HRTEM image in Figure 3A, which reveals that the 4H phase is
mostly stable at temperatures below 800 K, despite the geometric Rayleigh
instability (Figure 3). Meanwhile, the 4H phase transformed to FCC phase under
MEMS chip-induced heating at 800 K for 5 min, which was proved by the HRTEM
image and FFT pattern of pure FCC phase along the zone axis [011] (Figure 3D). It
is worth mentioning that the phase transitions of 4H Au NRBs and 2H Ag films from
the metastable hexagonal phases to FCC phase have also been reported earlier
under certain conditions.15,39,40 When heating stopped and the temperature drop-
ped at a rate of 10 K/s, no reversible phase transition from FCC to 4H phases
occurred, as shown in Video S2, which reveals that MEMS heating to high temper-
ature above 800 K could promote the phase transition from the metastable 4H to

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https://doi.org/10.1016/j.matt.2019.10.003

Figure 4. MD Simulations of Phase Evolutions of Ultrathin 4H Au NRBs at Different Temperatures


(A) Schematic illustration of a unit cell of the 4H Au NRB and its top-view crystallographic model.
The close-packed planes along the [001] 4H direction show a characteristic stacking sequence of
‘‘ABCB.’’
(B) Schematic illustration of a unit cell of the FCC Au NRs and its top-view crystallographic model.
(C) MD simulations of thermal effect on ultrathin 4H Au NRB at 600 K.
(D–G) MD simulations of thermal effect on ultrathin 4H Au NRBs at 800 K and different time
durations: (D) 5 ps, (E) 2 ns, (F) 12 ns, and (G) 20 ns. The thickness, width, and length in the model of
Au NRB in MD simulations are 1.3 nm, 9.9 nm, and 38.6 nm, respectively.
(H) The corresponding width evolution as a function of time for the 4H Au NRB being heated at
800 K.

thermodynamically stable FCC phases. However, this kind of phase transition is


irreversible as the temperature falls.

Based on the thermal responses of ultrathin 4H Au NRBs under the two different
heating modes, we can conclude that the 4H crystalline phase is stable enough
to sustain moderate heating, but phase transition from 4H to FCC phases does
occur when the temperature reaches as high as 800 K. To further understand the
temperature-dependent phase transition, we adopted molecular dynamics (MD)
simulations employing the embedded atom method (EAM)41–44 potential to
examine the thermal stability of ultrathin 4H Au NRBs under different tempera-
tures. Au atoms with different phase structures, 4H and FCC phases, were colored
by common neighbor analysis (CNA)44 as shown in Figures 4A and 4B, respec-
tively. First, a 4H Au NRB with thickness of 1.3 nm, width of 9.9 nm, and length
of 38.6 nm was constructed (Figure 4C), and relaxed at a lower temperature to
examine the stability of the 4H Au NRB. It was found that the 4H phase remained
stable within the attainable time scale of MD at temperature below 600 K, which is
consistent with the experimental results under E-beam irradiation-induced heating
(Figures 2D–2F). The temperature was then increased to 800 K (Figure 4D), and the
phase transition from 4H to FCC phases can be observed when the temperature
was maintained at 800 K for 2 ns, as shown in Figure 4E. Further details of this
phase transition are presented in Figure S3 and Video S3, in which the phase

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transition initiates from the edge (the blue dashed area in Figure S3B), which then
continues to expand (Figures S3C–S3F) across the entire cross-section of the Au
NRB. The phase evolutions in the cross-section of the Au NRB, marked by the pur-
ple dashed line as a function of time, are shown in Figures S3G–S3J. Such a phase
transition would continue to expand longitudinally along the length direction of
the NRB, as shown in the left panels and the expanded green region in Figures
4E–4G, eventually leading to geometric Rayleigh instability. These results are
consistent with the experimental results under MEMS heating (Figure 3). Due to
Rayleigh instability, the width of necking regions of Au NRB decreased gradually
while the thickness simultaneously became thicker as illustrated in the left panels,
i.e., the cross-section of Au NRB marked by the purple dashed line, in Figures
4D–4G. The NRB geometric evolution is quantitatively plotted in Figure 4H, which
shows the width change of a heated NRB as a function of simulation time. It is
worth mentioning that these results can be well reproduced by simulating Au
NRBs with larger dimensions at the longer simulation time scale, as demonstrated
in Figure S4 and Video S4. Moreover, MD simulations have been also performed at
higher temperatures, and the further increased temperature could considerably
accelerate the phase transition. As illustrated in Figures S3K and S3L, the phase
transition only occurred partially in the ultrathin 4H Au NRB at 800 K, whereas
the whole NRB would transform nearly completely to the FCC phase when the
temperature was increased to 900 K.

Conclusions
In summary, the geometry and crystal phase evolution of ultrathin 4H Au NRBs under
heating have been systematically investigated by in situ TEM. Under the thermal ef-
fect of E-beam irradiation, Rayleigh instability occurred in ultrathin 4H Au NRBs even
under moderate heating to less than 400 K. When the temperature reached about
800 K via dedicated MEMS chip heating, the phase transition from 4H to FCC phases
occurred in Au NRBs. MD simulations were used to reasonably interpret the afore-
mentioned experimental results. The results indicate that, despite the geometric
Rayleigh instability, the 4H phase can be quite stable upon moderate heating, mak-
ing ultrathin Au nanostructures with unique 4H phase an ideal candidate for various
practical applications in the future.

EXPERIMENTAL PROCEDURES
Materials Synthesis and Characterization
In brief, the ultrathin 4H Au NRBs were synthesized by heating the mixture of
HAuCl4, oleylamine, hexane, and 1,2-dichloropropane in a closed glass vial at
58 C for 16 h. The detailed synthetic information was described in our previous
work.15 The thickness and width of ultrathin 4H Au NRBs are in the range of several
nanometers and several to tens of nanometers, respectively, showing a typical rib-
bon shape.

Investigation of Thermal Stability Using In Situ TEM


Thermal stability of the ultrathin 4H Au NRBs was investigated by means of in situ
TEM.24 The experiment was performed in a JEOL JEM-2100F transmission electron
microscope with a voltage of 200 kV. The thermal effect was introduced through two
kinds of heating modes. The first is E-beam irradiation, whereby the ultrathin 4H Au
NRBs were irradiated under a well-controlled E-beam with a constant current density
of 50 pA/cm2 for a certain period of time, with the thermal effect occurring during
continuous E-beam irradiation. The second is MEMS chip-induced heating by using
a Fusion Select holder from Protochips for higher temperature. The responses of the
thermal effect on the ultrathin 4H Au NRBs were characterized by in situ TEM.

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https://doi.org/10.1016/j.matt.2019.10.003

SUPPLEMENTAL INFORMATION
Supplemental Information can be found online at https://doi.org/10.1016/j.matt.
2019.10.003.

ACKNOWLEDGMENTS
The authors acknowledge financial supports from the Research Grants Council (RGC)
of Hong Kong under GRF project 11209914, and the Natural Science Foundation of
Guangdong Province, China (2018A030313793). H.Z. thanks the support from ITC
via the Hong Kong Branch of the National Precious Metals Material Engineering
Research Center, and a Start-Up Grant from City University of Hong Kong.

AUTHOR CONTRIBUTIONS
Y.L. proposed the research. Z.F. and H.Z. synthesized the samples. P.L. and Y.H. de-
signed and performed the experiments. P.L., Y.H., Z.F., S.X., K.C., F.M., L.G., H.Z.,
and Y.L. analyzed and discussed the experimental results. X.Z. and J.S. performed
the MD simulations. P.L., Y.H., X.Z., Z.F., J.S., H.Z., and Y.L. wrote the manuscript.
All authors contributed to the manuscript.

DECLARATION OF INTERESTS
The authors declare no competing financial interests.

Received: July 21, 2019


Revised: September 30, 2019
Accepted: October 8, 2019
Published: November 6, 2019

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