Letter

Cite This: ACS Energy Lett. 2018, 3, 2823−2828 http://pubs.acs.org/journal/aelccp

Factors that Determine the Length Scale for

Uniform Tinting in Dynamic Windows Based
on Reversible Metal Electrodeposition
Michael T. Strand,† Christopher J. Barile,‡ Tyler S. Hernandez,§ Teresa E. Dayrit,† Luca Bertoluzzi,†
Daniel J. Slotcavage,† and Michael D. McGehee*,†,∥
†
Department of Materials Science and Engineering, Stanford University, Stanford, California 94305, United States
See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.

‡
Department of Chemistry, University of NevadaReno, Reno, Nevada 89557, United States
§
Department of Chemistry, Stanford University, Stanford, California 94305, United States
∥
Downloaded via UNIV OF NEVADA RENO on April 3, 2023 at 05:26:23 (UTC).

Department of Chemical Engineering, University of ColoradoBoulder, Boulder Colorado 80303, United States
*
S Supporting Information

ABSTRACT: Dynamic windows based on reversible metal

electrodeposition are attractive compared to conventional
electrochromics because they can have neutral color, high
contrast, and potentially lower cost, yet they are not nearly
as developed, and the design rules for making them
function at large scale are not presented in the literature.
We model the voltage drops that occur in the transparent
electrodes to get insight on how to obtain uniform
electrodeposition of metals over large area. By optimizing
the surface and density of the Pt nanoparticles used to
nucleate metal growth, we lower the nucleation barrier for
electrodeposition by 70 mV. We show that the growth rate
of the metal films is determined by diffusion rather than reaction kinetics, which makes it possible to achieve uniform film
deposition over a range of potentials from −300 to −700 mV. We demonstrate 100 cm2 dynamic windows that are color-
neutral and tint uniformly from a clear state (>60%) to a dark state (<5%) in less than 1 min.

D ynamic windows that allow electronic control of

visible light and solar heat gain are desirable for
improving energy efficiency in buildings and
automobiles and reducing glare without obstructing views.1−3
Despite decades of research, however, traditional approaches
to dynamic windows have not widely penetrated the market
due to problems with color, cost, speed, and durability.4
Dynamic windows based on reversible metal electrodeposition
(RME) represent an undeveloped class of electrochromic
devices posed to overcome the challenges inherent to existing
technologies. We recently demonstrated dynamic windows
based on the reversible electrodeposition of Bi, Cu, and Ag that
switch uniformly between transparent and opaque states over
thousands of cycles.5,6 We developed transparent electrodes
decorated with Pt nanoparticles that enable uniform electro-
deposition of metal films on the 25 cm2 scale.5 We verified that
dynamic windows using metals can be color-neutral and
require no additional power to be held in the desired optical
state.6 Finally, we proposed that our design allows dynamic
windows to be manufactured at a fraction of the cost of
conventional technologies. In this Letter, we evaluate what is
needed for dynamic windows based on RME to be realized at a
practical scale.
A challenge hindering large-scale RME windows is
associated with the limitations of transparent conductors.
The majority of electrochromic devices use glass coated with
transparent conducting oxides as the conductive electrodes.7
Indium tin oxide (ITO) is the most commonly used
transparent conductor and possesses a resistivity of ∼10−4 Ω·
cm and a visible transmittance greater than 80%.8 The sheet
resistance is typically 10 Ω/sq. The resistivity is 2 orders of
magnitude higher than that of opaque conductors like metals,
and maintaining a uniform current density leaving the ITO
electrodes during electroplating or stripping necessitates a
voltage drop that increases with the electrode area.9 The
voltage distribution can be calculated by integrating Ohm’s
Law over a two-dimensional surface. This calculation yields the
following equation
Received: September 20, 2018
Accepted: October 23, 2018
Published: October 23, 2018

© 2018 American Chemical Society 2823 DOI: 10.1021/acsenergylett.8b01781

ACS Energy Lett. 2018, 3, 2823−2828
ACS Energy Letters Letter

Figure 1. Schematic of a 100 cm2 dynamic window. The device consists of a 100 cm2 Pt-modified ITO working electrode, a Bi−Cu gel
electrolyte, and a semitransparent Cu grid counter electrode mounted to a 100 cm2 glass backing. The device is sealed using 2 mm thick
butyl rubber edge sealant that doubles as an electrode spacer.

Figure 2. (a) Cyclic voltammetry in a Bi−Cu electrolyte comparing bare ITO, an evaporated Pt film [3 nm Pt/3 nm Ti/ITO], and a Pt
nanoparticle array on ITO and (b) corresponding transmission (at 550 nm) versus voltage curves. Measurements were taken versus a Ag/
AgCl reference at a scan rate of 20 mV/s.

Jρ may be required for sufficient current to travel across sizable

ΔV = (L2 − x 2)(L2 − y 2 )
2t (1)
where J is the current density, ρ is the resistivity, t is the film
thickness, L is the electrode length, and x and y are positions
on the electrode surface defined by a Cartesian coordinate
system with the origin at the corner of the electrode (a detailed
derivation is presented in the Supporting Information). Figure
1 shows a schematic view of a 100 cm2 dynamic window and
the simulated voltage distribution across an ITO electrode with
a sheet resistance of 10 Ω/sq using the maximum current
density observed experimentally in a device that switches from
T = 60% to 10% in 30 s. As shown, these devices must tolerate
a 0.3 V difference from edge to center. Large-scale RME
windows, then, must be engineered with a tolerance to the
voltage drop across the transparent electrodes to maintain
optical uniformity during device operation.
The devices with the best performance to date use aqueous
electrolytes because metal salts have high solubility and
dissociation constants in water, and thus, water-based electro-
lytes benefit from relatively low deposition overpotentials.10
However, undesired side reactions like hydrogen evolution set
strict limits on the potentials that may be applied in devices.
This limit poses a challenge at scale where higher potentials
2824
electrodes. The ideal electrodes will enable uniform nucleation
and growth of metal films over the potential range set by side
reactions inherent to the electrolyte and the voltage drop
inherent to transparent conductors.
In this Letter, we investigate the nucleation and growth
kinetics in an aqueous electrolyte based on the reversible
deposition of Bi and Cu and identify design criteria for
achieving uniform deposition at scale. We improve upon our Pt
nanoparticle seed layer design and demonstrate electrodes that
exhibit a 2.5× improvement in contrast ratio at a fixed voltage
sweep and a 70 mV reduction in deposition overpotential
compared to our previous work.5,6 We show that film growth
in our system is diffusion-limited and that enhanced electrodes
enable uniform switching curves over a 400 mV potential
range. Thus, we verify that lowering the nucleation barrier (i.e.,
deposition overpotential) and achieving a high nucleation
density allow us to deposit uniform metallic films over 100 cm2
electrodes, despite the significant voltage drop. Finally, we
demonstrate 100 cm2 dynamic windows that switch uniformly
from a clear state (>60% transmission) to an opaque state
(<5% transmission) in less than 1 min.
Electrode Morphology and Nucleation. In RME-based dynamic
windows, the working electrode serves two primary functions:
DOI: 10.1021/acsenergylett.8b01781
ACS Energy Lett. 2018, 3, 2823−2828
ACS Energy Letters Letter

Figure 3. SEM images of bare ITO (left), the evaporated Pt film [3 nm Pt/3 nm Ti/ITO] (center), and the Pt nanoparticle array on ITO
(right). The “white” particles in the image on the right are the 3 nm Pt nanoparticles.

Figure 4. Transmission versus time curves for switching at a series of deposition voltages. Each set of curves represents electrodeposition at
different voltages from −200 to −700 mV. Deposition was performed for 30 s followed by a 90 s stripping sequence at +800 mV. The Pt-
modified ITO allows facile nucleation of metal electrodeposits and thus uniform transmission change over a wide potential window.

(i) as a source of electrons to reduce solvated metal ions to
their elemental form and (ii) as a scaffold for metal nucleation
and growth. The working electrode must be transparent,
conductive, and inert and must promote uniform and
reversible electrocrystallization of metal films. Transparent
conducting oxides like ITO and fluorine-doped tin oxide
(FTO) satisfy the first three requirements; however, direct
electroplating onto transparent conductive oxides is difficult.11
The poor wettability and heterogeneous surface chemistry of
ITO, for example, leads to a large excess energy for metal
nucleation and nonuniform deposition.12 Pt, in contrast, is an
excellent template for RME. Therefore, modifying ITO
electrodes with Pt offers a pathway for fabricating high-
performing electrodes.
Figure 2a shows cyclic voltammograms (CVs) in a Bi−Cu
aqueous electrolyte on a bare ITO surface, an ITO electrode
coated with a 3 nm thick Pt film that was thermally evaporated,
and an ITO electrode coated with an array of Pt nanoparticles
anchored by a self-assembled monolayer of 3-mercaptopro-
pionic acid (a thiol-terminated surface modifier). The bare
ITO and the evaporated Pt film represent two surface
extremes, while the Pt nanoparticle array combines the
beneficial properties of both materials (e.g., high transparency
and high catalytic activity). Both surfaces with Pt show a + 70
mV shift for the onset potential for metal electrodeposition.
This result confirms that Pt surfaces offer a lower overpotential
for nucleation compared to ITO. Figure 2b shows correspond-
2825
ing transmission versus voltage curves measured in a
spectroelectrochemical half-cell during the CV experiments.
The Pt nanoparticle array yields a 75% contrast ratio over one
CV scan compared to 40% for the bare ITO and the
evaporated Pt film. This improved contrast ratio with Pt occurs
because the Pt nanoparticles act as preferred nucleation sites
and enable uniform nucleation and growth of metal electro-
deposits without sacrificing any transmission in the transparent
state. While the evaporated Pt film also exhibits a lowered
nucleation barrier, the maximum transmission is limited to
45% (at 550 nm) because the continuous Pt film along with
the nontransparent Ti adhesion layer that is necessary to
prevent the Pt film from delaminating from the ITO surface
reflects and absorbs more light than an array of Pt
nanoparticles.13 SEM images demonstrate that the evaporated
Pt film displays a similar morphology to the bare ITO surface
(Figure 3). The “bright” particles on the micrograph of the Pt
nanoparticle array are the 3 nm Pt nanoparticles used, and the
particle surface density is about 8000 particles/μm.2
Overcoming Electrode Voltage Drop. While lab-size prototypes
with a 25 cm2 active area demonstrate impressive performance,
significant challenges arise when increasing the size of
electrochromic devices, particularly due to nonuniform voltage
distribution across the electrode surfaces. The current density
required for device operation and the sheet resistance of the
transparent electrodes set the voltage drop inherent to dynamic
windows. As shown in Figure 1 and calculated in eq 1, there is
DOI: 10.1021/acsenergylett.8b01781
ACS Energy Lett. 2018, 3, 2823−2828
ACS Energy Letters
Figure 5. Transmission measurements at the device edge and center and photographs of 100 cm2 dynamic windows made with a Pt-modified
ITO electrode (top) and a bare ITO electrode (bottom). The devices were switched under an applied bias of −600 mV for 60 s.
Transmission was measured at 550 nm. A coin with 17.91 mm diameter is shown for scale.
a 0.3 V drop from edge to center for a 100 cm2 dynamic
window using the experimental conditions in our system. This
voltage drop, of course, presents a significant challenge when
uniform deposition of metallic films is critical to device
operation. However, dynamic windows based on reversible
electrodeposition have unique current transient properties.
A typical current transient in a RME device, analogous to a
standard electroplating experiment under Cottrell conditions,
is an exponential decay (Figure S2). The large, initial current
density is followed by a rapid decay because nanoscale metallic
nuclei form on the electrode surface at early times, followed by
a decay in current as the metallic clusters coalesce and the
concentration of active ions near the surface is depleted (i.e.,
the electrodeposition becomes diffusion-limited).14 With
sufficient potential for nucleation to occur everywhere, uniform
growth of the metal film is possible once diffusion takes over.
Of course, promoting nucleation over the wide range of
voltages present during the first few seconds is essential to
achieving uniformity at a large scale.
The key to solving the voltage drop challenge is controlling
the nucleation process by using an inert nanoparticle seed
layer. By increasing the nanoparticle surface density, we
demonstrate increased current density at a fixed voltage sweep
and a corresponding improvement in contrast ratio (Figures S3
and S4). We show that a 250 °C anneal effectively removes
surfactant molecules from the nanoparticle surfaces and yields
the catalytic properties of a continuous Pt film (Figure S5). We
attribute the +70 mV shift in onset potential compared to our
previous work (Figure 2a) to the removal of surfactant
molecules. The Pt nanoparticle nucleation layer developed in
this study exhibits significant performance improvement
compared to surface modifications presented in previous
work.5,6 Most importantly, the Pt nanoparticle array enables
uniform transmission modulation over a wide potential
2826
Letter
window. This result demonstrates a route to overcoming the
problems with nonuniform voltage distribution across the
electrode surface. Despite the variance in electrostatic potential
across the surface, the diffusion-limited nature of the
deposition process enables uniform transmission−time rela-
tionships because the concentration gradient becomes uniform
across the electrode area.
Figure 4 shows transmission versus time curves for a bare
ITO electrode and an ITO electrode modified with a Pt
nanoparticle array. We performed measurements in a
spectroelectrochemical half-cell during potentiostatic deposi-
tion and stripping sequences at a series of applied voltages
ranging from −200 to −700 mV. The difference between the
two electrodes is apparent in comparing the two curves at
lower applied voltages. At an applied voltage of −200 mV, for
example, negligible transmission change (and hence minimal
metal deposition) is observed on the bare ITO electrode, while
transmission through the Pt-modified electrode decreases
below 40% after 30 s. This result is expected because the Pt
nanoparticles act as catalysts for nucleation of metal deposits
and lower the onset potential for electrodeposition, as shown
in Figure 2. As the overpotential is increased, the transmission
versus time relationship for the two electrodes saturates
because there is sufficient energy available for metal to nucleate
on either surface (Pt nanoparticle or ITO). The nucleation in
this system is governed by a three-dimensional instantaneous
nucleation model, followed by diffusion-limited growth as
described by the Cottrell equation (Figure S7). The
implication of the growth being diffusion-limited is that it is
possible to achieve even transmission change in a window
despite a nonuniform electrostatic potential across the
electrode surface.
100 cm2 Devices with Uniform Tinting. With indication that
uniform switching is possible on a larger scale (i.e., tolerance of
DOI: 10.1021/acsenergylett.8b01781
ACS Energy Lett. 2018, 3, 2823−2828
ACS Energy Letters
the 0.3 V drop calculated above), we fabricated dynamic
windows with an active area of 100 cm2. The devices consist of
a Pt-modified ITO working electrode, a Bi−Cu aqueous gel
electrolyte, and a semitransparent copper mesh counter
electrode to provide a uniform source of metal ions (see
Figure 1). We sealed the devices using 2 mm thick butyl rubber
edge sealant that doubles as an electrode spacer. Figure 5
shows transmission versus time curves and photographs of two
devices: one constructed with the Pt-modified electrode
developed in this work and one with a bare ITO electrode.
Transmission (at 550 nm) was measured at the device edge
and the center during a 60 s tinting sequence under an applied
potential of −600 mV. The potential of −600 mV was chosen
based on the onset potential for hydrogen adsorption on the
Pt-modified surface (Figure S8). Complete optical properties
measured using integrating sphere measurements are shown in
Figure S9. The measured transmission through the device with
a Pt nanoparticle array is relatively uniform from edge to center
(±5%), showing little evidence of “irising” or uneven switching
due to the voltage drop. The deposited metal is color-neutral,
and the haze through the device is less than 6%. The bare ITO
device, in contrast, is unacceptably nonuniform in the dark
state. Therefore, the electrodes developed in this work yield a
robust platform for uniform switching under nonuniform
potential conditions.
In this Letter, we demonstrated large-area dynamic windows
based on RME. We derived the voltage distribution across the
electrode in eq 1 and modeled the voltage drop that must be
tolerated in RME devices. We tested electrodes modified with
Pt seed layers to determine the optimal coating for facile
nucleation of metal deposits. We showed that the rapid metal
nucleation followed by diffusion-limited metal growth in our
system enabled uniform transmission change over a 400 mV
potential range. Finally, we successfully fabricated 100 cm2
dynamic windows based on the reversible electrodeposition of
Bi and Cu that tint uniformly from a clear state (>60%
transmission) to a dark state (<5% transmission) in less than 1
min.
Several challenges remain before RME windows achieve
commercial success. While this work is a critical step for
solving challenges with nonuniformity on the working
electrode surface, the counter electrode limits the durability
of the devices. We manage 300 cycles with no signs of
degradation, but after some time, nonuniform growth occurs
on the Cu mesh counter electrode, which leads to a decay in
maximum transmission (Figure S10). This growth occurs
because we are repeatedly reducing and oxidizing the copper
counter electrode over many cycles. Further, ions from the
counter electrode may leach into the system over time and
increase the overall concentration in the electrolyte. These
effects are limiting factors in surpassing the 1000 stable cycles
that we demonstrated for this electrolytic system in previous
work.6 Thus, future work must target a transparent and inert
counter electrode material to achieve the durability needed for
the 25 year lifetime expected for commercial building windows.
Further scalability may be achieved by relaxing the voltage
drop in RME devices. Equation 1 predicts that a decrease in
current density and electrode resistivity would lower the
potential difference from edge to center. Lower current density
could be achieved by improving the coloration efficiency
(defined as the change in optical density per unit charge) of
metal-based systems. Leveling agents used in electroplating
baths could yield a denser metal film, which would allow
2827
Letter
greater contrast for the same amount of charge passed (or
metal ions reduced) but could make the film smoother and
more reflective, which might not be appealing in all
applications.10 Transparent conductive electrodes based on
meshes of metal lines with width less than 10 μms can have
transmission greater than 95% and sheet resistance < 1 Ω/sq.15
They could be used to further mitigate the nonuniform
potential distribution in large-scale dynamic windows. Efforts
involving the proposed electrolytic and electrode improve-
ments could bring RME-based window technology another
step closer to commercial viability.
■ EXPERIMENTAL SECTION
Pt-Modif ied Electrodes. Pt nanoparticles with average diameters
of 3 nm dispersed in water were purchased from Sigma-
Aldrich. For working electrodes modified with a SAM of Pt
nanoparticles, ITO-coated glass substrates (10 Ω/, Xin Yan)
were immersed in an ethanolic solution of 10 mM 3-
mercaptopropionic acid for 24 h. Next, the substrates were
thoroughly rinsed with ethanol and deionized H2O before
immersing them in a Pt nanoparticle suspension for 24 h. After
Pt immersion, the substrates were rinsed with water and dried
with a N2 gun. The substrates were then annealed at 250 °C on
a hot plate for 30 min. For working electrodes modified with a
Pt film, 3 nm of Ti was evaporated on ITO as an adhesion
layer, followed by 3 nm of evaporated Pt. For three-electrode
experiments, electrochemical potentials were measured and
reported using a Biologic SP-150 potentiostat with respect to a
“no-leak” Ag/AgCl (3 M KCl) reference electrode.
Window Assembly. Dynamic windows were constructed in
two-electrode configurations. Pt-modified or bare ITO (100
cm2) on glass served as working electrodes. Transparent
copper mesh (TWP, Inc., wire diameter: 0.0012 in.) served as
both the counter and reference electrodes. The Bi−Cu gel
electrolyte was prepared according to our previous work.6
Butyl rubber edge sealant (Quanex, 2 mm) served as an
electrode spacer and as containment for the electrolyte.
Characterization. Transmission spectra recorded were
measured with an Ocean Optics USB2000 spectrometer
coupled with an Ocean Optics halogen light source (HL-
2000-FHSA). SEM images were obtained using an FEI
Magellan 400 XHR scanning electron microscope operated
at an accelerating voltage of 10 kV.
A detailed experimental section can be found in the
Supporting Information.
■
ASSOCIATED CONTENT
*
S Supporting Information
The Supporting Information is available free of charge on the
ACS Publications website at DOI: 10.1021/acsenergy-
lett.8b01781.
Derivation of the voltage drop in a square resistor,
Figures S1−S12, showing a transmission−time plot,
chronoamperometry transients, cyclic voltammograms,
SEM images, XPS spectra, linear scan voltammograms,
and transmission, absorbance, and reflectance plots, and
an experimental section with expanded detail (PDF)
■
AUTHOR INFORMATION
Corresponding Author
*E-mail: michael.mcgehee@colorado.edu.
DOI: 10.1021/acsenergylett.8b01781
ACS Energy Lett. 2018, 3, 2823−2828
ACS Energy Letters Letter

ORCID (14) Radisic, A.; Ross, F. M.; Searson, P. C. In Situ Study of the
Michael T. Strand: 0000-0002-2144-2735 Growth Kinetics of Individual Island Electrodeposition of Copper. J.
Phys. Chem. B 2006, 110 (15), 7862−7868.
Christopher J. Barile: 0000-0002-4893-9506 (15) Ellmer, K. Past Achievements and Future Challenges in the
Tyler S. Hernandez: 0000-0003-1885-4656 Development of Optically Transparent Electrodes. Nat. Photonics
Michael D. McGehee: 0000-0001-9609-9030 2012, 6 (12), 809−817.
Notes
The authors declare no competing financial interest.

■ ACKNOWLEDGMENTS
This research was funded by the U.S. Department of Energy
(DOE) under DE-EE0008226. Part of this work was
performed at the Stanford Nano Shared Facilities (SNSF),
supported by the National Science Foundation under Award
ECCS-1542152. M.T.S. and T.S.H. acknowledge financial
support of National Science Foundation Graduate Research
Fellowships (No. NSF DGE-1656518). M.T.S. also acknowl-
edges financial support of a Stanford Graduate Fellowship.
C.J.B. acknowledges Research & Innovation at the University
of Nevada, Reno.

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2828 DOI: 10.1021/acsenergylett.8b01781

ACS Energy Lett. 2018, 3, 2823−2828