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General rights Copyright and moral rights for the publications made accessible in the public portal are retained by the authors and/or other copyright owners and it is a condition of accessing publications that users recognise and abide by the legal requirements associated with these rights.
Users may download and print one copy of any publication from the public portal for the purpose of private study or research.
You may not further distribute the material or use it for any profit-making activity or commercial gain
You may freely distribute the URL identifying the publication in the public portal If you believe that this document breaches copyright please contact us providing details, and we will remove access to the work immediately and investigate your claim.
Downloaded from orbit.dtu.dk on: Dec 26, 2020
Bottom-Up Nanofabrication of Supported Noble Metal Alloy Nanoparticle Arrays forPlasmonics
Nugroho, Ferry A. A.; Iandolo, Beniamino; Wagner, Jakob Birkedal; Langhammer, Christoph
Published in:A C S Nano
Link to article, DOI:10.1021/acsnano.5b08057
Publication date:2016
Document VersionPeer reviewed version
Link back to DTU Orbit
Citation (APA):Nugroho, F. A. A., Iandolo, B., Wagner, J. B., & Langhammer, C. (2016). Bottom-Up Nanofabrication ofSupported Noble Metal Alloy Nanoparticle Arrays for Plasmonics. A C S Nano, 10(2), 2871-2879.https://doi.org/10.1021/acsnano.5b08057
The manuscript was written through contributions of all authors. All authors have given approval
to the final version of the manuscript. ‡These authors contributed equally.
ACKNOWLEDGMENTS
We acknowledge financial support from the Swedish Foundation for Strategic Research
Framework Program RMA11-0037 (FAAN & CL), the ERC Starting Grant project SINCAT
(CL), the Swedish Research Council (CL), and the Knut and Alice Wallenberg Stiftelse for their
support of the µ-fab cleanroom infrastructure in Sweden. The research leading to these results
has also received funding from the People Programme (Marie Curie Actions) of the European
30
Union's Seventh Framework Programme (FP7/2007-2013) under REA grant agreement n°
609405 (COFUNDPostdocDTU) (BI).
31
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TOC Figure
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Supporting Information
Bottom-Up Nanofabrication of Supported Noble Metal Alloy Nanoparticle Arrays for Plasmonics
Ferry A. A. Nugroho*,‡,1, Beniamino Iandolo‡,2, Jakob B. Wagner2 and Christoph Langhammer*,1
1 Department of Physics, Chalmers University of Technology, 412 96 Göteborg, Sweden
2 Center for Electron Nanoscopy, Technical University of Denmark, 2800, Kongens Lyngby, Denmark
Scheme S1. The geometrical considerations for alloy composition determination for the case of a tapered cone. Each metal constituent layer (𝑀𝑀𝑖𝑖 , 𝑖𝑖 = 1,2,3 … ,𝑛𝑛) is defined by its diameter (𝑑𝑑𝑖𝑖) and height (ℎ𝑖𝑖). However, as described in the text below, the alloy proportions are dictated solely by the thickness of each layer, given the total height (ℎ), base diameter (𝑑𝑑1) and taper angle (𝛼𝛼).
The atomic composition of the alloy nanoparticles is controlled by varying the volume of their constituent layers. As discussed in the main text, material deposition through a mask creates a tapered structure,1,2 as sketched in Scheme S1. The volume of a tapered cone (𝑉𝑉tc) is known as:
𝑉𝑉tc = 112𝜋𝜋ℎtc �3𝑑𝑑𝑡𝑡𝑡𝑡2 − 6ℎtc 𝑑𝑑𝑡𝑡𝑡𝑡
tan𝛼𝛼+ 4ℎtc
2
tan2𝛼𝛼� (1)
where 𝛼𝛼, 𝑑𝑑tc and ℎtc are the cone’s taper angle, diameter and height, respectively. Hence a general formula for each constituent layer with diameter 𝑑𝑑𝑖𝑖 and height ℎ𝑖𝑖 (Scheme S1) is:
𝑉𝑉i = 112𝜋𝜋ℎi �3𝑑𝑑𝑖𝑖2 − 6ℎi 𝑑𝑑𝑖𝑖
tan𝛼𝛼+ 4ℎi
2
tan2𝛼𝛼�. (2)
However, from the schematic it is clear that each constituent diameter is related to the height and the diameter of the prior constituent(s) as
𝑑𝑑i = 𝑑𝑑i−1 − 2 ℎ𝑖𝑖−1tan𝛼𝛼
, (3)
which in the end can be expressed as a function of the base diameter 𝑑𝑑1
𝑑𝑑i = 𝑑𝑑1 − 2 (ℎ𝑖𝑖−1+ℎ𝑖𝑖−2+⋯+ℎ1)tan𝛼𝛼
. (4)
Furthermore, the height of each constituent layer ℎ𝑖𝑖 is related to each other as:
ℎ1 + ℎ2 + ⋯+ ℎi = ℎ (5)
By substituting equation 4 and 5 into equation 2, the layer volume can be expressed as a function of taper angle, base diameter and total height.
2
Knowing the volume of the respective constituent layers, it is then straightforward to define the number of atoms in each layer (in other words, the number of atoms for each metal) as:
𝑛𝑛i = 𝜌𝜌𝑖𝑖𝑉𝑉𝑖𝑖𝑀𝑀𝑖𝑖
𝑁𝑁𝐴𝐴 (6)
where ρ, M, and NA are the density, molar mass and Avogadro number, respectively.
And lastly their atomic percentage can be determined,
𝑎𝑎𝑎𝑎. %𝑖𝑖 = 𝑛𝑛𝑖𝑖∑ 𝑛𝑛𝑗𝑗𝑛𝑛𝑗𝑗=1
(7)
For our work, we fabricated the alloy nanoparticles with 190 nm diameter and 25 nm height by depositing the Au layer first. The angle α will be material dependent. In our case, we have estimated α to be ~ 60° for previous work.3 Knowing all these parameters, we can plot the Au thickness required for any desired AuAg, AuCu and AuPd compositions, as shown in Figure S1.
Figure S1. Au content for different Au layer thicknesses in binary alloy systems AuAg, AuCu and AuPd with 190 nm diameter, 25 nm height and 60o taper angle. The relation holds true if the Au layer is deposited first.
3
2. Plasmonic Response of Layered Nanostructures Prior to Annealing
Figure S2. Plasmonic response of unalloyed layered of (a) AuAg, (b) AuCu and (c) AuPd nanodisks with different layer thicknesses for the intended alloy compositions (cf. Figure S1).
3. SEM/EDS Analysis
Table S1. SEM/EDS analysis of the binary alloy AuAg, AuCu and AuPd compositions.
Table S2. SEM/EDS analysis of the ternary alloy AuAgPd composition.
Nominal Elemental Content (at. %) Measured Elemental Content (at. %) Au Ag Pd Au Ag Pd 33 34 33 32.80 ± 0.50 33.20 ± 0.30 34.00 ± 0.40
4
4. TEM EDS Elemental Maps of AuAg 10:90 and 90:10 Alloy
Figure S3. EDS elemental maps of AuAg of (a) 10:90 and (b) 90:10 composition, respectively. The right panels reveal homogenous distribution of both alloy constituents throughout the particles. The left panels show high-angular annular dark field (HAADF) STEM images of representative single alloy nanoparticles and a corresponding elemental profile acquired across them (red dashed lines). These results together with the one from 50:50 AuAg alloy (cf. Figure 1c in the main text) demonstrate a reliable fabrication of homogenous alloy nanoparticles across the entire range of compositions considered in our work.
5. Shape Preservation upon Annealing
Figure S4. SEM images of AuAg 50:50 nanodisk arrays before (left) and after (right) annealing at 773 K for 24 h, shown together with their corresponding size distributions. The observed distribution of the unannealed nanodisks is inherited from the polydispersity of the used colloidal particles during fabrication. This size distribution is basically preserved after annealing. Even though the overall diameter slightly shrinks, excellent shape preservation is observed after annealing. Scale bars are 1 μm.
5
Figure S5. SEM images of AuAg 50:50 nanoellipse arrays before (left) and after (right) annealing at 773 K for 24 h, shown together with their corresponding size distributions. It becomes clear that the anticipated structural anisotropy of the ellipses is retained after annealing. In fact, the anisotropy is even slightly enhanced, as it can be seen by comparing the aspect ratio between ellipse long and short axis. At the same time, a slight change of shape (from more elliptical to more rod-like) is observed, however, without detrimental consequences for the overall purpose of the structure, that is, to exhibit distinct structural anisotropy. Scale bars are 1 μm.
6. Hydrogen Sensing
Figure S6. Hydrogen absorption and desorption isotherms of AuPd 30:70 (blue) and 25:75 (green) binary alloy systems. The result is similar to the Figure 7 in the main text but with peak position change (Δλpeak) as readout. The AuPd 25:75 data is adapted from Wadell et al.3
6
7. References
(1) Fredriksson, H.; Alaverdyan, Y.; Dmitriev, A.; Langhammer, C.; Sutherland, D. S.; Zäch, M.; Kasemo, B. Hole–Mask Colloidal Lithography. Adv. Mater. 2007, 19, 4297–4302.
(2) Syrenova, S.; Wadell, C.; Langhammer, C. Shrinking-Hole Colloidal Lithography: Self-Aligned Nanofabrication of Complex Plasmonic Nanoantennas. Nano Lett. 2014, 14, 2655–2663.
(3) Wadell, C.; Nugroho, F. A. A.; Lidström, E.; Iandolo, B.; Wagner, J. B.; Langhammer, C. Hysteresis-Free Nanoplasmonic Pd-Au Alloy Hydrogen Sensors. Nano Lett. 2015, 15, 3563–3570.