Nanolab 600 dual beam

Cross sections of the samples were prepared by FIB and the SEM cross section images were taken using a FEI Helios NanoLab600 Dual Beam FIB-SEM at a 5 kV accelerating voltage.

For SEM studies using a Helios Nanolab 600 Dual Beam (FEI, OR), the shells were coated with an ultra-thin carbon layer to reduce charging effects before imaging. Cross-sectional samples and TEM samples were prepared using FIB milling with the same system. Final polishing using the ion beam at 2 kV was critical for obtaining a clean surface with a minimum amount of damage. TEM imaging with typical bright-field, dark-field and selected-area electron diffraction techniques was carried out using a JEOL 2011 operated at 120 kV. High-resolution TEM imaging was performed on a JEOL 2010 F operated at 200 kV.
AFM imaging was performed with a Digital Instruments Multimode SPM IIIA (Veeco, CA) (NANOSENSORS Si TMAFM cantilevers, PPP-NCHR-10).

The triangular lattices of circular holes are patterned on the top of the first metallic layer of the MIM structure via a one-step focused ion beam milling (FEI Helios Nanolab 600 DualBeam) with a gallium ion current of 9.7 pA and an accelerating voltage of 30 KeV. Then a thin layer of PMMA (950-A2 in anisole, Michrochem), a commonly used positive electron-beam resist, is spin-coated (2,000 rounds per min) on top of the fabricated nanostructures. We choose PMMA in the present work due to its chemical and mechanical stability and the accurate control of the thickness via control of the spin speed or molecule concentration used. The thickness of the coated PMMA polymer layer is also determined through X-ray reflectivity (Philips X’Pert-MRD) measurement.

The focused ion beam of a FEI Helios NanoLab 600 DualBeam (FIB/SEM) was used to cut at an angle into the surface of a baked and cooled down (see Fabrication of DSSCs) photoanode. Using the electron beam, images were taken of the surfaces with varying magnifications.

The morphologies
of the Cu powder samples and of the top surface of the cured ICA samples
(filler dispersion and microstructure) were characterized using a
Zeiss 1530VP field emission gun scanning electron microscope (FEG-SEM).
Elemental mapping was also conducted within the FEG-SEM using energy-dispersive
X-ray spectroscopy (EDS). Samples of Cu powder and ICAs printed on
glass were attached to carbon adhesive tape mounted on SEM stubs and
coated with a thin layer of gold/palladium (Au/Pd) alloy (80/20) using
a Quorum Q150R S sputter coater. The Au/Pd coating applied was sufficiently
thin to not be recognized in the images. The cross-sectional microstructures
of the ICAs were prepared and characterized using a focused ion beam
(FIB-SEM) system (FEI Nanolab 600 Dual Beam). A platinum (Pt) layer
(∼2 μm thick) was deposited on the surface of the sample
prior to FIB milling to preserve the outermost surface.
A standard
lift-out procedure using FIB-SEM was followed to prepare the lamella
for TEM to achieve a thickness of ∼200 nm. The nanostructure
of the ICA sample sections was then studied using an FEI Tecnai F20
scanning transmission electron microscope (STEM) equipped with Oxford
Instruments energy-dispersive X-ray spectroscopy (EDS) with a windowless
detector (X-Max^N 80 TLE).