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57 protocols using nvision 40

1

Perovskite Film Preparation and Aging

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The 0.5 M perovskite solution was prepared by dissolving the powders methylammonium bromide (CH3NH3Br; Dyesol), formamidinium iodide (CH(NH2)2I; Sigma Aldrich), lead(II) iodide (PbI2; Sigma Aldrich) and lead bromide (PbBr2; Alfa Aesar) in a mixed solvent of N,N-dimethylformamide (DMF; Sigma Aldrich) and dimethylsulfoxide (DMSO; Sigma Aldrich) at a volume ratio of 4:1. The spray deposition was conducted inside a custom-made chamber in a normal atmosphere. Nitrogen with a pressure of 2 bar was applied as a carrier gas, and the substrate was placed on a heating stage with a temperature of 100 °C. To obtain the defined dimensions, focused ion beam (FIB; Zeiss NVision 40) milling was carried out on the spray-cast perovskite film at a high milling current of 1.6 nA and high acceleration voltage of 30 kV (Ga+ ion source). Afterwards, the samples were stored at ambient conditions for around 30 days without special encapsulations to allow for moisture induced aging.
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2

Ag NWs Bonding on Au Substrate

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A sputtered Au electrode on a Si substrate was cleaned and used for bonding the Ag NWs onto a Au substrate. Ag NWs with a pentagonal cross section were synthesized using a previously described method [19 (link)]. A polyvinylpyrrolidone (PVP) organic layer with a thickness of 2–3 nm was fabricated on the surface of Ag NWs. Their diameter was approximately 100–300 nm. A nanoindenter (Hysitron TriboIndenter) with a Berkovich tip (diamond) and visualization system were employed for both the locating and bonding processes. The bonding forces had a range of 200–500 µN, with a loading speed of 20 µN s−1. The morphologies and microstructures were characterized using scanning electron microscopy (SEM, LEO 1530, Zeiss). A focused ion beam (FIB, NVision 40, Zeiss) was used to slice the Ag–Au bonding interface, which was also observed using a high-resolution transmission electron microscope (HRTEM, JEOL 2010) equipped with an energy-dispersive X-ray spectroscope (EDS).
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3

FIB-SEM Sample Preparation for TEM Analysis

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Cross-sectional, electron transparent samples were prepared using conventional focused ion beam (FIB) milling procedures FIB SEM (NVision 40, Zeiss, Jena, Germany) equipped with a Schottky field emission gun. Firstly, a thin layer of tungsten was deposited over the site of interest to prevent ion beam damage from the bulk milling procedure. At 30 keV, trenches around the site were milled using Ga+ ions. The lamella was then attached to a micromanipulator, detached from the bulk sample, attached to a copper grid and milled to electron transparency with a 10 keV ion beam [25 (link),32 (link)].
TEM (Titan 80-300LB, FEI, Eindhoven, The Netherlands) operated at 300 keV was used for imaging, generating electron diffraction patterns of the samples. High-angle annular dark-field scanning transmission electron microscopy (HAADF STEM) was used for imaging to visualize compositional contrast.
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4

Fabrication of Micro-Coils with Soft Magnetic Wires

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First, a photo patterned SU8 mask is applied on a Si-wafer. A 40 nm Al2O3 layer is deposited on the opposite face by atomic layer deposition (ALD) in a FlexAL (Oxford Instruments Plasma Technology). The wafer undergoes a silanization process to promote the adhesion of the polymers. Afterwards, four polymer layers are photo-patterned successively on top of the Al2O3: sacrificial layer, polyimide, hydrogel, and polyimide. On top of the polymer stack Ti–Cu–Ti (5–300–5 nm) layers are sputtered (with a HZM-P4, Von Ardenne) and photo patterned by a lift-off process (with AZ 5214E, MicroChemicals). Afterwards, an aperture is etched on the Si-wafer with 0.0225 or 0.04 mm2 area (depending on the design) with the Bosch Process (BP) in a PlasmaPro 100 ICP (Oxford Instruments Plasma Technology). The wafer is now diced into single samples in a SS10 (ACCRETECH (Europe)) dicing machine. Finally, the micro-coils are self-assembled, the soft magnetic wire is inserted and fixed in the coils, and then modified by Focussed Ion Beam (FIB) milling. This step was done in a CrossBeam XB 1540 (Zeiss) and an NVision40 (Zeiss). In both devices Ga+ ions of 30 kV were used for milling with ion currents up to some 10 nA. The devices were also used for SEM imaging.
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5

Cross-Sectional Imaging of FIB-Prepared Samples

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Secondary electron SEM images of FIB-prepared cross sections (Fig. 3a, b) were obtained in a Zeiss NVision 40 (Zeiss, Germany). The procedure for cross-sectional imaging involved the deposition of a carbon protection layer, first with the electron beam and then with a gallium beam, on Au-coated layer stacks. Cross-sections were prepared with a gallium ion beam current of 3–1.5 nA (at an acceleration voltage of 30 kV). In-lens secondary electron SEM images were acquired with a beam voltage of 2 kV.
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6

Characterization of Au Nanostructures

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A full morphological, optical and magneto-optical (in T-MOKE configuration) characterization of the resulting Au nanostructures prepared onto solid transparent substrates has been performed.
The morphology and size of the Au nanoparticles were characterized by Scanning Electron Microscopy (SEM), by using a Zeiss NVISION 40 dual-beam Focused Ion Beam machine, equipped with a high resolution SEM Gemini column.
The optical absorption of the Au nanoparticle deposited onto glass substrates was characterized by a Cary500 UV-visible spectrophotometer. Investigation of the effect of thermal annealing on the nanoparticle optical properties was performed by measuring the absorption spectra in the UV-VIS spectral range for different samples at increasing annealing time.
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7

Comprehensive Perovskite Film Characterization

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The XRD measurements were performed with a Bruker D8 Advance diffractometer (CuKα, λ = 1.5406 Å) in the range of 2θ = 3–35° with 0.02° step and 0.1 s step time for perovskite films. The morphology of the films was investigated using Carl Zeiss NVision 40 field-emission scanning electron microscope with EDX detector (Oxford instruments). For cross-section observations, the samples were coated with an ultrathin (<10 nm) layer of Cr to avoid sample charging. The IR spectra of the as-grown Phase-1 crystals were recorded in the attenuated total reflection mode in spectral range 400–4000 cm−1 with a resolution of 4 cm−1 on IR Fourier spectrometer Perkin Elmer Spectrum 65. For each spectrum as well as for the background, 128 scans were averaged.
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8

Atom Probe Tomography of Ge/InAlAs Nanocomposite

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APT specimens were prepared by standard focused ion beam (FIB) lift-out procedures. Using a Zeiss NVision 40 dual beam SEM/FIB (Ga+) equipped with an Omniprobe micromanipulator, sections of the Ge/InAlAs nanocomposite were attached to prefabricated micro tip coupons. Individual needle-shaped APT specimens were then fabricated using FIB annular milling at an accelerating voltage of 30 keV, followed by final sharpening and cleanup with an accelerating voltage of 5 kV. Finished specimens had a tip radius-of-curvature of ∼30 nm, and a shank half-angle of ∼18 degrees, as measured by SEM. APT was performed using a Cameca LEAP 4,000 HR equipped with a 355 nm laser; specimens were run with a base temperature of 40 K, laser energy of 5 pJ per pulse, repetition rate of 100 kHz and target detection rate of 1%. At these conditions, significant As clustering was observed, as is common in III–V materials. APT data sets were then reconstructed and analysed using Cameca's integrated visualization and analysis software.
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9

FIB Milling for Nanoscale Tomography

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The sample preparation using FIB milling was performed on a Zeiss NVision 40 dual-beam SEM/FIB system at the Center of Nanoscale Materials (CNM) of ANL. The sample was placed at a working distance of 5.4 mm and tilted at 54° with respect to the electron beam. A 30-kV and 10-pA Ga beam was used to remove the nearby HeLa cells of the ROI on the specimen to clear the beam path for subsequent nanoscale tomography data collection.
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10

Structural and Compositional Analysis

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A JEOL-ARM 200 F Cold FEG transmission electron microscope (TEM) was used to investigate the samples’ structure. The operating voltage of the setup is 200 kV with a point resolution of 0.12 nm. A Carl Zeiss NVision 40 SEM/EDS workstation was used to analyze the chemical composition by plotting the energy-dispersive X-ray spectroscopy (EDX) mapping, which collected the Fe K, Ge K, Te L, O K, and Al K edges.
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