Abstract
A simple and cost effective alternative for fabricating custom Scanning Electron Microscope (SEM) sample holders using 3D printers and conductive polylactic acid filament is presented. The flexibility of the 3D printing process allowed for the fabrication of sample holders with specific features that enable the high-resolution imaging of nanoelectrodes and nanopipettes. The precise value of the inner semi cone angle of the nanopipettes taper was extracted from the acquired images and used for calculating their radius using electrochemical methods. Because of the low electrical resistivity presented by the 3D printed holder, the imaging of non-conductive nanomaterials, such as alumina powder, was found to be possible. The fabrication time for each sample holder was under 30 minutes and the average cost was less than $0.50 per piece. Despite being quick and economical to fabricate, the sample holders were found to be sufficiently resistant, allowing for multiple uses of the same holder.
Highlights
Scanning Electron Microscopy (SEM) is a powerful analytical tool for studying chemical composition, material structure and morphology on the submicron level and has been widely used to characterize new materials with a broad applications spectrum. [1,2] SEM is a well-established technique for characterizing nanomaterials, such as nanoparticles, it has been used lately to characterize samples that have macroscopic physical dimensions, such as electrode surfaces, ultramicroelectrodes (UME), nanoelectrodes and nanopipettes
The printing speed was set to 150% of the maximum printer speed, bed temperature to 65 ̊C and extruder temperature to 210 ̊C for all prints
This is mainly to create an electrical connection between the sample holder and the SEM chassis which is held at ground potential
Summary
Scanning Electron Microscopy (SEM) is a powerful analytical tool for studying chemical composition, material structure and morphology on the submicron level and has been widely used to characterize new materials with a broad applications spectrum. [1,2] SEM is a well-established technique for characterizing nanomaterials, such as nanoparticles, it has been used lately to characterize samples that have macroscopic physical dimensions, such as electrode surfaces, ultramicroelectrodes (UME), nanoelectrodes and nanopipettes. [1,2] SEM is a well-established technique for characterizing nanomaterials, such as nanoparticles, it has been used lately to characterize samples that have macroscopic physical dimensions, such as electrode surfaces, ultramicroelectrodes (UME), nanoelectrodes and nanopipettes Other techniques, such as Atomic Force Microscopy (AFM) [3], Transmission Electron Microscopy (TEM) [4] and Scanning Transmission Electron Microscopy (STEM) [5] can be used to characterize those samples, SEM is still the “first line of defense” as it is widely available, can give results fairly fast, and can still give important information such as the outer body dimensions of electrodes,[6,7,8,9] imperative for a precise calculation of the radius of glass in UMEs. Other techniques, such as Atomic Force Microscopy (AFM) [3], Transmission Electron Microscopy (TEM) [4] and Scanning Transmission Electron Microscopy (STEM) [5] can be used to characterize those samples, SEM is still the “first line of defense” as it is widely available, can give results fairly fast, and can still give important information such as the outer body dimensions of electrodes,[6,7,8,9] imperative for a precise calculation of the radius of glass in UMEs. [10] some of those parameters can be estimated by electrochemical methods, [11,12,13,14] without the knowledge of the precise geometry of the samples one can, misleadingly, interpreter the electrochemical results wrongly and assume false characteristics for the electrode in hand. [15]
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