High-voltage energy dispersive x-ray spectrometry using a low-energy primary beam

Wu, Ying; Klyachko, Dimitri; Davilla, S. D.; Spallas, J. P.; Indermuehle, Scott; Muray, L. P.

doi:10.1116/1.4901883

Journal of Vacuum Science &Amp; Technology B, Nanotechnology and Microelectronics: Materials, Processing, Measurement, and Phen

2014

DOI: 10.1116/1.4901883

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High-voltage energy dispersive x-ray spectrometry using a low-energy primary beam

Ying Wu

Dimitri Klyachko

S. D. Davilla

et al.

Abstract: This paper proposes a way to do energy dispersive x-ray spectroscopy (EDS) at high accelerating voltages using a low-voltage field emission scanning electron microscope (FESEM). By biasing the sample to a positive voltage, the electron landing energy (also known as the x-ray excitation energy) is increased, effectively extending the EDS capabilities of the low-voltage SEM. This positive biasing reduces the signal-to-noise ratio of the FESEM image, but it also introduces scaling and offset errors. A one-time ca… Show more

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Cited by 3 publications

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“…Excitation energies >10keV are necessary to obtain the unique the x-ray signature of most materials, yet miniature columns currently cannot operate above a few keV. This problem is overcome by biasing the sample to > +13keV, which creates post-lens acceleration and 15keV -20keV landing energies [5]. The result is good EDS performance (with a few limitations described elsewhere), and interesting new physics in the x-ray generation process.…”

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Miniature Electron Beam Columns: From the Lab to the Field

2016

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Scanning electron microscopes (SEMs) have been the workhorse of high-technology research and development for well over 50 years with applications ranging from the life sciences to forensic sciences. Improvements in SEM performance, operating conditions, ability to accommodate analytical instrumentation, portability, user interface, software, and automation, have progressed at a rapid rate bringing SEM into main stream usage. Today, innovations such as low-voltage imaging and compound or cathode lenses allow researchers to routinely image and analyze nanoscale structures at <2nm resolution [1]. However, the fundamental architecture of SEMs-a high-brightness macro-scale electron source coupled with precision-machined magnetic and electrostatic lens, deflection and correction elements-has also imposed, with few exceptions, the requirement that the sample be brought to the system rather than the system to the sample. Removing this constraint could create new types of field applications which would benefit from the SEM's high resolution imaging and analytical capabilities. An example from space exploration is shown in Fig 1, where undetected fine-grained lunar dust can create potentially life threatening situations [2]. Miniature electron beam columns, shown in Fig 2, are a relatively new class of electrostatic columns fabricated from silicon using standard microfabrication processes. The defining characteristics of these columns are a thermal field emission (TFE) source, low voltage operation (typically < 3keV), simple design (two lenses, no crossover), aperture lenses, ceramic carriers and impedance-controlled patterned interconnects. Production versions of miniature columns achieve <10 nm resolution at 1keV, and have demonstrated <6nm resolution at higher beam energies [3]. Currently, they are available only in a desktop SEM, but, with the small size, low power and high performance, miniature columns are ideal candidates for field applications.

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Miniature Electron Beam Columns: From the Lab to the Field

2016

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Novel biocompatible magnetron-sputtered silver coating for enhanced antibacterial properties and osteogenesis in vitro

Juma,

Wang,

Cao

et al. 2024

Sci Rep

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Peri-implant infection is a serious complication in orthopedic surgery. This study aimed to reduce the incidence of peri-implant infection by developing a durable and safe antibacterial silver coating. We compared the antibacterial properties and process controllability of various coating techniques to identify the most effective method for silver coating. We refined substrate treatment techniques and coating thicknesses through antibacterial and scratch tests. Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) were used to analyze the coating’s morphology and composition. Micron-sized magnetron sputtering silver coating samples underwent in vitro antibacterial testing, cytotoxicity testing, silver ion release testing, and osteogenic testing using membrane contact culture, CCK-8 assay, inductively coupled plasma (ICP) detection, and alkaline phosphatase (ALP) activity/osteogenic gene PCR. Magnetron sputtering demonstrated superior antibacterial properties, uniformity, and process controllability compared to alternative techniques. The optimal adhesion strength was achieved with a 0.5 μm coating thickness and a 400 mesh sandpaper pretreatment process, without compromising antibacterial efficacy. The coating showed near-perfect antiseptic results in antibacterial and anti-biofilm tests. Fibroblasts cultured in silver ion precipitation medium exhibited growth rates of 89% on day 30 and 88% on day 90, compared to 95% in the control group. The osteogenic test indicated that the magnetron sputtering silver coating promotes osteogenesis effectively. Our study demonstrated that micron-sized magnetron sputtering silver coating has potential for clinical use to prevent peri-implant infections in the future. Supplementary Information The online version contains supplementary material available at 10.1038/s41598-024-77270-4.

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Ultralow voltage imaging using a miniature electron beam column

Spallas

Meisburger

Muray

2016

Journal of Vacuum Science &Amp; Technology B, Nanotechnology and Microelectronics: Materials, Processing, Measurement, and Phen

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Miniature columns that are fabricated from silicon using advanced micromachining processes are a relatively new class of electron beam column. The defining characteristics of these columns are a thermal field emitter source, low voltage operation (typically <3 keV), simple design (two lenses, no crossover), microfabricated lenses, and all electrostatic components. Current production versions of miniature columns achieve <10 nm resolution at 1 keV, and have demonstrated <7 nm resolution at higher beam energies [Spallas et al., J. Vac. Sci. Technol., B 24, 2892 (2006)]. The resolution of miniature columns is limited by competing requirements to minimize optical aberrations, relax physical or geometric constraints (e.g., working distance and electrode–electrode distance), and maintain manufacturable mechanical tolerances of the column components (e.g., alignment, diameter, and placement). In this paper, the authors investigate imaging using a miniature electron beam column in a commercial field emission electron microscope equipped with a retarding field lens. Using a retarding field allows high-resolution imaging at landing energies lower than are possible by reducing the beam voltage because the aberrations are lower. The authors show that for the same landing energy, the resolution is better when using the retarding field. High-resolution imaging at landing energies down to 50 eV and imaging is down to 10 eV are demonstrated. Imaging nonconductive samples at landing energies less than the stable unity yield energy is not expected to be beneficial, yet the authors show that in some cases the ability to image nonconducting samples improves. Finally, the authors image a gas shale sample to demonstrate energy dependent contrast.

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High-voltage energy dispersive x-ray spectrometry using a low-energy primary beam

Cited by 3 publications

References 10 publications

Miniature Electron Beam Columns: From the Lab to the Field

Miniature Electron Beam Columns: From the Lab to the Field

Novel biocompatible magnetron-sputtered silver coating for enhanced antibacterial properties and osteogenesis in vitro

Ultralow voltage imaging using a miniature electron beam column

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