Low-voltage SEM of air-sensitive powders: From sample preparation to micro/nano analysis with secondary electron hyperspectral imaging

Nohl, James F; Farr, Nicholas T. H.; Sun, Yige; Hughes, Gordon; Cussen, Serena A.; Rodenburg, Cornelia

doi:10.1016/j.micron.2022.103234

Cited by 17 publications

(14 citation statements)

References 118 publications

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“…SEHI data collection and processing: The methodology of the application of SEHI has been published in depth previously [ 23 , 24 , 25 , 26 ]. Briefly, SE spectra generation was performed on PGS-M using the Helios FEI Helios G4 CX DualBeam microscope by applying consistent operating conditions of 1 kV and a 50 pA immersion mode.…”

Section: Methodsmentioning

confidence: 99%

Revealing Localised Mechanochemistry of Biomaterials Using In Situ Multiscale Chemical Analysis

Farr

2022

Materials

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The study of mechanical and chemical phenomena arising within a material that is being subjected to external stress is termed mechanochemistry (MC). Recent advances in MC have revealed the prospect not only to enable a greener route to chemical transformations but also to offer previously unobtainable opportunities in the production and screening of biomaterials. To date, the field of MC has been constrained by the inability of current characterisation techniques to provide essential localised multiscale chemically mapping information. A potential method to overcome this is secondary electron hyperspectral imaging (SEHI). SEHI is a multiscale material characterisation technique applied within a scanning electron microscope (SEM). Based on the collection of secondary electron (SE) emission spectra at low primary beam energies, SEHI is applicable to the chemical assessment of uncoated polymer surfaces. Here, we demonstrate that SEHI can provide in situ MC information using poly(glycerol sebacate)-methacrylate (PGS-M) as an example biomaterial of interest. This study brings the use of a bespoke in situ SEM holder together with the application of SEHI to provide, for the first time, enhanced biomaterial mechanochemical characterisation.

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Section: Methodsmentioning

confidence: 99%

Revealing Localised Mechanochemistry of Biomaterials Using In Situ Multiscale Chemical Analysis

Farr

2022

Materials

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“…The morphological structure of the raw and activated BP before and aer adsorption was investigated using SEM (FEI, INSPCT-F50, Germany). The procedure and operating conditions were set according to the method used by J. F. Nohl et al 21 2.3.6 X-ray diffraction (XRD). The crystallographic structure formed in the activated BP was analyzed using an X-ray diffractometer (XRD-7000S, Cu-Ka radiation) operating at a voltage of 40 kV and current of 30 mA in a continuous scanning path.…”

Section: Brunauer Emmett Teller (Bet)mentioning

confidence: 99%

The use of banana peel as a low-cost adsorption material for removing hexavalent chromium from tannery wastewater: optimization, kinetic and isotherm study, and regeneration aspects

Ameha,

Nadew,

Tedla

et al. 2024

RSC Adv.

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“…shown to be able to differentiate bonds on carbonaceous material surfaces [35][36][37][38][39] and extract information about the work function of metal oxide surfaces. 21,40 Figure 6D,E show the SE spectra (SES) generated. In previously published SEHI data, a SE Ti peak was identified at 4.9-5.3 eV, with Ti oxides found in a peak range of 5.5-6.2 eV.…”

Section: Sehi Is a Novel Highly Surface Sensitive Technique That Has ...mentioning

confidence: 99%

Characterization in respect to degradation of titanium‐coated polypropylene surgical mesh explanted from humans

2023

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Titanium-coated polypropylene (Ti-PP) mesh was introduced in 2002 as a surgical mesh for the treatment of hernias and shortly after for pelvic floor surgery, with the aim of improving biocompatibility when compared to non-titanised/regular PP mesh implants. The application of a titanium coating could also be beneficial to address concerns regarding the exposure of PP in an in vivo environment. Many studies have shown that PP, although it is widely accepted as a stable polymer, is subject to oxidation and degradation, such degradation affects the mechanical behavior, that is, the stiffness and tensile strength of PP mesh. Despite the wide clinical use of Ti-PP surgical meshes, no study has yet investigated the residual material properties post clinical deployment and subsequent explantation. In this study, two explanted Ti-PP mesh samples each having different incorporation durations from two patients were examined. Material analysis conducted within this study includes the following techniques: attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), Raman spectroscopy, low voltagescanning electron microscopy (LV-SEM), backscattered electron (BSE) imaging, energy dispersive X-ray spectroscopy (EDS) and secondary election hyperspectral imaging (SEHI). The hypothesis of this study is that the Ti coating successfully shields the PP mesh from oxidative stress in vivo and thus protects it from degradation. The results of this analysis show for the first time evidence of bulk oxidation, surface degradation, and environmental stress cracking on explanted Ti-PP meshes.

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Low-voltage SEM of air-sensitive powders: From sample preparation to micro/nano analysis with secondary electron hyperspectral imaging

Cited by 17 publications

References 118 publications

Revealing Localised Mechanochemistry of Biomaterials Using In Situ Multiscale Chemical Analysis

Revealing Localised Mechanochemistry of Biomaterials Using In Situ Multiscale Chemical Analysis

The use of banana peel as a low-cost adsorption material for removing hexavalent chromium from tannery wastewater: optimization, kinetic and isotherm study, and regeneration aspects

Characterization in respect to degradation of titanium‐coated polypropylene surgical mesh explanted from humans

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