Focused Ion Beams (FIB) — Novel Methodologies and Recent Applications for Multidisciplinary Sciences

Considered as the newest field of electron microscopy, focused ion beam (FIB) technologies are used in many fields of science for site-specific analysis, imaging, milling, deposition, micromachining, and manipulation. Dual-beam platforms, combining a high-resolution scanning electron microscope (HR-SEM) and an FIB column, additionally equipped with precursor-based gas injection systems (GIS), micromanipulators, and chemical analysis tools (such as energy-dispersive spectra (EDS) or wavelength-dispersive spectra (WDS)), serve as multifunctional tools for direct lithography in terms of nano-machining and nano-prototyping, while advanced specimen preparation for transmission electron microscopy (TEM) can practically be carried out with ultrahigh precision. Especially, when hard materials and material systems with hard substrates are concerned, FIB is the only technique for site-specific micro- and nanostructuring. Moreover, FIB sectioning and sampling techniques are frequently used for revealing the structural and morphological distribution of material systems with three-dimensional (3D) network at micro-/nanoscale.This book chapter includes many examples on conventional and novel processes of FIB technologies, ranging from analysis of semiconductors to electron tomography-based imaging of hard materials such as nanoporous ceramics and composites. In addition, recent studies concerning the active use of dual-beam platforms are mentione

Production of carbon nanotubes over Fe-FSM-16 catalytic material: effect of acetylene flow rate and CVD temperature

In this article, a high-yield synthesis of high-quality CNTs using Fe catalysts trapped within channels of Folded Sheet Mesoporous Materials, FSM-16 by Chemical Vapor Deposition CVD using acetylene as a hydrocarbon source is reported. The effect of reaction temperature and acetylene flow rate on the formation of CNTs was investigated. It was found that the yield, diameter and quality of CNTs synthesized strongly depend on reaction temperature during CVD. The resulting materials were characterized by scanning electron microscopy (SEM), Raman spectroscopy, and thermogravimetric analysis (TGA). Our research found that carbon deposition, diameter and quality of the CNTs strongly depend on CVD temperature. However acetylene flow rate did not have any significant effect on diameter distribution. Raman measurement indicated that the synthesized products were MWCNTs. High-resolution transmission electron micrographs of samples reveal the multilayer sidewalls of individual MWCNTs with a diameter of 40 nm, in which hollow and tubal structures were observed

The use of focused electron and ion beams for the functionalization and nanostructuring of polymer surfaces

Polymers are nowadays actively used in numerous applications owing their low cost and optimized structural properties. Besides, the miniaturization of the novel materials down to nano and even atomic scale needs the use of Electron Microscopy techniques both for imaging and structuring abilities. When used for surface modification, electrons and ions allow altering the surface properties towards special material designs. This study mainly focuses on investigation, optimization and modification of polymers’ surface properties by the use of electron and ion beam treatment assisted by gas enhanced etching processes in FIB-SEM dual-beam platforms. Direct electron/ion beam etching and XeF2 assisted etching were applied on high density polyethylene (HDPE), Melinex® and polypropylene (PP) samples, in order to obtain different forms of functionalized surfaces. The alterations in the surface properties provided by electron/ion beam and gas assisted modification processes were examined using complementary advanced analysis techniques, such as HR-SEM and AFM

Production of carbon nanotubes over Fe-FSM-16 catalytic material: effect of acetylene flow rate and CVD temperature

In this article, a high-yield synthesis of high-quality CNTs using Fe catalysts trapped within channels of Folded Sheet Mesoporous Materials, FSM-16 by Chemical Vapor Deposition CVD using acetylene as a hydrocarbon source is reported. The effect of reaction temperature and acetylene flow rate on the formation of CNTs was investigated. It was found that the yield, diameter and quality of CNTs synthesized strongly depend on reaction temperature during CVD. The resulting materials were characterized by scanning electron microscopy (SEM), Raman spectroscopy, and thermogravimetric analysis (TGA). Our research found that carbon deposition, diameter and quality of the CNTs strongly depend on CVD temperature. However acetylene flow rate did not have any significant effect on diameter distribution. Raman measurement indicated that the synthesized products were MWCNTs. High-resolution transmission electron micrographs of samples reveal the multilayer sidewalls of individual MWCNTs with a diameter of 40 nm, in which hollow and tubal structures were observed

Rubidium Focused Ion Beam Induced Platinum Deposition

This work presents characterization of focused ion beam induced deposition (FIBID) of platinum using both rubidium and gallium ions. Trimethylplatinum [(MeCp)Pt(Me)3] was used as the deposition precursor. Under similar beam energies, 8.5 keV for Rb+ and 8.0 keV for Ga+, and beam current, near 10 pA, the two ion species deposited Pt films at 0.90 µm3/nC and 0.73 µm3/nC respectively. Energy-dispersive x-ray spectroscopy shows that the Rb+ FIBID-Pt consists of similar Pt contents (49% for Rb+ FIBID and 37% for Ga+ FIBID) with much lower primary ion contents (5% Rb and 27% Ga) than the Ga+ FIBID-Pt. The deposited material was also measured to have a resistivity of 8.1×104 µΩ· cm for the Rb+ FIBID-Pt and 5.7×103 µΩ· cm for the Ga+ FIBID-Pt

Synthesis of PLGA /nano-ZnO composite particles for biomedical applications

Copolymer poly (DL-lactide-co-glycolide) (PLGA), due of its biodegradable and biocompatible nature, is widely used in various medical applications; controlled release of delivering drugs, carriers in the tissue engineering, etc. On the other hand, zinc oxide (ZnO) is extensively used in medicine and pharmacy for personal care products, as well as in biomedical materials like dental composites, as a material for treatment of a variety of skin irritations, to enhance the antibacterial activity of different medicaments, etc. In this research we have dealt with a procedure to prepare particles of poly (lactide-co-glycolide) and nano zinc oxide (PLGA/nano-ZnO). Nano-ZnO has been synthesized using a microwave synthesis method and additionally immobilized within PLGA by physicochemical solvent/non-solvent method. Firstly, ZnO has been dispersed in acetone and then additionally added dropwise in the PLGA/ethyl acetate (PLGA/nano-ZnO(EtAc) or PLGA/acetone (PLGA/nano-ZnO(Ac)) solutions, respectively. The as-prepared dispersions were dried in air atmosphere for 24 h. The characterization of the prepared samples was performed using X-ray powder diffraction (XRPD) method for the structure properties, field emission scanning electron microscopy (FE SEM) for the investigation of particles morphology, as well as Malvern’s Mastersizer instrument for particle size distribution. DTA-TG measurements were performed in order to investigate the samples thermal stability and mass loss percentage. The antimicrobial behavior of the synthesized PLGA/nano-ZnO particles was tested against gram-negative and gram-positive bacteria cultures and also against Candida Albicans, diploid fungus

Supporting information for the article: Lukić, M.J., Kuzmanović, M., Sezen, M., Bakan, F., Egelja, A., Veselinović, L., 2018. Inert atmosphere processing of hydroxyapatite in the presence of lithium iron phosphate. Journal of the European Ceramic Society 38, 2120–2133. https://doi.org/10.1016/j.jeurceramsoc.2017.12.023

Supporting information for the article: [https://doi.org/10.1016/j.jeurceramsoc.2017.12.023].Related to the peer-reviewed manuscript: [https://hdl.handle.net/21.15107/rcub_dais_4924]Related to the published version: [https://hdl.handle.net/21.15107/rcub_dais_3357