In Situ FIB-TEM-TOF-SIMS Combination Technique: Application in the Analysis of Ultra-Light and Trace Elements in Phyllosilicates

Abstract

At present, a single technical method has difficulty in obtaining microscopic data of ultra-light elements, trace elements, and crystal structures in samples simultaneously. This work combined an in situ focused ion beam—transmission electron microscopy—time of flight secondary ion mass spectrometry (FTT) technique and analyzed the composition and crystal structure of four phyllosilicate samples. These materials were comprised of antigorite, clinochlore, and cookeite phases. An FIB sample preparation technique was found to provide a sample thickness suitable for TEM observations and a degree of surface roughness appropriate for TOF-SIMS analysis. In addition, the relative amounts and distributions of various elements could be obtained, as well as crystal structure data, such that the composition and crystal structure of each specimen were determined. The in situ FTT method demonstrated herein successfully combines the advantages of all three analytical techniques and offers unique advantages with regard to analyzing ultra-light and trace elements as well as the structural data of phyllosilicates.

The 3D Controllable Fabrication of Nanomaterials with FIB-SEM Synchronization Technology

“…preparation of inorganic materials, metal alloys, crystals, and polymers, etc. [38,39]. By integrating APT, a sharp tip with a radius of curvature less than 50 nm can be formed using a sample thinning technique and the polishing of constantly small beams [37].…”

“…Recently, great progress has been made in FIB fabrication with atom probe tomography (APT) [ 37 ] and the transmission electron microscope (TEM) sample preparation of inorganic materials, metal alloys, crystals, and polymers, etc. [ 38 , 39 ]. By integrating APT, a sharp tip with a radius of curvature less than 50 nm can be formed using a sample thinning technique and the polishing of constantly small beams [ 37 ].…”

“…The mechanisms of phase evolution during the sintering process can be achieved by integrating in situ SPS technology [ 72 ]. Combined with electron beam (EM) technology, the range of FIB applications has been greatly expanded for micro–nano electromechanical systems (MEMS/NEMS), site-specific device production, IC repairment, and complex TEM sample preparation [ 3 , 15 , 39 , 73 ]. In early FIB-SEM systems, FIB and SEM worked by switching, as the magnetic field of the SEM objective lens would affect the performance of the FIB greatly.…”