Characterization of size, aspect ratio and degree of dispersion of particles in filled polymeric composites using FIB

Clay Minerals ◽  
2009 ◽  
Vol 44 (2) ◽  
pp. 195-205 ◽  
Author(s):  
Y. Zhu ◽  
G. C. Allen ◽  
J. M. Adams ◽  
D. Gittins ◽  
P. J. Heard ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Aspect Ratio ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Polymeric Composites ◽  
Degree Of Dispersion ◽  
Transmission Electron ◽  
Twin Screw ◽  
Mineral Fillers

AbstractTwo types of mineral fillers, talc and mica, were compounded into polypropylene (PP) via a twin-screw extruder. The morphologies and mechanical properties of the resultant composites were investigated. The dispersion of minerals in PP was observed using Focused Ion Beam (FIB) techniques. The particle size distribution (PSD) and aspect ratio (AR) of particles in the polymer phase were obtained from FIB image analysis. It was found that FIB imaging displays directly the micron to mesoscale level dispersion of particles in polymeric composites. The technique has significant potential for characterizing such materials, having some advantages over ‘traditional’ scanning and transmission electron microscopy in terms of generating representative data in a realistic timescale. The PSD and AR distribution and degree of dispersion in the composites give insights into the modification of mechanical properties of the composites studied.

Physical Failure Analysis Techniques for Front-End-of-Line Defect Analysis

2016 ◽  
Author(s):  
Dirk Doyle ◽  
Lawrence Benedict ◽  
Fritz Christian Awitan
Keyword(s):  
Cross Section ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Gate Oxide ◽  
Top Down ◽  
New Techniques ◽  
First Case ◽  
Transmission Electron ◽  
Scanning Transmission

Abstract Novel techniques to expose substrate-level defects are presented in this paper. New techniques such as inter-layer dielectric (ILD) thinning, high keV imaging, and XeF2 poly etch overflow are introduced. We describe these techniques as applied to two different defects types at FEOL. In the first case, by using ILD thinning and high keV imaging, coupled with focused ion beam (FIB) cross section and scanning transmission electron microscopy (STEM,) we were able to judge where to sample for TEM from a top down perspective while simultaneously providing the top down images giving both perspectives on the same sample. In the second case we show retention of the poly Si short after removal of CoSi2 formation on poly. Removal of the CoSi2 exposes the poly Si such that we can utilize XeF2 to remove poly without damaging gate oxide to reveal pinhole defects in the gate oxide. Overall, using these techniques have led to 1) increased chances of successfully finding the defects, 2) better characterization of the defects by having a planar view perspective and 3) reduced time in localizing defects compared to performing cross section alone.

Metallic Nanoneedles Arrays for TEM Sample Preparation “Lift-Out”

2012 ◽  
Author(s):  
Romaneh Jalilian ◽  
David Mudd ◽  
Neil Torrez ◽  
Jose Rivera ◽  
Mehdi M. Yazdanpanah ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Electron Microscope ◽  
Sample Preparation ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Beam System ◽  
Transmission Electron ◽  
Nanoneedle Array ◽  
Superior Mechanical Properties ◽  
And Performance

Abstract The sample preparation for transmission electron microscope can be done using a method known as "lift-out". This paper demonstrates a method of using a silver-gallium nanoneedle array for a quicker sharpening process of tungsten probes with better sample viewing, covering the fabrication steps and performance of needle-tipped probes for lift-out process. First, an array of high aspect ratio silver-gallium nanoneedles was fabricated and coated to improve their conductivity and strength. Then, the nanoneedles were welded to a regular tungsten probe in the focused ion beam system at the desired angle, and used as a sharp probe for lift-out. The paper demonstrates the superior mechanical properties of crystalline silver-gallium metallic nanoneedles. Finally, a weldless lift-out process is described whereby a nano-fork gripper was fabricated by attaching two nanoneedles to a tungsten probe.

The Effect of the Compounding Procedure on the Morphology and Mechanical Properties of PLA/PBAT-Based Nanocomposites

2021 ◽  
Vol 36 (2) ◽  
pp. 219-227
Author(s):  
P. Saiprasit ◽  
A. K. Schlarb
Keyword(s):  
Mechanical Properties ◽  
Residence Time ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Extrusion Process ◽  
Poly Lactic Acid ◽  
Silicon Dioxide Nanoparticles ◽  
Twin Screw ◽  
One Step ◽  
Thermodynamic Driving Force

Abstract Poly(lactic acid) (PLA)/poly(butylene adipate-co-terephthalate) (PBAT)-based nanocomposites filled with 1 vol.% silicon dioxide nanoparticles (nano-SiO2) were prepared using a co-rotating twin-screw extruder and injection molding. The nanocomposites with various blending sequences were investigated using PLA-based and PBAT-based nanocomposite masterbatches. Morphology of the PLA/PBAT/SiO2 nanocomposites was examined using a scanning electron microscope (SEM) and a focused ion beam (FIB) SEM. It is found that the nano-SiO2 locates in the original polymer phase, in which it is firstly incorporated in the masterbatch process, as well as at the interface between the two polymers. However, as the residence time in the extrusion process increases, the nanoparticles migrate from the original phase to the interface, governed by the thermodynamic driving force. The best optimization of mechanical properties is achieved by using the PBAT-based masterbatches with a one-step process or short residence time. The processing history, therefore, has a tremendous impact on the final properties of the resulting materials.

Characterization of FIB Damage in Silicon

1999 ◽  
Vol 5 (S2) ◽  
pp. 740-741 ◽  
Author(s):  
C.A. Urbanik ◽  
B.I. Prenitzer ◽  
L.A. Gianhuzzi ◽  
S.R. Brown ◽  
T.L. Shofner ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Target Material ◽  
Beam Current ◽  
Specimen Preparation ◽  
Transfer Energy ◽  
Transmission Electron ◽  
Preparation Techniques ◽  
Reactive Gas

Focused ion beam (FIB) instruments are useful for high spatial resolution milling, deposition, and imaging capabilities. As a result, FIB specimen preparation techniques have been widely accepted within the semiconductor community as a means to rapidly prepare high quality, site-specific specimens for transmission electron microscopy (TEM) [1]. In spite of the excellent results that have been observed for both high resolution (HREM) and standard TEM specimen preparation applications, a degree of structural modification is inherent to FIB milled surfaces [2,3]. The magnitude of the damage region that results from Ga+ ion bombardment is dependent on the operating parameters of the FIB (e.g., beam current, beam voltage, milling time, and the use of reactive gas assisted etching).Lattice defects occur as a consequence of FIB milling because the incident ions transfer energy to the atoms of the target material. Momentum transferred from the incident ions to the target atoms can result in the creation of point defects (e.g., vacancies, self interstitials, and interstitial and substitutional ion implantation), the generation of phonons, and plasmon excitation in the case of metal targets.

scholarly journals Fabrication and Characterization of Solid Composite Yarns from Carbon Nanotubes and Poly(dicyclopentadiene)

Nanomaterials ◽  
2020 ◽  
Vol 10 (4) ◽  
pp. 717 ◽  
Author(s):  
Wenbo Xin ◽  
Joseph Severino ◽  
Arie Venkert ◽  
Hang Yu ◽  
Daniel Knorr ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Carbon Nanotubes ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Strengthening Mechanism ◽  
Composite Yarn ◽  
Transmission Electron ◽  
Frictional Forces ◽  
Mechanical Consolidation

In this report, networks of carbon nanotubes (CNTs) are transformed into composite yarns by infusion, mechanical consolidation and polymerization of dicyclopentadiene (DCPD). The microstructures of the CNT yarn and its composite are characterized by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), and a focused ion beam used for cross-sectioning. Pristine yarns have tensile strength, modulus and elongation at failure of 0.8 GPa, 14 GPa and 14.0%, respectively. In the composite yarn, these values are significantly enhanced to 1.2 GPa, 68 GPa and 3.4%, respectively. Owing to the consolidation and alignment improvement, its electrical conductivity was increased from 1.0 × 105 S/m (raw yarn) to 5.0 × 105 S/m and 5.3 × 105 S/m for twisted yarn and composite yarn, respectively. The strengthening mechanism is attributed to the binding of the DCPD polymer, which acts as a capstan and increases frictional forces within the nanotube bundles, making it more difficult to pull them apart.

scholarly journals Characterization of Dental Bonded Interface Degradation Using Focused Ion Beam and High-Resolution Transmission Electron Microscopy

2009 ◽  
Vol 15 (S2) ◽  
pp. 368-369 ◽  
Author(s):  
S Duarte ◽  
A Avishai ◽  
A Sadan
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
High Resolution ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Bonded Interface ◽  
Transmission Electron

Extended abstract of a paper presented at Microscopy and Microanalysis 2009 in Richmond, Virginia, USA, July 26 – July 30, 2009

Microstructural Characterization of Automated Specimen Preparation for TEM Analysis

2000 ◽  
Vol 6 (S2) ◽  
pp. 528-529
Author(s):  
C. Urbanik Shannon ◽  
L. A. Giannuzzi ◽  
E. M. Raz
Keyword(s):  
Focused Ion Beam ◽  
Preparation Method ◽  
Ion Beam ◽  
Microstructural Characterization ◽  
Specimen Preparation ◽  
Tem Analysis ◽  
Area Of Interest ◽  
Transmission Electron ◽  
Preparation Techniques

Automated specimen preparation for transmission electron microscopy has the obvious advantage of saving personnel time. While some people may perform labor intensive specimen preparation techniques quickly, automated specimen preparation performed in a timely and reproducible fashion can significantly improve the throughput of specimens in an industrial laboratory. The advent of focused ion beam workstations for the preparation of electron transparent membranes has revolutionized TEM specimen preparation. The FIB lift-out technique is a powerful specimen preparation method. However, there are instances where the “traditional” FIB method of specimen preparation may be more suitable. The traditional FIB method requires that specimens must be prepared so that the area of interest is as thin as possible (preferably less than 50 μm) prior to FIB milling. Automating the initial specimen preparation for brittle materials (e.g., Si wafers) may be performed using the combination of cleaving and sawing techniques as described below.

Microstructural Characterization of Dehydrogenated Products of the LiBH4-YH3 Composite

2014 ◽  
Vol 20 (6) ◽  
pp. 1798-1804 ◽  
Author(s):  
Ji Woo Kim ◽  
Kee-Bum Kim ◽  
Jae-Hyeok Shim ◽  
Young Whan Cho ◽  
Kyu Hwan Oh
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Microstructural Characterization ◽  
Static Vacuum ◽  
Lithium Borohydride ◽  
Transmission Electron ◽  
Resolution Imaging ◽  
Yttrium Hydride ◽  
Beam Technique

AbstractThe dehydrogenated microstructure of the lithium borohydride-yttrium hydride (LiBH4-YH3) composite obtained at 350°C under 0.3 MPa of hydrogen and static vacuum was investigated by transmission electron microscopy combined with a focused ion beam technique. The dehydrogenation reaction between LiBH4 and YH3 into LiH and YB4 takes place under 0.3 MPa of hydrogen, which produces YB4 nano-crystallites that are uniformly distributed in the LiH matrix. This microstructural feature seems to be beneficial for rehydrogenation of the dehydrogenation products. On the other hand, the dehydrogenation process is incomplete under static vacuum, leading to the unreacted microstructure, where YH3 and YH2 crystallites are embedded in LiBH4 matrix. High resolution imaging confirmed the presence of crystalline B resulting from the self-decomposition of LiBH4. However, Li2B12H12, which is assumed to be present in the LiBH4 matrix, was not clearly observed.

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