scholarly journals Nanomechanical testing of freestanding polymer films: in situ tensile testing and Tg measurement

2021 ◽  
Author(s):  
Nathan R. Velez ◽  
Frances I. Allen ◽  
Mary Ann Jones ◽  
Jenn Donohue ◽  
Wei Li ◽  
...  
Keyword(s):  
Polymer Films ◽  
Tensile Testing ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Small Scale ◽  
Specimen Preparation ◽  
In Situ Tem ◽  
Preparation Technique ◽  
Characterization Methods

Abstract A method for small-scale testing and imaging of freestanding, microtomed polymer films using a push-to-pull device is presented. Central to this method was the development of a sample preparation technique which utilized solvents at cryogenic temperatures to transfer and deposit delicate thin films onto the microfabricated push-to-pull devices. The preparation of focused ion beam (FIB)-milled tensile specimens enabled quantitative in situ TEM tensile testing, but artifacts associated with ion and electron beam irradiation motivated the development of a FIB-free specimen preparation method. The FIB-free method was enabled by the design and fabrication of oversized strain-locking push-to-pull devices. An adaptation for push-to-pull devices to be compatible with an instrumented nanoindenter expanded the testing capabilities to include in situ heating. These innovations provided quantitative mechanical testing, postmortem TEM imaging, and the ability to measure the glass transition temperature, via dynamic mechanical analysis, of freestanding polymer films. Results for each of these mentioned characterization methods are presented and discussed in terms of polymer nanomechanics. Graphic Abstract

scholarly journals Preparation of Multilayered Materials in Cross-Section for in-Situ Tem Tensile Deformation Studies

1997 ◽  
Vol 480 ◽  
Author(s):  
M. A. Wall ◽  
T. W. Barbee
Keyword(s):  
Focused Ion Beam ◽  
Tensile Deformation ◽  
Crack Nucleation ◽  
Ion Beam ◽  
Specimen Preparation ◽  
In Situ Tem ◽  
Transmission Electron ◽  
Gauge Section ◽  
In Situ Deformation

AbstractThe success of in-situ transmission electron microscopy experimentation is often dictated by proper specimen preparation. We report here a novel technique permitting the production of crosssectioned tensile specimens of multilayered films for in-situ deformation studies. Of primary importance in the development of this technique is the production of an electron transparent microgauge section using focused ion beam technology. This micro-gauge section predetermines the position at which plastic deformation is initiated; crack nucleation, growth and failure are then subsequently observed.

Ga Aggregation in Cu Layer on In-situ TEM Analysis: Observation and Alternative Solutions

2020 ◽  
Author(s):  
Seo-Jin Kim ◽  
Byung-Kyu Park ◽  
Christopher H. Kang
Keyword(s):  
Sample Preparation ◽  
Semiconductor Manufacturing ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
In Situ Tem ◽  
Preparation Technique ◽  
Tem Analysis ◽  
The Impact ◽  
Alternative Solutions

Abstract In semiconductor manufacturing technology, copper has been widely used for BEOL process due to better conductivity than aluminum. TEM (Transmission Electron Microscopy) characterization has been played in key role to understand the process of semiconductor manufacturing. Gallium base Focused Ion Beam (FIB) is widely used on TEM sample preparation. The experiment to understand the impact of gallium which is from sample preparation process on Cu layer was performed. In-situ TEM studies have shown real time material characteristic of Cu at various temperature [1]. We observed the gallium aggregation phenomenon on Cu layer at round the temperature of 400°C. This thermal aggregation of gallium on Cu layer has been confirmed by EDS analysis in the study. Detectable amount of gallium was found in whole area in the sample before heating the sample at in-situ TEM work. This paper also introduces alternative solutions to resolve this gallium aggregation in copper layer including the sample preparation technique using Xe Plasma Focused Ion Beam (PFIB) [2]. This Xe PFIB showed the substantial improvement of specimen quality for the in-situ TEM experiment of sample preparation.

Transmission Electron Microscopy (TEM) Specimen Preparation Technique using Focused Ion Beam (FIB): Application to Material Characterization of Chemical Vapor Deposition of Tungsten (W) and Tungsten Silicides (WSix)

1997 ◽  
Author(s):  
K. Doong ◽  
J.-M. Fu ◽  
Y.-C. Huang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Chemical Vapor Deposition ◽  
Vapor Deposition ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Chemical Vapor ◽  
Specimen Preparation ◽  
Preparation Technique ◽  
Transmission Electron

Abstract The specimen preparation technique using focused ion beam (FIB) to generate cross-sectional transmission electron microscopy (XTEM) samples of chemical vapor deposition (CVD) of Tungsten-plug (W-plug) and Tungsten Silicides (WSix) was studied. Using the combination method including two axes tilting[l], gas enhanced focused ion beam milling[2] and sacrificial metal coating on both sides of electron transmission membrane[3], it was possible to prepare a sample with minimal thickness (less than 1000 A) to get high spatial resolution in TEM observation. Based on this novel thinning technique, some applications such as XTEM observation of W-plug with different aspect ratio (I - 6), and the grain structure of CVD W-plug and CVD WSix were done. Also the problems and artifacts of XTEM sample preparation of high Z-factor material such as CVD W-plug and CVD WSix were given and the ways to avoid or minimize them were suggested.

scholarly journals Fiducial marker application method for position alignment of in situ multimodal X-ray experiments and reconstructions

2016 ◽  
Vol 49 (2) ◽  
pp. 700-704 ◽  
Author(s):  
Paul A. Shade ◽  
David B. Menasche ◽  
Joel V. Bernier ◽  
Peter Kenesei ◽  
Jun-Sang Park ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Tensile Specimen ◽  
Material Behavior ◽  
Validation Data ◽  
Great Opportunity ◽  
Characterization Methods ◽  
X Ray ◽  
Multiple Data Sets

An evolving suite of X-ray characterization methods are presently available to the materials community, providing a great opportunity to gain new insight into material behavior and provide critical validation data for materials models. Two critical and related issues are sample repositioning during an in situ experiment and registration of multiple data sets after the experiment. To address these issues, a method is described which utilizes a focused ion-beam scanning electron microscope equipped with a micromanipulator to apply gold fiducial markers to samples for X-ray measurements. The method is demonstrated with a synchrotron X-ray experiment involving in situ loading of a titanium alloy tensile specimen.

Microstructural Observation of Focused Ion Beam Modification of Ni Silicide/Si Thin Films

1996 ◽  
Vol 439 ◽  
Author(s):  
Miyoko Tanaka ◽  
Kazuo Furuya ◽  
Tetsuya Saito
Keyword(s):  
Structural Changes ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Dark Field ◽  
In Situ Tem ◽  
Si Substrate ◽  
Ion Beam Modification ◽  
Surrounding Matrix ◽  
Transmission Electron

AbstractFocused ion beam (FIB) irradiation of a thin Ni2Si layer deposited on a Si substrate was carried out and studied using an in-situ transmission electron microscope (in-situ TEM). Square areas on sides of 4 by 4 and 9 by 9 μm were patterned at room temperature with a 25keV Ga+-FIB attached to the TEM. The structural changes of the films indicate a uniform milling; sputtering of the Ni2Si layer and the damage introducing to the Si substrate. Annealing at 673 K results in the change of the Ni2Si layer into an epitaxial NiSi2 layer outside the FIB irradiated area, but several precipitates appear around the treated area. Precipitates was analyzed by energy dispersive X-ray spectroscopy (EDS). Larger amount of Ni than the surrounding matrix was found in precipitates. Selected area diffraction (SAD) patterns of the precipitates and the corresponding dark field images imply the formation of a Ni rich silicide. The relation between the FIB tail and the precipitation is indicated.

In-Situ Tem Characterization of Whiskers on Al Electrodes for Thin-Film Transistors

1996 ◽  
Vol 441 ◽  
Author(s):  
K. Tsujimoto ◽  
S. Tsuji ◽  
H. Saka ◽  
K. Kuroda ◽  
H. Takatsuji ◽  
...  
Keyword(s):  
Thin Film ◽  
High Voltage ◽  
Focused Ion Beam ◽  
Liquid Crystal Display ◽  
Ion Beam ◽  
Thin Film Transistor ◽  
Dark Field ◽  
Growth Stages ◽  
In Situ Tem

AbstractThe recent attention paid to stress migration of aluminum (Al) electrodes in thin-film transistor liquid crystal display (TFT-LCD) applications indicates that wiring materials with low electrical resistivities are of considerable interest for their potential use in higher-resolution displays. In this paper, we firstly describe how as-grown Al whiskers on Al electrodes fabricated on a LCD-grade glass substrate can be characterized by means of a high-voltage transmission electron microscope (HV-TEM) operated at 1 MV. The whiskers ranging from 300 to 400 nm in diameter are sufficient to be transparent to high-voltage electrons. This allows detailed observation of whisker characteristics such as its morphology and crystallography. In most cases, the as-grown Al whiskers in our study had straight rod shapes, and could be regarded as single crystals. Secondly, we report on the in-situ fabrication and observation of Al whiskers at elevated temperature with the HV-TEM. Since relatively thick TEM samples (up to about 1 mm) can be set on a sample holder in the HV-TEM, various growth stages of Al whiskers can be investigated under various heating conditions. Finally, we demonstrate a TEM sample preparation method for the cross-section of an individual Al whisker, using focused ion beam (FIB) etching. This technique makes it possible to reduce the thickness of an Al whisker close to the root. Both bright- and dark-field TEM images provide nanostructural information on the whisker/Al thin-film interface.

Fast Preparation of Ultrathin FIB Lamellas for MEMs-Based In Situ TEM Experiments

2016 ◽  
Vol 850 ◽  
pp. 722-727 ◽  
Author(s):  
Hui Wang ◽  
Shang Gang Xiao ◽  
Qiang Xu ◽  
Tao Zhang ◽  
Henny Zandbergen
Keyword(s):  
Sample Preparation ◽  
Focused Ion Beam ◽  
Preparation Method ◽  
Ion Beam ◽  
Metallic Alloy ◽  
In Situ Tem ◽  
Ion Milling ◽  
Electrochemical Polishing ◽  
Argon Ion

The preparation of thin lamellas by focused ion beam (FIB) for MEMS-based in situ TEM experiments is time consuming. Typically, the lamellas are of ~5μm*10μm and have a thickness less than 100nm. Here we demonstrate a fast lamellas’ preparation method using special fast cutting by FIB of samples prepared by conventional TEM sample preparation by argon ion milling or electrochemical polishing methods. This method has been applied successfully on various materials, such as ductile metallic alloy Ti68Ta27Al5, brittle ceramics K0.5Na0.5NbO3-6%LiNbO3 and semiconductor Si. The thickness of the lamellas depends on the original TEM sample.

TEM FIB Lift-Out of Mount Saint Helens Volcanic Ash

1999 ◽  
Vol 5 (S2) ◽  
pp. 908-909
Author(s):  
J.L. Drown-MacDonald ◽  
B.I. Prenitzer ◽  
T.L. Shofner ◽  
L.A. Giannuzzi
Keyword(s):  
Cross Sections ◽  
Volcanic Ash ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Preparation Technique ◽  
Tem Analysis ◽  
Plan View ◽  
Transmission Electron ◽  
Silver Paint

Focused Ion Beam (FIB) specimen preparation for both scanning and transmission electron microscopy (SEM and TEM respectively) has seen an increase in usage over the past few years. The advantage to the FIB is that site specific cross sections (or plan view sections) may be fabricated quickly and reproducibly from numerous types of materials using a finely focused beam of Ga+ ions [1,2]. It was demonstrated by Prenitzer et al. that TEM specimens may be acquired from individual Zn powder particles by employing the FIB LO specimen preparation technique [3]. In this paper, we use the FIB LO technique to prepare TEM specimens from Mount Saint Helens volcanic ash.Volcanic ash from Mount Saint Helens was obtained at the Microscopy and Microanalysis 1998 meeting in Atlanta. TEM analysis of the ash was performed using the FIB lift out technique [1]. Ash powders were dusted onto an SEM sample stud that had been coated with silver paint.

In-situ TEM investigation of deformation behavior of metallic glass pillars

2009 ◽  
Vol 1185 ◽  
Author(s):  
Changqiang Chen ◽  
Yutao Pei ◽  
Jeff De Hosson
Keyword(s):  
Metallic Glass ◽  
Focused Ion Beam ◽  
Axial Stress ◽  
Ion Beam ◽  
Shear Banding ◽  
Shear Bands ◽  
Deformation Mode ◽  
In Situ Tem ◽  
Compression Tests

AbstractWe show results of in situ TEM (Transmission electron microscope) quantitative investigations on the compression behaviors of amorphous micropillars fabricated by focused ion beam from Cu47Ti33Zr11Ni6Sn2Si1 metallic glass (MG) ribbon. Pillars with well defined gauge sections and tip diameter ranging from 100 nm to 640 nm are studied. Quantitative compression tests were performed by a recently developed Picoindenter TEM holder, with the evolution of individual shear bands monitored in real time in TEM. It is found that the deformation of the MG pillars at the present size domain is still dominated by discrete shear banding as demonstrated by intermittent events in the load-displacement curves. However, the frequency, amplitude and distribution of these shear banding events are clearly size dependent at submicrometer scale, leading to an apparently transition in deformation mode from highly localized inhomogeneous deformation to less localized and more distributed deformation with decreasing pillars diameter. Deformation of a 105 nm diameter pillar having rounded tips is characterized with fully homogeneous bulge at the initial stage of deformation, indicating prompting effect of multi-axial stress state on transition to fully homogeneous deformation.

scholarly journals In Situ Preparation of Pr1-xCaxMnO3 and La1-xSrxMnO3 Catalysts Surface for High-Resolution Environmental Transmission Electron Microscopy

Catalysts ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 751 ◽  
Author(s):  
Roddatis ◽  
Lole ◽  
Jooss
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Residual Water ◽  
Environmental Transmission ◽  
Transmission Electron ◽  
Environmental Transmission Electron Microscopy

The study of changes in the atomic structure of a catalyst under chemical reaction conditions is extremely important for understanding the mechanism of their operation. For in situ environmental transmission electron microscopy (ETEM) studies, this requires preparation of electron transparent ultrathin TEM lamella without surface damage. Here, thin films of Pr1-xCaxMnO3 (PCMO, x = 0.1, 0.33) and La1-xSrxMnO3 (LSMO, x = 0.4) perovskites are used to demonstrate a cross-section specimen preparation method, comprised of two steps. The first step is based on optimized focused ion beam cutting procedures using a photoresist protection layer, finally being removed by plasma-etching. The second step is applicable for materials susceptible to surface amorphization, where in situ recrystallization back to perovskite structure is achieved by using electron beam driven chemistry in gases. This requires reduction of residual water vapor in a TEM column. Depending on the gas environment, long crystalline facets having different atomic terminations and Mn-valence state, can be prepared.

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