scholarly journals A novel method for in situ TEM measurements of adhesion at the diamond–metal interface

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
P. A. Loginov ◽  
D. A. Sidorenko ◽  
A. S. Orekhov ◽  
E. A. Levashov
Keyword(s):  
Bonding Strength ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Tensile Tests ◽  
Mechanical Tests ◽  
In Situ Tem ◽  
Dog Bone ◽  
Ni Alloy ◽  
Novel Method

AbstractThe procedure for in situ TEM measurements of bonding strength (adhesion) between diamond and the metal matrix using a Hysitron PI 95 TEM Picoindenter holder for mechanical tests and Push-to-Pull devices was proposed. For tensile tests, dog-bone shaped lamellae 280–330 nm thick and ~ 2.5 µm long were used as objects of study. The lamellae were manufactured using the focused ion beam technology from the metal–diamond interface of diamond-containing composite material with a single-phase binder made of Fe–Co–Ni alloy. The experimentally determined bonding strength was 110 MPa.

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.

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 The Perfect Cut: Focused Ion Beam Preparation for In Situ TEM

2015 ◽  
Vol 21 (S3) ◽  
pp. 1403-1404
Author(s):  
Andrew Lang ◽  
Wayne Harlow ◽  
Michael Jablonski ◽  
James Hart ◽  
Christopher Barr ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
In Situ Tem

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.

In-Situ TEM Electrical Characterization of Void Formation and Growth Along Cu Interconnect Via: FIB Based Sample Preparation Method

2020 ◽  
Author(s):  
Hagit Barda ◽  
Irina Geppert ◽  
Avraham Raz ◽  
Rémy Berthier
Keyword(s):  
Sample Preparation ◽  
Focused Ion Beam ◽  
Preparation Method ◽  
Ion Beam ◽  
Void Formation ◽  
Electrical Characterization ◽  
In Situ Tem ◽  
Sample Preparation Method ◽  
Transition Electron Microscopy

Abstract An experimental setup is presented, that allows in-situ Transition Electron Microscopy (TEM) investigation of void formation and growth within fully embedded interconnect structure, as a response to an external bias. A special TEM holder is employed to perform in-situ I-V measurements across the Via, simultaneously monitoring the morphological and chemical changes surrounding the void. This work presents in detail a Focused Ion Beam (FIB) based sample preparation method that allows the analysis of a Cu single Via structure found in the advanced microelectronic 14nm FinFET technology, as well as preliminary TEM observations.

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.

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

1996 ◽  
Vol 438 ◽  
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.

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