In-Situ Transmission Electron Microscopy of the Solid-Phase Epitaxial Growth of GaAs: Sample Preparation and Artifact Characterization

1997 ◽  
Vol 480 ◽  
Author(s):  
K. B. Belay ◽  
M. C. Ridgway ◽  
D. J. Llewellyn
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Epitaxial Growth ◽  
Solid Phase ◽  
Ion Beam ◽  
Ex Situ ◽  
In Situ Tem ◽  
Transmission Electron

AbstractIn-situ transmission electron microscopy (TEM) has been used to characterize the solidphase epitaxial growth of amorphized GaAs at a temperature of 260°C. To maximize heat transfer from the heated holder to the sample and minimize electron-irradiation induced artifacts, non-conventional methodologies were utilized for the preparation of cross-sectional samples. GaAs (3xI) mm rectangular slabs were cut then glued face-to-face to a size of (6x3) mm stack by maintaining the TEM region at the center. This stack was subsequently polished to a thickness of ~ 200 ýtm. A 3 mm disc was then cut from it using a Gatan ultrasonic cutter. The disc was polished and dimpled on both sides to a thickness of ~15 mimT.h is was ion-beam milled at liquid nitrogen temperature to an electron-transparent layer. From a comparison of in-situ and ex-situ measurements of the recrystallization rate, the actual sample temperature during in-situ characterization was estimated to deviate by ≤ 20°C from that of the heated holder. The influence of electron-irradiated was found to be negligible by comparing the recrystallization rate and microstructure of irradiated and unirradiated regions of comparable thickness. Similarly, the influence of “thin-foil effect” was found to be negligible by comparing the recrystallization rate and microstructure of thick and thin regions, the former determined after the removal of the sample from the microscope and further ion-beam milling of tens of microns of material. In conclusion, the potential influence of artifacts during in-situ TEM can be eliminated by the appropriate choice of sample preparation procedures.

scholarly journals Ion Beam Annealing of Si Co-Implanted with Ga and As

1989 ◽  
Vol 157 ◽  
Author(s):  
S. P. Withrow ◽  
O. W. Holland ◽  
S. J. Pennycook ◽  
J. Pankove ◽  
A. Mascarenhas
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Epitaxial Growth ◽  
Solid Phase ◽  
Ion Beam ◽  
Ion Pairing ◽  
Si Substrate ◽  
Transmission Electron ◽  
Amorphous Si

ABSTRACTIon beam annealing of amorphous Si(100) layers formed by co-implantation of overlapping Ga and As distributions is studied. Annealing was done using 750 keV Si+ ions with the Si substrate held at 300°C. The samples were characterized using 2.0 and 5.0 MeV He+ backscattering/channeling as well as by transmission electron microscopy (TEM). Crystallization of the amorphous Si layer occurs during irradiation via solid-phase-epitaxial growth without impurity precipitation or segregation. Both the Ga and As are mainly substitutional in the Si lattice, even at concentrations in excess of 7 at. % for each species. These results are attributed to compensation effects, most likely through ion pairing of the dopants.

In Situ TEM Heating Study of the γ Lamellae Formation inside the α2 Matrix of a Ti-45Al-7.5Nb Alloy

2010 ◽  
Vol 146-147 ◽  
pp. 1365-1368 ◽  
Author(s):  
Li Mei Cha ◽  
Helmut Clemens ◽  
Gerhard Dehm ◽  
Zao Li Zhang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ex Situ ◽  
In Situ Tem ◽  
Transmission Electron ◽  
Initial Stage ◽  
Heat Treated ◽  
The Matrix ◽  
In Situ Heating

In-situ heating transmission electron microscopy (TEM) was employed to investigate the initial stage of lamellae formation in a high Nb containing γ-TiAl based alloy. A Ti-45Al-7.5Nb alloy (at %), which was heat treated and quenched in a non-equilibrium state such that the matrix consists of ordered a2 grains, was annealed inside a TEM up to 750 °C. The in-situ TEM study reveals that g laths precipitate in the a2 matrix at ~ 750 °C possessing the classical Blackburn orientation relationship, i.e. (0001)a2 // (111)g and [11-20]a2 // <110]g. The microstructure of the in-situ TEM experiment is compared to results from ex-situ heating and subsequent TEM studies.

scholarly journals Method of Ga removal from a specimen on a microelectromechanical system-based chip for in-situ transmission electron microscopy

2020 ◽  
Vol 50 (1) ◽  
Author(s):  
Yena Kwon ◽  
Byeong-Seon An ◽  
Yeon-Ju Shin ◽  
Cheol-Woong Yang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Beam ◽  
Thin Foil ◽  
Ex Situ ◽  
Ion Milling ◽  
Microelectromechanical System ◽  
Transmission Electron ◽  
Foil Specimen

Abstract In-situ transmission electron microscopy (TEM) holders that employ a chip-type specimen stage have been widely utilized in recent years. The specimen on the microelectromechanical system (MEMS)-based chip is commonly prepared by focused ion beam (FIB) milling and ex-situ lift-out (EXLO). However, the FIB-milled thin-foil specimens are inevitably contaminated with Ga+ ions. When these specimens are heated for real time observation, the Ga+ ions influence the reaction or aggregate in the protection layer. An effective method of removing the Ga residue by Ar+ ion milling within FIB system was explored in this study. However, the Ga residue remained in the thin-foil specimen that was extracted by EXLO from the trench after the conduct of Ar+ ion milling. To address this drawback, the thin-foil specimen was attached to an FIB lift-out grid, subjected to Ar+ ion milling, and subsequently transferred to an MEMS-based chip by EXLO. The removal of the Ga residue was confirmed by energy dispersive spectroscopy.

scholarly journals A method of Ga removal from a specimen fabricated on MEMS-based chip for in-situ transmission electron microscopy

2020 ◽  
Author(s):  
Yena Kwon ◽  
Byeong-Seon An ◽  
Yeon-Ju Shin ◽  
Cheol-Woong Yang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Beam ◽  
Thin Foil ◽  
Type Specimen ◽  
Ex Situ ◽  
Ion Milling ◽  
Transmission Electron ◽  
Foil Specimen

Abstract In-situ transmission electron microscopy (TEM) holders, which are widely used in recent years, employ a chip-type specimen stage. To prepare the specimen on the microelectromechanical system (MEMS)-based chip, focused ion beam (FIB) and ex-situ lift-out (EXLO) techniques has been widely used. However, thin foil specimens prepared using the FIB inevitably contain the contamination induced by Ga+ ions. In particular, when the specimen is heated for real time observation, it is observed that Ga+ ions influence the reaction or aggregate in the protection layer. An effective method of removing the Ga residue is demonstrated using Ar+ ion milling within FIB. In the case of lifting the thin foil specimen from the trench by the EXLO technique, Ga still remained even if Ar+ ion milling was conducted. To avoid this problem, the thin foil specimen was attached to FIB lift-out grid, performing Ar+ ion milling, and then transferred to a MEMS chip using EXLO technique. The removal of the Ga residue was confirmed using energy dispersive spectroscopy (EDS).

In-Situ Annealing Transmission Electron Microscopy Study of Pd/Ge/Pd/GaAs Interfacial Reactions

1999 ◽  
Vol 589 ◽  
Author(s):  
F. Radulescu ◽  
J.M. Mccarthy ◽  
E. A. Stach
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Solid State ◽  
Epitaxial Growth ◽  
Ohmic Contact ◽  
Ion Beam ◽  
Solid State Reactions ◽  
Cross Sectional ◽  
Transmission Electron

AbstractIn-situ TEM annealing experiments on the Pd (20 nm) / a-Ge (150 nm) / Pd (50 nm) GaAs ohmic contact system have permitted real time determination of the evolution of contact microstructure. As-deposited cross-sectional samples of equal thickness were prepared using a focused ion beam (FIB) method and then subjected to in-situ annealing at temperatures between 130-400 °C. Excluding Pd-GaAs interactions, four sequential solid state reactions were observed during annealing of the Pd:Ge thin films. First, interdiffusion of the Pd and Ge layers occurred, followed by formation of the hexagonal Pd2Ge phase. This hexagonal phase then transformed into orthorhombic PdGe, followed by solid state epitaxial growth of Ge at the contact / GaAs interface. The kinetics of the solid state reactions, which occur during ohmic contact formation, were determined by measuring the grain growth rates associated with each phase from the videotape observations. These data agreed with a previous study that measured the activation energies through a differential scanning calorimetry (DSC) method. We established that the Ge transport to the GaAs interface was dependent upon the grain size of the PdGe phase. The nucleation and growth of this phase was demonstrated to have a significant effect on the solid phase epitaxial growth of Ge on GaAs. These findings allowed us to engineer an improved two step annealing procedure that would control the shape and size of the PdGe grains. Based on these results, we have established the suitability of combining FIB sample preparation with in-situ cross-sectional transmission electron microscopy (TEM) annealing for studying thin film solid-state reactions.

Characterization of the Solid-Phase Epitaxial Growth of Amorphized Gaas with In-Situ Electron Microscopy

1996 ◽  
Vol 421 ◽  
Author(s):  
K. B. Belay ◽  
M. C. Ridgway ◽  
D. J. Llewellyn
Keyword(s):  
Electron Microscopy ◽  
Single Crystal ◽  
Epitaxial Growth ◽  
Solid Phase ◽  
Ex Situ ◽  
In Situ Tem ◽  
Recrystallization Process ◽  
Time Resolved ◽  
Rich Material

AbstractThe influence of non-stoichiometry on the solid-phase epitaxial growth of amorphized GaAs has been studied with in-situ Transmission Electron Microscopy (TEM). Ion-implantation has been used to produce microscopic non-stoichiometry via Ga and As implants and macroscopic non-stoichiometry via Ga or As implants. It has been demonstrated that amorphous GaAs recrystallizes into a thin single-crystal layer and a thick heavily twinned layer. Video images of the recrystallization process have been quantified for the first time to study the velocity of the crystalline/amorphous (c/a)-interface as a function of depth and ion species. Regrowth rates of the single crystal and twinned layers as functions of non-stoichiometry have been calculated. The phase transformation is rapid in Ga-rich material. In-situ TEM results are consistent with conventional in-situ Time Resolved Reflectivity, ex-situ Rutherford Backscattering Spectroscopy and Channelling measurements and ex-situ TEM.

Transmission Electron Microscopy of Epitaxial silicides grown by ultra high vacuum deposition

1989 ◽  
Vol 47 ◽  
pp. 462-463
Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Electron Diffraction ◽  
High Vacuum ◽  
High Energy ◽  
Energy Electron ◽  
Ultra High Vacuum ◽  
Ex Situ ◽  
Transmission Electron

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.

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