In Situ Annealing Observations of Silicon Cross-Sectional TEM Specimens

Author(s):  
E.M. Fiore ◽  
R.A. Herring

With conventional transmission electron microscopy (TEM), dynamic events are pieced together with micrographs from a multitude of specimens annealed at different temperatures over the range of interest. Real-time imaging of dynamic events in the microscope provides the ability to view the entire anneal temperature span with one specimen. As reported by Parker, cross-sectional TEM can be used to observe real-time kinetic phenomena in silicon. Fiore and Herring later reported a new technique for preparing cross-sectional specimens that are annealable to temperatures as high as 1300°C. Both of these recently developed techniques have been used to observe the amorphous-to-crystalline phase transformation and defect network formation in high-energy ion implanted silicon.Cross-sectional specimens were annealed in a Philips CM 12 transmission electron microscope equipped with a heating holder. The specimens were prepared from [111 ]-oriented silicon wafers implanted with 5.5 Mev Ga ions at a dose of lO15 cm-2. Using a ramp-up temperature from ∽30°C to 1000°C over a 5-minute period, the dynamic events were recorded on 3/4-inch video tape from a TEM TV system.

1993 ◽  
Vol 312 ◽  
Author(s):  
Richard Mirin ◽  
Mohan Krishnamurthy ◽  
James Ibbetson ◽  
Arthur Gossard ◽  
John English ◽  
...  

AbstractHigh temperature (≥ 650°C) MBE growth of AlAs and AlAs/GaAs superlattices on (100) GaAs is shown to lead to quasi-periodic facetting. We demonstrate that the facetting is only due to the AlAs layers, and growth of GaAs on top of the facets replanarizes the surface. We show that the roughness between the AlAs and GaAs layers increases with increasing number of periods in the superlattice. The roughness increases to form distinct facets, which rapidly grow at the expense of the (100) surface. Within a few periods of the initial facet formation, the (100) surface has disappeared and only the facet planes are visible in cross-sectional transmission electron micrographs. At this point, the reflection high-energy electron diffraction pattern is spotty, and the specular spot is a distinct chevron. We also show that the facetting becomes more pronounced as the substrate temperature is increased from 620°C to 710°C. Atomic force micrographs show that the valleys enclosed by the facets can be several microns long, but they may also be only several nanometers long, depending on the growth conditions.


1996 ◽  
Vol 441 ◽  
Author(s):  
J. Marien ◽  
T. Wagner ◽  
M. Rühle

AbstractThin Nb films were grown by MBE in a UHV chamber at two different temperatures (50°C and 950°C) on the (110) surface of TiO2 (rutile).At a growth temperature of 50°C, reflection high energy electron diffraction (RHEED) revealed epitaxial growth of Nb on rutile: (110)[001] TiO2 ¦¦ (100)[001] Nb. In addition, investigations with Auger electron spectroscopy (AES) revealed that a chemical reaction took place between the Nb overlayer and the TiO2 substrate at the initial growth stage. A 2 nm thick reaction layer at the Nb/TiO2 interface has been identified by means of conventional transmission electron microscopy (CTEM) and high-resolution transmission electron microscopy (HRTEM).At a substrate temperature of 950°C, during growth, the Nb film was oxidized completely, and NbO2 grew epitaxially on TiO2. The structure and the chemical composition of the overlayers have been investigated by RHEED, AES, CTEM and HRTEM. Furthermore, it was determined that the reaction of Nb with TiO2 is governed by the defect structure of the TiO2 and the relative oxygen affinities of Nb and TiO2.


1993 ◽  
Vol 313 ◽  
Author(s):  
I. Hashim ◽  
H.A. Atwater ◽  
Thomas J. Watson

ABSTRACTWe have investigated structural and magnetic properties of epitaxial Ni80Fe20 films grown on relaxed epitaxial Cu/Si (001) films. The crystallographic texture of these films was analyzed in situ by reflection high energy electron diffraction (RHEED), and ex situ by x-ray diffraction and cross-sectional transmission electron Microscopy (XTEM). In particular, RHEED intensities were recorded during epitaxial growth, and intensity profiles across Bragg rods were used to calculate the surface lattice constant, and hence, find the critical epitaxial thickness for which Ni80Fe20 grows pseudomorphically on Cu (100). XTEM analysis indicated that the epitaxial films had atomically-abrupt interfaces which was not the case for polycrystalline Cu and Ni80Fe20 film interfaces. The Magnetic properties of these epitaxial films were Measured in situ using Magneto-optic Kerr effect magnetometry and were compared with those of polycrystalline films grown on SiO2/Si. Large Hc (∼ 35 Oe) was observed for epitaxial Ni80Fe20 films less than 3.0 nm thick whereas for increasing thickness, Hc decreased approximately monotonically to a few Oersteds. Correlations were made between magnetic properties of these epitaxial films, the strain in the film and the interface roughness obtained from XTEM analysis.


1992 ◽  
Vol 280 ◽  
Author(s):  
I. Hashim ◽  
B. Park ◽  
H. A. Atwater

ABSTRACTEpitaxial Cu thin films have been grown on H-terminated Si(OOl) substrates at room temperature by D.C. ion-beam sputter deposition in ultrahigh vacuum. The development of orientation and microstructure during epitaxial growth from the initial stages of Cu growth up to Cu thicknesses of few hundred nm has been investigated. Analysis by in-situ reflection high energy electron diffraction, thin film x-ray diffraction, and plan-view and cross-sectional transmission electron microscopy indicates that the films are well textured with Cu(001)∥ Si(001) and Cu[100]∥ Si[110]. Interestingly, it is found that a distribution of orientations occurs at the early stages of Cu epitaxy on Si(001) surface, and that a (001) texture emerges gradually with increasing Cu thickness. The effect of silicide formation and deposition conditions on the crystalline quality of Cu epitaxy is also discussed.


1991 ◽  
Vol 220 ◽  
Author(s):  
Q. F. Xiao ◽  
J. R. Jimenez ◽  
L. J. Schowalter ◽  
L. Luo ◽  
T. E. Mitchell ◽  
...  

ABSTRACTEpitaxial Si layers have been grown under a variety of growth conditions on CoSi2 (001) by molecular beam epitaxy (MBE). The structural properties of the Si overgrowth were studied by in-situ Reflection High Energy Electron Diffraction (RHEED), as well as ex-situ MeV4He+ ion channeling and High Resolution Transmission Electron Microscopy (HRTEM). Strong influences of the CoSi2 surface reconstruction on the Si overgrowth have been observed. RHEED studies show islanding growth of Si on the CoSi2 (001) (3/√2 × √2)R45 reconstructed surface, but smooth growth of Si on the CoSi2 (001) {√2 × √2)R45 reconstructed surface, under the same growth conditions. The growth of Si on thin layers of CoSi2 (2nm-6nm) with (√2 × √2)R45 reconstructed surface at 460°C results in high crystalline quality for the Si top layer, as indicated by good channeling minimum yield (Xmin < 6%), but cross-sectional TEM shows that the CoSi2 layers are discontinuous. We also report preliminary results on Si grown on a 2 × 2 reconstructed CoSi2 (001) surface.


1994 ◽  
Vol 357 ◽  
Author(s):  
T. Wagner ◽  
M. Ruhle

AbstractThe A1/MgO system has been used as a model system to study growth processes and structure at metal/ceramic interfaces. Aluminum films were grown on air-cleaved MgO (100) substrates in ultra high vacuum (UHV) by molecular beam epitaxy (MBE). The substrates and films were characterized by reflection high energy electron diffraction (RHEED), x-ray diffraction (XRD), conventional transmission electron microscopy (CTEM), and high resolution transmission electron microscopy (HREM). XRD measurements exhibited a pronounced {100} texture. Employing electron diffraction in the TEM on cross sectional samples, we observed the following orientation relationship between Al and MgO: (100)A1 II (100)MgO; [010]A1 II [010]MgO. The atomistic structure of the interface was investigated by HREM. Regions of structural defects can be identified clearly at the interface.


2007 ◽  
Vol 15 (2) ◽  
pp. 48-51
Author(s):  
Bernt Johannessen ◽  
David J. Llewellyn ◽  
Patrick Kluth ◽  
Mark C. Ridgway

Nanoparticles (1-10 nm in diameter) are particularly susceptible to disorder, amorphization, deformation and/or dissolution upon ion irradiation as compared to their bulk counterparts, which is a consequence of the enhanced surface area to volume ratio of the former (structural disorder is often observed to be preferentially located at the surface). Synchrotron-radiation-based analytical techniques are ideally suited for the elucidation of structural perturbations as compared to the bulk material. Such techniques are commonly complemented by cross-sectional transmission electron microscopy (XTEM). XTEM offers invaluable information with respect to shape and morphology of the nanoparticles.For the present work, Cu nanoparticles were synthesized within a 2 μm amorphous SiO2 matrix on a 520 μm Si support by ion implantation and thermal annealing following a procedure described elsewhere. In order to study the influence that ion irradiation has on the nanoparticles, the sample was then irradiated with 1x1015 ions / cm2 high-energy (5 MeV) Sn+ ions.


1990 ◽  
Vol 199 ◽  
Author(s):  
R. J. Young ◽  
E. C. G. Kirk ◽  
D. A. Williams ◽  
H. Ahmed

ABSTRACTA new technique using a focused ion beam has been developed for the fabrication of transmission electron microscopy specimens in pre-selected regions. The method has been proven in the fabrication of both cross-sectional and planar specimens, with no induced artefacts. The lateral accuracy achievable in the selection of an area for cross-sectional analysis is better than one micrometre. The technique has been applied to a number of silicon and III-V based integrated circuits, and is expected to be suitable for many other materials and structures.


Author(s):  
С.В. Рябцев ◽  
Д.А.А. Гхариб ◽  
С.Ю. Турищев ◽  
Л.А. Обвинцева ◽  
А.В. Шапошник ◽  
...  

PdO films were obtained by thermal deposition of palladium metal with a thickness of 30 and 90 nm, followed by its oxidation in air at different temperatures. PdO oxide films are characterized by transmission electron microscopy (TEM) and reflection high-energy electron diffraction (RHEED). Data on the semiconductor properties and gas sensitivity to different concentrations of ozone in the air are obtained. The optimal temperature conditions for the oxidation of the films are established, which ensure their uniform phase composition and the absence of electrical noise during the detection of gases. The mechanism of the electrical noise appearance in ultrathin films associated with their fragmentation during oxidative annealing is proposed and justified. The possibility of detecting ozone impurities in the air below the maximum permissible concentration (MPC) by PdO semiconductor films is shown.


Author(s):  
I.M. Robertson ◽  
T.C. Lee ◽  
D.K. Dewald ◽  
H.K. Birnbaum

The in-situ TEM straining technique has been used to investigate the micromechanisms of deformation and fracture in several ductile and semi-brittle systems. Attention has been focussed on the dislocation structures ahead of advancing cracks and on the interaction between lattice dislocations and grain boundaries.The deformation experiments were performed in-situ in a transmission electron microscope equipped with a video camera system. The dynamic events were recorded on video tape with a time resolution of l/30th of a second. Static interactions were recorded using the regular microscope plate system. The straining stage deforms the samples in Mode I and can operate at a displacement rate of 4 in sec-1.An example of one of the possible interactions between lattice dislocations and a ∑- 3 ([ll)/60°) grain boundary in 310 stainless steel is shown in the micrograph in Figure 1. The dislocations on slip systems A (a/2[110)1 (ll) 1 ) and B (a/2[101] (11) 1 ) impinge on the grain boundary, generating slip systems C (a/2[l0) 2/(111) 2) and D (a/2[l0) 2/(111) 2). To understand this effect three conditions were considered:


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