Oxygen Bubble Formation and Transformation During High-Dose Oxygen Implantation and Annealing of Silicon

1990 ◽  
Vol 201 ◽  
Author(s):  
S. J. Krause ◽  
S. Seraphin ◽  
B. L. Chen ◽  
B. Cordts ◽  
P. Roitman

AbstractThe formation of bubbles during high dose implantation of oxygen into silicon, and the subsequent transformation of the bubbles during annealing, were studied with transmission electron microscopy (TEM). There was a threshold for bubble formation at a minimum dose of 0.3 × 1018 oxygen/cm2 and a lower temperature of 550°C. As dose increased the bubbles grew larger and the bubble trails lengthened. However, increasing beam current by a factor of 10 or increasing temperature to 700°C did not affect bubble formation. Bubble evolution during intermediate temperature annealing was also studied using TEM techniques. For 2 hour anneals between 1000 and 1100°C the oxygen bubbles transform into SiO2 particles by first forming a “shell” of SiO2, which then facets, grows inward, and finally completely transforms the bubble into an oxide particle. At temperatures greater than 1100°C the oxide particles dissolve by outdiffusion of the oxygen to the wafer surface.

1994 ◽  
Vol 373 ◽  
Author(s):  
P. Zheng ◽  
R.G. Saint-Jacques ◽  
B. Terreault ◽  
G. Veilleux

AbstractIn order to explain the relatively easy laser-induced desorption of hydrogen implanted in silicon, and particularly the lower temperature needed for desorption at higher implantation energy, the microstructural modifications produced by laser pulses were studied by means of transmission electron microscopy. The structural damage, such as defect clusters and hydrogen gas bubbles was observed. In the case of low dose implantation (H/Si ≤ 15&), most of the bubbles were produced during laser annealing rather than during implantation. This bubble formation in the course of desorption explains the higher temperature needed. When blisters are already present on the as-implanted surface, desorption starts at a lower temperature.


Author(s):  
S J. Krause ◽  
J.D. Lee ◽  
B.L. Chen ◽  
S. Seraphin ◽  
B. Cordts ◽  
...  

Silicon-on-insulator (SOI) material fabricated by high dose oxygen implantation (SIMOX) is a material increasingly used for higher speed and radiation hard circuits. During implantation a variety of structural changes occur, including the formation of defects, bubbles, precipitates, and the buried oxide layer. The topic of bubble formation and evolution has received only limited study. Sjoreen et al. first reported the presence of spherical, randomly distributed precipitates near the top surface of the silicon layer. El-Ghor et al. further examined these precipitates and proposed that they were cavities filled with oxygen. Maszara confirmed the presence of spheroids filled with oxygen in the silicon top surface region in the 1mA cm-2 as-implanted samples. In this work, transmission electron microscopy (TEM) techniques were used to investigate the effect of implantation conditions on the bubble formation and the effect of subsequent annealing conditions on the evolution of bubbles.


2014 ◽  
Vol 29 (S1) ◽  
pp. S84-S88 ◽  
Author(s):  
Anita M. D'Angelo ◽  
Nathan A. S. Webster ◽  
Alan L. Chaffee

X-ray diffraction (XRD) was used to determine the temperature at which the transformation of Ce2O(CO3)2·H2O to ceria (CeO2) occurs under both a flow of nitrogen and air as a function of temperature. The Ce2O(CO3)2·H2O synthesised from Ce(NO3)3·6H2O and urea was further investigated using thermal gravimetric analysis (TGA), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). XRD results indicate that, under a flow of nitrogen, CeO2 is formed at temperatures greater than 500 °C and that this occurs via an as yet unidentified intermediate phase, which is present between 430 and 540 °C. Results obtained by the XRD correspond to those obtained using TGA, which show weight  losses commencing at 430 and at 465 °C. No further weight loss occurs above 540 °C, because of the formation of CeO2 as the stable product. The crystallite size was also determined and observed to increase with increasing temperature. Under a flow of air the transformation occurred at a lower temperature, as CeO2 was formed at 250 °C. SEM and TEM reveal the particles have a rod-shaped morphology which is retained after calcination. These results may be used to optimise synthesis methods to minimise crystallite size growth and reduce sintering that is undesirable in many applications, particularly catalysis.


Author(s):  
J. F. DeNatale ◽  
D. G. Howitt

The electron irradiation of silicate glasses containing metal cations produces various types of phase separation and decomposition which includes oxygen bubble formation at intermediate temperatures figure I. The kinetics of bubble formation are too rapid to be accounted for by oxygen diffusion but the behavior is consistent with a cation diffusion mechanism if the amount of oxygen in the bubble is not significantly different from that in the same volume of silicate glass. The formation of oxygen bubbles is often accompanied by precipitation of crystalline phases and/or amorphous phase decomposition in the regions between the bubbles and the detection of differences in oxygen concentration between the bubble and matrix by electron energy loss spectroscopy cannot be discerned (figure 2) even when the bubble occupies the majority of the foil depth.The oxygen bubbles are stable, even in the thin foils, months after irradiation and if van der Waals behavior of the interior gas is assumed an oxygen pressure of about 4000 atmospheres must be sustained for a 100 bubble if the surface tension with the glass matrix is to balance against it at intermediate temperatures.


Author(s):  
J. R. Michael ◽  
K. A. Taylor

Although copper is considered an incidental or trace element in many commercial steels, some grades contain up to 1-2 wt.% Cu for precipitation strengthening. Previous electron microscopy and atom-probe/field-ion microscopy (AP/FIM) studies indicate that the precipitation of copper from ferrite proceeds with the formation of Cu-rich bcc zones and the subsequent transformation of these zones to fcc copper particles. However, the similarity between the atomic scattering amplitudes for iron and copper and the small misfit between between Cu-rich particles and the ferrite matrix preclude the detection of small (<5 nm) Cu-rich particles by conventional transmission electron microscopy; such particles have been imaged directly only by FIM. Here results are presented whereby the Cu Kα x-ray signal was used in a dedicated scanning transmission electron microscope (STEM) to image small Cu-rich particles in a steel. The capability to detect these small particles is expected to be helpful in understanding the behavior of copper in steels during thermomechanical processing and heat treatment.


Author(s):  
T. L. Benning ◽  
P. Ingram ◽  
J. D. Shelburne

Two benzofuran derivatives, chlorpromazine and amiodarone, are known to produce inclusion bodies in human tissues. Prolonged high dose chlorpromazine therapy causes hyperpigmentation of the skin with electron-dense inclusion bodies present in dermal histiocytes and endothelial cells ultrastructurally. The nature of the deposits is not known although a drug-melanin complex has been hypothesized. Amiodarone may also cause cutaneous hyperpigmentation and lamellar lysosomal inclusion bodies have been demonstrated within the cells of multiple organ systems. These lamellar bodies are believed to be the product of an amiodarone-induced phospholipid storage disorder. We performed transmission electron microscopy (TEM) and energy dispersive x-ray microanalysis (EDXA) on tissue samples from patients treated with these drugs, attempting to detect the sulfur atom of chlorpromazine and the iodine atom of amiodarone within their respective inclusion bodies.A skin biopsy from a patient with hyperpigmentation due to prolonged chlorpromazine therapy was fixed in 4% glutaraldehyde and processed without osmium tetroxide or en bloc uranyl acetate for Epon embedding.


Author(s):  
R.D. Leapman ◽  
S.B. Andrews

Elemental mapping of biological specimens by electron energy loss spectroscopy (EELS) can be carried out both in the scanning transmission electron microscope (STEM), and in the energy-filtering transmission electron microscope (EFTEM). Choosing between these two approaches is complicated by the variety of specimens that are encountered (e.g., cells or macromolecules; cryosections, plastic sections or thin films) and by the range of elemental concentrations that occur (from a few percent down to a few parts per million). Our aim here is to consider the strengths of each technique for determining elemental distributions in these different types of specimen.On one hand, it is desirable to collect a parallel EELS spectrum at each point in the specimen using the ‘spectrum-imaging’ technique in the STEM. This minimizes the electron dose and retains as much quantitative information as possible about the inelastic scattering processes in the specimen. On the other hand, collection times in the STEM are often limited by the detector read-out and by available probe current. For example, a 256 x 256 pixel image in the STEM takes at least 30 minutes to acquire with read-out time of 25 ms. The EFTEM is able to collect parallel image data using slow-scan CCD array detectors from as many as 1024 x 1024 pixels with integration times of a few seconds. Furthermore, the EFTEM has an available beam current in the µA range compared with just a few nA in the STEM. Indeed, for some applications this can result in a factor of ~100 shorter acquisition time for the EFTEM relative to the STEM. However, the EFTEM provides much less spectral information, so that the technique of choice ultimately depends on requirements for processing the spectrum at each pixel (viz., isolated edges vs. overlapping edges, uniform thickness vs. non-uniform thickness, molar vs. millimolar concentrations).


Author(s):  
A. De Veirman ◽  
J. Van Landuyt ◽  
K.J. Reeson ◽  
R. Gwilliam ◽  
C. Jeynes ◽  
...  

In analogy to the formation of SIMOX (Separation by IMplanted OXygen) material which is presently the most promising silicon-on-insulator technology, high-dose ion implantation of cobalt in silicon is used to synthesise buried CoSi2 layers. So far, for high-dose ion implantation of Co in Si, only formation of CoSi2 is reported. In this paper it will be shown that CoSi inclusions occur when the stoichiometric Co concentration is exceeded at the peak of the Co distribution. 350 keV Co+ ions are implanted into (001) Si wafers to doses of 2, 4 and 7×l017 per cm2. During the implantation the wafer is kept at ≈ 550°C, using beam heating. The subsequent annealing treatment was performed in a conventional nitrogen flow furnace at 1000°C for 5 to 30 minutes (FA) or in a dual graphite strip annealer where isochronal 5s anneals at temperatures between 800°C and 1200°C (RTA) were performed. The implanted samples have been studied by means of Rutherford Backscattering Spectroscopy (RBS) and cross-section Transmission Electron Microscopy (XTEM).


1998 ◽  
Vol 536 ◽  
Author(s):  
V. P. Popov ◽  
A. K. Gutakovsky ◽  
I. V. Antonova ◽  
K. S. Zhuravlev ◽  
E. V. Spesivtsev ◽  
...  

AbstractA study of Si:H layers formed by high dose hydrogen implantation (up to 3x107cm-2) using pulsed beams with mean currents up 40 mA/cm2 was carried out in the present work. The Rutherford backscattering spectrometry (RBS), channeling of He ions, and transmission electron microscopy (TEM) were used to study the implanted silicon, and to identify the structural defects (a-Si islands and nanocrystallites). Implantation regimes used in this work lead to creation of the layers, which contain hydrogen concentrations higher than 15 at.% as well as the high defect concentrations. As a result, the nano- and microcavities that are created in the silicon fill with hydrogen. Annealing of this silicon removes the radiation defects and leads to a nanocrystalline structure of implanted layer. A strong energy dependence of dechanneling, connected with formation of quasi nanocrystallites, which have mutual small angle disorientation (<1.50), was found after moderate annealing in the range 200-500°C. The nanocrystalline regions are in the range of 2-4 nm were estimated on the basis of the suggested dechanneling model and transmission electron microscopy (TEM) measurements. Correlation between spectroscopic ellipsometry, visible photoluminescence, and sizes of nanocrystallites in hydrogenated nc-Si:H is observed.


1987 ◽  
Vol 93 ◽  
Author(s):  
Witold P. Maszara

ABSTRACTSilicon wafers with and without protective1Ahermil oxide were implanted with oxygen at 150keV with doses 1.6 – 2.0×1018 cm−2. Transmission electron microscopy (TEM) and secondary ion mass spectroscopy (SIMS) were used to study the top silicon layer remaining above the implanted buried oxide. regular array of spheroidal voids filled with oxygen gas was observed only in the samples that were not protected by the oxide. The voids were aligned into individual columns whose crystallographic orientation with respect to the host silicon lattice matched the direction of the implantation. The origin and the kinetics of their formation are discussed.


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