Preparation of Elemental Thin Foils for Exploring Collision-Induced Atomic Processes

2021 ◽  
pp. 163-170
Author(s):  
Ch Vikar Ahmad ◽  
Ruchika Gupta ◽  
Kajol Chakraborty ◽  
G. R. Umapathy ◽  
Punita Verma
Keyword(s):  
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):  
L.J. Chen ◽  
Y.F. Hsieh

One measure of the maturity of a device technology is the ease and reliability of applying contact metallurgy. Compared to metal contact of silicon, the status of GaAs metallization is still at its primitive stage. With the advent of GaAs MESFET and integrated circuits, very stringent requirements were placed on their metal contacts. During the past few years, extensive researches have been conducted in the area of Au-Ge-Ni in order to lower contact resistances and improve uniformity. In this paper, we report the results of TEM study of interfacial reactions between Ni and GaAs as part of the attempt to understand the role of nickel in Au-Ge-Ni contact of GaAs.N-type, Si-doped, (001) oriented GaAs wafers, 15 mil in thickness, were grown by gradient-freeze method. Nickel thin films, 300Å in thickness, were e-gun deposited on GaAs wafers. The samples were then annealed in dry N2 in a 3-zone diffusion furnace at temperatures 200°C - 600°C for 5-180 minutes. Thin foils for TEM examinations were prepared by chemical polishing from the GaA.s side. TEM investigations were performed with JE0L- 100B and JE0L-200CX electron microscopes.


Author(s):  
N. E. Paton ◽  
D. de Fontaine ◽  
J. C. Williams

The electron microscope has been used to study the diffusionless β → β + ω transformation occurring in certain titanium alloys at low temperatures. Evidence for such a transformation was obtained by Cometto et al by means of x-ray diffraction and resistivity measurements on a Ti-Nb alloy. The present work shows that this type of transformation can occur in several Ti alloys of suitable composition, and some of the details of the transformation are elucidated by means of direct observation in the electron microscope.Thin foils were examined in a Philips EM-300 electron microscope equipped with a uniaxial tilt, liquid nitrogen cooled, cold stage and a high resolution dark field device. Selected area electron diffraction was used to identify the phases present and the ω-phase was imaged in dark field by using a (101)ω reflection. Alloys were water quenched from 950°C, thinned, and mounted between copper grids to minimize temperature gradients in the foil.


Author(s):  
E. U. Lee ◽  
P. A. Garner ◽  
J. S. Owens

Evidence for ordering (1-6) of interstitial impurities (O and C) has been obtained in b.c.c. metals, such as niobium and tantalum. In this paper we report the atomic and microstructural changes in an oxygenated c.p.h. metal (alpha titanium) as observed by transmission electron microscopy and diffraction.Oxygen was introduced into zone-refined iodide titanium sheets of 0.005 in. thickness in an atmosphere of oxygen and argon at 650°C, homogenized at 800°C and furnace-cooled in argon. Subsequently, thin foils were prepared by electrolytic polishing and examined in a JEM-7 electron microscope, operated at 100 KV.


Author(s):  
E. A. Kenik ◽  
J. Bentley

Cliff and Lorimer (1) have proposed a simple approach to thin foil x-ray analy sis based on the ratio of x-ray peak intensities. However, there are several experimental pitfalls which must be recognized in obtaining the desired x-ray intensities. Undesirable x-ray induced fluorescence of the specimen can result from various mechanisms and leads to x-ray intensities not characteristic of electron excitation and further results in incorrect intensity ratios.In measuring the x-ray intensity ratio for NiAl as a function of foil thickness, Zaluzec and Fraser (2) found the ratio was not constant for thicknesses where absorption could be neglected. They demonstrated that this effect originated from x-ray induced fluorescence by blocking the beam with lead foil. The primary x-rays arise in the illumination system and result in varying intensity ratios and a finite x-ray spectrum even when the specimen is not intercepting the electron beam, an ‘in-hole’ spectrum. We have developed a second technique for detecting x-ray induced fluorescence based on the magnitude of the ‘in-hole’ spectrum with different filament emission currents and condenser apertures.


Author(s):  
R. Hutchings ◽  
I.P. Jones ◽  
M.H. Loretto ◽  
R.E. Smallman

There is increasing interest in X-ray microanalysis of thin specimens and the present paper attempts to define some of the factors which govern the spatial resolution of this type of microanalysis. One of these factors is the spreading of the electron probe as it is transmitted through the specimen. There will always be some beam-spreading with small electron probes, because of the inevitable beam divergence associated with small, high current probes; a lower limit to the spatial resolution is thus 2αst where 2αs is the beam divergence and t the specimen thickness.In addition there will of course be beam spreading caused by elastic and inelastic interaction between the electron beam and the specimen. The angle through which electrons are scattered by the various scattering processes can vary from zero to 180° and it is clearly a very complex calculation to determine the effective size of the beam as it propagates through the specimen.


Author(s):  
W. T. Donlon ◽  
S. Shinozaki ◽  
E. M. Logothetis ◽  
W. Kaizer

Since point defects have a limited solubility in the rutile (TiO2) lattice, small deviations from stoichiometry are known to produce crystallographic shear (CS) planes which accomodate local variations in composition. The material used in this study was porous polycrystalline TiO2 (60% dense), in the form of 3mm. diameter disks, 1mm thick. Samples were mechanically polished, ion-milled by conventional techniques, and initially examined with the use of a Siemens EM102. The electron transparent thin foils were then heat-treated under controlled atmospheres of CO/CO2 and H2 and reexamined in the same manner.The “as-received” material contained mostly TiO2 grains (∼5μm diameter) which had no extended defects. Several grains however, aid exhibit a structure similar to micro-twinned grains observed in reduced rutile. Lattice fringe images (Fig. 1) of these grains reveal that the adjoining layers are not simply twin related variants of a single TinO2n-1 compound. Rather these layers (100 - 250 Å wide) are alternately comprised of stoichiometric TiO2 (rutile) and reduced TiO2 in the form of Ti8O15, with the Ti8O15 layers on either side of the TiO2 being twin related.


Author(s):  
D.I. Potter ◽  
A. Taylor

Thermal aging of Ni-12.8 at. % A1 and Ni-12.7 at. % Si produces spatially homogeneous dispersions of cuboidal γ'-Ni3Al or Ni3Si precipitate particles arrayed in the Ni solid solution. We have used 3.5-MeV 58Ni+ ion irradiation to examine the effect of irradiation during precipitation on precipitate morphology and distribution. The nearness of free surfaces produced unusual morphologies in foils thinned prior to irradiation. These thin-foil effects will be important during in-situ investigations of precipitation in the HVEM. The thin foil results can be interpreted in terms of observations from bulk irradiations which are described first.Figure 1a is a dark field image of the γ' precipitate 5000 Å beneath the surface(∿1200 Å short of peak damage) of the Ni-Al alloy irradiated in bulk form. The inhomogeneous spatial distribution of γ' results from the presence of voids and dislocation loops which can be seen in the bright field image of the same area, Fig. 1b.


Author(s):  
S. Naka ◽  
R. Penelle ◽  
R. Valle

The in situ experimentation technique in HVEM seems to be particularly suitable to clarify the processes involved in recrystallization. The material under investigation was unidirectionally cold-rolled titanium of commercial purity. The problem was approached in two different ways. The three-dimensional analysis of textures was used to describe the texture evolution during the primary recrystallization. Observations of bulk-annealed specimens or thin foils annealed in the microscope were also made in order to provide information concerning the mechanisms involved in the formation of new grains. In contrast to the already published work on titanium, this investigation takes into consideration different values of the cold-work ratio, the temperature and the annealing time.Two different models are commonly used to explain the recrystallization textures i.e. the selective grain growth model (Beck) or the oriented nucleation model (Burgers). The three-dimensional analysis of both the rolling and recrystallization textures was performed to identify the mechanismsl involved in the recrystallization of titanium.


Author(s):  
N. Ridley ◽  
S.A. Al-Salman ◽  
G.W. Lorimer

The application of the technique of analytical electron microscopy to the study of partitioning of Mn (1) and Cr (2) during the austenite-pearlite transformation in eutectoid steels has been described in previous papers. In both of these investigations, ‘in-situ’ analyses of individual cementite and ferrite plates in thin foils showed that the alloying elements partitioned preferentially to cementite at the transformation front at higher reaction temperatures. At lower temperatures partitioning did not occur and it was possible to identify a ‘no-partition’ temperature for each of the steels examined.In the present work partitioning during the pearlite transformation has been studied in a eutectoid steel containing 1.95 wt% Si. Measurements of pearlite interlamellar spacings showed, however, that except at the highest reaction temperatures the spacing would be too small to make the in-situ analysis of individual cementite plates possible, without interference from adjacent ferrite lamellae. The minimum diameter of the analysis probe on the instrument used, an EMMA-4 analytical electron microscope, was approximately 100 nm.


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