The buckling of thin EM specimens

Author(s):  
A.R. Thölén

Thin electron microscope specimens often contain irregular bend contours (Figs. 1-3). Very regular bend patterns have, however, been observed around holes in some ion-milled specimens. The purpose of this investigation is twofold. Firstly, to find the geometry of bent specimens and the elastic properties of extremely thin foils and secondly, to obtain more information about the background to the observed regular patterns.The specimen surface is described by z = f(x,y,p), where p is a parameter, eg. the radius of curvature of a sphere. The beam is entering along the z—direction, which coincides with the foil normal, FN, of the undisturbed crystal surface (z = 0). We have here used FN = [001]. Furthermore some low indexed reflections are chosen around the pole FN and in our fcc crystal the following g-vectors are selected:

Author(s):  
J. J. Kelsch ◽  
A. Holtz

A simple solution to the serious problem of specimen contamination in the electron microscope is presented. This is accomplished by the introduction of clean helium into the vacuum exactly at the specimen position. The local pressure gradient thus established inhibits the migration of hydrocarbon molecules to the specimen surface. The high ionization potential of He permits the use of relatively large volumes of the gas, without interfering with gun stability. The contamination rate is reduced on metal samples by a factor of 10.


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):  
H. Hashimoto ◽  
Y. Sugimoto ◽  
Y. Takai ◽  
H. Endoh

As was demonstrated by the present authors that atomic structure of simple crystal can be photographed by the conventional 100 kV electron microscope adjusted at “aberration free focus (AFF)” condition. In order to operate the microscope at AFF condition effectively, highly stabilized electron beams with small energy spread and small beam divergence are necessary. In the present observation, a 120 kV electron microscope with LaB6 electron gun was used. The most of the images were taken with the direct electron optical magnification of 1.3 million times and then magnified photographically.1. Twist boundary of ZnSFig. 1 is the image of wurtzite single crystal with twist boundary grown on the surface of zinc crystal by the reaction of sulphur vapour of 1540 Torr at 500°C. Crystal surface is parallel to (00.1) plane and electron beam is incident along the axis normal to the crystal surface. In the twist boundary there is a dislocation net work between two perfect crystals with a certain rotation angle.


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.


Author(s):  
S. McKernan ◽  
C. B. Carter

The oxidation of natural olivine has previously been performed on bulk samples and the reactions followed by preparation of TEM specimens from the annealed material. These results show that below ∼1000°C hematite and amorphous silica are formed, particularly around dislocations. At higher temperatures magnetite and some enstatite-like phase are formed. In both cases the olivine is left almost totally Fe depleted. By performing the oxidation on characterized thin TEM specimens it is possible to obtain more information on the nucleation and growth of the second phases formed. The conditions in a thin foil, however, are very different from those in the bulk especially with regard to surface effects. The nucleation of precipitates in particular may be expected to occur differently in these thin foils than in the bulk.TEM specimens of natural olivine (approximate composition Mg+Fe+Si2o4) which had been annealed at 1000°C for 1 hr were prepared by mechanical polishing and dimpling, followed by Ar ion milling to perforation. The specimens were characterized in the electron microscope and then heated in air in alumina boats to 900°C for between 30 and 180 minutes.


Author(s):  
P. R. Okamoto ◽  
N.Q. Lam ◽  
R. L. Lyles

During irradiation of thin foils in a high voltage electron microscope (HVEM) defect gradients will be set up between the foil surfaces and interior. In alloys defect gradients provide additional driving forces for solute diffusion since any preferential binding and/or exchange between solute atoms and mobile defects will couple a net flux of solute atoms to the defect fluxes. Thus, during irradiation large nonequilibrium compositional gradients can be produced near the foil surfaces in initially homogeneous alloys. A system of coupled reaction-rate and diffusion equations describing the build up of mobile defects and solute redistribution in thin foils and in a semi-infinite medium under charged-particle irradiation has been formulated. Spatially uniform and nonuniform damage production rates have been used to model solute segregation under electron and ion irradiation conditions.An example calculation showing the time evolution of the solute concentration in a 2000 Å thick foil during electron irradiation is shown in Fig. 1.


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