FIB ‐ TEM analysis of cometary material in 10 Stardust foil craters

2020 ◽  
Vol 55 (6) ◽  
pp. 1349-1370 ◽  
Author(s):  
Brendan A. Haas ◽  
Christine Floss ◽  
Rhonda M. Stroud ◽  
Ryan C. Ogliore
Author(s):  
D.E. Brownlee ◽  
A.L. Albee

Comets are primitive, kilometer-sized bodies that formed in the outer regions of the solar system. Composed of ice and dust, comets are generally believed to be relic building blocks of the outer solar system that have been preserved at cryogenic temperatures since the formation of the Sun and planets. The analysis of cometary material is particularly important because the properties of cometary material provide direct information on the processes and environments that formed and influenced solid matter both in the early solar system and in the interstellar environments that preceded it.The first direct analyses of proven comet dust were made during the Soviet and European spacecraft encounters with Comet Halley in 1986. These missions carried time-of-flight mass spectrometers that measured mass spectra of individual micron and smaller particles. The Halley measurements were semi-quantitative but they showed that comet dust is a complex fine-grained mixture of silicates and organic material. A full understanding of comet dust will require detailed morphological, mineralogical, elemental and isotopic analysis at the finest possible scale. Electron microscopy and related microbeam techniques will play key roles in the analysis. The present and future of electron microscopy of comet samples involves laboratory study of micrometeorites collected in the stratosphere, in-situ SEM analysis of particles collected at a comet and laboratory study of samples collected from a comet and returned to the Earth for detailed study.


Author(s):  
S. Shinozaki ◽  
J. W. Sprys

In reaction sintered SiC (∽ 5um average grain size), about 15% of the grains were found to have long-period structures, which were identifiable by transmission electron microscopy (TEM). In order to investigate the stability of the long-period polytypes at high temperature, crystal structures as well as microstructural changes in the long-period polytypes were analyzed as a function of time in isothermal annealing.Each polytype was analyzed by two methods: (1) Electron diffraction, and (2) Electron micrograph analysis. Fig. 1 shows microdensitometer traces of ED patterns (continuous curves) and calculated intensities (vertical lines) along 10.l row for 6H and 84R (Ramsdell notation). Intensity distributions were calculated based on the Zhdanov notation of (33) for 6H and [ (33)3 (32)2 ]3 for 84R. Because of the dynamical effect in electron diffraction, the observed intensities do not exactly coincide with those intensities obtained by structure factor calculations. Fig. 2 shows the high resolution TEM micrographs, where the striped patterns correspond to direct resolution of the structural lattice periodicities of 6H and 84R structures and the spacings shown in the figures are as expected for those structures.


Author(s):  
N. Qiu ◽  
J. E. Wittig

PtCo hard magnets have specialized applications owing to their relatively high coercivity combined with corrosion resistance and ductility. Increased intrinsic coercivity has been recently obtained by rapid solidification processing of PtCo alloys containing boron. After rapid solidification by double anvil splat quenching and subsequent annealing for 30 minutes at 650°C, an alloy with composition Pt42Co45B13 (at.%) exhibited intrinsic coercivity up to 14kOe. This represents a significant improvement compared to the average coercivities in conventional binary PtCo alloys of 5 to 8 kOe.Rapidly solidified specimens of Pt42Co45B13 (at.%) were annealed at 650°C and 800°C for 30 minutes. The magnetic behavior was characterized by measuring the coercive force (Hc). Samples for TEM analysis were mechanically thinned to 100 μm, dimpled to about 30 nm, and ion milled to electron transparency in a Gatan Duomill at 5 kV and 1 mA gun current. The incident ion beam angle was set at 15° and the samples were liquid nitrogen cooled during milling. These samples were analyzed with a Philips CM20T TEM/STEM operated at 200 kV.


Author(s):  
Charles W. Allen

Irradiation effects studies employing TEMs as analytical tools have been conducted for almost as many years as materials people have done TEM, motivated largely by materials needs for nuclear reactor development. Such studies have focussed on the behavior both of nuclear fuels and of materials for other reactor components which are subjected to radiation-induced degradation. Especially in the 1950s and 60s, post-irradiation TEM analysis may have been coupled to in situ (in reactor or in pile) experiments (e.g., irradiation-induced creep experiments of austenitic stainless steels). Although necessary from a technological point of view, such experiments are difficult to instrument (measure strain dynamically, e.g.) and control (temperature, e.g.) and require months or even years to perform in a nuclear reactor or in a spallation neutron source. Consequently, methods were sought for simulation of neutroninduced radiation damage of materials, the simulations employing other forms of radiation; in the case of metals and alloys, high energy electrons and high energy ions.


Author(s):  
M. J. Carr ◽  
J. F. Shewbridge ◽  
T. O. Wilford

Strong solid state bonds are routinely produced between physical vapor deposited (PVD) silver coatings deposited on sputter cleaned surfaces of two dissimilar metal parts. The low temperature (200°C) and short time (10 min) used in the bonding cycle are advantageous from the standpoint of productivity and dimensional control. These conditions unfortunately produce no microstructural changes at or near the interface that are detectable by optical, SEM, or microprobe examination. Microstructural problems arising at these interfaces could therefore easily go undetected by these techniques. TEM analysis has not been previously applied to this problem because of the difficulty in specimen preparation. The purpose of this paper is to describe our technique for preparing specimens from solid state bonds and to present our initial observations of the microstructural details of such bonds.


Author(s):  
R.A. Herring

Rapid thermal annealing (RTA) of ion-implanted Si is important for device fabrication. The defect structures of 2.5, 4.0, and 6.0 MeV As-implanted silicon irradiated to fluences of 2E14, 4E14, and 6E14, respectively, have been analyzed by electron diffraction both before and after RTA at 1100°C for 10 seconds. At such high fluences and energies the implanted As ions change the Si from crystalline to amorphous. Three distinct amorphous regions emerge due to the three implantation energies used (Fig. 1). The amorphous regions are separated from each other by crystalline Si (marked L1, L2, and L3 in Fig. 1) which contains a high concentration of small defect clusters. The small defect clusters were similar to what had been determined earlier as being amorphous zones since their contrast was principally of the structure-factor type that arises due to the difference in extinction distance between the matrix and damage regions.


Author(s):  
Stanley J. Klepeis ◽  
J.P. Benedict ◽  
R.M Anderson

The ability to prepare a cross-section of a specific semiconductor structure for both SEM and TEM analysis is vital in characterizing the smaller, more complex devices that are now being designed and manufactured. In the past, a unique sample was prepared for either SEM or TEM analysis of a structure. In choosing to do SEM, valuable and unique information was lost to TEM analysis. An alternative, the SEM examination of thinned TEM samples, was frequently made difficult by topographical artifacts introduced by mechanical polishing and lengthy ion-milling. Thus, the need to produce a TEM sample from a unique,cross-sectioned SEM sample has produced this sample preparation technique.The technique is divided into an SEM and a TEM sample preparation phase. The first four steps in the SEM phase: bulk reduction, cleaning, gluing and trimming produces a reinforced sample with the area of interest in the center of the sample. This sample is then mounted on a special SEM stud. The stud is inserted into an L-shaped holder and this holder is attached to the Klepeis polisher (see figs. 1 and 2). An SEM cross-section of the sample is then prepared by mechanically polishing the sample to the area of interest using the Klepeis polisher. The polished cross-section is cleaned and the SEM stud with the attached sample, is removed from the L-shaped holder. The stud is then inserted into the ion-miller and the sample is briefly milled (less than 2 minutes) on the polished side. The sample on the stud may then be carbon coated and placed in the SEM for analysis.


Author(s):  
U. Dahmen ◽  
K.H. Westmacott

Despite the increased use of convergent beam diffraction, symmetry concepts in their more general form are not commonly applied as a practical tool in electron microscopy. Crystal symmetry provides an abundance of information that can be used to facilitate and improve the TEM analysis of crystalline solids. This paper draws attention to some aspects of symmetry that can be put to practical use in the analysis of structures and morphologies of two-phase materials.It has been shown that the symmetry of the matrix that relates different variants of a precipitate can be used to determine the axis of needle- or lath-shaped precipitates or the habit plane of plate-shaped precipitates. By tilting to a special high symmetry orientation of the matrix and by measuring angles between symmetry-related variants of the precipitate it is possible to find their habit from a single micrograph.


Author(s):  
J.P. Benedict ◽  
Ron Anderson ◽  
S. J. Klepeis

Traditional specimen preparation procedures for non-biological samples, especially cross section preparation procedures, involves subjecting the specimen to ion milling for times ranging from minutes to tens of hours. Long ion milling time produces surface alteration, atomic number and rough-surface topography artifacts, and high temperatures. The introduction of new tools and methods in this laboratory improved our ability to mechanically thin specimens to a point where ion milling time was reduced to one to ten minutes. Very short ion milling times meant that ion milling was more of a cleaning operation than a thinning operation. The preferential thinning and the surface topography that still existed in briefly ion milled samples made the study of interfaces between materials such as platinum silicide and silicon difficult. These two problems can be eliminated by completely eliminating the ion milling step and mechanically polishing the sample to TEM transparency with the procedure outlined in this communication. Previous successful efforts leading to mechanically thinned specimens have shown that problems center on tool tilt control, removal of polishing damage, and specimen cleanliness.


2003 ◽  
Vol 762 ◽  
Author(s):  
Hwang Huh ◽  
Jung H. Shin

AbstractAmorphous silicon (a-Si) films prepared on oxidized silicon wafer were crystallized to a highly textured form using contact printing of rolled and annealed nickel tapes. Crystallization was achieved by first annealing the a-Si film in contact with patterned Ni tape at 600°C for 20 min in a flowing forming gas (90 % N2, 10 % H2) environment, then removing the Ni tape and further annealing the a-Si film in vacuum for2hrsat600°C. An array of crystalline regions with diameters of up to 20 μm could be formed. Electron microscopy indicates that the regions are essentially single-crystalline except for the presence of twins and/or type A-B formations, and that all regions have the same orientation in all 3 directions even when separated by more than hundreds of microns. High resolution TEM analysis shows that formation of such orientation-controlled, nearly single crystalline regions is due to formation of nearly single crystalline NiSi2 under the point of contact, which then acts as the template for silicide-induced lateral crystallization. Furthermore, the orientation relationship between Si grains and Ni tape is observed to be Si (110) || Ni (001)


Sign in / Sign up

Export Citation Format

Share Document