Valence determinations and oxybarometry on FIB‐sectioned olivine and pyroxene using correlated Ti, V, and Cr micro‐XAFS spectroscopy: Evaluation of ion‐milling effects and application to Antarctic micrometeorite grains

2020 ◽  
Author(s):  
S. R. Sutton ◽  
A. J. Brearley ◽  
E. DobricĂ ◽  
A. Lanzirotti ◽  
M. Newville ◽  
...  
Keyword(s):  
Ion Milling ◽  
Xafs Spectroscopy

High Voltage Electron Microscopy of Ion-Milled Dental Enamel

1974 ◽  
Vol 32 ◽  
pp. 60-61
Author(s):  
L. D. Ackerman ◽  
S. H. Y. Wei
Keyword(s):  
Electron Microscopy ◽  
High Voltage ◽  
Third Molar ◽  
Polarized Light ◽  
Dental Enamel ◽  
Longitudinal Section ◽  
Ion Milling ◽  
High Voltage Electron Microscopy ◽  
Voltage Electron ◽  
High Voltage Electron

Mature human dental enamel has presented investigators with several difficulties in ultramicrotomy of specimens for electron microscopy due to its high degree of mineralization. This study explores the possibility of combining ion-milling and high voltage electron microscopy as a means of circumventing the problems of ultramicrotomy.A longitudinal section of an extracted human third molar was ground to a thickness of about 30 um and polarized light micrographs were taken. The specimen was attached to a single hole grid and thinned by argon-ion bombardment at 15° incidence while rotating at 15 rpm. The beam current in each of two guns was 50 μA with an accelerating voltage of 4 kV. A 20 nm carbon coating was evaporated onto the specimen to prevent an electron charge from building up during electron microscopy.

Techniques for Transmission Electron Microscopy of Fiber-Matrix Interfaces in Aluminum Alloy-Boron Composites by Ion Erosio

1971 ◽  
Vol 29 ◽  
pp. 204-205
Author(s):  
G. G. Shaw
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Aluminum Alloy ◽  
Electron Beam ◽  
Pure Aluminum ◽  
Ion Milling ◽  
Transmission Electron ◽  
Fiber Matrix ◽  
Ion Erosion ◽  
Row Of Fibers

The morphology and composition of the fiber-matrix interface can best be studied by transmission electron microscopy and electron diffraction. For some composites satisfactory samples can be prepared by electropolishing. For others such as aluminum alloy-boron composites ion erosion is necessary.When one wishes to examine a specimen with the electron beam perpendicular to the fiber, preparation is as follows: A 1/8 in. disk is cut from the sample with a cylindrical tool by spark machining. Thin slices, 5 mils thick, containing one row of fibers, are then, spark-machined from the disk. After spark machining, the slice is carefully polished with diamond paste until the row of fibers is exposed on each side, as shown in Figure 1.In the case where examination is desired with the electron beam parallel to the fiber, preparation is as follows: Experimental composites are usually 50 mils or less in thickness so an auxiliary holder is necessary during ion milling and for easy transfer to the electron microscope. This holder is pure aluminum sheet, 3 mils thick.

Microtomy of spherical Al2O3 powders

1983 ◽  
Vol 41 ◽  
pp. 74-75
Author(s):  
E.J. Jenkins ◽  
D.S. Tucker ◽  
J.J. Hren
Keyword(s):  
Thin Film ◽  
Size Range ◽  
Particle Aggregation ◽  
Ion Milling ◽  
Thin Sections ◽  
Α Phase ◽  
Convenient Means ◽  
Van Der Waals Attraction ◽  
Negative Feature ◽  
Film Substrate

The size range of mineral and ceramic particles of one to a few microns is awkward to prepare for examination by TEM. Electrons can be transmitted through smaller particles directly and larger particles can be thinned by crushing and dispersion onto a substrate or by embedding in a film followed by ion milling. Attempts at dispersion onto a thin film substrate often result in particle aggregation by van der Waals attraction. In the present work we studied 1-10 μm diameter Al2O3 spheres which were transformed from the amprphous state to the stable α phase.After the appropriate heat treatment, the spherical powders were embedded in as high a density as practicable in a hard EPON, and then microtomed into thin sections. There are several advantages to this method. Obviously, this is a rapid and convenient means to study the microstructure of serial slices. EDS, ELS, and diffraction studies are also considerably more informative. Furthermore, confidence in sampling reliability is considerably enhanced. The major negative feature is some distortion of the microstructure inherent to the microtoming operation; however, this appears to have been surprisingly small. The details of the method and some typical results follow.

Comparative Microstructures of Ion Milled and Electrochemically Thinned Composite Materials

1974 ◽  
Vol 32 ◽  
pp. 546-547
Author(s):  
R.R. Russell
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Composite Materials ◽  
Great Difficulty ◽  
Ion Milling ◽  
Transmission Electron ◽  
Ion Damage ◽  
Intermetallic Composite

Transmission electron microscopy of metallic/intermetallic composite materials is most challenging since the microscopist typically has great difficulty preparing specimens with uniform electron thin areas in adjacent phases. The application of ion milling for thinning foils from such materials has been quite effective. Although composite specimens prepared by ion milling have yielded much microstructural information, this technique has some inherent drawbacks such as the possible generation of ion damage near sample surfaces.

Effects of Ion Beam Milling on Surface Topography

1973 ◽  
Vol 31 ◽  
pp. 84-85
Author(s):  
P.G. Pawar ◽  
P. Duhamel ◽  
G.W. Monk
Keyword(s):  
Surface Topography ◽  
Ion Beam ◽  
Solid Material ◽  
Beam Current ◽  
Atomic Mass ◽  
Micro Milling ◽  
Ion Milling ◽  
Controlled Atmospheres ◽  
Milling Operations ◽  
Sufficient Energy

A beam of ions of mass greater than a few atomic mass units and with sufficient energy can remove atoms from the surface of a solid material at a useful rate. A system used to achieve this purpose under controlled atmospheres is called an ion miliing machine. An ion milling apparatus presently available as IMMI-III with a IMMIAC was used in this investigation. Unless otherwise stated, all the micro milling operations were done with Ar+ at 6kv using a beam current of 100 μA for each of the two guns, with a specimen tilt of 15° from the horizontal plane.It is fairly well established that ion bombardment of the surface of homogeneous materials can produce surface topography which resembles geological erosional features.

An Electron Microscope Study of Interdiffusion and Compound Formation in Ta-Au Thin Films

1973 ◽  
Vol 31 ◽  
pp. 32-33 ◽  
Author(s):  
T. C. Tisone ◽  
S. Lau
Keyword(s):  
Electron Microscope ◽  
Electron Microscope Study ◽  
Thermally Grown Oxide ◽  
Ion Milling ◽  
Compound Formation ◽  
Technology Application ◽  
Transmission Electron ◽  
Before And After ◽  
Au Thin Films

In a study of the properties of a Ta-Au metallization system for thin film technology application, the interdiffusion between Ta(bcc)-Au, βTa-Au and Ta2M-Au films was studied. Considered here is a discussion of the use of the transmission electron microscope(TEM) in the identification of phases formed and characterization of the film microstructures before and after annealing.The films were deposited by sputtering onto silicon wafers with 5000 Å of thermally grown oxide. The film thicknesses were 2000 Å of Ta and 2000 Å of Au. Samples for TEM observation were prepared by ultrasonically cutting 3mm disks from the wafers. The disks were first chemically etched from the silicon side using a HNO3 :HF(19:5) solution followed by ion milling to perforation of the Au side.

High Resolution Observations of Ion-Milling Induced Transformation in Synthetic Hollandses

1981 ◽  
Vol 39 ◽  
pp. 114-115 ◽  
Author(s):  
T. J. Headley
Keyword(s):  
High Resolution ◽  
Radioactive Waste Disposal ◽  
Ion Milling ◽  
Minor Elements ◽  
Waste Forms ◽  
Carbon Substrates ◽  
Structural Differences ◽  
Oxide Phases ◽  
Argon Ions ◽  
High Resolution Microscopy

Oxide phases having the hollandite structure have been identified in multiphase ceramic waste forms being developed for radioactive waste disposal. High resolution studies of phases in the waste forms described in Ref. [2] were initiated to examine them for fine scale structural differences compared to natural mineral analogs. Two hollandites were studied: a (Ba,Cs,K)-titan-ate with minor elements in solution that is produced in the waste forms, and a synthesized BaAl2Ti6O16 phase containing ∼ 4.7 wt% Cs2O. Both materials were consolidated by hot pressing at temperatures above 1100°C. Samples for high resolution microscopy were prepared both by ion-milling (7kV argon ions) and by crushing and dispersing the fragments on holey carbon substrates. The high resolution studies were performed in a JEM 200CX/SEG operating at 200kV.

Growth of hematite by surface oxidation of olivine

1988 ◽  
Vol 46 ◽  
pp. 800-801
Author(s):  
S. McKernan ◽  
C. B. Carter
Keyword(s):  
Electron Microscope ◽  
Surface Oxidation ◽  
Thin Foil ◽  
Nucleation And Growth ◽  
Ion Milling ◽  
Annealed Material ◽  
Thin Foils ◽  
Natural Olivine ◽  
Approximate Composition ◽  
Second Phases

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.

TEM examination of 2014-SiC metal matrix composite

1988 ◽  
Vol 46 ◽  
pp. 726-727
Author(s):  
M. G. Burke ◽  
M. N. Gungor ◽  
P. K. Liaw
Keyword(s):  
Metal Matrix Composite ◽  
Metal Matrix Composites ◽  
Matrix Composite ◽  
Metal Matrix ◽  
Tensile Deformation ◽  
Microstructural Characterization ◽  
Thin Foil ◽  
Matrix Alloy ◽  
Matrix Composites ◽  
Ion Milling

Aluminum-based metal matrix composites offer unique combinations of high specific strength and high stiffness. The improvement in strength and stiffness is related to the particulate reinforcement and the particular matrix alloy chosen. In this way, the metal matrix composite can be tailored for specific materials applications. The microstructural characterization of metal matrix composites is thus important in the development of these materials. In this study, the structure of a p/m 2014-SiC particulate metal matrix composite has been examined after extrusion and tensile deformation.Thin-foil specimens of the 2014-20 vol.% SiCp metal matrix composite were prepared by dimpling to approximately 35 μm prior to ion-milling using a Gatan Dual Ion Mill equipped with a cold stage. These samples were then examined in a Philips 400T TEM/STEM operated at 120 kV. Two material conditions were evaluated: after extrusion (80:1); and after tensile deformation at 250°C.

Crystal Structure Analysis of Cu-Zr Alloys by Convergent Beam Diffraction

1981 ◽  
Vol 39 ◽  
pp. 354-355
Author(s):  
A. F. Marshall ◽  
J. W. Steeds ◽  
D. Bouchet ◽  
S. L. Shinde ◽  
R. G. Walmsley
Keyword(s):  
Crystal Structure ◽  
Point Group ◽  
Intermetallic Phase ◽  
Three Dimensional ◽  
Crystal Structure Analysis ◽  
Ion Milling ◽  
Composition And Structure ◽  
Unit Cells ◽  
Sputter Deposited ◽  
Convergent Beam

Convergent beam electron diffraction is a powerful technique for determining the crystal structure of a material in TEM. In this paper we have applied it to the study of the intermetallic phases in the Cu-rich end of the Cu-Zr system. These phases are highly ordered. Their composition and structure has been previously studied by microprobe and x-ray diffraction with sometimes conflicting results.The crystalline phases were obtained by annealing amorphous sputter-deposited Cu-Zr. Specimens were thinned for TEM by ion milling and observed in a Philips EM 400. Due to the large unit cells involved, a small convergence angle of diffraction was used; however, the three-dimensional lattice and symmetry information of convergent beam microdiffraction patterns is still present. The results are as follows:1) 21 at% Zr in Cu: annealed at 500°C for 5 hours. An intermetallic phase, Cu3.6Zr (21.7% Zr), space group P6/m has been proposed near this composition (2). The major phase of our annealed material was hexagonal with a point group determined as 6/m.

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