Mechanical fragmentation vs. electrodynamic pulse disaggregation for weak acid leach sample preparation: Implications for the exploration of unconformity-hosted uranium deposits

2022 ◽  
pp. 105206
Author(s):  
Collette Pilsworth ◽  
Daniel Layton-Matthews ◽  
Matthew I. Leybourne ◽  
Alexandre Voinot ◽  
Donald Chipley
Keyword(s):  
Sample Preparation ◽  
Weak Acid ◽  
Uranium Deposits ◽  
Acid Leach ◽  
Mechanical Fragmentation

scholarly journals Lead Isotopes in Exploration for Basement-Hosted Structurally Controlled Unconformity-Related Uranium Deposits: Kiggavik Project (Nunavut, Canada)

Minerals ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 512
Author(s):  
David Quirt ◽  
Antonio Benedicto
Keyword(s):  
Inductively Coupled Plasma ◽  
Structural Control ◽  
Lead Isotopes ◽  
Isotope Ratios ◽  
Uranium Content ◽  
Weak Acid ◽  
Pb Isotopes ◽  
Pb Isotope ◽  
Acid Leach ◽  
Partial Digestion

Pb-isotopes have been proposed as pathfinders for sandstone-hosted unconformity-related U deposits, with isotope ratios providing information on mineralization timing and element remobilization and migration. Pb-isotopes proximal to mineralization display radiogenic signatures, often with ‘excess Pb’ suggestive of derivation from greater U concentrations than are currently present. The U deposits in the Kiggavik project area (west of Baker Lake, NU, Canada) are basement-hosted, contain several generations of pitchblende mineralization, display a strong structural control, and are located in fault-related fracture systems and foliation-parallel veinlets. Drill core samples were analysed by Inductively-Coupled Plasma-Mass Spectrometer (ICP-MS) for Pb isotopes following multi-acid total-digestion, reverse Aqua Regia partial-digestion, and weak-acid-leach attacks, to evaluate the utility of the respective dissolution methods in Pb-isotope pathfinder geochemistry. Partial-digestion results are similar to weak-acid-leach results, indicating that interpretation of Pb-isotope signatures can be carried out from partial-digestion data if weak-acid-leach data are unavailable. Application of this pathfinder method at Kiggavik shows that Pb-isotope ratios display systematic trends useful for exploration vectoring. Uranium-content-adjusted 206Pb/204Pb ratios and 206Pb/204Pb ‘excess-lead’ data highlight anomalous isotopic values. 207Pb/206Pb ratios display downhole trends complementary to location of mineralization. Three-dimensional (3D) distributions of Pb-isotope data at the Contact U prospect show systematic trends and form halos around the mineralization. Isotopic footprints are limited to <50 m from the mineralization outline, reflecting host-rock and structural control, but indicate areas with elevated potential for U mineralization and provide vectoring information within basement lithologies.

Pollutant Identification by Selected Area Electron Diffraction

1974 ◽  
Vol 32 ◽  
pp. 532-533
Author(s):  
R. E. Ferrell ◽  
G. G. Paulson ◽  
C. W. Walker
Keyword(s):  
Thermal Treatment ◽  
Electron Diffraction ◽  
Sample Preparation ◽  
Crystal Structures ◽  
Water Samples ◽  
Environmental Samples ◽  
Short Review ◽  
Selected Area Electron Diffraction ◽  
Multiple Component

Selected area electron diffraction (SAD) has been used successfully to determine crystal structures, identify traces of minerals in rocks, and characterize the phases formed during thermal treatment of micron-sized particles. There is an increased interest in the method because it has the potential capability of identifying micron-sized pollutants in air and water samples. This paper is a short review of the theory behind SAD and a discussion of the sample preparation employed for the analysis of multiple component environmental samples.

Preparation of Thin Cadmium Telluride Samples for Electron Microscope Studies

1974 ◽  
Vol 32 ◽  
pp. 548-549
Author(s):  
T. J. Magee ◽  
J. Peng ◽  
J. Bean
Keyword(s):  
Electron Microscope ◽  
Sulfuric Acid ◽  
Solid State ◽  
Sample Preparation ◽  
Cadmium Telluride ◽  
Potassium Dichromate ◽  
Optical Components ◽  
The Past ◽  
Solid State Devices

Cadmium telluride has become increasingly important in a number of technological applications, particularly in the area of laser-optical components and solid state devices, Microstructural characterizations of the material have in the past been somewhat limited because of the lack of suitable sample preparation and thinning techniques. Utilizing a modified jet thinning apparatus and a potassium dichromate-sulfuric acid thinning solution, a procedure has now been developed for obtaining thin contamination-free samples for TEM examination.

A Freeze Shadow Technique for the Preparation of Soft Paint Latexes for Electron Microscopy

1977 ◽  
Vol 35 ◽  
pp. 314-315
Author(s):  
Earl R. Walter ◽  
Glen H. Bryant
Keyword(s):  
Sample Preparation ◽  
High Vacuum ◽  
Vacuum System ◽  
Latex Particles ◽  
New Methods ◽  
Diffusion Pump ◽  
Film Forming ◽  
Routine Basis ◽  
Distribution Studies ◽  
Preparation Techniques

With the development of soft, film forming latexes for use in paints and other coatings applications, it became desirable to develop new methods of sample preparation for latex particle size distribution studies with the electron microscope. Conventional latex sample preparation techniques were inadequate due to the pronounced tendency of these new soft latex particles to distort, flatten and fuse on the substrate when they dried. In order to avoid these complications and obtain electron micrographs of undistorted latex particles of soft resins, a freeze-dry, cold shadowing technique was developed. The method has now been used in our laboratory on a routine basis for several years.The cold shadowing is done in a specially constructed vacuum system, having a conventional mechanical fore pump and oil diffusion pump supplying vacuum. The system incorporates bellows type high vacuum valves to permit a prepump cycle and opening of the shadowing chamber without shutting down the oil diffusion pump. A baffeled sorption trap isolates the shadowing chamber from the pumps.

SEM evaluation of the TEM cold-stage double-film specimen

1984 ◽  
Vol 42 ◽  
pp. 272-273
Author(s):  
Jayesh Bellare
Keyword(s):  
Spatial Distribution ◽  
Sample Preparation ◽  
Sample Thickness ◽  
Specimen Preparation ◽  
Preparation Technique ◽  
Liquid Sample ◽  
Thin Specimen ◽  
Sample Preparation Technique ◽  
Cold Stage ◽  
Film Specimen

Seeing is believing, but only after the sample preparation technique has received a systematic study and a full record is made of the treatment the sample gets.For microstructured liquids and suspensions, fast-freeze thermal fixation and cold-stage microscopy is perhaps the least artifact-laden technique. In the double-film specimen preparation technique, a layer of liquid sample is trapped between 100- and 400-mesh polymer (polyimide, PI) coated grids. Blotting against filter paper drains excess liquid and provides a thin specimen, which is fast-frozen by plunging into liquid nitrogen. This frozen sandwich (Fig. 1) is mounted in a cooling holder and viewed in TEM.Though extremely promising for visualization of liquid microstructures, this double-film technique suffers from a) ireproducibility and nonuniformity of sample thickness, b) low yield of imageable grid squares and c) nonuniform spatial distribution of particulates, which results in fewer being imaged.

Advanced TEM sample preparation techniques for submicron Si devices

1995 ◽  
Vol 53 ◽  
pp. 516-517 ◽  
Author(s):  
P. B. Basham ◽  
H. L. Tsai
Keyword(s):  
Sample Preparation ◽  
Process Development ◽  
Light Transmission ◽  
Specific Area ◽  
Turnaround Time ◽  
Small Hole ◽  
Area Of Interest ◽  
Transmission Electron ◽  
Polished Side ◽  
Preparation Techniques

The use of transmission electron microscopy (TEM) to support process development of advanced microelectronic devices is often challenged by a large amount of samples submitted from wafer fabrication areas and specific-spot analysis. Improving the TEM sample preparation techniques for a fast turnaround time is critical in order to provide a timely support for customers and improve the utilization of TEM. For the specific-area sample preparation, a technique which can be easily prepared with the least amount of effort is preferred. For these reasons, we have developed several techniques which have greatly facilitated the TEM sample preparation.For specific-area analysis, the use of a copper grid with a small hole is found to be very useful. With this small-hole grid technique, TEM sample preparation can be proceeded by well-established conventional methods. The sample is first polished to the area of interest, which is then carefully positioned inside the hole. This polished side is placed against the grid by epoxy Fig. 1 is an optical image of a TEM cross-section after dimpling to light transmission.

Quantitative defect studies in semiconductor TEM samples prepared by low angle ion milling

1995 ◽  
Vol 53 ◽  
pp. 512-513
Author(s):  
L. Mulestagno ◽  
J.C. Holzer ◽  
P. Fraundorf
Keyword(s):  
Sample Preparation ◽  
Milling Time ◽  
High Density ◽  
Low Density ◽  
Ion Milling ◽  
High Quality ◽  
Variable Angle ◽  
Major Disadvantage ◽  
Induced Defects

Due to the wealth of information, both analytical and structural that can be obtained from it TEM always has been a favorite tool for the analysis of process-induced defects in semiconductor wafers. The only major disadvantage has always been, that the volume under study in the TEM is relatively small, making it difficult to locate low density defects, and sample preparation is a somewhat lengthy procedure. This problem has been somewhat alleviated by the availability of efficient low angle milling.Using a PIPS® variable angle ion -mill, manufactured by Gatan, we have been consistently obtaining planar specimens with a high quality thin area in excess of 5 × 104 μm2 in about half an hour (milling time), which has made it possible to locate defects at lower densities, or, for defects of relatively high density, obtain information which is statistically more significant (table 1).

Recent applications of TEM to the study of interfaces

1990 ◽  
Vol 48 (4) ◽  
pp. 308-309
Author(s):  
C. Barry Carter
Keyword(s):  
High Resolution ◽  
Sample Preparation ◽  
Grain Boundaries ◽  
Diffuse Scattering ◽  
Imaging Techniques ◽  
Amorphous Material ◽  
Contrast Imaging ◽  
Current State ◽  
Actual Nature ◽  
High Resolution Images

This paper will review the current state of understanding of interface structure and highlight some of the future needs and problems which must be overcome. The study of this subject can be separated into three different topics: 1) the fundamental electron microscopy aspects, 2) material-specific features of the study and 3) the characteristics of the particular interfaces. The two topics which are relevant to most studies are the choice of imaging techniques and sample preparation. The techniques used to study interfaces in the TEM include high-resolution imaging, conventional diffraction-contrast imaging, and phase-contrast imaging (Fresnel fringe images, diffuse scattering). The material studied affects not only the characteristics of the interfaces (through changes in bonding, etc.) but also the method used for sample preparation which may in turn have a significant affect on the resulting image. Finally, the actual nature and geometry of the interface must be considered. For example, it has become increasingly clear that the plane of the interface is particularly important whenever at least one of the adjoining grains is crystalline.A particularly productive approach to the study of interfaces is to combine different imaging techniques as illustrated in the study of grain boundaries in alumina. In this case, the conventional imaging approach showed that most grain boundaries in ion-thinned samples are grooved at the grain boundary although the extent of this grooving clearly depends on the crystallography of the surface. The use of diffuse scattering (from amorphous regions) gives invaluable information here since it can be used to confirm directly that surface grooving does occur and that the grooves can fill with amorphous material during sample preparation (see Fig. 1). Extensive use of image simulation has shown that, although information concerning the interface can be obtained from Fresnel-fringe images, the introduction of artifacts through sample preparation cannot be lightly ignored. The Fresnel-fringe simulation has been carried out using a commercial multislice program (TEMPAS) which was intended for simulation of high-resolution images.

A technique for preparing semiconductor cross sections for both TEM and SEM analysis

1989 ◽  
Vol 47 ◽  
pp. 712-713
Author(s):  
Stanley J. Klepeis ◽  
J.P. Benedict ◽  
R.M Anderson
Keyword(s):  
Sample Preparation ◽  
Cross Section ◽  
Cross Sections ◽  
Sem Analysis ◽  
Preparation Technique ◽  
Ion Milling ◽  
Tem Analysis ◽  
Polished Cross Section ◽  
Area Of Interest ◽  
Polished Side

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.

TEM sample preparation of wear-tested room-temperature pulsed-laser-deposited thin films of MoS2 by ultramicrotomy

1993 ◽  
Vol 51 ◽  
pp. 1118-1119
Author(s):  
Pamela F. Lloyd ◽  
Scott D. Walck
Keyword(s):  
Thin Films ◽  
Sample Preparation ◽  
Room Temperature ◽  
High Vacuum ◽  
Pulsed Laser ◽  
Ultra High Vacuum ◽  
Wear Testing ◽  
Preparation Technique ◽  
Cross Sectional ◽  
Aerospace Applications

Pulsed laser deposition (PLD) is a novel technique for the deposition of tribological thin films. MoS2 is the archetypical solid lubricant material for aerospace applications. It provides a low coefficient of friction from cryogenic temperatures to about 350°C and can be used in ultra high vacuum environments. The TEM is ideally suited for studying the microstructural and tribo-chemical changes that occur during wear. The normal cross sectional TEM sample preparation method does not work well because the material’s lubricity causes the sandwich to separate. Walck et al. deposited MoS2 through a mesh mask which gave suitable results for as-deposited films, but the discontinuous nature of the film is unsuitable for wear-testing. To investigate wear-tested, room temperature (RT) PLD MoS2 films, the sample preparation technique of Heuer and Howitt was adapted.Two 300 run thick films were deposited on single crystal NaCl substrates. One was wear-tested on a ball-on-disk tribometer using a 30 gm load at 150 rpm for one minute, and subsequently coated with a heavy layer of evaporated gold.

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