Evaluation of characterization methods for thin sections of silver halide microcrystals by analytical electron microscopy

Abstract

SummarySilver halide microcrystals are usually composed of different phases with varying halide compositions. These microcrystals can be sectioned with an ultramicrotome with a certain thickness in a specific direction. The scanning electron microscopical analysis of these sections provides information on the internal halide profile.During sample sectioning, many deformations can be induced in the material, and usually dominate the different scanning electron images.By acquiring X-ray maps, it is possible to locate the different phases in the sections. This technique, however, is very time-consuming, and can only be used when the local halide variations are very high.When an EDX line scan is acquired over the section, information on the position of the phases with different halide composition is obtained in a reasonable time, and shows no dependence on the section deformations. From this knowledge, several positions on the section are selected where local X-ray analyses are performed. After quantifying the results, the internal halide distribution is obtained. The analytical lateral resolution is about 30 nm for sections Ϸ100 nm thick.

Combined characterization of composite tabular silver halide microcrystals by cryo-EFTEM/EELS and cryo-STEM/EDX techniques

“…The quality/speed ratio of the former is higher at medium and high densities. During the last decade an increased interest has been demonstrated to the structural and analytical characterization of individual microcrystals and their compositional arrangement by various instrumental methods, i.e., conventional transmission electron microscopy (CTEM, Goessens et al, 1991Goessens et al, , 1994Goessens et al, , 1995; high-resolution electron microscopy (Shiozawa et al, 1987); scanning electron microscopy (SEM) and lowtemperature luminescence microscopy (Maskasky, 1987a,b); scanning transmission electron microscopy (STEM) and analytical electron microscopy (AEM) techniques (Gao et al, 1989;Gregory et al, 1997;King et al, 1987;Lavergne et al, 1994a,b;Oleshko et al, 1995aOleshko et al, ,b, 1996Wu et al, 1992Wu et al, , 1993; secondary ion mass spectrometry (Maternaghan et al, 1990;Verlinden et al, 1997) and scanning probe microscopies (Keyes et al, 1992;Rogers et al, 1995;Schwarz et al, 1992). This activity was stimulated by the introduction of novel types of silver halide systems with improved photographic functions such as efficiency of light quanta detection, photohole trapping, and storage of the latent image, etc.…”

Automated Particle Analysis of Populations of Silver Halide Microcrystals by Electron Probe Microanalysis under Cryogenic Conditions

“…Transmission electron microscopy 2 allows for the structure determination of individual crystals. With analytical electron microscopy, − electron energy loss spectroscopy, and electron spectroscopic imaging, local chemical analysis can be performed within individual microcrystals.…”

Introduction to microscopic research of silver halides and related dispersed systems

“…One can refer to a bibliography dealing mainly with electron microscopy (stationary and scanning methods), scanning probe techniques, light microscopy, ion-beam compositional imaging, and digital image analysis (Oleshko et al, 1995). The last decade alone gave a number of excellent examples of successful solution of highly diverse and complicated tasks of imaging science by the use of low-temperature luminescence, bright-and darkfield optical and scanning electron microscopy (SEM) (Maskasky, 1987(Maskasky, , 1991, conventional transmission electron microscopy (CTEM) (Goessens et al, 1991(Goessens et al, , 1994(Goessens et al, , 1995Haefke et al, 1991a), high-resolution electron microscopy (HREM) (Shiozawa et al, 1987; Kobayashi, 1988, 1989), automated electron probe X-ray microanalysis (Raeymaekers et al, 1987), cryoanalytical electron microscopy (AEM) techniques (Gregory et al, 1997;Oleshko et al, 1995Oleshko et al, , 1996, secondary ion mass-spectroscopy compositional imaging (Maternaghan et al, 1990;Verlinden et al, 1997), atomic force microscopy (AFM) (Haefke et al, 1991b;Keyes et al, 1992), and correlative near-field direct/fluorescence imaging and spectroscopy of sensitizing dyes (Rogers et al, 1995).The papers in this topical issue of MRT deal with methodology, sample preparation, and applications of CTEM, HREM, SEM, cryo-AEM (cryo-energy-filtering TEM [EFTEM]/electron energy-loss spectroscopy [EELS], cryo-scanning TEM [STEM]/energy-dispersive X-ray [EDX] analysis, cathodoluminescence), scanning tunneling microscopy (STM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS) for studying microcrystals of contemporary photographic emulsions, aggregated photosensitive dye-stuffs, deposited AgX adlayers, photolytic and developed Ag particles of colloidal dispersity.The issue commences with a review by Goessens et al covering the results of cryo-CTEM studies of crystalline and defect structures and phase composition of AgX (111) twinned microcrystals. Parallel (AgBr) and nonparallel (core-shell AgBr-AgBrI) twinning modes yielding tabular and needle or tetrahedral-shaped microcrys-*Corespondence to: Vladimir Oleshko, Department of Chemistry, Micro-and Trace Analysis Centre, University of Antwerp, B-2610 Antwerpen-Wilrijk, Belgium MICROSCOPY RESEARCH AND TECHNIQUE 42:82-84 (1998) 1998 WILEY-LISS, INC. tals are discussed.…”