EXPERIMENTAL AND THEORETICAL SUBSTANTIATIONS OF STEPWISE MECHANISM OF CRYSTAL FORMATION FROM LIQUID PHASE

The advent of the scanning electron microscope (SCEM) has renewed interest in preparing specimens by avoiding the forces of surface tension. The present method of freeze drying by Boyde and Barger (1969) and Small and Marszalek (1969) does prevent surface tension but ice crystal formation and time required for pumping out the specimen to dryness has discouraged us. We believe an attractive alternative to freeze drying is the critical point method originated by Anderson (1951; for electron microscopy. He avoided surface tension effects during drying by first exchanging the specimen water with alcohol, amy L acetate and then with carbon dioxide. He then selected a specific temperature (36.5°C) and pressure (72 Atm.) at which carbon dioxide would pass from the liquid to the gaseous phase without the effect of surface tension This combination of temperature and, pressure is known as the "critical point" of the Liquid.

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Elucidation of block boundaries as the dissolution channels in hydrated cement

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100109562 ◽

1978 ◽

Vol 36 (1) ◽

pp. 484-485

Author(s):

N.V. Belov ◽

U.I. Papiashwili ◽

B.E. Yudovich

Keyword(s):

Liquid Phase ◽

Grain Boundaries ◽

Benzoyl Peroxide ◽

Phase Contrast ◽

Active Role ◽

Point Of View ◽

Hardened Cement ◽

Hydrated Cement ◽

Hardened Cement Paste

It has been almost universally adopted that dissolution of solids proceeds with development of uniform, continuous frontiers of reaction.However this point of view is doubtful / 1 /. E.g. we have proved the active role of the block (grain) boundaries in the main phases of cement, these boundaries being the areas of hydrate phases' nucleation / 2 /. It has brought to the supposition that the dissolution frontier of cement particles in water is discrete. It seems also probable that the dissolution proceeds through the channels, which serve both for the liquid phase movement and for the drainage of the incongruant solution products. These channels can be appeared along the block boundaries.In order to demonsrate it, we have offered the method of phase-contrast impregnation of the hardened cement paste with the solution of methyl metacrylahe and benzoyl peroxide. The viscosity of this solution is equal to that of water.

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Techniques for cryoultramicrotomy of propane jet frozen biological samples

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s042482010014292x ◽

1986 ◽

Vol 44 ◽

pp. 260-261

Author(s):

B. Craig ◽

L. Hawkey ◽

A. LeFurgey

Keyword(s):

Freeze Fracture ◽

Freeze Substitution ◽

Heart Cells ◽

Crystal Formation ◽

X Ray ◽

Transmission Electron ◽

Scanning Transmission ◽

Chick Heart ◽

Embryonic Chick Heart ◽

A New Technique

Ultra-rapid freezing followed by cryoultramicrotomy is essential for the preservation of diffusible elements in situ within cells prior to scanning transmission electron microscopy and quantitative energy dispersive x-ray microanalysis. For cells or tissue fragments in suspension and for monolayer cell cultures, propane jet freezing provides cooling rates greater than 30,000°C/sec with regions up to 40μm in thickness free of significant ice crystal formation. While this method of freezing has frequently been applied prior to freeze fracture or freeze substitution, it has not been widely utilized prior to cryoultramicrotomy and subsequent x-ray microanalytical studies. This report describes methods devised in our laboratory for cryosectioning of propane jet frozen kidney proximal tubule suspensions and cultured embryonic chick heart cells, in particular a new technique for mounting frozen suspension specimens for sectioning. The techniques utilize the same specimen supports and sample holders as those used for freeze fracture and freeze substitution and should be generally applicable to any cell suspension or culture preparation.

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Identification of hepatitis a virus in cell cultures by solid phase immune electron microscopy

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100142815 ◽

1986 ◽

Vol 44 ◽

pp. 238-239

Author(s):

C.D. Humphrey ◽

T.L. Cromeans ◽

E.H. Cook ◽

D.W. Bradley

Keyword(s):

Electron Microscopy ◽

Liquid Phase ◽

Cell Cultures ◽

Rapid Detection ◽

Hepatitis A ◽

Hepatitis A Virus ◽

Solid Phase ◽

Immune Electron Microscopy ◽

Detection And Identification

There is a variety of methods available for the rapid detection and identification of viruses by electron microscopy as described in several reviews. The predominant techniques are classified as direct electron microscopy (DEM), immune electron microscopy (IEM), liquid phase immune electron microscopy (LPIEM) and solid phase immune electron microscopy (SPIEM). Each technique has inherent strengths and weaknesses. However, in recent years, the most progress for identifying viruses has been realized by the utilization of SPIEM.

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High-pressure freezing and freeze substitution of plant tissue

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100124148 ◽

1992 ◽

Vol 50 (1) ◽

pp. 748-749

Author(s):

William P. Sharp ◽

Robert W. Roberson

Keyword(s):

High Pressure ◽

Cell Structure ◽

Leaf Tissue ◽

Freeze Substitution ◽

Crystal Formation ◽

Ice Crystal ◽

High Pressure Freezing ◽

Cell Components ◽

Cold Metal ◽

Brome Grass

The aim of ultrastructural investigation is to analyze cell architecture and relate a functional role(s) to cell components. It is known that aqueous chemical fixation requires seconds to minutes to penetrate and stabilize cell structure which may result in structural artifacts. The use of ultralow temperatures to fix and prepare specimens, however, leads to a much improved preservation of the cell’s living state. A critical limitation of conventional cryofixation methods (i.e., propane-jet freezing, cold-metal slamming, plunge-freezing) is that only a 10 to 40 μm thick surface layer of cells can be frozen without distorting ice crystal formation. This problem can be allayed by freezing samples under about 2100 bar of hydrostatic pressure which suppresses the formation of ice nuclei and their rate of growth. Thus, 0.6 mm thick samples with a total volume of 1 mm3 can be frozen without ice crystal damage. The purpose of this study is to describe the cellular details and identify potential artifacts in root tissue of barley (Hordeum vulgari L.) and leaf tissue of brome grass (Bromus mollis L.) fixed and prepared by high-pressure freezing (HPF) and freeze substitution (FS) techniques.

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The “KIMWIPE” Effect in Ultra-Thin Cryosections

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100119119 ◽

1985 ◽

Vol 43 ◽

pp. 458-459

Author(s):

I. Taylor ◽

P. Ingram ◽

J.R. Sommer

Keyword(s):

Skeletal Muscle ◽

Electrical Stimulation ◽

Muscle Fibers ◽

Ice Crystals ◽

Crystal Formation ◽

Ice Crystal ◽

Thin Sections ◽

Skeletal Muscle Fibers ◽

Freeze Dried ◽

Ice Crystal Formation

In studying quick-frozen single intact skeletal muscle fibers for structural and microchemical alterations that occur milliseconds, and fractions thereof, after electrical stimulation, we have developed a method to compare, directly, ice crystal formation in freeze-substituted thin sections adjacent to all, and beneath the last, freeze-dried cryosections. We have observed images in the cryosections that to our knowledge have not been published heretofore (Figs.1-4). The main features are that isolated, sometimes large regions of the sections appear hazy and have much less contrast than adjacent regions. Sometimes within the hazy regions there are smaller areas that appear crinkled and have much more contrast. We have also observed that while the hazy areas remain still, the regions of higher contrast visibly contract in the beam, often causing tears in the sections that are clearly not caused by ice crystals (Fig.3, arrows).

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HREM observation of NiO growth on submicron spheres of pure nickel

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100154718 ◽

1989 ◽

Vol 47 ◽

pp. 548-549

Author(s):

C.M. Teng ◽

T.F. Kelly ◽

J.P. Zhang ◽

H.M. Lin ◽

Y.W. Kim

Keyword(s):

Nickel Oxide ◽

Grain Boundaries ◽

Pure Nickel ◽

Submicron Particles ◽

Crystal Formation ◽

Nickel Wire ◽

Liquid Droplets ◽

Oxide Interface ◽

Nickel Chromium ◽

Chromium Alloys

Spherical submicron particles of materials produced by electrohydrodynamic (EHD) atomization have been used to study a variety of materials processes including nucleation of alternative crystallization phases in iron-nickel and nickel-chromium alloys, amorphous solidification in submicron droplets of pure metals, and quasi-crystal formation in nickel-chromium alloys. Some experiments on pure nickel, nickel oxide single crystals, the nickel/nickel(II) oxide interface, and grain boundaries in nickel monoxide have been performed by STEM. For these latter studies, HREM is the most direct approach to obtain particle crystal structures at the atomic level. Grain boundaries in nickel oxide have also been investigated by HREM. In this paper, we present preliminary results of HREM observations of NiO growth on submicron spheres of pure nickel.Small particles of pure nickel were prepared by EHD atomization. For the study of pure nickel, 0.5 mm diameter pure nickel wire (99.9975%) is sprayed directly in the EHD process. The liquid droplets solidify in free-flight through a vacuum chamber operated at about 10-7 torr.

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Microanalysis of silicate glass films grown on α-Al2O3 by pulsed-laser deposition

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100148022 ◽

1993 ◽

Vol 51 ◽

pp. 438-439

Author(s):

Michael P. Mallamaci ◽

James Bentley ◽

C. Barry Carter

Keyword(s):

Liquid Phase ◽

Single Crystal ◽

Pulsed Laser Deposition ◽

Pulsed Laser ◽

Ceramic Materials ◽

Laser Deposition ◽

Triple Junctions ◽

Ion Milling ◽

Multicomponent Oxides ◽

Glass Films

Glass-oxide interfaces play important roles in developing the properties of liquid-phase sintered ceramics and glass-ceramic materials. Deposition of glasses in thin-film form on oxide substrates is a potential way to determine the properties of such interfaces directly. Pulsed-laser deposition (PLD) has been successful in growing stoichiometric thin films of multicomponent oxides. Since traditional glasses are multicomponent oxides, there is the potential for PLD to provide a unique method for growing amorphous coatings on ceramics with precise control of the glass composition. Deposition of an anorthite-based (CaAl2Si2O8) glass on single-crystal α-Al2O3 was chosen as a model system to explore the feasibility of PLD for growing glass layers, since anorthite-based glass films are commonly found in the grain boundaries and triple junctions of liquid-phase sintered α-Al2O3 ceramics.Single-crystal (0001) α-Al2O3 substrates in pre-thinned form were used for film depositions. Prethinned substrates were prepared by polishing the side intended for deposition, then dimpling and polishing the opposite side, and finally ion-milling to perforation.

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Effect of furnace atmosphere and silica content on the consolidation behaviour of magnesia partially stabilised zirconia

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100178410 ◽

1990 ◽

Vol 48 (4) ◽

pp. 1056-1057

Author(s):

J. Drennan ◽

R.H.J. Hannink ◽

D.R. Clarke ◽

T.M. Shaw

Keyword(s):

Liquid Phase ◽

Silica Content ◽

Liquid Phase Sintering ◽

Furnace Atmosphere ◽

Boundary Phase ◽

Analytical Electron ◽

Analytical Electron Microscope ◽

Series Of Experiments ◽

Compositional Gradients ◽

Mobile Liquid

Magnesia partially stabilised zirconia (Mg-PSZ) ceramics are renowned for their excellent nechanical properties. These are effected by processing conditions and purity of starting materials. It has been previously shown that small additions of strontia (SrO) have the effect of removing the major contaminant, silica (SiO2).The mechanism by which this occurs is not fully understood but the strontia appears to form a very mobile liquid phase at the grain boundaries. As the sintering reaches the final stages the liquid phase is expelled to the surface of the ceramic. A series of experiments, to examine the behaviour of the liquid grain boundary phase, were designed to produce compositional gradients across the ceramic bodies. To achieve this, changes in both silica content and furnace atmosphere were implemented. Analytical electron microscope techniques were used to monitor the form and composition of the phases developed. This paper describes the results of our investigation and the presentation will discuss the work with reference to liquid phase sintering of ceramics in general.

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