Swelling pressure and microstructure of an activated swelling clay with temperature

Clay Minerals ◽  
1998 ◽  
Vol 33 (2) ◽  
pp. 255-267 ◽  
Author(s):  
D. Tessier ◽  
M. Dardaine ◽  
A. Beaumont ◽  
A. M. Jaunet

AbstractClay from Fourges has been selected by the Commissariat à l'Energie Atomique as a support in radioactive waste disposal studies. This material was activated by adding Na2CO3, then compacted at 60 MPa. Subsequently, its swelling behaviour was monitored at 90°C and 145°C for 330 days and at the end of this period the samples were examined by transmission electron microscopy (TEM). For this, they were embedded in a resin then sectioned with an ultramicrotome for mineralogical and chemical analyses. The initial material is essentially composed of kaolinite and smectite. Addition of Na2CO3 at room temperature induces a replacement of Ca ions by Na ions and the precipitation of finely divided carbonates on the surface of the constituents. At the end of 330 days at 90°C under a hydraulic pressure of 1 MPa, the initial particles combine and the material exerts a swelling pressure of 20 MPa. A complete reorganisation of the clay crystallites is observed without significant dissolution of the solid phases. After the same time at 145°C under a hydraulic pressure of 10 MPa, in a basic medium, the combined conditions are such that a high proportion of the clay is dissolved with formation of amorphous aluminosilicates correlated with a marked drop in the swelling pressure to 5 MPa. This work establishes the advantages of following the macroscopic properties in parallel with the microstructure variations for understanding the changes in the properties of clays.


Author(s):  
Joseph J. Comer

Domains visible by transmission electron microscopy, believed to be Dauphiné inversion twins, were found in some specimens of synthetic quartz heated to 680°C and cooled to room temperature. With the electron beam close to parallel to the [0001] direction the domain boundaries appeared as straight lines normal to <100> and <410> or <510> directions. In the selected area diffraction mode, a shift of the Kikuchi lines was observed when the electron beam was made to traverse the specimen across a boundary. This shift indicates a change in orientation which accounts for the visibility of the domain by diffraction contrast when the specimen is tilted. Upon exposure to a 100 KV electron beam with a flux of 5x 1018 electrons/cm2sec the boundaries are rapidly decorated by radiation damage centers appearing as black spots. Similar crystallographio boundaries were sometimes found in unannealed (0001) quartz damaged by electrons.



Author(s):  
A.J. Tousimis ◽  
T.R. Padden

The size, shape and surface morphology of human erythrocytes (RBC) were examined by scanning electron microscopy (SEM), of the fixed material directly and by transmission electron microscopy (TEM) of surface replicas to compare the relative merits of these two observational procedures for this type specimen.A sample of human blood was fixed in glutaraldehyde and washed in distilled water by centrifugation. The washed RBC's were spread on freshly cleaved mica and on aluminum coated microscope slides and then air dried at room temperature. The SEM specimens were rotary coated with 150Å of 60:40- gold:palladium alloy in a vacuum evaporator using a new combination spinning and tilting device. The TEM specimens were preshadowed with platinum and then rotary coated with carbon in the same device. After stripping the RBC-Pt-C composite film, the RBC's were dissolved in 2.5N HNO3 followed by 0.2N NaOH leaving the preshadowed surface replicas showing positive topography.



Author(s):  
S. Mahajan

The evolution of dislocation channels in irradiated metals during deformation can be envisaged to occur in three stages: (i) formation of embryonic cluster free regions, (ii) growth of these regions into microscopically observable channels and (iii) termination of their growth due to the accumulation of dislocation damage. The first two stages are particularly intriguing, and we have attempted to follow the early stages of channel formation in polycrystalline molybdenum, irradiated to 5×1019 n. cm−2 (E > 1 Mev) at the reactor ambient temperature (∼ 60°C), using transmission electron microscopy. The irradiated samples were strained, at room temperature, up to the macroscopic yield point.Figure 1 illustrates the early stages of channel formation. The observations suggest that the cluster free regions, such as A, B and C, form in isolated packets, which could subsequently link-up to evolve a channel.



Author(s):  
T.E. Pratt ◽  
R.W. Vook

(111) oriented thin monocrystalline Ni films have been prepared by vacuum evaporation and examined by transmission electron microscopy and electron diffraction. In high vacuum, at room temperature, a layer of NaCl was first evaporated onto a freshly air-cleaved muscovite substrate clamped to a copper block with attached heater and thermocouple. Then, at various substrate temperatures, with other parameters held within a narrow range, Ni was evaporated from a tungsten filament. It had been shown previously that similar procedures would yield monocrystalline films of CU, Ag, and Au.For the films examined with respect to temperature dependent effects, typical deposition parameters were: Ni film thickness, 500-800 A; Ni deposition rate, 10 A/sec.; residual pressure, 10-6 torr; NaCl film thickness, 250 A; and NaCl deposition rate, 10 A/sec. Some additional evaporations involved higher deposition rates and lower film thicknesses.Monocrystalline films were obtained with substrate temperatures above 500° C. Below 450° C, the films were polycrystalline with a strong (111) preferred orientation.



Author(s):  
S.K. Streiffer ◽  
C.B. Eom ◽  
J.C. Bravman ◽  
T.H. Geballet

The study of very thin (<15 nm) YBa2Cu3O7−δ (YBCO) films is necessary both for investigating the nucleation and growth of films of this material and for achieving a better understanding of multilayer structures incorporating such thin YBCO regions. We have used transmission electron microscopy to examine ultra-thin films grown on MgO substrates by single-target, off-axis magnetron sputtering; details of the deposition process have been reported elsewhere. Briefly, polished MgO substrates were attached to a block placed at 90° to the sputtering target and heated to 650 °C. The sputtering was performed in 10 mtorr oxygen and 40 mtorr argon with an rf power of 125 watts. After deposition, the chamber was vented to 500 torr oxygen and allowed to cool to room temperature. Because of YBCO’s susceptibility to environmental degradation and oxygen loss, the technique of Xi, et al. was followed and a protective overlayer of amorphous YBCO was deposited on the just-grown films.



Author(s):  
W. P. Wergin ◽  
S. Roy ◽  
E. F. Erbe ◽  
C. A. Murphy ◽  
C. D. Pooley

Larvae of the nematode, Steinernema carpocapsae Weiser strain All, were cryofixed and freezesubstituted for 3 days in acetone containing 2% osmium tetroxide according to established procedures. Following chemical fixation, the nematodes were brought to room temperature, embedded in Spurr's medium and sectioned for observation with a Hitachi S-4100 field emission scanning electron microscope that was equipped with an Oxford CT 1500 Cryotrans System. Thin sections, about 80 nm thick, similar to those generally used in conventional transmission electron microscope (TEM) studies were mounted on copper grids and stained with uranyl acetate for 30 min and lead citrate for 5 min. Sections about 2 μm thick were also mounted and stained in a similar fashion. The grids were mounted on an Oxford grid holder, inserted into the microscope and onto a cryostage that was operated at ambient temperature. Thick and thin sections of the larvae were evaluated and photographed in the SEM at different accelerating voltages. Figs. 4 and 5 have undergone contrast conversion so that the images would resemble transmitted electron micrographs obtained with a TEM.



Author(s):  
Jane Payne ◽  
Philip Coudron

This transmission electron microscopy (TEM) procedure was designed to examine a gram positive spore-forming bacillus in colony on various solid agar media with minimal artifact. Cellular morphology and organization of colonies embedded in Poly/Bed 812 resin (P/B) were studied. It is a modification of procedures used for undecalcified rat bone and Stomatococcus mucilaginosus.Cultures were fixed and processed at room temperature (RT) under a fume hood. Solutions were added with a Pasteur pipet and removed by gentle vacuum aspiration. Other equipment used is shown in Figure 3. Cultures were fixed for 17-18 h in 10-20 ml of RT 2% phosphate buffered glutaraldehyde (422 mosm/KgH2O) within 5 m after removal from the incubator. After 3 (30 m) changes in 0.15 M phosphate buffer (PB = 209-213 mosm/KgH2O, pH 7.39-7.41), colony cut-outs (CCO) were made with a scalpel.



Author(s):  
A.C. Daykin ◽  
C.J. Kiely ◽  
R.C. Pond ◽  
J.L. Batstone

When CoSi2 is grown onto a Si(111) surface it can form in two distinct orientations. A-type CoSi2 has the same orientation as the Si substrate and B-type is rotated by 180° degrees about the [111] surface normal.One method of producing epitaxial CoSi2 is to deposit Co at room temperature and anneal to 650°C.If greater than 10Å of Co is deposited then both A and B-type CoSi2 form via a number of intermediate silicides .The literature suggests that the co-existence of A and B-type CoSi2 is in some way linked to these intermediate silicides analogous to the NiSi2/Si(111) system. The phase which forms prior to complete CoSi2 formation is CoSi. This paper is a crystallographic analysis of the CoSi2/Si(l11) bicrystal using a theoretical method developed by Pond. Transmission electron microscopy (TEM) has been used to verify the theoretical predictions and to characterise the defect structure at the interface.



Author(s):  
Kazue Nishimoto ◽  
Miki Muraki ◽  
Ryuji Tamura

AbstractTernary Ag–In–(Eu, Ce) 1/1 approximants are synthesized and their structures are studied by transmission electron microscopy (TEM). For both the approximants, superlattice spots are clearly observed at room temperature, and the superstructures of the Ag–In–(Eu, Ce) approximants are found to be similar to those of Cd



1981 ◽  
Author(s):  
A Sturk ◽  
L M Burt ◽  
T Hakvoort ◽  
J W ten cate ◽  
N Crawford

Platelet concentrates were stored for one, two or three days at 4°C (unagitated) or room temperature (unagitated and linearly agitated). The morphology of platelets in platelet concentrates, directly after twice washing at room temperature and after 60 min incubation of the washed platelets at 37°C was investigated by both scanning and transmission electron microscopy.Platelets in the freshly prepared concentrates are slightly activated, i.e. show some pseudopod formation. At 4°C platelets rapidly loose their discoid shape. After three days their surface membrane shows extensive folding, they are slightly vacuolated and have lost most of their granules. Incubation of these cold-stored platelets at 37°C does not induce reversal to the discoid shape.Room temperature storage results in reversal of the slight initial platelet activation. After three days unagitated platelets are slightly more vacuolated than platelets stored with agitation. Room temperature storage usually results in remarkably well preserved, discoid platelets. Occasionally however, agitated platelet concentrates contain a high proportion of odd shaped cells. As platelets stored at 4°C did not became discoid after incubation at 37°, the altered membrane structure could provide an explanation for their short survival upon transfusion. Our results also provide a morphological correlation with the slightly better recovery and survival of platelets stored agitated vs.- non-agitated platelets at room temperature.



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