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Query: UMLS:C0851184 (thinning)
 11,252 document(s) hit in 31,850,051 MEDLINE articles (0.00 seconds)

A new preparation method has been developed in order to avoid the breaking of brittle samples for plan-view TEM investigation during and after mechanical and ion beam thinning. The thinning procedure is carried out on a reduced size piece of the sample (about 1.6 x 0.8 mm(2) or about 1-1.6 mm diameter) that is embedded into a 3-mm-diameter Ti disk, which fits the sample holder of the TEM. The small sample size and the supporting metal disk assure the mechanical stability and minimize the possibility of breaking during and after the preparation: The Ti disk is placed on adhesive kapton tape, a cut piece of the sample is put into the slot of the disk, pressed onto the tape and embedded with glue. The tape keeps the parts in place and in the same plane, keeps the sample surface safe from the embedding glue and can be removed easily after the glue solidifies. Subsequently, the embedded sample is thinned from the rear by well-known mechanical and ion beam techniques until electron transparency. This simple solution lowers the risk of failed sample preparation remarkably and makes it possible to reduce the thickness of the sample to about 50 microm by mechanical thinning. As a result, dimpling becomes unnecessary and low angle ion milling gives a large transparent area for TEM. Its efficiency has been proved by successful preparation of numerous thin film samples on Si, sapphire, and glass substrates. The method is compatible with the widespread cross-sectional thinning procedures, and can be easily adopted by TEM laboratories.
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PMID:Novel method for the plan-view TEM preparation of thin samples on brittle substrates by mechanical and ion beam thinning. 1187 8

Single layers of MgF2 and LaF3 were deposited upon superpolished fused-silica and CaF2 substrates by ion-beam sputtering (IBS) as well as by boat and electron beam (e-beam) evaporation and were characterized by a variety of complementary analytical techniques. Besides undergoing photometric and ellipsometric inspection, the samples were investigated at 193 and 633 nm by an optical scatter measurement facility. The structural properties were assessed with atomic-force microscopy, x-ray diffraction, TEM techniques that involved conventional thinning methods for the layers. For measurement of mechanical stress in the coatings, special silicon substrates were coated and analyzed. The dispersion behavior of both deposition materials, which was determined on the basis of various independent photometric measurements and data reduction techniques, is in good agreement with that published in the literature and with the bulk properties of the materials. The refractive indices of the MgF2 coatings ranged from 1.415 to 1.440 for the wavelength of the ArF excimer laser (193 nm) and from 1.435 to 1.465 for the wavelength of the F2 excimer laser (157 nm). For single layers of LaF3 the refractive indices extended from 1.67 to 1.70 at 193 nm to approximately 1.80 at 157 nm. The IBS process achieves the best homogeneity and the lowest surface roughness values (close to 1 nm(rms)) of the processes compared in the joint experiment. In contrast to MgF2 boat and e-beam evaporated coatings, which exhibit tensile mechanical stress ranging from 300 to 400 MPa, IBS coatings exhibit high compressive stress of as much as 910 MPa. A similar tendency was found for coating stress in LaF3 single layers. Experimental results are discussed with respect to the microstructural and compositional properties as well as to the surface topography of the coatings.
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PMID:Ultraviolet optical and microstructural properties of MgF2 and LaF3 coatings deposited by ion-beam sputtering and boat and electron-beam evaporation. 1206 2

Recently several long-term studies have reported evidence of the hydrolytic degradation of collagen fibrils based on fractured surface observations after bond testing. Those studies suggested that one cause of the decline in the bond strength was the degradation of the collagen fibrils within the bonds. However, one concern has been raised that the dentinal collagen fibrils may be stable in water that does not contain oral bacteria or enzymes. Therefore, the present study aimed to clarify the micromorphological change in naked collagen fibrils after 500 days of water storage. To prepare exposed collagen fibrils, sectioned and polished human dentin surfaces were acid conditioned for 15 s with the use of two commercially available acid conditioners: All-Etch (10% phosphoric acid) and Uni-Etch (32% phosphoric acid) (Bisco, Inc.). Those specimens were stored in distilled water at 37 degrees C for 1 day (control) for 500 days. After the storage periods, the samples were examined with the use of SEM and TEM. Under SEM and TEM examination, micromorphological alterations (disarrangement of collagen web, widening the interfibrillar space, and the thinning diameter of collagen fibrils) were found in the specimens after 500 days in water.
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PMID:SEM and TEM analysis of water degradation of human dentinal collagen. 1280 86

The disease progression in oral submucous fibrosis (OSF) seems to be in a biphasic manner, along both fibroblastic and keratinocytic lineages. The epithelial malignancy is considered to be a sequel of connective tissue changes. "Atrophy" of epithelium makes it amenable to the effect of oral carcinogens. This concept looks rather simplistic in the light of the current understanding of epithelial cell biology. So the concept of epithelial "atrophy" needs redressal against the backdrop of recent investigations. 12 cases of clinically and histologically advanced OSF cases (M:F = 4:8) who were habitual areca-quid chewers comprise the study group. 5 (M:F=1:4) non-OSF, non-areca-nut chewing healthy volunteers, constituted the control group. Biopsy was done and the sections were processed for light and electron microscopy. Cell countings were made based on established criteria for apoptosis and necrosis under the high resolution of a TEM and electron micrographs were taken. The Apoptotic Index (A1) calculated for the diseased mucosa was 3.0 +/- 1.3 and for the control was 2.1 +/- 1.5 (X2 = 1.21, df= 1, p>0.05). The necrotic indices (NI) were respectively, 2.5 +/- 0.6 and 2.0 +/- 1.3 (X2 = 0.24, df = 1, p>0.05). The Absolute Cell death Index (ACI), which is the cumulative figure of apoptosis and necrosis indices, was 5.5 and 4.2 respectively for diseased and normal samples (X2 = 1.8, df = 1, p>0.05). The inability to compute an increased ACI in OSF epithelium, when compared to normal, goes against the concept of epithelial "atrophy". Atrophy envisages an increased apoptotic cell death of keratinocytes, induced by the same signals that caused atrophy and this may contribute to loss of cell of an entire organ. This basic concept in pathology seems to be unfounded with disease. This prompted us for an alternative concept in favour of a reduced proliferation index of the adult stem cell compartment of the oral epithelium. So this study favours the concept of epithelial hypoplasia, rather than atrophy, which causes thinning of surface epithelium in advanced OSF.
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PMID:Cell death does not herald epithelial involution ("atrophy") in oral sub mucous fibrosis: a TEM study. 1568 90

The pore structure of chromatographic adsorbents directly influences macromolecular partitioning and transport in chromatography. Quantitative structural characterization of chromatographic media has generally been performed in terms of the mean pore size or, at best, the pore size distribution (PSD), but more detailed information on, e.g., connectivity has been lacking. We have applied electron tomography, a 3D TEM technique that views a sample from multiple perspectives and allows reconstruction of the volumetric structure, to capture the internal details of microporous chromatographic media with nanometer-scale resolution. Visualization of reconstructions of three adsorbents, Toyopearl SP-650 C, SP-550 C, and CM Sepharose FF, provides thorough and direct information on the geometry and the interconnectivity of the pore network. The structures are qualitatively consistent with in situ AFM images, and quantitative data for the porosities and PSDs from the analysis of tomographic data agree reasonably well with inverse size-exclusion chromatography results. For a more straightforward representation of the networking and size features of the disordered pore space, a 3D thinning algorithm was used to derive pore skeletons and consequently quantitative data on distributions of local path lengths, widths, tortuosities, and connectivities. Such enriched structural information can be instrumental in more discriminate structural evaluation and construction of engineered pore models for the study of solute intraparticle transport.
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PMID:Three-dimensional pore structure of chromatographic adsorbents from electron tomography. 1715 96

TEM specimens of a LaAlO(3)/SrTiO(3) multilayer are prepared by FIB with internal lift out. Using a Ga(+1) beam of 5 kV, a final cleaning step yielding top, top-angle, side, and bottom-angle cleaning is performed. Different cleaning procedures, which can be easily implemented in a dual beam FIB system, are described and compared; all cleaning types produce thin lamellae, useful for HRTEM and HAADF-STEM work up to atomic resolution. However, the top cleaned lamellae are strongly affected by the curtain effect. Top-angle cleaned specimens show an amorphous layer of around 5 nm at the specimen surfaces, due to damage and redeposition. Furthermore, it is observed that the LaAlO(3) layers are preferentially destroyed and transformed into amorphous material, during the thinning process.
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PMID:Evaluation of top, angle, and side cleaned FIB samples for TEM analysis. 1772 55

Polystyrene nanocomposites using hybrid organic inorganic (O/I) layered double hydroxide (LDH) and 4[12-(methacryloylamino)dodecanoylamino]benzenesulfonate (MADABS) interleaved molecules were studied as a function of the filler miscibility, dispersion, and the rheological behavior. Incorporation of the I/O filler gave rise to an expanded intercalated PS nanocomposite structure, while an immiscible structure was obtained after a thermal pre-treatment. However the utmost non-linear viscoelasticity in the low-omega region was obtained from the immiscible PS nanocomposite structure. Indeed, the presence of a sub-micrometer percolated structure was here depicted resulting in a jammed structure that progressively changed the typical low-frequency Newtonian flow behavior of PS to a shear-thinning behavior against the filler percentage, having as a consequence to restrict the plastic deformation in the low-omega region by obstructing polymer chain motion. From several characterizations XRD, TEM, and rheology, we demonstrated the presence of LDH agglomerates in spite of PS chain crawling in between the layers, whereas the apparent immiscible structure was composed of well dispersed LDH tactoids forming a three-dimensional percolated network. The gel-like behavior illustrated by the frequency power law dependence of the complex viscosity |eta(*)| proportional to omega(n), n approximately = -0.75 at 10 wt% of MADABS/LDH hybrid filler was then explained by the interconnected and concatenated hybrid LDH platelets domains developing an interfacial attrition with PS chains.
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PMID:A comprehensive study of an unusual jammed nanocomposite structure using hybrid layered double hydroxide filler. 1915 74

Very stable titania hydrosols were prepared by fast hydrolysis of titanium isopropoxide in a large excess of water. XRD patterns show that these sols contain nanocrystals (5-6 nm) of anatase (70%) and brookite (30%). TEM images indicate that these primary particles form aggregates whose mean hydrodynamic diameter, determined by photon correlation spectroscopy, is in the range of 80-90 nm. The flow curves of these colloids, recorded for several volume fractions of nanoparticles, can be perfectly fitted, in the range 0-100 s(-1), with a power-law model. In this range the behavior is Newtonian but for larger shear rates a shear thinning is observed. The viscosity dependence on particle concentration can be predicted by a Batchelor-type model were the volume fraction of particles is replaced by an effective volume fraction of aggregates, taking into account their fractal dimension. Addition of polyethylene glycol (PEG 2000) induced a marked decrease (more than 50%) of the sol viscosity down to a minimum. This is explained by assuming that PEG adsorbs on the surface of TiO(2) particles producing stabilization by steric effects and leading to formation of more compact aggregates. Without PEG the sol viscosity strongly decreases on aging. This effect is not caused by the growth of primary particles. It is rather interpreted as a progressive reorganization of the aggregates toward a more compact packing.
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PMID:Effect of PEG on rheology and stability of nanocrystalline titania hydrosols. 1950 38

The paper describes steady and dynamic rheological characterization of a system in which polyaniline (PAn) is dispersed in aqueous medium by the effect of a surfactant sodium dodecyl sulphate (SDS). During polymerization of aniline in SDS medium, large and agglomerated micelle-polymer structures are formed (supported by TEM and DLS) resulting in high viscosity of the medium. On application of steady shear micellar entanglements are ruptured and the system exhibits yield properties followed by shear thinning. From the frequency dependence of storage and loss modulii (G' and G'') it seems that the system behaves more like a viscous fluid rather than an elastic liquid. Carrying out the same experiments on another dispersion in which PAn is stabilized by dodecyl benzenesulphonic acid (DBSA), very different viscoelastic response was received. DBSA molecules become counter-ions to PAn chains and this way large and interconnected PAn-DBSA structures are formed by mutual sharing of DBSA anions and PAn chains. This system therefore, exhibits gel like properties and encounters a gel to sol transition at larger deformation. Detailed studies have established that PAn-SDS is a stabilized dispersion that resembles entangled polymeric solutions to some extent while PAn-DBSA is a partially flocculated system. Therefore, rheological response of the system is mainly governed by the mutual orientation of PAn with respect to the micelles rather than the individual properties of the components. None of these systems, however, follow the established Maxwell's model and a single relaxation time is not obtained. Rather, Rouse model of multiple relaxation times is partially applicable to PAn-SDS dispersion.
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PMID:Exploring properties of polyaniline-SDS dispersion: a rheological approach. 1966 41

Despite their immense potential, the ability to control the dispersion and microstructure of carbon nanotubes remains a hurdle for their widespread use. Poly(N-cyclopropylacrylamide), containing 5 mol % pyrene-bearing repeat units (p-PNCPA), is shown to vary the dispersion state of single-walled carbon nanotubes (SWNTs) in water. This is a thermo-responsive polymer whose conformation changes with temperature, which in turn leads to changes in the nanotube dispersion state. Cryo-TEM micrographs show that SWNTs stabilized using p-PNCPA transitions from a more exfoliated to a more bundled state as the aqueous suspension temperature is raised above the lower critical solution temperature (LCST) of the polymer (approximately 30 degrees C). Viscosity measurements on SWNT/p-PNCPA aqueous suspensions show shear thinning and near Newtonian behavior at 10 and 50 degrees C, respectively. Drying of these suspensions produces composites whose microstructure and electrical conductivity vary with drying temperature. This behavior has significant implications for the processing of carbon nanotubes and tailoring of composite properties. Such stimuli-controlled dispersion of carbon nanotubes could have a variety of applications in nanoelectronics, sensing, and drug and gene delivery systems.
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PMID:Temperature controlled dispersion of carbon nanotubes in water with pyrene-functionalized poly(N-cyclopropylacrylamide). 1973 43


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