Silica-protein composite layers of the giant basal spicules from Monorhaphis: Basis for their mechanical stability

2010 ◽  
Vol 82 (1) ◽  
pp. 175-192 ◽  
Author(s):  
Xiaohong Wang ◽  
Ute Schloßmacher ◽  
Klaus Peter Jochum ◽  
Lu Gan ◽  
Brigitte Stoll ◽  
...  

The hexactinellid sponge Monorhaphis chuni possesses with its giant basal spicules the largest biosilica structure on Earth. The approximately 8.5-mm-thick spicules are composed of up to 800 lamellae. By application of high-resolution electron microscopy (HR-SEM), it is shown that within the siliceous lamellae a proteinaceous scaffold exists which is composed of one protein of a size of 27 kDa. Analyses with Fourier transform infrared (FT-IR) emission and energy-dispersive X-ray (EDX) spectroscopy support this localization of the protein. No evidence for the presence of protein on the surfaces of the lamellae could be obtained. Heating the giant basal spicule to 600 °C destroys and eliminates the protein scaffold. At a temperature of 1600 °C, the lamellae fuse to solid glass via a nonstructured, foamed-up molten transition state. Elevation of the temperature to 2700 °C results in the formation of silica drops (Euplectella aspergillum). After the elimination of the protein scaffold from the silica lamellae, the spicules lose their mechanical characteristics of the original hydrated silica/protein composite to be flexible and simultaneously stiff and tough. The data presented here are expected to contribute to technologies suited to fabricate novel organic/inorganic (silica) hybrid fibers.

2006 ◽  
Vol 959 ◽  
Author(s):  
Floriana Vitale ◽  
Luciana Mirenghi ◽  
Emanuela Piscopiello ◽  
Maria Lucia Protopapa ◽  
Leander Tapfer ◽  
...  

ABSTRACTWe report on the synthesis and microstructural and microanalytical analysis of dodecanethiol and benzylthiol-stabilized Au nanoparticles (diameter range between 2 nm and 10 nm). Stable functionalized gold nanoparticles were synthesized by using two different routes: a two-phase liquid-liquid method and a one-phase method. The size, strain, shape and crystalline structure of the nanocrystals were determined by a full-pattern X-ray powder diffraction analysis and high-resolution electron microscopy. The chemical environment of the Au nanocrystals and their interaction with the thiols was investigated by X-ray photoelectron spectroscopy. Photoluminescence spectroscopy measurements show a characteristic IR emission at λ=960 nm of small sized Au nanocrystals (∼3 nm). The origin of this IR emission line seems to be correlated to the Au-S bonding and the size of the nanoparticles.


Author(s):  
Robert A. Grant ◽  
Laura L. Degn ◽  
Wah Chiu ◽  
John Robinson

Proteolytic digestion of the immunoglobulin IgG with papain cleaves the molecule into an antigen binding fragment, Fab, and a compliment binding fragment, Fc. Structures of intact immunoglobulin, Fab and Fc from various sources have been solved by X-ray crystallography. Rabbit Fc can be crystallized as thin platelets suitable for high resolution electron microscopy. The structure of rabbit Fc can be expected to be similar to the known structure of human Fc, making it an ideal specimen for comparing the X-ray and electron crystallographic techniques and for the application of the molecular replacement technique to electron crystallography. Thin protein crystals embedded in ice diffract to high resolution. A low resolution image of a frozen, hydrated crystal can be expected to have a better contrast than a glucose embedded crystal due to the larger density difference between protein and ice compared to protein and glucose. For these reasons we are using an ice embedding technique to prepare the rabbit Fc crystals for molecular structure analysis by electron microscopy.


Author(s):  
Y. Y. Wang ◽  
H. Zhang ◽  
V. P. Dravid ◽  
H. Zhang ◽  
L. D. Marks ◽  
...  

Azuma et al. observed planar defects in a high pressure synthesized infinitelayer compound (i.e. ACuO2 (A=cation)), which exhibits superconductivity at ~110 K. It was proposed that the defects are cation deficient and that the superconductivity in this material is related to the planar defects. In this report, we present quantitative analysis of the planar defects utilizing nanometer probe xray microanalysis, high resolution electron microscopy, and image simulation to determine the chemical composition and atomic structure of the planar defects. We propose an atomic structure model for the planar defects.Infinite-layer samples with the nominal chemical formula, (Sr1-xCax)yCuO2 (x=0.3; y=0.9,1.0,1.1), were prepared using solid state synthesized low pressure forms of (Sr1-xCax)CuO2 with additions of CuO or (Sr1-xCax)2CuO3, followed by a high pressure treatment.Quantitative x-ray microanalysis, with a 1 nm probe, was performed using a cold field emission gun TEM (Hitachi HF-2000) equipped with an Oxford Pentafet thin-window x-ray detector. The probe was positioned on the planar defects, which has a 0.74 nm width, and x-ray emission spectra from the defects were compared with those obtained from vicinity regions.


Author(s):  
W. Coene ◽  
F. Hakkens ◽  
T.H. Jacobs ◽  
K.H.J. Buschow

Intermetallic compounds of the type RE2Fe17Cx (RE= rare earth element) are promising candidates for permanent magnets. In case of Y2Fe17Cx, the Curie temperature increases from 325 K for x =0 to 550 K for x = 1.6 . X ray and electron diffraction reveal a carbon - induced structural transformation in Y2Fe17Cx from the hexagonal Th2Ni17 - type (x < 0.6 ) to the rhombohedral Th2Zn17 - type ( x ≥ 0.6). Planar crystal defects introduce local sheets of different magnetic anisotropy as compared with the ordered structure, and therefore may have an important impact on the coercivivity mechanism .High resolution electron microscopy ( HREM ) on a Philips CM30 / Super Twin has been used to characterize planar crystal defects in rhombohedral Y2Fe17Cx ( x ≥ 0.6 ). The basal plane stacking sequences are imaged in the [100] - orientation, showing an ABC or ACB sequence of Y - atoms and Fe2 - dumbbells, for both coaxial twin variants, respectively . Compounds resulting from a 3 - week annealing treatment at high temperature ( Ta = 1000 - 1100°C ) contain a high density of planar defects.


2003 ◽  
Vol 764 ◽  
Author(s):  
D.N. Zakharov ◽  
Z. Liliental-Weber ◽  
A. Motayed ◽  
S.N. Mohammad

AbstractOhmic Ta/Ti/Ni/Au contacts to n-GaN have been studied using high resolution electron microscopy (HREM), energy dispersive X-ray spectrometry (EDX) and electron energy loss spectrometry (EELS). Two different samples were used: A - annealed at 7500C withcontact resistance 5×10-6 Ω cm2 and B-annealed at 7750C with contact resistance 6×10-5 Ω cm2. Both samples revealed extensive in- and out-diffusion between deposited layers with some consumption ofGaNlayerand formation of TixTa1-xN50 (0<x<25) at the GaN interface. Almost an order of magnitude difference in contact resistances can be attributed to structure and chemical bonding of Ti-O layers formed on the contact surfaces.


2002 ◽  
Vol 20 (7) ◽  
pp. 619-632 ◽  
Author(s):  
A.A. Ali ◽  
F.A. Al-Sagheer ◽  
M.I. Zaki

Three different modifications of manganese(IV) oxide, viz. cryptomelane, nsutite and todorokite-like, were synthesized by hydrothermal methods. The bulk chemical composition, phase composition, crystalline structure and particle morphology of the resulting materials were determined by thermogravimetry, atomic absorption spectroscopy, X-ray diffractometry, infrared spectroscopy and scanning electron microscopy. The surface chemical composition, texture and structure were assessed using X-ray photoelectron microscopy, nitrogen sorptiometry and high-resolution electron microscopy. The results highlighted the hydrothermal conditions under which such tunnel-structured modifications of manganese(IV) oxide can be successfully synthesized. Moreover, they revealed that (i) the bulk was microcrystalline, (ii) the crystallites were either fibrils (cryptomelane and nsutite) or rod-like (todorokite) with low-index exposed facets, (iii) the surface chemical composition mostly reflected that of the bulk and (iv) the surface texture was linked with high specific areas, slit-shaped mesopores associated with particle interstices and micropores which allowed surface accessibility to the bulk tunnels of the test oxides. The application of such test oxides as shape-selective oxidation catalysts appears worthy of investigation.


1986 ◽  
Vol 77 ◽  
Author(s):  
Mary Beth Stearns ◽  
Amanda K. Petford-Long ◽  
C.-H. Chang ◽  
D. G. Stearns ◽  
N. M. Ceglio ◽  
...  

ABSTRACTThe technique of high resolution electron microscopy has been used to examine the structure of several multilayer systems (MLS) on an atomic scale. Mo/Si multilayers, in use in a number of x-ray optical element applications, and Mo/Si multilayers, of interest because of their magnetic properties, have been imaged in cross-section. Layer thicknesses, flatness and smoothness have been analysed: the layer width can vary by up to 0.6nm from the average value, and the layer flatness depends on the quality of the substrate surface for amorphous MLS, and on the details of the crystalline growth for the crystalline materials. The degree of crystallinity and the crystal orientation within the layers have also been investigated. In both cases, the high-Z layers are predominantly crystalline and the Si layers appear amorphous. Amorphous interfacial regions are visible between the Mo and Si layers, and crystalline cobalt suicide interfacial regions between the Co and Si layers. Using the structural measurements obtained from the HREM results, theoretical x-ray reflectivity behaviour has been calculated. It fits the experimental data very well.


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