Nano-Structural Elucidation in Carbon Black Loaded NR Vulcanizate by 3D-TEM and In Situ WAXD Measurements

2007 ◽  
Vol 80 (2) ◽  
pp. 251-264 ◽  
Author(s):  
Yuko Ikeda ◽  
Atsushi Kato ◽  
Junichi Shimanuki ◽  
Shinzo Kohjiya ◽  
Masatoshi Tosaka ◽  
...  
Keyword(s):  
Carbon Black ◽  
Computerized Tomography ◽  
3D Visualization ◽  
Tensile Elongation ◽  
Three Dimensional ◽  
Structural Features ◽  
Field Method ◽  
Transmission Electron ◽  
Sample Chamber

Abstract Three dimensional (3D) visualization of nanometer structure of carbon black dispersion in rubbery matrix has successfully been studied and reported in this paper. Use of 3D-TEM, which is computerized tomography combined with transmission electron microscopy (TEM), enabled us to reconstruct 3D images of carbon black aggregates in natural rubber (NR) matrix. The TEM measurements were conducted by a bright-field method on thin samples without any electron staining. The sample was subject to uni-axial tilting (+65 degree to −65 degree with 2 degree increment) in the sample chamber, and 66 TEM images were taken on each sample. These TEM images were used for computerized tomography to reconstruct the 3D image. This technique is designated as 3D-TEM. The nano-structural features observed by 3D-TEM were in conformity with the electron-conductivity results, and the percolation behavior was recognized. These results were further supplemented by in situ wide-angle X-ray diffraction (WAXD), i.e., simultaneous WAXD and tensile measurements on the sample to observe the strain-induced crystallization in NR vulcanizate. Upon tensile elongation, the crystallization was clearly observed in WAXD in the presence of carbon black, and it contributed to the tensile properties. In order to understand the performances of filled NR vulcanizates, it surely is necessary to know the structural states of the mixed nano-filler and the crystallites produced upon elongation.

Nanostructure in Traditional Composites of Natural Rubber and Reinforcing Silica

2007 ◽  
Vol 80 (4) ◽  
pp. 690-700 ◽  
Author(s):  
Atsushi Kato ◽  
Shinzo Kohjiya ◽  
Yuko Ikeda
Keyword(s):  
Electron Microscopy ◽  
Carbon Black ◽  
Natural Rubber ◽  
Electron Tomography ◽  
3D Visualization ◽  
Three Dimensional ◽  
Rubber Matrix ◽  
3D Images ◽  
Transmission Electron ◽  
Filler Dispersion

Abstract Usual rubber products are a composite from rubber and nano-filler (e.g. silica, carbon black, etc.), and it is believed that the good dispersion of the nano-filler is the most important issue determining the performance of rubber vulcanizates. So far, transmission electron microscopy (TEM) has been the most useful tool for evaluation of the dispersion. However, it affords images of the sample projected on an x, y-plane, and the information along the thickness (z-axis) direction is missing. Three-dimensional (3D) visualization of nanometer structure of nano-filler dispersion in a rubber matrix is what all rubber technologists have been dreaming of. This dream is at last realized, and described in this paper. Use of TEM combined with computerized tomography (abbreviated as 3D-TEM in this paper, which is sometimes called electron tomography) enabled us to reconstruct 3D images of nano-filler (silica or carbon black) aggregates in rubbery matrix. It is said that nano-filler aggregate is a structure of size from 10 nm to 1000 nm, and agglomerate is an even larger structure. The 3D-TEM results on silica aggregates in natural rubber were presented in this paper. Silica aggregates were characterized by combining the 3D images of the vulcanizates. Furthermore, density of silica loaded natural rubber as an example of physical properties, was measured, and explained by the structure elucidated by 3D-TEM.

Three-Dimensional Morphology of Carbon Black in NR Vulcanizates as Revealed by 3D-Tem and Dielectric Measurements

2006 ◽  
Vol 79 (4) ◽  
pp. 653-673 ◽  
Author(s):  
Atsushi Kato ◽  
Junichi Shimanuki ◽  
Shinzo Kohjiya ◽  
Yuko Ikeda
Keyword(s):  
Carbon Black ◽  
Natural Rubber ◽  
Physical Properties ◽  
Rational Design ◽  
Electron Tomography ◽  
3D Visualization ◽  
Three Dimensional ◽  
Rubber Matrix ◽  
3D Images ◽  
Transmission Electron

Abstract Usual rubber products are a composite from rubber and nano-filler (e.g. carbon black, silica, etc.), and it is believed that the good dispersion of the nano-filler is the most important issue determining the performance of rubber vulcanizates. So far, transmission electron microscopy (TEM) has been the most useful tool for evaluation of the dispersion. However, it affords images of the sample projected on an x, y-plane, and the information along the thickness (z-axis) direction is missing. Three-dimensional (3D) visualization of nanometer structure of nano-filler dispersion in a rubber matrix is what all rubber technologists have been dreaming of. This dream is at last realized, and described in this paper. Use of TEM combined with computerized tomography (abbreviated as 3D-TEM in this paper, which is sometimes called electron tomography) enabled us to reconstruct 3D images of nano-filler aggregates in rubbery matrix. The 3D-TEM results on carbon black in natural rubber were presented in this paper. The network structure formed by agglomeration of carbon black aggregates was elucidated by combining the 3D images and physical properties of the vulcanizates. Density, electrical resistivity and dielectric relaxation of carbon black loaded natural rubber as an example of physical properties, were measured, and explained by the structure elucidated by 3D-TEM. This technique will prove to be more and more important for the rational design of the nano-composites of rubbery matrix.

Dynamics of Nanoparticle Chain Aggregates of Carbon Under Tension

2003 ◽  
Vol 778 ◽  
Author(s):  
Rajdip Bandyopadhyaya ◽  
Weizhi Rong ◽  
Yong J. Suh ◽  
Sheldon K. Friedlander
Keyword(s):  
Mechanical Properties ◽  
Carbon Black ◽  
Polymer Film ◽  
Elastic Behavior ◽  
Small Strains ◽  
Transmission Electron ◽  
Chain Aggregates ◽  
Nanoparticle Chains ◽  
Reinforcing Filler

AbstractCarbon black in the form of nanoparticle chains is used as a reinforcing filler in elastomers. However, the dynamics of the filler particles under tension and their role in the improvement of the mechanical properties of rubber are not well understood. We have studied experimentally the dynamics of isolated nanoparticle chain aggregates (NCAs) of carbon made by laser ablation, and also that of carbon black embedded in a polymer film. In situ studies of stretching and contraction of such chains in the transmission electron microscope (TEM) were conducted under different maximum values of strain. Stretching causes initially folded NCA to reorganize into a straight, taut configuration. Further stretching leads to either plastic deformation and breakage (at 37.4% strain) or to a partial elastic behavior of the chain at small strains (e.g. 2.3% strain). For all cases the chains were very flexible under tension. Similar reorientation and stretching was observed for carbon black chains embedded in a polymer film. Such flexible and elastic nature of NCAs point towards a possible mechanism of reinforcement of rubber by carbon black fillers.

scholarly journals Morphology and Mechanical Properties of Fossil Diatom Frustules from Genera of Ellerbeckia and Melosira

Nanomaterials ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 1615
Author(s):  
Qiong Li ◽  
Jürgen Gluch ◽  
Zhongquan Liao ◽  
Juliane Posseckardt ◽  
André Clausner ◽  
...  
Keyword(s):  
Fracture Behavior ◽  
Three Dimensional ◽  
Mechanical Tests ◽  
Fracture Force ◽  
Thickness Change ◽  
X Ray ◽  
Transmission Electron ◽  
Percentage Concentration ◽  
Morphology Characterization

Fossil frustules of Ellerbeckia and Melosira were studied using laboratory-based nano X-ray tomography (nano-XCT), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS). Three-dimensional (3D) morphology characterization using nondestructive nano-XCT reveals the continuous connection of fultoportulae, tube processes and protrusions. The study confirms that Ellerbeckia is different from Melosira. Both genera reveal heavily silicified frustules with valve faces linking together and forming cylindrical chains. For this cylindrical architecture of both genera, valve face thickness, mantle wall thickness and copulae thickness change with the cylindrical diameter. Furthermore, EDS reveals that these fossil frustules contain Si and O only, with no other elements in the percentage concentration range. Nanopores with a diameter of approximately 15 nm were detected inside the biosilica of both genera using TEM. In situ micromechanical experiments with uniaxial loading were carried out within the nano-XCT on these fossil frustules to determine the maximal loading force under compression and to describe the fracture behavior. The fracture force of both genera is correlated to the dimension of the fossil frustules. The results from in situ mechanical tests show that the crack initiation starts either at very thin features or at linking structures of the frustules.

scholarly journals Correlation between structure and mass distribution of the nuclear pore complex and of distinct pore complex components.

1990 ◽  
Vol 110 (4) ◽  
pp. 883-894 ◽  
Author(s):  
R Reichelt ◽  
A Holzenburg ◽  
E L Buhle ◽  
M Jarnik ◽  
A Engel ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Nuclear Envelope ◽  
Three Dimensional ◽  
Structural Features ◽  
Nuclear Pore ◽  
Xenopus Laevis Oocyte ◽  
Three Dimensional Model ◽  
Transmission Electron ◽  
Freeze Dried

Nuclear pore complexes (NPCs) prepared from Xenopus laevis oocyte nuclear envelopes were studied in "intact" form (i.e., unexposed to detergent) and after detergent treatment by a combination of conventional transmission electron microscopy (CTEM) and quantitative scanning transmission electron microscopy (STEM). In correlation-averaged CTEM pictures of negatively stained intact NPCs and of distinct NPC components (i.e., "rings," "spoke" complexes, and "plug-spoke" complexes), several fine structural features arranged with octagonal symmetry about a central axis could reproducibly be identified. STEM micrographs of unstained/freeze-dried intact NPCs as well as of their components yielded comparable but less distinct features. Mass determination by STEM revealed the following molecular masses: intact NPC with plug, 124 +/- 11 MD; intact NPC without plug, 112 +/- 11 MD; heavy ring, 32 +/- 5 MD; light ring, 21 +/- 4 MD; plug-spoke complex, 66 +/- 8 MD; and spoke complex, 52 +/- 3 MD. Based on these combined CTEM and STEM data, a three-dimensional model of the NPC exhibiting eightfold centrosymmetry about an axis perpendicular to the plane of the nuclear envelope but asymmetric along this axis is proposed. This structural polarity of the NPC across the nuclear envelope is in accord with its well-documented functional polarity facilitating mediated nucleocytoplasmic exchange of molecules and particles.

High-Efficiency Three-Dimensional Visualization of Complex Microstructures via Multidimensional STEM Acquisition and Reconstruction

2020 ◽  
Vol 26 (2) ◽  
pp. 240-246 ◽  
Author(s):  
Kevin G. Field ◽  
Benjamin P. Eftink ◽  
Chad M. Parish ◽  
Stuart A. Maloy
Keyword(s):  
High Efficiency ◽  
3D Visualization ◽  
Accurate Determination ◽  
Three Dimensional ◽  
High Energy ◽  
Scanning Transmission Electron Microscope ◽  
Chromium Steel ◽  
Transmission Electron ◽  
Scanning Transmission

AbstractComplex material systems in which microstructure and microchemistry are nonuniformly dispersed require three-dimensional (3D) rendering(s) to provide an accurate determination of the physio-chemical nature of the system. Current scanning transmission electron microscope (STEM)-based tomography techniques enable 3D visualization but can be time-consuming, so only select systems or regions are analyzed in this manner. Here, it is presented that through high-efficiency multidimensional STEM acquisition and reconstruction, complex point cloud-like microstructural features can quickly and effectively be reconstructed in 3D. The proposed set of techniques is demonstrated, analyzed, and verified for a high-chromium steel with heterogeneously situated features induced using high-energy neutron bombardment.

Anisometry Measurements in Carbon Black Aggregate Populations

1997 ◽  
Vol 70 (5) ◽  
pp. 727-746 ◽  
Author(s):  
Tyler C. Gruber ◽  
Charles R. Herd
Keyword(s):  
Carbon Black ◽  
Three Dimensional ◽  
Aggregate Size ◽  
Automated Image Analysis ◽  
Morphological Parameters ◽  
Aggregate Structure ◽  
Transmission Electron ◽  
Area And Perimeter ◽  
Dimensional Shape ◽  
Lower Structure

Abstract Transmission electron microscopy with automated image analysis (TEM/AIA) was used to characterize the three-dimensional morphology and anisometry of carbon black aggregates. Individual carbon black aggregates were imaged at multiple goniometer angles, and their three-dimensional aggregate structure was modeled, yielding greatly enhanced morphological information. Aggregate size distributional properties were determined at multiple goniometer orientations for N300 and N600 series grades of varying aggregate structure levels. Aggregate projections were found to exhibit statistical decreases of 10 to 25% in area and perimeter with rotation. Decreases in other morphological parameters, including non-dimensional shape parameters, were also observed. In general, higher structure grades (aggregates) were found to display larger relative changes in morphological parameters with rotation than lower structure grades. Ramifications for conventional TEM/AIA and void-volume/polymer occlusion capacity measurements are addressed. Further analysis includes an assessment of aggregate anisometry on the TEM sample grid and new insights into the three dimensional nature of carbon black aggregate structure.

3D Morphological Characterization of Carbon-Black Aggregates Using Transmission Electron Microscopy

1994 ◽  
Vol 67 (2) ◽  
pp. 280-287 ◽  
Author(s):  
Tyler C. Gruber ◽  
T. W. Zerda ◽  
Michel Gerspacher
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Carbon Black ◽  
Three Dimensional ◽  
Reconstruction Algorithm ◽  
Morphological Characterization ◽  
Three Dimensional Modeling ◽  
Transmission Electron ◽  
Best Fitting ◽  
Using Data

Abstract A three-dimensional modeling technique is used to characterize the structure of carbon-black aggregates. The relative positions of individual particles in aggregates are determined using transmission electron microscopy (TEM). Data are acquired from two-dimensional projections taken with the aggregates at two different orientations with respect to the electron beam. Computerized aggregate models are generated using data from TEM projections in our reconstruction algorithm. Inspection of these models shows that their projections very closely replicate the TEM micrographs. Quantitative analysis of the aggregate models reveals that aggregates generally exhibit anisotropy, in the form of a reduction of aggregate breadth, or “flatness,” in one direction. The flat sides tend to align preferentially, along the plane of the TEM sample grid. The dimensions for each aggregate with respect to its best-fitting plane of flatness are determined, and are related through a “flatness index.”

Crystallographic Features of the A-Type and CE-Type Antiferromagnetic States in the Simple-Perovskite Manganite System Sr1-xNdxMnO3

2011 ◽  
Vol 409 ◽  
pp. 532-537
Author(s):  
Yusuke Onezawa ◽  
Yasuhide Inoue ◽  
Masazumi Arao ◽  
Yasumasa Koyama
Keyword(s):  
Room Temperature ◽  
Three Dimensional ◽  
Electronic System ◽  
Paramagnetic State ◽  
Heating Process ◽  
In Situ Observation ◽  
Perovskite Manganite ◽  
Transmission Electron ◽  
Highly Correlated

The electronic states of Sr1-xNdxMnO3 with the simple perovskite structure are characterized by a three-dimensional highly-correlated electronic system. To understand the detailed features of the A-and CE-type antiferromagnetic states in this system, their crystallographic features for x = 0.47, 0.48, and 0.50 have been investigated mainly by both x-ray powder diffraction and transmission electron microscopy. It was found at room temperature that the crystal structure for x = 0.47 was determined to have the monoclinic C2/m symmetry, while the orthorhombic Imma structure was confirmed for x = 0.48 and 0.50. The in-situ observation for x = 0.47 indicated that, in the heating process from room temperature, the C2/m-to-Imma transition occurred in the paramagnetic state, and that the A-type antiferromagnetic state appeared below about 200 K on cooling. In addition, the cooling from room temperature for x = 0.48 and 0.50 resulted in the direct transitions from the orthorhombic Imma state to the A-and CE-type antiferromagnetic states, respectively. Based on these features, we simply discussed the physical origin of the appearance of the paramagnetic state with the monoclinic symmetry for x = 0.47.

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