Nano-structural observation of carbon black dispersion in natural rubber matrix by three-dimensional transmission electron microscopy

2005 ◽  
Vol 40 (9-10) ◽  
pp. 2553-2555 ◽  
Author(s):  
S. Kohjiya ◽  
A. Katoh ◽  
J. Shimanuki ◽  
T. Hasegawa ◽  
Y. Ikeda
2007 ◽  
Vol 80 (4) ◽  
pp. 690-700 ◽  
Author(s):  
Atsushi Kato ◽  
Shinzo Kohjiya ◽  
Yuko Ikeda

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.


2006 ◽  
Vol 514-516 ◽  
pp. 353-358 ◽  
Author(s):  
Shinzo Kohjiya

. Generally rubber products are a typical soft material, and a composite of a nano-filler (typically, carbon black or particulate silica) and a rubber (natural rubber and various synthetics are used). The properties of these soft nano-composites have been well known to depend on the dispersion of the nano-filler in the rubbery matrix. The most powerful tool for the elucidation of it has been transmission electron microscopy (TEM). The microscopic techniques are based on the projection of 3-dimensional (3D) body on a plane (x, y plane), thus the structural information along the thickness (z axis) direction of the sample is difficult to obtain. This paper describes our recent results on the dispersion of carbon black (CB) and particulate silica in natural rubber (NR) matrix observed by TEM combined with electron tomography (3D-TEM) technique, which enabled us to obtain images of 3D nano-structure of the sample. Thus, 3D images of CB and silica in NR matrix are visualized and analyzed in this communication. These results are precious ones for the design of soft nano-composites, and the technique will become an indispensable one in nanotechnology.


1994 ◽  
Vol 67 (2) ◽  
pp. 280-287 ◽  
Author(s):  
Tyler C. Gruber ◽  
T. W. Zerda ◽  
Michel Gerspacher

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.”


2006 ◽  
Vol 79 (4) ◽  
pp. 653-673 ◽  
Author(s):  
Atsushi Kato ◽  
Junichi Shimanuki ◽  
Shinzo Kohjiya ◽  
Yuko Ikeda

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.


Author(s):  
W. D. Cooper ◽  
C. S. Hartley ◽  
J. J. Hren

Interpretation of electron microscope images of crystalline lattice defects can be greatly aided by computer simulation of theoretical contrast from continuum models of such defects in thin foils. Several computer programs exist at the present time, but none are sufficiently general to permit their use as an aid in the identification of the range of defect types encountered in electron microscopy. This paper presents progress in the development of a more general computer program for this purpose which eliminates a number of restrictions contained in other programs. In particular, the program permits a variety of foil geometries and defect types to be simulated.The conventional approximation of non-interacting columns is employed for evaluation of the two-beam dynamical scattering equations by a piecewise solution of the Howie-Whelan equations.


1990 ◽  
Vol 110 (4) ◽  
pp. 883-894 ◽  
Author(s):  
R Reichelt ◽  
A Holzenburg ◽  
E L Buhle ◽  
M Jarnik ◽  
A Engel ◽  
...  

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.


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