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.

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 Dispersion of Nano-Fillers in Soft Composite as Revealed by Transmission Electron Microscopy/Electron Tomography (3D-TEM)

2006 ◽  
Vol 514-516 ◽  
pp. 353-358 ◽  
Author(s):  
Shinzo Kohjiya
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Carbon Black ◽  
Natural Rubber ◽  
Structural Information ◽  
Electron Tomography ◽  
Nano Composites ◽  
Nano Structure ◽  
Transmission Electron ◽  
Particulate Silica

. 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.

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.

Extraction and identification of fillers and pigments from pyrolyzed rubber and tire samples

1996 ◽  
Vol 54 ◽  
pp. 174-175
Author(s):  
P. Sadhukhan ◽  
J. B. Zimmerman
Keyword(s):  
Zinc Oxide ◽  
Electron Microscope ◽  
Carbon Black ◽  
Natural Rubber ◽  
Transmission Electron Microscope ◽  
Rolling Resistance ◽  
Synthetic Polymers ◽  
Nitrogen Atmosphere ◽  
Transmission Electron ◽  
Curing Agents

Rubber stocks, specially tires, are composed of natural rubber and synthetic polymers and also of several compounding ingredients, such as carbon black, silica, zinc oxide etc. These are generally mixed and vulcanized with additional curing agents, mainly organic in nature, to achieve certain “designing properties” including wear, traction, rolling resistance and handling of tires. Considerable importance is, therefore, attached both by the manufacturers and their competitors to be able to extract, identify and characterize various types of fillers and pigments. Several analytical procedures have been in use to extract, preferentially, these fillers and pigments and subsequently identify and characterize them under a transmission electron microscope.Rubber stocks and tire sections are subjected to heat under nitrogen atmosphere to 550°C for one hour and then cooled under nitrogen to remove polymers, leaving behind carbon black, silica and zinc oxide and 650°C to eliminate carbon blacks, leaving only silica and zinc oxide.

A Novel Method for Automated Acquisition of Tilt Series for Electron Tomography Based on Pre-Calibration of the Specimen Stage

2000 ◽  
Vol 6 (S2) ◽  
pp. 1148-1149
Author(s):  
U. Ziese ◽  
A.H. Janssen ◽  
T.P. van der Krift ◽  
A.G. van Balen ◽  
W.J. de Ruijter ◽  
...  
Keyword(s):  
High Resolution ◽  
3D Reconstruction ◽  
Cell Biology ◽  
Electron Tomography ◽  
Three Dimensional ◽  
Imaging Method ◽  
3D Images ◽  
Tilt Series ◽  
3D Information ◽  
Structural Arrangements

Electron tomography is a three-dimensional (3D) imaging method with transmission electron microscopy (TEM) that provides high-resolution 3D images of structural arrangements. Conventional TEM images are in first approximation mere 2D-projections of a 3D sample under investigation. With electron tomographya series of images is acquired of a sample that is tilted over a large angular range (±70°) with small angular tilt increments (so called tilt-series). For the subsequent 3D-reconstruction, the images of the tilt series are aligned relative to each other and the 3D-reconstruction is computed. Electron tomography is the only technique that can provide true 3D information with nm-scale resolution of individual and unique samples. For (cell) biology and material science applications the availability of high-resolution 3D images of structural arrangements within individual samples provides unique architectural information that cannot be obtained otherwise. Routine application of electron tomography will comprise a major revolutionary step forward in the characterization of complex materials and cellular arrangements.

Properties of Natural Rubber Nanocomposites Reinforced with Carbon Nanotubes

2015 ◽  
Vol 1109 ◽  
pp. 195-199 ◽  
Author(s):  
Abd Aziz Azira ◽  
Dayang Habibah Abangismawi I. Hassim ◽  
D. Verasamy ◽  
Abu Bakar Suriani ◽  
M. Rusop
Keyword(s):  
Electron Microscopy ◽  
Mechanical Properties ◽  
Natural Rubber ◽  
Considerable Increase ◽  
Physical And Mechanical Properties ◽  
Rubber Matrix ◽  
Rubber Composites ◽  
Transmission Electron ◽  
Maximum Conductivity ◽  
Polymer Latex

In order to achieve improvements in the performance of rubber materials, the development of carbon nanotube (CNT)-reinforced rubber composites was attempted. The CNT/epoxidised natural rubber (ENR) nanocomposite was prepared through latex technology. Physical and mechanical properties of the CNT/ENR nanocomposites were characterized in contrast to the carbon black (CB)/ENR composite. The dispersion of the CNTs in the rubber matrix and interfacial bonding between them were rather good; monitored transmission electron microscopy and scanning electron microscopy. The mechanical properties of the CNT-reinforced ENR showed a considerable increase compared to the neat ENR and traditional CB/ENR composite. The storage modulus of the CNT/ENR nanocomposites greatly exceeds that of neat ENR and CB/ENR composites and a maximum conductivity of about 1 S m-1 can be achieved. The approach presented can be adapted to other CNT/polymer latex systems.

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