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.”

Rapid and Semi-automated Method for Analysis of the Number of Atoms of Ultra-small Platinum Clusters on Carbon

2000 ◽  
Vol 6 (4) ◽  
pp. 353-357
Author(s):  
J.C. Yang ◽  
S. Bradley ◽  
J.M. Gibson
Keyword(s):  
Three Dimensional ◽  
Scanning Transmission Electron Microscope ◽  
Dark Field ◽  
Spectroscopic Technique ◽  
Automated Method ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Dimensional Shape ◽  
Three Dimensional Shape

Abstract Very high angle (~100 mrad) annular dark-field (HAADF) images in a dedicated scanning transmission electron microscope (STEM) can be used to quantitatively measure the number of atoms in a cluster on a support material. We have developed a computer program which will automatically find the location of the particles and then integrate the intensity to find the number of atoms per cluster. We have examined ultra-small Pt clusters on a C substrate by this novel mass-spectroscopic technique. We discovered that the Pt clusters maintain their three-dimensional shape, and are probably spherical.

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.

Characterization of Dispersions

1991 ◽  
Vol 64 (3) ◽  
pp. 386-449 ◽  
Author(s):  
W. M. Hess
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Carbon Black ◽  
Phase Distribution ◽  
Automated Image Analysis ◽  
Carbon Blacks ◽  
Transmission Electron ◽  
Vehicle Systems ◽  
Scanning Electron

Abstract The methods of pigment dispersion analysis have been reviewed in regard to their application to rubber, plastics, and other vehicle systems. The characteristics of dispersions have been divided into three categories: (1) agglomeration (2) microdispersion (networking) and (3) polymer-phase distribution. Stylus roughness measurements on cut surfaces offer the combination of simplicity and speed of operation with high accuracy and precision for measuring pigment agglomeration in elastomer systems of known composition. This method may also be applied to the surface of thin plastic extrudates. However, optical analyses of thin cryosections are preferred for most plastics or unknown rubber compounds containing high loadings of carbon black. X-radiography is generally preferable for the analysis of inorganic agglomeration in most polymeric vehicle systems. The scanning electron microscope is also applicable for this type of analysis and has the added capability of identifying unknown agglomerates by energy dispersive x-ray analysis. Automated image-analysis techniques may also be utilized in conjunction with microscopical methods for quantifying the agglomeration of most types of pigments. For carbon blacks, the most suitable materials for on-line image analyses with transmitted light are plastics, paints, and inks which contain low black loadings. Higher carbon-black loadings in rubber can be analyzed by incident light using metallographic polishing of sulfur-hardened specimens. The microdispersion of carbon blacks at the primary aggregate level can be measured by means of electrical conductivity. This method is not applicable to inorganic pigments, large-particle-size carbon blacks, or blacks at very high or low loadings. Pigment microdispersion in different vehicle systems may also be assessed by means of scanning electron microscopy of thick cross sections (plasma etched to enhance contrast) or by transmission electron microscopy of thin cryosections. The tendency for the finer pigments to form 3-dimensional network structures in elastomers may also be measured as a function of the augmentation of dynamic modulus from high to low strain amplitudes. Pigment phase distribution in elastomer blends may be studied by scanning electron microscopy or transmission electron microscopy of thin cryosections, in conjunction with a staining or etching procedure to produce contrast between the separate polymer components. Selective staining is applicable to blends of polymers which differ significantly in their relative levels of unsaturation (e.g., NR/CIIR). Pyrolytic etching (under vacuum) may be used to produce interzone contrast in blends of polymers which differ significantly in their resistance to thermal degradation (e.g., NR/BR, NR/SBR). Pyrolysis GC may be utilized to determine the amount of carbon black in the separate phases of certain elastomer blends. This method is based on the relative intensity of the primary GC peaks for the individual polymers. The chromatographs are obtained from the bound rubber (carbon-polymer gel) that is developed during the mixing of the compound.

Three Dimensional Ultra-Small Pt Clusters on Carbon As Studied by A Novel Stem Technique

1998 ◽  
Vol 549 ◽  
Author(s):  
J. C. Yang ◽  
S. Bradley ◽  
J. M. Gibson
Keyword(s):  
Three Dimensional ◽  
Scanning Transmission Electron Microscope ◽  
Dark Field ◽  
Spectroscopic Technique ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Dimensional Shape ◽  
Three Dimensional Shape ◽  
Very High

AbstractVery high angle (∼ 100mrad) annular dark-field (HAADF) images in a dedicated scanning transmission electron microscope (STEM) can be used to quantitatively measure the number of atoms in a cluster on a support material. We have developed a computer program which will automatically find the location of the particles and then integrate the intensity to find the number of atoms per cluster. We have examined ultra-small Pt clusters on a C substrate by this novel mass-spectroscopic technique. We discovered that the Pt clusters maintain their three-dimensional shape, and are probably spherical in shape.

Rapid and Semi-automated Method for Analysis of the Number of Atoms of Ultra-small Platinum Clusters on Carbon

2000 ◽  
Vol 6 (4) ◽  
pp. 353-357 ◽  
Author(s):  
J.C. Yang ◽  
S. Bradley ◽  
J.M. Gibson
Keyword(s):  
Three Dimensional ◽  
Scanning Transmission Electron Microscope ◽  
Dark Field ◽  
Spectroscopic Technique ◽  
Automated Method ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Dimensional Shape ◽  
Three Dimensional Shape

AbstractVery high angle (~100 mrad) annular dark-field (HAADF) images in a dedicated scanning transmission electron microscope (STEM) can be used to quantitatively measure the number of atoms in a cluster on a support material. We have developed a computer program which will automatically find the location of the particles and then integrate the intensity to find the number of atoms per cluster. We have examined ultra-small Pt clusters on a C substrate by this novel mass-spectroscopic technique. We discovered that the Pt clusters maintain their three-dimensional shape, and are probably spherical.

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.

scholarly journals CaCO3–Polymer Nanocomposite Prepared with Supercritical CO2

2018 ◽  
Vol 2018 ◽  
pp. 1-6 ◽  
Author(s):  
Hiroaki Wakayama
Keyword(s):  
Polymer Matrix ◽  
Three Dimensional ◽  
Polymer Nanocomposite ◽  
Laser Raman Spectroscopy ◽  
Poly Vinyl Alcohol ◽  
Laser Raman ◽  
Transmission Electron ◽  
Dimensional Shape ◽  
Ca Ions ◽  
Three Dimensional Shape

A novel process for generation of a CaCO3–polymer nanocomposite with a controlled three-dimensional shape was developed. Specifically, a nanocomposite with a high CaCO3 content was produced by introducing supercritical CO2 into a polymer matrix containing Ca ions. A mixture of poly(vinyl alcohol), Ca acetate, and poly(acrylic acid) was poured into a mold, the mold was placed in an autoclave, and CO2 was introduced to precipitate CaCO3 within the polymer matrix. Laser Raman spectroscopy and transmission electron microscopy showed that this process produced a nanocomposite containing highly dispersed CaCO3 (aragonite) nanoparticles. The flexural strength of the nanocomposite was larger than the flexural strengths of limestone and CaCO3 produced by hydrothermal hot pressing. The use of supercritical CO2 facilitated CO2 dissolution, which resulted in rapid precipitation of CaCO3 in the polymer matrix. The above-described process has potential utility for fixation of CO2.

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