The Dark Field Cut Surface (DFCS) Test for Estimating the Dispersion of Carbon Black in Rubber Compounds

1997 ◽  
Vol 70 (1) ◽  
pp. 50-59 ◽  
Author(s):  
G. A. W. Murray ◽  
D. W. Southwart ◽  
P. K. Freakley

Abstract A test for estimating the dispersion of carbon black in rubber compounds is described. It works by examining the freshly cut surface of a specimen at low magnification in dark field illumination. Roughness of the surface related to the presence of carbon black causes increased reflection under dark field illumination. The illumination of each field of view is examined as 100 subdivisions and the relative values of these readings give a numerical estimate of the dispersion. Details of how this is done and the corrections applied to the results are described. A second paper reports some initial results obtained with the test. The test works well for certain elastomers, notably NR and SBR. The biggest advantage of the test is its ability to work rapidly and cheaply on small zones at relatively high magnification. This opens up the possibility of detailed studies of macroscopic variations in dispersion, done in reasonable times and at reasonable costs.

1997 ◽  
Vol 70 (1) ◽  
pp. 38-49
Author(s):  
G. A. W. Murray ◽  
B. H. R. Ng ◽  
M. R. Vaseghi Jahromi ◽  
D. W. Southwart

Abstract The Dark Field Cut Surface (DFCS) test is a quantitative method for determining the state of dispersion of carbon black in rubber compounds. The method has been described fully in another paper. Here are reported some of the first applications of the test and some trials that were carried out specifically to investigate and develop the DFCS test. The test is demonstrated to follow accurately the progress of dispersion of carbon black in milled or mixed compounds of NR and SBR. Some tests have been carried out using large batches of test results and these have demonstrated a good fit with a normal distribution. By this means, some recommendations have been derived for suitable sampling rates. The relative merits of the standard deviation and the average for characterizing dispersion have been highlighted. A further way of presenting the results as distribution curves has been demonstrated. A check has been performed to demonstrate that mastication of rubber has little or no influence on the DFCS test results. The DFCS test has been used to give an interesting (provisional) insight to the best ways to operate a rubber mixer. To date, the measured patterns of scattered light show a promising correlation with the anticipated dispersion of carbon black in the specimens tested.


1930 ◽  
Vol 3 (4) ◽  
pp. 755-763
Author(s):  
Raymond P. Allen

Abstract THE possibility of seeing pigment particles in a rubber stock has always been a desire of rubber chemists. There has been a natural belief that if the particles in rubber could actually be observed with a microscope more could be learned about their action and properties. The main difficulty in attaining this end lies in the preparation of sufficiently thin sections. For clear observation of highly loaded gas-black stocks the sections must be less than 1 micron thick. For bright-field work with light-colored or colorless pigments, such as litharge and zinc oxide, the sections may be somewhat thicker. However, if the examination is to be made with dark-field illumination the sections for even the colorless pigments must again be very thin. Several methods have been proposed and utilized for making thin sections, and the names of Dannenberg (2), Depew (3), Green (4), Grenquist (5), Hauser (7), Moore (11), Pohle (9), Ruby (3), Spear (11), and Walton (12) are identified with the skilful manipulation which is necessary for achieving the desired result. There have been many other workers in this field, including Weber (13), Breuil (1), Loewen (8), Regnaud (10), and Hardman (6). The method to be described was developed in this laboratory in 1926. It has been used continually since that time and has proved valuable in the study of rubber compounds and pigments. While it bears a slight similarity to some of the other methods, it has certain unique and distinct advantages of its own.


2004 ◽  
Vol 77 (4) ◽  
pp. 691-710 ◽  
Author(s):  
Archie P. Smith ◽  
Toni L. Aybar ◽  
Ricky W. Magee ◽  
Charles R. Herd

Abstract A new method for characterizing the carbon black dispersion in rubber compounds is introduced. This technique is based on interferometric microscopy (IFM) and utilizes the interference fringes between in-phase light beams reflected from the rubber sample and a smooth reference surface to measure the three-dimensional surface topography. The peaks and valleys present on the fresh-cut surface are representative of the carbon black agglomerates and are used to characterize the dispersion. A series of samples with different base rubbers and varying dispersion levels were created and characterized by both light microscopy and IFM. These results were used to generate a universal dispersion index based on the IFM data that correlates well with the LM dispersion index values. In addition, three-dimensional peak statistics were obtained from the IFM data and used to provide additional information about the carbon black agglomerate distribution. This data can be used for a more complete understanding of the compound behavior as a function of the carbon black dispersion and agglomerate distribution.


Author(s):  
Akira Tanaka ◽  
David F. Harling

In the previous paper, the author reported on a technique for preparing vapor-deposited single crystal films as high resolution standards for electron microscopy. The present paper is intended to describe the preparation of several high resolution standards for dark field microscopy and also to mention some results obtained from these studies. Three preparations were used initially: 1.) Graphitized carbon black, 2.) Epitaxially grown particles of different metals prepared by vapor deposition, and 3.) Particles grown epitaxially on the edge of micro-holes formed in a gold single crystal film.The authors successfully obtained dark field micrographs demonstrating the 3.4Å lattice spacing of graphitized carbon black and the Au single crystal (111) lattice of 2.35Å. The latter spacing is especially suitable for dark field imaging because of its preparation, as in 3.), above. After the deposited film of Au (001) orientation is prepared at 400°C the substrate temperature is raised, resulting in the formation of many square micro-holes caused by partial evaporation of the Au film.


2017 ◽  
Vol 59 (11-12) ◽  
pp. 1054-1060 ◽  
Author(s):  
Mohan Kumar Harikrishna Kumar ◽  
Subramaniam Shankar ◽  
Rathanasamy Rajasekar ◽  
Pal Samir Kumar ◽  
Palaniappan Sathish Kumar

2020 ◽  
Vol 64 (3) ◽  
Author(s):  
Eva Jennische ◽  
Stefan Lange ◽  
Ragnar Hultborn

A simple dark field microscopy technique was used for visualization of blood vessels in normal human renal tissues and carcinoma. Phase contrast condenser ring apt for high power objectives was combined with a 10x objective in order to create a dark field illumination of the specimens examined. The endothelial lining of the vessels had been stained by using CD31 monoclonal antibodies combined with conventional peroxidase immunohistochemistry. The final DAB addition used for this technique induced an intense light scatter in the dark field microscope. This scattered light originating from the endothelial lining made the walls of the bright vessels easily detectable from the dark background.


2020 ◽  
Vol 39 (1) ◽  
pp. 81-90
Author(s):  
An Zhao ◽  
Xuan-Yu Shi ◽  
Shi-Hao Sun ◽  
Hai-Mo Zhang ◽  
Min Zuo ◽  
...  

2009 ◽  
Vol 26 (6) ◽  
pp. 068701 ◽  
Author(s):  
Zhou Jin-Hua ◽  
Tao Run-Zhe ◽  
Hu Zhi-Bin ◽  
Zhong Min-Cheng ◽  
Wang Zi-Qiang ◽  
...  

1979 ◽  
Vol 52 (2) ◽  
pp. 294-303 ◽  
Author(s):  
R. Caspary ◽  
P. Kretschmer

Abstract The dependence of the Index of Elasticity, E, the reciprocal value of sound velocity, on temperature and pressure is related to specific volume and compressibility of rubbers. The sensitivity of E towards changes of temperature and pressure was calculated, indicating a new versatile possibility for the control of rubber extruders. To confirm this, extruder experiments were carried out with an SHR compound, of which a working diagram was established showing the complete behavior of E=f(p,T). The effect of compound composition, especially of plasticizer and carbon black content, was examined. Viscosity in the extruder primarily determines changes in E. The method was shown to be applicable up to a die diameter of at least 200 mm. The method may also be applied to follow degradation of rubber compounds during mastication.


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