Quantitative study of filled rubber microstructure by optical and atomic force microscopy

Abstract

a b s t r a c tA comprehensive approach is proposed for studying the microstructure of filled rubbers by optical and atomic force microscopy (AFM). The optical results are found to be dependent on the illumination angle. Algorithms based on the mathematical morphology are developed for the processing of optical images (removing scratches, identifying agglomerates). AFM-images are treated by a segmentation method which separates a continuous surface into segments that match filler. Parameters of secondary filler structures and the size of an area of homogeneous filler dispersion are obtained from the analysis of the segmented images. Seven carbon black filled rubbers with different mixing times are investigated. The combination of AFM with optical imaging techniques makes it possible to perform a quantitative structural analysis at scales from tens of nanometers to tens of microns, and to establish the relationship between the mixing time and the filler microstructure over the whole range of filler peculiarities.

Rapid formation of carbon nanotubes–natural rubber films cured with glutaraldehyde for reducing percolation threshold concentration

“…To examine the dispersion of CNT in NR matrix, disperse grader testing were performed according to ASTM D 7723 by using Alphaview Dispergrader (Alpha Technologies, USA) incorporated with ShuttleXpress software to analyze %dispersion of the composite. According to the standard [ 18 ], illumination was at 30º to the sample surface.…”

In Situ Nanostress Visualization Method to Reveal the Micromechanical Mechanism of Nanocomposites by Atomic Force Microscopy

“…Over the past decade, advanced characterization tools and instru- ments have brought extensive new information to help us better understand the filler reinforcement process. 16−18 In particular, high-resolution microscopic imaging techniques have made it possible to visualize materials at the nanoscale, such as atomic force microscopy (AFM), 19,20 scanning electron microscopy, 21,22 and transmission electron microscopy. 23−25 Among them, AFM not only provides nanoscale morphological information about material surfaces but also visualizes nanomechanical properties; thus, it is widely used for researching rubber.…”

“…Polymer nanocomposites (PNCs) are widely used for reinforcing and modifying polymers to meet the present demands for superior material performance and low carbon emissions. − Nanoparticle-filled rubber is a typical PNC with substantially better mechanical properties than those of original rubbers. − The most prevalent filler type in the rubber industry is carbon black (CB), which has been used for over 100 years to improve the elastic modulus, fracture strength, and wear resistance of rubber in a simple and significant manner. , Over the past few decades, the use of silica in tire rubber has attracted considerable attention, , while nanofillers with special geometries, such as carbon nanotubes and graphene, have also been extensively studied. − Although various nanofillers have been applied to rubber, it is still crucial to understand the mechanisms of CB-filled rubber to improve and design other types of PNCs. Over the past decade, advanced characterization tools and instruments have brought extensive new information to help us better understand the filler reinforcement process. − In particular, high-resolution microscopic imaging techniques have made it possible to visualize materials at the nanoscale, such as atomic force microscopy (AFM), , scanning electron microscopy, , and transmission electron microscopy. − Among them, AFM not only provides nanoscale morphological information about material surfaces but also visualizes nanomechanical properties; thus, it is widely used for researching rubber. , AFM can evaluate the thickness of the bound rubber layer between the filler and the rubber and investigate the effects of fillers on the physical properties of rubber matrices through nanoelastic modulus mappings. , In addition, a nanorheological AFM technique provides a new approach for studying the viscoelastic behaviors of rubber samples by measuring the nanoscale storage and loss moduli through the contact oscillation of a probe on the material surface …”

Acid surface modified carbon nanotube-filled fluoroelastomers aging test in oil-based drilling fluids

“…6 Many researchers have investigated the surface of CNT-filled and nanofiller-filled rubber using AFM. The parameters they studied included topography, 7 the degree of dispersion [8][9][10] and interaction of nanofiller and rubber, and interphase region between nanofiller and rubber matrix. [11][12][13][14] Oxidized CNT compared to unmodified CNT can change these parameters, particularly the interacting layer over the nanoparticles (bound rubber), and therefore can change the properties of nanocomposite rubber such as resistance to chemicals.…”