Atomic force microscopy based quantitative mapping of elastic moduli in phase separated polyurethanes and silica reinforced rubbers across the length scales

2011 ◽  
Vol 1318 ◽  
Author(s):  
Peter Schön ◽  
Kristóf Bagdi ◽  
Kinga Molnár ◽  
Patrick Markus ◽  
Saurabh Dutta ◽  
...  

ABSTRACTIn the work presented here atomic force microscopy (AFM) based mechanical mapping techniques - HarmoniX imaging and Peak Force Tapping - were applied to determine the surface elastic modulus of phase separated polyurethanes and silica reinforced rubbers across the length scales. Segmented polyether polyurethanes (PUs) were prepared with varying stoichiometric ratio of the isocyanate and hydroxyl groups. The effect of molar mass, as well as the type and number of end-groups on their morphology was investigated. Smooth PU samples for AFM imaging were prepared by ultramicrotonomy. The micro phase separated morphology of the phase separated PUs showed characteristic “fingerprint” AFM phase images. Surface modulus values obtained by AFM were compared to bulk modulus values obtained by tensile testing. The moduli were mapped quantitatively with nanoscale resolution and were in excellent agreement for both AFM modes. Surface mean moduli values do not coincide with bulk values obtained via tensile testing which is attributed to fundamentally different averaging procedures and effects that lead to the respective modulus values obtained via surface and volume averaging. EPDM and SBR rubbers and rubber blends thereof were prepared with varying concentrations of silica nanoparticles and studied in order to investigate the effect of different composition on the resulting morphology (filler distribution) and elastic moduli on a specific rubber or rubber blend sample. Elastic moduli of the rubber and rubber blend samples were first measured by bulk tensile testing. The morphology of the rubber samples was visualized by height and phase imaging. Surface elastic moduli of silica reinforced rubbers and rubber blends were mapped quantitatively and compared with bulk tensile test results. AFM allowed the determination of modulus distributions at the sections imaged. As potential reasons for the observed differences between bulk and surface modulus different averaging procedures like surface and bulk averaging of AFM vs. tensile testing, different filler distributions in SBR and EPDM and the AFM modulus calibration procedures can be named.

2004 ◽  
Vol 19 (3) ◽  
pp. 716-728 ◽  
Author(s):  
A. Kovalev ◽  
H. Shulha ◽  
M. Lemieux ◽  
N. Myshkin ◽  
V.V. Tsukruk

The approach developed for the microindentation of layered elastic solids was adapted to analyze atomic force microscopy probing of ultrathin (1–100 nm-thick) polymer films on a solid substrate. The model for analyzing microindentation of layered solids was extended to construct two- and tri-step graded functions with the transition zones accounting for a variable gradient between layers. This “graded” approach offered a transparent consideration of the gradient of the mechanical properties between layers. Several examples of recent applications of this model to nanoscale polymer layers were presented. We considered polymer layers with elastic moduli ranging from 0.05 to 3000 MPa with different architecture in a dry state and in a solvated state. The most sophisticated case of a tri-layered polymer film with thickness of 20–50 nm was also successfully treated within this approach. In all cases, a complex shape of corresponding loading curves and elastic modulus depth profiles obtained from experimental data were fitted by the graded functions with nanomechanical parameters (elastic moduli and transition zone widths) close to independently determined microstructural parameters (thickness and composition of layers) of the layered materials.


2008 ◽  
Vol 20 (3) ◽  
pp. 035706 ◽  
Author(s):  
G Stan ◽  
C V Ciobanu ◽  
T P Thayer ◽  
G T Wang ◽  
J R Creighton ◽  
...  

2019 ◽  
Vol 36 (3) ◽  
pp. 196-242
Author(s):  
Abitha Vayyaprontavida Kaliyathan ◽  
KM Varghese ◽  
A Sreekumaran Nair ◽  
Sabu Thomas

The blending of different rubbers is one of the effective methods to achieve required performance properties in their final products. This article reviews the thermodynamic considerations of rubber–rubber blends and their filled systems. Factors affecting the rubber blend morphology (i.e. distribution mechanism of fillers, curatives and other compounding ingredients) and preparation techniques for rubber–rubber blends emphasizing their advantages and disadvantages are well discussed in this review. Microscopy is the field of interest to all material scientists. In the case of rubber blends, microscopy is an essential tool in order to understand the morphology, that is, size, shape and distribution of phases and filler particles in the rubber–rubber blend. In this review, selected scientific reports based on optical microscopy, electron microscopy and atomic force microscopy in rubber–rubber blends are discussed. Rubber material is a complex macromolecule; it has significant proportion of fillers, processing aids and curing agents; therefore, only a very few studies have been reported on the microscopic aspects of filled rubber–rubber blends. In particular, influence of rubber blend composition, fillers (micro and nano length scales) and processing additives on the morphology of rubber blends systems has not been systematically reviewed and discussed in the scientific literature. Therefore, in the present scenario, this review was thought of, which deals with the essential background to rubber–rubber blends, miscibility and morphological characterization of various rubber blend systems by microscopy. It is very important to add that although there is scattered information on these aspects in the scientific literature, to date a comprehensive review has not been published. The pros, cons, artefacts and the new challenges on the use of microscopy for the characterization of rubber–rubber blends are also discussed here.


2012 ◽  
Vol 23 (32) ◽  
pp. 325703 ◽  
Author(s):  
F Federici Canova ◽  
A S Foster ◽  
M K Rasmussen ◽  
K Meinander ◽  
F Besenbacher ◽  
...  

2006 ◽  
Vol 1 (2) ◽  
pp. 137-141 ◽  
Author(s):  
Paul A. Wiggins ◽  
Thijn van der Heijden ◽  
Fernando Moreno-Herrero ◽  
Andrew Spakowitz ◽  
Rob Phillips ◽  
...  

MRS Advances ◽  
2018 ◽  
Vol 3 (44) ◽  
pp. 2719-2724
Author(s):  
D.L.P. Lacerda ◽  
F. Ptak ◽  
R. Prioli

AbstractAtomic force microscopy (AFM) and nanoindentation were used to characterize poly (methyl methacrylate) (PMMA) films with a wide distribution of pores. Pores with diameters ranging from tens of nanometers to few micrometers were measured by AFM and cross-section scanning electron microscopy (SEM). Atomic force acoustic microscopy (AFAM) mapping of the elastic modulus were correlated with the samples topography and pore distribution. The elastic moduli of the samples were additionally measured by nanoindentation.


2003 ◽  
Vol 424 (2) ◽  
pp. 267-273 ◽  
Author(s):  
P.O. Renault ◽  
P. Villain ◽  
C. Coupeau ◽  
P. Goudeau ◽  
K.F. Badawi

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