SEM study of worn surface morphology of an indigenous ‘EPDM’ rubber

Ethylene Propylene Diene Monomer (EPDM) rubber emerges as a dominant elastomer for major engineering applications like automobiles, constructions, electric and electronic industries and many more. The major engineering properties of EPDM are its outstanding heat, ozone and weather resistance ability. The resistance to polar substances and steam is also good. EPDM rubber has a common use as seals in automobiles.In the present work friction and sliding wear behaviors of ethylene propylene diene monomer rubbers (EPDM) of different hardness have been studied against steel counterpart under dry working condition. Different hardness of EPDM have been achieved by adding different proportion (parts per hundred) of carbon black (CB) content with the main ingredients of EPDM. Tribo-testing has been carried out in a multi tribo-tester (Ducom, India). EPDM rubber of different hardness like 55 Å, 70 Å and 85 Å has been slid against EN-8 stainless steel roller of the tester. Experiments have been conducted with different rotational speeds of the wheel at a constant load of 25N for a constant duration of 900 s. The coefficient of friction (COF), mass loss and wear of EPDM rubbers have been determined from the test data. The worn surface morphology has also been studied using scanning electron microscope (SEM) and concluded accordingly.Present experimental work attempts to highlight some important tribo-characteristics of an indigenous EPDM rubber as well as to shed light on various possible areas of further research works.     

Morphology development and phase inversion during dynamic vulcanisation of EPDM/PP blends

Morphology development and phase inversion were investigated during dynamic vulcanisation of ethylene–propylene–diene terpolymer (EPDM)/polypropylene (PP) blends. The effects of viscosity ratio and cross-linking reactions were also addressed. EPDM/PP blends were dynamically vulcanised in a Haake batch mixer using resole and SnCl₂ as cross-linking agents. The morphology development and cross-linking degree with reaction time were followed by morphology analysis (SEM and TEM) and measurement of EPDM gel content, respectively. For the same reaction time, it was found that the EPDM gel content decreased when the low-molecular-weight EPDM was used. As a result, the morphological development was delayed and the phase-inversion point was shifted to higher reaction times, allowing us to monitor morphological development during a thermoplastic vulcanisate (TPV) preparation. Using the low-molecular-weight EPDM and increasing the PP viscosity accelerated the morphological development, shifting phase-inversion to lower reaction times. While blend composition influenced final TPV morphology, it had a minor effect on the mechanism of morphological development. A correlation between cross-linking degree and morphology development was established. The results obtained allowed to propose a mechanism of morphology development during dynamic vulcanisation of the EPDM/PP blends, including phase inversion.     

Synergistic effects of cerium phosphate and intumescent flame retardant on EPDM/PP composites

An intumescent flame retardant system composed of ammonium polyphosphate (APP) and pentaerythritol (PER) was used for flame retarding ethylene–propylene–diene‐modified elastomer (EPDM)/polypropylene (PP) blends. Cerium phosphate (CeP) was synthesized and the effect on flame retardancy and thermal stability of EPDM/PP composites based on intumescent flame retardant (IFR) were studied by limiting oxygen index (LOI), UL‐94, and thermogravimetic analysis (TGA), respectively. Scanning electron microscopy (SEM) and Fourier transform infrared spectrometry (FTIR) were used to analyze the morphological structure and the component of the residue chars formed from the EPDM/PP composites, and the mechanical properties of the materials were also studied. The addition of CeP to the EPDM/PP/APP/PER composites gives better flame retardancy than that of EPDM/PP/APP/PER composites. TGA and RT‐FTIR studies indicated that an interaction occurs among APP, PER, and EPDM/PP. The incorporation of CeP improved the mechanical properties of the materials. Copyright © 2010 John Wiley & Sons, Ltd.     

Morphology development in thermoplastic vulcanizates (TPV): Dispersion mechanisms of a pre-crosslinked EPDM phase

The fragmentation and dispersion in molten polypropylene (PP) of several pre-crosslinked and plasticized ethylene–propylene–diene terpolymer (EPDM) networks was studied. Thus, the morphologies and mechanical properties of PP/EPDM blends having similar compositions but made from either un-crosslinked, pre-crosslinked or dynamic-crosslinked EPDMs were compared. The results first highlight the importance of the gel fraction of the pre-crosslinked EPDMs, as well as the impact of the thermoplastic matrix proportion on the quality of the dispersion of such networks. As a result, pre-crosslinked EPDM having a gel fraction below g_EPDM = 0.7 can be finely and homogeneously fragmented and dispersed in presence of PP. It can be then admitted a collision–coalescence–separation type erosion mechanism of the EPDM domains. Nevertheless, contrarily to some theoretical model expectations, a partial fragmentation of the chemical networks was always observed even at very high crosslink density (g_EPDM > 0.7). Finally, the blends crosslinked under shearing (dynamic-crosslinked) showed a clear mechanical property synergy due to their fine and homogeneous morphology coupled with the full crosslinking of the elastomer. In the end, these results brought significant information on TPV morphology stabilization and their related mechanical properties.     

Chemical and mechanical stability of EPDM in a PEM fuel cell environment

Proton exchange membrane (PEM) fuel cell stack requires elastomeric gaskets in each cell to keep the reactant gases within their respective regions. Long-term durability of the fuel cell stacks depends heavily on the functionality of the elastomeric gasket material. Chemical and mechanical stability of the elastomeric material is of great concern to the overall performance of the fuel cell stacks. The degradation of a commercially available gasket material, ethylene-propylene-diene monomer (EPDM), was investigated in a simulated PEM fuel cell environment in this work. One solution and two temperatures, based on actual fuel cell operation, were used in this study. Optical microscopy was used to show the topographical changes on the sample surface. Attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy was employed to study the surface chemistry of the gasket material before and after exposure to the simulated PEM fuel cell environment over time. Atomic absorption spectrometry was used to identify the leachants in the soaking solution from the elastomeric material. Microindentation test and dynamic mechanical analysis (DMA) were conducted to assess the change of mechanical properties of the samples exposed to the environment. The atomic absorption spectrometer analysis shows that silicon and calcium were leached from the material into the soaking solution. The ATR-FTIR results indicate that the chemical changes were not apparent. The microindentation test and DMA results reveal that mechanical properties were not changed significantly.     

On the Development of Titanium κ1-Amidinate Complexes,Commercialized as Keltan ACE™ Technology,Enabling the Production of an Unprecedented Large Variety of EPDM Polymer Structures

ARLANXEO Elastomers has developed and commercialized Keltan ACE™ technology, a class of half-sandwich cyclopentadienyl κ¹-amidinate metal complexes, which are extremely active for the production of first-class ethylene/propylene/diene copolymers (EPDM). In this review, the development and some of the key features of the Keltan ACE™ catalyst system are presented. Many different ACE catalysts have been synthesized over the past years, including bridged and bimetallic catalysts. With Keltan ACE™, a complete range of EPDM products with similar polymer characteristics as their Ziegler–Natta (ZN) counterparts can be produced, including variations containing very high 5-ethylidene-2-norbornene (ENB) contents, controlled long chain branching, very high molecular weight, as well as oil-extended products. Moreover, other EPDM structures can be polymerized. The Keltan ACE™ catalyst technology also allows the production of EPDMs with very high amounts of dicyclopentadiene (DCPD) or 5-vinyl 2-norbornene (VNB) without excessive gelation and reactor fouling, that is, products that cannot or are extremely difficult to obtain via classical ZN catalysis. In a next step, high-VNB-EPDM can be postreactor modified, for example, via metathesis chemistry. In addition, EPDM polymers with a very broad or even bimodal molecular weight distribution can be obtained in a single reactor with certain ACE catalyst structures at particular activator/precatalyst ratios. © 2017 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017 , 55, 2877–2891     

Ductile–brittle‐transition phenomenon in polypropylene/ethylene‐propylene‐diene rubber blends obtained by dynamic packing injection molding: A new understanding of the rubber‐toughening mechanism

For a more complete understanding of the toughening mechanism of polypropylene (PP)/ethylene‐propylene‐diene rubber (EPDM) blends, dynamic packing injection molding was used to control the phase morphology and rubber particle orientation in the matrix. The relative impact strength of the blends increased at low EPDM contents, and then a definite ductile–brittle (D–B) transition was observed when the EPDM content reached 25 wt %, at which point blends should fail in the ductile mode with conventional molding. Wide‐angle X‐ray diffraction (WAXD), differential scanning calorimetry (DSC), and scanning electron microscopy (SEM) were used to investigate the shear‐induced crystal structure, morphology, orientation, and phase separation of the blends. WAXD results showed that the observed D–B transition took place mainly for a constant crystal structure (α form). Also, no remarkable changes in the crystallinity and melting point of PP were observed by DSC. The highly oriented and elongated rubber particles were seen via SEM at high EPDM contents. Our results suggest that Wu's criterion is no longer valid when dispersed rubber particles are elongated and oriented. The possible fracture mechanism is discussed on the basis of the stress concentration in a filler‐dispersed matrix. It can be concluded that not only the interparticle distance but also the stress fields around individual particles play an important role in polymer toughening. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 2086–2097, 2002     

Mechanical,Thermal, and Rheological Properties of EPDM-graft-methyl Methacrylate and Styrene (EPDM-g-MS)/Methyl Methacrylate-Styrene Copolymer (MS Resin) Blends

EPDM-graft-methyl methacrylate and styrene (EPDM-g-MS) were synthesized by solution graft copolymerization of methyl methacrylate (MMA) and styrene (St) onto ethylene-propylene-diene terpolymer (EPDM). EPDM-g-MS/MS resin blends (MES) tht were prepared by melt blending EPDM-g-MS and methyl methacrylate-styrene copolymer (MS resin). The mechanical properties, compatibility, thermal stabilities and rheological properties of MES were studied by the pendulum impact tester and the tension tester, differential scanning calorimetric (DSC), thermogravimetry analysis (TGA), and the capillary rheometry, respectively. The results showed that EPDM-g-MS had an excellent toughening effect on MS resin; the notched Izod impact strength of MES reached 20.7 kJ/m² when EPDM content in MES was 25 wt%, about 14 times that of MS resin. EPDM-g-MS and MS resin were partially compatible, and the compatibility increased with an increasing MMA/St ratio of EPDM-g-MS. MES had excellent heat-resistance, which increased as the EPDM content in MES and MMA/St ratio of EPDM-g-MS rose. MES melt flow confirmed pseudoplastic flow characteristics. The apparent viscosity (η _a ) of MES decreased with an increasing shearing rate (γ) and temperature, but increased with an increasing EPDM content in MES and MMA/St ratio of EPDM-g-MS. The flow activation energy of MES was lower than that of MS resin.     

Olefin terpolymerizations. II. 4-vinylcyclohexene and cyclooctadiene

4-Vinylcyclohexene (VCH) and cyclooctadiene (COD) were investigated as termonomers in EPDM (ethylene/propylene/diene) synthesis by using rac-ethylenebis (1-η⁵-indenyl) zir-conium dichloride ( 1 ) as a catalyst precursor. Homopolymerizations of VCH, vinylcycloh-exane and cyclohexene were compared. The parameter K_πκ_p, which is the apparent rate constant for Ziegler-Natta polymerization, is about the same for VCH and vinylcyclohexanebut is 10 times smaller for cyclohexene. Therefore, the linear olefinic double bond is more active than the cyclic internal double bond. VCH reduces ethylene polymerization rate but not propylene polymerization rate in copolymerizations. In terpolymerizations, VCH tends to suppress ethylene incorporation especially at elevated polymerization temperature and Lowers the polymer MW by about two-fold. COD has very low activity as a termonomer. © 1995 John Wiley & Sons, Inc.     

Interactions between the components in isotactic polypropylene blended with EPDM

The interaction of isotactic polypropylene with ethylene propylene diene terpolymer in their blends has been investigated by use of differential scanning calorimetry, dynamic mechanical analysis, wide- and small-angle x-ray scattering, and by investigating the nucleation and kinetics of crystallization of the iPP component under the polarization microscope. It is found, that the dispersion of the EPDM component in the iPP matrix is dependent on blend composition and is maximal at 10% EPDM content. An interface layer between the two components is formed by migration of iPP molecules into the EPDM phase. A model for this interface is proposed.