CHANGES OF CHEMICAL STRUCTURE AND MECHANICAL PROPERTY LEVELS DURING THERMO-OXIDATIVE AGING OF NBR

2013 ◽  
Vol 86 (4) ◽  
pp. 591-603 ◽  
Author(s):  
Jiaohong Zhao ◽  
Rui Yang ◽  
Rossana Iervolino ◽  
Stellario Barbera
Keyword(s):  
Mechanical Property ◽  
Thermal Aging ◽  
Chemical Structure ◽  
Structural Changes ◽  
Elevated Temperatures ◽  
Chain Scission ◽  
Bending Test ◽  
Cross Linking ◽  
Butadiene Rubber ◽  
Oxidative Aging

ABSTRACT The accelerated thermo-oxidative aging of acrylonitrile–butadiene rubber (NBR) was studied at elevated temperatures. The chemical structure characterized by attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR) and pyrolysis gas chromatography–mass spectroscopy (PGC-MS) showed the loss of low-molecular-weight additives, such as antioxidants and paraffin, and the formation of carbonyl groups and unsaturated double bonds. The cross-linking degree characterized by NMR and a swelling test showed that aging is a competitive process of cross-linking and chain scission. Cross-linking dominated the thermal aging of NBR most of the time, whereas chain scission began to increase after a long time at high temperatures. The changes of mechanical property magnitudes during thermal aging of NBR were studied by using the recovery from bending test (RFB) and tensile test. By comparing the physical property results and the structural changes, their relationship is discussed.

Mechanical Property and Oxidation Behavior of LPS-SiC Materials

2006 ◽  
Vol 321-323 ◽  
pp. 913-916
Author(s):  
Sang Ll Lee ◽  
Yun Seok Shin ◽  
Jin Kyung Lee ◽  
Jong Baek Lee ◽  
Jun Young Park
Keyword(s):  
Mechanical Property ◽  
Fracture Toughness ◽  
Oxidation Behavior ◽  
Elevated Temperatures ◽  
Indentation Test ◽  
Bending Test ◽  
Secondary Phases ◽  
Three Point Bending ◽  
Different Temperatures

The microstructure and the mechanical property of liquid phase sintered (LPS) SiC materials with oxide secondary phases have been investigated. The strength variation of LPS-SiC materials exposed at the elevated temperatures has been also examined. LPS-SiC materials were sintered at the different temperatures using two types of Al2O3/Y2O3 compositional ratio. The characterization of LPS-SiC materials was investigated by means of SEM with EDS, three point bending test and indentation test. The LPS-SiC material with a density of about 3.2 Mg/m3 represented a flexural strength of about 800 MPa and a fracture toughness of about 9.0 MPa⋅√m.

scholarly journals Scission, Cross-Linking, and Physical Relaxation during Thermal Degradation of Elastomers

Polymers ◽  
2019 ◽  
Vol 11 (8) ◽  
pp. 1280 ◽  
Author(s):  
Zaghdoudi ◽  
Kömmling ◽  
Jaunich ◽  
Wolff
Keyword(s):  
Operating Time ◽  
Thermal Exposure ◽  
Chain Scission ◽  
Cross Linking ◽  
Butadiene Rubber ◽  
Compression Set ◽  
Model Compression ◽  
Relaxation Measurements ◽  
Thermally Driven

Elastomers are susceptible to chemical ageing, i.e., scission and cross-linking, at high temperatures. This thermally driven ageing process affects their mechanical properties and leads to limited operating time. Continuous and intermittent stress relaxation measurements were conducted on ethylene propylene diene rubber (EPDM) and hydrogenated nitrile butadiene rubber (HNBR) samples for different ageing times and an ageing temperature of 125 °C. The contributions of chain scission and cross-linking were analysed for both materials at different ageing states, elucidating the respective ageing mechanisms. Furthermore, compression set experiments were performed under various test conditions. Adopting the two-network model, compression set values were calculated and compared to the measured data. The additional effect of physical processes to scission and cross-linking during a long-term thermal exposure is quantified through the compression set analysis. The characteristic times relative to the degradation processes are also determined.

Stress Relaxation during the Thermal Oxidation of Vulcanized Natural Rubber

1960 ◽  
Vol 33 (2) ◽  
pp. 423-432
Author(s):  
J. R. Dunn ◽  
J. Scanlan ◽  
W. F. Watson
Keyword(s):  
Free Radical ◽  
Stress Relaxation ◽  
Natural Rubber ◽  
Thermal Aging ◽  
Elevated Temperatures ◽  
The Other ◽  
Tetramethylthiuram Disulfide ◽  
Oxidative Aging ◽  
Relaxation Measurements ◽  
Cross Links

Abstract The photoinitiated oxidative aging of peroxide vulcanized natural rubber (which contains only carbon-carbon cross-links) was found by stress relaxation measurements to be autocatalytic and to be sensitive to the presence of free radical retarders and catalysts. Similar behavior would be expected in thermal aging. However, earlier work in these laboratories indicated that the thermal aging of peroxide vulcanizates was not autocatalytic. Because of this discrepancy the stress relaxation of peroxide vulcanizates at elevated temperatures has now been reinvestigated and the study has been extended to include also the aging of the other types of networks which are produced on vulcanization by tetramethylthiuram disulfide in the absence of sulfur, by sulfenamide-sulfur, and by sulfur alone.

Embedding Procedure for Water Swollen Samples

1970 ◽  
Vol 28 ◽  
pp. 504-505
Author(s):  
Ann M. Thomas ◽  
Virginia Shemeley
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Exchange ◽  
Structural Changes ◽  
Cross Linking ◽  
Ion Exchange Resins ◽  
Transmission Electron ◽  
First Pass ◽  
Exchange Resins

Those samples which swell rapidly when exposed to water are, at best, difficult to section for transmission electron microscopy. Some materials literally burst out of the embedding block with the first pass by the knife, and even the most rapid cutting cycle produces sections of limited value. Many ion exchange resins swell in water; some undergo irreversible structural changes when dried. We developed our embedding procedure to handle this type of sample, but it should be applicable to many materials that present similar sectioning difficulties.The purpose of our embedding procedure is to build up a cross-linking network throughout the sample, while it is in a water swollen state. Our procedure was suggested to us by the work of Rosenberg, where he mentioned the formation of a tridimensional structure by the polymerization of the GMA biproduct, triglycol dimethacrylate.

scholarly journals Best Practice for De-Vulcanization of Waste Passenger Car Tire Rubber Granulate Using 2-2′-dibenzamidodiphenyldisulfide as De-Vulcanization Agent in a Twin-Screw Extruder

Polymers ◽  
2021 ◽  
Vol 13 (7) ◽  
pp. 1139
Author(s):  
Hans van Hoek ◽  
Jacques Noordermeer ◽  
Geert Heideman ◽  
Anke Blume ◽  
Wilma Dierkes
Keyword(s):  
Best Practice ◽  
Chain Scission ◽  
Styrene Butadiene Rubber ◽  
Butadiene Rubber ◽  
Twin Screw Extruder ◽  
Screw Extruder ◽  
Passenger Car ◽  
Tire Rubber ◽  
Twin Screw ◽  
Styrene Butadiene

De-vulcanization of rubber has been shown to be a viable process to reuse this valuable material. The purpose of the de-vulcanization is to release the crosslinked nature of the highly elastic tire rubber granulate. For present day passenger car tires containing the synthetic rubbers Styrene-Butadiene Rubber (SBR) and Butadiene Rubber (BR) and a high amount of silica as reinforcing filler, producing high quality devulcanizate is a major challenge. In previous research a thermo-chemical mechanical approach was developed, using a twin-screw extruder and diphenyldisulfide (DPDS) as de-vulcanization agent.The screw configuration was designed for low shear in order to protect the polymers from chain scission, or uncontrolled spontaneuous recombination which is the largest problem involved in de-vulcanization of passenger car tire rubber. Because of disadvantages of DPDS for commercial use, 2-2′-dibenzamidodiphenyldisulfide (DBD) was used in the present study. Due to its high melting point of 140 °C the twin-screw extruder process needed to be redesigned. Subsequent milling of the devulcanizate at 60 °C with a narrow gap-width between the mill rolls greatly improved the quality of the devulcanizate in terms of coherence and tensile properties after renewed vulcanization. As the composition of passenger car tire granulate is very complex, the usefulness of the Horikx-Verbruggen analysis as optimization parameter for the de-vulcanization process was limited. Instead, stress-strain properties of re-vulcanized de-vulcanizates were used. The capacity of the twin-screw extruder was limited by the required residence time, implying a low screw speed. A best tensile strength of 8 MPa at a strain at break of 160% of the unblended renewed vulcanizate was found under optimal conditions.

EXPERIMENTAL VALIDATION OF THE CHARLESBY AND HORIKX MODELS APPLIED TO DE-VULCANIZATION OF SULFUR AND PEROXIDE VULCANIZATES OF NR AND EPDM

2016 ◽  
Vol 89 (4) ◽  
pp. 671-688 ◽  
Author(s):  
M. A. L. Verbruggen ◽  
L. van der Does ◽  
W. K. Dierkes ◽  
J. W. M. Noordermeer
Keyword(s):  
Experimental Validation ◽  
Main Chain ◽  
Sol Gel ◽  
Chain Scission ◽  
Cross Linking ◽  
Cross Link ◽  
Practical Reality ◽  
Cross Links ◽  
The Cross ◽  
Theoretical Considerations

ABSTRACT The theoretical model developed by Charlesby to quantify the balance between cross-links creation of polymers and chain scission during radiation cross-linking and further modifications by Horikx to describe network breakdown from aging were merged to characterize the balance of both types of scission on the development of the sol content during de-vulcanization of rubber networks. There are, however, disturbing factors in these theoretical considerations vis-à-vis practical reality. Sulfur- and peroxide-cured NR and EPDM vulcanizates were de-vulcanized under conditions of selective cross-link and random main-chain scissions. Cross-link scission was obtained using thiol-amine reagents for selective cleavage of sulfur cross-links. Random main-chain scission was achieved by heating peroxide vulcanizates of NR with diphenyldisulfide, a method commonly employed for NR reclaiming. An important factor in the analyses of these experiments is the cross-linking index. Its value must be calculated using the sol fraction of the cross-linked network before de-vulcanization to obtain reliable results. The values for the cross-linking index calculated with sol-gel data before de-vulcanization appear to fit the experimentally determined modes of network scission during de-vulcanization very well. This study confirms that the treatment of de-vulcanization data with the merged Charlesby and Horikx models can be used satisfactorily to characterize the de-vulcanization of NR and EPDM vulcanizates.

Tensile Behavior after Oxidative Aging of Gum and Black-Filled Vulcanizates of SBR and NR

1999 ◽  
Vol 72 (4) ◽  
pp. 721-730 ◽  
Author(s):  
G. R. Hamed ◽  
J. Zhao
Keyword(s):  
Tensile Strength ◽  
Natural Rubber ◽  
Tensile Behavior ◽  
Styrene Butadiene Rubber ◽  
Butadiene Rubber ◽  
Oxidative Aging ◽  
Prolonged Aging ◽  
Aging Period ◽  
Early Aging ◽  
Styrene Butadiene

Abstract Typical sulfur-cured vulcanizates of styrene-butadiene rubber (SBR) and natural rubber (NR) were prepared, and subjected to air-oven aging at 100 °C. Gum specimens exhibited an initial aging period in which stiffness was unchanged, while tensile strength and strain-to-break were significantly reduced. In contrast, black-filled vulcanizates stiffened during early aging. After intermediate aging times, NR specimens softened, while SBR stiffened. With prolonged aging, all compositions became hard and inextensible.

scholarly journals Membrane-Based Separation of Phenol/Water Mixtures Using Ionically and Covalently Cross-Linked Ethylene-Methacrylic Acid Copolymers

2008 ◽  
Vol 2008 ◽  
pp. 1-12 ◽  
Author(s):  
Alexander Mixa ◽  
Claudia Staudt
Keyword(s):  
Methacrylic Acid ◽  
Elevated Temperatures ◽  
Type Equation ◽  
Enrichment Factors ◽  
Cross Linking ◽  
Temperature Dependent ◽  
Monomer Content ◽  
Phenol Water ◽  
Feed Temperature ◽  
Acetyl Acetonate

Membrane-based separation of phenol/water mixtures with concentrations of phenol between 3 wt% and 8 wt% in the feed has been performed with nonmodified as well as cross-linked ethylene-methacrylic acid (E-MAA) copolymers with different amounts of methacrylic acid. As cross-linking agents, aluminium acetyl acetonate, which leads to ionically cross-linked membranes, and 2,3,5,6-tetramethyl-1,4-phenylene diamine and glycerine digycidether, leading to covalently cross-linked membranes, have been used. Generally, it was found that with increasing phenol content in the feed, the total flux is increasing whereas the enrichment factor is decreasing. Using nonmodified membranes with higher methacrylic acid monomer content in the polymer, lower fluxes and higher enrichment factors were observed. Investigation of different cross-linked membranes showed that with high phenol concentration in the feed, ionic cross-linking seems to be very promising. Furthermore, variation of feed temperature shows that ionically cross-linked membranes reached higher fluxes as well as higher enrichment factors at elevated temperatures. The temperature-dependent data were fitted based on an Arrhenius-type equation, and activation energies for the permeation of phenol and water through the membrane were calculated.

Comparative study of thermoplastic liner materials with regard to mechanical and permeation barrier properties before and after cyclic thermal aging

2021 ◽  
Vol 63 (4) ◽  
pp. 311-316
Author(s):  
Simon Backens ◽  
Jan Siering ◽  
Stefan Schmidt ◽  
Nikolai Glück ◽  
Wilko Flügge
Keyword(s):  
Thermal Aging ◽  
Barrier Properties ◽  
Tensile Tests ◽  
Polyamide 6 ◽  
Pressure Vessels ◽  
Cross Linking ◽  
Polyamide 12 ◽  
Type Iv ◽  
Before And After ◽  
Permeation Properties

Abstract Lightweight pressure vessels of type IV for hydrogen storage consist of a thermoplastic inner liner, commonly from polyethylene or polyamide. The liner is the permeation barrier against the compressed gas and must prevent the formation of cracks, also after temperature changes, for example after refueling processes. In the present work high-density polyethylene, cross-linked polyethylene, polyamide 6 and polyamide 12 were characterized by tensile tests, single notch impact tests and permeations measurements before and after a cyclic thermal aging process. The aging only lead to slight changes of mechanical properties due to post-crystallization, but to a significant decrease of permeation properties. This decrease was contributed to weakened, amorphous regions where chain splitting occurred. Considerable differences in properties resulted from different peroxide cross-linking times of polyethylene at the same temperature. A longer holding time at 200 °C led to an improvement in impact strength by a factor of more than three. However, the permeation properties decreased by about 50 %, indicating that peroxide cross-linking in the melt inhibited the formation of crystalline regions.

Bending and flexural-buckling strength of steel members considering strain-rate-effects at elevated temperatures

2021 ◽  
Vol ahead-of-print (ahead-of-print) ◽  
Author(s):  
Fuminobu Ozaki ◽  
Takumi Umemura
Keyword(s):  
Strain Rate ◽  
Elevated Temperatures ◽  
Bending Strength ◽  
Transient State ◽  
Bending Test ◽  
Content Type ◽  
Buckling Strength ◽  
Flexural Buckling ◽  
Steel Members ◽  
Collapse Temperature

PurposeIn this study, the bending strength, flexural buckling strength and collapse temperature of small steel specimens with rectangular cross-sections were examined by steady and transient state tests with various heating and deformation rates.Design/methodology/approachThe engineering stress and strain relationships for Japan industrial standard (JIS) SN400 B mild steels at elevated temperatures were obtained by coupon tests under three strain rates. A bending test using a simple supported small beam specimen was conducted to examine the effects of the deformation rates on the centre deflection under steady-state conditions and the heating rates under transient state conditions. Flexural buckling tests using the same cross-section specimen as that used in the bending test were conducted under steady-state and transient-state conditions.FindingsIt was clarified that the bending strength and collapse temperature are evaluated by the full plastic moment using the effective strength when the strain is equal to 0.01 or 0.02 under fast strain rates (0.03 and 0.07 min–1). In contrast, the flexural buckling strength and collapse temperature are approximately evaluated by the buckling strength using the 0.002 offset yield strength under a slow strain rate (0.003 min–1).Originality/valueRegarding both bending and flexural buckling strengths and collapse temperatures of steel members subjected to fire, the relationships among effects of steel strain rate for coupon test results, heating and deformation rates for the heated steel members were minutely investigated by the steady and transient-state tests at elevated temperatures.

Sign in / Sign up

Export Citation Format

Share Document