Bertrand Huneau

STRAIN-INDUCED CRYSTALLIZATION OF NATURAL RUBBER: A REVIEW OF X-RAY DIFFRACTION INVESTIGATIONS

Abstract Strain-induced crystallization of natural rubber was discovered in 1925 by the means of x-ray diffraction and has been widely investigated by this technique until today. The studies devoted to the structure of the crystalline phase of natural rubber are first reviewed. This structure is strongly anisotropic and can be related to the exceptionally good strength and fatigue properties of this material. The relationships between strain-induced crystallization of natural rubber and its mechanical response, during static or tension-retraction tests, are also reviewed and discussed; in particular, the hysteresis of the stress-strain curve is mainly explained by strain-induced crystallization. The kinetics of crystallization under both static and cyclic deformation is also discussed, as well as the influence of different factors, depending either on material composition (crosslink density, carbon black fillers) or on external parameters (temperature, strain rate…).

Precipitate stability and recrystallisation in the weld nuggets of friction stir welded Al–Mg–Si and Al–Mg–Sc alloys

Abstract Two different precipitate hardening aluminium alloys processed by friction stir welding were investigated. The microstructure and the hardness of the as delivered materials were compared to that of the weld nugget. Transmission electron microscopy observations combined with three-dimensional atom probe analyses clearly show that β’’ precipitates dissolved in the nugget of the Al-Mg-Si giving rise to some supersaturated solid solution. It is shown that the dramatic softening of the weld could be partly recovered by post-welding ageing treatments. In the Al-Mg-Sc alloy, Al 3 Sc precipitate size and density are unchanged in the nugget comparing to the base metal. These precipitates strongly reduce the boundary mobility of recrystallised grains, leading to a grain size in the nugget much smaller than in the Al-Mg-Si alloy. Both coherent and incoherent precipitates were detected. This feature may indicate that a combination of continuous and discontinuous recrystallisation occurred in the weld nugget.

Friction stir diffusion bonding of dissimilar metals

Abstract This paper reports on a new method based on the friction stir welding process to join dissimilar metals in butt joint configuration. Two different systems were considered: AA1050 H16 aluminium/ASTM A284 steel and AA1050 H16/UNS C12200 H01 copper. The unthreaded steel tool pin was positioned in the aluminium plate so that it was tangential to the opposing metal. Bonding was accompanied by interfacial chemical reactions with no significant mechanical mixing. This new solid state welding process is called friction stir diffusion bonding. Room temperature cross-weld tensile strengths up to 82 MPa were obtained for both metal combinations. Microstructure characterisation suggested that higher joint strengths were associated with thinner, <1 μm thick intermetallic reaction layers at joint interfaces.

In situ synchrotron wide-angle X-ray diffraction investigation of fatigue cracks in natural rubber.

Natural rubber exhibits remarkable mechanical fatigue properties usually attributed to strain-induced crystallization. To investigate this phenomenon, an original experimental set-up that couples synchrotron radiation with a homemade fatigue machine has been developed. Diffraction-pattern recording is synchronized with cyclic loading in order to obtain spatial distributions of crystallinity in the sample at prescribed times of the mechanical cycles. Then, real-time measurement of crystallinity is permitted during uninterrupted fatigue experiments. First results demonstrate the relevance of the method: the set-up is successfully used to measure the crystallinity distribution around a fatigue crack tip in a carbon black filled natural rubber for different loading conditions.

Effect of Laser Assistance Machining on Residual Stress and Fatigue Strength for a Bearing Steel (100Cr6) and a Titanium Alloy (Ti 6Al 4V)

The use of Laser Assisted Machining (LAM) can improve different aspects of the machinability of high strength materials. A study was undertaken to determine the optimum cutting parameters and to quantify their influence on fatigue strength according to the type of microstructure created. Two different materials were studied: a bearing steel (100Cr6 / AISI 52100) and an aeronautical titanium alloy (Ti6Al4V). In the bearing steel a significant increase of the fatigue resistance was observed due to the transformation of the surface layer into martensite. For the titanium alloy, a slight reduction in the fatigue strength was found as in this case the microstructure and residual stress state of the surface layer was less beneficial. The surface roughness has also been measured and no significant variation has been observed for different laser powers in each material.

Failure analysis of carbon black filled styrene butadiene rubber under fatigue loading conditions

Abstract The present paper deals with the fatigue crack growth in a carbon black-filled styrene butadiene rubber (CB-SBR) under fully relaxing loading conditions. More precisely, it is devoted to the determination of the scenario of crack growth. For that purpose, an original ‘microcutting’ technique, previously applied by the authors on natural rubber (NR), is used to observe microscopic phenomena involved in fatigue crack growth thanks to scanning electron microscopy (SEM). Results show that the crack tip grows following a tearing line by generating ligaments; it explains the differences between fatigue responses of crystallisable and non-crystallisable rubbers during crack propagation. So, contrary to crystallisable elastomers such as NR, the microstructure of SBR is similar at crack tip and in the bulk material, and the crack tip does not resist crack propagation. Moreover, the morphology of fracture surfaces only depends on particles encountered by the fatigue crack during its propagation.

In situ synchrotron X-ray diffraction study of strain induced crystallisation of natural rubber during fatigue tests

Abstract A homemade stretching machine has been developed to perform fatigue tests on natural rubber in the synchrotron facility Soleil. Strain induced crystallisation is investigated by wide angle X-ray diffraction during in situ fatigue tests of different minimum and maximum strain levels. The index of crystallinity χ decreases with the number of cycles when the minimum strain level reached during the fatigue test is lower than the critical stretch ratio for melting λM. On the contrary, when the stretch ratio is maintained higher than the critical stretch ratios for melting λM and crystallisation λC, χ increases with the number of cycles. The size of the crystallites has the same evolution during fatigue testing as χ. On the contrary, the misorientation of the crystallites does not depend on the minimum strain level reached and decreases with the number of cycles for all the fatigue tests.