Mechanical spectroscopy of interface stress relaxation in magnesium matrix composites

Magnesium matrix composites made of pure (99.98%) magnesium reinforced with long carbon (Mg/C) and stainless steel (Mg/steel) fibers were processed by low pressure infiltration method. Mg/C composites were then oriented from the crystallographic point of view by Bridgman technique and finally three composites were obtained with γ = 0°, 45° and 90° (γ is the angle between the matrix-fiber interface and the normal to the basal plane). The results show that the damping level in the composite for γ = 0° is almost 3 and 7 times higher than that of the composites with γ = 45° and γ = 90°, respectively. From the result analysis it was possible to conclude that the damping originates in the hysteretic motion of dislocations in the magnesium matrix. As such a mechanism is not thermally activated, high damping is observed over a broad frequency range. The complete evolution of the mechanical loss as a function of the vibration amplitude has been measured. The obtained result has been found to be in excellent agreement with the Granato-Lücke model for dislocation breakaway. The fit of the experimental points with the theoretical curve and the straight Granato-Lücke plot confirm that the microstructure evolution is controlled by the breakaway of dislocation segments from randomly segregated point defects (hysteretic damping). According to the Granato-Lücke model the critical stress for the breakaway could be estimated. As a consequence of this analysis, the transient damping due to interface thermal stress relaxation has been interpreted by a model based on a solid friction mechanism. It has been shown that the model of Mayencourt and Schaller justifies the whole mechanical loss behavior. The model predicts two fit parameters C1 and C2, which account for the respective evolution of the mobile dislocation density and interfacial strength. An anomalous behavior is observed for the parameter C2 as well upon heating as upon cooling, which is being reflected in the shear modulus evolution. This anomalous behavior is due to a "bonding-debonding" mechanism at the fiber-matrix interface due to the motion of dislocations, which depends on the orientation of the glide plane. Also, at high temperature, the interface is strong, which helps in creep resistance of the composite, and at low temperature, the interface is weak, which is positive for improving toughness by interface crack deflection.

High Temperature Behavior of Nano-Structured Ceramic Composites Studied by Mechanical Spectroscopy

Mehdi Mazaheri

Silicon nitride based ceramics (SiAlONs); tetragonal polycrystalline zirconia (3Y‐TZP); alumina and their composites reinforced with different amount of multi‐ walled carbon‐nanotubes (CNTs) have been processed by Spark Plasma Sintering (SPS). High temperature mechanical spectroscopy measurements were performed in each material between room temperature and 1600 K. In each of these materials, anelastic and viscoplastic relaxation phenomena were investigated and responsible mechanisms were explained. In particular, grain boundary (GB) sliding, which is responsible for high temperature plasticity in fine grained ceramics, gives rise to a peak or an exponential increase in the high temperature mechanical loss. Peak and exponential background depend on two forces, which control the GB sliding: a friction force due to the GB viscosity and a restoring force due to the elasticity of the surrounding grains. In the present thesis, ceramics and composites have been processed, which allow one to study the role played by these forces on the thermo‐ mechanical behavior of these refractory materials. SiAlON ceramics were chosen for studying the viscous force due to the inter‐granular glassy phase. In zirconia and alumina, it is shown how the CNT reinforcements may improve the restoring force and consequently the creep resistance. Different grades of SiAlON ceramics, processed with different sintering aids (Ca2+, Y3+, Yb3+), with oxygen rich (CaO, Y2O3 and Yb2O3) and nitrogen rich (CaH2, YN and YbN) compounds, have been studied. Mechanical spectroscopy has been used to analyze the behavior of the residual glassy phase, present after sintering, either as grain‐boundary glassy (GB) films or glass pockets located in GB triple junctions. The mechanical loss spectra show a relaxation peak, which is due to a relaxation phenomenon (the so called “α‐relaxation”) associated with the glass transition in the amorphous phase. The peak position depends on the glass viscosity and the peak height is mainly affected by the glassy phase amount and the SiAlON bimodal microstructure, namely equiaxed versus elongated grains. Moreover the peak height depends on the restoring force provided by the neighboring grains, which limit the GB sliding process. As a matter of fact, a good correlation between the mechanical loss peak and plastic deformation in a compression test has been observed. It is concluded that the elongated grains in the bimodal microstructure provide a higher restoring force, which limits the GB sliding of smaller equiaxed grains. In the case of equiaxed fine grained oxide ceramics, such as zirconia and alumina, the restoring force has been increased by CNT additions, which can reinforce the GBs. 3Y‐TZPcomposites with a homogenous distributions of CNTs, ranging within 0.5 – 5 wt%, were processed by SPS. A significant improvement in room temperature fracture toughness and shear modulus as well as creep performance at high temperature were obtained, and interpreted as due to the GB reinforcing role of the CNTs. To support this interpretation, high‐resolution electron microscopy and Raman spectroscopy have been carried out. Moreover, a remarkable enhancement of the electrical conductivity up to ten orders of magnitude due to CNT additions has been obtained with respect to the pure ceramics. The isothermal spectrum of the 3Y‐TZP composites (measured at 1600 K) is composed of a mechanical loss peak at a frequency of about 0.1 Hz, which is superimposed on an exponential increase at lower frequency. This is interpreted as primarily due to GB sliding. The absence of a well‐marked peak in monolithic 3Y‐ TZP is justified by considering that the restoring force decreases at low frequencies or high temperatures. Therefore, GB sliding is no more restricted and the mechanical loss increases exponentially, which is correlated to macroscopic creep. With CNT additions the mechanical loss decreases and the relaxation peak is better resolved with respect to the background. This is interpreted by the pinning effect of CNTs on GBs, providing addition source of restoring force, which can hinder GB sliding at high temperature, resulting in a creep resistance improvement. Similarly to 3Y‐TZP based composites, alumina specimens (3 different types of alumina powders) reinforced with different amount of CNTs were sintered by SPS. It is shown how the initial particle size of the powders may affect the dispersion of CNTs. Measurement of different properties, such as hardness, fracture toughness and mechanical loss at high temperature, have evidenced the crucial role of the CNT dispersion in the obtained mechanical properties.

EPFL2013

Thermal stress relaxation in magnesium matrix composites studied by mechanical spectroscopy

Abu Salek Md. Fahim Chowdhury, Daniele Mari, Robert Schaller

Thermal stress relaxtion at the interfaces in magnesium matrix composite has been studied by mechanical spectroscopy. Two specimens were processed by a gas pressure infiltration method. In one sample, the metallic matrix was unidirectionally oriented with respect to the matrix-reeinforcement interface by a Bridgeman technique, while the other was kept as infiltrated. The results show a strong dependence of the damping on the orientation of the matrix. The results are compared with a model of thermal stress relaxation by dislocation motion controlled by a solid friction mechanism. A fitting parameter proportional to the mobile dislocation density is obtained showing the entire evolution of the mobile dislocation density with respect to the temperature.

2008

Spectroscopie mécanique de la relaxation des contraintes d'interface dans les composites à matrice métallique

Metal matrix composites are known for their excellent specific mechanical properties. Nevertheless, because of the thermal expansion mismatch between the matrix and the reinforcements, thermal stresses arise at the interfaces of such materials. In order to relax these stresses, dislocations are emitted from the interface and propagate in the matrix, which can influence the mechanical behavior of the composite material. Mechanical spectroscopy, which characterizes the ability of a solid to dissipate energy under an external excitation, was used to study the relaxation mechanisms occurring at the interface of MMCs. Indeed, the mobile matrix dislocations near the interface are the main sources of damping, making this technique very sensitive to these mechanisms. Composites studied here were processed by gas-pressure infiltration of the reinforcement preform by the molten metal. The processed composites were based on aluminum, magnesium and Mg-2%Si alloy, which is known for its high damping level. They were reinforced by short misorientated alumina fibers or long and aligned carbon and silicon carbide fibers. In the case of long fibers, two types of orientation were obtained: parallel or perpendicular to the composite axis. In order to modify the interface morphology, a heat treatment was carried out on aluminium matrix composites reinforced by alumina fibers during the infiltration process. By increasing the contact time between the molten matrix and the fibers, alumina crystals were formed on the surface of the fibers, whose size increased with time. The specific elastic moduli of the processed composites were clearly superior to those of matrix alone and their value agreed well with the existing theoretical models. Composites were submitted to thermal cycles from 120 K to 500 K and the internal friction and dynamical modulus were measured as a function of temperature. It was shown that the behavior of these two parameters, the large maximum at low temperatures and the modulus anomaly in the case of magnesium composites was driven by the motion of the dislocations activated in the matrix in order to relax thermal stresses. The internal friction was also characterized by a transient contribution, depending on the heating or cooling rate dT/dt and the excitation frequency ω. By using a model developed by Mayencourt and al., it was possible to determine two parameters C1 and C2 which were sensitive respectively to the mobile dislocation density relaxing the thermal stresses and the interface strength. The difference in the behavior of these two parameters as a function of temperature tended to show the great potential of the magnesium matrix composites. Indeed, the interface strength was decreasing at low temperature, allowing a better toughness whereas it was increasing at high temperature, improving the creep resistance. Finally, in the case of the aluminum matrix composites reinforced by short fibers with alumina crystals at the interface, it was observed that the elastic modulus was decreasing as crystal size increased. However, when the crystals exceeded a certain size, they were acting as pinning points between matrix and fibers, resulting in the increase of the modulus almost to its initial value. By determining the parameter C1 from the transient damping, it was shown that this parameter followed the same trend as the elastic modulus, which made it a good probe for the interface quality.

EPFL2004

High Temperature Behavior of Nano-Structured Ceramic Composites Studied by Mechanical Spectroscopy

Mehdi Mazaheri

EPFL2013

Spectroscopie mécanique de la relaxation des contraintes d'interface dans les composites à matrice métallique

EPFL2004