Microstructure and high temperature 4-point bending creep of sol-gel derived mullite ceramics

Four-point bending creep behavior of mullite ceramics with monomodal and bimodal distribution of grain sizes was studied in the temperature range of 1320-1400 °C under the stresses between 40 and 160 MPa. Mullite ceramic with bimodal grain size distribution was prepared using aluminum nitrate nonahydrate as alumina precursor. When ã-Al2 O3 or boehmite were used as alumina precursors, mullite grains are equiaxial with mean particle size of 0.6 ìm for the former and 1.3 ìm for the latter alumina precursor. The highest creep rate exhibited the sample with monomodal morphology and grains in size of 0.6 ìm, which is about one order of magnitude greater than that for the monomodal morphology but with grains in size of 1.3 ìm. The highest activation energy for creep (Q = 742 ± 33 kJ/mol) exhibits mullite with equiaxial grains of 1.3 ìm, whereas for sample with smaller equiaxial grains the activation energy is much smaller and similar to mullite ceramics with bimodal grain morphology. Intergranular fracture is predominant near the tension surface, while transgranular more planar fracture is predominant near the compression surface zone

Crystallization kinetics of mullite formation in diphasic gels containing different alumina components

The crystallization kinetics of mullite formation in diphasic gels containing TEOS-derived amorphous silica and alumina component in different crystalline form and particle size has been studied using quantitative X-ray diffraction (QXRD) with 3:2 mullite as a standard and transmission electron microscopy (TEM). As the source of alumina component, aluminum nitrate nonahydrate, commercial gamma-Al2O3 and boehmite (gamma-AlOOH) were used. The results were consistent with previous studies which indicated that mullite forms initially by nucleation and growth. During the second slow stage of transformation, mullite with approximate 2:1 composition subsequently converts further into 3:2. This process is the fastest in the precursor with the smallest particle size of alumina, and the slowest in the sample with boehmite-derived alumina. In very fine scale of morphology the conversion of 2:1 mullite started even in the first stage of transformation

Influence of alumina precursors on microstructure and creep behavior of sol-gel derived mullite ceramics

The effect of alumina precursors on microstructure, sintering and creep behavior of sol-gel derived mullite ceramics was studied by scanning and transmission electron microscopy (SEM, TEM and HRTEM), dilatometry and measuring the creep resistance in 4-point bending mode. When aluminum nitrate nonahydrate was used as a precursor, elongated crystals (with longer axis about 5-7 µm) were embedded into a matrix of polyhedral much smaller grains. This morphology was due to overlapping of mullite crystallization and viscous flow sintering. Equiaxial mullite grains with 1.3 µm mean sizes were obtained using boehmite (γ-AlOOH) as alumina precursor. Transient alumina formed in situ by the decomposition of boehmite shifted the mullite formation above the sintering temperature, and allowed the formation of equiaxial mullite grains. Four-point bending creep behavior of mullite ceramics was studied in the temperature range of 1320-1400°C under the stresses between 40 and 160 MPa. The higher creep rate and the smaller activation energy (Q= 606 +/- 33 kJ/mol) exhibited the sample with bimodally distributed grain sizes, whereas a smaller creep rate and the higher activation energy (Q=743 +/- 18 kJ/mol) were obtained for mullite ceramic with monomodally distributed grain sizes

Correlation of the precursor type with densification behavior and microstructure of sintered mullite ceramics

The effect of alumina component in diphasic mullite precursors containing alkoxy-derived silica on the crystallization and sintering behavior of compacts was studied. The phenomena observed were characterized using differential thermal analysis (DTA), powder X-ray diffraction (XRD), dilatometry and transmission and scanning electron microscopy (TEM, SEM). In order to change the characteristics of as-prepared gels, the alumina source was varied while keeping the silica source constant. Al(NO3)(3).9H(2)O, gamma-Al2O3 and boehmite (gamma-AlOOH) were used as the alumina source and TEOS as the silica source. Clear differences were found in the microstructure of sintered samples derived from the precursors with aluminum nitrate nonahydrate in comparison to the samples containing gamma-Al2O3 or boehmite (gamma-AlOOH). The former exhibited elongated mullite grains embedded into the "equiaxial mullite matrix". This morphology is due to the overlapping of mullite crystallization and viscous flow sintering temperatures. Transient alumina, either added as gamma-Al2O3 or formed in situ by decomposition of boehmite, shifts the mullite formation above the sintering temperature, and enables formation of equiaxial mullite. The smaller are the transient alumina particles, the smaller are mullite grains of sintered bodies

MECHANICAL SPECTROSCOPY OF ORDERED BINARY Au-Cu

We have studied a binary Au-Cu single crystal by mechanical spectroscopy. Upon very slow cooling from high temperatures, additional relaxation peaks arise at lower frequencies in isothermal spectra after the disappearing of the Zener peak below 665 K due to ordering. A high transient peak is visible at 660 K and it progressively disappears on cooling until 625 K. Another high peak is clearly visible upon following heating until 660 K. Above that temperature it decreases in parallel with the increase of the Zener peak. If the ordered structure is obtained by slowly heating the sample that has been quenched from the disordered state, no low-frequency peak is visible in the isothermal spectra, only a much lower background, which further decreases in parallel with the reappearance of the Zener peak. The low frequency relaxations are possibly due to the movement of antiphase boundaries and twin interfaces in the ordered structures

Influence of alumina precursors on microstructure and creep behavior of sol-gel derived mullite ceramics

The effect of alumina precursors on microstructure, sintering and creep behavior of sol-gel derived mullite ceramics was studied by scanning and transmission electron microscopy (SEM, TEM and HRTEM), dilatometry and measuring the creep resistance in 4-point bending mode. When aluminum nitrate nonahydrate was used as a precursor, elongated crystals (with longer axis about 5-7 µm) were embedded into a matrix of polyhedral much smaller grains. This morphology was due to overlapping of mullite crystallization and viscous flow sintering. Equiaxial mullite grains with 1.3 µm mean sizes were obtained using boehmite (γ-AlOOH) as alumina precursor. Transient alumina formed in situ by the decomposition of boehmite shifted the mullite formation above the sintering temperature, and allowed the formation of equiaxial mullite grains. Four-point bending creep behavior of mullite ceramics was studied in the temperature range of 1320-1400°C under the stresses between 40 and 160 MPa. The higher creep rate and the smaller activation energy (Q= 606 +/- 33 kJ/mol) exhibited the sample with bimodally distributed grain sizes, whereas a smaller creep rate and the higher activation energy (Q=743 +/- 18 kJ/mol) were obtained for mullite ceramic with monomodally distributed grain sizes

Grain boundary relaxation in yellow gold bi-crystals

The mechanical loss spectrum of a yellow gold bi-crystal is presented and analyzed in detail. The relaxation strength is monitored as a function of several geometrical parameters such as sample width, length and thickness. It is found that the relaxation strength is proportional to the GB density (the inverse width), whereas it depends linearly on the sample thickness. The experimental findings are compared to finite elements (FE) simulations, where the material can glide frictionless along the grain boundary. The simulations show the same dependencies as the mechanical loss measurements. The relaxation peak in the loss spectrum can be interpreted as due to GB sliding accommodated by the elastic deformation of the grains. (C) 2015 Elsevier B.V. All rights reserved