Abstract

Superplastic deformation of a fully dense TZ3Y material, having a starting grain size around 135–145 nm and depleted of any amorphous phase at grain boundaries, has been investigated using compressive creep tests in air in the temperature range of 1100°–1300°C and the real stress range of 50–100 MPa. The key parameters of the creep law have been determined by performing temperature changes at a fixed stress and stress jumps at a fixed temperature. From such experiments, an average value for the apparent stress exponent of around 3 is obtained when the applied stress varied from 50 to 100 MPa and the temperature was kept constant in the range of 1100°–1300°C. The apparent activation energy of the mechanism controlling the creep deformation is evaluated at 577±75 kJ/mol in the temperature range of 1200°–1300°C, for a real stress of 70 MPa. The values of the apparent grain size exponent can be calculated from the initial grain size in the as-sintered samples and the grain size in the crept samples. In all cases, it was determined to be around 2. Observation of the microstructure of the crept samples, using scanning electron microscopy, reveals grain growth but does not show any significant elongation of the elemental grains. Transmission electron microscopy of a sample crept under 100 MPa at 1300°C reveals clear intragranular dislocation activity. This dislocation activity seems to be mainly confined in folds emitted at triple points. Because the creep parameters (experimental and calculated using a simple geometric model) and the microstructure observed are in good agreement, we propose that the creep mechanism involved is grain boundary sliding accommodated by dynamic grain growth and the formation of triple-point folds.

Highlights

  • THE first observations of a high-temperature superplastic-like behavior for polycrystalline ceramic materials were reported at the end of the seventies and concerned UO2[1] and MgO,[2] deformed under compression in air (MgO) or in a specific atmosphere (UO2).Further experiments in the 1980s by Wakai et al.[3] revealed superplasticity in fine-grained zirconia

  • high-resolution transmission electron microscopy (HRTEM) reveals the lack of an amorphous thin film at the grain boundaries and some rare tiny residual porosities are detected at triple points (Fig. 3)

  • They concluded that the pileups structures observed by Morita must be formed during the cooling step following creep, the cooling step being completed under load.[15]

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Summary

Introduction

THE first observations of a high-temperature superplastic-like behavior for polycrystalline ceramic materials were reported at the end of the seventies and concerned UO2 (in the grain size range of 2–10 mm)[1] and MgO (initial grain size around 0.1 mm),[2] deformed under compression in air (MgO) or in a specific atmosphere (UO2).Further experiments in the 1980s by Wakai et al.[3] revealed superplasticity in fine-grained zirconia. A 3 mol% Y2O3-tetragonal ZrO2 polycrystal (TZ3Y), with a grain size around 0.3 mm, exhibited an unusual, large strain (over 120% by nominal strain) when elongated in ambient atmosphere, at a constant displacement rate from 1.1 Â 10À4 to 5.5 Â 10À4/s, for a given temperature of 14501C.3. Numerous investigations have since been completed on finegrained TZ3Y (grain size always below the micrometer) to identify the mechanism(s) possibly involved in the control of the high-temperature superplastic behavior.[4,5,6,7,8,9,10] Creep (constant load) or constant displacement rate tests were conducted. Interesting reviews, by collecting and interpreting a lot of results originating from different teams around the world, have been published.[11,12]

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