Non-destructive Electrical Characterization of Controlled Waspaloy Microstructures

Abstract

In this research, controlled Waspaloy microstructures were produced with the objective of studying microstructural evolution in this alloy via electrically-based ac/dc non-destructive techniques. Correlations were developed between electrical measurements and alternate characterization techniques such as Ultra Small Angle X-ray Scattering (USAXS), Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD) to gain a complete understanding of the microstructural transformations and the associated mechanisms. Three different sets of controlled microstructures were produced in this research. In Set I microstructures, matrix (gamma) grain sizes of 13, 52 and 89 micrometers were obtained after solution-treatments at 1045 and 176;C, 1090 and 176;C and 1145 and 176;C respectively. A vacancy stabilization treatment at 1045 and 176;C followed after which, the specimens were aged at 800 and 176;C for times ranging from 0.1 hrs to 100 hrs to vary the gamma prime precipitate size distribution. In Sets II and III, the solution-treatment was only conducted at 1145 and 176;C, with the stabilization treatment conducted only in Set II. Subsequently, aging experiments were conducted at 725 and 176;C (or 700 and 176;C in Set II), 800 and 176;C and 875 and 176;C for times up to 100 hrs.

DC four-point probe resistivity of specimens increased to a maximum upon initial aging from the solution-treated condition and showed a decreasing trend thereafter with successive aging. This, in addition to complementary evidence from SEM and USAXS, led to the conclusion that gamma prime nucleation-growth was complete by the time the resistivity maximum was observed. Resistivity variations that ensued upon successive aging after the maximum were attributed to microstructural/compositional changes due to gamma prime coarsening. The height of the maximum decreased drastically with increase in aging temperature from 725 and 176;C to 800 and 176;C, while the resistivity did not increase from the solution-treated condition upon aging at 875 and 176; C. Coarsening studies based on USAXS analysis indicated an LSW type volume diffusion mechanism of coarsening in Waspaloy, with an average coarsening rate constant of 3.25x10-29 [m3/sec] for Set I specimens aged at 800 and 176;C.

Analytical and Finite Element (FE) models of two-probe impedance and dc four-point probe resistivity methods were developed to gain insight into the measured response and the accurate determination of material properties.

AFM-based localized electrical examination of sub-grain Waspaloy microstructures was successfully conducted using electrostatic force microscopy (EFM), scanning Kelvin probe microscopy (SKPM) and current-AFM (I-AFM) electrical modes. I-AFM experiments revealed that the conductivity of the gamma prime phase was lower than that of the gamma phase.