Lise Durand

Dog-bone copper specimens prepared by one-step spark plasma sintering

Copper dog-bone specimens are prepared by one-step spark plasma sintering (SPS). For the same SPS cycle, the influence of the nature of the die (graphite or WC–Co) on the microstructure, microhardness, and tensile strength is investigated. All samples exhibit a high Vickers microhardness and high ultimate tensile strength. A numerical electro-thermal model is developed, based on experimental data inputs such as simultaneous temperature and electrical measurements at several key locations in the SPS stack, to evaluate the temperature and current distributions for both dies. Microstructural characterizations show that samples prepared using the WC–Co die exhibit a larger grain size, pointing out that it reached a higher temperature during the SPS cycle. This is confirmed by numerical simulations demonstrating that with the WC–Co die, the experimental sample temperature at the beginning of the dwell is higher than the experimental control temperature measured at the outer surface of the die. This difference is mostly ascribed to a high vertical thermal contact resistance and a higher current density flowing through the WC–Co punch/die interface. Indeed, simulations show that current density is maximal just outside the copper sample when using the WC–Co die, whereas by contrast, with the graphite die, current density tends to flow through the copper sample. These results are guidelines for the direct, one-step, preparation of complex-shaped samples by SPS which avoids waste and minimizes machining.

A spark plasma sintering densification modeling approach: from polymer, metals to ceramics

The powder compaction modeling of advanced sintering techniques such as spark plasma sintering is a crucial step in the conception of complex shape objects and the understanding of the process. The complete identification of common powder compaction models requires lengthy experimental investigations based on creep and compaction tests. In order to circumvent this problem, a semi-theoretical approach can be employed whereby the mechanical behavior of the powder material is determined theoretically and the temperature-dependent equivalent creep behavior of the material is determined experimentally. Extending the use of this approach to polymers, metals and ceramics is discussed and compared to other independent methods.

Local Strain Measurements at Dislocations, Disclinations and Domain Boundaries

We present the state of the art in strain mapping at the nanoscale using aberration - corrected high - resolution transmission electron microscopy, HRTEM and HAADF - STEM, and dark - field electron holography (DFEH) [1]. In particular, we will focus on the examination of localized strains around defects. A broader comparison of TEM strain mapping techniques can be found i n a recent review [2]. High - resolution images can be analysed by geometric phase analysis (GPA) [3] or applying peak - finding routines to determine the positions of individual atomic columns. GPA is best adapted to measuring the deformation of the crystall ine lattice, as the example concerning a five - fold twinned Pt nanoparticle will show (Figure 1). These star - shaped particles [4] have a disclination - like strain fields around their centres, as found for Au nanoparticles [5]. In multiferroic materials, peak - finding can be used to determine the relative displacements of atom columns within a unit cell [6]. The local polarization and strain can be mapped around dislocations and in the vicinity of domain walls (Figure 2). DFEH was developed to measure strain over wide fields of view to high precision and nanometre spatial resolution. We have nevertheless been applying the technique to the study of quantum dots to relatively high resolution [7]. As with any TEM technique the samples are necessarily thin which allows some of the strain to be relaxed: the well - known thin film effect. In addition, dynamical scattering effects the strain information [8]. These issues will be addressed using a combination of finite - element modelin g (FEM) and dynamical - scattering simulations. This overview will, in addition, show results from the recently installed I2TEM microscope (Hitachi), an instrument specifically designed for DFEH experiments and aberration - corrected HRTEM over wide fields of view and for in - situ experiments (Figure 3).