Background <p>Characterizing deformation and failure mechanisms through small-scale testing has helped in the fundamental understanding of material response, and direct loading in a transmission electron microscope (TEM) has played a large role in this effort. However, crystalline materials exhibit incoherent scattering within the TEM and the resulting intensity variations inhibit direct optical metrology.</p> Objective <p>In this work, we seek to both validate an<i> in situ</i> optical full-field metrology method in the TEM for use with crystalline materials, and measure fracture properties of a MgAl<sub>2</sub>O<sub>4</sub>spinel single crystal at the microscale.</p> Methods <p>Microscale single edge notch bend beams were machined from a spinel single crystal and loaded in the TEM. <i>In situ</i> imaging of a nanoscale speckle pattern allowed use of particle tracking (PT) to extract full-field measurements of the displacement field. A numerical analysis methodology was then used to obtain mixed mode stress intensity factor values.</p> Results <p>A discrepancy between PT and far-field actuator measurements of applied displacement was found (about a maximum of 35% difference), indicating the advantage of using near-field optical measurements in the TEM. For such small-scale testing it is also generally unavoidable to introduce asymmetry in loading. However, the PT results allowed measurement of both <i>K</i><sub>I</sub> and <i>K</i><sub>II</sub>, which were found to be at the time of crack initiation <i>K</i><sub>IC</sub> = 1.51± 0.03 MPa∙m<sup>0.5</sup>, K<sub>IIC</sub> = 0.04± 0.002 MPa∙m<sup>0.5</sup>, respectively.</p> Conclusions <p>The application of PT enables full-field deformation measurements on crystalline materials deformed in the TEM. The effectiveness of the inverse property extraction was demonstrated by good agreement between the full-field PT measurements and FEM results. The MgAl<sub>2</sub>O<sub>4</sub> spinel toughness values extracted also agreed well with previous literature results.</p>

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Opening-Dominated Fracture Characterization of Single Crystal Spinel in the Transmission Electron Microscope

  • Y. Zhang,
  • S.J. Dillon,
  • J. Lambros

摘要

Background

Characterizing deformation and failure mechanisms through small-scale testing has helped in the fundamental understanding of material response, and direct loading in a transmission electron microscope (TEM) has played a large role in this effort. However, crystalline materials exhibit incoherent scattering within the TEM and the resulting intensity variations inhibit direct optical metrology.

Objective

In this work, we seek to both validate an in situ optical full-field metrology method in the TEM for use with crystalline materials, and measure fracture properties of a MgAl2O4spinel single crystal at the microscale.

Methods

Microscale single edge notch bend beams were machined from a spinel single crystal and loaded in the TEM. In situ imaging of a nanoscale speckle pattern allowed use of particle tracking (PT) to extract full-field measurements of the displacement field. A numerical analysis methodology was then used to obtain mixed mode stress intensity factor values.

Results

A discrepancy between PT and far-field actuator measurements of applied displacement was found (about a maximum of 35% difference), indicating the advantage of using near-field optical measurements in the TEM. For such small-scale testing it is also generally unavoidable to introduce asymmetry in loading. However, the PT results allowed measurement of both KI and KII, which were found to be at the time of crack initiation KIC = 1.51± 0.03 MPa∙m0.5, KIIC = 0.04± 0.002 MPa∙m0.5, respectively.

Conclusions

The application of PT enables full-field deformation measurements on crystalline materials deformed in the TEM. The effectiveness of the inverse property extraction was demonstrated by good agreement between the full-field PT measurements and FEM results. The MgAl2O4 spinel toughness values extracted also agreed well with previous literature results.