An in situ ion irradiation scanning electron microscope (I3SEM) has been developed, installed, and integrated into the Ion Beam Laboratory at Sandia National Laboratories. The I3SEM facility combines a field emission, variable pressure, scanning electron microscope, a 6 MV tandem accelerator, high flux low energy ion source, an 808 nm-wavelength laser, and multiple stages to control the thermal and mechanical state of the sample observed. The facility advances real-time understanding of materials evolution under combined environments at the mesoscale. As highlighted in multiple examples, this unique combination of tools is optimized for studying mesoscale material response in overlapping extreme environments, allowing for simultaneous ion irradiation, implantation, laser bombardment, conductive heating, cooling, and mechanical deformation.
A facility for continuously monitoring the thermal and elastic performance of materials under exposure to ion beam irradiation has been designed and commissioned. By coupling an all-optical, non-contact, non-destructive measurement technique known as transient grating spectroscopy (TGS) to a 6 MV tandem ion accelerator, bulk material properties may be measured at high fidelity as a function of irradiation exposure and temperature. Ion beam energies and optical parameters may be tuned to ensure that only the properties of the ion-implanted surface layer are interrogated. This facility provides complementary capabilities to the set of facilities worldwide which have the ability to study the evolution of microstructure in situ during radiation exposure, but lack the ability to measure bulk-like properties. Here, the measurement physics of TGS, design of the experimental facility, and initial results using both light and heavy ion exposures are described. Lastly, several short- and long-term upgrades are discussed which will further increase the capabilities of this diagnostic.
Irradiation-induced void swelling remains a major challenge to nuclear reactor operation. Swelling may take years to initiate and often results in rapid material property degradation once started. Alloy development for advanced nuclear systems will require rapid characterization of the swelling breakaway dose in new alloys, yet this capability does not yet exist. We demonstrate that transient grating spectroscopy (TGS) can detect void swelling in single crystal copper via changes in surface acoustic wave (SAW) velocity. Scanning transmission electron microscopy (STEM) links the TGS-observed changes with void swelling-induced microstructural evolution. These results are considered in the context of previous work to suggest that in situ TGS will be able to rapidly determine when new bulk materials begin void swelling, shortening alloy development and testing times.
Materials designed for nuclear reactors undergo microstructural changes resulting from a combination of several environmental factors, including neutron irradiation damage, gas accumulation and elevated temperatures. Typical ion beam irradiation experiments designed for simulating a neutron irradiation environment involve irradiating the sample with a single ion beam and subsequent characterization of the resulting microstructure, often by transmission electron microscopy (TEM). This method does not allow for examination of microstructural effects due to simultaneous gas accumulation and displacement cascade damage, which occurs in a reactor. Sandia's in situ ion irradiation TEM (I3TEM) offers the unique ability to observe microstructural changes due to irradiation damage caused by concurrent multi-beam ion irradiation in real time. This allows for time-dependent microstructure analysis. A plethora of additional in situ stages can be coupled with these experiments, e.g.; for more accurately simulating defect kinetics at elevated reactor temperatures. This work outlines experiments showing synergistic effects in Au using in situion irradiation with various combinations of helium, deuterium and Au ions, as well as some initial work on materials utilized in tritium-producing burnable absorber rods (TPBARs): zirconium alloys and LiAlO2.
Conductive polymers have become an extremely useful class of materials for many optical applications. We have developed an electrochemical growth method for depositing highly conductive ({approx}100 S/cm) polypyrrole. Additionally, we have adapted advanced fabrication methods for use with the polypyrrole resulting in gratings with submicron features. This conductive polymer micro-wire grid provides an optical polarizer with unique properties. When the polymer is exposed to ionizing radiation, its conductivity is affected and the polarization properties of the device, specifically the extinction ratio, change in a corresponding manner. This change in polarization properties can be determined by optically interrogating the device, possibly from a remote location. The result is a passive radiation-sensitive sensor with very low optical visibility. The ability to interrogate the device from a safe standoff distance provides a device useful in potentially dangerous environments. Also, the passive nature of the device make it applicable in applications where external power is not available. We will review the polymer deposition, fabrication methods and device design and modeling. The characterization of the polymer's sensitivity to ionizing radiation and optical testing of infrared polarizers before and after irradiation will also be presented. These experimental results will highlight the usefulness of the conductive infrared polarizer to many security and monitoring applications.