Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source.

Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. However, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality elastic and inelastic neutron scattering experiments to be made of reactive metallic and other liquids in the equilibrium and supercooled temperature regime. The apparatus is comprised of a high vacuum chamber, external and internal neutron collimation optics, and a sample exchange mechanism that allows up to 30 samples to be processed between chamber openings. Two heating lasers allow excellent sample temperature homogeneity, even for samples approaching 500 mg, and an automated temperature control system allows isothermal measurements to be conducted for times approaching 2 h in the liquid state, with variations in the average sample temperature of less than 0.5%. To demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr64Ni36 measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample (∼100 mg).

Appearance of metastable B2 phase during solidification of Ni50Zr50 alloy: electrostatic levitation and molecular dynamics simulation studies.

High-energy x-ray diffraction measurements of undercooled, electrostatically levitated Ni50Zr50 liquid droplets were performed. The observed solidification pathway proceeded through the nucleation and growth of the metastable B2 phase, which persisted for several seconds before the rapid appearance of the stable B33 phase. This sequence is shown to be consistent with predictions from classical nucleation theory using data obtained from molecular dynamics (MD) simulations. A plausible mechanism for the B2-B33 transformation is proposed and investigated through further MD simulations.

Noncontact technique for measuring the electrical resistivity and magnetic susceptibility of electrostatically levitated materials.

We describe the development of a new method for measuring the electrical resistivity and magnetic susceptibility of high temperature liquids and solids. The technique combines a tunnel diode oscillator with an electrostatic levitation furnace to perform noncontact measurements on spherical samples 2-3 mm in diameter. The tank circuit of the oscillator is inductively coupled to the sample, and measurements of the oscillator frequency as a function of sample temperature can be translated into changes in the sample's electrical resistivity and magnetic susceptibility. Particular emphasis is given on the need to improve the positional stability of the levitated samples, as well as the need to stabilize the temperature of the measurement coil. To demonstrate the validity of the technique, measurements have been performed on solid spheres of pure zirconium and low-carbon steel. In the case of zirconium, while absolute values of the resistivity were not determined, the temperature dependence of the resistivity was measured over the range of 640-1770 K and found to be in good agreement with literature data. In the case of low-carbon steel, the ferromagnetic-paramagnetic transition was clearly observable and, when combined with thermal data, appears to occur simultaneously with the solid-solid structural transition.