ABSTRACT
In this article, we report on the design, manufacture, and testing of a high-pressure cell for simultaneous dielectric and neutron spectroscopy. This cell is a unique tool for studying dynamics on different time scales, from kilo- to picoseconds, covering universal features such as the α relaxation and fast vibrations at the same time. The cell, constructed in cylindrical geometry, is made of a high-strength aluminum alloy and operates up to 500 MPa in a temperature range between roughly 2 and 320 K. In order to measure the scattered neutron intensity and the sample capacitance simultaneously, a cylindrical capacitor is positioned within the bore of the high-pressure container. The capacitor consists of two concentric electrodes separated by insulating spacers. The performance of this setup has been successfully verified by collecting simultaneous dielectric and neutron spectroscopy data on dipropylene glycol, using both backscattering and time-of-flight instruments. We have carried out the experiments at different combinations of temperature and pressure in both the supercooled liquid and glassy state.
ABSTRACT
An experimental setup, including a cryostat and a temperature control system, has been constructed to meet the demands of measuring linear and nonlinear macroscopic relaxation properties of glass-forming liquids in the extremely viscous state approaching the glass transition. In order to be able to measure such frequency-dependent response functions accurately (including dielectric permittivity, specific heat, thermal expansivity, and shear and bulk moduli), as well as nonlinear relaxations following a temperature jump, one must have the ability to hold temperatures of liquids steady over the span of several days or even several weeks. To maximize temperature stability, special care is taken to thermally isolate the sample chamber of the cryostat. The main temperature control system is capable of maintaining temperatures within a few millikelvins. If liquid is deposited into a special transducer assembly that includes a subcryostat unit, the temperature of liquids can be maintained even more precisely, within a few tenths of a millikelvin. This subcryostat unit is more responsive to temperature changes because (i) it is equipped with a Peltier element that provides secondary heating and cooling, (ii) the transducer contains a layer of liquid that is only 50 micfom thick, and (iii) feedback proportional-integral-derivative temperature control is implemented by a fully analog circuit. The subcryostat permits us to change and stabilize temperatures quickly; it takes only 10 s to stabilize the temperature within tenths of a millikelvin after a jump of 1 K, for example, a capability that is highly advantageous for accurately observing relaxation processes following a temperature step.
ABSTRACT
An electronics system has been assembled to measure frequency-dependent response functions of glass-forming liquids in the extremely viscous state approaching the glass transition. We determine response functions such as dielectric permittivity and shear and bulk moduli by measuring electrical impedances of liquid-filled transducers, and this technique requires frequency generators capable of producing signals that are reproducible over the span of several days or even several weeks. To this end, we have constructed a frequency generator that produces low-frequency (1 mHz-100 Hz) sinusoidal signals with voltages that are reproducible within 10 ppm. Two factors that partly account for this precision are that signals originate from voltages stored in a look-up table and that only coil-less filters are used in this unit, which significantly reduces fluctuations of output caused by changes of temperatures of circuits. This generator also includes a special triggering facility that makes it possible to measure up to 512 voltages per cycle that are spaced apart at uniform phase intervals. Fourier transformations of such data yield precise determinations of complex amplitudes of voltages and currents applied to a transducer, which ultimately allows us to determine electrical impedances of transducers with a reproducibility error that is only a few parts per hundred thousand. This equipment is used in tandem with a commercial LCR meter and/or impedance analyzer that give(s) impedance measurements at higher frequencies, up to 1 MHz. The experimental setup allows measurements of the transducer impedance over nine decades of frequency within a single run.
