J. C. Cooley

Critical examination of heat capacity measurements made on a Quantum Design physical property measurement system

Abstract We examine the operation and performance of an automated heat-capacity measurement system manufactured by Quantum Design (QD). QD’s physical properties measurement system (PPMS) employs a thermal-relaxation calorimeter that operates in the temperature range of 1.8–395 K. The accuracy of the PPMS specific-heat data is determined here by comparing data measured on copper and synthetic sapphire samples with standard literature values. The system exhibits an overall accuracy of better than 1% for temperatures between 100 and 300 K, while the accuracy diminishes at lower temperatures. These data confirm that the system operates within the ±5% accuracy specified by QD. Measurements on gold samples with masses of 4.5 and 88 mg indicate that accuracy of ±3% or better can be achieved below 4 K by using samples with heat capacities that are half or greater than the calorimeter addenda heat capacity. The ability of a PPMS calorimeter to accurately measure sharp features in Cp(T) near phase transitions is determined by measuring the specific heat in the vicinity of the first-order antiferromagnetic transition in Sm2IrIn8 (T0=14 K) and the second-order hidden order (HO) transition in URu2Si2 (TN=17 K). While the PPMS measures Cp(T) near the second-order transition accurately, it is unable to do so in the vicinity of the first-order transition. We show that the specific heat near a first-order transition can be determined from the PPMS-measured decay curves by using an alternate analytical approach. This correction is required because the latent heat liberated/absorbed at the transition results in temperature–decay curves that cannot be described by a single relaxation time constant. Lastly, we test the ability of the PPMS to measure the specific heat of Mg11B2, a superconductor of current interest to many research groups, that has an unusually strong field-dependent specific heat in the mixed state. At the critical temperature the discontinuity in the specific heat is nearly 15% lower than measurements made on the same sample using a semi-adiabatic calorimeter at Lawrence Berkeley National Laboratory.

The effect of alloying on the properties of (Nb, Ti)Cr2 C15 laves phases

Abstract The effect of composition on the ternary (NbCr 2 –TiCr 2 ) C 15 phase properties has been investigated, focusing upon the defect structure, elastic properties, and mechanical behavior. The C 15 phase field is continuous between NbCr 2 –TiCr 2 , with a maximum phase field width of at least 7 at.% solubility. The defect mechanism is governed by anti-site constitutional defects for all alloys. Mechanically, the alloys display a maximum in hardness in the center of the ternary phase field (and a minimum of toughness). The ternary phase field has features that are characteristic of solid-solution strengthening mechanisms. Finally, the elastic properties indicate that the alloys become stiffer in the middle of the ternary phase field. The best compromise of properties occurs furthest from stoichiometry in the ternary phase field at the nominal composition of Nb 19 Ti 19 Cr 62 . The relationships between the defect structure, elastic properties, and mechanical response for the C15 phases are discussed using a combination of atomic size arguments and electronic structure analyses. From these relationships, alloy design strategies for NbCr 2 -based alloys are evaluated.

Progress toward fabrication of graded doped beryllium and CH capsules for the National Ignition Facilitya)

Current ignition designs require graded doped beryllium or CH capsules. This paper reports on the progress toward fabricating both beryllium and CH capsules that meet the current design criteria for achieving ignition on the National Ignition Facility (NIF) [S. Hann et al., Phys. Plasmas 12, 056316 (2005)]. NIF scale graded copper doped beryllium capsules have been made by sputter coating, while graded germanium doped CH capsules have been made by plasma polymer deposition. The sputtering process used for fabricating graded beryllium shells was produced with a void fraction of ∼5%. Varying the deposition parameters can lead to several different beryllium microstructures, which have been tuned to reduce the void size and fraction to within specifications. In addition, polishing of beryllium-coated shells reduces the outer surface roughness of shells to ignition specifications. Transmission electron microscopy has been used to characterize void fraction and grain structure of beryllium coatings. The plasma ...

BERYLLIUM CAPSULE COATING DEVELOPMENT FOR NIF TARGETS

Abstract Various morphologies have been observed in sputter-deposited Be ablator capsules, including nodular growth, cone growth and twisted grain growth. By devising an agitation method that includes both bouncing and rolling the spherical mandrels during deposition, and by reducing the coating rate, consistent columnar grain structure has now been obtained up to 170 mm. Low mode deformation of the shells is observed on thin CH mandrels, but is suppressed if stiffer mandrels are used. Ablator density measured by weighing and x-ray radiography is 93%–95% of bulk density of Be. Transmission electron microscopy shows 100.200 nm size voids in the film and striations inside the grains. Be shells produced with rolling agitation have met most of the NIF specifications. Some of the few remaining issues will be discussed.

Versatile and compact capacitive dilatometer

We describe the design, construction, calibration, and operation of a relatively simple differential capacitive dilatometer suitable for measurements of thermal expansion and magnetostriction from 300 to below 1K with a low-temperature resolution of about 0.05A. The design is characterized by an open architecture permitting measurements on small samples with a variety of shapes. Dilatometers of this design have operated successfully with a commercial physical property measurement system, with several types of cryogenic refrigeration systems, in vacuum, in helium exchange gas, and while immersed in liquid helium (magnetostriction only) to temperatures of 30mK and in magnetic fields to 45T.

Tin telluride: a weakly co-elastic metal

We report resonant ultrasound spectroscopy (RUS), dilatometry/magnetostriction, magnetotransport, magnetization, specific-heat, and 119Sn Mossbauer spectroscopy measurements on SnTe and Sn0.995Cr0.005Te. Hall measurements at T=77 K indicate that our Bridgman-grown single crystals have a p-type carrier concentration of 3.4×1019 cm−3 and that our Cr-doped crystals have an n-type concentration of 5.8×1022 cm−3. Although our SnTe crystals are diamagnetic over the temperature range 2≤T≤1100 K, the Cr-doped crystals are room-temperature ferromagnets with a Curie temperature of 294 K. For each sample type, three-terminal capacitive dilatometry measurements detect a subtle 0.5 μm distortion at Tc≈85 K. Whereas our RUS measurements on SnTe show elastic hardening near the structural transition, pointing to co-elastic behavior, similar measurements on Sn0.995Cr0.005Te show a pronounced softening, pointing to ferroelastic behavior. Effective Debye temperature, θD, values of SnTe obtained from 119Sn Mossbauer studies show a hardening of phonons in the range 60–115 K (θD=162 K) as compared with the 100–300 K range (θD=150 K). In addition, a precursor softening extending over approximately 100 K anticipates this collapse at the critical temperature and quantitative analysis over three decades of its reduced modulus finds ΔC44/C44=A|(T−T0)/T0|−κ with κ=0.50±0.02, a value indicating a three-dimensional softening of phonon branches at a temperature T0∼75 K, considerably below Tc. We suggest that the differences in these two types of elastic behaviors lie in the absence of elastic domain-wall motion in the one case and their nucleation in the other.

DISLOCATIONS IN MO5SIB2 T2 PHASE

Abstract Dislocation structures in a nearly single phase annealed Mo5SiB2 T2 alloy have been investigated by transmission electron microscopy (TEM). The dislocations have been subjected to Burgers vector and trace analyses to determine the slip directions and planes with the aid of image simulations generated using single crystal elastic constants derived from first principles calculations. The experimental results are compared to predicted slip directions and planes from anisotropic elasticity calculations. Thermal expansion coefficients have been measured by dilatometry and are compared to both calculated and previous experimental values measured using diffraction techniques. Lastly, preliminary compression testing has been performed on the single phase material at 1200°C.

Magnetic-field-induced lattice anomaly inside the superconducting state of CeCoIn5: anisotropic evidence of the possible Fulde-Ferrell-Larkin-Ovchinnikov state.

We report high magnetic field linear magnetostriction experiments on CeCoIn5 single crystals. Two features are remarkable: (i) a sharp discontinuity in all the crystallographic axes associated with the upper superconducting critical field B(c2) that becomes less pronounced as the temperature increases and (ii) a distinctive second orderlike feature observed only along the c axis in the high field (10 T < or approximately B< or = B(c2)) low temperature (T < or approximately 0.35 K) region. This second order transition is observed only when the magnetic field lies within 20 degrees of the ab planes and there is no signature of it above B(c2), which raises questions regarding its interpretation as a field induced magnetically ordered phase. Good agreement with previous results suggests that this anomaly is related to the transition to a possible Fulde-Ferrel-Larkin-Ovchinnikov superconducting state.

Low-frequency ac measurement of the Seebeck coefficient

We have analyzed the sources of error in the measurement of the Seebeck coefficient and designed a low frequency ac method to reduce them. This method has high precision in a short time period compared to commonly used dc methods while it minimizes some major sources of error that other ac methods do not. Furthermore, the setup can be fit into a 3 mm diam × 7 mm Teflon pressure cell and has minimal side effects due to the heat conductance of the pressure medium. We have also proposed and tested several methods to calibrate the Seebeck coefficient of thermocouples under pressure.

Fabrication of Beryllium Capsules with Copper-Doped Layers for NIF Targets: A Progress Report

Abstract The sputtering of beryllium (Be) has been used at LLNL for nearly 30 years in the fabrication of laser targets. Several years ago the prospect of using sputtering to fabricate spherical Be capsules for National Ignition Facility (NIF) targets began to be explored and a basic strategy was developed that involved sputtering down onto plastic mandrels bouncing in a pan. While this appears to be very straightforward in principle, in practice sputtering has been used almost exclusively to make thin films (< 1 micron) on flat substrates. Thick films pose a significant challenge for sputtering while materials on spherical substrates are essentially unexplored. More recently, based on computational results, the point design for the first NIF ignition target capsule was specified as a Be capsule with Cu-doped layers of specific thickness, each layer with a different concentration of copper. While the work described here was motivated by the need to make these layered capsules, progress has been made in developing a more complete metallurgical understanding of the materials that are fabricated and the relationship between the sputter processing and microstructure of these spherical samples.