Subboundaries in hcp4He crystals studied by SR X-ray topography

The internal structure of hcp⁴He crystals was studied by SR (synchrotron radiation) X-ray topography. Subboundaries in the crystals appeared as black or white bands in the X-ray topographs. In one of the hcp⁴He crystals, the subboundaries turned out to be flat planes perpendicular to the basal plane. They were small-angle tilt boundaries which consisted of basal edge dislocations. The dislocation spacing in one of the subboundaries was determined to be 800 nm and the total density of the boundary dislocations to be 2.6 × 10⁵ cm^–2. The subboundaries in another hcp⁴He crystal were curved and/or branching, indicating that the crystal was strained.     

On the Mobile Behavior of Solid 4He at High Temperatures

We report studies of solid helium contained inside a torsional oscillator, at temperatures between 1.07 K and 1.87 K. We grew single crystals inside the oscillator using commercially pure ⁴He and ³He-⁴He mixtures containing 100 ppm ³He. Crystals were grown at constant temperature and pressure on the melting curve. At the end of the growth, the crystals were disordered, following which they partially decoupled from the oscillator. The fraction of the decoupled He mass was temperature and velocity dependent. Around 1 K, the decoupled mass fraction for crystals grown from the mixture reached a limiting value of around 35%. In the case of crystals grown using commercially pure ⁴He at temperatures below 1.3 K, this fraction was much smaller. This difference could possibly be associated with the roughening transition at the solid-liquid interface.     

4He Adsorption and Superfluid Transition on C60

We present adsorption isotherm data of⁴He on C₆₀ for 1.50 K<T<1.68 K determined by measurements of the frequency of quartz crystal microbalances (QCM’s) coated with C₆₀ films. We find a Kosterlitz-Thouless transition with a jump in the areal superfluid density close to predictions. By comparing the adsorbed⁴He on two QCM’s we derive an upper limit for the amount of⁴He intercalated into C₆₀ at low temperature of 0.05⁴He atoms per C₆₀ molecule. The low coverage portion of the adsorption data shows an apparent excess adsorption of⁴He onto the C₆₀.     

Sorption studies of helium and neon by crystals of C60 and C70

We present sorption measurements for³He and⁴He in the temperature range of 1.5 K to 4.1 K, and for²⁰Ne in the temperature range of 22 K to 27 K by crystals of C₆₀, C₇₀ and crystals of the mixture of these two molecules, 80% C₆₀, 20% C₇₀ We analyze these data by taking into account the non-ideality of the gas in equilibrium with the adsorbate. We calculate chemical potentials and isosteric heats. We find that there is no obvious evidence of intercalation of helium in these crystals at low temperatures. At higher temperatures there are some anomalies in the helium isotherms, and indication of excess sorption. The isosteric heat shows a minimum in this region which can be interpreted as penetration of the helium into a region of repulsive potential. We also find that levels of sorption, at the same chemical potential difference from saturation, are higher for⁴He than for³He. They are also higher for⁴He on C₇₀ than for the other crystals. For neon our work is concentrated around the triple point. We find that the isotherms indicate the formation of liquid or solid films. Below the triple point, and above a few atomic layers, the neon film does not grow uniformly.     

Thin Film Adsorption of 4He To C60

Low temperature adsorption isotherms of ⁴ He on C ₆₀ films are presented. Data is obtained by monitoring the frequency of C ₆₀ -coated quartz crystal microbalances versus pressure as ⁴ He gas is added to an experimental cell at constant temperature. Results which indicate excess low coverage ⁴ He adsorption to C ₆₀ are presented for T=1.5 K and T=1.68 K.     

Anomalous 4He Adsorption to in situ Baked C60

We present data for ⁴ He adsorption to thermally evaporated C ₆₀ films for 1.30 K < T < 2.17 K. This work minimizes possible effects due to the presence of adsorbed species other than ⁴ He. We observe an anomalous mass adsorption to the C ₆₀ films close to ⁴ He saturation which amounts to 3 times the expected mass loading due to the saturated ⁴ He film on the C ₆₀ surface at T = 1.30K.     

Structural and Superfluid Properties of the 4He Monolayer on a C28 Molecule

We have performed path-integral Monte Carlo calculations to study the adsorption of N ⁴He atoms on a single C₂₈ fullerene molecule. Radial density distributions show a layer-by-layer growth of ⁴He with the first adlayer being located at a distance of 5.3 Å from the center of C₂₈. The monolayer is found to show a commensurate structure at N=16 with each of the 16 adsorption sites on the molecular surface being occupied by one ⁴He atom. As more helium atoms are adsorbed beyond N=16, the adlayer is in a mixed state consisting of 4 localized atoms at the hexagonal faces and the other atoms delocalized over the pentagonal faces. Another structurally-ordered state is observed at N=32, where the helium layer shows the same crystalline structure with an icosahedral symmetry as observed for 32 ⁴He atoms on a C₆₀ molecule. It is found that more ⁴He atoms can be squeezed into the first layer to disrupt this icosahedral structure when enough ⁴He atoms are added in the second layer. Finally we observe the reentrant superfluid response of the monolayer with superfluidity being quenched completely at the ordered states of N=16 and 32.     

Realization of a 3He�C4He Vapor-Pressure Thermometer for Temperatures Between 0.65?K and 5?K at LNE-CNAM

In the temperature range between 0.65 K and 5 K, the International Temperature Scale of 1990 (ITS-90) is based on ³He and ⁴He vapor-pressure thermometers. Between 0.65 K and 1 K, the ITS-90 overlaps with the Provisional Low Temperature Scale of 2000 (PLTS-2000), defined in term of the melting pressure of ³He. Some differences, up to more than 1 mK, exist between the two scales in the overlapping interval. The LNE-CNAM has recently started the construction of a ³He?C⁴He vapor-pressure thermometer to realize the ITS-90 in its lowest subrange at the highest degree of accuracy. The device is provided with two separate vapor-pressure chambers, one for ³He and the other for ⁴He, built in a single copper block, and is installed in the experimental space of a dilution refrigerator. The vapor-pressure thermometer is designed to accommodate on the same copper block several transfer standards, an acoustic thermometer, and the ³He melting-pressure thermometer. This configuration is intended for realizing calibrations of transfer standards down to 0.65 K, for investigating the possibility to extend the acoustic thermometer below 4 K, and to perform a direct comparison between the ITS-90 and the PLTS-2000 in the overlapping temperature range, in order to study their differences. The realization of the system has been recently accomplished, and this report illustrates the characteristics of such an experimental device.     

4He Impurities in 3He: Energetics and Dynamics

We have developed the optimized Fermi Hypernetted Chain Theory of a single impurity atom in a Fermi liquid, and have applied the theory to a ⁴He atom in bulk ³He. Previous applications of the theory for one component have produced excellent agreement with the experimental equation of state of ⁴He; the resulting equation of state of bulk ³He is about 0.4 K above the experimental one. Within the same theory, we obtain the pressure dependence of the chemical potential of ⁴He in bulk ⁴He, ³He in ³He, as well as the chemical potential of a ⁴He impurity in ³He. The pressure dependence of the impurity chemical potential agrees well with the experimental data, but we have a constant energy offset of about 1.2 K that disallows conclusive statements. This offset is partly explained by the relative inaccuracy of the ³He equation of state. We then calculate the self-energy of a single ⁴He impurity in ³He. Our results for the effective mass m^* ₄ fall within the experimental error of the best available data; they increase from about m^* ₄/m₄1.4 at zero pressure, to m^* ₄/m₄1.6 at p=20 atm. We show that this effective mass enhancement is, to about equal parts, due to hydrodynamic backflow and to the coupling to particle-hole excitations. When the latter are turned off in the collective approximation of the impurity-background correlations one obtains a significantly lower effective mass, m^* ₄/m₄1.2–1.35.     

3He Impurity Effects on the Growth Kinetics of 4He Crystals

We report the growth kinetics of the⁴He crystals with a small amount of³He impurities around 0.8 K. The growth resistance was measured using the response of the charged interface with respect to an externally applied voltage. In 5 ppm and 10 ppm³He mixtures, it is found that (1) the relaxation process can be expressed as an exponential behavior, (2) the growth resistance becomes larger compared to pure⁴He and does not have a strong³He concentration dependence, and (3) the temperature dependence of the growth resistance is much the same as pure⁴He. We discuss several possible explanations of the present experiment.     

New vapor pressure equations for4He and3He

Attention is drawn to new vapor pressure equations which have been derived for⁴He and³He in terms of the Provisional 0.5 to 30 K temperature Scale (EPT-76). These equations should now be used in place of the T₅₈ table for⁴He and the T₆₂ equation for³He. Although the EPT-76 extends only to 0.5 K, the new³He equation is valid down to 0.2 K.     

Annealing behavior of single mode planar waveguide in YVO4 produced by He ion implantation

We report, for the first time to our knowledge, the formation of single mode planar waveguide in z-cut YVO₄ by 400 keV, 500 keV He ion implantation in fluence of 3 × 10¹⁶ ions/cm² at room temperature or at liquid nitrogen temperature (77 K). We investigated annealing behavior of the guiding mode and near-field image in the waveguide by prism-coupling method and end-face coupling method respectively. We found that the effective refractive index of the TE₀ mode was different before and after annealing for the samples implanted at room temperature, while, annealing had nearly no influence on the effective refractive index of the TE₀ mode of the samples implanted at liquid nitrogen temperature (77 K). After annealing at 600 K for 1 h, no guiding mode was observed in the sample implanted by 400 keV He ion in fluence of 3 × 10¹⁶ ions/cm² at room temperature. The Rutherford backscattering/channeling technique was used to investigate the damage reduction after annealing treatments. The minimum yield of the implanted, annealed sample was 5.43%. We reconstructed the refractive index profiles in the waveguide under different condition by applying intensity calculation method.     

Direct measurements of thermal vacancies in BCC4He

X-ray lattice parameters of bcc⁴He crystals in contact with superfluid⁴He were measured with 300 ppm accuracy in the temperature range 1.494–1.711 K, corresponding to solid molar volumes between 20.88 and 21.09 cm³. Thermal vacancy concentrations in the solid at melting were estimated from a comparison of these lattice parameters with bulk solid molar volumes from the literature. Independently, temperature-dependent x-ray lattice parameter measurements on a bcc sample, held at constant macroscopic volume from 1.700 to 1.735 K, were referenced to the same solid sample (at 20.90 cm³) in the hcp phase near 0.8 K, where thermal vacancy content is small. The value of the free energy of formation for vacancies in bcc⁴He obtained from these measurements isf=9±1 K. The relationship between this value and indirect inferences about vacancy formation from ion mobility and NMR experiments is discussed. Comparisons are made between vacancy properties in bcc⁴He and in the more extensively studied bcc phase of³He. There are many parallels between the two systems. But a puzzling apparent difference between the vacancy relaxation energies in the two solids is pointed out.     

Adsorption of3He and4He on copper and on argon-coated copper below 20 K

Measurements have been made of adsorption isotherms of ³ He and of ⁴ He on copper and on a monolayer of argon deposited on copper in the temperature range 6.18–18.55 K and in the pressure range 0.25 to 75 Torr. From these many isotherms, calculations have been made of the isosteric heat of adsorptionQ _st/R. In the limit of zero coverage on the argon monolayerQ _st/R=76±2 K for ³ He and 76±2 K for ⁴ He. For adsorption on the bare copper,Q _st/R is difficult to extrapolate to zero coverage, but it probably lies (for both ³ He and ⁴ He) between 135 and 165 K. At theoretical monolayer helium coverage,Q _st/R=44±2 K for ³ He on the argon monolayer and 47±2 K for ⁴ He. At theoretical monolayer helium coverage on the bare copper,Q _st/R=61±4 K for ³ He and 77±5 K for ⁴ He. The results are compared with theoretical evaluations for helium adsorbed on an argon monolayer and with some previous experimental data, and the agreement is found to be fair. All the data are summarized in tables. Finally, a review is given of evaluations, including those from this work, of the monolayer capacity of ³ He and ⁴ He on the substrates studied.Work supported by a contract with the Department of Defense (Themis Program) and with the Office of Naval Research and by a Grant from the National Science Foundation.     

The Fermi Liquid theory of4He in3He

The Zharkov-Silin Fermi Liquid theory of solutions of⁴He in normal (non-superfluid) liquid³He is reviewed and slightly extended. The theory is expected to be valid only below 0.1 K, and it predicts that there should be a hundred-fold increase in the diffusion coefficient as the temperature is lowered into this region. The limited range of validity explains the apparent disagreement between the recent very low temperature measurements of the phase separation line by Nakamura et al. and extrapolations from higher temperatures. In the low temperature experiments the⁴He concentration X₄ is so small that there is no macroscopic phase separation, only a gradual thickening of the⁴He-rich film on the walls. We confirm that the phase separation temperature T_ps(X₄) estimated from the thickening is close to the values which would be observed in an ideal experiment with a macroscopic phase. Fits to T_ps(X₄) including the new data show that the⁴He effective mass m ₄ ^* is close to, and may be equal to, the bare mass m₄. The difference in binding at zero pressure between⁴He in liquid⁴He and in liquid³He is (E₄₄–EE₄₃)/k_B=(0.21+0.03/–0.01)) K. Using the volume measurements of Laheurte to calculate the pressure dependence of E₄₃ indicates that the difference in binding has a minimum of (0.0±0.2) K near 11 atm. This implies that the solubility of⁴He in³He is enhanced in this region of pressure. The behavior of the spinodal line at low temperature, and the possibility of observing Bose condensation in a metastable solution of⁴He in liquid³He are also discussed.     

Self Diffusion in Solid 4He and 3He-4He Mixtures Near the bcc-hcp Phase Transition

We report experiments on the plastic flow of solid ⁴ He and ³ He- ⁴ He mixtures of 1.4% and 2.8% near the bcc-hcp transition. Plastic flow was generated by moving a wire through a macroscopic single crystal. We found that the plastic flow rate both in pure ⁴ He and in mixture helium crystals is enhanced in vicinity of the bcc-hcp phase transition. The results are interpreted in terms of self diffusion in the solid. Values of the self diffusion coefficient D_s at the respective transition temperatures of pure ⁴ He and of the mixtures are very close, and reach that found in normal liquids. The activation energy for self diffusion in the mixtures is lower by up to 3 K than in pure ⁴ He. We suggest that similar to what is observed in bcc metals, self-diffusion in solid He takes place through phonon assisted atom-vacancy exchange. The enhancement of the diffusion near the bcc-hcp transition is a result of the softening of a short wavelength transverse phonon. The temperature dependence of the energy of the phonon calculated using our data is in accord with the Landau theory of a phase transition driven by a soft mode. Work hardening was observed in mixture crystals, but not in pure ⁴ He. This implies that ³ He impurities pin dislocation lines.     

Nuclear magnetic relaxation of3He gas. II.3He-4He mixtures

Longitudinal relaxation timesT ₁ have been measured in³He-⁴He gas mixtures, using pulsed NMR, in the temperature range 0.6–15 K. Helium-3 number densities of the order of 10²⁴ atoms m^–3 were used. Relaxation takes place on or near the walls of the Pyrex sample cells and measurements ofT ₁ give information about the surface phases. A cryogenic precoating of solid molecular hydrogen was used to reduce the helium-substrate binding energy from 100 K on Pyrex to 13 K for³He and 15 K for⁴He. TheT ₁ data at high temperatures were similar to those observed previously in the pure³He-H₂ system. The presence of⁴He generally causedT ₁ to rise on cooling below 2 K due to the preferential adsorption of⁴He over³He at the surface. However,³He atoms that go into quasiparticle states in the superfluid helium film can be an extra source of relaxation. In uncleaned cells, relaxation probably takes place in quasiparticle states at the free surface of the superfluid film, which are bound with an energy of 5.1±0.3 K. Baking the Pyrex cells under vacuum and rf discharge cleaning the walls before sealing in the sample gas were found to increase the bulk gasT ₁ by two or three orders of magnitude. In a cleaned, sealed cell aT ₁ of 8 h was measured at 7.7 MHz and 0.8 K. In this case relaxation is probably occurring two or three helium layers away from the helium-hydrogen interface. It may be possible to observe a predicted minimum in the intrinsic dipolarT ₁ of the bulk gas by using a⁴He wall coating to suppress wall relaxation effects (which usually dominate the nuclear relaxation of the bulk gas).     

Comparison between Torsional Oscillator and Ultrasonic Measurements of 4He Confined in Nano-Porous Media

We have performed torsional oscillator and ultrasonic measurements for ⁴He confined in 2D nano-porous substrate, hectorite. For ⁴He films, the resonance frequency of the torsional oscillator increases rapidly just below a superfluid transition temperature (T _C ), and then becomes constant at the lower temperature. In contrast, the sound velocity below T _C increases monotonically with decreasing temperature. For liquid ⁴He the sound velocity has a small bend at T _b of about 0.9 K. Its increase below T _b is enhanced as the pressure is increased.     

3He Impurities in 4He Systems Adsorbed on Curved Substrates

It is shown that ³He impurities in sufficiently large ⁴He systems adsorbed onto substrates with curved geometries form surface bound states, analogous to the Andreev state on a planar liquid--vapor interface. We report the analysis performed for superfluid ⁴He adsorbed on the external surface of the nano-fullerene C₆₀ and on cylindrical nano-wires of Au. It is found that a single ³He impurity diluted into such adsorbed structures behaves as on films on planar substrates and as on pure ⁴He clusters.     

Fast Diffusion Process in Quenched hcp Dilute Solid 3He–4He Mixture

The study of phase structure of dilute ³He–⁴He solid mixtures of differing quality is performed by the spin echo NMR technique. The diffusion coefficient is determined for each coexistent phase. Two diffusion processes are observed in rapidly quenched (non-equilibrium) hcp samples: the first process has a diffusion coefficient corresponding to hcp phase and the second one has huge diffusion coefficient corresponding to liquid phase, which is evidence of liquid-like inclusions formation during fast crystal growing. It is established that these inclusions disappear in equilibrium crystals after careful annealing.