Lattice dynamics of solid molecular hydrogen for densities 26.18 + 60.78 nm−3, as seen from total neutron interaction cross section measurements

Abstract

The total neutron interaction cross sections versus energy measurements have been carried out on solid parahydrogen for almost 100% change of its density. Some integral parameters of hydrogen very anharmonic phonon spectrum have been determined fro. an analysis of these data.     

A nano-polycrystalline diamond anvil cell with bulk metallic glass cylinder for single-crystal neutron diffraction

ABSTRACT

A high-pressure cell for in-situ single-crystal neutron diffraction was developed. The cell uses nano-polycrystalline diamond anvils in a tubular load frame made of bulk metallic glass which is highly transparent to neutrons and does not produce Bragg reflections. Diffraction peaks from a sample can be measured from almost any direction and the simple geometry of the cell allows accurate attenuation corrections. We demonstrate the operation of the cell by ambient-pressure experiment using a single-crystal of NaCl on the D9 diffractometer at the Institute-Laue-Langevin. A high-pressure experiment was also carried out on a single crystal of ice VII at 2.35?GPa showing the potential to detect weak diffraction spots. The correct integration of weak reflections together with the simple attenuation correction will help to carry out precise structure analysis and address new scientific problems using neutron diffraction.     

High pressure neutron diffraction studies using the Paris-Edinburgh cell

Abstract

Neutron diffraction was until recently confined to pressures below ～ 3 GPa. This restricted range has limited the high-pressure structural information that is available for a wide range of phenomena for which neutron diffraction is the technique of choice. But now the recently-developed Paris-Edinburgh cell can achieve pressures up to ～ 30 GPa with a sample volume large enough to allow accurate structural studies with neutrons. After a period of development of the neutron scattering techniques needed to obtain the best possible results using the cell, a variety of successful structural studies have been performed. These illustrate the value of neutron diffraction in important areas such as locating hydrogen and other low-Z atoms in structures, the measurement of accurate structural pressure dependence and the examination of the changes in atomic thermal motion with pressure.     

Small angle neutron scattering setup for high pressure measurements at IBR-2

Abstract

The experiments which were carried out showed the possibility of using a titanium-zirconium high pressure cell for small angle neutron scattering. We report on some curves measured by SANS with the help of this setup to illustrate the capabilities of the method.     

Study of matter at high pressure using small angle scattering and depolarization of neutrons

Abstract

The method of studying matter under high pressure using the measurement of the transmitted neutron beam is proposed. Method is based on the very small angle scattering and depolarization of neutrons combined with the anvil pressure technique. Test experiments have been carried out demonstrating feasibility of the method for studying phase transitions accompanied with the change of density or magnetization and equations of state. The obtainable pressure range of the method is discussed.     

Neutron scattering studies of structural transformations and vibrational spectra of ice after high pressure treatment

Abstract

The transitions of the recovered high-pressure phase ice VIII first to high-density amorphous (hda) and low-density amorphous ices, and finally to cubic Ic, and hexagonal Ih ice were observed at heating using real-time neutron diffraction. Inelastic incoherent neutron scattering measurements on the hdu ice, ice Ih and high-pressure phase ice VI revealed similarity between the amorphous phase and crystalline ice VI and led to the new proposition that hda ice consists of two interpenetrating hydrogen-bounded networks with no hydrogen bonds between “sublattices”.     

Spectroscopic Studies of the Hydrogen Bond

Abstract

Since the publication of the proceedings of the Ljubljana symposium on hydrogen bonding by Hadzi [1] and the excellent book on the hydrogen bond by Pimentel and McClellan [2], a very large number of publications on the spectroscopic studies of hydrogen bonding have appeared in the literature. The present authors prepared a review on hydrogen bonding covering the period 1958–1963 for limited circulation [3]. In view of the very enthusiastic reception for this review by a number of workers and also the vast amount of published information on the subject after 1963, it was considered valuable to present an up-to-date review on the subject. The present review covers the period from 1958 to 1967 and embodies most of the studies on the hydrogen bond employing spectroscopic methods. The review does not include studies on crystals and macromolecules; hydrogen bonding in crystals has been recently reviewed by Hamilton and Ibers [4]. Electronic theories of the hydrogen bond have been reviewed by Bratoz [5]. Even though we have attempted to write a comprehensive review to include most of the published work on spectroscopic studies, it is possible that we have missed some of the papers in this field; we apologize for such oversights and omissions which become unavoidable in such an undertaking.     

Multi-sample loading technique for comparative physical property measurements in the diamond-anvil cell

ABSTRACT

We present a method to perform improved measurements of the effects of chemical variability on physical properties of single-crystal samples in the diamond-anvil cell by employing a multi-sample approach. By customizing the sizes and shapes of the samples using a focused ion beam machine the simultaneous loading of relatively large crystals into a single sample chamber becomes feasible. To illustrate the potential of this approach, elastic properties of four single crystals of ringwoodite with different chemical compositions have been measured at high pressure. Our results suggest that the multi-sample approach allows for the quantification of small effects of chemical variations, such as iron and hydrogen incorporation, on physical properties. Furthermore, we discuss the possibility of using the multi-sample approach to load several crystals with different crystallographic orientations of the same material into one sample chamber in order to map out the direction dependence of anisotropic physical properties.     

High pressure neutron diffraction using the paris-edinburgh cell: Experimental possibilities and future prospects

Abstract

High pressure neutron diffraction using the Paris-Edinburgh cell has attracted considerable interest ever since it has been shown that full structural data can be obtained at pressures up to 10 GPa. In this paper we will focus on the current state of this technique. Specifically, we report on new experimental possibilities concerning: i) access to “ultrahigh” pressures beyond 20 GPa, ii) experiments at variable temperatures down to 100 K, and iii) experiments on single crystals in inelastic neutron scattering. Current attempts to increase the pressure and temperature range are discussed.     

High-pressure neutron diffraction studies of KH2PO4-type phase transitions

Abstract

High-pressure neutron-diffraction studies have been carried out on KH₂PO₄, KD₂PO₄, H₂C₄O₄ and PbHPO₄, using single-crystal samples. The results show that changes in the H-ordering temperature, T_C, with pressure (or deuteration) in these systems can be largely attributed to the variation of the H-site separation, δ, with pressure (or deuteration).     

Neutron diffraction studies on La2−x Dy x Ca2xBa2Cu4+2x Oz superconductors

Structural studies on Dy-substituted La-2125 type superconductors have been carried out by neutron diffraction experiments at room temperature using a monochromatic neutron beam of wavelength (λ) = 1.249 Å. A series of samples with La_2-xDy_xCa_2xBa₂Cu_4+2xO_z stoichiometric composition, forx = 0.1–0.5, have been studied for their structural properties. A tetragonal Y-123 unit cell was taken as the starting model for the Rietveld analysis. All the samples fit into the starting model, with no structural transition taking place with increasing dopant concentration. The results of Rietveld analysis and structural properties will be discussed in detail.

     

High-pressure neutron diffraction and models of titan

Saturn's largest moon Titan is the only planetary satellite to have a significant atmosphere. The nature of this atmosphere and the origins of the ～5% of methane in it are a source of longstanding debate. The high-pressure properties of the icy components - ammonia monohydrate and methane hydrate - from which Titan formed are crucial to modelling of Titan and yet until recently were poorly known. We have now carried out neutron diffraction studies of both systems across the entire pressure and temperature range relevant to Titan. We found several new phases in ammonia monohydrate and have been able to construct an equation of state for this material. And we have shown that methane hydrate does not decompose into ice and methane at 1.2 GPa as had been calculated. These results move modelling of Titan onto new ground.     

High pressure studies at the photon factory

Abstract

The Photon Factory has unique features from the point of view of high pressure research. Six beamlines have been used for high pressure experiments, two of which were constructed as dedicated beamlines for large high pressure devices. Various kinds of high pressure studies, such as powder and single crystal x-ray diffraction and absorption experiments, have been carried out on these beamlines by more than 30 user groups, including foreign visitors. Two types of high pressure apparatuses are most frequently used. One is the large volume high pressure devices (MAX80 and MAX90) combined with high energy and/or high brightness synchrotron radiation. The other is a system combining the diamond anvil cell with a 2-dimensional detector, the IMAGE PLATE. Many improvements have been made both in the high pressure techniques and the diffraction measurement methods.

Presented at the IUCr Workshop on ‘Synchrotron Radiation Instrumentation for High Pressure Crystallography’. Daresbury Laboratory 20-21 July 1991     

Neutron diffraction studies of hydrogen-bonded ices at high pressure

Abstract

The development of the Paris-Edinburgh cell has extended the pressure range for neutron diffraction by a full order of magnitude to 30 GPa. This advance has provided a wealth of new information on the high-pressure behaviour of ices such as water-ice, ammonia, methane and hydrogen sulphide. We have now put in place technique developments to permit loading of water-gas mixtures into the Paris-Edinburgh cell.     

Neutron diffraction study of ammonium tartrate (NH4)2C4H4O6

A neutron diffraction study of ammonium tartrate has been carried out. Using the diffractometer in symmetrical setting, intensities of 750 reflections have been measured. The positions of all the hydrogen atoms have been determined. A good agreement is noticed between the present neutron and the earlier x-ray heavy atom parameters. The tartrate ion consists of two nearly identical planar halves, with an interplanar angle of 62°. Tre structure is stabilized by a net-work of hydrogen bonds. Details of hydrogen bonding and the ammonium ions environment are discussed.     

The influence of hydrogen bonds upon diffusion of simple amines and binary mixtures of ammonia

Abstract

Self diffusion coefficients of monomethylamine and trimethylamine and intradiffusion coefficients of some model mixtures containing ammonia have been measured up to pressures of 200 MPa at temperatures between the melting pressure curve and 423 K by pulsed field gradient Spin Echo NMR. Compared to water and the lower alcohols the self diffusion coefficients of pure fluid ammonia shows no clear influence from hydrogen bonds in contrast to other thermodynamic properties. Therefore the methylated substance monomethylamine has been studied to see weather a more structured charge distribution on the molecular surface compared to ammonia is needed to hinder fast rearrangements of the hydrogen bonds. For comparison also trimethylamine has been studied where no hydrogen bonds can be formed. Additionally binary mixtures of ammonia with methanol, benzene, trimethylamine and acetonitrile have been studied to see effects of intermolecular interactions.     

Exploiting optical properties of nanopolycrystalline diamond in high pressure experiments

ABSTRACT

We investigated the optical properties (absorption, luminescence and Raman spectra) of nanopolycrystalline diamond (NPD) aiming at exploring its capabilities as a pressure sensor and as a pressure-cell anvil for combined X-ray/neutron and optical studies. Notably, we analysed the Raman peak shift and broadening with pressure using a Moissanite Anvil Cell (MAC). The results are compared with those obtained in a DAC, where Raman signals from NPD chips and diamond anvils strongly overlap. Its pressure behaviour in the hydrostatic and non-hydrostatic regimes were investigated. We showed that the nanopolycrystalline structure induces remarkable differences in the peak shift and broadening between NPD and natural type IIa single-crystal diamond, making NPD suitable as pressure gauge for pressure determination and testing hydrostaticity of pressure transmitting medium.     

Dynamical and structural properties of adsorbed water molecules at the TiO2 rutile-(110) surface: interfacial hydrogen bonding probed by ab-initio molecular dynamics

ABSTRACT

Ab-initio molecular dynamics (AIMD) simulations have been carried out to study a range of different and energetically-accessible adsorbed-water configurations and motifs for their vibrational and structural characteristics, in contact with rutile-(110) interfaces at 100?K. The radial pair distribution function between the titanium atoms at the interface and the hydrogen and oxygen atoms in the water monolayer show an orientation of the water molecules parallel to the surface of titania, and with hydrogen atoms pointed in the opposite direction to the surface. In some cases, a distinctive vibrational frequency region between 2500 and 3000?cm^?1 has also been observed, due to a strong dispersion interaction between water molecules. This behaviour is also seen in experimental studies of thin-film water coverage on TiO₂ surfaces.