O. Kirichek

Cryogen-free low temperature sample environment for neutron scattering based on pulse tube refrigeration

Recent rapid progress in cryogen-free technology has become possible due to a new generation of commercial cryo-coolers developed during the last decade. The most successful example is the pulse tube refrigerator (PTR). A unique feature of the PTR is the absence of cold moving parts. This considerably reduces the generated noise and vibration and increases the reliability of the cold head, as expensive high-precision seals are no longer required and the cold head can be operated without service inspection. In this paper we present preliminary test results of a development system, based on the PTR, which provides a low temperature sample environment for neutron scattering experiments. The main aim of the development is to create a cryogen-free system suitable as a substitute for the conventional ILL-type Orange cryostat, the cryogenic workhorse of the neutron community for many years.

Absence of low temperature anomaly in the Debye-Waller factor of solid He-4

The mean-square atomic displacement in hcp-phase solid {sup 4}He has been measured in crystals with a molar volume of 21.3 cm{sup 3}. It is temperature independent from 1 K to 140 mK, with no evidence for an anomaly in the vicinity of the proposed supersolid transition. The mean-square displacement is different for in-plane motions (0.122{+-}0.001 A{sup 2}) and out-of-plane motions (0.150{+-}0.001 A{sup 2})

A high temperature cell for simultaneous electrical resistance and neutron diffraction measurements

An in situ cell that allows the electrical resistance of a sample pellet to be measured while performing neutron diffraction experiments has been developed at the ISIS pulsed neutron source. The sample is held between two spring loaded platinum electrodes embedded in a boron nitride clamp assembly with the resistance measured using the four-probe method. An outer quartz glass jacket allows the atmosphere within the sample enclosure to be controlled, and the entire device can be accommodated within a standard ISIS neutron furnace for measurements at temperatures up to 1270 K. The operation of this cell is illustrated using data for the structural, magnetic, and electrical properties of chalcopyrite CuFeS(2) collected over the temperature range of 398-873 K on the Polaris powder diffractometer at ISIS.

Bose-Einstein condensation in solid 4He.

We present neutron scattering measurements of the atomic momentum distribution n(k) in solid helium under a pressure p=41 bar (molar volume Vm=20.01+/-0.02 cm3/mol) and at temperatures between 80 and 500 mK. The aim is to determine whether there is Bose-Einstein condensation (BEC) below the critical temperature, Tc=200 mK, where a superfluid density has been observed. Assuming BEC appears as a macroscopic occupation of the k=0 state below Tc, we find a condensate fraction of n0=(-0.10+/-1.20)% at T=80 mK and n0=(0.08+/-0.78)% at T=120 mK, consistent with zero. The shape of n(k) also does not change on crossing Tc within measurement precision.

Cryogen free low temperature sample environment for neutron scattering experiments

Recent increase in liquid helium cost caused by global helium supply problems rose significant concern about affordability of conventional cryogenic equipment. Luckily the progress in cryo-cooler technology offers a new generation of cryogenic systems with significantly reduced consumption and in some cases nearly complete elimination of cryogens. These cryogen-free systems also offer the advantage of operational simplicity and require less space than conventional cryogen-cooled systems. The ISIS facility carries on an internal development program intended to substitute gradually all conventional cryogenic systems with cryogen free systems preferably based on pulse tube refrigerators. A unique feature of this cryo-cooler is the absence of cold moving parts. This considerably reduces vibrations and increases the reliability of the cold head. The program includes few development projects which are aiming to deliver range of cryogen free equipment including top-loading cryostat, superconducting magnets and dilution refrigerators. Here we are going to describe the design of these systems and discuss the results of prototypes testing.

High-pressure cell for neutron diffraction with in situ pressure control at cryogenic temperatures.

Pressure generation at cryogenic temperatures presents a problem for a wide array of experimental techniques, particularly neutron studies due to the volume of sample required. We present a novel, compact pressure cell with a large sample volume in which load is generated by a bellow. Using a supply of helium gas up to a pressure of 350 bar, a load of up to 78 kN is generated with leak-free operation. In addition, special fiber ports added to the cryogenic center stick allow for in situ pressure determination using the ruby pressure standard. Mechanical stability was assessed using finite element analysis and the dimensions of the cell have been optimized for use with standard cryogenic equipment. Load testing and on-line experiments using NaCl and BiNiO3 have been done at the WISH instrument of the ISIS pulsed neutron source to verify performance.

Strong Isotope Effects on Melting Dynamics and Ice Crystallisation Processes in Cryo Vitrification Solutions

The nucleation and growth of crystalline ice during cooling, and further crystallization processes during re-warming are considered to be key processes determining the success of low temperature storage of biological objects, as used in medical, agricultural and nature conservation applications. To avoid these problems a method, termed vitrification, is being developed to inhibit ice formation by use of high concentration of cryoprotectants and ultra-rapid cooling, but this is only successful across a limited number of biological objects and in small volume applications. This study explores physical processes of ice crystal formation in a model cryoprotective solution used previously in trials on vitrification of complex biological systems, to improve our understanding of the process and identify limiting biophysical factors. Here we present results of neutron scattering experiments which show that even if ice crystal formation has been suppressed during quench cooling, the water molecules, mobilised during warming, can crystallise as detectable ice. The crystallisation happens right after melting of the glass phase formed during quench cooling, whilst the sample is still transiting deep cryogenic temperatures. We also observe strong water isotope effects on ice crystallisation processes in the cryoprotectant mixture. In the neutron scattering experiment with a fully protiated water component, we observe ready crystallisation occurring just after the glass melting transition. On the contrary with a fully deuteriated water component, the process of crystallisation is either completely or substantially supressed. This behaviour might be explained by nuclear quantum effects in water. The strong isotope effect, observed here, may play an important role in development of new cryopreservation strategies.

IMPACT OF THE CRYOGEN FREE REVOLUTION ON NEUTRON SCATTERING LABORATORIES

A global shortage of helium gas can seriously jeopardise the scientific programmes of neutron scattering laboratories due to the use of cryogenic sample environment in the majority of the neutron scattering experiments. Recently developed cryogen-free technology allows a significant reduction or even a complete elimination of liquid helium consumption. Here we review the impact of the cryogen-free revolution on cryogenic equipment used at large neutron facilities, such as cryostats, dilution refrigerators, superconducting magnets and other cryogenic systems. Particular attention is given to the newly developed superconducting magnets for neutron diffraction and spectroscopy experiments. Use of the cryogen-free approach, as well as cutting-edge superconducting magnet technology and advanced neutron optics allows researcher to achieve extraordinary performance in their experiments, opening up new opportunities in neutron scattering research.

Hydrogen gas sample environment for TOSCA

The idea of using hydrogen as a fuel has gained immense popularity over many years. Hydrogen is abundant, can be produced from renewable resources and is not a greenhouse gas. However development of hydrogen based technology is impossible without understanding of physical and chemical processes that involve hydrogen sometime in extreme conditions such as high pressure or low and high temperatures. Neutron spectroscopy allows measurement of a hydrogen atom motion in variety of samples. Here we describe and discuss a sample environment kit developed for hydrogen gas experiment in a broad range of pressure up to 7 kbar and temperatures from 4 K to 473 K. We also describe para-hydrogen rig which produces para-hydrogen gas required for studying the rotational line of molecular hydrogen.

A non-destructive experimental investigation of elastic plastic interfaces of autofrettaged thick-walled cylindrical aluminium high pressure vessels

Positions of elastic plastic interfaces play a vital role in safe design and safe use of high pressure vessels. The ENGIN-X neutron diffractometer at the ISIS facility was used to measure the residual strain profiles in a series of aluminium vessels which had been subjected to different pressure levels. The positions of elastic plastic interfaces of the autofrettaged pressure vessels were identified. The results revealed that the residual strain magnitude and the depth of the plastic region will increase with increasing autofrettage pressure level. When autofrettage pressure produces an elastic-plastic boundary at a greater depth than the geometric mean position of the vessel wall, reverse yielding will occur, hence the loss of the vessels’ elastic ability to its subsequent loading. The neutron experimental results agreed well with both the suggestions from existing literatures and the results from FE simulations.