A high pressure cell for small angle neutron scattering up to 500 MPa in combination with light scattering to investigate liquid samples

We report on a high pressure cell to use with small angle neutron scattering (SANS) in a pressure range up to 500 MPa. The cell offers the new possibility to investigate liquid samples by a specially designed sample chamber, which allows changing of samples relatively easily. Since the cell construction uses sapphire as window material, also light scattering investigations can be performed simultaneously to the SANS measurements. In this article we describe the construction of a high pressure cell and we demonstrate the applicability of the construction for SANS in combination with dynamic light scattering showing data on the biological molecule lysozyme.     

Pressure cell for investigations of solid-liquid interfaces by neutron reflectivity

We describe an apparatus for measuring scattering length density and structure of molecular layers at planar solid-liquid interfaces under high hydrostatic pressure conditions. The device is designed for in situ characterizations utilizing neutron reflectometry in the pressure range 0.1-100 MPa at temperatures between 5 and 60?°C. The pressure cell is constructed such that stratified molecular layers on crystalline substrates of silicon, quartz, or sapphire with a surface area of 28 cm(2) can be investigated against noncorrosive liquid phases. The large substrate surface area enables reflectivity to be measured down to 10(-5) (without background correction) and thus facilitates determination of the scattering length density profile across the interface as a function of applied load. Our current interest is on the stability of oligolamellar lipid coatings on silicon surfaces against aqueous phases as a function of applied hydrostatic pressure and temperature but the device can also be employed to probe the structure of any other solid-liquid interface.     

Development of a variable temperature mechanical loading device for in situ neutron scattering measurements

Understanding the phase transformation and failure mechanism of NiTi shape memory alloys under variable environments of high and low temperatures is critical to the establishment of constitutive properties and to the realization of controllable design. Information regarding the correlation between the phase transformation and deformation can be obtained by in situ neutron scattering measurements. Therefore, a variable temperature mechanical loading device is designed, which can be used for mechanical loading and in situ neutron scattering measurements in a variable temperature environment. Specifically, the device can achieve precise temperature control with a temperature change from −55 °C to 200 °C in a protective atmosphere. The rated load in the axial direction is 6 kN, and the maximum displacement of the unilateral grip is larger than 30 mm. In situ neutron scattering measurements can be performed through neutron windows, and the strain can be measured by digital image correlation technology. Moreover, the force sensor is calibrated to improve test precision. Through an evaluation of temperature uncertainty, the temperature measurement performance is estimated. Tensile tests of the NiTi alloy at variable temperatures are carried out, and preliminary results are given. The four deformation stages of the NiTi alloy can be seen from the stressstrain curve, which corresponds to the existing results. This demonstrates that the designed variable temperature mechanical loading device can supply the testing demands. The device provides a new way to study the relationship between the phase transformation and mechanical properties of NiTi shape memory alloys at variable temperatures.

     

A furnace with rotating load frame for in situ high temperature deformation and creep experiments in a neutron diffraction beam line

A resistive furnace combined with a load frame was built that allows for in situ neutron diffraction studies of high temperature deformation, in particular, creep. A maximum force of 2700 N can be applied at temperatures up to 1000 °C. A load control mode permits studies of, e.g., creep or phase transformations under applied uni-axial stress. In position control, a range of high temperature deformation experiments can be achieved. The examined specimen can be rotated up to 80° around the vertical compression axis allowing texture measurements in the neutron time-of-flight diffractometer HIPPO (High Pressure - Preferred Orientation). We present results from the successful commissioning, deforming a Zr-2.5 wt.% Nb cylinder at 975 °C. The device is now available for the user program of the HIPPO diffractometer at the LANSCE (Los Alamos Neutron Science Center) user facility.     

Continuous flow time-resolved small-angle x-ray scattering and X-ray absorption spectroscopy

A continuous flow device to characterize the growth of nanometer particles was assembled. In-situ millisecond or second-order time-resolved small angle x-ray scattering and x-ray absorption spectroscopy was performed using this device at the Beijing Synchrotron Radiation Facility. The time resolution was adjusted from 10 ms to 1.0 s by changing the flow rate of the solution. The temperature was variable from 5–95°C. Custom-designed pulse eliminators were employed to eliminate adverse pump fluctuations and improve the quality of measurements. The system was used to characterize zinc sulfide nanoparticles by small angle x-ray scattering and x-ray absorption spectroscopy.     

Extensional rheometer for in situ x-ray scattering study on flow-induced crystallization of polymer

We designed and constructed an extensional rheometer for in situ small and wide angle x-ray study on flow-induced crystallization of polymer. Two rotating drums with an axis distance of 20 mm are employed to impose extensional deformation on the samples. With a constant angular velocity, the two drums generate a constant Henkcy strain rate as sample length for testing keeps constant during deformation. An ionic liquid is used as heating medium to prevent polymer melt from bending downward due to gravity, which is excellent in terms of high thermal stability, low viscosity, and relative low adsorption on x-ray. Flow-induced crystallization experiments are conducted with this apparatus on x-ray scattering station in Shanghai Synchrotron Radiation Facility (SSRF), which allows us to collect rheological and structural data simultaneously and may lead to a better understanding on flow-induced crystallization of polymer.     

Environmental chamber for in situ dynamic control of temperature and relative humidity during x-ray scattering

We have designed, constructed, and evaluated an environmental chamber that has in situ dynamic control of temperature (25 to 90?°C) and relative humidity (0% to 95%). The compact specimen chamber is designed for x-ray scattering in transmission with an escape angle of 2θ = ±30°. The specimen chamber is compatible with a completely evacuated system such as the Rigaku PSAXS system, in which the specimen chamber is placed inside a larger evacuated chamber (flight path). It is also compatible with x-ray systems consisting of evacuated flight tubes separated by small air gaps for sample placement. When attached to a linear motor (vertical displacement), the environmental chamber can access multiple sample positions. The temperature and relative humidity inside the specimen chamber are controlled by passing a mixture of dry and saturated gas through the chamber and by heating the chamber walls. Alternatively, the chamber can be used to control the gaseous environment without humidity. To illustrate the value of this apparatus, we have probed morphology transformations in Nafion(?) membranes and a polymerized ionic liquid as a function of relative humidity in nitrogen.     

SANS准直器的蒙特卡罗模拟

本文采用基于蒙特卡罗方法的谱仪设计软件VITESS,对中子小角散射谱仪上三种不同形状的准直器进行了模拟。比较了这三种不同准直器在输入条件相同的情况下,它们出口处的中子注量率、水平面和竖直面的中子角分布。通过分析,采用具有超镜因子m=1．5的bender类型的准直器可以获得较高的中子注量率,但是其水平面角分布相对其它两种稍微偏大。这为中子小角散射谱仪设计中准直器的选择提供了一个参考。     

Magnetic compound refractive lens for focusing and polarizing cold neutron beams

Biconcave cylindrical lenses are used to focus beams of x rays or neutrons using the refractive properties of matter. In the case of neutrons, the refractive properties of magnetic induction can similarly focus and simultaneously polarize the neutron beam without the concomitant attenuation of matter. This concept of a magnetic refractive lens was tested using a compound lens consisting of 99 pairs of cylindrical permanent magnets. The assembly successfully focused the intensity of a white beam of cold neutrons of one spin state at the detector, while defocusing the other. This experiment confirmed that a lens of this nature may boost the intensity locally by almost an order of magnitude and create a polarized beam. An estimate of the performance of a more practically dimensioned device suitable for incorporation in reflectometers and slit-geometry small angle scattering instruments is given.     

Construction and testing of the instrument for neutron holographic study at the Budapest Research Reactor

Neutron scattering device dedicated to neutron holography experiments is described. The device is operating at a constant wavelength prepared by a double focusing monochromator. It is equipped by highly efficient shielding, proper collimator, Eulerian cradle, monitor detector, gamma-ray, and neutron detectors as well. Relevant software serves as control for the measurement and data collection. The harmonized application of the components enumerated above makes our device extremely efficient and unparalleled. Two atomic resolution neutron holographic experiments carried out illustrate the efficiency and power of the instrument.     

Large volume high-pressure cell for inelastic neutron scattering

Inelastic neutron scattering measurements typically require two orders of magnitude longer data collection times and larger sample sizes than neutron diffraction studies. Inelastic neutron scattering measurements on pressurised samples are particularly challenging since standard high-pressure apparatus restricts sample volume, attenuates the incident and scattered beams, and contributes background scattering. Here, we present the design of a large volume two-layered piston-cylinder pressure cell with optimised transmission for inelastic neutron scattering experiments. The design and the materials selected for the construction of the cell enable its safe use to a pressure of 1.8 GPa with a sample volume in excess of 400 mm(3). The design of the piston seal eliminates the need for a sample container, thus providing a larger sample volume and reduced absorption. The integrated electrical plug with a manganin pressure gauge offers an accurate measurement of pressure over the whole range of operational temperatures. The performance of the cell is demonstrated by an inelastic neutron scattering study of UGe(2).     

Development and application of setup for ac magnetic field in neutron scattering experiments

We report on a new setup developed for neutron scattering experiments in periodically alternating magnetic fields at the sample position. The assembly consisting of rf generator, amplifier, wide band transformer, and resonance circuit. It allows to generate homogeneous ac magnetic fields over a volume of a few cm(3) and variable within a wide range of amplitudes and frequencies. The applicability of the device is exemplified by ac polarized neutron reflectometry (PNR): a new method established to probe remagnetization kinetics in soft ferromagnetic films. Test experiments with iron films demonstrate that the ac field within the accessible range of frequencies and amplitudes produces a dramatic effect on the PNR signal. This shows that the relevant ac field parameters generated by the device match well with the scales involved in the remagnetization processes. Other possible applications of the rf unit are briefly discussed.     

Angular correlations in detection of α-γ coincidences in the nanosecond tagged neutron technology

The characteristics of the setup for analyzing the elemental composition of organic substances using spectroscopy of γ rays induced by tagged neutrons with an energy of ～14 MeV in an inelastic neutron scattering reaction are discussed. An ING-27 D-T neutron generator with a built-in position-sensitive α detector, fast neutron and γ detectors, and a multichannel detecting system providing a subnanosecond time resolution are parts of the experimental setup. The correlation between the exit angle of a neutron and the number of the α pixel, as well as the anisotropy in emission of γ rays in the inelastic neutron scattering reaction, are measured, and the errors of these measurements are estimated.     

The new cold neutron chopper spectrometer at the Spallation Neutron Source: design and performance

The design and performance of the new cold neutron chopper spectrometer (CNCS) at the Spallation Neutron Source in Oak Ridge are described. CNCS is a direct-geometry inelastic time-of-flight spectrometer, designed essentially to cover the same energy and momentum transfer ranges as IN5 at ILL, LET at ISIS, DCS at NIST, TOFTOF at FRM-II, AMATERAS at J-PARC, PHAROS at LANSCE, and NEAT at HZB, at similar energy resolution. Measured values of key figures such as neutron flux at sample position and energy resolution are compared between measurements and ray tracing Monte Carlo simulations, and good agreement (better than 20% of absolute numbers) has been achieved. The instrument performs very well in the cold and thermal neutron energy ranges, and promises to become a workhorse for the neutron scattering community for quasielastic and inelastic scattering experiments.     

Thermoelectric temperature control device for vapor pressure measurements

The static method of measuring equilibrium vapor pressure requires locating the sample at the coldest part of the apparatus to avoid errors due to evaporation and recondensation elsewhere. This paper describes a device that can hold the sample 1 K below the temperature of the surrounding air without a liquid bath. It comprises a pair of thermoelectric elements and two thermometers attached to an insulated aluminum block. The device can operate as high as 200?°C while controlling the sample with a precision of 0.02 K; below 110?°C, the precision is 2 mK. Also described is a method to measure the small temperature offset due to heat flow between the sample and the surrounding aluminum block. The uncertainty due to the offset is small compared to the 6 mK uncertainty due to the thermometer.     

Experimental and theoretical evidence for the magic angle in transmission electron energy loss spectroscopy

We present experimental measurements of the C K-ELNES of high temperature pyrolysed graphite and related crystalline materials as a function of collection angle and sample tilt. These results together with a corresponding theoretical analysis indicate that the so-called "magic angle" for EELS measurements of an anisotropic crystal such as graphite, where spectra are independent of sample orientation, is approximately two times the characteristic scattering angle. We briefly discuss the implications of this result for the experimental measurement of anisotropic structures, including interfaces, as well as for the detailed modelling of ELNES structures using advanced electronic structure calculations.     

A versatile automated sample changer for texture measurements on the high pressure-preferred orientation neutron diffractometer

An automated sample changer with an Eulerian cradle for neutron texture measurements is described. This device has been measuring over 2300 texture and almost 400 powder samples at ambient conditions since it became operational in 2002 for use in the high pressure-preferred orientation diffractometer at the LANSCE neutron scattering facility. Operation for almost a decade resulted in sustained enhancements of mechanics, electronics, and software which significantly improved reliability and resiliency. We also describe in this paper our platform independent computer program POD2K which we use to create publication quality pole figure plots for texture samples.     

A new device for performing reference point indentation without a reference probe

Here we describe a novel, hand-held reference point indentation (RPI), instrument that is designed for clinical measurements of bone material properties in living patients. This instrument differs from previous RPI instruments in that it requires neither a reference probe nor removal of the periosteum that covers the bone, thus significantly simplifying its use in patient testing. After describing the instrument, we discuss five guidelines for optimal and reproducible results. These are: (1) the angle between the normal to the surface and the axis of the instrument should be less than 10°, (2) the compression of the main spring to trigger the device must be performed slowly (>1 s), (3) the probe tip should be sharper than 10 μm; however, a normalized parameter with a calibration phantom can correct for dull tips up to a 100 μm radius, (4) the ambient room temperature should be between 4?°C and 37 °C, and (5) the effective mass of the bone or material under test must exceed 1 kg, or if under 1 kg, the specimen should be securely anchored in a fixation device with sufficient mass (which is not a requirement of previous RPI instruments). Our experience is that a person can be trained with these guidelines in about 5 min and thereafter obtain accurate and reproducible results. The portability, ease of use, and minimal training make this instrument suitable to measure bone material properties in a clinical setting.     

磁流变胶泥流变学特性测试装置研究

现有的商用磁流变仪不能满足磁流变胶泥高剪切率和高剪切应力测试的要求,对比设计了密闭圆筒剪切模式的磁流变胶泥流变特性测试装置。在完成总体结构设计的基础上,建立了剪切通道励磁磁路的分析模型,得出了剪切通道磁场强度与励磁电流的关系,并进行了有限元仿真验证。考虑转子与外筒存在倾斜,建立了磁流变胶泥转矩传递的力学模型,得到了转子与外筒倾斜角度与传递转矩误差的理论关系。完成了测量装置样机的制作,开展了磁流变胶泥流变学特性测试,在低剪切率下测量装置测试结果与安东帕流变仪测试结果能较好吻合。研究表明,测试装置能够实现25 000 s-1的高剪切率和200 k Pa的高剪切应力测试。     

Characterisation of the early stages of solute clustering in 1Ni–1.3Mn welds containing Cu

Microstructural characterisation of neutron irradiated low alloy steels is important for developing mechanistic understanding of irradiation embrittlement. This work is focused on the early stages of irradiation-induced clustering in a low Cu (0.03 wt%), high Ni (∼1 wt%) weld. The weld was irradiated at a very high dose rate and then examined by atom probe (energy-compensated position-sensitive atom probe (ECOPoSAP) and local electrode atom probe (LEAP)) with supporting microstructural information obtained by small angle neutron scattering (SANS) and positron annihilation (PALA).