Lowell Crow

The IMAGINE instrument: first neutron protein structure and new capabilities for neutron macromolecular crystallography.

The first high-resolution neutron protein structure of perdeuterated rubredoxin from Pyrococcus furiosus (PfRd) determined using the new IMAGINE macromolecular neutron crystallography instrument at the Oak Ridge National Laboratory is reported. Neutron diffraction data extending to 1.65 Å resolution were collected from a relatively small 0.7 mm(3) PfRd crystal using 2.5 d (60 h) of beam time. The refined structure contains 371 out of 391, or 95%, of the D atoms of the protein and 58 solvent molecules. The IMAGINE instrument is designed to provide neutron data at or near atomic resolution (1.5 Å) from crystals with volume <1.0 mm(3) and with unit-cell edges <100 Å. Beamline features include novel elliptical focusing mirrors that deliver neutrons into a 2.0 × 3.2 mm focal spot at the sample position with full-width vertical and horizontal divergences of 0.5 and 0.6°, respectively. Variable short- and long-wavelength cutoff optics provide automated exchange between multiple-wavelength configurations (λmin = 2.0, 2.8, 3.3 Å to λmax = 3.0, 4.0, 4.5, ∼20 Å). These optics produce a more than 20-fold increase in the flux density at the sample and should help to enable more routine collection of high-resolution data from submillimetre-cubed crystals. Notably, the crystal used to collect these PfRd data was 5-10 times smaller than those previously reported.

Transmission Bragg edge spectroscopy measurements at ORNL Spallation Neutron Source

Results of neutron transmission Bragg edge spectroscopic experiments performed at the SNAP beamline of the Spallation Neutron Source are presented. A high resolution neutron counting detector with a neutron sensitive microchannel plate and Timepix ASIC readout is capable of energy resolved two dimensional mapping of neutron transmission with spatial accuracy of ~55 μm, limited by the readout pixel size, and energy resolution limited by the duration of the initial neutron pulse. A two dimensional map of the Fe 110 Bragg edge position was obtained for a bent steel screw sample. Although the neutron pulse duration corresponded to ~30 mA energy resolution for 15.3 m flight path, the accuracy of the Bragg edge position in our measurements was improved by analytical fitting to a few mA level. A two dimensional strain map was calculated from measured Bragg edge values with an accuracy of ~few hundreds μistrain for 300s of data acquisition time.

Demonstration of a novel focusing small-angle neutron scattering instrument equipped with axisymmetric mirrors

Small-angle neutron scattering (SANS) is the most significant neutron technique in terms of impact on science and engineering. However, the basic design of SANS facilities has not changed since the techniques inception about 40 years ago, as all SANS instruments, save a few, are still designed as pinhole cameras. Here we demonstrate a novel concept for a SANS instrument based on axisymmetric focusing mirrors. We build and test a small prototype, which shows a performance comparable to that of conventional large SANS facilities. By using a detector with 48-μm pixels, we build the most compact SANS instrument in the world. This work, together with the recent demonstration that such mirrors could increase the signal rate at least 50-fold, for large samples, while improving resolution, paves the way to novel SANS instruments, thus affecting a broad community of scientists and engineers.

In-situ Polarized 3He system for the Magnetism Reflectometer at the Spallation Neutron Source

We report on the in situ polarized (3)He neutron polarization analyzer developed for the time-of-flight Magnetism Reflectometer at the Spallation Neutron Source at Oak Ridge National Laboratory. Using the spin exchange optical pumping method, we achieved a (3)He polarization of 76% ± 1% and maintained it for the entire three-day duration of the test experiment. Based on transmission measurements with unpolarized neutrons, we show that the average analyzing efficiency of the (3)He system is 98% for the neutron wavelength band of 2-5 Å. Using a highly polarized incident neutron beam produced by a supermirror bender polarizer, we obtained a flipping ratio of >100 with a transmission of 25% for polarized neutrons, averaged over the wavelength band of 2-5 Å. After the cell was depolarized for transmission measurements, it was reproducibly polarized and this performance was maintained for three weeks. A high quality polarization analysis experiment was performed on a reference sample of Fe/Cr multilayer with strong spin-flip off-specular scattering. Using a combination of the position sensitive detector, time-of-flight method, and the excellent parameters of the (3)He cell, the polarization analysis of the two-dimensional maps of reflected, refracted, and off-specular scattered intensity above and below the horizon were obtained, simultaneously.

From X-Ray Telescopes to Neutron Focusing

In the case of neutrons the refractive index is slightly less than unity for most elements and their isotopes [1]. Consequently, thermal and cold neutrons can be reflected from smooth surfaces at grazing-incidence angles. Hence, the optical technologies developed for x-ray astronomy can be applied for neutron focusing. The focusing capabilities of grazing incidence neutron imaging optics have been successfully demonstrated using nickel mirrors. The mirrors were fabricated using an electroformed nickel replication process at Marshall Space Flight Center. Results of the neutron optics experiments and current status of the multilayer coating replication technique development are presented.

High efficiency angular selective detection of thermal and cold neutrons

We present a new neutron detection technology capable of high efficiency detection of thermal and cold neutrons with high spatial resolution. It is based on neutron-sensitive microchannel plates (MCPs) converting incident neutrons to electrons, which are then amplified and detected by a variety of different position sensitive readouts. The detection efficiency of those detectors can exceed 50% for thermal neutrons, while the spatial resolution can be better than 20 μm FWHM. Another attractive feature is the capability to time-stamp each incoming neutron with ~microsecond resolution, allowing energy/material resolved studies with pulsed neutron sources. The MCP-based neutron detectors can also be combined with novel MCP-based neuron optics, allowing high resolution angular selective neutron imaging.

High resolution neutron Larmor diffraction using superconducting magnetic Wollaston prisms

The neutron Larmor diffraction technique has been implemented using superconducting magnetic Wollaston prisms in both single-arm and double-arm configurations. Successful measurements of the coefficient of thermal expansion of a single-crystal copper sample demonstrates that the method works as expected. The experiment involves a new method of tuning by varying the magnetic field configurations in the device and the tuning results agree well with previous measurements. The difference between single-arm and double-arm configurations has been investigated experimentally. We conclude that this measurement benchmarks the applications of magnetic Wollaston prisms in Larmor diffraction and shows in principle that the setup can be used for inelastic phonon line-width measurements. The achievable resolution for Larmor diffraction is comparable to that using Neutron Resonance Spin Echo (NRSE) coils. The use of superconducting materials in the prisms allows high neutron polarization and transmission efficiency to be achieved.

A neutron sensitive microchannel plate detector with cross delay line readout

Microchannel plates containing neutron absorbing elements such as boron and gadolinium in the bulk glass are used as the sensing element in high spatial resolution, high rate neutron imaging systems. In this paper we describe one such device, using both 10B and natural Gd, which employs cross delay line signal readout, with time-of-flight capability. This detector has a measured spatial resolution under 40 μm FWHM, thermal neutron efficiency of 19%, and has recorded rates in excess of 500 kHz. A physical and functional description is presented, followed by a discussion of measurements of detector performance and a brief survey of some practical applications.

Neutron intensity modulation and time-focusing with integrated Larmor and resonant frequency techniques

The analysis of neutron diffraction experiments often assumes that neutrons are elastically scattered from the sample. However, there is growing evidence that a significant fraction of the detected neutrons is in fact inelastically scattered, especially from soft materials and aqueous samples. Ignoring these inelastic contributions gives rise to inaccurate experimental results. To date, there has been no simple method with broad applicability for inelastic signal separation in neutron diffraction experiments. Here, we present a simple and robust method that we believe could be suited for this purpose. We use two radio frequency resonant spin flippers integrated with a Larmor precession field to modulate the neutron intensity and to encode the inelastic scattering information into the neutron data. All three components contribute to the spin encoding. The Larmor field serves several additional purposes. Its usage facilitates neutron time-focusing, eliminates the need for stringent magnetic shielding, and allows for compact setups. The scheme is robust, simple, and flexible. We believe that, with further improvements, it has the potential of adding inelastic signal discrimination capabilities to many existing diffraction instruments in the future.

A High Count Rate Neutron Beam Monitor for Neutron Scattering Facilities

Beam monitors are an important diagnostic tool in neutron science facilities. Present beam monitors use either ionization chambers in integration mode, which are slow and have no timing information, or pulse counters which can easily be saturated by high beam intensities. At high flux neutron scattering facilities, neutron beam monitors with very low intrinsic efficiency (10-5) are presently selected to keep the counting rate within a feasible range, even when a higher efficiency would improve the counting statistics and yield a better measurement of the incident beam. In this work, we report on a high count rate neutron beam monitor. This beam monitor offers good timing with an intrinsic efficiency of 10-3 and a counting rate capability of over 1,000,000 cps without saturation.