ARTICLE IN PRESS Nuclear Instruments and Methods in Physics Research A ] (]]]]) ]]]–]]] www.elsevier.com/locate/nima Characterisation of the polarised neutron beam at the small angle scattering instrument SANS-I with a polarised proton target V.K. Aswala, B. van den Brandtb, P. Hautleb,, J. Kohlbrecherc, J.A. Konterb, A. Michelsd, F.M. Piegsab, J. Stahnc, S. Van Petegemb, O. Zimmere a Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai, India b Paul Scherrer Institut, CH-5232 Villigen PSI, Switzerland c Laboratory for Neutron Scattering, ETH Zurich & Paul Scherrer Institut, CH-5232 Villigen PSI, Switzerland d Technische Physik, Universität des Saarlandes, DE-66041 Saarbrücken, Germany e Technische Universität München, James-Franck Strasse, DE-85748, Germany Abstract A transmission neutron polariser (Fe/Si supermirror) has been successfully implemented in the small angle neutron scattering instrument SANS-I at the SINQ neutron source. The polariser is needed for investigations of magnetic nanostructures as well as for spin contrast variation techniques relying on the spin-dependent neutron scattering length of polarised nuclei. The V-shaped polariser is installed in the first section of the collimator system of the SANS instrument and its performance is optimised for neutrons with a wavelength between 0.5 and 1.0 nm. For a precise polarisation analysis of a beam with selectable incident divergence, such as in SANS experiments, an opaque spin filter is ideal. We used a solid polarised proton target exploiting the strong spin-dependent neutron scattering cross-section of hydrogen and determined the neutron beam polarisation to a precision of dp=p0:5% for different collimations in a broad wavelength band. r 2008 Elsevier B.V. All rights reserved. PACS: 61.12.Ex; 29.25.Pj; 76.70.Fz Keywords: Neutron polarisation analysis; Spin filters; Dynamic nuclear polarisation 1. Introduction Small angle scattering of a polarised neutron beam is a unique tool to investigate samples with combined magnetisation, density or compositional fluctuations which are not accessible to conventional SANS. The polarisation degree of freedom allows one to discern contributions of magnetic and nuclear scattering. It has been successfully applied, e.g. to study interfaces and surfaces of magnetic nanocrystalline materials [1]. Other fields of application are in biology and polymer chemistry where the strong spin dependent nuclear scattering of protons is exploited and a scattering contrast in hydrogenous samples is created by dynamic nuclear polarisation (DNP) [2–4]. Corresponding author. E-mail address: [email protected] (P. Hautle). A polarisation option has already been implemented at many SANS instruments. Our set up is similar to the one installed at HMI/Berlin [5], as both SANS instruments have a similar design (Fig. 1). In the following we briefly describe its components and then discuss in some detail the advantages of using a spin filter to analyse the neutron beam polarisation. The results of this characterisation show the excellent performance of the polarising device. The measurements also demonstrate the high accuracy that can be readily achieved employing a polarised proton spin filter as an analysing device. 2. Layout of the polarisation option at SANS-I The following requirements had to be met by the beam polariser: (1) the supermirror has to polarise neutrons with l40:5 nm in transmission, i.e. without changing the 0168-9002/$ - see front matter r 2008 Elsevier B.V. All rights reserved. doi:10.1016/j.nima.2007.11.062 Please cite this article as: V.K. Aswal, et al., Nucl. Instr. and Meth. A (2008), doi:10.1016/j.nima.2007.11.062 ARTICLE IN PRESS 2 V.K. Aswal et al. / Nuclear Instruments and Methods in Physics Research A ] (]]]]) ]]]–]]] Fig. 1. Sketch of the polarisation option at SANS-I. The polarising cavity is located inside a neutron guide (not shown) within the first exchangeable segment of the collimator. direction of the beam incident on the SANS instrument, (2) it should be removable for experiments requiring an unpolarised beam and (3) placed far away from the sample position to suppress parasitic scattering from the polariser itself. We therefore decided to install a polarising cavity in the first exchangeable collimation section, following a design of Mezei [5,6]. This reduces to 15 m the longest collimation distance possible for polarised neutrons. Since magnets could not be installed within the collimation tube, a supermirror coating requiring a rather weak magnetization field was favoured. Due to its low absorption and high magnetic remanence an Fe/Si supermirror (SM) coating [7,8] on Si substrate was selected. The polariser has a V-shape to reduce its overall length. Nevertheless, due to the size of the neutron guide of 50 50 mm2 into which the polariser had to be fitted, and even using a coating with m ¼ 2:6, a length of 2 m was still needed to cover the wavelength range between 0.5 and 1.0 nm. On the 15 m flight path between polariser and sample a small magnetic guide field of about 1–2 mT has to be applied to preserve the neutron polarisation. Such a small field is easily produced by iron plates magnetized by FeNdB permanent magnets. The layout of the beamline is sketched in Fig. 1. The wavelength range of the polarising cavity is limited by the fixed mean angle of incidence of the beam upon the supermirror. Since the Fe/Si coating (and the Si wafer substrate) reflects both spin states below the critical momentum transfer on pure Si, the transmittance of the device goes down for long wavelengths. The measured data shown in Fig. 2 illustrate this effect. On the other hand both spin states will be transmitted above the critical momentum transfer of the supermirror coating. This takes effect first for the neutrons with the largest angle of incidence. If these are filtered afterwards by a strong collimation, the polarisation can be kept high. Thus, a wavelength- and collimation dependence of the efficiency of the device might be expected and was actually measured (see Fig. 4). In principle the supermirror coatings chosen would allow to switch the polarisation just by inverting the magnetization direction with respect to the applied magnetic field. However, this results in slightly different transmitted Fig. 2. Transmittance of the Fe/Si supermirror neutron polariser in comparison to the piece of neutron guide installed for unpolarised beam measurements. The measurement error is smaller than 2%. Fig. 3. Schematic drawing of the spin flipper setup with (1) the gradient field, (2) the radio-frequency solenoid, (3) the magnetic shielding box and (4) the magnetic guiding field. intensities, due to increased small angle scattering in one state. For this reason an adiabatic radio frequency spin flipper (see, e.g. Ref. [9]) was installed within a magnetic shielding at the end of the collimation section, about 1.5 m in front of the sample position. A schematic drawing is shown in Fig. 3. A static field transverse to the beam is Please cite this article as: V.K. Aswal, et al., Nucl. Instr. and Meth. A (2008), doi:10.1016/j.nima.2007.11.062 ARTICLE IN PRESS V.K. Aswal et al. / Nuclear Instruments and Methods in Physics Research A ] (]]]]) ]]]–]]] 3 produced by a wedge shaped iron yoke, with magnitude 9 mT in the center of the spin flipper, and with a gradient of 0:3 mT cm1 along the beam. The oscillating field amplitude of 1.8 mT is produced by a solenoid. Its frequency (260 kHz) is chosen to meet the resonance condition for the neutron magnetic moment in the center of the gradient field. The theoretically expected spin-flip probability is better than 0.999 for neutrons with wavelength above 0.5 nm [10]. In order to shield the spin flipper from external fields, e.g. stray fields from magnets of the sample environment, it is placed in a double walled iron box. Tests performed in combination with a spin analysing bender indicate that the flipper has indeed an efficiency very close to 1. in the present application, a smooth transition to a lower value that stays practically constant from 200 meV up to the sub-MeV region. A detailed study comparing the three methods (supermirrors, 3He, protons) for cold neutrons has shown the principle advantages of spin filters for high precision neutron polarimetry [14,15]. 3. Neutron spin filters where the þ and the stand for the two eigenstates of the neutron spin with respect to the target’s polarisation axis. The part depending on the neutron spin is the product of the ‘‘polarisation cross-section’’ sp and the nuclear polarisation P. s0 denotes the neutron spin-independent cross-section. The exponential attenuation factors expðs NdÞ for the respective beam polarisation components lead to a filter analysing power A (defined here as positive to avoid confusion with signs), Supermirror type polarisers, which rely on spin-dependent neutron optical reflection, are very popular for neutron beam polarisation and analysis of scattered neutrons. They are easy to set up and use, have a high polarising efficiency for cold and thermal neutrons and need no maintenance. However, if high accuracy is requested for polarisation analysis, the spin- and momentum-transfer-dependent analysing efficiency and transmission of such instruments leads to systematic limitations. Neutron spin filters on the other hand rely on spindependent nuclear scattering, e.g. on polarised protons [11], or absorption on polarised 3He [12]. They can polarise the whole range of cold, thermal and hot neutrons. With the advent of strong pulsed neutron spallation sources this property becomes crucial since time-of-flight information can be employed to analyse all wavelengths in a single experiment. More important for the present purpose, the analysing power and transmission of a homogeneous spin filter with parallel entrance and exit windows perpendicular to the beam are practically independent on the beam divergence. For a typical value of some 10 mrad the relative difference of neutron flight paths through the spin filter has negligible influence on the neutron polarisation analysis. The spin filter of optically polarised 3He has become very popular at several neutron research centers. Filter cells suited to polarise wide beams are available. A comprehensive overview of the current state-of-the-art can be found in Ref. [13]. The strong energy dependence of the absorption cross-section makes it however difficult to optimise the filter thickness if a large neutron energy range is to be used in the experiment. On the other hand, hydrogenous materials with dynamically polarised protons offer an attractive alternative for a broadband spin filter, as realised and demonstrated already long ago [11]. The singlet crosssection for slow neutrons is more than twenty times higher than the triplet cross-section; neutrons polarised antiparallel to the protons will thus be much stronger scattered in 4p solid angle than those with polarisation parallel. The large scattering cross-section has very little energy dependence below 20 meV and shows, however not of relevance 4. Opaque spin filter polarisation analysis of the SANS-I neutron beam A spin filter may be characterised by its thickness d, the number density N of the polarised nuclei and by a spindependent effective cross-section s ¼ s0 sp P A ¼ j tanhðsp PNdÞj. (1) (2) A simple way to determine an unknown neutron beam polarisation p employs a single analyser with known analysing power A. One measures a ‘‘flipping ratio’’ Rðp; A; f Þ ¼ N 0 =N 1 of two count rates with an inactive, respectively, active spin flipper with efficiency f, situated between polariser and analyser. The accuracy of the polarisation analysis is limited by the knowledge of A and f. Whereas it is difficult to characterise the analysing power A of a single supermirror analyser, for a spin filter one may choose the value of the opacity x ¼ sp PNd sufficiently large and thereby approximate an ideal analyser with A ! 1 (opaque spin filter). As demonstrated in Ref. [14], already a modest knowledge of the actual filter parameters results in a precise knowledge of A, the corresponding uncertainties being related by dA 2x dx ¼ . A sinhð2xÞ x (3) On the other hand, the closer A is to unity, the smaller the transmission becomes. Hence, using the freedom in the choice of x, there is a tradeoff between the systematic uncertainty of A and the time required to reach the corresponding counting statistical uncertainty. As pointed out in Ref. [16], the free choice of the polarisation direction of a dynamically polarised nuclear target can be employed to measure two different flipping ratios with the opaque spin filter either polarised parallel or antiparallel to the polarising direction of the beam. One ratio is almost insensitive to the flipper efficiency. As a result one can easily determine f from only four neutron count rates. A first experimental demonstration of this Please cite this article as: V.K. Aswal, et al., Nucl. Instr. and Meth. A (2008), doi:10.1016/j.nima.2007.11.062 ARTICLE IN PRESS V.K. Aswal et al. / Nuclear Instruments and Methods in Physics Research A ] (]]]]) ]]]–]]] 4 14.5 m was chosen to achieve a precision for the neutron polarisation measurement of dp=p5 103 within reasonable time. In about 2 h the necessary statistics was accumulated for one polarisation orientation and for four different wavelengths. In order to determine the second count rate appearing in the ratio (4), the direction of the proton polarisation was reversed by DNP within a few minutes. The whole procedure was performed for several collimation lengths and the results are shown in Fig. 4. 5. Conclusion Fig. 4. Polarisation of the neutron beam at SANS-I at SINQ for different collimation lengths. For clarity the measurement error is shown for one data set only. The polariser was designed to reach a polarisation 497% for l40:5 nm for all collimations. The decay for smaller l is due to the transmission of both spin states above the critical momentum transfer, starting with the neutrons with a large angle of incidence. This explains the collimation dependence. method was published in Ref. [17]. In the present study, the spin flipper was not yet available, and therefore we decided to determine the beam polarisation simply from the ratio of count rates with an opaque spin filter polarised parallel and antiparallel to the neutron beam, respectively. This ratio is given by R¼ N þ T þ 1 þ pAþ coshðsp Pþ NdÞ 1 þ p ¼ N T 1 pA coshðsp P NdÞ 1 p (4) where Aþ and A are the analysing powers for the ‘‘bright’’ and the ‘‘dark’’ state of the opaque analyser, and T þ and T are corresponding transmission factors. Since the nuclear polarisation in the two states, Pþ and P , may be different, Aþ and A may possess different numerical values. However, they are close to unity in the opaque spin filter limit. Note that the ratio of transmission factors appears here as a consequence of not using a neutron spin flipper. However, choosing Pþ P , which requires only simple relative NMR measurements during DNP, their uncertainty does not dominate the final accuracy attained in the present study. For the polarisation analysis of the neutron beam of SANS-I we employed a polarised target system previously used for a series of spin contrast variation experiments. It is described in Ref. [18]. The protons contained in frozen 1,2propanediol (with N ¼ 6:7 1022 cm3 ) doped with CrV complexes (1020 cm3 ) were polarised by dynamic nuclear polarisation [19] at a temperature of 1 K in a magnetic field of 3.5 T to about 42%. The polarisation cross-section of this material was determined previously [17] and is sp ðlÞX51 1024 cm2 in the wavelength range l40:2 nm. A beam 1 mm wide and 10 mm high was defined by a cadmium aperture close to the target, which was a frozen platelet with cross-section 4:5 16 mm2 . 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