Small-angle polarized neutron scattering study of spherical Fe16N2 nano-particles for magnetic recording tape

We have performed small-angle polarized neutron scattering experiments of spherical Fe₁₆N₂ nano-particles, which are potential candidate materials for high density magnetic recording tape. The results were analyzed based on a core-shell model, and we evaluated the magnetic structure of the particles. The correlation between the magnetic structure and magnetic stability of the particles were discussed in terms of high density recordings.     

Characterisation of novel magnetic materials using the USANSPOL technique

USANSPOL is a novel ultra-small-angle scattering technique with polarised neutrons for investigation of magnetic materials. It represents a polarised neutron extension to traditional USANS which works with unpolarised neutrons. The high angular resolution of this technique relies on the narrow reflection width of perfect crystal reflections and is employed in a double-crystal diffractometer. Corresponding to the μrad resolution of the set-up, micro-structures of the order of a few tenths of a micrometre up to a few tens of micrometres may be investigated. Neutron polarisation is achieved by insertion of birefringent magnetic prisms between the monochromator crystal and the sample. Rocking the analyser crystal produces a scattering pattern for both neutron spin states in a single measurement but well separated in reciprocal space. By this technique, we have recently studied various amorphous Galfenol soft-magnetic ribbons which were produced by spinning from melt at different manufacturing conditions. USANSPOL allows for a determination of domain sizes of the non-magnetised samples and a study of the growing of magnetically homogeneous regions with increasing externally applied magnetic field. The manufacturing process of the ribbons is reflected in the magnetic micro-structure of the different specimens.     

A polarised neutron study of magnetic moment density in Cu2MnAl

A polarised neutron study of the ferromagnetic Heusler alloy Cu₂Mn_0.863Al_1.057 has been made. It has been concluded that the magnetic moment density is primarily situated on the Mn ions. On assigning the Mn-moment value, the observed magnetic form factor is found to be in good agreement with the Mn²⁺ free ion form factor calculated by Watson and Freeman. A slight asphericity has been observed in the moment density. It is estimated that there are about 3% excess 3d-electrons in the Eg states compared to spherical distribution. There is evidence of a very small positive polarisation of the Cu atoms. No appreciable conduction electron polarisation is found.     

Spatial modulation of a neutron beam by Larmor precession

We modulated the intensity of a neutron beam using Larmor precession techniques. We simulated triangular coils by using magnetised foils in electromagnets with rectangular pole shoes. Reversing the orientation of two of the magnetised foils in the spin-echo small-angle neutron scattering (SESANS)-instrument in Delft and changing the field settings was sufficient to obtain a modulation with a period in the order of 1 mm. We expect to be able to go to a modulation with a period of .This technique can be used to measure small-angle neutron scattering, analogous to the method used in SESANS, but with the advantage that all the manipulation of the neutron spin occurs before the sample. This means that the technique is insensitive to magnetic perturbations at the sample position. By positioning several of these devices after each other it will be possible to obtain a sharper modulation, or a modulation in two directions.     

On the magnetic structure of magnetite/oleic acid/benzene ferrofluids by small-angle neutron scattering

Magnetic small-angle scattering of non-polarized and polarized neutrons from ferrofluds (magnetite covered by oleic acid in benzene) is analyzed. A complex correlation in the magnetic structure is observed. It takes place at the length of more than the particle size, and has a core-shell-like organization. Along with it no spatial interparticle correlation in the nuclear structure is detected.     

On the possibility of using short chain length mono-carboxylic acids for stabilization of magnetic fluids

Short chain length mono-carboxylic acids (lauric and myristic acids) are used to coat magnetite nanoparticles in non-polar organic liquids, which results in highly stable magnetic fluids. The new fluids are compared with classical organic fluids stabilized by oleic acid (OA). Magnetic granulometry and small-angle neutron scattering (polarized mode) reveal a great difference in the particle size distribution function for the studied magnetic fluids, particularly a decrease in the characteristic particle radius of magnetite when lauric and myristic acids are used instead of OA.     

Contrast variation SANS experiments to the study of detergent-induced micellization of block copolymers

PEO—PPO—PEO triblock copolymer P85 [(EO)₂₆(PO)₃₉(EO)₂₆] dissolves as unimers and detergent sodium dodecyl sulfate (SDS) forms micelles in aqueous solution at 20°C. The mixing of detergent with triblock copolymer induces the micellization of triblock copolymers. Contrast variation small-angle neutron scattering measurements show that triblock copolymer forms mixed micelles with detergent and the mixing of two components in the mixed micelles is uniform.     

Combined SANS and SAXS study of the action of ultrasound on the structure of amorphous zirconia gels

In the present work, we have studied for the first time the combined effect of both sonication and precipitation pH on the structure of amorphous zirconia gels synthesized from zirconium(IV) propoxide. The techniques of small-angle neutron and X-ray scattering (SANS and SAXS) and low temperature nitrogen adsorption provided the integral data on the changes in the microstructure and mesostructure of these materials caused by ultrasonic (US) treatment. Amorphous ZrO₂·xH₂O synthesized under ultrasonic treatment was found to possess a very structured surface, characterized by the surface fractal dimension 2.9–3.0, compared to 2.3–2.5 for the non US-assisted synthesis, and it was also found to possess a higher specific surface area, while the sizes of the primary particles remain unchanged.     

Small-angle neutron scattering study of dynamically polarized polyethylenes

We carried out a small-angle neutron scattering (SANS) study of dynamically polarized polyethylene (PE) samples doped with 2,2,6,6-tetramethylpiperidine 1-oxyl (TEMPO). The transmission of the PE with almost fully polarized neutrons (98.5%) increased with increasing the proton polarization, P. The incoherent scattering cross section decreased with increasing P. The effect of P on the polarized neutrons’ transmission and the incoherent scattering cross section agreed well with the theory. The q-dependence of the coherent scattering, which reflects a two-phase structure of PE composed of crystalline and amorphous domains, was kept unchanged by the proton polarization, but the intensity increased by a factor of 3 and 6 for P=+23% and −23%, respectively. The results mean that the contrast between the two phases was successfully enhanced by a dynamic nuclear polarization (DNP) technique. However, the enhancement is only 1/13–1/16 of the enhancement calculated by assuming a homogeneous polarization through the PE sample. The discrepancy suggests that P in amorphous domains (25%) should be higher than that in crystalline domains (22%) by 3%, which in turn may suggest the partial depolarization of proton spins on the way of the spin diffusion from amorphous domains, where TEMPO radicals localize, to crystalline domains.     

Structural changes during the unfolding of Bovine serum albumin in the presence of urea: A small-angle neutron scattering study

The native form of serum albumin is the most important soluble protein in the body plasma. In order to investigate the structural changes of Bovine serum albumin (BSA) during its unfolding in the presence of urea, a small-angle neutron scattering (SANS) study was performed. The scattering curves of dilute solutions of BSA with different concentrations of urea in D₂O at pH 7.2 ± 0.2 were measured at room temperature. The scattering profile was fitted to a prolate ellipsoidal shape (a, b, b) of the protein witha = 52.2 Å andb = 24.2 Å. The change in the dimensions of the protein as it unfolds was found to be anisotropic. The radius of gyration of the compact form of the protein in solution decreased as the urea concentration was increased.     

Small-angle neutron scattering study of structural evolution of different phases in protein solution

Small-angle neutron scattering (SANS) has been used to study the structural evolution of different phases in protein solution leading to crystallization, denaturation and gelation. The protein solution under crystallization mostly consists of monomers and dimers, and higher-mers are not observed as they are perhaps formed in very small numbers. The onset and the rate of crystallization strongly depend on the salt concentration. Protein denaturation on addition of surfactant occurs due to the formation of micelle-like clusters along the unfolded polypeptide chains of the protein. The structure of such protein-surfactant complex is found to be independent of the size of the micelles in their pure surfactant solutions. The structure of temperature-induced protein gels shows a fractal structure. Rheology of these gels shows a strong dependence on varying pH or protein concentration, whereas the structure of such gels is found to be similar.      

National facility for neutron beam research

In this talk, the growth of neutron beam research (NBR) in India over the past five decades is traced beginning with research at Apsara. A range of problems in condensed matter physics could be studied at CIRUS, followed by sophisticated indegenous instrumentation and research at Dhruva. The talk ends with an overview of current scenario of NBR world-wide and future of Indian activities.     

Small-angle neutron scattering studies on water soluble complexes of poly(ethylene glycol)-based cationic random copolymer and SDS

The interaction of cationic random copolymers of methoxy poly(ethylene glycol) monomethacrylate and (3-(methacryloylamino)propyl) trimethylammonium chloride with oppositely charged surfactant, sodium dodecyl sulphate, and the influence of surfactant association on the polymer conformation have been investigated by small-angle neutron scattering. SANS data showed a positive indication of the formation of RCPSDS complexes. Even though the complete structure of the polyion complexes could not be ascertained, the results obtained give us the information on the local structure in these polymer-surfactant systems. The data were analysed using the log-normal distribution of the polydispersed spherical aggregate model for the local structure in these complexes. For all the systems the median radius and the polydispersity were found to be in the range of 20 ± 2 Å and 0.6 ± 0.05, respectively.     

Carbide precipitates in solution-quenched PH13-8 Mo stainless steel: A small-angle neutron scattering investigation

This paper deals with the small-angle neutron scattering (SANS) investigation on solution-quenched PH13-8 Mo stainless steel. From the nature of the variation of the functionality of the profiles for varying specimen thickness and also from the transmission electron microscopy (TEM), it has been established that the small-angle scattering signal predominantly originates from the block-like metallic carbide precipitates in the specimen. The contribution due to double Bragg reflection is not significant in the present case. The single scattering profile has been extracted from the experimental profiles corresponding to different values of specimen thickness. In order to avoid complexity and non-uniqueness of the multi-parameter minimization for randomly oriented polydisperse block-like precipitate model, the data have been analyzed assuming randomly oriented polydisperse cylindrical particle model with a locked aspect ratio.     

Spin chirality of polycrystalline MnSi, or, difficult way from rumours to the solid ground

Six different polycrystalline samples of MnSi were produced as a rapidly frozen melt after the single crystal growth in the Czochralski process. With the help of small-angle scattering of polarized neutrons we show that the magnetic spin chirality being scanned along the sample length oscillates strongly on a scale of 2-3 mm, revealing the volumes of the samples with high degree of an enantiomeric excess. The average chirality of the samples deviates from zero value.     

Dynamic nuclear polarization system for the SANS-J-II spectrometer at JAEA

We have developed a dynamic nuclear polarization (DNP) system for the SANS-J-II spectrometer at the JRR-3 atomic research reactor of Japan Atomic Energy Agency (JAEA). The DNP system is composed of a split-type horizontal superconducting magnet (3.3 T), a Gunn oscillator as a microwave source (94 GHz), and a cryostat (1.2 K). In particular, a sample cell with 40 in inner diameter and the magnet with a field homogeneity of 5×10⁻⁵ in a volume of 25 mm×8 mm were employed to polarize samples with a diameter of 20 mm for the ultra small-angle scattering experiment using the magnetic lens installed at the SANS-J-II spectrometer [S. Koizumi, H. Iwase, J. Suzuki, T. Oku, R. Motokawa, H. Sasao, H. Tanaka, D. Yamaguchi, H.M. Shimizu, T. Hashimoto, J. Appl. Crystallogr. 40 (2007) s474]. We obtained the proton polarization |P|=32% in the polyethylene doped with 2,2,6,6-tetra-methyl-piperidine-1-oxyl (TEMPO).     

Small-angle neutron scattering from micellar solutions

Micellar solutions are the suspension of the colloidal aggregates of the sur-factant molecules in aqueous solutions. The structure (shape and size) and the interaction of these aggregates, referred to as micelles, depend on the molecular architecture of the surfactant molecule, presence of additives and the solution conditions such as temperature, concentration etc. This paper gives the usefulness of small-angle neutron scattering to the study of micellar solutions with some of our recent results.     

Tracking the evolution of magnetic ordering in Co/Ru multilayers with inhomogeneous interlayer coupling using polarised neutron reflectometry

We report the measurement of reflected neutron intensity “hysteresis loops” from Co/Ru multilayers that have both antiferromagnetically and ferromagnetically coupled regions. We show that by measuring the four neutron spin-resolved reflectivities at a particular value of wavevector transfer, the normalised value of the relevant magnetic order parameter may be determined. The response of that order parameter to an applied magnetic field may hence be tracked. We have benchmarked our results against conventional magnetometry and magnetotransport measurements.     

Effect of substitution on aniline in inducing growth of anionic micelles

Small-angle neutron scattering (SANS) measurements were carried out on sodium dodecyl sulfate (SDS) micelles in the presence of three different hydrophobic salts, i.e. aniline hydrochloride,o-toluidine hydrochloride andm-toluidine hydrochloride. All these salts induce a uniaxial growth of micelles to form prolate ellipsoidal structures. A progressive decrease in the surface charge of the micelles was observed with the addition of salts followed by a rapid growth of the micelles. The presence of a methyl substitution at the ortho position of aniline does not alter the growth behavior significantly. However, when the substitution is at meta position micellar growth is favored at lower salt concentration than that is observed for aniline. This can be explained in terms of the difference in the chemical environments of the substituents at the ortho and meta positions.