Investigation of a magnetic phase transition in fcc iron-nickel alloys

A magnetic phase transition in carbon-doped (0.1 and 0.7 at. %) Fe₇₀Ni₃₀ Invar alloys was investigated by the method of depolarization of a transmitted neutron beam and by small-angle scattering of polarized neutrons. It is shown that for both alloys, two characteristic length scales of magnetic correlations coexist above T _c. Small-angle scattering by critical correlations with radius R _c is described well by the Ornstein-Zernike (OZ) expression. The longer-scale (second) correlations, whose size can be estimated from depolarization data, are not described by the OZ expression, and hypothetically can be modeled by a squared OZ expression, which in coordinate space corresponds to the relation 〈M(r)M(0)〉∝exp(−r/R _d), where R _d is the correlation length of the second scale. The temperature dependence of the correlation radius R _c was obtained: R _c ∝ ((T−T _c)/Tc)^−ν , where ν≈2/3 is the critical exponent for ferromagnets, over a wide temperature range up to T _c ^exp , at which the correlation radius becomes constant and equals its maximum value R _c(T _c)=R _c ^max . The maximum correlation radius established (R _c ^max =140 Å and 230 Å for the first and second alloys, respectively) characterizes the length-scale of the fluctuation for which the appearance of critical correlations first results in the formation of a ferromagnetic phase, and the phenomenon itself exhibits a “disruption” of the second-order phase transition at T=T _c ^exp , as a result of which a first-order transition arises. Temperature hysteresis was also detected in the measured polarization of the transmitted beam and intensity of small-angle neutron scattering in the alloy above T _c, confirming the character of this magnetic transition as a first-order transition close to a second-order transition. Zh. éksp. Teor. Fiz. 112, 2134–2155 (December 1997)     

Structure of aluminum alloys irradiated with reactor neutrons

Samples of the CAB-1 alloy in the initial state and irradiated with fast neutrons at an fluence of 2 × 10²¹ neutrons/cm² have been studied by small-angle neutron scattering. It has been demonstrated that the observed large scattering cross sections are associated with the presence of nanosized pores with radii R ∼ 5–50 nm in the alloy, whereas for possible inclusions of the Mg₂Si and Si phases, the contrast factors and limiting volume fractions lead to the estimated cross sections that are two orders of magnitude smaller than those observed in the experiment. As a result of the irradiation, the volume fraction of scattering objects (pores) 40–50 nm in radius decreases by a factor of more than two. This is compensated, to a large extent, by an increase in the total fraction of particles with radii of 5–8 and 20–25 nm as the total surface area of the scattering objects increases by 40%.     

Small-angle light scattering studies of dense AOT-water-decane microemulsions

Summary We have performed extensive studies of a three-component microemulsion system composed of AOT-water-decane (AOT=sodium-bis-ethylhexyl-sulfosuccinate is an ionic surfactant) using small-angle light scattering (SALS). The small-angle scattering intensities are measured in the angular interval 0.001–0.1 radians, corresponding to a Bragg wave number range of 0.14 μm⁻¹<Q<<1.4 μm⁻¹. The measurements were made by changing temperature and volume fraction ϕ of the dispersed phase (water + AOT) in the range 0.05<ϕ<0.75. All samples have a fixed water-to-AOT molar ratio,w=[water]/[AOT]=40.8, in order to keep the same average droplet size in the stable one-phase region. With the SALS technique, we have been able to observe all the phase boundaries of a very complex phase diagram with a percolation line and many structural organizations within it. We observe at the percolation transition threshold, a scaling behavior of the intensity data. This behavior is a consequence of a clustering among microemulsion droplets near the percolation threshold. In addition, we describe in detail a structural transition from a droplet microemulsion to a bicontinuous one as suggested by a recent small-angle neutron scattering experiment. The loci of this transition are located several degrees above the percolation temperatures and are coincident with the maxima previously observed in shear viscosity. From the data analysis, we show that both the percolation phenomenon and this novel structural transition are derived from a large-scale aggregation between microemulsion droplets.     

Quasi-free Compton scattering and the polarizabilities of the neutron

Differential cross-sections for quasi-free Compton scattering from the proton and neutron bound in the deuteron have been measured using the Glasgow/Mainz photon tagging spectrometer at the Mainz MAMI accelerator together with the Mainz [48]cm ;SPMOslash; × [64]cm NaI(Tl) photon detector and the G?ttingen SENECA recoil detector. The data cover photon energies ranging from [200]MeV to [400]MeV at θ^LAB _γ = 136.2^°. Liquid deuterium and hydrogen targets allowed direct comparison of free and quasi-free scattering from the proton. The neutron detection efficiency of the SENECA detector was measured via the reaction p(γ,π⁺ n). The “free” proton Compton scattering cross-sections extracted from the bound proton data are in reasonable agreement with those for the free proton which gives confidence in the method to extract the differential cross-section for free scattering from quasi-free data. Differential cross-sections on the free neutron have been extracted and the difference of the electromagnetic polarizabilities of the neutron has been determined to be α_n - β_n = 9.8±3.6(stat)^+2.1 _-1.1(syst)±2.2(model) in units of [10^-4]fm ³. In combination with the polarizability sum α_n + β_n = 15.2±0.5 deduced from photoabsorption data, the neutron electric and magnetic polarizabilities, α_n = 12.5±1.8(stat)^+1.1 _-0.6(syst)±1.1(model) and β_n = 2.7±1.8(stat)^+0.6 _-1.1(syst)±1.1(model) are obtained. The backward spin polarizability of the neutron was determined to be γ⁽ⁿ⁾ _π = (58.6±4.0)×10^-4 fm ⁴. Received: 21 August 2002 / Accepted: 16 October 2002 / Published online: 11 February 2003 RID="a" ID="a"Part of the Doctoral Thesis. RID="b" ID="b"Present address: Physikalisch-Technische Bundesanstalt, Bundesallee 100, D-38116 Braunschweig. RID="a" ID="a"Part of the Doctoral Thesis. RID="b" ID="b"Present address: Physikalisch-Technische Bundesanstalt, Bundesallee 100, D-38116 Braunschweig. RID="c" ID="c"Part of the Habilitation Thesis. RID="d" ID="d"e-mail: schumacher@physik2.uni-goettingen.de Communicated by Th. Walcher     

Mesoscopic structure of Ni<Subscript>2 + <Emphasis Type="Italic">x</Emphasis></Subscript>Mn<Subscript>1 − <Emphasis Type="Italic">x</Emphasis></Subscript>Ga alloys in the concentration range corresponding to a coupled magnetic-structural phase stransition

The Ni_{2 + x} Mn_{1 − x} Ga magnetic shape memory alloys at concentrations x = 0.18–0.36 have been studied using small-angle polarized neutron scattering in magnetic fields 0 < H ≤ 5.7 kOe. In this concentration range, the alloy undergoes a coupled magnetic-structural phase transition. At x < 0.18, the martensitic phase transition occurs, as usual, in the ferromagnetic state, i.e., T _m < T _C (T _m and T _C are the temperatures of the martensitic and magnetic phase transitions, respectively). However, at x > 0.27, the relationship between the characteristic temperatures is changed, i.e., T _m > T _C. The small-angle polarized neutron scattering data indicate that, in the concentration range under investigation, there occurs a complex transformation of the magnetic and atomic structures. All phase transitions exhibit a temperature hysteresis of scattering and polarization, which is characteristic of first-order phase transitions. A comparative analysis of the mesoscopic structures of the Ni_{2 + x} Mn_{1 − x} Ga and Ni_{2 + x + y} Mn_{1 − x} Ga_{1 − y} alloys studied using the small-angle polarized neutron scattering technique has been carried out.     

Resonance Scattering Spectral Detection of Catalase Activity Using Au@Ag Nanoparticle as Probe and Coupling Catalase Catalytic Reaction with Fenton Reaction

The Au_coreAg_shell (Au@Ag) nanoparticles in size of 30 nm were prepared using 10 nm gold nanoparticles as seeds at 90°C, and were purified by high-speed centrifugation to remove the excess trisodium citrate to obtain Au@Ag nanoprobe. In the medium of pH 4.0 acetate buffer solution—7.2 μmol/L H₂O₂–67 μmol/L Fe(II), Au@Ag nanoparticles exhibited a resonance scattering (RS) peak at 538 nm. Upon addition of Catalase (Ct), the system produced hydroxyl radical that oxidized the Au@Ag nanoprobe to form the AuAg nanoparticles with partly bare nanogold. Those AuAg nanoparticles aggregated to large nanoclusters that led to the RS peak wavelength red-shift and its RS peak intensity enhanced. The catalase activity (C) is linear to the enhanced RS intensity (ΔI) in the range of 6 to 2,800 U/L, with regression equation of ΔI = 0.168 C-0.2, the correlation coefficient of 0.9952, and detection limit of 2.8 U/L. This method was applied to the detection of serum samples, and the results were agreement with that of the spectrophotometry. A new catalytic mechanism of catalase was proposed with oxywater principle that was agreement with the results of resonance scattering spectroscopy, absorption spectrophotometry, transmission electron microscopy and laser scattering.     

Counterion condensation in ionic micelles as studied by a combined use of SANS and SAXS

We report a combined use of small-angle neutron scattering (SANS) and small-angle X-ray scattering (SAXS) to the study of counterion condensation in ionic micelles. Small-angle neutron and X-ray scattering measurements have been carried out on two surfactants cetyltrimethylammonium bromide (CTABr) and cetyltrimethylammonium chloride (CTACl), which are similar but having different counterions. SANS measurements show that CTABr surfactant forms much larger micelles than CTACl. This is explained in terms of higher condensation of Br⁻ counterions than Cl⁻ counterions. SAXS data on these systems suggest that the Br⁻ counterions are condensed around the micelles over smaller thickness than those of Cl⁻ counterions.     

Real-time icosahedral to fcc structure transition during CoPt nanoparticles formation

Nucleation and growth of supported CoPt nanoparticles were studied in situ and in real time by combined grazing incidence small-angle x-ray scattering (GISAXS) and grazing incidence x-ray diffraction (GIXD). GISAXS provides morphological features of nanoparticles as a function of size, shape and correlation distance between particles, while GIXD allows the determination of the atomic structure. We focus on the formation of ultrasmall CoPt nanoparticles, in the 1–4 nm size range at 500^○C. The structural analysis method based on the Debye equation is coupled with cluster model calculations performed by Monte Carlo simulations using a semi-empirical tight-binding potential to interpret diffraction spectra and structural transitions. Our results show that the cluster structure evolution during the growth is size-dependent and composition-dependent, yielding an icosahedral to fcc structure transition.     

Investigation of the Mesostructure of Transition-Metal Monogermanides Synthesized under Pressure

The mesostructure of transition-metal monogermanides Mn_{1 – x}Co _x Ge is studied by small-angle neutron scattering in a wide range of concentrations x = 0–0.95. These compounds were synthesized under high pressure and are metastable under normal conditions. The experimental dependences I(Q) obtained for the whole series of samples in the range of transferred momenta (6 × 10^–2 nm^–1 < Q< 2.5 nm^–1) are described by the power dependence Q^–n with an exponent n = 2.99 ± 0.02, uniquely related to the fractal properties of the system under study. The dependence obtained indicates that the superatomic structure of the samples is characterized by the presence of defects with a spatial organization described by a fractal model with a logarithmic dependence of the correlation function of the defect density. It is interesting to note that such defects are absent in the isostructural FeGe compound, i.e., the experimental dependences of the intensity are described well by the expression Q^–n with an exponent n = 4.1 ± 0.1, which demonstrates the presence of crystallites with a uniform density distribution inside and a sharp boundary characterizing the surface.

     

A precise measurement of the spin-dependent neutron scattering length of 3He

The poor knowledge of the spin-dependent neutron scattering length of ³He has until now handicapped nuclear four body theory and the interpretation of excitations in the quantum liquid. We have measured, for the first time directly, the real part of the bound incoherent neutron scattering length, b_i′ of ³He. A neutron spin echo spectrometer was used to detect pseudomagnetic precession of polarised neutrons passing through polarised ³He gas. Any absolute calibrations of sample and beam parameters were avoided using simple transmission measurements with non-polarised neutrons. The only a priory information required was the spin-dependent neutron absorption cross section of ³He. The result is b_i′ = -2.365(20) fm, which reduces the prior uncertainty by a factor 30. The corresponding new value of the bound incoherent scattering cross section is σ_i = 1.532(12) barn. Including the known value of the coherent neutron scattering length, we obtain new values for the real parts of the free triplet and singlet neutron scattering lengths, a_-′ = 7.370(58) fm and a₊′ = 3.278(53) fm.     

Investigation of the evolution of the hydrated zirconia mesostructure at different stages of heat treatment

The mesostructure of amorphous xerogels based on hydrated zirconia ZrO₂ and its evolution at different stages of heat treatment have been investigated using the small-angle neutron scattering method. A correlation function of the nuclear scattering amplitude density has been obtained from experimental neutron scattering cross sections, and the characteristic radii of ZrO₂ nanoparticles and their specific surface areas have been determined. The influence of the annealing temperature on the fractal properties of the zirconia surface has been elucidated.     

Surface spin-glass-like behavior of monodispersed superparamagnetic Mn0.5Zn0.5Fe2O4 magnetic fluid

Zero field cooled dc-magnetization measurements of monodispersed Mn_0.5Zn_0.5Fe₂O₄ nanoparticles dispersed in kerosene exhibit two transitions at low temperatures. These transitions correspond to (i) the superparamagnetic to blocked superparamagnetic and (ii) the blocked superparamagnetic to surface spin-glass like/quantum superparamagnetic state upon lowering the temperature. The existence of a disorder surface is confirmed by recording small-angle neutron scattering data below and above the Curie temperature. Magnetic relaxation analysis shows a plateau at low temperature (below 5 K) with a slight minimum at 3 K, which is a characteristic of the surface spin-glass-like state. This is analyzed considering the energy distribution n(E)∼1/E. The existence of surface disorder dominates at low temperature and mimics the transition from superparamagnetic to quantum superparamagnetic states.     

Microphase separation in weakly charged hydrophobic polyelectrolytes

Aqueous solutions of a well-defined poly(N-isopropylacrylamide-co-sodium 2-acrylamido-methylpropanesulfonate) (NIPAM/NaAMPS in a 95/5 molar ratio) have been investigated by means of small-angle neutron scattering (SANS) and rheological experiments as a function of temperature ( 25^° C T 60^° C) and polymer concentration ( 0.5wt% C 12wt%). The solutions remain optically transparent and isotropic over the whole temperature range, in contrast with the homopolyNIPAM which precipitates above its lower critical solution temperature (LCST = 32^° C). Upon addition of salt, the systems undergo a micro-macrophase separation. At temperatures above 45^° C, the SANS spectra exhibit a sharp peak at a scattering wave vector, q _max, which increases slightly with temperature. At high temperature ( T∼ 60^° C), the scattered intensity follows a power law I(q) ∼q ^-4 in the asymptotic regime, characteristic of two-density media with sharp interfaces, and q _max is found to vary with polymer concentration as q _max∼C ^0.22. Estimates of the typical sizes give values between 40 ? and 200 ?. These results provide a strong evidence of a thermally induced microphase separation, which is corroborated by the very sharp increases of the viscosity (over 2 decades) and of the stress relaxation time of the solutions, occurring in the temperature range where the scattering peak is observed. The results are discussed and compared with the theoretical models proposed for weakly charged polyelectrolytes in a poor solvent. Received 1 October 2001     

Anisotropic Hubbard model on a triangular lattice — spin dynamics in HoMnO3

The recent neutron scattering data for spin-wave dispersion in HoMnO₃ are well-described by an anisotropic Hubbard model on a triangular lattice with a planar (XY) spin anisotropy. Best fit indicates that magnetic excitations in HoMnO₃ correspond to the strong-coupling limit U/t >∼ 15, with planar exchange energy J = 4t ² /U ≃ 2.5 meV and planar anisotropy ΔU ≃ 0.35 meV.      

Study of the heavy-fermion compound CeRu<Subscript>2</Subscript>Si<Subscript>2</Subscript> by the small-angle neutron scattering method

In order to directly observe neutron scattering by heavy fermion quasiparticles at low temperatures, a CeRu₂Si₂ single crystal has been studied by the small-angle neutron scattering method. In the experiment, neutron scattering is observed at T = 0.85 K for momentum transfers q ≤ 0.04 Å^?1, which is treated as the orbital component of magnetic scattering by heavy fermion quasiparticles. It has been found that the application of a magnetic field H = 1 T leads to both an increase in the observed scattering and its anisotropy with respect to the field direction. Moreover, measurements in the magnetic field reveal additional scattering for q > 0.04 Å^?1, which is well described by a Lorentzian and is interpreted as neutron magnetic scattering by spin-density fluctuations with a correlation radius R_c ≈ 30 Å.     

Small angle diffuse neutron scattering: Measurements on V2O3 in the temperature range 400–600 K

Cold neutron small-angle scattering measurements on pure V₂O₃ in the high-temperature transition domain shows an anomalous feature namely a peak and a bump in the range 500–570 K. It is suggested that a plausible origin of this anomaly is the formation of giant “correlation” clusters of size ～ 600 Å and a magnetic moment density ～ 10^-7 μ/ų as the system suffers a broad M-I transition.     

Concerning the two magnetic correlation lengths above T c in an Invar iron-nickel alloy

The magnetic phase transition in the Invar alloy Fe₇₀Ni₃₀ is investigated by means of small-angle neutron scattering over a wide range of momentum transfer. This method was used to measure two magnetic correlation lengths R _c 1 and R _c 2 which coexist in the alloy above the phase transition temperature T _c . The critical correlations with correlation length R _c 1 are described well by an Ornstein-Zernicke expression, and the critical correlations with the second correlation length, an order of magnitude larger than R _c 2, are described well by a squared Ornstein-Zernicke expression. The temperature dependences obtained for the correlation lengths R _c 1 and R _c 2 satisfy the power law R _c ∼((T−T _c )/T _c ) ^−υ with critical exponents υ₁=0.65±0.05 and υ₂=1.3±0.1 for the shorter and longer scales, respectively. Pis’ma Zh. éksp. Teor. Fiz. 66, No. 1, 53–57 (10 July 1997)     

The effect of neutron and gamma irradiation on the dislocation relaxation peak in silver

Summary The internal-friction spectrum has been determined in extremely pure polycrystalline silver crystals after being subjected to neutron and gamma irradiation. The spectra obtained for an applied frequency of 10 MHz show that the mechanical losses due to dislocation relaxation decrease as the doses of neutron and gamma radiation increase. The effect of gamma radiation was found to be more significant than that of neutron irradiation. The relationship between damping neutron and gamma dose was found to be of the formQ _max ⁻¹ α ΛD ^η, where η is equal to −1.2 for neutron and −1.45 for gamma irradiation. The variations of the peak height and width, and temperature of the dislocation relaxation peak as functions of neutron and gamma doses are explained in terms of the pair-kink formation model.     

A comprehensive,time-resolved SANS investigation of temperature-change-induced sponge-to-lamellar and lamellar-to-sponge phase transformations in comparison with <Superscript>2</Superscript>H -NMR results

Time-resolved small-angle neutron scattering (TR-SANS) was employed to observe temperature-induced phase transitions from the sponge (L ₃ to the lamellar ( L _α phase, and vice versa, in the water-oil (n -decane)-non-ionic surfactant ( C₁₂E₅ system using both bulk and film contrast. Samples of different bilayer volume fractions φ and solvent viscosities η were investigated applying various amplitudes of temperature jump ΔT . The findings of a previous ²H -NMR study could be confirmed, where the lamellar phase formation was determined to occur through a nucleation and growth process, while it was concluded that the L ₃ -phase develops in a mechanistically different and more rapid manner involving uncorrelated passage formation. Likewise, the kinetic trends of the nucleation and growth transition (decreased transition time with increase of φ and ΔT were witnessed once again. Additionally, NMR and SANS data that demonstrate a strong dependency of that process on solvent viscosity η are presented. Contrariwise, it is made evident via both SANS and NMR results that the L _α -to-L ₃ transition time is independent (within experimental sensitivity) of the varied parameters (φ , ΔT , η . Unusual scattering evolution in one experiment, originating from a highly ordered lamellar phase, intriguingly hints that a major rate determining factor is the disruption of long-range order. Furthermore, the bulk contrast investigations give insight into structure peak shifts/development during the transitions, while the film contrast experiments prove the bilayer thickness to be constant throughout the phase transitions and show that there is no evidence for a change in the short-range order of the bilayer structure. The latter was considered possible, due to the different topology of the L ₃ and L _α phases. Lastly, an unexpected yet consistent appearance of anisotropic scattering is detected in the L ₃ -to- L _α transitions.     

Study of CdSe/CdS quantum dots in solutions and gels by small-angle X-ray scattering

The sizes of semiconductor nanocrystals of CdSe/CdS quantum dots (QDs) synthesized by the colloidal method were estimated using small-angle X-ray scattering. The distribution of QD nanocrystals in organic solvents of different polarities and in polymer gels and matrices is studied. Structural invariants of scattering QD particles (heterogeneities of the electron density)—namely, inertia radii and sizes, forms, and dispersive composition of particles—are determined. The contribution of scattering by QDs in solutions and gels is calculated. The effective sizes of particles and their aggregates are determined, and the parameters of the distribution over the QD sizes in organic solvents and polymer matrices are estimated. The typical distance between particles in samples is determined. The position of the maximum at the beginning of the small-angle scattering curves corresponds to the distance d _m = 2π/h ₀ between the planes (here, h ₀ is the position of the maximum on the scale h). It is 74–76.9 ? for solutions, 60 ? for gels, and 99 ? for polymer matrices with concentrations of up to 0.15% and 77 ? for those with the concentrations exceeding 0.15%, which is close to the estimation of the sizes of separate CdSe QDs that was obtained from the distribution histograms (60–80 ?). This result shows that CdSe/CdS QDs introduced in the polymer matrices disperse to form either separate particles or small aggregates and located at a distance on the order of 80 ? from each other.