We have used small angle neutron scattering (SANS) to study solutions of cetyltrimethylammonium 2,6-dichlorobenzoate (2,6) at rest and as a function of shear. These solutions are Newtonian, and up to a concentration of at least 100mM contain spherical micelles. Comparison with viscoelastic solutions of the closely related, and much studied, cetyltrimethylammonium 3,5-dichlorobenzoate (3,5) is made. While spheres are not expected to align under shear, a shear induced sphere to rod transition has been postulated for this system. In the results presented here, no shear induced sphere to rod transition was observed even at the highest accessible shear rate. Addition of sufficient supporting electrolyte (up to 1M NaCl) does cause such a transition in the quiescent solution. Hoffmann et al. have seen what they refer to as the formation of a shear induced structure (SIS or type II micelles) on similar systems where short rods form in the absence of supporting electrolyte. Shearing of the salted system produces rapid though not spectacular alignment, with no evidence of a SIS forming.

Small angle neutron scattering, SANS, was used to describe the magnetic alignment and in situ shear ordering of polyelectrolytic, liquid crystalline cellulose microfibrils in aqueous (D2O) suspension. In a 2.4 Tesla magnetic field, microfibril suspensions exhibit anisotropic chiral nematic (cholesteric) ordering in which the distance between nematic planes along the cholesteric axis is shorter than between rods within a nematic plane. This is consistent with the hypothesis that cellulose microfibrils are helically twisted rods. During shear, the SANS interference peaks perpendicular to the flow direction sharpen with increasing shear rate. Yet, the highest degree of alignment (for microfibrils with axial ratios of ~45) was observed a short period after the cessation of shear flow.

Dense silica gels, prepared from suspensions of 24 nm colloidal silica particles, have been studied by small angle neutron scattering. Provided the volume fraction, φ, of the silica is less than about 0.18, the scattered intensity increases at low wavevector, q, as the gelation proceeds and the structure factor, S(q), of the final gel exhibits apparent power law behavior, usually interpreted as a signature of fractal growth. The power law behavior, however, was observed for all measured φ (≤0.30) when the gelation occurred in the presence of an applied shear. Furthermore, the first diffraction maximum, corresponding to the inter-particle contact distance, was more sharply peaked in the high density sheared gels, indicating that the structural arrangement of the silica particles under shear is more densely packed than in gels produced without shear under equivalent conditions. Although it is clear that shear has a marked influence on the gel structure at higher densities, a quantitative interpretation of the diffraction results is difficult because cluster-cluster interference might be present. Such difficulties encountered when trying to interpret the scattering from these dense systems are outlined, and a computer simulation that includes cluster-cluster interference is presented.

We have performed a series of spinodal decomposition measurements of a three-component microemulsion system made of a surfactant AOT, water, and decane. The measurements were made by a temperature jump from a one-phase droplet microemulsion to a two-phase droplet microemulsion along the critical iso-volume fraction line (10%) using the time resolved light scattering intensity technique. All three stages of the evolution were studied. The typical scattering intensity distribution is in good agreement with recent dynamic scaling theories.

Small angle neutron scattering has been used to study phase separation in a quantum alloy, solid 3Hex-4He1-x. The onset of phase separation is marked by a dramatic increase in the measured scattering. A simple interpretation of the results suggests that the late-stage phase separation kinetics are dominated by an increase in the concentration of 3He atoms in preexisting precipitate regions.

Small angle neutron scattering experiments were performed on a eicosane-based ferrofluid. An average size of 88 Å can be extracted from the data, in agreement with results from electron microscopy. Below the frozen temperature of eicosane, however, the particles are seen to be in larger aggregates with a fractal dimension of 2.15, similar to those formed under reaction-limited cluster aggregation (RLCA) conditions. At high concentrations, particles form larger aggregates even in the liquid state. Applying a magnetic field introduces new structure and changes the density inside the aggregates.

An enhanced multiple small-angle neutron scattering (MSANS) formulation has been developed to interpret the beam-broadening, arising from coarse, concentrated pore/grain microstructures in porous ceramics and similar materials. Prolific scattering from such systems precludes single-scattering studies (apart from Porod surface determinations). Previous MSANS techniques, which have been developed to extract the mean pore dimensions, either treat a range of scattering morphologies, while assuming that the scattering is in the diffraction limit, or they consider refraction effects, while assuming that the scattering features are spherical. Many systems of interest violate both these assumptions. In the enhanced formulation, the previous method, which allowed fully for refraction, is extended to non-spherical scattering morphologies. Applications of the MSANS formulation to sintering studies of Si3N4 and silica gels, and to the microstructural characterization of plasma-spray coatings are currently of interest.

The microstructral characteristics of titanium dioxide aerogels were studied by Small Angle Neutron Scattering (SANS). A variety of models were used to extract the morphological parameters from the SANS data. The evaluation of scattering data was found to be consistent with nitrogen gas adsorption and TEM measurements of a model of aerogel consisting of a light density matrix in which meso- and macro-pores are embedded.

Studies of microstructure evolution as a function of sintering parameters are necessary to better control the microstructure of nanophase ceramic compacts during processing. Small-angle scattering provides a comprehensive probe of the statistically-representative microstructures present in nanophase ceramics. A complete characterization includes complementary density, electron microscopy, nitrogen desorption and x-ray diffraction measurements. Small-angleneutron and ultra-small-angle x-ray scattering have been used to determine the effects of different sintering temperatures, pressures and additives during sintering of nanophase zirconia compacts. The samples were of sufficient size and uniformity to permit absolute calibration of the scattering data, making it possible to confirm that scattering from the pore/grain interface dominates the total scattering cross-section. A quantitative microstructural model was developed for this system, resulting in the determination of specific pore surface area, total pore volume fraction, pore number size distribution and grain size as a function of sintering parameters.

Failure of ceramic materials for high-temperature applications is initiated by the formation of creep pores. Thus, the determination of the sizes and number densities of pores induced during creep testing is one key to a understanding of their failure mechanisms and related life-time predictions. For this purpose small-angle neutron scattering (SANS) techniques are one of the most potential tools as demonstrated by an analysis of creep pores in liquid-phase-sintered, hot isostatically pressed alumina. The exploration of creep induced pores requires the analysis of SANS intensity over an extremely extended region of scattering vectors, the scanning of which needs joint use of both conventional SANS and double crystal diffractometry (DCD), an ultra small angle scattering technique.

Dissolution and growth of precipitates in a room temperature aged Al-11.8 at % Zn alloy have been studied under electron irradiation using small angle neutron scattering (SANS). A series of electron irradiations were performed on each sample and SANS measurements were made on each irradiation. In general for low doses the results show an initial decrease in the magnitude of the scattering, but associated with an increase in the precipitate size. This is followed on prolonged irradiation by an increase in the magnitude of the scattering with a continued increase in precipitate size. It is believed, that at low doses some precipitate grow in size but others may dissolve in the matrix, which then becomes supersaturated. With the enhanced rate of diffusion as a result of the irradiation, the remaining precipitates grow rapidly. As the supersaturation reduces, a coarsening mechanism takes over, via a radiation enhanced diffusion mechanism.

In situ small angle neutron scattering (SANS) was used to characterize the formation of the random 3-dimensional porous structure created during the free corrosion of a Ag0.7Au0.3 alloy in concentrated HNO3. The evolution of the porosity was followed in situ for a period of 21 hours. The average ligament width evolved from a size of approximately 6 nm following only 7 minutes of dealloying to approximately 22.5 nm after 21 hours of de-alloying. Using a model developed by N.F. Berk (Phys. Rev. Lett., 58 (1987) 2718) for the scattering properties of random porous media, we were able to characterize the average ligament width distribution as a function of time. Our results represent the first in situ nanoscale characterization of the formation of 3-dimensional porosity in a corrosion system.

Neutron diffraction has been used as tool for measuring stress fields (type-I stresses) and intergranular or microstresses (type-II stresses) for a decade. The experimental methods for measuring the two types of stresses are outlined. Emphasis is placed on maximizing the precision and accuracy of the measurements. Some serious sources of error in measurements near surfaces and some subtle wavelength effects are considered.

The presence of residual stress in engineering components can effect their mechanical properties and structural integrity. Neutron diffraction in the only technique that can make nondestructive measurements in the interior of components. By recording the change in crystalline lattice spacings, elastic strains can be measured for individual lattice reflections. Using a pulsed neutron source, all lattice reflections are recorded in each measurement, which allows for easy examination of heterogeneous materials such as metal matrix composites. Measurements made at the Manuel Lujan Jr. Neutron Scattering Center (LANSCE) demonstrate the potential at pulsed sources for in-situ stress measurements at ambient and elevated temperatures.

Neutron scattering experiments have been carried out with undeformed and creep deformed samples of the superalloy CMSX-4. From the measured constrained misfit data, obtained from different reflecting planes with respect to the external load axis, two strain tensors for horizontal and vertical matrix plates can be extracted.

A careful data analysis is necessary since the technical manufactured single crystals show a mosaic spreading of 0.5° and the wavelength spreading of the incident neutron beam, Δλ/λ is about 410-3 This is in the same range as the unknown constrained misfit quantities δc. A method has been developed which allows a calculated intensity distribution to be fitted to the measured one.

The dependence of residual stresses in martensitic-austenitic age-hardenable steels on a different technological treatment (welding by electron beam, postweld heat treatment) were investigated using a neutron diffraction. Experiments were performed in NPI Řež on a high-resolution diffractometer equipped with cylindrically bent perfect crystals. The resolution of the instrument (Δd/d ≈ 10-4; d-lattice spacing) enabled us to investigate plastic strains in weld joints.

Investigation of strongly distorted crystal structures caused by dislocations, stacking-faults etc. in both plastically deformed f.c.c. and b.c.c. metallic materials was performed by the analysis of the neutron diffraction line broadening. Measurements were realized by means of the high resolution triple-axis neutron diffractometer equipped by bent Si perfect crystals as monochromator and analyzer at the NPI Řež. The substructure parameters obtained in this manner are in good agreement with the results of X-ray diffraction analysis.

Variation of internal stress states in cold rolled sheet metal can essentially influence the result of forming processes. Therefore it is important to control the forming process by a practicable in line testing method. For this purpose magnetic and ultrasonic nondestructive methods are available. However, it is necessary to calibrate these techniques. This paper describes a first step of such a calibration procedure making use of the neutron diffraction method. On the basis of the diffraction results an assessment of the magnetic and ultrasonic methods for the estimation of residual stress in the cold rolled iron-disks was made. Reasonable measuring concepts for practical applications to forming processes with cold rolled sheet metal are discussed.

The main objective of the present investigation is to determine the evolution of residual stresses by neutron powder diffraction in an Al/SiC composite (Al 7075 reinforced by 27 vol.% SiC whiskers), originating from thermal treatment and mechanical loading. The results show that residual stresses in the matrix and in the reinforcement decrease in magnitude with increasing temperature and they reach the stress free state at the 'equivalent temperature'. As the temperature further increases, these stresses increase numerically in a reverse sense for both phases. The data obtained are analysed in terms of a simple model based on Eshelby's equivalent inclusion method.

Increasingly, sub-surface residual stress measurements by means of neutron diffraction are being conducted at various laboratories around the world. Unlike X-ray diffraction residual stress measurement setups, neutron instruments in use worldwide vary widely in design, neutron flux, and level of dedication towards residual stress measurements. Although confidence in the neutron technique has increased within the materials science and engineering communities, no demonstration of standardization or consistency between laboratories has been made. One of the steps in the direction of such standardization is the development of standard specimens, that have well characterized residual stress states and which could be examined worldwide.

In this paper we will examine two options for a neutron stress standard specimen. 1) A steel ring-plug specimen with very well defined diametrical interference. 2) A spot weld in a High Strength Low Alloy steel disk. The results of neutron residual stress measurements on these specimens will be discussed and conclusions as to their usefulness as neutron stress standards will be presented.