Small-angle X-ray Scattering Spectra Research Articles

Interfacial polarization and electrorheological effect of homo-poly(ionic liquid) and poly(ionic liquid)-hexyl methacrylate copolymer microsphere particles

Homo-poly(ionic liquid) (HomoPIL) microsphere particles of poly[2-(methacryloyloxy)ethyltrimethylammonium][bis(trifluoromethanesulfonyl)imide] (P[MTMA][TFSI]) and poly[2-(methacryloyloxy)ethyltrimethylammonium][hexafluorophosphate] (P[MTMA][PF6]), as well as their corresponding copolymer microsphere particles obtained through copolymerization with hexyl methacrylate (HMA), were synthesized as electrorheological (ER) materials. The morphology and structure of these synthesized particles were characterized using scanning electron microscopy (SEM), 1H nuclear magnetic resonance spectroscopy (1H NMR), Fourier-transform infrared spectroscopy (FT-IR), and small-angle X-ray scattering spectra (SAXS). Electrorheological measurements were conducted for these polyelectrolyte-based suspensions at room temperature, revealing that the HMA composition has a different effect on the ER effect of the two poly(ionic liquid)s. Differential scanning calorimetry (DSC) and temperature-modulated dielectric analysis (TMDA) were employed to investigate the effect of HMA composition on the glass transition temperature and interfacial polarization of these polyelectrolytes, suggesting that the incorporation of HMA affect the ER effect of PILs via changing the density of charge carriers and the counterion mobility. This study presents a potential approach for enhancing the electrorheological properties of poly(ionic liquid)s.

Small-Angle X-ray Scattering (SAXS) Used for the Identification of Nicomorphine Polymorphic Changes at the Early Stage to Avoid Varied Stability and Possible Side Effects.

In this paper, we present the identification of polymorphisms at an early stage, identified by applying non-standard methods such as SAXS. We provide an analytical approach to polymorphism in the quality/purity of an active pharmaceutical ingredient (API), supplied to a generic company by two different suppliers (i.e., manufacturers). Changes in thermodynamic polymorphism firstly become visible in traces in the larger crystal lattices, which are visible on the SAXS spectrum only using the logarithmic scale, as shown in the result figures. Hence, we are here on the trail of the beginning of a new polymorph in nicomorphine, whose crystal waviness at the early stage is visible only in the additional symmetrical peaks identified and calculated using SAXS, while the chemical analyses excluded all kinds of chemical impurities. The chemical and structural properties were studied using the following techniques: SAXS, WAXS, DSC, dissolution, Raman spectroscopy, and FTIR. Only the SAXS technique could identify crucial differences and calculate the additional signals related to giant crystals, whilst a standard method such as WAXS showed none, and nor did the chemical analyses, such as Raman spectroscopy and FT-IR. This means that due to water in crystallization (known in nicomorphine) or thermodynamic waviness, the formation of the new polymorph starts first in traces, which become visible at larger distances from the crystal lattice, detectible only in the SAXS range. This is a very important premise and hypothesis for further research, and we believe that this work lays a new stone in understanding the origin of new unknown polymorphs and their mixtures. Therefore, the aim of this work is to show that the use of non-standard methods (i.e., SAXS) can be of great benefit to API analysis and the identification of polymorphic changes in the early phase, which can cause varied stability, solubility and bioavailability and thus different therapeutic effects or side effects.

Autonomous screening of complex phase spaces using Bayesian optimization for SAXS measurements

The advent of modern, ultrafast X-ray experiments has enabled scientists to probe physical phenomena at an ever smaller scale. However, this has come at a cost of excessive data generation, to the point where current storage and hardware capabilities are routinely surpassed. As such, handling the data efficiently and selectively storing only the information of most relevance is crucial. In this paper, we propose to use Bayesian optimization as a method to alleviate this problem. We apply the method to locate global features in Small Angle X-ray Scattering spectra obtained from conducting experiments with supercritical CO2. By evaluating the algorithm on more than 250 data points, we show that the implementation is versatile, robust, and computationally efficient, often converging with just a few iterations and with a minimal error penalty. This paves the way for creating fully autonomous experiments, where data science algorithms such as the one presented herein operate hand-in-hand with the expert user to maximize scientific discovery and minimize the associated experimental cost.

Influence of Charge Block Length on Conformation and Solution Behavior of Polyampholytes.

We investigate the effect of charge block length on polyampholyte chain conformation and phase behavior using small-angle X-ray scattering (SAXS) and implicit-solvent molecular simulations. To this end, we use solid phase peptide synthesis to precision-tailor a series of polyampholytes consisting of l-glutamic acid (E) and l-lysine (K) monomers arranged in alternating blocks from 2 to 16 monomers. We observe that the polyampholytes tend to phase separate as block size increases. With addition of NaCl, phase separated polyampholytes exhibit a salting-in effect dependent on charge block length. Fourier-transform infrared (FTIR) spectroscopy reveals the presence of intramolecular hydrogen bonds that are disrupted upon the addition of NaCl, implicating both electrostatic interactions and hydrogen bonding in the phase behavior. SAXS spectra at no-added salt conditions show minimal dependence of charge block length on the radius of gyration (Rg) for soluble polyampholytes, but local chain stiffening is found to be dependent on charge block length. With increasing NaCl, consistent with electrostatic screening, all polyampholytes expand and behave as neutral or swollen chains in good solvent conditions. Molecular simulations are qualitatively consistent with experiments. Implications for understanding intracellular condensates and material design are noted.

Salt Weakens Intermicellar Interactions and Structuring in Bulk Solutions and Foam Films.

Drainage via stratification in micellar foam films formulated with ionic surfactants shows dramatic changes on salt addition: both the step size and the number of steps in their stepwise thinning diminish. As the stratification process is governed by supramolecular oscillatory structural forces that arise due to confinement-induced structuring of micelles, it is apparent that salt addition reduces the magnitude, periodicity, and decay length of the oscillatory forces. In this contribution, we characterize the changes in micellar size, shape, and interactions on salt addition in bulk solutions using small-angle X-ray scattering (SAXS) to understand and elucidate the influence of salt on stratification in micellar foam films and, more broadly, on the oscillatory structural forces. Adding salt leads to a significant reduction in long-range correlations between micelles and smaller intermicellar distances. These effects manifest as a weakening of the primary peak of the structure factor, ascertained from SAXS spectra, accompanied by its shift to higher wave vectors. Weakened long-range correlations diminish the magnitude and periodicity of the oscillatory disjoining pressure leading to smaller step sizes, fewer steps, and a rich nanoscopic topography, due to the influence of disjoining pressure on the deformable interfaces. The step sizes in stratifying thin films and intermicellar distances in bulk solutions present incongruous values, implying an imperfect analogy with studies on charged nanoparticles with matched and salt concentration-independent values of measured interparticle distances that equal the periodicity of force-distance curves. We anticipate that our findings are significant for multicomponent soft and biological matter containing self-assembled supramolecular structures wherein screened Coulomb interactions govern the self-assembly, interfacial adsorption, interactions, dynamics, and stability.

Small Angle X-ray Scattering Sensing Membrane Composition: The Role of Sphingolipids in Membrane-Amyloid β-Peptide Interaction.

Simple SummaryThe early impairments in Alzheimer’s disease are related to neuronal membrane damage. Different lipids are present in biological membranes, playing relevant physiological roles. Some of them, such as sphingomyelin, cholesterol, and ganglioside GM1, interact with each other and, importantly, with the Aβ peptide. Here, these interactions are studied using small angle X-ray scattering in model membrane systems, such as large unilamellar liposomes. This technique gives information on the width of the bilayer and reveals structural differences due to the different lipid compositions, as well as some small differences due to the presence of the Aβ peptide. The analysis highlights the concentration-dependent effect of GM1 on membrane thickness and the interaction with the Aβ-peptide, together with the inhibiting effect that the presence of sphingomyelin has on the GM1–Aβ interaction.The early impairments appearing in Alzheimer’s disease are related to neuronal membrane damage. Both aberrant Aβ species and specific membrane components play a role in promoting aggregation, deposition, and signaling dysfunction. Ganglioside GM1, present with cholesterol and sphingomyelin in lipid rafts, preferentially interacts with the Aβ peptide. GM1 at physiological conditions clusters in the membrane, the assembly also involves phospholipids, sphingomyelin, and cholesterol. The structure of large unilamellar vesicles (LUV), made of a basic POPC:POPS matrix in a proportion of 9:1, and containing different amounts of GM1 (1%, 3%, and 4% mol/mol) in the presence of 5% mol/mol sphingomyelin and 15% mol/mol cholesterol, was studied using small angle X-ray scattering (SAXS). The effect of the membrane composition on the LUVs–Aβ-peptide interaction, both for Aβ1–40 and Aβ1–42 variants, was, thus, monitored. The presence of GM1 leads to a significant shift of the main peak, towards lower scattering angles, up to 6% of the initial value with SM and 8% without, accompanied by an opposite shift of the first minimum, up to 21% and 24% of the initial value, respectively. The analysis of the SAXS spectra, using a multi-Gaussian model for the electronic density profile, indicated differences in the bilayer of the various compositions. An increase in the membrane thickness, by 16% and 12% when 2% and 3% mol/mol GM1 was present, without and with SM, respectively, was obtained. Furthermore, in these cases, in the presence of Aβ40, a very small decrease of the bilayer thickness, less than 4% and 1%, respectively, was derived, suggesting the inhibiting effect that the presence of sphingomyelin has on the GM1–Aβ interaction.

Structural studies on fluid Hg and fluid Se at high temperatures and high pressures by means of X-ray diffraction and small angle X-ray scattering

Abstract X-ray diffraction (XRD) and small angle X-ray scattering (SAXS) measurements for fluid Hg and fluid Se up to the supercritical region have been carried out using synchrotron radiation at SPring-8. We obtained the structure factor, S ( Q ) $S\left(Q\right)$ , including a small angle region, and the pair distribution function, g ( r ) $g\left(r\right)$ , for both fluids from the liquid to the dense vapor region. Change of the local structure and medium-range correlations at the metal-insulator transition in fluid Hg were revealed. On the other, the average coordination number of two was preserved at the semiconductor-metal transition in fluid Se. From a SAXS experiment of fluid Se in 2012, SAXS spectra near the semiconductor-metal transition region show the Ornstein–Zernike profile and the SAXS intensity is reduced with increasing pressure. These results indicate difficulties of separating fluctuations intrinsic to the semiconductor-metal transition from those arising from the liquid-vapor critical point in fluid Se, although fluctuations intrinsic to the electronic transitions are largely expected in both fluids.

Interaction among Spherical Polyelectrolyte Brushes in Concentrated Aqueous Solution

Interaction among concentrated spherical polyelectrolyte brushes (SPB) dispersions in water was systematically investigated by means of small-angle X-ray scattering (SAXS), wide-angle X-ray scattering (WAXS), and rheological methods. SPB consist of a core of polystyrene (PS) and a poly(acrylic acid) (PAA) brush shell. The "polyelectrolyte peak" appeared in SAXS spectra and was observed in WAXS curves for the first time. The size of the polyelectrolyte peak and the rheological properties of SPB were found to be strongly effected by SPB concentration, pH, and ionic strength. Combined with SAXS, WAXS, and rheological results, it is confirmed that the polyelectrolyte peak is originated from local ordered structures of polyelectrolyte chains bridged by counterions in the overlapping area among SPB driven by electrostatic interactions.

Charge effects in water solution of a low generation sodium carboxylate terminated dendrimers

Dendrimers, a class of novel nano-sized materials characterized by a highly ramified structure and a relevant number of functional surface groups, represent a versatile platform for a wide range of nanotechnology applications. The number and characteristic of their modifiable surface groups strongly influence the solution properties as well as some relevant processes involved in molecular recognition, signal processing as well as for binding various targeting or guest molecules. Owing to these properties dendrimers have attracted the interest of the researchers in the development of new prototypes implicated in many technological applications. However, despite of their recent extensive studies, their colloidal stability in solution environment have been relatively less investigated. With the aim to furnish useful insight about the inter-dendrimer interaction in solution, a Small Angle X-ray Scattering (SAXS) structural investigation on the sodium carboxylate terminated (-COO-Na) generations G1.5 of poly(amidoamine) dendrimers in water solution has been performed. The presence of a pronounced interference peak in the SAXS spectra in a wide range of concentrations gives evidence of a long range electrostatic interaction which has been ascribed to the ionisation of the surface carboxylate terminal end-groups. The experimental inter-dendrimer structure factor S(q) has been analysed in the framework of liquid integral equation theory. From that, we derived an effective inter-particle interaction composed of a screened Coulombic plus hard-sphere repulsion potential, which allows the estimation of the dendrimer effective surface charge Z eff . The present analysis strongly supports the finding that colloidal stability and interaction of dendrimers in solution environment is strongly influenced by charge effects.

Application of Quantitative Graphical Method Based on Small Angle X-Ray Scattering Spectrum in Crop Starch Study

Application of Quantitative Graphical Method Based on Small Angle X-Ray Scattering Spectrum in Crop Starch Study

Nanoscale Structure of Urethane/Urea Elastomeric Films

The nanostructure of urethane/urea elastomeric membranes was investigated by small-angle X-ray scattering (SAXS) in order to establish relationships between their structure and mechanical properties. The networks were made up of polypropylene oxide (PPO) and polybutadiene (PB) segments. The structural differences were investigated in two types of membranes with the same composition but with different thermal treatment after casting. Type I was cured at 70–80 °C and type II at 20 °C. Both membranes showed similar phase separation by TEM, with nanodomains rich in PB or PPO and 25 nm dimensions. The main difference between type I and type II membranes was found by SAXS. The type I membrane spectra showed, besides a broad band at a 27-nm q value (modulus of the scattering vector), an extra band at 6 nm, which was not observed in the type II membrane. The SAXS spectra were interpreted in terms of PPO, PB soft segments, and urethane/urea links, as well as hard moiety segregation in the reaction medium. This additional segregation (q = 7 nm), although subtle, results in diverse mechanical behavior of in both membranes.

Small-angle X-ray scattering in sodium dodecyl sulfate solutions and micelle clustering

The small-angle X-ray scattering (SAXS) in micellar sodium dodecyl sulfate solutions has been studied in the range of overall concentrations c from 8 mM (CMC1) to 300 mM and the absolute values of scattering vector q from 0.07 to 3.0 nm–1. The total intensity of isotropic scattering has been revealed to increase with solution concentration. At c > 27 mM, the SAXS spectra have been found to exhibit an interference peak, which testifies a correlation in the arrangement of micelles in the bulk solution. This peak corresponds to the magnitude of q close to 1.55 nm–1. Using the position of this maximum, average distance r 0 between the centers of micelles has been determined, which is equal to 4.1 nm and remains almost unchanged upon an increase in the overall concentration of sodium dodecyl sulfate. The observed regularities have been explained in terms of the DLVO theory taking into account the electrostatic and molecular intermicellar interaction.

Temperature Assisted in-Situ Small Angle X-ray Scattering Analysis of Ph-POSS/PC Polymer Nanocomposite.

Inorganic/organic nanofillers have been extensively exploited to impart thermal stability to polymer nanocomposite via various strategies that can endure structural changes when exposed a wide range of thermal environment during their application. In this abstraction, we have utilized temperature assisted in-situ small angle X-ray scattering (SAXS) to examine the structural orientation distribution of inorganic/organic nanofiller octa phenyl substituted polyhedral oligomeric silsesquioxane (Ph-POSS) in Polycarbonate (PC) matrix from ambient temperature to 180 °C. A constant interval of 30 °C with the heating rate of 3 °C/min was utilized to guise the temperature below and above the glass transition temperature of PC followed by thermal gravimetric, HRTEM, FESEM and hydrophobic analysis at ambient temperature. The HRTEM images of Ph-POSS nano unit demonstrated hyperrectangular structure, while FESEM image of the developed nano composite rendered separated phase containing flocculated and overlapped stacking of POSS units in the PC matrix. The phase separation in polymer nanocomposite was further substantiated by thermodynamic interaction parameter (χ) and mixing energy (Emix) gleaned via Accelrys Materials studio. The SAXS spectra has demonstrated duplex peak at higher scattering vector region, postulated as a primary and secondary segregated POSS domain and followed by abundance of secondary peak with temperature augmentation.

UV–Vis Absorption and Small Angle X-ray Scattering Spectra of Commercial Polyurethane Coating Filled with Zinc Oxide

Surface-modified hexagonal zinc oxide (ZnO) prisms were incorporated into commercial polyurethane (PU) coating. Dip-coated PU/ZnO composite films on polypropylene sheets exhibited a broad dip in ultraviolet (UV) transmittance corresponding to the ZnO band gap. Compared to 5 and 10 wt% loading, optical properties of PU composites were significantly modified by 20 wt% ZnO fillers in terms of the blue shift and splitting of UV peaks with substantially increased absorption. The morphology effect is demonstrated by replacing the hexagonal ZnO with sword-like ZnO. The sword-like ZnO gave rise to a lower UV absorption and the two slope characteristic in small angle X-ray scattering spectrum corresponding to the thin parts at tapered ends. The proposed procedure and materials used in this work are appropriate for economic large-scale production of composites.

Synchrotron-based small-angle x-ray scattering from biogenic materials

We examine the small-angle x-ray scattering (SAXS) from samples of biogenic nature to study soft-matter and the associated biology. Biogenic samples are prepared from soft tissues. SAXS from different tissues varies according to both genetic (species) and environmental (habitant differences) factors. SAXS spectra (intensity versus energy (MeV)) at different Q momentum transfer values provide the crucial tool for determining the structure and enhancement of the desired property, e.g. biological activity. Fourier transform infrared (FTIR) spectroscopy was used to characterize the presence of specific chemical groups in the materials. These methods are valuable to identify various phases of calcium carbonate (CaCO3). FTIR spectra were obtained in the range of wavenumbers from 4000 to 400 cm−1 for the external shell, soft tissue and operculum at room temperature. Finding information about the biological structures from these low-absorbing materials is one of the most important goals in the field of biological and environmental sciences and to know the mechanisms involved in bio-mineralization. These results will be utilized for the development of bio-systems.

Characterization of the Nanostructure of Complexes Formed by Single- or Double-Stranded Oligonucleotides with a Cationic Surfactant

We report the use of dynamic light scattering (DLS), small-angle neutron scattering (SANS), and small-angle X-ray scattering (SAXS) to characterize the nanostructure of complexes formed by either single- or double-stranded oligonucleotides with a cationic surfactant (cetyltrimethylammonium bromide, CTAB) in aqueous solution (1 mM Li(2)SO(4)). For single-stranded oligonucleotides 5'-A(20)-3' and 5'-CCCCATTCTAGCAGCCCGGG-3', both the appearance of two Bragg peaks (at 0.14 and 0.28 Å(-1)) in SAXS spectra with a spacing of 1:2 and form factor fits to SANS spectra are consistent with the presence of multilamellar vesicles (with, on average, 6-9 layers with a periodicity of 45-48 Å). Some samples showed evidence of an additional Bragg peak (at 0.20 Å(-1)) associated with periodic packing (with a periodicity of 31 Å) of the oligonucleotides within the lamellae of the nanostructure. The nucleotide composition of the single-stranded oligonucleotides was also found to impact the number and size of the complexes formed with CTAB. In contrast to 5'-A(20)-3' and 5'-CCCCATTCTAGCAGCCCGGG-3', 5'-T(20)-3' did not change the state of aggregation of CTAB (globular micelles) over a wide range of oligonucleotide:CTAB charge ratios. These results support the proposition that hydrophobic interactions, as well as electrostatics, play a central role in the formation of complexes between cationic amphiphiles and single-stranded oligonucleotides and thus give rise to nanostructures that depend on nucleotide composition. In contrast to the single-stranded oligonucleotides, for double-stranded oligonucleotides mixed with CTAB, three Bragg peaks (0.13, 0.23, and 0.25 Å(-1)) in SAXS spectra with a spacing ratio of 1:√3:√4 and characteristic changes in SANS spectra indicate formation of a hexagonal nanostructure. Also, the composition of the double-stranded oligonucleotides did not measurably impact the nanostructure of complexes formed with CTAB, suggesting that electrostatic interactions dominate the formation of these complexes. Overall, these results provide insights into the intermolecular interactions that occur between cationic amphiphiles and oligonucleotides and establish that single and double-stranded oligonucleotides form complexes with cationic surfactants that differ in nanostructure. The results also provide guidance for the design of oligonucleotide complexes with cationic amphiphiles.

Sodium Glycodeoxycholate and Glycocholate Mixed Aggregates in Gas and Solution Phases

This paper deals with electrospray ionization mass spectrometry (ESIMS), small-angle X-ray scattering (SAXS), and dynamic light scattering (DLS) measurements in order to provide information on the existence, aggregation, composition, and structure of the two-component aggregates of sodium glycocholate (NaGC) and sodium glycodeoxycholate (NaGDC) in the gas and solution phases. Five samples, containing 100% NaGC and 100% NaGDC, and NaGDC/NaGC molar ratios of 3 (75D), 1 (50D), and 1/3 (25D), have been analyzed by ESIMS in positive-ion detection mode starting from 10(-3) and 10(-2) M total bile salt concentration in aqueous solutions. Generally, dimers or trimers prevail in the 100% NaGC or NaGDC samples, respectively, as observed in the preceding one-component ESIMS measurements and in agreement with the proposed micellar aggregate structures in aqueous solution. Moreover, it is observed that the composition of multimers in the samples 75D, 50D, and 25D deviates from the one expected on the basis of a random association of the monomers, the NaGDC contribution generally prevailing on the NaGC one. It happens also under the same percentage condition (50D sample), in agreement with a greater aggregation ability of NaGDC with respect to NaGC. SAXS and DLS data were recorded on six samples containing a NaGC+NaGDC 40 mM total concentration, one bile salt having 40, 32, 24, 16, 8, and 0 mM concentration and the other the complementary one, keeping constant the NaCl concentration (0.6 M). The NaGDC 40 mM sample presents SAXS curves in agreement with a cylindrical shape of the aggregates as shown in a previous paper. For the bile salt mixtures, the progressive decrease of the sizes and change of the aggregate morphology, toward a globular-like geometry, are observed by increasing the NaGC fraction, thus confirming the hypothesis about the ability of trihydroxy salts to inhibit the growth of dihydroxy salt aggregates. Fits on the basis of cylindrical model can be accomplished for all the SAXS spectra, however, when the extracted cylinder parameters are used to estimate theoretical hydrodynamic radii a reasonable agreement is obtained only for the samples at high fraction of NaGDC (NaGDC>or=24 mM).

Liquid-like Ordering of Negatively Charged Poly(amidoamine) (PAMAM) Dendrimers in Solution

A structural investigation in water solution of the sodium carboxylate-terminated (generation G3.5) Tomalia-type poly(amidoamine) dendrimers has been performed by means of the small angle X-ray scattering (SAXS) technique. A long-range intermolecular interaction, revealed by the presence of sharp peaks in SAXS spectra, gives evidence of a considerable structural order in the system, even at low concentration of the dispersed phase. The experimental interdendrimer structure factor S(q) was analyzed in the framework of the Ornstein-Zernike integral equation by using the hypernetted chain approximation (HNCA) as closure relation. The effective interdendrimer interaction, modeled as a screened Coulombic plus hard-sphere repulsion potential, allows the estimation of the dendrimers' effective surface charge Z(eff). The present analysis strongly supports the findings that the effective intra- and interdendrimer charge interactions, as well as the dendrimer solution environment conditions, are crucial parameters for the modulation of the degree of structural organization in solution, suitable for a number of potential applications.

Small-Angle X-ray Scattering and Light Scattering on Lysozyme and Sodium Glycocholate Micelles

Small-angle X-ray scattering (SAXS) together with static (SLS) and dynamic light scattering (DLS) measurements were carried out on aqueous solutions of lysozyme (LY) and of the ionic biological detergent sodium glycocholate (NaGC). Apparent diffusion coefficients (D app), excess Rayleigh ratio, and SAXS spectra were measured for 0.1 M NaGC solutions at different ionic strengths (0.05-0.30 M NaCl). The same data were collected for LY in sodium acetate buffer 50 mM without and with 92 mM NaCl as a function of protein concentration (10-80 g L(-1)). A correlated analysis of SLS data and SAXS spectra was first tested on the LY samples and then extended to the interpretation of the NaGC data to infer information on particle structure and interaction potential. A hard-core (HC) interaction shell of uniform thickness, a screened Coulomb potential of the electric double layer (EDL) or the complete DLVO potential were alternatively used to represent the long-range tail of the interaction potential. Whenever an essentially repulsive tail is expected, all the representations give reasonable results, but the data analysis does not allow the discrimination between the oblate and the prolate symmetries of the NaGC aggregates. The DLVO model allows the interpretation of the data even when the attractive component determines the tail character. With this model an overall fit of the micelle data at all the NaCl concentrations was successfully performed by assuming a simple spherical symmetry of the micelles and invariant values of their ionization degree and Hamaker constant, thus considering just the screening effect of the added electrolyte. Whatever model is used, the results point out that the aggregates are quite hydrated (26-38 water molecules per monomer) and very slightly grow by increasing the NaCl concentration. When spherical symmetry is assumed the aggregate radii for all the samples fall in the range 15-16 A. From the SAXS and SLS, best fitting geometrical parameters, and interparticle structure factor, a D app value was calculated for each sample. An excellent consistence is achieved for LY results. On the contrary, calculated D app values systematically lower than the experimental values are always obtained for the NaGC micelles. Micelle polydispersity and internal dynamics seem to be the most probable reasons of the bad agreement.

EFFECT OF ANNEALING TEMPERATURE OF CERIUM OXIDE NANOPARTICLES STUDIED BY SMALL-ANGLE X-RAY SCATTERING

The evolution of microstructure of cerium oxide nanoparticles prepared in a sol-gel process was investigated by small-angle X-ray scattering (SAXS) measurements, in which the range of annealing temperature was from 298 K to 973 K in air. It was found that their scattering intensities increased dramatically and was proportional to h-a as the temperature went up to 873 K. Meanwhile, the average radius of gyration Rg, increased. This suggested that these cerium oxide nanoparticles have self-similar structure behavior or mass fractal structure. When the temperature was higher than 873 K, the feature of the SAXS spectra became identical to that of the sactterers with surface fractal structure rather than the mass fractal structure.