The measurement of superparamagnetic particle shapes and size distribution
Measurement of superparamagnetic particle shapes and size distribution
SEARCH · Search NASA
Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.
Measurement of superparamagnetic particle shapes and size distribution
A technique of magnetic granulometry is applied to previously reported data for the temperature dependence of isothermal remanent magnetization (IRM) in 13 lunar surface samples, including three soils. Observed increases in IRM with decreasing temperature are attributed to changes from superparamagnetic to single-domain types of behavior for fine metallic-iron particles. Based on this hypothesis, the temperature dependence of IRM in the examined samples is analyzed to obtain particle-size distributions over the range of mean diameters from 30 to 130 A. It is found that the distribution functions for the soils and a low-grade breccia vary as the inverse square of particle volume and that the distributions for recrystallized breccias and igneous rocks apparently peak about mean values.
Samples containing variable amounts of superparamagnetic hematite (sp-Hm) were prepared by a method in which the sp-Hm particles were dispersed throughout larger particles of silica gel, and the optical and magnetic properties of these samples were compared with those of larger-diameter hematite (bulk-Hm). It is shown that the optical properties of sp-Hm are different from those of bulk-Hm. Implications of the results for mineralogical interpretations of spectral data for the Martian surface and its terrestrial analogues are discussed. It is concluded that features resulting from ferric iron in the Martian spectral data and the results of the Viking magnetic properties experiment are both consistent with hematite present as both sp-Hm and bulk-Hm; the hematite particles most likely occur in pigmentary form, i.e., as particles dispersed throughout the volume of a spectrally neutral material.
The effect of the matrix on the reflectivity spectra of nanophase (superparamagnetic) hematite (np-Hm) dispersed within the matrix was investigated in four series of powder samples containing np-Hm dispersed within discrete powder particles (of two size ranges) of silica gel and activated alumina. The spectral data show that matrix effects are large. Samples with the same Fe2O3 content can have np-Hm absorption edges characterized by very different positions and curvature and slope indices, while samples with equivalent absorption edges can have very different Fe2O3 concentrations. Thus, quantitative relationships between the positions of ferric absorption edges and Fe2O3 concentrations are unreliable without knowledge of matrix properties of the system. It is shown that it was possible to match the Fe2O3 concentration, magnetic properties, and spectral data for Martian surface material with a laboratory mixture whose only ferric-bearing phase was hematite.
In view of the demonstrated value of Iron Moessbauer Spectroscopy (FeMS) in the study of extraterrestrial iron and the fact that, after silicon and oxygen, iron is the most abundant element on the surface of Mars, we proposed, and have under development, a backscatter Moessbauer spectrometer with x ray fluorescence capability (BaMS/XRF) for use on Mars as a geophysical prospecting instrument. Specifically, we have proposed BaMS/XRF as part of the geochemistry instrumentation on NASA's Mars Environment Survey (MESUR) mission. BaMS/XRF will have applications in: (1) the study of past environments through the examination of sedimentary material; (2) the study of the contemporary Martian environment; and (3) the study of iron-containing minerals of possible biogenic origin. Development of a reference library from a geophysical point of view for putative Martian surface materials at appropriate temperatures is now underway. We carried out preliminary optical reflectance and FeMS measurements on mineral products (iron oxyhydroxides) of deep-sea hydrothermal activity. Various aspects of this investigation are presented.
The results of magnetization and Mossbauer experiments are described which give evidence for superparamagnetism in the quenched face-centered-cubic (gamma) phase of the ternary system Fe .34, C .52, V .14 (Vicalloy II). Magnetometer data are given which clearly show that splat-cooled Vicalloy II does not exhibit long-range magnetic order. These data together with the Mossbauer data indicate that short-range magnetic ordering occurs which is temperature-dependent with coalescence of magnetic clusters over a limited temperature range. The model presented reasonably accounts for the observed effects and indicates that this ternary system is superparamagnetic down to 4.2 K.
Studies of porous aggregates of a regolith analog system composed of a 50:50-wt% mixture of labradorite and bronzite shocked at approximately 100-kbar intervals up to approximately 500 kbar are described, and characteristics of the well-indurated 'rock' formed at all pressures are reported. Ferromagnetic resonance studies of diopside and bronzite that were shocked at approximately 500 kbar are also reported. The formation of metallic particles in the superparamagnetic and single-domain size range as well as the metal fractionation are characterized, and the results suggest that the superparamagnetic and single-domain metallic particles in lunar soils may be produced by shock-induced dissemination of meteoritic and indigenous metal.
Results are presented on spectral, Moessbauer, static magnetic, petrographic, and compositional data for a Hawaiian palagonitic soil from Mauna Kea (HWMK1). It was found that reflectivity spectra of size separates smaller than 20 microns resemble spectra for Martian bright regions, while spectra of larger size separates show characteristics in common with spectra for Martian dark regions. Data on the HWMK1 soil are consistent with the partitioning of iron among the following minerals: olivine, titanomagnetite, hematite, and a superparamagnetic colored ferric oxide. These mineralogies are heterogeneously distributed within the soil with respect to both particle type and soil-particle diameter. The strongly magnetic titanomagnetite is associated with black particles and is responsible for the magnetic nature of the soil, while the colored weakly magnetic superparamagnetic ferric oxide and minor hematite are associated with orange particles.
A document discusses polymer nano - composite superparamagnetic actuators that were prepared by the addition of organically modified superparamagnetic nanoparticles to the polymer matrix. The nanocomposite films exhibited large deformations under a magnetostatic field with a low loading level of 0.1 wt% in a thermoplastic polyurethane elastomer (TPU) matrix. The maximum actuation deformation of the nanocomposite films increased exponentially with increasing nanoparticle concentration. The cyclic deformation actuation of a high-loading magnetic nanocomposite film was examined in a low magnetic field, and it exhibited excellent reproducibility and controllability. Low-loading TPU nanocomposite films (0.1-2 wt%) were transparent to semitransparent in the visible wavelength range, owing to good dispersion of the magnetic nanoparticles. Magnetoactuation phenomena were also demonstrated in a high-modulus, high-temperature polyimide resin with less mechanical deformation.
Stable colloidal dispersions of subdomain magnetite particles correlated for magnetic properties in terms of size distribution and volumetric concentration by superparamagnetic theory
Lunar samples have reduced coercive force, high values of R sub H (ratio of remanent coercive force to coercive force), and constriction in their magnetic hysteresis loops due to the presence of superparamagnetic and multidomain iron grains. The high R sub H values are also attributable to the magnetic shape effects of the iron grains. Spheres, cubes, and needles, as well as more irregular metal grains were observed. The coercive force values are quite meaningless unless the size and shape distributions are determined. The R sub H and the ratio of saturation remanence to saturation magnetization values can be considered characteristic of the size and shape modes of the ferromagnetic grains in a natural sample, and a classification of natural materials based on their hysteresis characteristics is presented with special reference to lunar samples.
The results of magnetization and Mossbauer experiments are reported which give evidence for superparamagnetism in the quenched face centered cubic (gamma) phase of the ternary system Fe(0.34)C(0.52)V(0.14) (Vicalloy 2). while the magnetization data agree with the limited data of Nesbitt et al., this more complete study shows clearly that this alloy does not acquire long-range ferromagnetic order, nor does it indicate either antiferromagnetic long-range ordering or mictomagnetic behavior, down to 4.2 K. The data can best be described as resulting from ferromagnetic clusters in a weakly magnetic lattice. The Mossbauer data show a slightly broadened single line spectrum of 300 K which broadens with decreasing temperature without development of resolvable hyperfine splitting down to 4.2 K. The broadening is attributed to relaxation effects associated with magnetic cluster coalescence.
Extra terrestrial materials, certain materials which have their origin at the earth's surface due to meteoritic impact, or under highly reducing conditions, such as in the case of basaltic flows in contact with coal beds or serpentenites, all contain Fe and FeNi phases with high magnetization values and spherical shape. Normally, the demagnetizing field (H sub D = NI sub S: where N is the demagnetizing factor and I is the saturation magnetization) is corrected for. In disperse systems, such as most natural materials, the particle shape effects are analyzed in terms of the saturation fields, Hs = H sub D = NI sub S and the magnetization differences (Delta I sub S). Discrete size modes of superparamagnetic (SP), multidomain (MD), and single domain (SD) particles result in reduced coercive force (Hc), increase in the value R sub H (ratio of remanent coercive force, H sub R, to H sub C), and decrease in the value R sub I (ratio of remanent magnetization, I sub R, to saturation magnetization, T sub S). The main distinctions between the various natural materials can be made by this approach. Hysteresis loops for terrestrial basalts, Fe and Ni rods and spheres, chondrite meteorites, lunar samples, impactites, and chondritic fusion crust are presented.
Mossbauer Fe-57 absorption spectra of superparamagnetic F.C.C. Fe sub .34 Co sub .52 V sub 14 (Vicalloy II) have been analyzed using a cluster model and magnetic resonance relaxation theory. The number and magnetic moment of the clusters were determined from magnetization data. A least squares fit to the spectrum at 4.2 K gives sub Hhyp = 175. kG, substantially greater than the value 55 kG inferred just from the observed broadening of the single line spectrum. From this broadening an estimate of 40 kG is obtained for the width of the distribution in Hhyp at 4.2 K arising from compositional fluctuations sub and small cluster effects.
Lunar breccias of low metamorphic grade offer a unique opportunity to investigate the magnetic properties of dispersed fine-grained iron. These rocks exhibit a pronounced time-dependent magnetization whose acquisition and decay are well explained by Neel's single-domain theory. The effect is due to iron grains in the range from 120 to 150 A in diameter, which covers the transition from superparamagnetic to stable single-domain behavior.
Analysis of the Moessbauer spectra of two Apollo 16 rocks showed that 60315,51 is much richer in iron metal and troilite, but poorer in olivine, than 62295,27. The values of magnetic parameters, derived from hysteresis loops at 175 and 300 K, indicate the high metal contents and the predominance of coarse multidomain grains in both rocks. These coexist with a superparamagnetic grain fraction in 60315 and with a small single-domain grain fraction in 62295. The high Fe(0)/Fe(2+) ratios, the nonlinear acquisition of laboratory thermoremanence, and the drastic changes in magnetic parameters upon heating support the proposed formation of both rocks from the lunar regolith, with incorporation of shocked meteoritic metal grains during high-temperature impact events and simultaneous acquisition of magnetic remanence. Values estimated for ancient lunar magnetic fields by comparing the natural remanence with laboratory thermoremanence acquired in fields of 0.05 and 0.5 Oe, range from 0.01 to more than 1 Oe.
The theory of superparamagnetic (SP) threshold calculations and single-domain (SD) to nonuniform spin threshold calculations is considered. The SD upper grain size limit and the SP-to-SD threshold size are calculated. The size and shape criteria for the stable SD behavior of metallic iron have implications for lunar magnetism and the mechanism of iron-silicate fractionation in the solar nebula.
Using a recently developed furnace, ferromagnetic resonance (FMR) thermomagnetic studies up to 900 C were employed to measure the Curie points of the superparamagnetic (SP) and single domain (SD) particles in lunar soils and potential magnetic analogue materials. Based on measured Curie points of 775 C, the SP and SD particles in lunar soils 10084-853, 12070-29, 14161-46, and 67010-4 are essentially pure metallic Fe. Synthetic and terrestrial samples containing magnetite, titanomaghemites, and magnetite-like particles have measured Curie points below 600 C are thus not magnetic analogues of lunar soils.