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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.

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At least 1,639 records · Page 91
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Investigation and characterization of ZnO single crystal microtubes

Morphological, structural, and optical characterization of microwave synthesized ZnO single crystal microtubes were investigated in this work. The structure and morphology of the ZnO microtubes are characterized using X-ray diffraction (XRD), single crystal diffraction (SCD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM). The results reveal that the as-synthesized ZnO microtube has a highly regular hexagonal cross section and smooth surfaces with an average length of 650–700 μm, an average outer diameter of 50 μm and wall thickness of 1–3 μm, possessing a single crystal wurtzite hexagonal structure. Optical properties of ZnO single crystal microtubes were investigated by photoluminescence (PL) and ultraviolet-visible (UV-vis) absorption techniques. Room-temperature PL spectrum of the microtube reveal a strong UV emission peak at around 375.89 nm and broad and a weak visible emission with a main peak identified at 577 nm, which was assigned to the nearest band-edge emission and the deep-level emission, respectively. The band gap energy of ZnO microtube was found to be 3.27 eV. - Highlights: • ZnO microtube length of 650–700 μm, diameter of 50 μm, wall thickness of 1–3 μm • ZnO microtube possesses a single crystal wurtzite hexagonal structure. • The crystal system is hexahedral oriented along a-axis with indices of (100). • A strong and sharp UV emission at 375.89 nm (3.29 eV) • One prominent absorption band around 378.88 nm (3.27 eV)

36 MATERIALS SCIENCE↗
DOE OSTI2016

Direct comparison of Fe-Cr unmixing characterization by atom probe tomography and small angle scattering

The fine microstructure obtained by unmixing of a solid solution either by classical precipitation or spinodal decomposition is often characterized either by small angle scattering or atom probe tomography. This article shows that a common data analysis framework can be used to analyze data obtained from these two techniques. An example of the application of this common analysis is given for characterization of the unmixing of the Fe-Cr matrix of a 15-5 PH stainless steel during long-term ageing at 350 °C and 400 °C. A direct comparison of the Cr composition fluctuations amplitudes and characteristic lengths obtained with both techniques is made showing a quantitative agreement for the fluctuation amplitudes. The origin of the discrepancy remaining for the characteristic lengths is discussed. - Highlights: •Common analysis framework for atom probe tomography and small angle scattering •Comparison of same microstructural characteristics obtained using both techniques •Good correlation of Cr composition fluctuations amplitudes from both techniques •Good correlation of Cr composition fluctuations amplitudes with classic V parameter.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Characterization of yttrium-rich precipitates in a titanium alloy weld

The yttrium-rich (Y-rich) precipitates that form in the fusion zone (FZ) of a Ti–5Al–1Sn–1Zr–1V–0.8Mo (wt.%) alloy, or Ti-5111, gas-tungsten arc welds (GTAW) were characterized. The filler metal was modified by a small concentration of Y in order to refine the microstructure and thus improve the FZ ductility. A high number density of nanoscale Y-rich precipitates were characterized in the weld FZ by atom probe tomography (APT) and scanning transmission electron microscopy (STEM). - Highlights: •A high number density of nanoscale precipitates were observed in the FZ matrix. •The nanoscale precipitates are enriched in yttrium. •Oxygen and sulfur are also present in the Y-rich precipitates and their interfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2017

X-ray micro computed tomography characterization of cellular SiC foams for their applications in chemical engineering

Open-cell SiC foams clearly are promising materials for continuous-flow chemical applications such as heterogeneous catalysis and distillation. X-ray micro computed tomography characterization of cellular β-SiC foams at a spatial voxel size of 13.6{sup 3} μm{sup 3} and the interpretation of morphological properties of SiC open-cell foams with implications to their transport properties are presented. Static liquid hold-up in SiC foams was investigated through in-situ draining experiments for the first time using the μ-CT technique providing thorough 3D information about the amount and distribution of liquid hold-up inside the foam. This will enable better modeling and design of structured reactors based on SiC foams in the future. In order to see more practical uses, μ-CT data of cellular foams must be exploited to optimize the design of the morphology of foams for a specific application. - Highlights: •Characterization of SiC foams using novel X-ray micro computed tomography. •Interpretation of structural properties of SiC foams regarding to their transport properties. •Static liquid hold-up analysis of SiC foams through in-situ draining experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Atomic scale characterization of white etching area and its adjacent matrix in a martensitic 100Cr6 bearing steel

Atom probe tomography was employed to characterize the microstructure and C distribution in the white etching area (WEA) of a martensitic 100Cr6 bearing steel subjected to rolling contact fatigue. Different from its surrounding matrix where a plate-like martensitic structure prevails, the WEA exhibits equiaxed grains with a uniform grain size of about 10 nm. Significant C grain boundary enrichment (>7.5at.%) and an overall higher C concentration than the nominal value are observed in the WEA. These results suggest that the formation of WEA results from severe local plastic deformation that causes dissolution of carbides and the redistribution of C. - Highlights: •APT has been applied to characterize the microstructure of white etching area (WEA). •Quantitative analyses of C distribution indicate that carbides are dissolved on the WEA. •WEA contains equiaxed grains with a uniform grain size of 10 nm. •C segregation at grain boundaries stabilizes the nanosized grain structure. •Formation of WEA is explained by severe local plastic deformation introduced by cyclic contact loading.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructure characterization of recycled IN718 powder and resulting laser clad material

Highlights: • A simple and efficient recycling procedure of IN718 powder has been defined for the laser cladding process. • Characterization of wasted and cleaned powder and comparison with new IN718 powder pointed out a slight diameter increase. • Microstructure characterization of clad builds showed differences between builds with new and recycled powders. • Clad microstructure and porosity increase remain constant static properties but decrease rupture strain after 3 reuses. • Without special precautions for cladding, the recycled powder can be reused twice without modifying the properties of IN718. - Abstract: The possibility to reuse the metal powder wasted in Laser Material Deposition (LMD) process has been evaluated and a simple procedure developed. LMD uses metal powder which is fed through a nozzle into the focal point of a laser, where it melts the powder and the substrate material. During the process, a high ratio of particles hits against an unmelted area and directly bounces off the deposited area. The efficiency ratio of deposition can drop to 40% depending on the configuration and spot size. This work deals with the design of a procedure to recollect and reuse the wasted powder of a nickel based superalloy IN718. After usage, powder is recollected, undesired fractions are magnetically segregated and aggregates are removed by sieving. The particles are mixed again and ready for reuse. In order to study the effectiveness of the process, no new powder has been added to the recovered fraction, and this procedure has been repeated five times. Experimental tests show that deposited material present similar properties than those obtained with new powder grains. But, after 3 reuses, the porosity content increases consequently and the rupture strain decreases strongly. The implementation of this process allows the improvement of the final efficiency, reducing costs and decreasing the hazardous powder amount.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Characterizing dislocation configurations and their evolution during creep of a new 12% Cr steel

Highlights: • Applicability of different techniques to characterize particular dislocation configuration. • XRD models in combination with TEM and EBSD to measure the dislocation density. • Substructure evolution during creep of a new 12% Cr steel is discussed. - Abstract: In this research, different types of dislocations are characterized and quantified in a newly developed 12% Cr steel in as-received as well as in crept conditions. X-ray diffraction (XRD) patterns are analyzed using three different models. The dislocation densities are determined employing the Convolution Multiple Whole Profile (CMWP) fitting, the analysis of the asymptotic part of the X-ray line profile (Groma's method), and the Rietveld refinement coupling Popa's and Williamson-Smallman approaches. CMWP method is used to measure the internal dislocation density inside the subgrains consisting of mobile and dipole dislocations, and the results show good agreement with Transmission Electron Microscopy (TEM) measurements. Groma's method is used to evaluate the total dislocation density, with results comparable to those obtained from the combination of Electron Backscatter Diffraction (EBSD) and TEM. Rietveld method gives the internal dislocation density or mobile dislocation density depending on the model chosen. The experimentally determined results such as creep strain, dislocation densities and subgrain size are compared with theoretical predictions and they are found in good agreement.

36 MATERIALS SCIENCE↗
DOE OSTI2018

EBSD characterization of the eutectic microstructure in hypoeutectic Fe-C and Fe-C-Si alloys

Highlights: • EBSD investigation of eutectic cementite and austenite in as-solidified low-alloy cast iron • Crystallographically independent growth of rapidly solidified cementite/austenite eutectic • Epitaxial growth of eutectic austenite from primary dendrites • Eutectic cementite and eutectoid ferrite frequently obey Bagaryatsky or Pitsch-Petch orientation relationship. - Abstract: Hypoeutectic Fe-C and Fe-C-Si model alloys were produced at different solidification conditions. Copper mold casting yields low cooling rates promoting the formation of a eutectic microstructure, which is characterized by two morphologies: elongated cementite plates and a rod structure growing perpendicular to the plates, i.e. austenite rods in a cementite matrix. Electron beam surface remelting generates a mainly plate-like eutectic due to rapid solidification. The microstructures were characterized by light-optical microscopy and electron backscatter diffraction (EBSD). The latter allows for a spatially resolved investigation of the growth crystallography of the eutectic phases. Thereby, a possible existence of crystallographic orientations relationships between cementite and austenite within the plate-like eutectic was assessed experimentally. The eutectic phases were found to grow largely crystallographically independently. Moreover, ferrite and eutectic cementite within the decomposed eutectic microstructure frequently comply with the Bagaryatsky or the Pitsch-Petch orientation relationship. Complementary X-ray diffraction (XRD) analysis reveals a pronounced cementite {002} texture in the microstructure produced by mold casting. Characteristic changes in the lattice parameters indicate that as-cast cementite is non-stoichiometric.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural characterization and comparison of Ti-6Al-4V manufactured with different additive manufacturing processes

In this work, the microstructures of Ti-6Al-4V manufactured by different additive manufacturing (AM) processes have been characterized and compared. The microstructural features that were characterized are the α lath thickness, grain boundary α (GB-α) thickness, prior β grain size and α colony size. In addition, the microhardnesses were also measured and compared. The microstructure of shaped metal deposited (SMD) Ti-6Al-4V material showed the smallest variations in α lath size, whereas the material manufactured with laser metal wire deposition-0 (LMwD-0) showed the largest variation. The prior β grain size was found to be smaller in material manufactured with powder bed fusion (PBF) as compared with corresponding material manufactured with the directed energy deposition (DED) processes. Parallel bands were only observed in materials manufactured with DED processes while being non-present in material manufactured with PBF processes.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Characterization of martensite-austenite constituents and micro-hardness in intercritical reheated and coarse-grained heat affected zones of API X70 HSLA steel

Highlights: • The influence of cold wire addition to the tandem submerged arc welding process on the ICRCGHAZ is investigated. • Comprehensive characterization of the microstructure and micro-hardness in the ICRCGHAZ of a HSLA steel is performed. • A lower fraction of finely distributed M-A formed in the ICRCGHAZ of TSAW + cold wire steel, leading to lower micro-hardness. • The aspect ratio and inter-particle spacing of M-A constituents decreased in the ICRCGHAZ through cold wire addition. - Abstract: The thermal cycles that high strength low alloy (HSLA) low carbon steels experience during welding inevitably affect the microstructure and mechanical properties of the weld joints. It is generally agreed that the coarse-grained heat affected zone (CGHAZ) and the intercritical reheated coarse-grained heat affected zone (ICRCGHAZ) in one-pass and multi-pass welding, respectively, have the poorest microstructure and mechanical properties relative to the rest of the steel joint. The martensite-austenite (M-A) constituents formed in the HAZ regions predominantly govern property deterioration in the CGHAZ and the ICRCGHAZ by promoting the initiation and propagation of micro-cracks. However, the characteristics of the M-A constituents, i.e., fraction, size, shape and aspect ratio, are strongly affected by the welding heat input. Accordingly, in this study, the aim was to evaluate the influence of a cold wire addition in conventional tandem submerged arc welding (TSAW + cold-wire) on the microstructure and micro-hardness in the CGHAZ and ICRCGHAZ. Microstructural characterization showed that a lower fraction of finely distributed M-A constituents associated with smaller prior austenite grains (PAGs) formed in the CGHAZ of the steel welded by the TSAW + cold-wire process (CW-OD weld) relative to that welded by the conventional TSAW process (TW-OD weld). Furthermore, the fraction of M-A constituents in the ICRCGHAZ of the CW-OD weld was decreased. A higher fraction of slender shaped M-A constituents in the ICRCGHAZ of the TW-OD weld resulted in an increase in the micro-hardness. The microstructure and micro-hardness changes associated with cold wire addition were attributed to the lower welding heat input and, consequently, the faster cooling rate with a corresponding reduction in the retention time in the austenitic region and ferrite/austenite region in the CGHAZ and ICRCGHAZ regions, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Characterization of hot extrusion and heat treatment on mechanical properties in a spray formed ultra-high strength Al-Zn-Mg-Cu alloy

Highlights: • The spray forming technology was used to fabricate ultra-high strength aluminum alloy. • The alloy under RRA state obtained the highest ultimate tensile strength of 732 MPa. • The effects of dislocations, solutes and precipitates etc., on yield strength were calculated. • Precipitation was characterized as the main strengthening mechanism for aging states. - Abstract: To obtain the optimal mechanical properties, several processes including spray forming technology, two passes hot extrusion and substantial heating treatments were operated on an Al-Zn-Mg-Cu-Zr alloy. The characterization methods used in this study include tensile tests, X-ray diffraction, differential scanning calorimetry and microstructure observations by optical microscope, scanning and transmission electron microscopy. The typical characteristics were the refined grain, homogeneous precipitates and porosity in the as-deposited pre-forms. The ultimate tensile strength, yield strength, hardness and elongation improved significantly after two passes hot extrusion. A good combination of ultimate tensile strength at 704 MPa and elongation at 9.7% were achieved under peak-aged treatment. The best ultimate tensile strength was obtained at 732 MPa after re-aging and regression. It was main dimple fracture in the extruded and aging treated specimens while brittle fracture for the as-deposited. The secondary phases were main MgZn{sub 2} and Al{sub 3}Zr dispersoids throughout all the states. The contributions of grain boundaries, dislocations, solid-solution and precipitates on the yield strength were analyzed using a quantitative equation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Characterization of advanced nuclear materials under extreme environments

The performance of materials under extreme environments poses important fundamental questions about the behavior of condensed matter under far-from-equilibrium conditions. These conditions create challenges in materials design, testing and evaluation. One important aspect of advancing nuclear power is the discovery and investigation of new classes of materials able to withstand the harsh environments in nuclear reactors. However, investigating and understanding the performance of these materials requires sophisticated tools and characterization techniques and skills. Furthermore, the goal of this special issue is to present recent research on the characterization of the response of candidate advanced nuclear materials to extreme environments.

36 MATERIALS SCIENCE↗
DOE OSTI2026

FIB-ToF-SIMS characterization of irradiated U-10Zr

Post-irradiation examination (PIE) is critical for the performance assessment and qualification of nuclear fuels. Secondary ion mass spectrometry (SIMS) is a powerful materials characterization technique that allows for elemental and isotopic mapping with a depth resolution greater than EDS and EPMA. However, it has not yet been applied to PIE of metallic nuclear fuel. Here, in this work, we characterize an fast neutron spectrum irradiated U-10Zr fuel sample using a time-of-flight SIMS (ToF-SIMS) system connected to a FIB/SEM system, which allows for flexible sample analysis compared to a dedicated ToF-SIMS instrument. Analysis of the resulting hyperspectral micrograph data was aided by the development of an unsupervised machine learning (ML) algorithm that iterates on existing methods to segment the 3D micrographic datasets based on the similarity of mass spectra. The results showed that the FIB-ToF-SIMS instrument was potentially capable of spatially resolving closed fission gas bubbles in 3D by continued ion sputtering of the analyzed volume. Additionally, the ML algorithm proved useful in revealing the chemical segregation of light fission products (those with an atomic mass between approximately 85–105 amu, such as ruthenium and rhodium) plus matrix zirconium, heavy fission products (those with an atomic mass between approximately 135–150 amu, such as the lanthanides) and uranium. Future studies are planned to conduct FIB-ToF-SIMS analysis on more irradiated U-Zr samples to study the constituent redistribution.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Multiscale characterization of an additively manufactured property graded Ni-base alloy for molten-salts\supercritical-CO 2 heat exchangers

The sequential optimization of strength and corrosion resistance in conventional alloy design procedures often results in a tradeoff between environmental degradation and optimal mechanical properties. A concurrent optimization of these two material properties is essential to efficiently develop high temperature alloys that can withstand harsh environments increasingly required for carbon–neutral energy technologies. In this work, we demonstrate the feasibility of directed energy deposition (DED) to manufacture a dual-corrosion resistant Ni-based alloy (Hastelloy N and Haynes 282), that meets the high temperature operation requirements of a molten-salts\supercritical-CO 2 (sCO 2 ) heat exchanger. A combination of multiscale characterization techniques and computational thermodynamics was employed to evaluate the cracking susceptibilities during fabrication and predict the microstructural stability of the material. Very good agreement was achieved between the observed and predicted phases and phase fractions of the as-printed material. A careful characterization of the transition zone between the two terminal alloy chemistries revealed potential precipitation strengthening (γ') on the Hastelloy N side while columnar-shaped M 23 C 6 and γ' precipitates that formed at grain boundaries (GBs) of the transition zone likely minimized the local interfacial energies. Both these mechanisms are believed to increase the interfacial stability but their performance at high temperatures requires further investigation.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Synthesis, characterization and catalytic activity of indium substituted nanocrystalline Mobil Five (MFI) zeolite

Highlights: • In situ modification of the MFI zeolite by incorporation of indium. • The samples were characterized by XRD, FTIR, TGA, UV–vis (DRS), SAA, EDX and SEM. • The incorporation of indium was confirmed by XRD, FT-IR, UV–vis (DRS), EDX and TGA. • Hydroxylation of phenol reaction was studied on the synthesized catalysts. - Abstract: A series of indium doped Mobil Five (MFI) zeolite were synthesized hydrothermally with silicon to aluminium and indium molar ratio of 100 and with aluminium to indium molar ratios of 1:1, 2:1 and 3:1. The MFI zeolite phase was identified by XRD and FT-IR analysis. In XRD analysis the prominent peaks were observed at 2θ values of around 6.5° and 23° with a few additional shoulder peaks in case of all the indium incorporated samples suggesting formation of pure phase of the MFI zeolite. All the samples under the present investigation were found to exhibit high crystallinity (∼92%). The crystallite sizes of the samples were found to vary from about 49 to 55 nm. IR results confirmed the formation of MFI zeolite in all cases showing distinct absorbance bands near 1080, 790, 540, 450 and 990 cm{sup −1}. TG analysis of In-MFI zeolites showed mass losses in three different steps which are attributed to the loss due to adsorbed water molecules and the two types TPA{sup +} cations. Further, the UV–vis (DRS) studies reflected the position of the indium metal in the zeolite framework. Surface area analysis of the synthesized samples was carried out to characterize the synthesized samples The analysis showed that the specific surface area ranged from ∼357 to ∼361 m{sup 2} g{sup −1} and the pore volume of the synthesized samples ranged from 0.177 to 0.182 cm{sup 3} g{sup −1}. The scanning electron microscopy studies showed the structure of the samples to be rectangular and twinned rectangular shaped. The EDX analysis was carried out for confirmation of Si, Al and In in zeolite frame work. The catalytic activities of the synthesized samples were investigated with respect to hydroxylation of phenol, in which catechol and hydroquinone were found to be the major products. It is observed that under all reaction conditions catechol selectivity was higher than the hydroquinone selectivity. In-MFI zeolites were successfully synthesized and were used as an effective catalyst for the hydroxylation of phenol to synthesize catechol and hydroquinone as the major product.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Synthesis and characterization of novel Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} perovskite material and possible application as a cathode for low–intermediate temperature SOFCs

Highlights: • Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} was synthesized using sol–gel methods. • Material was thoroughly characterized using Raman, FTIR, XRD, HRTEM, SEM, and TGA. • Electrochemical performance showed the materials are a promising new cathode material for low temperature SOFC. - Abstract: A novel perovskite material, Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} was synthesized using a sol–gel technique. The materials were calcined at temperatures of 800 °C, 900 °C, and 1000 °C and then characterized using X-ray diffraction, Raman and infrared spectroscopy, high resolution transmission electron microscopy and scanning electron microscopy (SEM). The particle sizes and crystallite sizes increased with increasing calcination temperature and formed perovskite type materials with some separate magnetite and iridium oxide. The powders were used to assemble button cells using samarium doped ceria as the electrolyte and NiO/SDC as the anode materials. The electrochemical properties were investigated using a Fiaxell open flanges test set-up and a Nuvant™ Powerstat-05 potentiostat/galvanostat. The Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} cathode material calcined at 1000 °C exhibited the most promising performance, with a maximum power density of 0.400 W/cm{sup 2}, a current density of 0.8 A/cm{sup 2}, and a corresponding area specific resistance of 0.247 Ωcm{sup 2} at 500 °C. The button cells were reasonably stable over15 h.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Synthesis, characterization and optical properties of ATiO{sub 3}–Pr thin films prepared by a photochemical method (where A = Ba and Ca)

Highlights: • A method of photochemical deposition has been used to the preparation of (Ba,Ca)TiO{sub 3} thin films doped Pr(III). • The (Ba,Ca)TiO{sub 3}/Pr(III) films under 375 nm excitation shows emissions attributable to {sup 1}D{sub 2} → {sup 3}H{sub 4} transition of Pr ion. • These PL signals decreased above 10 mol% of Pr(III). • Analysis suggests the presence of intermediate energy levels in the band gap influences in the PL processes. - Abstract: This article reports the characterization and optical properties of (Ba,Ca)TiO{sub 3} thin films doped with Pr at different proportions (0–15 mol%). The films were deposited on Si (1 0 0) and quartz substrates using a photochemical method and post-annealed at 900 °C. The evaluation of photo-reactivity of the precursor complexes was monitored by UV–vis and FT-IR spectroscopy. The obtained films were characterized by X-ray diffraction and X-ray photoelectron spectroscopy. The results indicate that Ba, Ca, Ti, O and Pr are present in the form of perovskite. Under UV light excitation (375 nm) the (Ba,Ca)TiO{sub 3}–Pr films show the characteristic emissions ascribed to {sup 1}D{sub 2} → {sup 3}H{sub 4} transition of Pr{sup 3+} ion. The optical measurements show the presence of intermediate energy levels in the band gap which influence the emission processes.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Structural and magnetic characterization of electro-crystallized magnetite nanoparticles under constant current

Graphical abstract: Structural and magnetic properties of electro-crystallized magnetite nanoparticles under constant current were studied. All samples were characterized using XRD, SEM, VSM, and Mössbauer spectrometry. - Highlights: • The effect of applied current on morphology and properties of Fe{sub 3}O{sub 4} is studied. • The particle size and morphology are controllable by adjusting the current. • The magnetization depends on particle size, type of surfactant and applied current. • The clear correlation between magnetization and the mean particle size is observed. - Abstract: The effect of applied current on the morphology, particle size, structure, and magnetic properties of magnetite nanoparticles prepared by electro-crystallization method was studied. The synthesis was performed in an electrochemical cell containing two iron electrodes and an aqueous solution of sodium sulfate, and either thiourea, sodium butanoate, or β-cyclodextrine as organic stabilizer. All the samples were characterized by XRD, SEM, VSM, and Mössbauer spectroscopy. X-ray diffraction patterns, clearly confirmed that all products have the cubic spinel Fe{sub 3}O{sub 4} crystal structure. Electron microscope images of the samples showed that their mean particle size is in the range 20–80 nm, and depends critically on the applied current and type of the organic additives. Specific magnetization of the samples at room temperature ranges from 60 to 90 A m{sup 2} kg{sup −1}, depending on the growth conditions. Room temperature Mössbauer spectra are typical of nonstoichiometric Fe{sub 3−δ}O{sub 4}, with a small excess of Fe{sup 3+}, 0.06 ≤ δ ≤ 0.17.

77 NANOSCIENCE AND NANOTECHNOLOGY↗