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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 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Magnetic Evaluation of the Nanoparticles Coated with Polyvinylpyrrolidone and Polyvinyl Chloride Nanoparticles Synthesized by Electro-deposition Method for Hyperthermia Application

Fe{sub 3}O{sub 4} nanoparticles, coated with polyvinylpyrrolidone (PVP) + polyvinyl chloride (PVC), were synthesized using cathodic electrochemical deposition (CED) technique. Physical properties of the uncoated and PVP + PVC-coated nanoparticles were investigated using several methods including X-ray diffraction (XRD), transmission electron microscopy (TEM), vibrating sample magnetometry (VSM), Fourier transform infrared (FT-IR), and AC susceptometer. In both the samples, single-phase formation in cubic spinel structure is detected in the XRD analysis. In this study, the mean crystallite size of the prepared specimens is found to be varied from 10.2 to 8.7 nm after PVP + PVC coating. The results of the FT-TR test thoroughly verified the existence of PVP/PVC layer onto the surface of the electrodeposited NPs, and magnetic results also confirmed a superparamagnetic (SPM) behavior at room temperature for both of them. Coercivity and magnetization saturation reduction have also been observed, despite having lower grain size. Also, weak magnetic interactions of inter-particle and a superspin glass-like behavior at low temperatures are confirmed. In addition, increasing of PVP + PVC content on the surface coating of the magnetic nanoparticles has decreased the inter-particle interactions.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Structural, Optical, Magnetic, and Dielectric Properties of Cr{sup 3+} Substituted Cobalt Aluminate Nanoparticles

The present study investigates the influence of Cr{sup 3+} substitution on structural, optical, dielectric, and magnetic properties of cobalt aluminates in the aluminates series CoAl{sub 2-x}Cr{sub x}O{sub 4}, 0.00 ≤ x ≤ 0.20. These series of nanoparticles are effectively synthesized using the co-precipitation method. The cubic spinel aluminate structure is confirmed by X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopic measurements. Transmission electron microscopy (TEM) analysis shows the formation of spherical nanoparticles, which are homogeneous in shape and size. The optical properties of the prepared samples have been investigated by means of optical absorbance spectra. The optical band gap E{sub opt}{sup i} and Urbach energy E{sub u} are estimated. At room temperature, the magnetization of undoped CoAl{sub 2}O{sub 4} reveals a weak ferromagnetic behavior. This ferromagnetism is increased for the sample with x = 0.05, and the samples with higher Cr{sup 3+} content have a tendency to be superparamagnetic on account of the formation of single-domain particles as a consequence of small particle size. Real part of dielectric constant (ε{sup ′}), dielectric loss (tanδ), ac conductivity (σ{sub ac}), real part of impedance (Z{sup ′}), and imaginary part of impedance (Z{sup ″}) are analyzed as a function of frequency and Cr{sup 3+} content. The results show that the dielectric loss (tanδ), dielectric permittivity (ε{sup ′}), and ac conductivity (σ{sub ac}) decrease with the increase in Cr{sup 3+} content, x = 0.05, and then increase with a further increase in Cr{sup 3+} content. The increase in these parameters has been explained on the basis of the hopping mechanism. From the Cole–Cole diagram, the value of the relaxation time τ can be calculated and it has been found to increase with increasing the Cr{sup 3+} content. Actually, a high dielectric constant makes these materials good for energy storage at high frequencies.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Hysteresis Cycle and Magnetization Behaviors of a Mixed-Spin (7/2, 3/2) Ferrimagnetic Ising Model: Monte Carlo Investigation

The effects of single-ion anisotropies and an external magnetic field on the magnetization of the mixed-spin (7/2, 3/2) ferrimagnetic Ising system are investigated within Monte Carlo simulation. Under certain values of the physical parameters, multiple hysteresis loop behaviors such as double, triple, and quintuple hysteresis cycles have been observed. Particularly, the superparamagnetic phase has been shown. The ground-state phase diagrams are presented.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Tracking of SPIONs in Barley (Hordeum vulgare L.) Plant Organs During its Growth

Barley plants were grown in water solutions containing nutrient elements and superparamagnetic iron oxide nanoparticles (SPIONs), particularly the magnetite nanoparticles (Fe{sub 3}O{sub 4}; 15–20-nm particle size). No visible detection of toxicity on plants’ growth had been observed. The different samples from two different organs of the plants, i.e., roots and leaves, were investigated using X-ray diffraction (XRD), bright-field microscope, and transmission electron microscope (TEM). To track the SPIONs, magnetic measurements using vibrating sample magnetometry (VSM) and Mössbauer spectroscopy at room temperature were also performed in the two different dried root and leaf organs of the plants. The magnetic signals measured in root and leaf organs clearly indicated an uptake of Fe{sub 3}O{sub 4} magnetic nanoparticles (MNPs) by the barley plant from aqueous medium containing Fe{sub 3}O{sub 4} MNPs and their subsequent accumulation in the plant organs. The different parameters such as hyperfine magnetic field, quadrupole splitting, isomer shift, and line width were deduced from Mössbauer spectroscopy data. The Mössbauer spectra are constituted of two magnetic sextets (A site, B site) and paramagnetic central doublet.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Synthesis and Characterization of Hydrophobic Fe{sub 3}O{sub 4} Magnetic Nanoparticles with High Saturation Magnetization

A simple one-step solvothermal method is proposed to prepare hydrophobic Fe{sub 3}O{sub 4} nanoparticles (MNPs) using iron acetylacetonate (Fe(acac){sub 3}), oleylamine (OAm), and ethylene glycol (EG). X-ray powder diffraction, scanning electron microscope, infrared spectroscopy, transmission electron microscopy, X-ray photoelectron spectrometry, and vibrating sample magnetometer are used to characterize the structure, morphology, and properties of products. The testing results indicate that the as-synthesized products are spherical-like hydrophobic MNPs, superparamagnetic at room temperature, with a saturation magnetization up to 76.8 emu/g. The good hydrophobic property of MNPs is attributed to the coverage of oleylamine, without causing a remarkable loss of magnetic property. In addition, the influences of material ratio, aging time, oleic acid, and stearic acid used as additives are studied in our research.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Prominent Study on Surface Properties and Diffusion Coefficient of Urease-Conjugated Magnetite Nanoparticles

Herein, the magnetite nanoparticles (MNs) were prepared by facile solvothermal method and its porous nature was modified using 3-(2-aminoethyl)-3-aminopropyl trimethoxysilane (AEAPS). Magnetite formation, successful amino tagging, and urease conjugation on the surface were confirmed from the presence of certain functional groups in Fourier transform infrared (FT-IR) spectra. Also, nanosize (13.2 nm) and spherical morphology of MNs were evaluated from diffraction patterns and electron micrographs respectively. Lower retentivity and coercivities in magnetization curve revealed the superparamagnetic behavior, and nitrogen adsorption/desorption curves exhibited decrease in its surface porosity. Conductivity measurements showed lower diffusion coefficient (D{sub e} = 1.9 × 10{sup −17} cm{sup 2}/min) and higher diffusion with limited hydrolytic reaction in native urease and improved activity of conjugated urease with higher D{sub e} (12.62 × 10{sup −16} cm{sup 2}/min). Hence, this study revealed that the surface porous nature of MNs can be altered effectively by amino tagging in order to overcome diffusional limitations thereby enhancing enzyme activity.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2011

Tumor-targeting magnetic lipoplex delivery of short hairpin RNA suppresses IGF-1R overexpression of lung adenocarcinoma A549 cells in vitro and in vivo

Highlights: {yields} We compared lipofection with magnetofection about difference of transfection efficiency on delivery a therapeutic gene in vitro and in vivo. {yields} We investigated the difference of shRNA induced by magnetofection and lipofection into A549 cell and subcutaneous tumor to knockdown IGF-1R overexpressed in A549 cell and A549 tumor. {yields} We investigated in vivo shRNA silenced IGF-1R overexpression 24, 48, and 72 h after shRNA intravenous injection into tumor-bearing mice by way of magnetofection and lipofection. {yields} Our results showed that magnetofection could achieve therapeutic gene targeted delivery into special site, which contributed to targeted gene therapy of lung cancers. -- Abstract: Liposomal magnetofection potentiates gene transfection by applying a magnetic field to concentrate magnetic lipoplexes onto target cells. Magnetic lipoplexes are self-assembling ternary complexes of cationic lipids with plasmid DNA associated with superparamagnetic iron oxide nanoparticles (SPIONs). Type1insulin-like growth factor receptor (IGF-1R), an important oncogene, is frequently overexpressed in lung cancer and mediates cancer cell proliferation and tumor growth. In this study, we evaluated the transfection efficiency (percentage of transfected cells) and therapeutic potential (potency of IGF-1R knockdown) of liposomal magnetofection of plasmids expressing GFP and shRNAs targeting IGF-1R (pGFPshIGF-1Rs) in A549 cells and in tumor-bearing mice as compared to lipofection using Lipofectamine 2000. Liposomal magnetofection provided a threefold improvement in transgene expression over lipofection and transfected up to 64.1% of A549 cells in vitro. In vitro, IGF-1R specific-shRNA transfected by lipofection inhibited IGF-1R protein by 56.1 {+-} 6% and by liposomal magnetofection by 85.1 {+-} 3%. In vivo delivery efficiency of the pGFPshIGF-1R plasmid into the tumor was significantly higher in the liposomal magnetofection group than in the lipofection group. In vivo IGF-1R specific-shRNA by lipofection inhibited IGF-1R protein by an average of 43.8 {+-} 5.3%; that by liposomal magnetofection inhibited IGF-1R protein by 43.4 {+-} 5.7%, 56.3 {+-} 9.6%, and 72.2 {+-} 6.8%, at 24, 48, and 72 h, respectively, after pGFPshIGF-1R injection. Our findings indicate that liposomal magnetofection may be a promising method that allows the targeting of gene therapy to lung cancer.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2015

Nanomedicine for the molecular diagnosis of cardiovascular pathologies

Predicting acute clinical events caused by atherosclerotic plaque rupture remains a clinical challenge. Anatomic mapping of the vascular tree provided by standard imaging technologies is not always sufficient for a robust diagnosis. Yet biological mechanisms leading to unstable plaques have been identified and corresponding biomarkers have been described. Nanosystems charged with contrast agents and targeted towards these specific biomarkers have been developed for several types of imaging modalities. The first systems that have reached the clinic are ultrasmall superparamagnetic iron oxides for Magnetic Resonance Imaging. Their potential relies on their passive accumulation by predominant physiological mechanisms in rupture-prone plaques. Active targeting strategies are under development to improve their specificity and set up other types of nanoplatforms. Preclinical results show a huge potential of nanomedicine for cardiovascular diagnosis, as long as the safety of these nanosystems in the body is studied in depth. - Highlights: • Ischemic stroke and myocardial infarction are the main causes of death in the world. • Their prevalence is related to late detection of high-risk atherosclerotic plaques. • Biomarkers of atherosclerosis evolution and potential ligands have been identified. • Nanosystems based on these ligands appear promising for early molecular diagnosis. • Preclinical and clinical nanosystems for common imaging modalities are described.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2011

Cation distribution and particle size effect on Raman spectrum of CoFe{sub 2}O{sub 4}

Moessbauer and Raman spectroscopic studies were carried out on CoFe{sub 2}O{sub 4} particles synthesized with size ranging from 6 to 500 nm (bulk). Cation distribution studies were carried out on the high temperature and room temperature phases of the microcrystalline CoFe{sub 2}O{sub 4} by Moessbauer and Raman spectroscopic methods. The high temperature phase of CoFe{sub 2}O{sub 4} showed a decreased inversion parameter of 0.69 as compared to the value of the room temperature phase of 0.95, indicating that the structure gradually transforms towards a normal spinel. Corresponding Raman spectra for these two phases of CoFe{sub 2}O{sub 4} showed a change in relative peak intensity of the vibrational mode at 695 cm{sup -1}(A{sub 1g}(1)) to 624 cm{sup -1} (A{sub 1g}(2)). The relative peak intensity ratio, I{sub v} between the A{sub 1g}(1) and A{sub 1g}(2) vibrational mode was decreasing with lowering of inversion parameter of the CoFe{sub 2}O{sub 4} spinel system. A variation of laser power on the sample surface was reflected in the cation distribution in ferrite phase. Superparamagnetic, single domain CoFe{sub 2}O{sub 4} particles (6 nm) showed a 20 cm{sup -1} red shift and broadening of phonon modes when compared to the macro-crystalline CoFe{sub 2}O{sub 4} (500 nm). Variation of Raman shift with particle size was studied by considering the bond polarization model. Raman spectroscopic studies clearly indicate the variation in the cation distribution in nano-sized particles and distribution tending to a normal spinel structural configuration. -- Graphical abstract: Variation of Raman shift difference ({Delta}{omega}) with size. Display Omitted

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

PVA and PEG functionalised LSMO nanoparticles for magnetic fluid hyperthermia application

La{sub 0.7}Sr{sub 0.3}MnO{sub 3} magnetic nanoparticles are synthesized by a solution combustion method and functionalised with polyvinyl alcohol and polyethylene glycol. The induction heating characteristics of coated magnetic nanoparticles (42 °C) were observed at a reasonably low concentration (5 mg/mL). Remarkably, coated magnetic nanoparticles exhibited a promisingly high specific absorption rate with varying magnetic field and constant frequency. The surface analysis is carried out by X-ray photoelectron spectroscopy. A reduction in the agglomeration of the particles was observed when the magnetic nanoparticles were functionalised with polyvinyl alcohol or polyethylene glycol and can be confirmed by transmission electron microscopy and dynamic light scattering studies. Vibrating sample magnetometer measurements indicate superparamagnetic behaviour at room temperature before and after coating. Colloidal stability revealed a considerably higher zeta potential value for coated system. In vitro cytotoxicity test of the magnetic nanoparticles indicates that coated nanoparticles have no significant effect on cell viability within the tested concentrations (1–5 mg mL{sup -1}) as compared to uncoated La{sub 0.7}Sr{sub 0.3}MnO{sub 3}. All these findings explore the potentiality of La{sub 0.7}Sr{sub 0.3}MnO{sub 3} nanoparticles for magnetic fluid hyperthermia. - Highlights: • Surface functionalization of LSMO nanoparticles — first time with PVA • Surface functionalization of LSMO nanoparticles — first time with PEG • BSA protein — first time used as dispersion medium for stability of LSMO nanoparticles • The heating ability observed at low concentration • Improved efficiency of magnetic fluid hyperthermia treatment with surfactants.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2010

Magnetization studies on {epsilon}-Fe{sub 2.4}Co{sub 0.6}N nanoparticles

{epsilon}-Fe{sub 2.4}Co{sub 0.6}N nanoparticles are prepared by nitridation of ultrafine iron-cobalt oxide in NH{sub 3} gas atmosphere at 873 K for 3 h. Their magnetic properties are studied using ac and dc magnetization techniques. Two peaks at 69 and 151 K are found in ac susceptibility study. The former peak is assigned to superparamagnetic blocking temperature (T{sub B} {approx} 69 K), whereas the origin of the latter one could not be ascertained since it is observed only from imaginary part of ac susceptibility study. The positions of peaks are found to be dependent on the applied fields and frequencies. Also, dc magnetization studies corroborate T{sub B}. Anisotropy constant (K{sub a}) is found to be 2.3 x 10{sup 5} erg/cm{sup 3}. The peaks disappear at high-applied field due to the overcome of applied filed over anisotropic energy. Ferromagnetic domains rotate incoherently. At low temperature, Bloch law cannot be applied, but Curie law can be applied above T{sub B}. Interestingly, spin relaxation is faster at 10 K as compared to that at 70 K indicating the presence of frustration of spins at lower temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Structural and magnetic properties of a mechanochemically activated Ti-Fe{sub 2}O{sub 3} solid mixture

The mechanochemical effects on the reactivity and properties of a titanium/hematite powder mixture with molar ratio of 1/2 are investigated. Crystalline-phase structure, composition, hyperfine and magnetic behaviors were analyzed as a function of activation time by means of X-ray diffraction, scanning electron microscopy, Moessbauer spectroscopy and vibrating sample magnetometry. The results showed that at relatively short activation times metallic Ti reduces part of the ferric ions, yielding a complex product formed mainly by a mix of two solid solutions Fe{sub 3-x}Ti{sub x}O{sub 4} (titanomagnetites), both with very different x values (0 < x < 1). Also metallic iron and superparamagnetic hematite particles were detected by Moessbauer spectroscopy. As the mechanical treatment extends the composition of the reactive mixture changes, prevailing in the end the solid solution with higher x value. In contrast, when these activated samples are thermally treated the fraction of the solid solution which is richer in Ti diminishes. This fact produces a significant variation of the saturation magnetization of the obtained material.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Magnetic phase composition of strontium titanate implanted with iron ions

Highlights: Black-Right-Pointing-Pointer The origin of RT-ferromagnetism in iron implanted strontium titanate. Black-Right-Pointing-Pointer Metallic iron nanoclusters form during implantation and define magnetic behaviour. Black-Right-Pointing-Pointer Paramagnetic at room temperature iron-substituted strontium titanate identified. -- Abstract: Thin magnetic films were synthesized by means of implantation of iron ions into single-crystalline (1 0 0) substrates of strontium titanate. Depth-selective conversion electron Moessbauer spectroscopy (DCEMS) indicates that origin of the samples magnetism is {alpha}-Fe nanoparticles. Iron-substituted strontium titanate was also identified but with paramagnetic behaviour at room temperature. Surface magneto-optical Kerr effect (SMOKE) confirms that the films reveal superparamagnetism (the low-fluence sample) or ferromagnetism (the high-fluence sample), and demonstrate absence of magnetic in-plane anisotropy. These findings highlight iron implanted strontium titanate as a promising candidate for composite multiferroic material and also for gas sensing applications.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Electromagnetic and microwave-absorbing properties of magnetite decorated multiwalled carbon nanotubes prepared with poly(N-vinyl-2-pyrrolidone)

Graphical abstract: The Fe{sub 3}O{sub 4}/MWNTs hybrids prepared with PVP achieve a maximum reflection loss is -35.8 dB at 8.56 GHz, and the bandwidth below -10 dB is more than 2.32 GHz. More importantly, a new reflection loss peak occurs at the frequency of 14.6 GHz, which indicates that the Fe{sub 3}O{sub 4}/MWNTs hybrids have better absorption properties in the high-frequency range. Highlight: Black-Right-Pointing-Pointer The Fe{sub 3}O{sub 4} decorated MWNTs hybrids were prepared using PVP as dispersant. Black-Right-Pointing-Pointer Many more Fe{sub 3}O{sub 4} particles were attached homogeneously on the surface of MWNTs. Black-Right-Pointing-Pointer The Fe{sub 3}O{sub 4}/MWNTs hybrids achieve a maximum reflection loss of -35.8 dB at 8.56 GHz. Black-Right-Pointing-Pointer A new reflection loss peak occurs at the high-frequency of 14.6 GHz. -- Abstract: The magnetite (Fe{sub 3}O{sub 4}) decorated multiwalled carbon nanotubes (MWNTs) hybrids were prepared by an in situ chemical precipitation method using poly(N-vinyl-2-pyrrolidone) (PVP) as dispersant. The structure and morphology of hybrids are characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and transmission electron-microscopy (TEM). The TEM investigation shows that the Fe{sub 3}O{sub 4}/MWNTs hybrids exhibit less entangled structure and many more Fe{sub 3}O{sub 4} particles are attached homogeneously on the surface of MWNTs, which indicated that PVP can indeed help MWNTs to disperse in isolated form. The electromagnetic and absorbing properties were investigated in a frequency of 2-18 GHz. The results show that the Fe{sub 3}O{sub 4}/MWNTs hybrids exhibit a superparamagnetic behavior and possess a saturation magnetization of 22.9 emu/g. The maximum reflection loss is -35.8 dB at 8.56 GHz, and the bandwidth below -10 dB is more than 2.32 GHz. More importantly, a new reflection loss peak occurs at the frequency of 14.6 GHz, which indicates that the Fe{sub 3}O{sub 4}/MWNTs hybrids have better absorption properties in the high-frequency.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Fe{sub 3}O{sub 4} and CdS based bifunctional core–shell nanostructure

Highlights: ► First report on a room temperature aqueous process for growth of a hybrid core shell nanostructure containing a magnetic core and a semiconducting shell. ► Formation of distinct core shell nanostructure revealed by high resolution transmission electron microscopy. ► A bifunctional nature combining magnetic as well as photoresponce for the as synthesised core shell nanostructures demonstrated. ► A tendency towards self organisation of the core–shell nanostructure. ► Possible applications including purification and isolation of biological materials, drug delivery system, bio-labels, spintronics, etc. -- Abstract: A room temperature solution process for synthesis of Fe{sub 3}O{sub 4} nanoparticles and their hybrid core shell nanostructures using CdS as the shell material has been described. The as grown particles have been characterised using XRD, Rietveld refinement, high resolution transmission electron microscopy, atomic force microscopy, superconducting quantum interference device, optical absorbance and photoluminescence spectroscopy. A superparamagnetic response revealed from the magnetisation measurements of the as synthesised magnetite nanoparticles was retained even after the growth of the CdS shell. From luminescence and high resolution atomic force microscopy measurements, it is shown that the core–shell structures advantageously combine magnetic as well as fluorescence response with a tendency towards self-organization.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Preparation of magnetic photocatalyst nanoparticles—TiO{sub 2}/SiO{sub 2}/Mn–Zn ferrite—and its photocatalytic activity influenced by silica interlayer

Highlights: ► TiO{sub 2}/SiO{sub 2}/Mn–Zn ferrite acts as magnetic photocatalyst nanoparticle. ► SiO{sub 2} interlayer is used to prevent electron migration between photocatalyst and magnetic core. ► TiO{sub 2}/Mn–Zn ferrite without SiO{sub 2} interlayer shows poor magnetic and photocatalytic property. -- Abstract: A magnetic photocatalyst, TiO{sub 2}/SiO{sub 2}/Mn–Zn ferrite, was prepared by stepwise synthesis involving the co-precipitation of Mn–Zn ferrite as a magnetic core, followed by a coating of silica as the interlayer, and titania as the top layer. The particle size and distribution of magnetic nanoparticles were found to depend on the addition rate of reagent and dispersing rate of reaction. The X-ray diffractometer and transmission electron microscope were used to examine the crystal structures and the morphologies of the prepared composites. Vibrating sample magnetometer was also used to reveal their superparamagnetic property. The UV–Vis spectrophotometer was employed to monitor the decomposition of methylene blue in the photocatalytic efficient study. It was found that at least a minimum thickness of the silica interlayer around 20 nm was necessary for the inhibition of electron transference initiated by TiO{sub 2} and Mn–Zn ferrite.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (0 ≤ x ≤ 1) nanocrystalline solid solution prepared by the polyol method: Characterization and magnetic properties

Highlights: ► Co–Zn ferrite nanoparticles were produced by soft chemistry. ► Cation distribution deviation from the thermodynamically stable one was evidenced. ► The magnetic characteristics were affected and differ from those of bulks. -- Abstract: Highly crystalline stoichiometric Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (0 ≤ x ≤ 1) nanoparticles were successfully synthesized by the polyol process. X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), transmission electron microscopy (TEM), infrared spectroscopy (IR), zero-field {sup 57}Fe Mössbauer spectrometry and magnetic measurements using a SQUID magnetometer were employed to investigate the effect of the substitution of Zn{sup 2+} ions for Co{sup 2+} ones on the structure, and the magnetic properties of the cobalt ferrite, CoFe{sub 2}O{sub 4}. The unit cell parameter almost increases linearly with increasing Zn concentration, x, following Vegard's law. The red and blue shifts observed for the metal-oxygen ν{sub 1} and ν{sub 2}IR vibration bands, respectively, were consistent with the preferential entrance of Zn{sup 2+} ions in tetrahedral sites. Besides, detailed magnetic investigation in correlation with the cation distribution has been reported. All the particles exhibit superparamagnetic behaviour at room temperature. In addition, the magnetic characteristics (blocking temperature, saturation magnetization, coercivity, Curie temperature) clearly depend on the chemical composition and cation distribution. Both the blocking temperature and Curie temperature decrease drastically with Zn composition, x, increase. Further, the saturation magnetization follows an almost bulk-like behaviour with values notably larger than that of the bulk, mainly attributed to cation distribution deviation.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Solvothermal in situ synthesis of Fe{sub 3}O{sub 4}-multi-walled carbon nanotubes with enhanced heterogeneous Fenton-like activity

Graphical abstract: After purification, the multi-wall carbon nanotubes (MWCNTs) act as seeds for Fe{sub 3}O{sub 4} nanoparticles heterogeneous nucleation. The Fe{sub 3}O{sub 4} nanoparticles with diameter range of 4.2–10.0 nm synthesized in situ on the MWCNTs under solvothermal condition. The formed nano Fe{sub 3}O{sub 4}-MWCNTs decolorized the Acid Orange II effectively via Fenton-like reaction. Highlights: ► The amount of water tunes size and size distribution of the Fe{sub 3}O{sub 4} nanoparticles (FNs). ► FNs are homogeneously coated on the multi-walled carbon nanotubes (MWCNTs). ► FNs have diameters in the range of 4.2–10.0 nm, average grain size of 7.4 nm. ► Fe{sub 3}O{sub 4}-MWCNTs are used as a Fenton-like catalyst to decompose Acid Orange II. ► Fe{sub 3}O{sub 4}-MWCNTs displayed a higher activity than nanometer-size Fe{sub 3}O{sub 4}. -- Abstract: Fe{sub 3}O{sub 4}-multi-walled carbon nanotubes (Fe{sub 3}O{sub 4}-MWCNTs) hybrid materials were synthesized by a solvothermal process using acid treated MWCNTs and iron acetylacetonate in a mixed solution of ethylene glycol and ultrapure water. The materials were characterized using X-ray powder diffraction, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, and vibrating sample magnetometry. The results showed that a small amount of water in the synthesis system played a role in controlling crystal phase formation, size of Fe{sub 3}O{sub 4}, and the homogeneous distribution of the Fe{sub 3}O{sub 4} nanoparticles deposited on the MWCNTs. The Fe{sub 3}O{sub 4} nanoparticles had diameters in the range of 4.2–10.0 nm. They displayed good superparamagnetism at room temperature and their magnetization was influenced by the reaction conditions. They were used as a Fenton-like catalyst to decompose Acid Orange II and displayed a higher activity than nanometer-size Fe{sub 3}O{sub 4}.

36 MATERIALS SCIENCE↗