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All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Depicting the roles of CuO secondary phase and heat treatment in driving the magnetic and magnetocaloric features of Pr 2/3 Sr 1/3 MnO 3 manganite

In this work, we report a detailed experimental study regarding the impact of copper oxide (CuO) secondary phase and heat treatments on the structural, magnetic, and magnetocaloric properties of the near-room temperature Pr 2/3 Sr 1/3 MnO 3 (PSMO) magnetic refrigerant. Our investigations are carried out by using structural and microstructural analyses, alongside magnetization measurements. Here, the analysis of X-ray diffraction data of PSMO(95%)-CuO(5%) (PSMO-CuO) samples shows the coexistence of both CuO and PSMO phases. Further, the microstructural analysis of PSMO-CuO reveals that the addition of CuO significantly enhances the grains size. On the other hand, the added secondary phase markedly reduces the Curie temperature (T c ) from 293 K for PSMO to about 273 K for PSMO-CuO composite while increasing the magnetocaloric effect. This decrease in T c is associated with a significant change from 162° to about 156° in the Mn-OII-Mn bond angle respectively. Moreover, performed investigations regarding the role of heat treatments unveil that the observed changes in the structural and magnetic features are mainly driven by the secondary phase that modify grains size and double-exchange interactions in the PSMO compound. Interestingly, our findings demonstrate that the Curie temperature of the PSMO and accordingly its magnetocaloric effect can be tailored by adding small amounts of CuO without need to substitution on cation sites. In the light of obtained results, a multilayered refrigerant composed of PSMO and PSMO-CuO is proposed to cover the magnetic cooling temperature range close to room-temperature. The resulting entropy change remains practically constant between 273 K and 293 K. Such a behavior is highly appreciated from a practical point of view, particularly in cases where the cooling process is carried out by using the AMR and Ericsson cycles.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Heterospin biradicals based on new piperidineoxyl-substituted 3,6-di-tert-butyl-o-benzoquinone

A nucleophilic addition reaction of 4-hydroxy-2,2,6,6-tetramethylpiperidine-1-oxyl (OH-TEMPO) to 3,6-di-tert-butyl-o-benzoquinone was used to obtain a new sterically hindered o-benzoquinone (1) containing 2,2,6,6-tetramethylpiperidineoxyl functional group, which was characterized by IR spectroscopy, mass spectrometry, elemental analysis, and X-ray diffraction. A one-electron reduction of 1 with potassium and thallium is an efficient method for the generation of earlier unknown heterospin biradicals 5a and 5b, respectively, containing nitroxide and o-semiquinone radical centers. Analysis of the hyperfine structure of the ESR spectra of biradicals 5a and 5b in solution showed that they belong to the group of heterospin biradicals with strong (J >> a) and fast exchange interaction between the radical centers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Synthesis and characterization of ester and amide derivatives of titanium(IV) carboxymethylphosphonate

A set of layered ester and amide derivatives of titanium(IV) carboxymethylphosphonate was prepared by solvothermal treatment of amorphous titanium(IV) carboxymethylphosphonate with corresponding 1-alkanols, 1,ω-alkanediols, 1-aminoalkanes, 1,ω-diaminoalkanes and 1,ω-amino alcohols and characterized by powder X-ray diffraction, IR spectroscopy and thermogravimetric analysis. Whereas alkyl chains with one functional group form bilayers tilted to the layers, 1,ω-diaminoalkanes and most of 1,ω-alkanediols form bridges connecting the adjacent layers. In the case of amino alcohols, the alkyl chains form bilayer and either hydroxyl or amino group is used for bonding. This simple method for the synthesis of ester and amide derivatives does not require preparation of acid chloride derivative as a precursor or pre-intercalation with alkylamines and can be used also for the preparation of ester and amide derivatives of titanium carboxyethylphosphonate and zirconium carboxymethylphosphonate. - Graphical abstract: Ester and amide derivatives of layered titanium carboxymethylphosphonate were prepared by solvothermal treatment of amorphous solid with alkanol or alkylamine. - Highlights: • Ester and amide derivatives of titanium carboxymethylphosphonate. • Solvothermal treatment of amorphous solid with alkanol or alkylamine. • Ester and amide formation confirmed by IR spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Gas adsorption/separation properties of metal directed self-assembly of two coordination polymers with 5-nitroisophthalate

Two new coordination polymers, namely, [Co(µ-nip)(µ-bpe)]{sub n} (1) and [Zn(µ-nip)(µ-bpe)]{sub n} (2) (nip: 5-nitroisophthalate, bpe: 1,2-bis(4-pyridyl)ethane) were hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction, IR spectroscopy, elemental analysis and thermal analysis. Moreover, atomically detailed simulation studies of complex 2 for CO{sub 2}/CH{sub 4} adsorption and separation were performed. Complex 1 consists of two dimensional (2D) (4,4) grid networks with the point symbol of 4{sup 4}.6{sup 2}. Complex 2 exhibits a 3-fold interpenetrating 3D framework with 6{sup 5}.8-dmp topology. Thermal properties of the complexes showed that both complexes were stable over 320 °C. Simulation studies demonstrated that complex 2 can separate CO{sub 2} from CH{sub 4} at low pressures at 273 K. - Graphical abstract: In this study, two new coordination polymers, namely, [Co(µ-nip)(µ-bpe)]{sub n} (1) and [Zn(µ-nip)(µ-bpe)]{sub n} (2) (nip: 5-nitroisophthalate, bpe: 1,2-bis(4-pyridyl)ethane) were hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction, IR spectroscopy, elemental analysis and thermal analysis. Moreover, atomically detailed simulation studies of complex 2 for CO{sub 2}/CH{sub 4} adsorption and separation were performed. Complex 1 consists of two dimensional (2D) (4,4) grid networks with the point symbol of 4{sup 4}.6{sup 2}. Complex 2 exhibits a 3-fold interpenetrating 3D framework with 6{sup 5}.8-dmp topology. Simulation studies demonstrated that complex 2 can separate CO{sub 2} from CH{sub 4} at low pressures at 273 K. Display Omitted - Highlights: • Two new coordination polymers with 5-nitroisophthalate and 1,2-bis(4-pyridyl)ethane. • Atomically detailed simulation studies of the complexes. • Complex 2 can be proposed as molecular sieve to separate CO{sub 2} from CH{sub 4} at low pressures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Role of Cations in the Cation-Driven Assembly Process and their Effect on the Charge Storage Properties of Bilayered Vanadium Oxide and Reduced Graphene Oxide Heterostructures in Alkali Ion Systems

Exfoliated δ-Li x V 2 O 5 ·nH 2 O (ex-LVO) and reduced graphene oxide (rGO) heterostructures were constructed using different assembling cations (i.e., Li⁺, Na⁺, and K⁺ ions). The ex-LVO and rGO nanoflakes were stacked together using a concentrated chloride solution of each assembling cation and vacuum annealed at 200 °C to form three distinct two-dimensional (2D) layered architectures. X-ray diffraction and thermogravimetric analysis confirmed that the assembling ions can control the interlayer spacing of the bilayered vanadium oxide (BVO) phase as well as impact the crystallographic water content, which in turn affects the electrochemical performance. Scanning electron microscopy, scanning transmission electron microscopy (STEM), electron energy-loss spectroscopy (EELS), and X-ray photoelectron spectroscopy confirmed that a 2D heterointerface formed between LVO and rGO and that the cations used to assemble the heterostructure are trapped in the interlayer BVO region. High-resolution STEM imaging also showed the rGO dispersion throughout the LVO layers. Moreover, STEM-EELS identified a V 2 O 3 phase that forms along the rGO interface and can stabilize the materials during cycling. A charge storage mechanism analysis, combined with the galvanostatic intermittent titration technique, found that increased interlayer spacings of the BVO phase and using the assembling cations to define intercalation sites for identical charge-carrying ions lead to improved ion diffusion and increased capacities during cycling. Therefore, the Li⁺ and Na⁺ ion assembled heterostructures showed improved charge-carrying ion diffusion and charge storage capacities in each of their respective charge storage systems (i.e., Li-ion and Na-ion half-cells). In total, the cation used for heterostructure assembly can modify the final material structure and tailor the ion diffusion and charge storage capacity to tune its properties for the desired electrochemical system using a variety of 2D materials.

25 ENERGY STORAGE↗
DOE OSTI2013

Dual phase polymer gel electrolyte based on non-woven poly(vinylidenefluoride-co-hexafluoropropylene)–layered clay nanocomposite fibrous membranes for lithium ion batteries

Graphical abstract: Display Omitted Highlights: ► P(VdF-co-HFP)–clay nanocomposite based electrospun membranes are prepared. ► The membranes are used as polymer gel electrolyte (PGE) in lithium ion batteries. ► The composite PGE shows ionic conductivity of 5.5 mS cm{sup −1} at room temperature. ► Li/PGE/LiFePO{sub 4} cell delivers initial discharge capacity of 160 mAh g{sup −1}. ► The use of prepared electrolyte significantly improved the cell performance. -- Abstract: A new approach for fabricating polymer gel electrolytes (PGEs) based on electrospun poly(vinylidenefluoride-co-hexafluoropropylene) (P(VdF-co-HFP)) incorporated with layered nanoclay has been employed to enhance the ionic conductivity and electrochemical properties of P(VdF-co-HFP) without compromising its mechanical strength. The effect of layered nanoclay on properties of membranes has been evaluated by X-ray diffraction (XRD), differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). Surface morphology of the membranes has been studied using field-emission scanning electron microscopy (FE-SEM). Polymer gel electrolytes are prepared by soaking the fibrous membrane into 1 M LiPF{sub 6} in EC/DEC. The electrochemical studies show that incorporation of layered nanoclay into the polymer matrix greatly enhanced the ionic conductivity and compatibility with lithium electrodes. The charge–discharge properties and cycling performance of Li/LiFePO{sub 4} cells comprising nanocomposite polymer gel electrolytes have been evaluated at room temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Effect of Ag in CdSe thin films prepared using thermal evaporation

It has been a general practice to dope thin films with suitable dopants to modify the properties of the films to make them more suitable for potential applications. When the dopant concentrations are low, they do not normally affect the structure and morphology of the films. However, it may lead to drastic changes in electronic properties of the films. This might result from the dopant getting incorporated into the lattice of the material of the films. Cadmium selenide is an important compound semiconductor material with an attractive energy band gap. The present work relates to an attempt made to dope CdSe thin films with silver. CdSe:Ag (1–5%) thin films were deposited on glass substrates at an optimized substrate temperature of 453 K using thermal evaporation technique. The grown films were analyzed using X-ray diffraction, scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDX) techniques. It is observed that undoped CdSe thin films and CdSe:Ag films have hexagonal structure. The grain size was found to increase marginally with an increase in the Ag concentration. The optical band gap of the films determined by optical transmission measurements agree with that of CdSe. Electrical conductivity is observed to increase from 10{sup –4} to 3.66 (Ω cm){sup –1} on addition of silver. The variation of resistance with temperature indicates that the prepared films consist of CdSe and Ag existing as two separate phases coexisting and contributing individually to the resistivity of the films.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microwave-assisted synthesis of well-shaped UiO-66-NH2 with high CO2 adsorption capacity

Highlights: • Well-shaped UiO-66-NH{sub 2} was prepared through microwave heating in a short time. • Addition of HAc improves crystallinity and CO{sub 2} adsorption capacity of the UiO-66-NH{sub 2}. • UiO-66-NH{sub 2} prepared by microwave heating shows a higher CO{sub 2}/N{sub 2} adsorption selectivity. - Abstract: In a detailed study, the influence of microwave irradiation, synthesis time and temperature, addition of acetic acid (HAc) as a modulator on the morphology, crystallinity and stability of UiO-66-NH{sub 2} is investigated to develop a reliable and reproducible strategy for the preparation of well-shaped UiO-66-NH{sub 2}. The UiO-66-NH{sub 2} were characterized by powder X-ray diffraction (PXRD), field emission scanning electron microscopy (FESEM), thermogravimetric analysis (TGA), and gas adsorption. It is found that well-shaped UiO-66-NH{sub 2} with a high CO{sub 2} adsorption capacity can be synthesized in a short time by microwave heating. The UiO-66-NH{sub 2} crystals synthesized by microwave heating are of high quality and show a superior CO{sub 2} adsorption capacity (5.8 mmol/g at 273k and 1 bar) due to the strong interactions between the −NH{sub 2} group and CO{sub 2}. The CO{sub 2}/N{sub 2} selectivity of the obtained UiO-66-NH{sub 2} at 298 K and 1 bar is 66, which is much higher than that of the pristine UiO-66 of 17.8.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Ion dynamics in nanocrystalline LiMnPO{sub 4} synthesised by novel template free hydrothermal approach

A dense core rectangular shaped nanocrystalline LiMnPO{sub 4} material was synthesized by template free sucrose assisted hydrothermal synthesis. The material possess orthorhombic crystal structure with Pnma, space group having four formula units. The structural characterization was accomplished through X-ray diffraction, thermo gravimetry/differential thermal analysis. Morphology was identified by the SEM, VSM was used to verify the magnetic behavior of the material and electrical characterization was done through impedance spectroscopy and the results were reported.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Structural and morphological characterization of Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} hydrotalcite produced by mechanochemistry method

Chlorine intercalated Mg–Al layered double hydroxides (Mg–Al–Cl–LDH) with a chemical formula Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} were successfully produced by the one-step mechanochemistry method and subsequent water washing followed by drying in oven for 1 h at 80 °C. The samples were characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FT–IR), field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS), elemental mapping analysis, transmission electron microscopy (TEM), X-ray fluorescence (XRF), and the differential thermogravimetric analysis (DTGA). Results revealed that the structural characteristics of Mg–Al–Cl–LDH were affected strongly by milling time. At the beginning of milling (up to 1 h), Hydrotalcite (HT) and Brucite were the dominant phases, while the progressive mechanical activation was completed as milling time increased, which resulted in the formation of nanostructured Mg–Al–Cl–LDH. Based on XRD and FTIR data, Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} with high purity was obtained at 5 h milling. The interlayer spacing of LDH is also strongly influenced by milling time so that it escalated from 7.737±0.001 to 8.005±0.002 (1–15 h) and then decreased to 7.937±0.001 for 20 h milled sample. Electron microscopic observation displayed that the final product had hexagonal platelet structure with lateral dimension of 20–100 nm. Therefore, the synthesis of Mg{sub 0.8}Al{sub 0.2}(OH){sub 2}Cl{sub 0.2} via mechanochemistry owing to simplicity and versatility can be a promising candidate for use in catalyst carriers, drug delivery, and gene delivery. - Graphical Abstract: TEM image of milled sample (Mg–Al–Cl–LDH). - Highlights: • Chlorine intercalated LDH was synthesized by a facile solid-state process. • Structural features of products were influenced strongly by the milling time. • XRD and FTIR spectra suggested predominant Mg–Al–Cl–LDH after 5 h milling. • Products showed hexagonal platelet structure with lateral dimension of 20–100 nm.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Synthesis and characterization of pure STW-zeotype germanosilicate, Cu- and Co-substituted STW-zeotype materials

Pure STW-type germanosilicate (denoted as GeSi-STW), Cu- and Co-containing STW-zeotype (denoted as Cu-STW and Co-STW) materials were synthesized by the hydrothermal method in the presence of an organic structure-directing agent (OSDA), N,N-diethylethylenediamine (DEEDA). The effects of the reaction mixture ratio and the incorporation of transition metals M (M=Cu and Co) on the synthesis of the pure product was investigated. The synthesized samples were characterized by powder and single-crystal X-ray diffraction (XRD), scanning electron microscopy (SEM), inductively coupled plasma analysis (ICP), thermogravimetric and differential scanning calorimetry (TG–DSC) analysis and UV–vis diffuse reflectance spectra (DRS). The results reveal that the crystallization time, the concentration of H{sub 2}O in the reaction mixture and the addition of HF all have an important impact on the synthesis of pure STW-type zeolite. GeSi-STW is stable up to 800 °C, and has much higher thermal stability than SU-32 (stable to 400 °C). Co and Cu have been introduced for the first time into STW-zeotype materials. - Graphical abstract: SEM images of GeSi-STW (A and B), Co-STW (C and D) and Cu-STW (E and F). - Highlights: • Pure STW-type germanosilicate materials were hydrothermally synthesized. • The STW-type germanosilicate has high thermal stability up to 800 °C. • Co and Cu have been introduced for the first time in the STW-zeotype materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Electron diffraction radial distribution function analysis of amorphous boron carbide synthesized by ion beam irradiation and chemical vapor deposition

Amorphous boron carbide (a-BxC) networks consist of light elements, and their low atomic scattering factors makes structural analysis by x-ray diffraction difficult. Electron diffraction has an advantage of detecting the light elements, because of the strong interaction between the matter and electrons. In this work, we prepared a-BxC by ion beam technologies and plasma-enhanced chemical vapor deposition, and characterized their structures via atomic pair-distribution functions derived from electron diffraction intensity profiles. It was found that a pentagonal pyramid is the most favorable cluster in a-B4C generated by ion irradiation, while C—C homonuclear bonds were formed in the deposited a-B x C thin film. X-ray photoemission spectroscopy revealed that the a-BxC thin film possesses more carbon than B 4 C, which is responsible for the formation of the homonuclear bonds.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Four thiophene-pyridyl-amide-based Zn{sup II}/Cd{sup II} coordination polymers: Assembly, structures, photocatalytic properties and fluorescent recognition for Fe{sup 3+}

By tuning metal ions and combining with different dicarboxylates, four new semi-rigid thiophene-bis-pyridyl-bis-amide-based coordination polymers, namely, [Zn(3-bptpa)(1,3-BDC)]·DMA·2H{sub 2}O (1), [Zn(3-bptpa)(5-MIP)] (2), [Cd(3-bptpa)(1,3-BDC)]·2H{sub 2}O (3) and [Cd(3-bptpa)(5-MIP)]·4H{sub 2}O (4) (3-bptpa=N,N′-bis(pyridine-3-yl)thiophene-2,5-dicarboxamide, 1,3-H{sub 2}BDC=1,3-benzenedicarboxylic acid, 5-H{sub 2}MIP=5-methylisophthalic acid, DMA=N,N-dimethylacetamide), were solvothermally/hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction analyses, IR spectra, UV–vis diffuse-reflectance spectra (DRS), powder X-ray diffraction (PXRD) and thermal gravimetric analyses (TG). The structural analysis reveals that Zn-complexes 1 and 2 are similar 2D networks. While Cd-complexes 3 and 4 exhibit similar 2-fold interpenetrating 3D α-Po frameworks with the (4{sup 12}·6{sup 3}) topology. The photocatalytic properties for the degradation of methylene blue (MB) under ultraviolet light irradiation of the title complexes have been investigated in detail. Furthermore, the luminescent sensing behaviors for metal cations of 1–4 have been studied, the results indicate that 3 is an excellent fluorescent probe, with high sensitivity, selectivity, and simple regeneration, for environmentally relevant Fe{sup 3+} ions. - Graphical abstract: Four Zn{sup II}/Cd{sup II} coordination polymers with a thiophene-pyridyl-amide ligand have been prepared. The photocatalytic activities and fluorescent sensing properties for metal ions of the title complexes have been investigated. - Highlights: • Four coordination polymers with thiophene-pyridyl-amide ligands have been obtained. • The central metal ions play an important role in the formation of the frameworks. • The photoluminescent sensing and the photocatalytic properties have been investigated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Rietveld refinement and dielectric relaxation of a new rare earth based double perovskite oxide: BaPrCoNbO{sub 6}

A new rare earth based double perovskite oxide barium praseodymium cobalt niobate, BaPrCoNbO{sub 6} (BPCN) is synthesized by solid-state reaction technique. Rietveld analysis of X-ray diffraction (XRD) data shows that the compound crystallizes in a perovskite like tetragonal structure which belongs to the I4/mmm space group with lattice parameters a=b=5.6828(9) Å, c=8.063(2) Å. Structural analysis reveals 1:1 ordered arrangement for the Co{sup 2+} and Nb{sup 5+} cations over the six-coordinate B-sites of BPCN. The superlattice line (1 0 1) at 2θ=19.10° arising from the alternate ordering of Co{sup 2+} and Nb{sup 5+} sites is observed in the XRD pattern which confirms the presence of cation ordering in BPCN. Fourier transform infrared spectrum shows two phonon modes of the sample due to the antisymmetric NbO{sub 6} stretching vibration. The relaxation dynamics of the conductive process in BPCN is investigated in the temperature range 303 to 503 K and in the frequency range 100 Hz to 1 MHz using impedance spectroscopy. The relaxation mechanism of the sample in the framework of electric modulus formalism is modeled by Davidson–Cole model (DCM). The values of α (distribution of relaxation time) for the DCM varies from 0.1 to 0.3 which suggests the asymmetric distribution of relaxation time for BPCN. The activation energy of the sample, calculated from both conductivity and modulus spectra, are found to be almost the same ∼0.4 eV, which indicates that the conduction mechanism for BPCN is polaron hopping. The scaling behaviour of the imaginary part of electric modulus suggests that the relaxation follows the same mechanism at various temperatures. - Graphical abstract: Rietveld refinement plot for BPCN. Inset shows the schematic presentation of the BPCN tetragonal unit cell. The Co{sup 2+} atoms are located at the centers of the CoO{sub 6} (blue) octahedra. The Nb{sup 5+} atoms are located at the centers of the NbO{sub 6} (green) octahedra. Display Omitted - Highlights: • BaPrCoNbO{sub 6} is synthesized for the first time. • Rietveld refinement of XRD data confirms tetragonal phase. • XRD confirms the presence of cation ordering in BaPrCoNbO{sub 6}. • The activation energy is ∼0.4 eV. • The conduction mechanism for BPCN is due to polaron hopping.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effects of Bi{sup 3+} Substitution on Structural, Morphological, and Magnetic Properties of Cobalt Ferrite Nanoparticles

In this research, the structural, morphological, and magnetic properties of Bi-doped cobalt ferrite (CoFe{sub 2-x}Bi{sub x}O{sub 4}) nanoparticles with x = 0.0, 0.05, 1, 0.15, and 0.2, prepared by the sol-gel method, were studied. In order to characterize the samples, several equipment and analyses including thermo-gravimetric and differential thermal analysis (TGA/DTA), X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), Fourier transform infrared spectrometer (FT-IR), and vibrating sample magnetometer (VSM) were used. The average crystallite sizes of the prepared CoFe{sub 2-x}Bi{sub x}O{sub 4} were calculated using the Scherer, UDM, SSP, and Halder-Wagner methods. The average crystallite sizes for the samples were found in the range of 26 to 44 nm, which can be attributed to the grain growth of the particles. FT-IR spectrum showed bands in the range of 430 to 590 cm{sup −1} due to the stretching vibration of an oxygen atom and metal ions (Fe-O), confirming the formation of spinel ferrite. Surface morphology of the samples was studied using FESEM. The VSM results showed that the saturation and remanence magnetizations increased by raising the doping values up to x = 0.1. The Curie temperature of the cobalt nanoferrites was determined using Faraday’s technique. The highest Curie temperature was found to be 580 °C for the undoped sample.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Ferromagnetic-to-Paramagnetic Phase Transition of MnAs Studied by Calorimetry and Magnetic Measurements

Manganese monoarsenide samples have been prepared by the sealed-ampule technique and characterized by X-ray diffraction, differential thermal analysis, and scanning electron microscopy. The hexagonal- to-orthorhombic phase transition of MnAs has been studied using differential scanning calorimetry (DSC) and magnetic measurements. The enthalpy and temperature range of the transition have been determined to be ΔH =–5.6 J/g and 312.5–319 K, respectively. The enthalpy and temperature range of the transition are influenced by the quality of the samples. The samples containing inclusions of the metastable, orthorhombic phase have a lower enthalpy and broader temperature range of the magnetostructural transformation of manganese monoarsenide. It has been demonstrated that DSC is an effective tool for assessing the quality of MnAs samples. Temperature dependences of specific magnetization and magnetic permeability for MnAs lend support to the DSC results. From these data, the Curie temperature of MnAs has been determined to be 40°C, in good agreement with previously reported data.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Synthesis and electrocatalytic performance for p-nitrophenol reduction of rod-like Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composites

Graphical abstract: The pure Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite with 5% Ag all exhibited rod-like morphology, and the microrods were actually composed of nanoparticles with mean size of 35 nm or so. - Highlights: • A facile route was designed to fabricate rod-like Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite nanomaterials. • Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite were modified on a GCE directly. • All samples exhibited enhanced catalytic property for p-nitrophenol reduction. - Abstract: Rod-like precursors of Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composites with different Ag contents were synthesized via a co-precipitation method. Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite samples were fabricated by calcining each precursor at 400 °C for 3 h. The as-prepared samples were characterized by thermogravimetric analysis and differential thermal gravimetric analysis (TGA/DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), respectively. Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composites were used as electrocatalyst modified on a glassy carbon electrode for p-nitrophenol reduction in basic solution. The results showed that p-nitrophenol could be reduced effectively on the modified electrode. By comparison with a bare glassy carbon electrode, peak current increased markedly with Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} samples, and peak potential decreased obviously with Ag/Co{sub 3}O{sub 4} samples. Ag/Co{sub 3}O{sub 4} composites with 4% Ag exhibited the highest electrocatalytic activity for p-nitrophenol reduction.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Magnetostructural martensitic transformations with large volume changes and magneto-strains in all-d-metal Heusler alloys

The all-d-metal Mn{sub 2}-based Heusler ferromagnetic shape memory alloys Mn{sub 50}Ni{sub 40−x}Co{sub x}Ti{sub 10} (x = 8 and 9.5) are realized. With a generic comparison between d-metal Ti and main-group elements in lowering the transformation temperature, the magnetostructural martensitic transformations are established by further introducing Co to produce local ferromagnetic Mn-Co-Mn configurations. A 5-fold modulation and (3, −2) stacking of [00 10] of martensite are determined by X-ray diffraction and HRTEM analysis. Based on the transformation, a large magneto-strain of 6900 ppm and a large volume change of −2.54% are observed in polycrystalline samples, which makes the all-d-metal magnetic martensitic alloys of interest for magnetic/pressure multi-field driven applications.

36 MATERIALS SCIENCE↗