Carboxyl group functionalization of mesoporous carbon nanocage through reaction with ammonium persulfate

Carbon nanocage, a three dimensional cage type mesoporous carbon with very high surface area and pore volume, has been functionalized with carboxyl groups for the first time via a simple oxidation using ammonium persulfate solution (APS). The carboxyl groups functionalized carbon nanocage materials have been unambiguously characterized by various sophisticated instruments such as FT-IR, HRSEM-EDX, XRD, nitrogen adsorption, and HRTEM. The degree of carboxyl group functionalization has been controlled by the simple adjustment of the oxidation parameters such as oxidation time, APS concentration and oxidation temperature. FT-IR spectroscopy combined with the HRSEM-EDX has been used to provide a quantitative analysis of the carboxyl groups on the surface of the carbon nanocage materials before and after the APS treatment. In addition, the effect of the oxidation parameters on the structural order and the textural parameters of the carbon nanocage materials has been studied. It has been found that the role of oxidation parameters is highly critical to obtain carbon nanocage materials with a high density of carboxyl groups without affecting the structural order and the pore parameters. Thus, the reaction parameters have been carefully optimized and the best condition for the preparation of carboxyl group functionalized carbon nanocage with well-ordered structure has been proposed.     

Magnetism in BiFe<Subscript>1−x</Subscript>Ni<Subscript>x</Subscript>O<Subscript>3</Subscript>: studied through electron spin resonance spectroscopy

The effect of Ni doping in BiFe_1?xNi_xO₃ (BFNO) multiferroics are studied by X-ray diffraction (XRD), Fourier transmission infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), hysteresis loop (M–H), temperature dependent magnetization (FC-ZFC) measurements and electron spin resonance (ESR) techniques. The XRD and FTIR studies indicate that the BFNO compounds remain in rhombohedral (R3c) phase without appearance of any structural transformation due to Ni doping. The XPS studies show the oxidation states of Fe ions as 3⁺, whereas Bi is found to be in a mixed valence state of 2⁺ and 3⁺ in BFNO. The Ni ion doping enhances the saturation magnetization from 0.179 emu/g (x?=?0.025) to 2.38 emu/g (x?=?0.20), which is higher than the reported values found in literature. The FC-ZFC magnetization studies suggest the presence of a magnetic phase transition from a weak ferromagnetic to a spin glass state at low temperature. The ESR studies confirm the ferromagnetic state of BFNO samples.     

Nitrogen doping of CVD multiwalled carbon nanotubes: Observation of a large g-factor shift

Nitrogen doped multi-walled carbon nanotubes (N-CNTs) and undoped multi-walled carbon nanotubes (MWCNTs) were synthesized by a chemical vapour deposition (CVD) floating catalyst method. The N-CNTs were synthesized by the decomposition of a ferrocene/N-source/toluene (N-source = triethylamine, dimethylamine, acetonitrile) mixture at 900 °C. The undoped MWCNTs were synthesized using a ferrocene–toluene mixture without a nitrogen source under similar reaction conditions. The structure of the N-CNTs and MWCNTs was ascertained using HRTEM, SEM and Raman spectroscopy. Systematic ESR measurements of the carbon products produced, in the temperature range of 293–400 K showed line widths that were in general very large ∼ kOe. Most importantly, a large g-factor shift in samples of N-CNTs from that of the free electron g-factor was observed. Further, the shift increased with increasing temperature. The large g shift has been analysed in terms of Elliott-Wagoner and Bottleneck models. The temperature dependence of the g shift in the N-CNT samples rules out the Elliott-Wagoner type spin–orbit coupling scenario. The large g shift and temperature dependence can be qualitatively explained in terms of the Bottleneck model.     

AFM nano-plough planar YBCO micro-bridges: critical currents and magnetic field effects

The critical current (Ic) of YBa2Cu3O7-x (YBCO) AFM plough micro-constrictions is measured as a function of temperature, width and the magnetic flux density (B), which was applied perpendicular to the YBCO ab-plane and surface of the bridges. C-axis oriented thin films of YBa2Cu3O7-x were deposited on MgO substrates using an inverted cylindrical magnetron (ICM) sputtering technique. The films were then patterned into 8-10 micron size strips, using standard photolithography and dry etching processes. Micro-bridges with widths between 1.9 microm to 4.1 microm were fabricated by using atomic force microscope (AFM) nanolithography techniques. Critical current versus temperature data shows a straight-line behavior, which is typical of constriction type Josephson junctions. The Ic versus B characteristics exhibited a modulation, and a suppression of the critical current of up to 84%. It was also found that the critical current increases with increasing constriction width.     

Non-Resonant Microwave Absorption in SmFeAs<Emphasis Type="Bold">O</Emphasis><Subscript>0.80</Subscript><Emphasis Type="Bold">F</Emphasis><Subscript>0.20</Subscript>: Line Shape and Structure Evolution with Temperature

‘Non-resonant Microwave Absorption’ (NRMA) or the ‘Low field microwave absorption’ (LFMA) measurements on high-quality polycrystalline SmFeAsO_0.80F_0.20 superconducting sample were carried as functions of temperature and microwave power. The LFMA line shape is complex with two peaks namely; broad peak 1 and narrow peak 2 akin to one reported in SmFeAsO_0.88F_0.12 as reported by Onyancha et al (Supercond. Nov. Magn. 28, 2927–2934, 2015). This unquestionably illustrates that these peaks are a common feature in F-doped SmFeAsO. The LFMA signal as a function of temperature reveals that T _c ? T _? = 1K in SmFeAsO_0.80F_0.20 compared to 4 K in SmFeAsO_0.88F_0.12 (T _? is the characteristic temperature at which the narrow peak appears as we cool down the sample below T _c); hence inferring that the narrow peak is fluorine doping dependent. Furthermore, LFMA signal evolution with microwave power does not show phase reversal (anomalous absorption) at 2.227 mW which is a stark contrast to what was observed in SmFeAsO_0.88F_0.12 as reported by Onyancha et al (Physica C: Supercond. Appl. 533:49–52, 2017). The absence of phase reversal within measured microwave power indicates presence of hysteretic Josephson junction. These findings establish few non-superconducting inclusions in SmFeAsO_0.80F_0.20 system.     

Synthesis of highly ordered mesoporous P63/mmc and p6mm phases by adding alcohols to the system for the SBA-1 synthesis

The influence of acidity, alkyl chain length of alcohols, synthesis temperature and time on the molecular sieve synthesis by adding alcohols to the system for the SBA-1 synthesis were studied. Upon increasing the concentration of alcohols (C_mH_2m+1OH) in the mixture of tetraethyl orthosilicate (TEOS), cetyltriethylammonium bromide (CTEABr), HCl and H₂O, highly ordered P6₃/mmc and p6mm phases were formed when m = 2 and 3 ≤ m ≤ 6, respectively. The amount of HCl was an important factor for the phase-selection under acidic conditions.     

Second and Third Peaks in the Non-resonant Microwave Absorption Spectra of Superconducting Bi2212 Crystals

Non-resonant microwave absorption (NMA) measurements at liquid nitrogen temperature with systematic microwave power variation showed a two-peak structure in the Bi-2212 textured crystals, similar to that observed in the Bi-2212 single crystals (Srinivasu et al., in J. Supercond. Incorp. Nov. Magn. 14:41, 2001). NMA signals from the aged Bi-2212 single crystals show an emergence of a ‘third peak’ as a function of microwave power. We qualitatively interpret these second and third peaks as due to the microwave power induced phase locking of several number of junctions into coherent groups and then the destruction of the phase locking by the applied DC field leading to decoupling or fluxon motion, which gives the loss in individual junctions belonging to these otherwise coherent groups.     

Room temperature multiferroicity in Bi rich Fe deficient Gd doped Bi1.2Gd0.1Fe0.8O3

A clean signature of room temperature multiferroicity in Bi_1.2Gd_0.1Fe_0.8O₃ ceramics is observed. Samples were prepared by slow step sintering technique at 850 °C. Impurity peaks normally present in original BiFeO₃ are completely suppressed with the increase of Bi concentration. Apart from this, structural transformation took place from R3_C to Pn2₁a space group and a clear orthorhombic grain growth habit is seen by SEM microstructure. Suppression of impurity phases favors the reduction of mobile oxygen vacancies and hence reduces leakage current for which ferroelectric properties of Bi_1.2Gd_0.1Fe_0.8O₃ are enhanced. We argue that the addition of Gd is likely to suppress the spiral spin modulation and at the same time increase the canting angle which favors the enhanced ferromagnetism. Excess Bi is expected to act as point defects and occupy interstitial positions which in turn surrounded by oxygen vacancies and is likely to promote defect driven ferromagnetism with enhanced spin and electric polarization. This finding encourages further revaluation of long-discounted BiFeO₃ for multiferroics research.     

Removal of fluoride from aqueous solution by polypyrrole/Fe3O4 magnetic nanocomposite

Polypyrrole (PPy)/Fe₃O₄ magnetic nanocomposite as a novel adsorbent was prepared via in-situ polymerization of pyrrole (Py) monomer using FeCl₃ oxidant in aqueous medium in which Fe₃O₄ nanoparticles were suspended. The adsorbent was characterized by Attenuated Total Reflectance Fourier transform infrared spectroscope (ATR-FTIR), Brunauer–Emmet–Teller (BET) method, field emission scanning electron microscope (FE-SEM), high resolution transmission electron microscope (HR-TEM), X-ray photoelectron spectroscope (XPS) and X-ray diffraction (XRD). Magnetic property of the adsorbent was measured by electron spin resonance (ESR). Subsequently, the ability of the adsorbent to remove fluoride ions from aqueous solution was demonstrated in a batch sorption mode. Results reveal that the adsorption is rapid and that the adsorbent has high affinity for fluoride, which depends on temperature, solution pH and adsorbent dose. From equilibrium modelling, the equilibrium data is well described by Freundlich and Langmuir–Freundlich isotherms while the adsorption kinetics is described by the pseudo-second-order model. Thermodynamic parameters confirm the spontaneity and endothermic nature of the fluoride adsorption. Meanwhile, the fluoride adsorption proceeds by an ion exchange mechanism.