High temperature annealing effect on structural and magnetic properties of Ti/Ni multilayers

High temperature annealing effect on structural and magnetic properties of Ti/Ni multilayer (ML) up to 600 °C have been studied and reported in this paper. Ti/Ni multilayer samples having constant layer thicknesses of 50 Å each are deposited on float glass and Si(1 1 1) substrates using electron-beam evaporation technique under ultra-high vacuum (UHV) conditions at room temperatures. The micro-structural parameters and their evolution with temperature for as-deposited as well as annealed multilayer samples up to 600 °C in a step of 100 °C for 1 h are determined by using X-ray diffraction (XRD) and grazing incidence X-ray reflectivity techniques. The X-ray diffraction pattern recorded at 300 °C annealed multilayer sample shows interesting structural transformation (from crystalline to amorphous) because of the solid-state reaction (SSR) and subsequent re-crystallization at higher temperatures of annealing, particularly at ≥400 °C due to the formation of TiNi₃ and Ti₂Ni alloy phases. Sample quality and surface morphology are examined by using atomic force microscopy (AFM) technique for both as-deposited as well as annealed multilayer samples. In addition to this, a temperature dependent dc resistivity measurement is also used to study the structural transformation and subsequent alloy phase formation due to annealing treatment. The corresponding magnetization behavior of multilayer samples after each stage of annealing has been investigated by using Magneto-Optical Kerr Effect (MOKE) technique and results are interpreted in terms of observed micro-structural changes.     

An automated laboratory EXAFS spectrometer of Johansson type: indigenous development and testing

An automated linear laboratory EXAFS spectrometer of the Johansson type has been indigenously developed. Only two translational motions are required to achieve the necessary Rowland circle configuration for the (fixed) X-ray source, the dispersing and focusing bent crystal and the receiving slit. With the available crystals the spectral region from 5 to 25 keV can be scanned. The linear motions of the crystal and receiving slit including the detector assembly are achieved by employing software-controlled DC motors and utilizing optical encoders for position sensing. The appropriate rotation of the crystal is achieved by the geometry of the instrument. There is a facility to place the sample alternately in the path of the X-ray beam and out of the path to record both the incident X-ray intensityI ₀ and the transmitted intensityI employing the scintillation detector. An arrangement with a two-window proportional detector before the sample to measureI ₀ and the scintillation detector to recordI is also developed; in this case it is not necessary to oscillate the sample. Fast electronic circuits are employed to minimize counting errors. The instrument is user-friendly and it is operated through a menu-driven IBM compatible PC. EXAFS spectra of high resolution have been recorded using the spectrometer and employing the Si(111) reflecting planes; the X-ray source being a Rigaku 12 kW rotating anode with Cu target. We describe the spectrometer and discuss its performance with a few representative spectra.     

An efficient total synthesis of sulfobacin A

A short and efficient enantioselective synthesis of sulfobacin A has been achieved using the Sharpless asymmetric dihydroxylation and the regiospecific nucleophilic opening of a cyclic sulfate as the key steps.     

Synthesis of novel chiral spirodione, (6R,7R)-7-phenyl-1-oxaspiro[5.5]undec-3-ene-2,5-dione: application to the asymmetric Diels-Alder reaction with high π-facial selectivity

The synthesis of the title spirodione, a new class of auxiliary based chiral synthon using (−)-trans-2-phenylcyclohexanol and its application to the asymmetric Diels-Alder reaction are described. Methodology for detachment of the chiral auxiliary from the cycloadduct has been developed.     

Synthesis and structural characterisation of a novel tris-methylene bridged compound (NO) 4Fe2 Se(μ-CH2)3

The tris-methylene bridged compound (NO)₄Fe₂Se(μ-CH₂)₃ has been isolated. It has been characterised by IR and ¹H, ¹³C, and ⁷⁷Se NMR spectroscopy. Its structure has been determined by single-crystal X-ray diffraction methods. The structure consists of a heavy atom triangle consisting of one Se and two Fe atoms. The Fe-Fe and the two Fe-Se edges are bridged by methylene groups.     

Intramolecular nitrone cycloaddition reaction on carbohydrate-based precursors: application in the synthesis of spironucleosides and spirobisnucleosides

A simple synthesis of chiral spironucleosides and spirobisnucleosides is described. Intramolecular 1,3-dipolar nitrone cycloaddition reaction of d-glucose-derived precursors having olefin at C-3 and nitrone at C-5, C-1, or C-2 (in nor-series) furnished bisisoxazolidinospirocycles 4-7, 11, and 12 in good yields. Reductive ring opening of the isoxazolidine moieties in 4-6 followed by construction of a nucleoside base upon the generated amino groups smoothly yielded spirobisnucleosides 17 and 18 and spironucleosides 20 and 21.     

Reaction kinetics of the selective liquid phase hydrogenation of styrene oxide to β-phenethyl alcohol

Liquid phase hydrogenation of styrene oxide using 1% Pd/C and NaOH as a promoter was found to give selectively β-phenethyl alcohol (PEA) under very mild conditions (313–333 K; 0.68–5.5 MPa). The kinetics of this system was investigated by collecting initial rate data in a batch slurry reactor. Rate of hydrogenation was found to decrease beyond a certain concentration of both hydrogen (>3 MPa) and styrene oxide (>0.5 kmol/m³). A Langmuir–Hinshelwood type rate equation has been proposed based on the initial rate data in the kinetic regime. The model predictions agree very well with the experimentally observed concentration–time data indicating the applicability of the proposed rate model.