Chemical etching of InP (1 0 0) wafer based on a volcanic mineral water

We have successfully demonstrated that a solution of spa water [Tamagawa Spa water (TaSW):H₂O₂ = 1:1] etches InP (1 0 0) wafer. The TaSW is a colorless acidic liquid of pH ∼1.1. It contains a considerable amount of positive ions, such as H⁺, Al³⁺, and Ca²⁺. The Cl⁻, HSO₄²⁻, and SO₄²⁻ ions are the main anions. The TaSW-etchant system provides shiny flat surfaces on the etched bottoms. The spa-etchant system has reproducible etching rates and does not erode photoresist masks. The etching kinetics is reaction-rate limited. The spa-etchant system is also found to etch GaAs (1 0 0) wafer, but the etched surface is considerably roughened.     

Synthesis of RuSr2GdCu2O8 − δ superconductors by the sol–gel route

The RuSr₂GdCu₂O_8 − δ (Ru-1212) superconductors have been prepared through the sol–gel route. We found that 1030 °C is the optimum annealing temperature for the formation of the Ru-1212 superconductors synthesized by the sol–gel route. X-ray powder diffraction analysis indicates that nearly all the peaks from the samples can be indexed to a single phase of Ru-1212, tetragonal symmetry with lattice parameters a = b = 3.382 Å, c = 11.478 Å and space group I4/mmm. The RuSr₂GdCu₂O_8 − δ superconductors prepared by the sol–gel method exhibit onset transition temperature T_c-onset near 55 K and zero resistance temperature T_c-zero at 45 K.     

Thermal behaviour of the O2/TiO2 (110)-(1 × 2) surface

Synchrotron radiation ultra-violet photoemission at different photon energies (17.1, 19.3, and 21.5 eV) has been used to study the interaction of O₂ with the TiO₂ (110)-(1 × 2) surface reconstruction at temperatures between 77 and 320 K. At 77 K the results show a weak molecular chemisorption of the O₂ molecule on the surface. By analysing the thermal behaviour of the O₂/TiO₂ system in a temperature range from 77 to 320 K, it has been found that between 120 and 200 K the O₂ molecule is dissociated.     

A thermal reduction route to nanocrystalline transition metal carbides from waste polytetrafluoroethylene and metal oxides

Starting from waste polytetrafluoroethylene (PTFE), metal oxides (TiO₂, V₂O₅, Nb₂O₅, and MoO₃) and metal sodium, several nanocrystalline transition metal carbides (TiC, VC, NbC, and Mo₂C) have been prepared through a thermal reduction route in an autoclave at 600 °C. It is found that the obtained NbC nanocrystallines have a superconducting transition temperature at 11.6 K.     

Photoluminescence properties of Y0.95 − xMxBO3:Eu3+ (M = Ca,Sr, Ba,Zn, Al, 0 ≤ x ≤ 0.1) in 100–450 nm regions

The single phases of Y_0.95 − xM_xBO₃:5%Eu³⁺ (M = Ca, Sr, Ba, Zn, Al, 0 ≤ x ≤ 0.1) were synthesized successfully by solid-state reaction. Their luminescent properties were studied under UV and VUV excitation. The results indicated that with the incorporation of Ca²⁺, Sr²⁺, Ba²⁺, Zn²⁺ or Al³⁺ into the host lattice of YBO₃:Eu³⁺, the high symmetry around Eu³⁺ was destroyed and the ratio of red emission(⁵D₀–⁷F₂) to orange one (⁵D₀–⁷F₁) increased, leading to a better chromaticity. Furthermore, the co-doping ions such as Ca²⁺, Zn²⁺ and Al³⁺ were beneficial to enhance the luminescent intensity of Eu³⁺. These phenomena were evaluated, and possible explanations were proposed.     

The influence of heat treatment on the corrosion behaviour of as-spun amorphous Al88Ni6La6 alloy in 0.01 M NaCl solution

The effect of the heat treatment on the corrosion behaviour of amorphous Al₈₈Ni₆La₆ made by melt-spun has been investigated by electrochemical measurements. Heat treatment was carried out at 523 K and 673 K for 4 min and 15 min respectively. The evolution of the crystallization process after annealing was identified by differential scanning calorimeter (DSC) as well as X-ray diffraction. The XRD patterns show that the structure of samples heat-treated at higher temperature changes towards a crystal state. The results obtained from the polarization curves reveal that all Al₈₈Ni₆La₆ alloys exhibit spontaneously passivated behaviour. Furthermore, it is noted that the partially crystallized alloy has the best corrosion resistance in comparison with as-spun amorphous and fully crystallized alloys, while the fully crystallized sample shows deterioration in the corrosion resistance.     

Preparation of MgH2 composite with a composition of 40%MgH2 + 30%LiBH4 + 30%(2LiBH4 + MgF2)

A mixture of containing two chemical equivalents of lithium borohyride and one equivalent of magnesium fluoride is known to yield hydrogen in an amount of about 7.6 wt% of the mixture when heated to about 150 °C at atmospheric pressure by the following reaction; 2LiBH₄ + MgF₂ = 2LiF + MgB₂ + 4H₂. In order to increase hydrogen storage capacity of Mg-based materials, a mixture with a composition of 2LiBH₄ + MgF₂ and LiBH₄with a higher hydrogen storage capacity of 18.4 wt% were added to MgH₂. MgH₂ composite with a composition of 40 wt%MgH₂ + 30 wt%LiBH₄ + 30 wt%(2LiBH₄ + MgF₂) was prepared by reactive mechanical grinding. The hydrogen storage properties of the sample were then examined. Hydrogen content vs. desorption time curves for consecutive 1st desorptions of 40 wt%MgH₂ + 30 wt%LiBH₄ + 30 wt%(2LiBH₄ + MgF₂) at 533–873 K showed that the total desorbed hydrogen quantity for consecutive 1st desorptions is 7.07 wt%.     

Effect of different annealing atmospheres on crystallization and corrosion resistance of Al86Ni9La5 amorphous alloy

The effect of different annealing atmospheres (H₂, air, Ar and N₂) on precipitated phases, corrosion resistance and hardness of Al₈₆Ni₉La₅ amorphous alloy was investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM), differential scanning calorimetry (DSC), thermogravimetry (TG), electrochemistry experiment and microhardness tester. During annealing at 523 K, the primary crystallized fcc-Al is independent on the annealing atmospheres. During annealing at 584 K, the final crystalline phases, i.e. fcc-Al + Al₁₁La₃ + Al₃Ni, are also independent on the different annealing atmospheres. However, during annealing at 523 K, H₂ and air can promote the eutectic crystallization process, and induce the formation of metastable Al₃Ni₂ phase. The promoting effect of different annealing atmospheres is in the order of H₂ > air > Ar > N₂. The microhardness and corrosion resistance in the 3.5 wt.% NaCl solution are improved by annealing in H₂ and air atmospheres. The property promotion caused by annealing process can be ascribed to the formation of nanocrystalline phases, which is possibly helpful to develop the alloy's application in the seawater environment.     

Microstructure and superplasticity of Mg–Al–Ca electromagnetic casting alloys after hot extrusion

Microstructure and superplastic properties of the plates extruded from the Ca containing Mg alloy (1 wt.% Ca–AZ31) billets fabricated by electromagnetic casting (EMC) without and with electromagnetic stirring (EMS) were examined. The linear intercept grain sizes of the extruded materials were 3.7 μm and 2.1 μm, respectively. The material extruded from the EMC + EMS billet exhibited good superplasticity at low temperatures as well as at high strain rates, including the tensile elongations of 370% at 1 × 10⁻³ s⁻¹, −523 K and 550% at 1 × 10⁻² s⁻¹, −673 K. These values largely exceeded those of the AZ31 alloys with the similar grain sizes. The superior superplasticity of the extruded EMC + EMS billet could be attributed to fine grains and high grain stability at elevated temperatures by the presence of finely dispersed particles of thermally stable (Al,Mg)₂Ca phase. The constitutive equations were developed for describing the high-temperature deformation behavior of the fine-grained 1 wt.% Ca–AZ31 alloys with different grain sizes in wide range of temperature and strain rate.     

Processing of enriched elemental boron (B ∼ 65 at. %)

Procedures were developed for purification and processing of electrodeposited enriched boron powder for control rod application in India's first commercial Proto Type Fast Breeder Reactor (PFBR). Methodology for removal of anionic (F⁻, Cl⁻, −₄BF${{\text{BF}}_4}^{\mathrm{-}}$) and cationic (Fe²⁺, Fe³⁺, Ni²⁺) impurities was developed. Parameters for grinding boron flakes obtained after electrodeposition were optimized to obtain the boron powder having particle size less than 100 μm. The rate of removal of impurities was studied with respect to time and concentration of the reagents used for purification. Process parameters for grinding and removal of impurities were optimized. A flowsheet was proposed which helps in minimizing the purification time and concentration of the reagent used for the effective removal of impurities. The purification methodology developed in this work could produce boron that meets the technical specifications for control rod application in a fast reactor.     

Calibration of ultrahigh vacuum gauge from 10 Pa to 10 Pa by the two-stage flow-dividing system

A new two-stage flow-dividing system has been developed for the calibration of ultrahigh vacuum gauges from 10⁻⁹ Pa to 10⁻⁵ Pa for N₂, Ar, and H₂. This system is designed based on the techniques for our previously developed calibration system in the range from 10⁻⁷ Pa to 10⁻² Pa. Three modifications were performed to extend the calibration pressure to a lower range. The relative standard uncertainty of the generated pressure (k = 1) is in the range from 2.3% to 2.6%, from 10⁻⁹ Pa to 10⁻⁵ Pa. The characteristics of ultrahigh vacuum gauges were also examined by using this system. The stabilities of the pressure reading, the linearity, the temperature dependence, and the long-term stability were examined. These results show that the calibration of ultrahigh vacuum gauges is possible in the range from 10⁻⁹ Pa to 10⁻⁵ Pa for N₂, Ar, and H₂ with the uncertainty of about 6.0% (k = 2) by this new system.     

Microwave dielectric ceramics in (Ca1− xBax)(Zn1 / 3Nb2 / 3)O3 system

(Ca_1−xBa_x)(Zn_1 / 3Nb_2 / 3)O₃ (x = 0–1.0) microwave dielectric ceramics were prepared and investigated. The Ba(Zn_1 / 3Nb_2 / 3)O₃-based solid solution was observed for x = 0.9, and the compositions with x = 0.1–0.7 resulted in the mixture of two phases. Dielectric constant ε_r and temperature coefficient of resonant frequency τ_f of the present ceramics varied anomalously and reached their maximum at x = 0.7–0.9, and these phenomena were originated from the partial substitution of small Ca²⁺ ions for larger Ba²⁺ at A-site. On the other hand, a good combination of microwave dielectric properties (ε_r = 36, Qf = 16,170 GHz, τ_f = − 12 ppm/°C) were obtained at x = 0.1, while the decreased Qf value was observed in other compositions.     

Electrical transport and magnetoresistance in La2 / 3Ca1 / 3MnO3/CuO composites

The electrical transport and magnetoresistance properties were experimentally studied for composites according to the nominal composition (1 − x)La_2 / 3Ca_1 / 3MnO₃/xCuO which were fabricated using a special chemical route (x is molar ratio). The composites display different transport behaviors for the range of x < 6% and > 6%. The introduction of CuO causes a large shift of the insulator–metal transition temperature (T_p) toward low temperature for x < 6%, while the T_p is almost independent on x for x > 6%. We also show that the magnetoresistance near T_p can be substantially increased through the introduction of CuO. The largest magnetoresistance with a value as high as ∼90% is obtained in the x = 20% composite for a rather small magnetic field (0.3 T). It is interesting to observe another transition in MR₀ vs. T curve at temperature range of 170∼200 K for the composites with CuO addition. Based on structural and microscopic analysis, unusual observations of transport and magnetoresistance are discussed.     

MgB<Subscript>2</Subscript> with addition of Sb<Subscript>2</Subscript>O<Subscript>3</Subscript> obtained by spark plasma sintering technique

Superconducting bulks of MgB₂ with addition of Sb₂O₃ and Sb with different stoichiometric compositions ((MgB₂) + (Sb₂O₃) _x , x = 0.0025, 0.005, 0.015, and (MgB₂) + (Sb)_y, y = 0.01) were obtained by the Spark Plasma Sintering (SPS) technique. All added samples have high density, above 95% and critical temperature, T _c, of 38.1–38.6 K. This result and XRD data suggest that Sb does not enter the lattice of MgB₂. Impurity phases are Mg₃Sb₂, MgO, and MgB₄. The optimum addition is Sb₂O₃ for x = 0.005. This sample shows the critical current density, J _c(5 K, 0 T) = 4 × 10⁵ A/cm² and J _c(5 K, 7 T) = 6 × 10² A/cm², while the irreversibility field, H _irr (5 K, 100 A/cm²) = 8.23 T. Indicated values of J _c and H _irr are higher than for the pristine sample. The mechanism of J _c and H _irr increase in the Sb₂O₃ added samples is complex and composed of opposite effects most probably involving morphology elements, the presence of nano metric MgB₄ and the indirect influence of oxygen or oxygen and Sb. Crystallite size of MgB₂ is decreasing when Sb-based additions are introduced and the effect is stronger for the Sb-metal addition. The sample with Sb-metal addition does not improve J _c and H _irr when compared with pristine sample.     

On the synthesis and dielectric studies of (1 − x)Bi(Mg1 / 2Zr1 / 2)O3 − xPbTiO3 piezoelectric ceramic system

Scandium free piezoelectric ceramics of the composition (1 − x)Bi(Mg_1 / 2Zr_1 / 2)O₃ − xPbTiO₃ (BMZ − xPT) were fabricated by the solid state reaction method. Dielectric and structural properties were measured and phase diagram was constructed from the temperature dependent dielectric and impedance data. The morphotropic phase boundary (MPB) was found to be located in the range 0.55 < x < 0.60 with paraelectric–ferroelectric phase transition temperature, T_C (∼ 280 °C). The ceramics near the MPB showed high room temperature dielectric constant (∼ 1387). The room temperature values of the remanent polarization (P_r) and coercive filed (E_C), were ∼ 29 μC/cm² and ∼ 23 kV/cm, respectively.     

The structural and electrical property of CuCr1 − xNixO2 delafossite compounds

A series of CuCr_1 − xNi_xO₂ (0 ≤ x ≤ 0.06) polycrystalline samples was prepared. The electrical conductivity was measured in the temperature range of 160–300 K. It was found that the electrical conductivity (σ) increases rapidly with the doping of Ni²⁺ ions. At room temperature, the σ is 0.047 S cm^− 1 for the sample with x = 0.06, which is two orders of magnitude larger than that of the CuCrO₂ sample (9.49E− 4 S cm^− 1). The Seebeck coefficients are positive for all samples, which indicate p-type conducting of the samples. The experimental results imply that it is possible to get higher electrical conductivity p-type transparent conducting oxides (TCO) from CuMO₂ by doping with divalent ions.     

Structural,optical, and electrical properties of flash-evaporated copper indium diselenide thin films

Copper indium diselenide (CuInSe₂) compound was synthesized by reacting its elemental components, i.e., copper, indium, and selenium, in stoichiometric proportions (i.e., 1:1:2 with 5% excess selenium) in an evacuated quartz ampoule. Structural and compositional characterization of synthesized pulverized material confirms the polycrystalline nature of tetragonal phase and stoichiometry. CuInSe₂ thin films were deposited on soda lime glass substrates kept at different temperatures (300–573 K) using flash evaporation technique. The effect of substrate temperature on structural, morphological, optical, and electrical properties of CuInSe₂ thin films were investigated using X-ray diffraction analysis (XRD), atomic force microscopy (AFM), optical measurements (transmission and reflection), and Hall effect characterization techniques. XRD analysis revealed that CuInSe₂ thin films deposited above 473 K exhibit (112) preferred orientation of grains. Transmission and reflectance measurements analysis suggests that CuInSe₂ thin films deposited at different substrate temperatures have high absorption coefficient (~10⁴ cm⁻¹) and optical energy band gap in the range 0.93–1.02 eV. Results of electrical characterization showed that CuInSe₂ thin films deposited at different substrate temperatures have p-type conductivity and hole mobility value in the range 19–136 cm²/Vs. Variation of energy band gap and resistivity of CuInSe₂ thin films deposited at 523 K with thickness was also studied. The temperature dependence of electrical conductivity measurements showed that CuInSe₂ film deposited at 523 K has an activation energy of ~30 meV.     

Fluorine intercalation in the n = 1 and n = 2 layered manganites Sr2MnO3.5+x and Sr3Mn2O6

Fluorine insertion into the oxygen defect superstructure manganite Sr₂MnO_3.5+x has been shown by transmission electron microscopy (TEM) to result in two levels of fluorination. In the higher fluorine content sections, the fluorine anions displace oxygen anions from their apical positions into the equatorial vacancies, thus destroying the superstructure and reverting to a K₂NiF₄-type structure (a = 3.8210(1) Å and c = 12.686(1) Å). Conversely, lower fluorine content sections retain the Sr₂MnO_3.5+x defect superstructure, crystallising in the P2₁/c space group. Fluorine intercalation into the reduced double-layer manganite Sr₃Mn₂O₆ occurs in a step-wise fashion according to the general formula Sr₃Mn₂O₆F_y with y = 1, 2, and 3. It is proposed that the y = 1 phase (a = 3.815(1) Å, c = 20.29(2) Å) is produced by the filling of all the equatorial oxygen vacancies by fluorine atoms whilst the y = 2 phase (a = 3.8222(2) Å, c = 21.2435(3) Å) has a random distribution of fluorine anions throughout both interstitial rocksalt and equatorial sites. Neutron powder diffraction data suggest that the fully fluorinated y = 3 phase (a = 3.8157(6) Å, c = 23.666(4) Å) corresponds to the complete occupation of all the equatorial oxygen vacancies and the interstitial sites by intercalated fluorine.