Chemical Synthesis and Characterization of Flaky h-BCN at High Pressure and High Temperature

Hexagonal boron carbonitrogen （h-BCN） compound is synthesized from a mixture of boron powder and CNH compound prepared by pyrolysis of melamine （CaH6N6） under high temperature （1400-1500℃） and high pressure （5.0-5.5 GPa）. X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and Raman spec- troscopy are used to determine the chemical composition and bonds of the product. The results show that the product has composition of B0.18C0.64N0.16 （near BC4N） and atomic-level hybrid. X-ray diffraction analysis indicates that the powder has a hexagonal network structure. Scanning and transmission electron microscopy results suggest that h-BCN compound morphology is mainly flaky in width about 1 μm and thickness 200nm.     

Preparation and capacitances of oriented attachment CuO nanosheets and the MWNT/CuO nanocomposites

CuO nanosheets formed by oriented attachment of adjacent particles and the MWNT/CuO nanocomposites have been prepared through a simple hydrothermal process. The oriented attachment of adjacent particles through [111] and [002] crystallographic planes give rise to the formation of sheetlike morphology and the related mechanisms are discussed. Some needlelike and tubelike CuO nanocrystals came into being when the nanosheets rolled up and the capacitances of as-prepared MWNT/CuO nanocomposites were measured.     

Synthesis of Cubic Boron Nitride by the Reaction of Li3N and B2O3

Cubic boron nitride is synthesized by the reaction of Li3N and B203 under high pressure and high temperature （4.0-5.0 GPa, 1350-1500℃）. The minimum pressure of cBN formation is 4.0 GPa. The present condition of cBN formation is clearly lower than the eutectic temperature of Li3BN2 and BN in the Li3N-hBN system （5.5 GPa, 1610℃）. The content of cBN in the sample increases, while the content of hBN decreases with the temperature and pressure. The maximum conversion rate （5.0 GPa, 1500℃） is about 34%, which is higher than that in the hBN-Li3N system. The cBN crystals are octahedral or tetrahedral in shape and approximately 20 μm in diameter.     

Microemulsion-mediated synthesis of cadmium zinc sulfide nanocrystals with composition-modulated optical properties

Cadmium zinc sulfide nanocrystals were synthesized by a microemulsion-mediated process, which involving two steps: the preparation of CdS (or ZnS) seeds and the succedent hydrothermal growth of ZnS (or CdS) component. The XRD results show that the cadmium zinc sulfide nanocrystals with CdS seeds present a hexagonally homogeneous alloyed structure, while the ones with ZnS seeds mainly take on the characteristic of hexagonal CdS nanocrystals. The intrinsic factors influencing the crystal structures were discussed. The UV-vis and photoluminescence (PL) spectra indicate that the optical properties of the obtained nanocrystals with CdS seeds can be continuously modulated by tuning their compositions, although their sizes and size distributions are not under a strict control. The composition-modulated strategy, along with the hydrothermal microemulsion process, will be an effective route to achieve semiconductor nanocrystals with tunable optical properties under more manageable conditions.     

Fabrication and characterization of suspended single-walled carbon nanotubes

Suspended single-walled carbon nanotubes (SWCNTs) between SiO₂ pillars via a direct lithographic route using a simple mixture of catalyst precursor [Co(III) acetylacetonate, Co(acac)₃] and conventional electron beam resist (ma-N2403) were fabricated. The catalytic electron beam resist (Cat-ER) layer plays dual roles as a catalyst and a resist layer for the growth and alignment of CNTs, respectively. The structure of the grown nanotube was characterized by Raman spectroscopy (633 nm laser excitation). Nanotubes grown from Cat-ER with Co(acac)₃ show the typical Raman spectra of SWCNTs which are characterized by the strong tangential bands near to 1590 cm⁻¹ and radial breathing modes (RBMs) in the low frequency region (<300 cm⁻¹). The calculated diameter of the probed nanotubes individually corresponds to the range 0.86-1.77 nm.     

Synthesis and optical properties of Co-doped ZnO nanofibers prepared by electrospinning

In this work, Co-doped ZnO nanofibers have been fabricated successfully by an electrospinning technique. The as-prepared nanofibers are characterized by themogravimetric analysis (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), Raman spectra and photoluminescence spectroscopy (PL). Results have showed that a wurtzite ZnO nanofibers were obtained and the PL spectrum showed a red-shift by 10 nm due to narrowing of the ZnO band gap (∼3.29 eV) as a result of Co doping. Meanwhile, Raman scattering spectra exhibited an unusual peak at 540 cm⁻¹.     

Effects of Raw Material Content on Efficiency of TiN Synthesized by Reactive Ball Milling Ti and Urea

Ti and urea mixed according to the molar ratios of 2：1, 3：1 and 4：1 axe milled under the same condition. The structures of the as-synthesized powders are analyzed by an x-ray diffractometer （XRD）. The decomposed temperature of the urea and the products decomposed are characterized by differential scanning calorimetry （DSC） and thermogravimetry analysis-Fourier transform infrared （TG-FTIR） spectrometry. The results show that the reaction progress is a diffusion reaction. The efficiency of TiN synthesized by reactive ball milling can be increased by increasing the content of Ti. The reactive ball milling time decreases from more than 90 h to 40 h correspond- ing to the content ratio between Ti and urea increasing from 2：1 to 4：1. Ammonia gas （NH3） and cyanic acid （HNCO）, the decomposed products of urea, react with the refined Ti to form TiN. The grain refinement of Ti has a significant effect on the efficiency of reactive ball milling.     

Reactive Mechanical Alloying Synthesis of Nanocrystalline Cubic Zirconium Nitride

Zirconium nitride powders with rock salt structure （γ-ZrNx） are prepared by mechanical milling of a mixture of Zirconium and hexagonal boron nitride （h-BN） powders. The products are analysed by x-ray diffraction （XRD）, scanning electron microscopy （SEM）, and Raman spectroscopy （ITS）. The formation mechanism of γ-ZrNx by ball milling technique is investigated in detail. N atoms diffuse from amorphous BN （a-BN） into Zr to form Zr（N） solid solution alloy, then the Zr（N） solid solution alloy decomposes into γf-ZrNx. No ZrB2 is observed in the as-milled samples or the samples annealed at 1050° C for 2h.     

Synthesis and magnetic properties of Ni-doped zinc oxide powders

Polycrystalline Zn_1−xNi_xO diluted magnetic semiconductors have been successfully synthesized by an auto-combustion method. X-ray diffraction measurements indicated that the 5 at% Ni-doped ZnO had the pure wurtzite structure. Refinements of cell parameters from powder diffraction data revealed that the cell parameters of Zn_0.95Ni_0.05O were a little bit larger than ZnO. Transmission electron microscopy observation showed that the as-synthesized powders were of the size ∼60 nm. Magnetic investigations showed that the nanocystalline Zn_0.95Ni_0.05O possessed room temperature ferromagnetism with the saturation magnetic moment of 0.1 emu/g (0.29 μ_B/Ni²⁺).     

Preparation and Dielectric Properties of Nanostructured ZnO Whiskers

By a novel controlled combustion synthesis method, a large number of nanostructured ZnO whiskers with different morphologies, such as tetra-needles, long-leg tetra-needles and multi-needles, are prepared without any additive in open air at high temperature. The morphologies and crystalline structures of the as-prepared ZnO nanostructured whiskers are investigated by SEM and XRD. The possible growth mechanism on the nanostructured ZnO whiskers is proposed. The experimental results indicate that the dielectric constants and losses of the nanostructured ZnO whiskers are very low, demonstrating that the nanostructured ZnO whiskers are low-loss materials for microwave absorption in X-band. However, obvious microwave absorption in nanostructured ZnO whiskers is observed. The quasi-microantenna model may be attributed to the microwave absorption of the ZnO whiskers.     

Synthesis of crystalline SrMoO4 nanowires from polyoxometalates

Crystalline SrMoO₄ nanowires were synthesized via a facile hydrothermal process at 180 °C for 10 h. α-(NH₄)₆-P₂Mo₁₈O₆₂·nH₂O, one of polyoxometalates with Dawson structure, was employed as the source of molybdates. The diameter and length of the obtained SrMoO₄ nanowires are about 20 nm and 5-10 μm, respectively. HRTEM results show that the SrMoO₄ nanowires are of high crystallinity with rough surface. However, when Na₂MoO₄·2H₂O was used, there are only SrMoO₄ nanorods with smaller aspect ratio (200/70 nm) in the similar hydrothermal process. The probable growth mechanism was discussed.     

Dielectric Response and Broadband Microwave Absorption Properties of Three-Layer Graded ZnO Nanowhisker/Polyester Composites

We design and prepare three-layer graded ZnO nanowhisker/polyester composites. The dispersion configuration of ZnO nanowhiskers in the polyester is investigated, and their microwave reflectivity curves are also measured. Experimental results have shown that the graded dispersion with ZnO nanowhiskers contributes to broadband microwave absorption. In other words, the absorption band depends on the graded dispersion configuration of ZnO nanowhiskers in polyester matrix.     

Real-time monitoring of diamond nucleation and growth using field-enhanced thermionic emission current

Diamond nucleation and growth in the combustion-flame method were monitored in real time using thermionic emission current from the deposited diamond films. It was observed that the emission current evolved over three periods, the incubation, the fast increase, and the saturation periods. Ball-shaped diamond particles, faceted diamond crystals, and diamond films with well-faceted crystals were formed in the three periods. The current from a diamond-seeded substrate started to increase immediately without an incubation period, confirming that the current is from the diamond. Therefore, the current could be used for real-time monitoring of the diamond nucleation and growth.     

The effect of microwave annealing on the electrical characteristics of lanthanum doped bismuth titanate films obtained by the polymeric precursor method

Lanthanum doped bismuth titanate thin films (Bi_3.25La_0.75Ti₃O₁₂ - BLT) were produced by the polymeric precursor method and crystallized in a domestic microwave oven and in conventional furnace. Using platinum coated silicon substrates configuration, ferroelectric properties of the films were determined with remanent polarization P_r and a coercive field E_c of 3.9 μC/cm² and 70 kV/cm for the film annealed in the microwave oven and 20 μC/cm² and 52 kV/cm for the film annealed in conventional furnace, respectively. The films annealed in conventional furnace exhibited excellent retention-free characteristics at low infant periods indicating that BLT thin films can be a promise material for use in non-volatile memories. On the other hand, the pinning of domains wall causes a strong decay at low infant periods for the films annealed in the microwave furnace which makes undesireable the application for future FeRAMS memories.     

Synthesis and physical properties of LiBC intermetallics

Polycrystalline samples of LiBC compounds, which were predicted as possible candidate for high-T_c superconductivity, have been synthesised by a flux method for a wide range of flux compositions Li_xBC (x=0.5-2.4). Scanning electron microscopy and X-ray diffraction patterns showed a plate-like morphology and a single-phase nature of LiBC samples for the starting flux composition of Li_1.25BC. The lattice constants a, c display a systematic variation with x and a maximum volume of the hexagonal unit cell at x=1.25. Electrical resistivity measurements revealed an extrinsic semiconducting behaviour of the single-phase LiBC with an activation energy of 18 meV and a maximum specific resistivity of 2.5 Ω cm at 300 K. In contrast to the theoretical prediction of high T_c, no superconducting features were detected down to 2 K both, by measurements of electrical resistivity and magnetic susceptibility. However, the results do not allow to refute the theoretical prediction because of the lack of accurate chemical analysis methods for the LiBC compounds synthesised.     

Enhanced diamond nucleation on copper substrates by graphite seeding and CO2 laser irradiation

Diamond nucleation on copper (Cu) substrates was investigated by graphite seeding and CO₂ laser irradiation at initial stages of the combustion-flame deposition. A graphite aerosol spray was used to generate a thin layer of graphite powders (less than 1 μm) on Cu substrates. The graphite-seeded Cu substrates were then heated by a continuous CO₂ laser to about 750 °C within 1 min. It was found that diamond nucleation density after this treatment was more than three times as much as that on the virgin Cu substrates. As a consequence, diamond films up to 4 μm were obtained in 5 min. The enhancement of diamond nucleation on the graphite-seeded Cu substrates was attributed to the formation of defects and edges during the etching of the seeding graphite layers by the OH radicals in the flame. The defects and edges served as nucleation sites for diamond formation. The function of the CO₂ laser was to rapidly heat the deposition areas to create a favorable temperature for diamond nucleation and growth.     

Determination of optical properties in nanostructured thin films using the Swanepoel method

We present the methodological framework of the Swanepoel method for the spectrophotometric determination of optical properties in thin films using transmittance data. As an illustrative case study, we determined the refractive index, thickness, absorption index, and extinction coefficient of a nanostructured 3 mol% Y₂O₃-doped ZrO₂ (yttria stabilized zirconia, 3YSZ) thin film prepared by the sol-gel method and deposited by dipping onto a soda-lime glass substrate. In addition, using the absorption index obtained with the Swanepoel method, we calculated the optical band gap of the film. The refractive index was found to increase, then decrease, and finally stabilize with increasing wavelength of the radiation, while the absorption index and extinction coefficient decreased monotonically to zero. These trends are explained in terms of the location of the absorption bands. We also deduced that this 3YSZ thin film has a direct optical band gap of 4.6 eV. All these results compared well with those given in the literature for similar thin films. This suggests that the Swanepoel method has an important role to play in the optical characterization of ceramic thin films.     

Electrical properties and stability of Tb-doped zinc oxide-based nonlinear resistors

The microstructure, electric field-current density (E-J), capacitance-voltage (C-V), and stability characteristics of Zn-Pr-Co-Cr-Tb oxide-based nonlinear resistors were investigated for different Tb₄O₇ amounts. It increased in the range of 8.9-42.0 in the nonlinear coefficient and in the range of 1026-6514 V/cm in the breakdown field with increasing Tb₄O₇ amount. As Tb₄O₇ amount increased, the donor density decreased in the range of 1.23×10¹⁸-0.70×10¹⁸/cm³, whereas the barrier height at grain boundaries increased in the range of 0.73-0.93 eV. A good stability was obtained in the range of 0.25-0.5 mol% in Tb₄O₇ amount.     

Long silicon nitride nanowires synthesized in a simple route

Long silicon nitride (Si₃N₄) nanowires with high purity were synthesized by heating mixtures of SiO₂ powders and short carbon fibers at 1430°C for 2 h in a flowing N₂ atmosphere. The nanowires had the length of 1–2 millimeters and the diameters of 70–300 nm, and were mainly composed of ⍺-Si₃N₄, growing along the [001] direction. The vapor–solid (VS) mechanism was employed to interpret the nanowires growth.     

On the compressive response of carbon nanotube tangles

The nonlinear bulk compressibility of entangled multiwalled carbon nanotubes is studied. The analogy with textile fibre assemblies is explored by means of the well established van Wyk model. In view of the small diameter of the nanotubes, the possible effect of adhesive van der Waals interactions at tube-tube contacts is analysed. It is found, however, that the contribution of adhesive contacts to the bulk stress should be negligible. Compression experiments are performed on multi-walled carbon nanotubes and show that van Wyk's model is able to describe the response, although the values of the dimensionless parameter k of van Wyk's model were lower than expected. There is indeed no indication that van der Waals interactions play any significant role.