PbS microcrystals with a magic‐square‐like structure prepared by a simple hydrothermal method

PbS microcrystals with a magic‐square‐shaped structure were successfully fabricated via a simple hydrothermal route, employing (CH₃COO)₂Pb and Na₂S₂O₃ as the lead and sulfur source without the assistance of any surfactant or template. S₂O₃^2‐ ions acted not only a supplier of S^2‐ ions but also a coordinating reagent. The formation of the above morphology was the direct result of the coordination between thiosulfate ions and lead ions. Researches indicated that the different synthetic approach could influence the morphology of the final product. A possible formation mechanism was suggested. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation of PbS nano‐microcrystals with different morphologies and their optical properties

PbS nano‐microcrystals were prepared from Pb(OAc)₂·3H₂O and sulfur in a solution without any surfactant using the solvothermal process. Different morphologies, mainly including polyhedron microcrystals and sphere‐like assemblies, were characterized using a scanning electron microscope (SEM) and a transmission electron microscope (TEM). PbS nano‐microcrystals with cubic crystal structure were detected using X‐ray diffraction (XRD), electron diffraction (ED) and high resolution transmission electron micrograph (HRTEM) techniques. The optical properties were investigated by ultraviolet‐visible (UV‐vis) spectroscopy, and photoluminescence spectroscopy (PL). The UV‐vis absorption peaks of PbS exhibited a large blue‐shift and the PL spectra had a strong and broad emission bands centered at 408 nm. The crystal growth mechanism of PbS was also discussed.     

Synthesis of flower‐like zinc oxide and polyaniline with worm‐like morphology and their applications in hybrid solar cells

ZnO with a “flower‐like” morphology was synthesized using a simple microwave assisted hydrothermal method and used as an acceptor material in hybrid solar cells. X‐Ray diffraction and Raman Spectroscopy confirmed the formation of a highly crystalline wurtzite ZnO structure. A highly crystalline and conductive polyaniline with “worm‐like” morphology was synthesized by chemical polymerization of aniline using KH(IO₃)₂ as an oxidant and was used as a donor material for solar cells. The morphology was probed by using scanning and transmission electron microscopy. Polyaniline with worm‐like morphology had a diameter of 160 nm and about 2 µm long. Solar cell device fabricated from PANI/ZnO active bilayer demonstrated a fill factor of about 22.8%. Upon blending PANI with ZnO the fill factor was improved to 25.6% and efficiency by almost 100 fold when PANI:ZnO 1:1 composite was used as an bulk heterogeneous active layer. The fill factor was further improved to 26.4% when device architecture was changed to diffused bilayer. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of 1‐phenyl‐3‐(propan‐2‐yl)‐1H‐pyrazol‐5‐ol single crystals

The synthesis of pyrazoles and its derivatives remains of great interest due to their wide applications in pharmaceutical and agrochemical industry. The 1‐phenyl‐3‐(propan‐2‐yl)‐1H‐pyrazol‐5‐ol was synthesized. The 1‐phenyl‐3‐(propan‐2‐yl)‐1H‐pyrazol‐5‐ol single crystals were grown by slow solvent evaporation technique using mixture of chloroform and methanol as a solvent. Yellowish and transparent crystals having maximum dimensions of 0.005 m × 0.004 m × 0.002 m were grown. The crystals were characterized by powder XRD, FT–IR, TG–DTA–DSC and dielectric study. The crystals remained stable up to 160 °C and then start decomposing. The DSC suggested both endothermic and exothermic reactions. One broad exothermic peak was observed at 558.1 °C due to complete decomposition of the sample into the gaseous phase and reaction within the products. Thermodynamic and Kinetic parameters of decomposition were calculated by Coats–Redfern formula. The dielectric study was carried out in the frequency range from 50 Hz to 5 MHz at room temperature. The dielectric constant decreased as the frequency of the applied field increased. The variations of dielectric loss, a.c. conductivity and a.c. resistivity also studied with the frequency of the applied field. Jonscher's power law was verified for a.c. conductivity.     

Ag@Fe3O4 nanowire: fabrication,characterization and peroxidase‐like activity

With a facile solvothermal method, Ag@Fe₃O₄ nanowire was successfully prepared and characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The obtained Ag@Fe₃O₄ nanowire posses enhanced peroxidase‐like activity with good stability and high absorbance. The optimization of pH, H₂O₂ concentration and loading capacity were carried out. The result of kinetic analysis indicates that the catalyzed reaction followed a Michaelis‐Menten behavior. The good peroxidase‐like activity makes Ag@Fe₃O₄ nanowire be promising for real application in biomedicine.     

A simple surfactant‐free route for preparation of flower‐like crystals of CoS with hierarchitectures

Hierarchical cobalt sulfide crystals with flower‐like microstructures were successfully prepared by a simple one‐pot solvothermal route, employing CoCl₂·6H₂O as a cobalt precursor and KSCN as a sulfur source. The morphology of these microstructures can be easily controlled by adjusting the molar ratio of glycol to DMF in the solvent. The products were characterized by XRD and SEM. Possible formation mechanisms of CoS hierarchical microspheres are proposed. The influences of the nature of reaction media on the morphological evolution were also investigated and it was found that the ratio of DMF to glycol was of great importance for the formation of CoS morphology.     

Growth and characterization of magneto‐optical YFeO3 crystals

The floating zone growth of magneto‐optical crystal YFeO₃ has been investigated. The polycrystalline feed rod was prepared by a pressure of 250MPa and sintering at about 1500°C. A crack‐ free YFeO₃ single crystal has been successfully grown. The crystal preferred to crystallize along <100> direction with about 10° deviation. The X‐ray rocking curve of the crystal has a FWHM of 24 arcsec, confirming the high crystal quality of the sample. The (100) plane was etched by hot phosphoric acid and the dislocation density was about 10⁴/cm². A thin outer layer with Y₂O₃‐rich composition was found at the periphery of as‐grown crystals, which was attributed to the Fe₂O₃ evaporation during growth. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation of dendritic‐like CdS by hydrothermal method and its photocatalytic performance

In this article, dendritic‐like CdS has been prepared by a hydrothermal method using thiourea as the sulfur source, and the effects of experimental conditions on the morphologies of CdS have been investigated. The performances of CdS have been analyzed by X‐ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and the fluorescence and photodegradation properties of CdS have also been investigated. The XRD result indicates that the dendritic‐like CdS are of hexagonal phase and they are highly crystallized. Also, the FESEM results show that the ratio of raw material affects the yield of CdS, the reaction time affects the morphology of CdS. The best morphology of CdS is dendritic structures and the length is about 6 μm. The fluorescence spectrum shows three peaks at 470 nm, 513 nm and 547 nm, which indicates that the dendritic‐like CdS mainly emits green and blue fluorescence. Moreover, the dendritic‐like CdS exhibits good photocatalytic activity and its photodegradation rate to methylene blue can reach 92%. The growth mechanism for the formation of CdS with dendritic structure is also described.     

Thermoelectrical properties of In1‐xGaxAs and InAs crystals irradiated with fast electrons

The thermoelectric power in In_1‐xGa_xAs (x = 0,01;0,04) solid solutions and InAs crystals irradiated with fast electrons by the energy of 6 MeV and dose of 10¹⁶‐ 2 x 10¹⁷ el/cm^‐2 on the interval 80‐400 K have been investigated. It is revealed that in the all crystals the value of the thermoelectric power is decreased under irradiation that resulted from the growth of the free electron concentration to form radiation induced defects of the donor type. It has been determined that in the initial InAs after irradiation, the charge carriers scatter on optical phonons and in In_1‐xGa_xAs solid solutions they do on optical phonons and ionized impurities. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Optical properties of flower‐like CdS prepared by a hydrothermal method with SDBS as surfactant

In this article, flower‐like CdS structures have been prepared by a hydrothermal method with SDBS as surfactant. The influences of different experimental conditions on the morphologies, UV‐Vis and fluorescence properties of CdS have been investigated. The performances of CdS have been analyzed by X‐ray diffraction (XRD), field emission scanning electron microscopy (FESEM), ultraviolet‐visible (UV–Vis) and room‐temperature photoluminescence (PL). The XRD result indicates that the flower‐like CdS structures are of hexagonal phase. The FESEM results indicate that the main role of SDBS is to make the CdS crystals assemble together to form the flower‐like structures. The UV–Vis results show CdS has a strong absorption in the ultraviolet region and visible‐light region. The PL results show CdS has two emission peaks, respectively at 461 nm and 553 nm. The growth mechanism for the formation of flower‐like CdS structures is also described.     

Growth,structural and optical properties of 12%‐deuterated KDP crystals

K(D_0.12H_0.88)₂PO₄ crystals were chosen to be used for quadratic nonlinear medium of wideband frequency doubling at 1 μm. A key limitation on this application is that little information can be found in the previous reports. In this work, growth as well as structural and optical properties of this crystal were investigated in detail. Experimental results in comparison with KDP indicate that lattice parameter along a‐axis changes much more than lattice parameter c and infra‐red absorption edge shift by 0.08 μm accompanied with increasing of transmittance in the whole region. With the introduction of deuterium atom, peak of ν₁(PO4) shifts to lower wave number and transverse stimulated Raman scattering was effectively suppressed. Extra‐ordinary and ordinary indices were also measured as function of wavelength. Good crystalline perfection and great performance of damage threshold also indicate that 12%‐DKDP is an appropriate choice in the application of wideband frequency doubling at 1 μm.     

Cobalt phthalocyanine nanowires: Growth,crystal structure,and optical properties

Cobalt phthalocyanine nanowires with new crystal structure and broad optical absorption spectra were fabricated by using organic vapor phase deposition method. The morphology, crystal structure and optical properties of CoPc nanowires were characterized by SEM, X‐ray diffraction, Fourier transform infrared and UV‐visible spectroscopies. Analyses of X‐ray diffraction patterns and Fourier transform infrared spectra indicate that the crystal structure of CoPc nanowires represents a new polymorph, which is designated J‐CoPc. These J‐CoPc nanowires with high directionality (average diameter ∼50 nm) surprisingly possess much broader optical absorption spectra in the visible spectral region than those of the α‐ and β‐phase CoPc, enabling high potential for practical applications in novel molecular electronic/optical devices.     

Crystal structure,spectroscopic studies and non‐linear optical properties of 2‐amino‐3‐nitropyridinium trichloroacetate

A new quadratic nonlinear optical crystal, 2‐amino‐3‐nitropyridinium trichloroacetate (2A3NPTCA), was synthesized and the single crystals were grown by slow evaporation method at room temperature. Single crystal X‐ray diffraction and powder X‐ray diffraction experiments were carried out in order to confirm the structure and crystalline nature of 2A3NPTCA crystal. The chemical bonding and various functional groups present in the 2A3NPTCA were identified from FT‐IR spectrum. The UV–visible–NIR transmission spectrum shows that it is suitable for frequency‐converting in the wavelength region of 431–1200 nm. Thermogravimetric (TG) and differential thermal analysis (DTA) were carried out to characterize the thermal behaviors of the grown crystals. Kurtz and Perry powder method for second harmonic generation (SHG) measurements demonstrate that 2A3NPTCA is a phase matching material and its nonlinear optical efficiency is two times that of KDP. All the above results suggest that 2A3NPTCA is a potential candidate of NLO material.     

Effect of γ‐irradiation on spectral properties of undoped Y2SiO5 crystals

The absorption spectra of undoped Y₂SiO₅ crystals were studied before and after γ‐irradiation. After γ‐irradiation, the additional absorption peaks at 260‐270 and 320nm were observed in as‐grown and H₂‐annealed Y₂SiO₅ crystal, but it did not occur in air‐annealed Y₂SiO₅ crystal. These absorption peaks were attributed to F color centers and O^– hole centers, respectively. Owing to more oxygen vacancies and color centers in H₂‐annealed Y₂SiO₅ crystal than that in as‐grown Y₂SiO₅ crystal after γ‐irradiation, the additional absorption peaks were more intense in the former than that in the latter. With the irradiation dose increasing from 20 to 220kGy, the intensity of additional absorption peaks increased. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Synthesis,characterization and X‐ray crystal structure of guanidinuim (pyridine‐2,6‐dicarboxylato)(pyridine‐2,6‐monocarboxylato) zincate(II) mono pyridine‐2,6‐dicarboxylic acid tetrahydrate

A new complex of Zinc(II) and guanidinium pyridine–2,6–dicarboxylate proton transfer compound, (GnH)₂ (pydc), was synthesized and characterized using IR, ¹H NMR and ¹³C NMR spectroscopy and single crystal X–ray diffraction. The chemical formula and space group of the resulting complex is (GnH)[Zn(pydc)(pydcH)] · (pydcH₂) · 4H₂O, P 1 where the final R value is 0.0310 for 13287 reflections collected. The [Zn(pydc)(pydcH)]^– anions and the (GnH)⁺ counter‐cations form a three‐dimensional solid‐state structure by a variety of noncovalent interactions such as ion pairing, hydrogen bonding and π–π stacking which are going to be discussed. (© 2007 WILEY ‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and optical damage resistance of Sc,Er Co‐doped LiNbO3 crystals

A series of Sc:Er:LiNbO₃ crystals have been grown by Czochralski method. Their ultraviolet‐visible (UV‐Vis) absorption spectra was measured and discussed to investigate their defect structure. The optical damage resistance of Sc:Er:LiNbO₃ crystals was characterized by the transmitted beam pattern distortion method. It increases remarkably when the concentration of Sc₂O₃ exceeds a threshold concentration. The optical damage resistance of Sc (3.0mol %):Er:LiNbO₃ is much higher than that of the Er:LiNbO₃. The intrinsic and extrinsic defects were discussed to explain the enhance of the optical damage resistance in the Sc:Er:LiNbO₃ crystals. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth,structure and optical characterization of Al‐doped ZnO nanoparticle thin films

Al‐doped ZnO nanoparticle thin films were prepared on glass substrate at the optimum temperature of (410±10) °C by spray pyrolysis technique using zinc nitrate as a precursor solution and aluminium chloride as a dopant. The dopant concentration (Al/Zn at%) was varied from 0 to 2 at%. Structural analysis of the films shows that all the films are of polycrystalline zinc oxide in nature, possessing hexagonal wurtzite structure. The films exhibit variation in peak intensities corresponding to (100), (002) and (101) reflection planes on Al‐doping. The crystallite size calculated by Scherrer formula has been found to be in the range of 35‐65 nm. The optical absorption study shows that the optical band gap in the Al‐doped films varies in the range of 3.11 – 3.22 eV. The width of localized states in the band gap estimated by the Urbach tail analysis has been found to be minimum in case of the 1 at% Al‐doped zinc oxide thin film. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation and structure of calcium peroxide‐templated porous calcium carbonate crystals

Crystalline calcium carbonate with randomly dispersed porous structure was prepared through co‐ crystallization with calcium peroxide and the following template elimination by a post heating treatment and washing with water. The artificial CaCO₃ possess abundant macro‐mesopores structures and high surface area. This approach may open a new general route for the preparation of crystals with high porosity and structure specialty. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Controllable synthesis,characterization and optical properties of Ag@AgCl coaxial core‐shell nanocables

Core‐shell structures often exhibit improved physical and chemical properties. Developing a relatively general, facile, and low temperature synthetic approach for core‐shell structures with complex compositions is still a particularly challenging work. Here we report a general chemical conversion route to prepare high quality Ag@AgCl coaxial core‐shell nanocables via the redox reaction between Ag nanowires and FeCl₃ in solution. The powder X‐ray diffraction of the Ag@AgCl coaxial core‐shell nanocables shows additional diffraction peaks corresponding to AgCl crystals apart from the signals from the Ag nanowire cores. Scanning electron microscopy and transmission electron microscopy images of the Ag@AgCl coaxial core‐shell nanocables reveal that the Ag nanowires are coated with AgCl nanoparticles. The effect of the molar ratio of Fe:Ag on the morphology and optical absorption of the Ag@AgCl coaxial core‐shell nanocables is systematically investigated. The result shows that the optical absorption of Ag nanowires decreases gradually and that of AgCl nanoparticles improves gradually with the increase of the molar ratio of Fe:Ag. The formation process of the Ag@AgCl coaxial core‐shell nanocables has been discussed in detail. The present chemical conversion approach is expected to be employed in a broad range of applications to fabricate innovative core‐shell structures with different compositions and shapes for unique properties. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a novel 2D Cu(I) complex with flexible ligand

An exploration of the Cu(I)‐L system under hydrothermal conditions, has led to the isolation of a novel framework [Cu(I)(L)]_n ( 1 ) (L = bis(3,3‐dimethyl‐4,4‐dihydro‐1H‐pyrazol‐4‐yl)methane). Single‐crystal X‐ray analysis reveals that it crystallizes in the monoclinic, space group C2/c, a = 19.781(4) Å, b =11.026(3) Å, c = 16.339(4) Å, β = 127.186(3)°. The Cu ions are linked into an extended rainbow‐like chain via L molecules. Further, these adjacent chains are united together through hydrogen‐bonded interaction to a 2D layer. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)