Facile synthesis of MnV2O6 nanostructures with controlled morphologies

MnV₂O₆ nanostructures including nanorods, nanobelts, and nanosheets, have been synthesized by a facile hydrothermal reaction between Mn(CH₃COO)₂·4H₂O and commercial V₂O₅. The synthesized products are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The influences of synthetic parameters, such as, reaction time, temperature and medium, on the morphologies of the resulting products have been investigated. As the reaction temperatures increase from 120 °C to 180 °C, MnV₂O₆ nanorods and nanobelts are obtained, respectively. The time-dependent experimental results at 180 °C reveal that the sizes of MnV₂O₆ nanobelts increase gradually with the reaction proceeding. Interestingly, as the reaction is carried out with the aid of H₂O₂ solution, flower-like MnV₂O₆ nanosheets are formed.     

Low temperature facile synthesis of anatase TiO2 coated multiwalled carbon nanotube nanocomposites

Anatase TiO₂ coated multiwalled carbon nanotube (MWNT) nanocomposites were prepared by combining the sol-gel method with a self assembly technique at a low temperature. XRD, TEM, FTIR and XPS spectra were applied to characterize the crystal phase, microstructure, and other physicochemical properties of the sample. The results showed that MWNTs were covered with a 12-20 nm thickness layer of anatase TiO₂ or surrounded by a 30 -290 nm thickness coating of anatase TiO₂. The layer or coating is constructed of TiO₂ nanoparticles about 5.8 nm. Furthermore, as-prepared composite was rich in surface hydroxyl groups.     

One-pot synthesis of intestine-like SnO2/TiO2 hollow nanostructures

In the present study the intestine-like binary SnO₂/TiO₂ hollow nanostructures are one-pot synthesized in aqueous phase at room temperature via a colloid seeded deposition process in which the intestine-like hollow SnO₂ spheres and Ti(SO₄)₂ are used as colloid seeds and Ti-source, respectively. The novel core (SnO₂ hollow sphere)-shell (TiO₂) nanostructures possess a large surface area of 122 m²/g (calcined at 350 °C) and a high exposure of TiO₂ surface. The structural change of TiO₂ shell at different temperatures was investigated by means of X-ray diffraction and Raman spectroscopy. It was observed that the rutile TiO₂ could form even at room temperature due to the presence of SnO₂ core and the unique core-shell interaction.     

Facile synthesis of nanocrystalline spinel NiFe2O4 via a novel soft chemistry route

A novel soft chemistry route (rheological phase reaction method) was developed to synthesize nanocrystalline NiFe₂O₄. The as-prepared samples were characterized by powder X-ray diffractometer (XRD), transmission electron microscope (TEM) and vibrating sample magnetometer (VSM). The effects of the calcination temperature on the particle sizes and magnetic properties of the samples were investigated. The results indicated that the samples obtained by this method had the single-phase spinel. Particle sizes estimated from Scherrer's formula increased with the calcination temperature, which were consistent with the results of TEM. The magnetic properties of the samples were strongly affected by the calcination temperature. The coercivity initially increased and then decreased with increasing calcination temperature whereas the saturation magnetization continuously increased.     

Mild solvothermal synthesis of complex fluorides Li2BeF4 and LiSrAlF6

The complex fluorides Li₂BeF₄ and LiSrAlF₆ were synthesized solvothermally at 180–240 °C and characterized by means of X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), thermogravimetric analysis (TGA), infrared spectroscopy (IR) and X-ray photoelectron spectroscopy (XPS). The different influence factors such as solvents, molar ratios of initial mixtures, reaction temperature and reaction time were investigated. The experimental results indicated that Li₂BeF₄ and LiSrAlF₆ powders could be controllably synthesized in the solvothermal process.     

Facile synthesis of rice-like anatase TiO2 nanocrystals

Rice-like anatase TiO₂ nanocrystals have been synthesized by hydrothermal treating Ti(OH)₃ precursor in deionized water, which is easy to form in-situ a stable TiO₂ aqueous dispersion and no post-synthetic purification process is required. The influences of synthetic parameters, such as reaction time and pH value, on the morphologies of the resulting nanocrystals have been investigated. It is found that the crystallinity and sizes of TiO₂ nanocrystals increase with the reaction time increased. The pH value is important for controlling the sizes and shapes of TiO₂ nanocrystals. As pH value increases from 2 to 11, spherical, rice-like, and rod-like TiO₂ nanocrystals are obtained, respectively. The formation mechanism of rice-like anatase TiO₂ nanocrystals is supposed to be a hydrothermal crystallization and Ostwald ripening process.     

Synthesis, structure and exchange bias in Cr2O3/CrO2/Cr2O5 particles

We report on the synthesis, structure and magnetic properties of a novel exchange bias system with Cr₂O₃/CrO₂/Cr₂O₅ interfaces. Chromium oxide particles with mixed chromium valences were prepared by sintering CrO₃ in air. X-ray diffraction patterns show that CrO₃ lost its oxygen gradually with increasing temperature and time through Cr₃O₈, Cr₂O₅, CrO₂, and finally Cr₂O₃ at temperatures above 760 K. X-ray photoelectron spectra indicate a low CrO₂ content and a binding energy of 579.3 eV for Cr 2p_3/2 photoelectrons in Cr₂O₅. Chromium dioxide was found to stably coexist with Cr₂O₃ and Cr₂O₅ in the particles. Magnetic measurements show hysteresis loop shifts in the sample, indicating an exchange bias induced by antiferromagnetic Cr₂O₃/Cr₂O₅ in ferromagnetic CrO₂. An exchange bias of 9 mT at 5 K and a coercivity of 26.3 mT were observed in the chromium oxide particles containing CrO₂.     

Microwave direct synthesis of MgB2 superconductor

Intermetallic compound superconductor MgB₂ was synthesized from spherical magnesium powder and lower purity amorphous boron powder by microwave direct heating. Powder X-ray diffraction (XRD) analysis indicates that the phases of the synthesis sample are MgB₂ (major phase) and a small amount of MgO. Scanning electron microscope (SEM) observation shows that the MgB₂ grain size is homogeneous and the particle size is about several hundreds of nanometers. The onset superconducting transition temperature of the MgB₂ sample measured by the temperature dependence of magnetization measurement is about 37.6 K. The critical current density J_c calculated according to the Bean model are about 2.0 × 10⁵ A/cm² at 20 K in self-field and 1.0 × 10⁵ A/cm² at 20 K in 1 T applied field.     

Large-scale hydrothermal synthesis of WO3 nanowires in the presence of K2SO4

WO₃ nanowires were fabricated by a hydrothermal method in the presence of K₂SO₄. The nanowires exhibit a well crystallized one-dimensional structure with 10 nm in diameter and several microns in length. Effects of other alkali salts (KNO₃, NaNO₃ and Na₂SO₄) on the morphologies of WO₃ nanocrystals were also investigated. The important role of K₂SO₄ salt in the WO₃ nanowires synthesis has been demonstrated.     

Thermo-optic properties of TiO2, Ta2O5 and Al2O3 thin films for integrated optics on silicon

The direct measurement of the thermo-optic coefficients of aluminium oxide, tantalum pentoxide and titanium dioxide thin films is presented. Using ellipsometry on monolithically integrated permutations of the layers of silicon, silicon dioxide and the material under test, allows the direct measurement of the overall thermo-optic coefficient accounting for thermally induced changes in the dielectric permittivity and density of the materials as well as the elasto-optic effect due to the non-matching thermal expansion coefficients of the different materials.     

Hydrothermal synthesis of CeO2 nano-octahedrons

CeO₂ nano-octahedrons were synthesized with a facile hydrothermal synthesis process where Ce(NO₃)₃·6H₂O and urea were used as a cerium resource and mineralizer respectively and no surfactant or template was applied. The effects of synthesis parameters such as reaction temperature, reaction time, as well as the dosages of Ce (NO₃)₃·6H₂O and urea were studied. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis were conducted to characterize the crystalline and morphology of the obtained CeO₂ powders. The optimal reaction condition to prepare the CeO₂ of the desired fluorite structure was established. The possible mechanism of synthesis of CeO₂ with a nano-octahedron morphology was illustrated.     

In-situ preparation of TiO2/SnO2 nanocrystalline sol for photocatalysis

A novel preparation method to synthesize TiO₂/SnO₂ nanocrystalline sol under mild conditions was presented. Ti(OC₄H₉)₄ used as a precursor was hydrolyzed in the rutile SnO₂ nanocrystalline sol, and in-situ formed TiO₂/SnO₂ nanocrystalline sol. The crystal structure, morphology and photocatalysis performance of samples were investigated. The results show that the additional rutile SnO₂ nano grains serve as heterogeneous crystal nucleus and exhibite the inducing effect on TiO₂ grains growth, thus leading to the changes in crystalline phase and particle morphology. In addition, the photoluminescence (PL) spectra analysis indicates that TiO₂/SnO₂ composite structure induces a better charge separation, and thus the photocatalytic activity of TiO₂/SnO₂ sol is increased significantly compared with TiO₂ sol.     

碳纳米管修饰LaFeO3/TiO2复合材料的光催化性能与机理

采用超声辅助溶胶凝胶法制备了LaFeO₃颗粒,进一步以碳纳米管(CNTs)为基底和钛酸丁酯为前体,通过一步水热法煅烧合成CNTs/TiO₂/LaFeO₃(CTF)三元异质结光催化复合材料。通过扫描电子显微镜(SEM)、X射线衍射分析(XRD)、氮气吸附-解吸等温线(BET)、紫外-可见分光光度计(UV-Vis)、光致发光光谱(PL)等表征手段对材料的形貌与特征结构、比表面积和孔径结构以及光学特征进行了分析,并在紫外光下通过降解活性黑五(RB5)测试样品的光催化性能。结果表明,以CNTs作为载体,能够有效提升LaFeO₃/TiO₂复合材料的光催化性能。当CNTs在复合材料中的质量占比为5%时,150 W汞灯照射下RB5的50 min去除率可达99.5%。CNTs一方面通过增加复合材料的比较面积为催化反应的进行提供了更多的活性位点,更为重要的是,CNTs作为光生载流子传输的通道加快了电荷分离效率,提升了复合材料的降解能力和催化反应动力学进程。     

Simple synthesis of ZrO2/SiOx core/shell nanofibers using ZrSi2 with gallium

ZrO₂/SiO_x core/shell nanofibers with diameter ~ 50 nm were synthesized by the thermal oxidation of ZrSi₂ substrates with gallium. The crystalline ZrO₂ cores were grown with amorphous SiO_x shells. It is proposed that the growth of crystalline ZrO₂ core was guided by the prior supersaturation of Zr species in the molten gallium film, whereas the amorphous SiO_x shell could be attributed to the deposition of SiO vapor on the surface of ZrO₂ core. In addition, the ZrO₂/SiO_x core/shell nanofibers show a wide visible photoluminescence (PL) emission at 480 nm, which should originate from the SiO_x shells.     

TiO2-SnO2 system for gas sensing—Photodegradation of organic contaminants

Catalytic photodegradation of organic contaminants by means of UV light has been demonstrated for gas sensors based on composites of TiO₂-SnO₂. Thin film resistive-type gas sensors of TiO₂-SnO₂ have been deposited at 350 °C by RF sputtering from a Ti-SnO₂ target with varying surface ratio of SnO₂/Ti. Photodegradation experiments of bromothymol blue by UV light have been performed by means of the optical spectrophotometry over the wavelength range extending from 300 nm to 600 nm. The influence of the UV illumination on the sensor response to 100-20,000 ppm of H₂ has been investigated in situ on motor oil contaminated sensors. It has been found that sequential exposures to UV light lead to a partial recovery of the sensor signal to hydrogen.     

等离子体电解氧化法制备多孔TiO2/V2O5复合物膜层及其增强光催化产氢活性

较差的光催化产氢效率极大地阻碍了TiO₂光催化剂的工业化应用。为此,本文在含有NH₄VO₃的磷酸盐溶液中,采用等离子体电解氧化(PEO)法制备了多孔TiO₂/V₂O₅复合膜光催化剂,通过扫描电子显微镜(SEM)、能谱仪(EDS)、X射线衍射(XRD)、X射线光电子谱(XPS)和紫外可见漫反射光谱(UV-Vis DRS)对其组成、结构及光吸收性质进行了表征,并采用气相色谱评价了薄膜催化剂的光催化产氢性能,研究了电解液中NH₄VO₃含量对膜的结构、组成和光催化产氢性能的影响。结果表明:复合膜催化剂主要由锐钛矿和金红石型TiO₂组成,具有微孔结构,V₂O₅主要以无定形形式存在于膜中,与TiO₂有很强的相互作用,影响TiO₂的晶面间距。研究发现,元素V抑制了TiO₂的结晶和金红石型TiO₂的形成,扩大了薄膜的光学吸收范围。针对Na₂S+ Na₂SO₃溶液中的光催化产氢性能的研究显示,在质量浓度为1 g/L NH₄VO₃的电解液中制备的TiO₂/V₂O₅薄膜的光催化活性最高,优于近年来报道的其他光催化剂。光催化重复实验表明,该复合膜催化剂具有较高的稳定性和较为恒定的光催化活性。     

Comparative analysis of crystal field effects and optical spectroscopy of six-coordinated Mn ion in the Y2Ti2O7 and Y2Sn2O7 pyrochlores

The electronic energy levels of the six-coordinated Mn⁴⁺ ion in the pyrochlores Y₂B₂O₇ (B = Sn⁴⁺, Ti⁴⁺) have been computed using the exchange charge model of crystal field theory. The calculated Mn⁴⁺ energy levels and their trigonal splitting are in good agreement with the experimental spectra. The calculated crystal field parameters show that the higher crystal field strength in Y₂Sn₂O₇ arises from an increased orbital overlap effect between the Mn⁴⁺ ion and the nearest oxygen ions, which are located at the 48f crystallographic position of the pyrochlore lattice. This increased overlap in Y₂Sn₂O₇ occurs despite the fact that the Mn⁴⁺-O²⁻ bond distance in Y₂Sn₂O₇ is longer than in Y₂Ti₂O₇ and is attributed to a lack of hybridization (covalent bonding) between the filled 2p orbital of oxygen ion occupying the 48f site of the pyrochlore lattice and the filled Sn⁴⁺ 4d¹⁰ orbital. The low temperature emission spectrum of Mn⁴⁺ activated Y₂Sn₂O₇ is analyzed in terms of a weak zero phonon line (R-line) with accompanying vibrational side bands.     

Single-step sputtered Cu2SnSe3 films using the targets composed of Cu2Se and SnSe2

Cu₂SnSe₃ thin films were prepared by single-step D.C. sputtering at 100-400 °C for 3 h using targets composed of Cu₂Se and SnSe₂ in three different ratios of 2/1 (target A), 1.8/1 (target B), and 1.6/1 (target C). The advantages of self-synthesized SnSe₂ instead of commercially available SnSe for depositing Cu₂SnSe₃ thin films were demonstrated. Effects of target composition and substrate temperature on the properties of Cu₂SnSe₃ thin films were investigated. Structure, surface morphology, composition, electrical and optical properties at different process conditions were measured. The 400 °C-sputtered films obtained from target B display with direct band gap of 0.76 eV, electrical resistivity of 0.12 Ω cm, absorption coefficient of 10⁴-10⁵ cm^− 1, carrier concentration of ∼ 1.8 × 10¹⁹ cm^− 3, and electrical mobility of 2.9 cm²/V s.     

Combined spectroscopic ellipsometry and attenuated total reflection analyses of Al2O3/HfO2 nanolaminates

The microstructure of thin HfO₂-Al₂O₃ nanolaminate high κ dielectric stacks grown by atomic vapor deposition has been studied by attenuated total reflection spectroscopy (ATR) and 8 eV spectroscopic ellipsometry (SE). The presence of Al₂O₃ below HfO₂ prevents the crystallisation of HfO₂ if an appropriate thickness is used, which depends on the HfO₂ thickness. A thicker Al₂O₃ is required for thicker HfO₂ layers. If crystallisation does occur, we show that the HfO₂ signature in both ATR and 8 eV SE spectra allows the detection of monoclinic crystallites embedded in an amorphous phase.     

Characteristics of stacked CuInS2 and CuGaS2 layers as determined by the growth sequence

CuInS₂ and CuGaS₂ thin films have been prepared sequentially from elemental evaporation sources onto conventional soda lime glass substrates heated at 350 °C during the deposition process. The gradient in the structure and composition of the stacked layers has been investigated for the two possible growth sequences. Structural depth profiling and crystallographic phase analysis were performed by grazing incidence X-ray diffraction. The atomic distribution in the films depth was analyzed by X-ray photoelectron spectroscopy combined with sputter etching. Formation of the quaternary compound CuIn_1 − xGa_xS₂, with a high Ga content x > 0.80, has been detected with different distribution depending on the growth sequence.