氮化铁催化剂的制备及其苯胺催化加氢性能

用α－Ｆｅ２Ｏ３与氨气程序升温还原方法制备出不同温度氮气的氮化铁系列催化剂。通过ＸＲＤ测试对氮化过程中的晶相转变进行了分析。在中压反应装置上考察了氮化铁系列催化剂上苯胺加氢活性以及反应条件对苯胺加氢反应活性的影响。结果表明，在７００℃氮化制香的氮化铁催化剂显示有较高的苯胺加氢活性，在氢压为３．０ＭＰａ，温度为２５０℃，ｎ（Ｈ２）／ｎ（ｏｉｌ）＝１８，液体空速（ＷＨＳＶ）为０．３ｈ＾－１时，该催化剂     

三价铟化合物在有机合成中的应用

综述了近年来三价铟化合物促进的多种有机反应及其在有机合成中的应用,其中重点讨论了三价铟化合物促进下的碳-碳键和碳-杂原子键的形成反应.     

Electron microscopic phase analysis of BN-thin films

A series of BN films was deposited by means of r.f. magnetron sputtering of a h-BN target onto Si(1OO) surfaces. Hereby, the substrate bias voltage was varied. Special interest is focussed to the influence of the deposition parameters on the orientation of the growing hexagonal BN film with respect to the substrate. For structural investigation, cross section samples were prepared. In addition to HRTEM and diffraction investigations, especially electron energy loss spectroscopy (EELS) was applied successfully for phase identification. For negative bias voltages of U _B =–300 V and U _B =–350V, we found a phase system consisting of a first-grown 25 nm thick layer of hexagonal structure with the c axis parallel to the substrate surface followed by the cubic phase.Dedicated to Professor Dr. rer. nat. Dr. h.c. Hubertus Nickel on the occasion of his 65th birthday     

Preparation and lithium doping of gallium oxynitride by ammonia nitridation via a citrate precursor route

Gallium oxynitride, isostructural to hexagonal gallium nitride (h-GaN), was obtained by ammonia nitridation of a precursor prepared from the addition of citric acid to an aqueous solution of gallium nitrate. Gallium oxynitride produced at 750 °C had a small amount of gallium vacancies, and was formulated as (Ga_0.89□_0.11) (N_0.66O_0.34) where the symbol □ stands for gallium vacancy. Both the gallium vacancies and oxygen substituted for nitrogen were randomly distributed within the structure. The amount of vacancies decreased with nitridation temperatures in the range of 750-850 °C. Approximately, 10 at% Li⁺ was doped into the gallium oxynitride, using a similar preparation with the additional presence of lithium nitrate, resulted in the random substitution of Ga³⁺ in an atomic ratio of Li/Ga<1 at 750 °C. Oxygen was codoped with lithium and substituted nitrogen in the wurtzite-type crystal lattice. These substitutions reduced the electrical conductivity in the gallium oxynitride semiconductor. A new oxynitride, Li₂Ga₃NO₄, was also obtained with Li₂CN₂ impurity using similar preparations from a mixture of Li/Ga?1. The crystal structure was isostructural with h-GaN, and was refined as P6₃mc with a=0.31674(1) nm, and c=0.50854(2) nm. The Ga and Li occupancies at the 2b site were refined to be 0.6085 and 0.3915, respectively, assuming that the other 2b site was randomly occupied with 1/5O and 4/5N. When the new compound was washed for over 1 min for the removal of Li₂CN₂ impurities, it was decomposed to a mixture of α-GaOOH and α-LiGaO₂. The as-prepared product with Li/Ga=1 showed the highest intensity in yellow luminescence among the products under excitation at 254 nm.     

铟参与的4-溴-1，1，1-三氟-2-丁烯与α-烷氧基醛亚胺的烯丙化反应：4，4，4-三氟-γ-羟基缬氨酸的合成

铟参与的4-溴-1,1,1-三氟-2-丁烯与α-烷氧基醛亚胺的烯丙化反应以中等的产率和高非对映选择性生成了高烯丙基胺3.从甘油醛亚胺和4-溴-1,1,1-三氟-2-丁烯反应制备的高烯丙基胺3g出发,以7步反应24%的总产率合成了4,4,4-三氟-γ-羟基缬氨酸11.     

Prepared Low Stress Cubic Boron Nitride Film by Physical Vapor Deposition

We present low stress cubic boron nitride (cBN) films with a transition layer deposited on the metal alloy substrates by tuned substrate radio-frequency magnetron sputtering. The films were characterized by Fourier transform infrared spectroscopy and transmission electron microscopy (TEM). The IR peak position of cubic boron nitride at 1006.3 cm⁻¹, which is close to the stressless state, indicates that the film has very low internal stress. The TEM image shows that pure CBN phase exists on the surface of the film. Several phases of boron nitride were found at the medium implantation dose. It is believed that the transition from the low ordered phases to cBN phase occurred during implantation.     

An Efficient and Green Synthesis of 5-Oxo-5, 6, 7, 8-tetrahydro- 4H-benzo-[b]-pyran Derivatives Promoted by InCl_3·4H_2O Under Microwave Irradiation

Construction of tetrahydropyran rings has attracted a great deal of interests in organic synthesis in recent years1, since tetrahydropyran moiety constitutes a structural unit in a number of natural products2. In addition, tetrahydropyran derivatives possess wide range of biological activities and pharmacological properties, such as anticancer activity3 and antihypersensitivity4. Many methods for the preparation of such compounds have already been developed5. Among them, condensation of α, β…     

基于氮化碳复合材料磁性固相萃取结合高效液相色谱法测定尿液中3种羟基多环芳烃

建立了测定尿液中3种羟基多环芳烃的氮化碳复合材料磁性固相萃取结合高效液相色谱-荧光检测法。所构筑的磁性氮化碳材料，经扫描电子显微镜、X射线衍射仪、振动样品磁强计和比表面积分析仪表征后，用于尿液中3种羟基多环芳烃的富集净化。考察了吸附剂用量、吸附时间、洗脱溶液和洗脱体积（单次洗脱体积×洗脱次数）对萃取效率的影响。结合高效液相色谱-荧光分析，在0.25~250 μg/L范围内线性关系良好（相关系数r=0.999），3种羟基多环芳烃的检出限和定量限分别为0.08和0.25 μg/L，回收率为90.1%~102%，日内和日间精密度分别为1.5%~7.7%和2.2%~8.7%。该本方法简单、快速、高效，可用于尿液中羟基多环芳烃的分析。     

Indium-mediated one-pot reductive conversion of nitroarenes to N-arylacetamides

N-Arylacetamides were prepared in excellent yields from nitroarenes in the presence of acetic anhydride, acetic acid and indium by a one-pot procedure.