Co-templating synthesis of highly dispersed 1D ZnO nanostructures in amorphous SiO2 under hydrothermal condition

One-dimensional (1D) ZnO nanostructures were grown in amorphous SiO₂ matrix by a co-templating method under hydrothermal condition. Using ethylenediamine (EDA) groups grafted mesoporous silica MCM-41 as a co-template, the growth of 1D ZnO nanostructures was oriented by soft EDA groups and confined inside the hard mesochannels of MCM-41. The microstructure and morphology of the 1D-ZnO-nanostructures/SiO₂ composite were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDS). All these results indicate that the 1D ZnO nanostructures were synthesized and highly dispersed in the amorphous SiO₂ matrix. Blue-shifted exciton absorption was observed from the co-templating synthesized sample.     

Polyaniline/SiO2 Nanocomposite Catalyzed Efficient Synthesis of Quinoxaline Derivatives at Room Temperature

Polyaniline/SiO₂ nanocomposite material has been synthesized by using chemical oxidative method. Prepared catalytic material was characterized by means of transmission electron microscopy (TEM), thermal analysis (TG‐DTA), X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and Fourier transform infrared spectroscopy (FT‐IR). Solvent stability for the catalyst has been screened using UV‐Visible spectroscopy. Polyaniline/SiO₂ catalyzed route has found to be an efficient and rapid protocol for the synthesis of quinoxaline derivatives by cyclocondensation of 1,2‐diketones and o‐phenylenediamines at room temperature. This protocol has several advantages such as high yield, good thermal stability, simple work up procedure, non‐toxic, clean, and easy recovery and reusability of the catalytic system.     

石墨烯-氧化钌纳米复合材料的水热法合成及电化学电容性能

通过水热法制备了石墨烯-氧化钌(G-RuO₂)纳米复合材料。对样品进行了X射线衍射(XRD),扫描电子显微镜(SEM),透射电子显微镜(TEM)和能量色散谱(EDS)表征。SEM结果表明氧化钌粒子均匀地分散在石墨烯层片上。TEM结果显示氧化钌纳米粒子的平均粒径约为3 nm。对样品进行了循环伏安和充放电性能测试,结果表明在1 A·g^-1的电流密度下,样品在H₂SO₄(1 mol·L^-1)溶液中具有219.7 F·g^-1的比电容。     

高酸位多级孔超稳Y型沸石的制备及催化性能

以表面活性剂十六烷基三甲基溴化铵（CTABr）为模板剂,在水热体系对水蒸气处理后的超稳Y型（USY）沸石进行晶化处理,获得高酸量和高水热稳定性的USY-c-w样品。利用X射线衍射、扫描电子显微镜、透射电子显微镜、固态核磁共振、N₂吸附-脱附、NH₃-程序升温脱附、傅里叶变换红外光谱及吡啶红外对所制备催化剂的物化性质进行详细表征。选用1,3,5-三异丙苯（TIPB）催化裂化作为探针反应,研究制备的催化剂的催化性能,并与工业USY沸石进行对比。结果表明,再次水热晶化后,样品的硅铝骨架局部重构,非骨架铝重新进入沸石骨架,合成样品的硅铝比（n_SiO2/n_Al2O3）由10降至3.0;再晶化后的USY沸石,不仅具有丰富的介孔结构,并且具有更多的弱酸和中强酸位点。在TIPB裂解反应中,再晶化后的USY沸石表现出比原样品更优异的催化性能。     

Ag作催化剂制备的GaN的形貌及其性能

用化学气相沉积法(CVD)在Si(100)衬底上以Ag纳米颗粒为催化剂制备了微纳米结构的GaN,原料是熔融态的金属Ga和气态的NH3。采用X射线衍射仪(XRD)、透射电镜(TEM)、X-ray能谱仪(EDS)、场发射扫描电子显微镜(SEM)、光致发光能谱(PL)和霍尔效应测试对样品进行了结构、成分、形貌和发光、电学性能分析。结果表明:生成的自组装GaN为六方纤锌矿的类似小梯子的微纳米单晶结构,且在不同的温度下,GaN的发光性能和电学性能也有所不同,相对于强的紫外发光峰,其它杂质发光峰很微弱,且均呈p型导电。对本实验所得到的GaN微纳米结构的可能形成机理进行了探讨。     

Morphology‐controlled Electrodeposition of Copper Nanospheres onto FTO for Enhanced Photocatalytic Hydrogen Production

Using CuSO₄ as the copper source, nanostructured copper with four different morphologies was obtained by electrodeposition method on FTO substrates. The as‐synthesized Cu/FTO samples were characterized by X‐ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), Raman, X‐ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy‐dispersive X‐ray spectroscopy (EDS), and transmission electron microscopy (TEM). The effects of electrodeposition potential and electrodeposition time on the Cu/FTO samples and the photocatalytic performance were investigated systematically. The results showed that the Cu/FTO samples were well‐crystallized and the morphologies could be changed from nanoslices to nanodendrites structure with the negative shift of the depositing potential. The electrodeposition potential and time have a significant effect on the amount of H₂ evolution. The obtained Cu nanospheres which were prepared at the potential of −0.65 V for 600 s showed the best photocatalytic behavior. The mechanisms for the photocatalytic activities were also discussed.     

CuO表面修饰锐钛矿TiO2纳米管阵列及其电化学嵌锂性能

以(CH_2OH)_2、NH4F和HCl为电解液,纯Ti片、CuCl_2和Na NO3为主要原料,联用阳极氧化和水热法制备CuO表面修饰锐钛矿TiO_2纳米管阵列锂离子电池负极材料(CuO/TiO_2)。使用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、能谱仪(EDS)、X射线光电子能谱仪(XPS)和X射线衍射(XRD),研究样品的形貌特征、元素分布、价态和微观物相组成。利用电池充放电测试仪和电化学工作站,探讨材料的电化学嵌锂性能。结果表明,表面修饰后的锐钛矿TiO_2纳米管阵列外侧出现了大量绒毛状纳米CuO,单个绒毛结构的宽度约4 nm,长度约10 nm。在0.3C的电流密度下进行恒电流充放电测试,首次放电容量为550 m Ah·g~(-1),充电容量为490 m Ah·g~(-1)。50次循环后,可逆电流容量仍保持在320 m Ah·g~(-1),具有良好的循环稳定性和电化学特性。     

CuO表面修饰锐钛矿TiO2纳米管阵列及其电化学嵌锂性能

以（CH₂OH）₂、NH₄F和HCl为电解液,纯Ti片、CuCl₂和NaNO₃为主要原料,联用阳极氧化和水热法制备CuO表面修饰锐钛矿TiO₂纳米管阵列锂离子电池负极材料（CuO/TiO₂）。使用扫描电子显微镜（SEM）、透射电子显微镜（TEM）、能谱仪（EDS）、X射线光电子能谱仪（XPS）和X射线衍射（XRD）,研究样品的形貌特征、元素分布、价态和微观物相组成。利用电池充放电测试仪和电化学工作站,探讨材料的电化学嵌锂性能。结果表明,表面修饰后的锐钛矿TiO₂纳米管阵列外侧出现了大量绒毛状纳米CuO,单个绒毛结构的宽度约4 nm,长度约10 nm。在0.3C的电流密度下进行恒电流充放电测试,首次放电容量为550 mAh·g^-1,充电容量为490 mAh·g^-1。50次循环后,可逆电流容量仍保持在320 mAh·g^-1,具有良好的循环稳定性和电化学特性。     

基于N-乙酰-L-半胱氨酸修饰的ZnFe2O4@SiO2纳米材料手性识别酪氨酸对映异构体

我们将N-乙酰-L-半胱氨酸（NALC）修饰于ZnFe₂O₄@SiO₂纳米材料表面,制备了一种新型的手性纳米复合物（ZnFe₂O₄@SiO₂-NALC）,该材料能够简便、快速及高选择性地识别手性酪氨酸（Tyr）对映体。利用X射线粉末衍射（XRD）、红外光谱（FT-IR）、能量色散X射线光谱（EDS）、扫描电子显微镜（SEM）、高分辨率透射电子显微镜（HRTEM）和振动样品磁力计（VSM）等一系列表征手段对首次合成出的ZnFe₂O₄@SiO₂-NALC进行测试表征,并将其应用于对手性识别领域的探究。实验结果表明,利用光谱技术（紫外-可见光谱和荧光光谱）,ZnFe₂O₄@SiO₂-NALC可对Tyr对映异构体进行手性识别。此外,我们进一步对Tyr浓度和pH值等实验参数进行了优化。     

Development of a new catalytic and sustainable methodology for the synthesis of benzodiazepine triazole scaffold using magnetically separable CuFe2O4@MIL-101(Cr) nano-catalyst in aqueous medium

Magnetically retrieval CuFe₂O₄@MIL-101(Cr) metal–organic framework was successfully prepared from easily available starting materials and characterized using various spectroscopic and analytical techniques such as powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray, transmission electron microscopy, elemental mapping, Fourier transform infrared spectroscopy, thermogravimetric analysis, X-ray photoelectron spectroscopy, Brunauer–Emmett–Teller, vibrating sample magnetometer, and inductively coupled plasma optical emission spectroscopy. The catalyst was then used in the synthesis of benzodiazepines containing a triazole moiety in water. The advantages of this protocol include high yields, reusability of the catalyst, and gram-scale synthesis.     

N2流量对GaN的形貌及光学和电学性能的影响

采用化学气相沉积法(CVD)在Si(100)衬底上以Ni为催化剂,金属Ga和NH3为原料合成了GaN微纳米结构,并研究了N2流量对产物GaN的形貌及光学和电学性能的影响。利用场发射扫描电子显微镜(SEM)、透射电镜(TEM)、X射线衍射仪(XRD)、Xray能谱仪(EDS)、光致发光谱(PL)和霍尔效应测试仪(HMS-3000)等测试手段对样品的形貌、结构、成分、光学和电学性能进行了分析。结果表明,随着N2流量的增加,产物GaN的形貌发生了由微米棒到蠕虫状线再到光滑纳米线的转变;生成的GaN均为六方纤锌矿结构;样品均表现出383 nm的近带边紫外发射峰和470 nm左右的蓝光发射峰;所有样品均为p型;并对产物GaN的形貌转变机理进行了分析。     

Ultrasound assisted synthesis of starch-capped Cu2O NPs towards the degradation of dye and its anti-lung carcinoma properties

A unique starch encapsulated Cu₂O nanoparticles were synthesized through a simple and ‘green’ route using ultrasonic irradiation. The polar functional groups on the starch (OH) facilitate the NP capping and stabilization. Structural features of the material were assessed over several advanced techniques like fourier transformed infra-red (FT-IR), UV–vis spectroscopy, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), energy dispersive X-ray analysis (EDX) elemental mapping, transmission electron microscopy (TEM), X-ray diffraction analysis (XRD), and inductively coupled plasma-atomic emission spectrometry (ICP-AES) analysis. It was catalytically explored in reducing an organic dye (Methylene blue - MB) in the presence of NaBH₄ at ambient conditions, being monitored in a UV–vis spectrophotometer. The nanocatalyst was recycled 11 times keeping consistency in its reactivity. Biologically, the nanocomposite exhibited excellent cytotoxicity against lung adenocarcinoma (PC-14, LC-2/ad and HLC-1) cell lines without affecting the normal (HUVEC) cell line. IC₅₀values of the nanocomposite were found at 618, 56 and 379 against HLC-1, LC-2/ad, and PC-14 cell lines respectively and accordingly, PC-14 afforded the best adenocarcinoma activity.     

Fe3O4磁性纳米粒子的超声包金及其表征

超声条件下, 在乙醇分散的3-氨丙基三乙氧基硅烷(APTES)功能化的磁性Fe₃O₄纳米粒子和四氯合金酸的混合溶液中滴加柠檬酸钠, 成功地制备了磁性Fe₃O₄/Au复合纳米粒子. 采用X射线粉末衍射仪(XRD)、紫外吸收可见光谱(UV-Vis)、带有电子能谱仪(EDS)的扫描电子显微镜(SEM)、透射电子显微镜(TEM)、光电子能谱(XPS)、超导量子干涉仪(SQUID)等方法, 对复合粒子的形态、结构、组成以及磁学性质进行了表征. 结果表明: 在此条件下制得的复合粒子粒径在30 nm左右, 室温下磁化强度可达63 emu/g.     

Shaped binderless ZSM-11 zeolite catalyst prepared via a dry-gel conversion method:Characterization and application for alkylation of benzene with dimethyl ether

Shaped binderless ZSM-11 zeolite catalysts were synthesized via a dry-gel conversion technique from 70ZSM-11/30 SiO_2mix extrudates. 1,6-hexanediamine combined with tetrabutylammonium bromide was proved to be the best structure directing agent for the synthesis of the binderless ZSM-11 catalyst, without adding other alkaline materials. The 70HZSM-11/30 SiO_2mix serials materials crystallized for different times were detected by X-ray diffraction(XRD), nuclear magnetic resonance(NMR), scanning electron microscopy(SEM), transmission electron microscopy(TEM), scanning transmission electron microscopy–energy dispersive spectroscopy(STEM–EDS) techniques, and so on. In order to investigate the possible crystallization mechanism, the textural and structural properties of 70HZSM-11/30 SiO_2mix serials samples were further characterized by N_2 adsorption–desorption. Acid properties were determined by temperature-programed desorption of NH_3(NH_3-TPD) and pyridine adsorption-infrared(Py-IR) measurements. In the alkylation of benzene with dimethyl ether, the serials catalysts exhibited different benzene conversions. 70HZSM-11/30 SiO_2mix showed the lowest benzene conversion while sample 70HZSM-11/30 SiO_2mix-6.5h synthesized only for 6.5h displayed a higher benzene conversion, even higher than the value over 70HZSM-11/30Al_2O_3mix. Extending the crystallization time, the obtained samples displayed the increased benzene conversion in general under the same reaction conditions. In the end, the relation of physicochemical properties with the reaction performance was investigated.     

Fe3O4‐supported Schiff‐base copper (II) complex: A valuable heterogeneous nanocatalyst for one‐pot synthesis of new pyrano[2,3‐b]pyridine‐3‐carboxamide derivatives

A novel Cu (II) Schiff‐base complex immobilized on core‐shell magnetic Fe₃O₄ nanoparticles (Fe₃O₄@SPNC) was successfully designed and synthesized. The structural features of these nanoparticles were studied and confirmed by using various techniques including FT‐IR spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy‐dispersive X‐ray spectroscopy (EDS), vibrating sample magnetometer (VSM), X‐Ray diffraction (XRD), wavelength dispersive X‐ray spectroscopy (WDX), and inductively coupled plasma (ICP). These newly synthesized nanoparticles have been used as efficient heterogeneous catalytic system for one‐pot multicomponent synthesis of new pyrano[2,3‐b]pyridine‐3‐carboxamide derivatives. Notably, the catalyst could be easily separated from the reaction mixture by using an external magnet and reused for several successive reaction runs with no significant loss of activity or copper leaching. The present protocol benefits from a hitherto unreported MNPs‐immobilized Cu (II) Schiff‐base complex as an efficient nanocatalyst for the synthesis of newly reported derivatives of pyrano[2,3‐b]pyridine‐3‐carboxamide from one‐pot multicomponent reactions.     

Palladium nanoparticles supported on modified hollow Fe3O4@TiO2: Preparation,characterization, and catalytic activity in Suzuki cross‐coupling reactions

Hollow Fe₃O₄@TiO₂‐NH₂/Pd as a light‐weight, magnetically heterogeneous catalyst was successfully prepared, and characterized by using different techniques including X‐ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT‐IR), field‐emission scanning electron microscopy (FE‐SEM), transmission electron microscopy (TEM), energy‐dispersive X‐ray spectroscopy (EDX), vibrating sample magnetometer (VSM) measurements, and thermogravimetric analysis (TGA). Then this heterogeneous catalyst was tested in the Suzuki cross‐coupling reaction, and the results confirmed the success of this method. The catalyst could be separated easily using an external magnet and reused at least in five runs successfully without any appreciable loss in its catalytic activity.     

紫外线辐照制备单分散ZnS纳米颗粒

以硫代硫酸钠和乙酸锌为反应物、柠檬酸为调控剂,在紫外光辐照下制备出单分散的ZnS纳米颗粒。采用XRD、TEM、低温氮吸附-脱附、HRTEM和EDS等方法研究了反应物浓度、辐照时间和柠檬酸用量等因素对产物颗粒尺寸和分布的影响。结果表明,随着反应时间延长,产物收率增高,平均晶粒度增大,比表面积变小。反应物浓度对产物组成和比表面积有较大影响,但对产物的平均晶粒度影响不大。适量添加柠檬酸,有利于制备单分散的ZnS纳米颗粒。     

Synthesis of Ag Nanoparticle Doped MnO2/GO Nanocomposites at a Gas/Liquid Interface and its Application in H2O2 Detection

Ag/MnO₂/GO nanocomposites were synthesized via the method of gas/liquid interface based on silver mirror reaction, and a non‐enzymatic H₂O₂ sensor was fabricated through immobilizing Ag/MnO₂/GO nanocomposites on GCE. The composition and morphology of the nanocomposites were studied by energy‐dispersive X‐ray spectroscopy (EDS), X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Electrochemical investigation indicated that it exhibited a favorable performance for the H₂O₂ detection. Its linear detection range was from 3 μM to 7 mM with a correlation coefficient of 0.9960; the sensitivity was 105.40 μA mM^?1 cm^?2 and the detection limit was estimated to be 0.7 μM at a signal‐to‐noise ratio of 3.     

Novel Bi/BiOBr/AgBr composite microspheres: Ion exchange synthesis and photocatalytic performance

Novel Bi/BiOBr/AgBr composite microspheres were prepared by a rational in situ ion exchange reaction between Bi/BiOBr microspheres and AgNO₃. The characteristic of the as-obtained ternary microspheres was tested by X-ray diffraction (XRD), energy dispersive X-ray spectrometer (EDS), scanning electron microscope (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectroscopy (UV–vis DRS) and photoluminescence (PL). Under visible light irradiation, Bi/BiOBr/AgBr microspheres exhibited an excellent photocatalytic efficiency for rhodamine B (RhB) degradation, which was about 1.4 and 4.9 times as high as that of Bi/BiOBr and BiOBr/AgBr, demonstrating that the highest separation efficiency of charge carriers in the heterostructured Bi/BiOBr/AgBr. The photocatalytic activity of Bi/BiOBr/AgBr microspheres just exhibited a slight decrease after three consecutive cycles. The photocatalytic mechanism investigation confirmed that the superoxide radicals (O₂^•−) were the dominant reactive oxygen species for RhB degradation in Bi/BiOBr/AgBr suspension.     

Biosynthesis of Pd/MnO2 nanocomposite using Solanum melongena plant extract and its application for the one‐pot synthesis of 5‐substituted 1H‐tetrazoles from aryl halides

In this work, for the first time, Solanum melongena plant extract was used for the green synthesis of Pd/MnO₂ nanocomposite via reduction osf Pd(II) ions to Pd(0) and their immobilization on the surface of manganese dioxide (MnO₂) nanoparticles (NPs) as an effective support. The synthesized nanocomposite were characterized by various analytical techniques such as Fourier transform infrared (FT‐IR), X‐ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), energy dispersive X‐ray spectroscopy (EDS) and UV–Vis spectroscopy. The catalytic activity of Pd/MnO₂ nanocomposite was used as a heterogeneous catalyst for the one‐pot synthesis of 5‐substituted 1H‐tetrazoles from aryl halides containing various electron‐donating or electron‐withdrawing groups in the presence of K ₄ [Fe (CN) ₆ ] as non‐toxic cyanide source and sodium azide. The products were obtained in good yields via a simple methodology and easy work‐up. The nanocatalyst can be recycled and reused several times with no remarkable loss of activity.