Fe3O4/壳聚糖磁性微球功能化SBA-15介孔分子筛的合成

通过反相悬液交联法制备出了Fe3O4壳聚糖磁性微球,以3-丙胺基三乙氧基硅烷(APTES)为硅烷偶联剂,采用后修饰法得到硅烷化SBA-15介孔分子筛.以戊二醛为交联剂将Fe3O4壳聚糖磁性微球接枝在硅烷化SBA-15介孔分子筛上.运用X射线衍射、傅里叶红外光谱等手段对Fe3O4壳聚糖磁性微球(MCS)接枝后的硅烷化SBA-15介孔分子筛进行了表征.分析结果表明,Fe3O4壳聚糖磁性微球通过硅烷偶联剂以化学键形式结合在SBA-15介孔分子筛上.     

大孔-介孔分级孔结构炭材料制备及性能研究

以聚苯乙烯微球以及F127嵌段共聚物自组装结构为模板,酚醛树脂低聚物为碳前驱体,双模板法合成了大孔-介孔分级孔结构的炭材料.对样品进行了X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和氮吸附-脱附测试,并研究了样品的电化学性能.结果表明,利用这种简便的合成方法可以得到具有三维连通大孔以及二维有序介孔结构的分级孔结构炭材料,大孔尺寸在1μm左右,介孔孔径集中分布在5nm,比表面积为353.8m2/g,孔容0.36cm3/g.利用三电极体系测试了产品作为电化学双电层电容器电极材料的性能,在50mA/g的电流密度下,放电质量比电容为40F/g.     

分级介孔结构组成的ZnO微球及光催化性能

以硝酸锌、脲素及酒石酸为反应物, 采用水热法制备碱式碳酸锌前驱体微球, 通过煅烧前驱体制备了介孔氧化锌微球。通过扫描电子显微镜(SEM)可以观察到, 氧化锌微球的直径约为2~4 μm, 由大量厚度约为10 nm的介孔纳米片组装而成。X 射线衍射(XRD)和透射电镜(TEM)结果表明: ZnO微球为六方纤锌矿结构, 并结晶较好。比表面积测试(BET)表明ZnO微球为介孔材料, 孔径为20~50 nm, ZnO微球比表面积约为29.8 m²/g。以亚甲基蓝为目标降解物, 对介孔氧化锌微球进行了光催化降解实验。实验结果表明, 所合成的介孔ZnO微球对亚甲基蓝的光催化性能较好。     

氧化镍/镍/碳微球原位制备及葡萄糖传感性能

以葡萄糖、六水合氯化镍和尿素为原料, 通过水热反应一步制备前驱体Ni(OH)₂/C, 在高纯度氮气中煅烧获得NiO/Ni/C微球三元复合材料。采用扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、X射线光谱(EDS)和拉曼(Raman)等手段, 分析NiO/Ni/C微球三元复合材料的形貌结构以及物相组成。结果表明: NiO/Ni/C微球为珊瑚花状结构, 直径约1.7 μm, Ni、NiO呈立方相。通过循环伏安法和计时电流法研究了NiO/Ni/C微球三元复合材料的电化学行为及葡萄糖传感性能。当Ni/NiO摩尔比为0.19时, 形成的NiO/Ni/C三元复合微球具有优异的葡萄糖传感性能, 其灵敏度为241.09 μA·mmol/(L·cm²), 线性响应范围为10 μmol/L~5.05 mmol/L, 最低检测限位10 μmol/L。该传感器具有灵敏度高、抗干扰能力强以及稳定性好等特点。     

磁性Fe_3O_4/P(St-co-MMA)微纳米复合物的制备和性能

以单分散的苯乙烯-甲基丙烯酸甲酯共聚物(P(St-co-MMA))微球为载体,Fe Cl3·6H2O和Fe SO4·7H2O为前驱体,用反相共沉淀法制备了Fe3O4/P(St-co-MMA)微纳米原位复合物。使用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶红外光谱仪(FTIR)、X射线衍射仪(XRD)、振动样品磁强计(VSM)以及氮吸附/脱附等温线等手段对Fe3O4/P(St-co-MMA)的形貌、结构、磁性能、孔径、孔体积和比表面积进行了表征。结果表明,纳米级Fe3O4已经成功地负载在微米级P(St-co-MMA)的表面。在制备的Fe3O4/P(St-co-MMA)微纳米复合物中有介孔,其平均孔径、孔体积和比表面积分别为15.41 nm、0.15953 cm3/g和32.82 m2/g。Fe3O4/P(St-co-MMA)微纳米复合物具有超顺磁性和较好的磁响应性,能满足固液相磁分离的要求。     

蜂窝状钡铁氧体空心微球的制备与表征

以Fe(NO3)3和Ba(NO3)2为原料,乙醇为扩孔剂,采用柠檬酸溶胶-凝胶自蔓延燃烧法制得蜂窝状钡铁氧体空心微球。采用红外光谱(IR)和综合热分析仪(TG-DSC)分析燃烧后样品的热分解过程;采用电子探针(EPMA)、粉体X-射线衍射(XRD)和振荡样品磁强计(VSM)对蜂窝状钡铁氧体空心微球的微观结构和磁性进行测试。结果表明:在700℃煅烧2h可得到具有介孔和大孔复杂微观结构的蜂窝状钡铁氧体空心微球,粒度约20μm,其矫顽力为4998.0Oe,比饱和磁化强度为53.4emu/g,比剩余磁化强度为31.5emu/g。     

以丝素蛋白微球为模板制备介孔SiO_2空心微球

以自组装方法制备的丝素蛋白(SF)微球为模板,采用溶胶-凝胶法直接在SF微球表面涂覆硅层,随后高温锻烧制备介孔二氧化硅(SiO_2)空心微球并研究了氨水用量对SF微球表面沉积SiO_2胶粒的影响。通过SEM表征显示,随着氨水用量的增加,SiO_2胶粒在SF微球表面的沉积量增大;SF/SiO_2复合微球锻烧后经TEM和比表面积测试表明,SiO_2微球具有良好的空腔结构,比表面积为92.127m~2/g,孔体积为0.477cm~3/g,孔径为4.56nm。研究证明,在没有添加任何表面活性剂或偶联剂条件下,SF能够诱导SiO_2胶粒沉积,为制备介孔SiO_2空心微球提供了一条简单有效的新途径。     

SiO_2微球的制备及药物溶出性能研究

采用模板法制备出分散的球形介孔SiO2微球,以红外光谱仪(FT-IR)、X射线衍射仪(XRD)、热失重差热(TG-DTA)、氮气吸附-脱附(BET)、扫描电镜(SEM)和透射电镜(TEM)等方法对SiO2微球的结构及微观形貌进行了表征,结果表明,SiO2微球为无定形介孔单分散型,粒径在200~500nm。将制备的SiO2微球用于盐酸金霉素载体,考察SiO2微球负载盐酸金霉素的溶出度,结果表明:SiO2微球提高了药物的溶出度,在1h左右累计溶出80%,表明制备的介孔SiO2微球可以作为水难溶性药物的优良载体。     

磁性Fe_3O_4/SPS微纳米复合物的制备与表征

以磺化聚苯乙烯微球(SPS)为载体,FeCl3·6H2O和FeSO4·7H2O为铁源,NaOH为沉淀剂,通过反相共沉淀法制备了Fe3O4/SPS微纳米原位复合物。采用SEM、TEM、XRD、FTIR、VSM和氮吸附/脱附等温线,对Fe3O4/SPS的形貌、结构、磁性能、孔径、孔体积和比表面积进行了表征分析。结果表明:纳米级的Fe3O4成功地负载在了微米级的SPS表面。所制备的Fe3O4/SPS微纳米复合物中存在介孔,平均孔径、孔体积和比表面积分别为13.85nm、0.049cm3/g和14.16m2/g。Fe3O4/SPS微纳米复合物具有超顺磁性和较好的磁响应性,在外加磁场条件下能够满足固液相磁分离的要求。     

含松香丙烯酸酯的磁性聚合物微球的制备及表征

以苯乙烯(St)为单体,松香丙烯酸与甲基丙烯酸-2-羟乙酯酯化物(RAH)为交联剂,在油酸改性的Fe3O4存在下,采用悬浮聚合法制备了含松香的磁性聚合物微球[P(St/RAH)/Fe3O4],研究了Fe3O4用量对聚合物微球性能的影响,采用红外光谱、X射线衍射、扫描电镜、透射电镜、X射线光电子能谱、热重和磁强计对磁性聚合物微球进行了分析表征。结果表明,成功制得了P(RAH/St)/Fe3O4;得到的磁性微球球形良好,表面光滑,Fe3O4包埋在聚合物中;微球为超顺磁性,在油酸改性Fe3O4用量为8%(质量分数)时磁性达到饱和,饱和磁化强度为3.13A·m2/kg。     

Facile procedure to synthesize highly crystalline Ag/NiO nanocomposite microspheres and their photocatalytic activity

The β-Ni(OH)₂ microspheres have been fabricated by a facile hydrothermal method in the assistance of biomolecule (l-arginine). The NiO microspheres were obtained with further calcination of β-Ni(OH)₂ precursor at 500 °C for 2 h. Subsequently, Ag/NiO nanocomposite microspheres were also prepared by the reduction of AgNO₃ solution. The as-synthesized products were characterized by X-ray power diffraction, scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, thermogravimetric analysis et al. The photocatalytic activity of Ag/NiO composite microspheres was also investigated by UV–Vis spectrophotometer and the results display enhanced photocatalytic activity in degradation of methyl orange.     

Fabrication of hollow mesoporous NiO hexagonal microspheres via hydrothermal process in ionic liquid

The novel NiO hexagonal hollow microspheres have been successfully prepared by annealing Ni(OH)₂, which was synthesized via an ionic liquid-assisted hydrothermal method. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), N₂ adsorption-desorption and Fourier transform infrared spectrometer (FTIR). The results show that the hollow NiO microstructures are self-organized by mesoporous cubic and hexagonal nanocrystals. The mesoporous structure possessed good thermal stability and high specific surface area (ca. 83 m²/g). The ionic liquid 1-butyl-3methylimidazolium tetrafluoroborate ([Bmim][BF₄]) was found to play a key role in controlling the morphology of NiO microstructures during the hydrothermal process. The special hollow mesoporous architectures will have potential applications in many fields, such as catalysts, absorbents, sensors, drug-delivery carriers, acoustic insulators and supercapacitors.     

Porous graphitized carbon monolith as an electrode material for probing direct bioelectrochemistry and selective detection of hydrogen peroxide

For the first time, graphitized carbon particles with a high surface area have been prepared and evaluated as a new material for probing direct electrochemistry of hemoglobin (Hb). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) imaging revealed that the carbon monolithic skeleton was constructed by a series of mesopores with irregular shapes and an average pore diameter of ~5.6 nm. With a surface area of 239.6 m(2)/g, carbon particles exhibited three major Raman peaks as commonly observed for carbon nanotubes and other carbon materials, i.e., the sp(3) and sp(2) carbon phases coexisted in the sample. A glassy carbon electrode modified with carbon monoliths and didodecyldimethylammonium bromide exhibited direct electron transfer between Hb molecules and the underlying electrode with a transfer rate constant of 6.87 s(-1). The enzyme electrode displayed a pair of quasi-reversible reduction-oxidation peaks at -0.128 and -0.180 V, reflecting the well-known feature of the heme [Fe(3+)/Fe(2+)] redox couple: a surface-controlled electrochemical process with one electron transfer. This reagentless biosensing approach was capable of detecting H(2)O(2), a simple molecule but plays an important role in analytical and biological chemistry, as low as 0.1 μM with linearity of 0.1-60 μM and a response time of <0.8 s, comparing favorably with other carbon based electrodes (5 s).     

Synthesis of nickel oxides nanoparticles on glassy carbon as an electron transfer facilitator for horseradish peroxidase: Direct electron transfer and H2O2 determination

In this study, horseradish peroxidase/nickel oxides nanoparticles/glassy carbon (HRP/NiO NPs/GC) electrode was prepared by first applying nickel oxides nanoparticles on glassy carbon surface and then horseradish peroxidase immobilized on the NiO NPs. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) have been used as a diagnostic tools to identify the synthesized NiO NPs. Immobilized HRP showed an electrochemical redox behavior pertained to HRP(Fe(III)–Fe(II)) by direct electron transfer between protein and nanoparticles with a formal potential (E^0′) of ? 55.5 mV (vs. Ag/AgCl and 141.5 mV vs. NHE) in 50 mM phosphate buffer solution (PBS). The anodic charge transfer coefficient (α) and heterogeneous electron transfer rate constant (k_s) were 0.42 and 0.75 s^? 1, respectively. Biocatalytic activity of HRP/NiO NPs/GC electrode for reduction of hydrogen peroxide and application to hydrogen peroxide determination was exemplified.     

基于沉淀转化法制备的纳米NiO混合电容器研究

运用沉淀转化法制备Ni(OH)2超微粉末,并通过热处理得到纳米NiO.利用TG、XRD、TEM、N2吸附,循环伏安和恒流充放电测试对样品进行了分析和表征.结果表明,实验制备的NiO粒径为10nm左右,比表面积达到186.3m2/g,并具有合适的孔径分布,NiO赝电容器的工作电压为0.35V,在电流密度为60mA/g时,其比容达到243F/g.以NiO和中孔活性炭分别作为正极和负极材料组装成NiO-AC混合电容器,混合电容器的工作电压达到1.5V,其能量密度为NiO赝电容器的17.2倍,并具有更好的功率特性.     

可控粒径mTiO2/mSiO2及其中空结构mSiO2微球制备

近年来,mTiO_2/mSiO_2复合材料和中空结构介孔二氧化硅在生物催化、药物控释等领域展现出良好的应用前景。在乙醇体系下,以十六胺为模板剂,运用自组装原理制备出介孔氧化钛;并运用晶种法,通过改变TEOS量、模板剂用量、异丙醇和水的用量制备出一种粒径大小在0.80~1.92μm范围内可控的mTiO_2/mSiO_2复合材料;最后在乙醇体系中加入盐酸冷凝回流制备出中空结构介孔二氧化硅微球。通过透射电子显微镜(TEM)、扫描电子显微镜(SEM)、X射线衍射(XRD)对合成的产物进行表征。     

铁铕共掺杂的TiO_2空心微球的制备及光催化活性

通过溶胶-凝胶法制备铁铕共掺杂的TiO_2(Fe~(3+)-Eu~(3+)/TiO_2)空心微球,采用XRD、TEM、BET和XPS等对样品进行表征,以亚甲基蓝(MB)的光催化降解为目标反应,评价其光催化活性。结果表明:SiO_2微球表面均匀地包覆了1层TiO_2,超声有利于提高SiO_2@TiO_2复合微球间的分散性,同时也发现煅烧前对SiO_2@TiO_2复合微球进行研磨处理后所得的Fe~(3+)-Eu~(3+)/TiO_2空心微球部分塌陷,而未研磨和煅烧后研磨所得Fe~(3+)-Eu~(3+)/TiO_2空心微球完整性较好。XRD和BET分析表明,Fe~(3+)-Eu~(3+)/TiO_2空心微球为锐钛矿且具有良好的介孔结构,铁铕共掺杂在TiO_2空心微球中产生协同作用,使Fe3+-Eu3+/TiO2空心微球的粒径进一步减小,比表面积增大。当Fe~(3+)的掺杂量为1.0%、Eu~(3+)的掺杂量为0.5%时,Fe~(3+)-Eu~(3+)/TiO_2空心微球的光催化活性最高。     

用于超级电容器的纳米氧化镍/石墨薄片/银复合电极材料的超声法合成及性能

通过简单超声法制备了球状NiO纳米颗粒、NiO/石墨薄片(NiO/GNS)和NiO/GNS/Ag纳米复合材料。在NiO/GNS和NiO/GNS/Ag复合材料中,GNS作为NiO和Ag纳米颗粒分散的模板,不仅有效避免了NiO和Ag纳米颗粒的团聚,还改善了复合材料的电化学性能。采用场发射扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线衍射对样品的成分、形貌和结构进行了表征。NiO/GNS/Ag复合材料(GNS质量分数为0.5%,Ag质量分数为3%)电极表现出优异的电化学性能。在1A/g时,其初始比电容为501.66F/g,2000次循环后其比电容衰减为440.45F/g。这表明所制备的复合材料是一种有应用价值的超级电容器电极材料。     

La_(0.7)Sr_(0.3)NiO_3/壳聚糖/聚吡咯/牛血红蛋白修饰玻碳电极的制备及构建过氧化氢传感器

在玻碳电极上修饰一层表面均匀的聚吡咯膜,然后利用钙钛矿和壳聚糖的复合膜来固定牛血红蛋白(Hb),制备出性能良好的过氧化氢生物传感器.采用循环伏安(CV)和扫描电镜对修饰电极进行了表征.该传感器对H2O2具有好的催化响应,且响应快.在优化的实验条件下,所制备的传感器对H2O2的线性范围为7.0×10-6～1.5×10-3mol/L,检测限为9.0×10-8mol/L.