Synthesis and characterization of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript> magnetic composite nanoparticles by a one-pot process

Fe₃O₄@SiO₂ core–shell composite nanoparticles were successfully prepared by a one-pot process. Tetraethyl-orthosilicate was used as a surfactant to synthesize Fe₃O₄@SiO₂ core–shell structures from prepared Fe₃O₄ nanoparticles. The properties of the Fe₃O₄ and Fe₃O₄@SiO₂ composite nanoparticles were studied by X-ray diffraction, transmission electron microscopy, energy dispersive spectroscopy, and Fourier transform infrared spectroscopy. The prepared Fe₃O₄ particles were approximately 12 nm in size, and the thickness of the SiO₂ coating was approximately 4 nm. The magnetic properties were studied by vibrating sample magnetometry. The results show that the maximum saturation magnetization of the Fe₃O₄@SiO₂ powder (34.85 A·m2·kg–1) was markedly lower than that of the Fe₃O₄ powder (79.55 A·m2·kg–1), which demonstrates that Fe₃O₄ was successfully wrapped by SiO₂. The Fe₃O₄@SiO₂ composite nanoparticles have broad prospects in biomedical applications; thus, our next study will apply them in magnetic resonance imaging.     

Mechanical properties of TiO2-hydroxyapatite nanostructured coatings on Ti-6Al-4V substrates by APS method

TiO₂-hydroxyapatite (HA) nanostructured coatings were produced by atmospheric plasma spray method. The effects of starting powder composition and grain size on their mechanical properties were investigated. The microstructure and morphology were characterized by X-ray diffraction and scanning electron microscopy (SEM). It is found that the coating with 10% HA has the best mechanical properties. Based on Rietveld refinement method, the mean grain size of the as-received powder (212 nm) extensively decreases to 66.4 nm after 20 h of high-energy ball milling. In spite of grain growth, the deposited coatings maintain their nanostructures with the mean grain size of 112 nm. SEM images show that there is a lower porosity in the coating with a higher HA content. Optical microscopy images show that uniform thickness is obtained for all the coatings.     

Synthesis of lanthanum oxide nanosheets by a green carbonation process

Two-dimensional metal oxide nanostructures, such as nanoplates, nanowalls, and nanosheets, have received further attentions in recent years, due to their outstanding properties resulted from the small thickness and quantum size effects. In this work, lanthanum oxide nanosheets with the thickness of 56 nm had been suc-cessfully prepared by an originally simple method of car- bon dioxide carbonation; the preparation process was green without using surfactants and detergent. The X-ray dif-fraction, transmission electron microscopy, and scanning electron microscopy were used to characterize the pro-ducts. Thermogravimetric-differential thermal analysis and FT-IR were introduced to prove that the lanthanum oxide precursor with lamellar morphology was La2（CO3）3.3H20. The carbon dioxide carbonation method would provide significant benefits containing mild reaction conditions, high efficiency, low cost, and easy to realize large-scale production.     

NaGdF_4:Yb;Er纳米颗粒的合成及对HeLa细胞的生物标记

以稀土硬脂酸盐为前驱体,采用溶剂热法合成了单分散的NaGdF4:Yb,Er上转换荧光纳米颗粒.通过透射电子显微镜(TEM)、X射线衍射仪(XRD)、荧光(FL)光谱仪、磁滞回线(MHL)等对合成的样品进行了表征.所合成的纳米颗粒粒径均一,平均粒径为20 nm左右,形状规则,结晶度高,发光性能良好,同时具有优越的顺磁性.利用经典的Stober法对纳米颗粒进行了表面氨基修饰,将修饰后的纳米颗粒与转铁蛋白结合制成探针,实现了对HeLa细胞的标记与成像.标记结果表明:该方法特异性较好,且红外光激发可有效避免来自生物样品的自体荧光干扰.     

核壳型Co-Pt纳米粒子的氧还原电催化性能

采用两步化学还原法制备不同壳层厚度的核壳型Co-Pt纳米粒子。采用X射线衍射光谱(XRD)、X射线光电子能谱(XPS)及透射电镜(TEM)技术表征催化剂的结构和组成,用旋转圆盘电极动电位扫描法测试其对氧还原反应的催化性能。结果表明:核壳型Co-Pt纳米粒子直径约30 nm;相对于Pt/C,Co-Pt/C具有更高的电催化氧还原活性和抗甲醇性,催化剂随着Pt壳层厚度的增加氧还原活性增大,抗甲醇能力逐渐降低。随着甲醇浓度的增加,氧还原起始过电位增大,峰电流密度减小。     

孔径可调的介孔磷酸铈的合成

采用中性表面活性剂十八胺为模板剂、硫酸铈为铈源，在水热条件下合成具有介孔结构的磷酸铈。通过X-射线衍射、透射电镜、高倍透射电镜和液氮吸附手段对介孔磷酸铈的介观结构、微观形貌和孔道结构进行了表征。结果表明，该材料是的有序的层状相介孔，层间距为2～3nm。产物主晶相为结晶性良好的单斜晶系的独居石磷酸铈，次晶相为正交晶系的磷酸铈。调整无机铈源与表面活性剂的摩尔比，实现磷酸铈介孔孔径在5.5～9.8nm之间可调。该介孔材料的最大比表面积高达113m²/g，孔体积为0.25mL/g。     

化学镀法制备多壁碳纳米管负载非晶态镍-磷纳米粒子催化剂的性能及其苯加氢催化活性研究

通过化学镀工艺,采用以次磷酸钠为还原剂的镀液将镍-磷（Ni-P）纳米粒子负载于多壁碳纳米管（MWCNTs）表面。通过场发射扫描电子显微镜（FE-SEM）、高分辨透射电镜（HR-TEM）、X射线衍射仪（XRD）、选区电子衍射仪（SAED）、电感耦合等离子体质谱（ICP-MS）、傅里叶变换红外光谱仪（FT-IR）、差示热分析仪（DTA）、X射线光电子能谱仪（XPS）等测试手段对催化剂的物理化学性能进行了表征,分析结果表明：Ni-P纳米粒子化学组成为Ni_73.8P_26.2,为非晶态结构实心圆球体,均匀分散负载于MWCNTs外壁,平均尺寸约100 nm,粒度分布窄,镍元素与磷元素之间无明显电子转移,催化剂在350℃以下结构和热稳定性较强。通过催化剂对于苯加氢反应的研究评价了其催化性能,结果表明在Ni-P/MWCNTs催化剂作用下,苯全部选择性地转化为环己烷,催化剂显示出较好的催化活性（71.2%）和高选择性（100%）。     

Preparation and characterization of aligned carbon nanotubes coated with titania nanoparticles

Titania (TiO2) is an environmental-friendly photo- catalyst material with high stability and efficiency, so its preparation methods received extensive atten- tion[1―4], and the products were advanced from dis- persed nano-powder and fastness nano-film[5,…     

电弧法合成填充金属纳米粒子的碳纳米管

用阳极弧法合成了碳纳米管内包覆铁和钴等金属纳米粒子.对合成物用透射电子显微镜(TEM)、X射线衍射(XRD)、电子能谱(EDS)和Raman光谱等方法进行了鉴定和表征.发现包覆粒子的多壁碳纳米管的平均直径约为35nm,其端部和内部包覆的粒子不连续分布、粒径基本均匀,约为20nm.分析了阳极弧等离子体法合成碳纳米管内包覆金属纳米粒子的形成机理.     

Catalytic self-assembly preparation and characterization of carbon nitride nano-tubes by a solvothermal method

A solvothermal reaction of anhydrous CaNaCl3 and sodium using cyclohexane as solvent and NiCI2 as catalyst precursor has been carried out to prepare carbon nitride nanotubes successfully at 230℃ and 1.8 MPa. The carbon nitride nanotubes were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED), electron energy loss spectrum (EELS) and Raman spectrum.SEM and TEM results indicated that the tubes have a length of 20-30 μm, a uniform outer diameter of about 50-60 nm,an inner diameter of 30-40 nm and are highly ordered assembled as bundles. The EELS measurement indicated that the ratio of N/C was about 1.00. The ED and XRD analyses revealed that the tube may have a new CN crystalline structure. The growth mechanism of nanotubes was discussed.     

Characterization of MCrAlY/nano-Al2O3 nanocomposite powder produced by high-energy mechanical milling as feedstock for high-velocity oxygen fuel spraying deposition

Al2O3 nanoparticles and MCrAlY/nano-Al2O3 nanocomposite powder (M = Ni, Co, or NiCo) were produced using high-energy ball milling. The MCrAlY/nano-Al2O3 coating was deposited by selecting an optimum nanocomposite powder as feedstock for high-velocity oxy-gen fuel thermal spraying. The morphological and microstructural examinations of the Al2O3 nanoparticles and the commercial MCrAlY and MCrAlY/nano-Al2O3 nanocomposite powders were investigated using X-ray diffraction analysis, field-emission scanning electron microscopy coupled with electron dispersed spectroscopy, and transmission electron microscopy. The structural investigations and Williamson–Hall res-ults demonstrated that the ball-milled Al2O3 powder after 48 h has the smallest crystallite size and the highest amount of lattice strain among the as-received and ball-milled Al2O3 owing to its optimal nanocrystalline structure. In the case of developing MCrAlY/nano-Al2O3 nanocompos-ite powder, the particle size of the nanocomposite powders decreased with increasing mechanical-milling duration of the powder mixture.     

Preparation and electrochemical property of CMC/MWCNT composite using ionic liquid as solvent

Carboxymethyl cellulose sodium(CMC)/multi-walled carbon nanotube(MWCNT) composite was prepared by dissolving CMC with ionic liquid as solvent.The microstructure and electrochemical properties of CMC/MWCNTs were studied using field emission scanning electron microscopy(FE-SEM),high-resolution transmission electron microscopy(HR-TEM),X-ray diffraction(XRD) system and electrochemical workstation.The experimental results indicated that the CMC dissolved with ionic liquid could be uniformly enwrapped on the surface of MWCNTs,and the coating thickness of CMC was about 5.4 nm.There are obvious oxidation peaks in the cyclic voltammograms curves of glassy carbon electrode coated with a CMC/MWCNT composite in H2O2 phosphate buffer solution.The MWCNT content and ultrasonic time strongly affected the dispersivity and electrochemical property of CMC/MWCNT composite.While the MWCNT content and ultrasonic processing time was 2 wt% and 2 h respectively,CMC/MWCNT composite exhibited excellent electrocatalytic activity.     

热轧态与回火态 AH80 DB 低碳贝氏体钢组织与冲击韧性

采用光学显微镜、扫描电子显微镜和透射电子显微镜对热轧态和回火态AH80DB低碳贝氏体钢的显微组织、马氏体/奥氏体( M/A)岛、第二相的析出行为以及晶界取向差、有效晶粒尺寸进行研究,揭示回火后低碳贝氏体钢冲击韧性得到改善的原因.结果表明：两种试样的组织均由板条状贝氏体、粒状贝氏体和针状铁素体组成,其中回火态试样中针状铁素体组织较多.热轧态钢中存在较大尺寸M/A岛且呈方向性分布,大角度晶界比例占17.33%,有效晶粒尺寸为3.57μm;而回火态钢中M/A岛的尺寸较小,大角度晶界比例增加3.43%,有效晶粒尺寸减小0.56μm.热轧态钢中析出相主要是( Nb,Ti) C,尺寸在50~150 nm之间,回火态试样中析出较多细小的球状( Nb,Ti) C析出相,尺寸在10 nm左右.     

Si含量对TiAlSiN纳米复合涂层的微观结构和力学性能的影响

采用不同Si含量的TiAlSi复合靶,在Si基底片上用射频磁控溅射工艺沉积了TiAlSiN纳米复合涂层,采用X射线衍射仪（XRD）、高分辨透射电子显微镜（HRTEM）和纳米压痕技术研究了Si含量对TiAlSiN涂层的微观结构和力学性能的影响.结果表明：TiAlSiN涂层内部形成了Si₃N₄界面相包裹TiAlN纳米等轴晶粒的纳米复合结构.随着Si含量的增加,TiAlSiN涂层的结晶程度先增加后降低,涂层内部的晶粒尺寸先减小后趋于平稳,涂层的力学性能先升高后降低.当Si与TiAl原子比为3：22时获得的最高硬度和弹性模量分别为37.1 GPa和357.3 GPa.     

蒸汽相水解法制备磁性光催化剂Fe_3O_4/SiO_2/TiO_2及其光催化性能

采用蒸汽相水解法,以Fe3O4纳米磁性颗粒为磁核,在其表面包覆一层SiO2来阻止光腐蚀,然后将锐钛矿相纳米氧化钛沉积在Fe3O4/SiO2颗粒表面,从而制得核壳结构的Fe3O4/SiO2/TiO2磁性复合光催化材料。用X射线粉末衍射仪(XRD)、场发射扫描电镜(FE-SEM)、高分辨率透射电子显微镜(HR-TEM)、探针式震动磁强计等手段对所制备的产物的结构、形貌、磁强度性能进行表征。以300W汞灯为光源,用亚甲基蓝和酸性红模拟污水中的有机染料来评价复合光催化剂的性能。结果表明,磁性纳米微球中TiO2的含量越大,其光催化性能越好,含TiO2质量分数50%的F3O4/SiO2/TiO2磁性纳米微球可在180min内降解亚甲基蓝模拟染料废水,降解率达99%,在80min内降解酸性模拟染料废水,降解率达98%。     

不同载硅量对Li2FeSiO4/C材料电性能的影响

以多壁纳米碳管和Si(OC2H5)4为原料,采用液相法合成包覆了SiO2的多壁碳纳米管(MWCNTs@SiO2),通过调节Si(OC2H5)4的加入量,制备出不同载硅量的前驱体MWCNTs@SiO2,并以此种前驱物合成硅酸铁锂Li2FeSiO4/C材料.采用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、恒流充放电对Li2FeSiO4/C材料进行了表征及电化学性能测试,实验结果表明载硅量为35.72%的MWCNTs@SiO2前驱体合成的Li2FeSiO4/C材料颗粒大小一致,在0.1C电流密度下循环50圈后获得180 mAh·g－1的稳定放电比容量,具有优良的电化学性能.     

密堆六方结构Ni纳米颗粒的合成及其磁性

采用溶胶-凝胶方法制备前驱体样品, 在氩气气氛中不同温度下热处理得到样品. 利用热分析仪、 X射线衍射(XRD)、 透射电子显微镜(TEM)和振动样品磁强计(VSM)研究材料的合成、 形貌、 结构及其磁性. 结果表明, 经300 ℃热处理的样品为具有密堆六方结构的球形Ni纳米颗粒, 且六方Ni单相具有铁磁性质, 平均晶粒尺寸即超顺磁临界尺寸约为12 nm, 室温下在-800~800 kA/m磁场范围内未表现出饱和趋势, 最大比磁化强度为0.58 (A·m2)/kg, 矫顽力为1.592 kA/m.      

热蒸发法制备TeO_2纳米线的生长机理

以金属碲粉为原料,在450℃下采用热蒸发法在镀金玻璃基板上成功合成TeO_2纳米线,利用X射线衍射、扫描电子显微镜、透射电子显微镜对TeO_2纳米线的结构和形貌进行表征,并对其生长机理进行探讨.研究结果表明,具有四方相晶体结构的TeO_2纳米线直径在70~200 nm之间,长度在几百微米至2 mm.通过对不同生长时间所获得产物的形貌观察,对TeO_2纳米线的生长过程进行了分析,推断TeO_2纳米线是通过气-固机制进行生长,镀金薄膜可能只是起到诱导和加速TeO_2纳米线生长的作用.     

热还原法制备LiFePO4/C复合材料的电化学性能

使用廉价的三价铁Fe2O3为铁源,以蔗糖为还原剂和导电剂,通过热还原法制备了LiFePO4/C复合材料。运用TGA-DAT曲线对反应机制进行了分析,利用X射线衍射(XRD)、扫描电镜(SEM)、恒流充放电和循环伏安测试等测试手段对不同覆碳量合成材料进行了表征和电化学性能检测。结果表明:所合成的LiFePO4均为纯相,其中含碳1.07%的样品0.2C倍率下的放电比容量为143.32 mAh/g。     

Aqueous phase synthesis and fluorescence properties of inverted core/shell ZnSe/CdSe nanocrystals

We report a facile aqueous phase synthesis for prepar-ing water-soluble inverted core/shell ZnSe/CdSe semiconductor nanocrystals. The samples were characterized by X-ray diffraction (XRD),transmission electron microscopy (TEM),and their optical properties were investigated by using UV-vis-NIR spectropho-tometer and fluorescence spectrophotometer. The results indicate that the synthesized ZnSe/CdSe nanocrystals are inverted core/shell structure with diameter of about 5 nm. Furthermore,their absorption band-edge is red-shifted with the growth of CdSe shell; correspondingly,their emission wavelength can be tuned from 460 nm to 604 nm.