液相化学还原法制备不同形貌的多晶纳米镍

采用液相化学还原法,在1,2-丙二醇体系中,分别使用吐温-80（Tween-80）、聚乙二醇-6000（PEG-6000）和十二烷基硫酸钠（SDS）与聚乙二醇-6000（PEG-6000）的混合物作为修饰剂,利用1,2-丙二醇还原相同母体醋酸镍,制备形貌分别为海绵体、纤维状、雪花状的多晶纳米镍;在水体系中,使用SDS为修饰剂,利用水合肼还原相同母体醋酸镍,制备球形多晶纳米镍。通过X射线衍射（XRD）、透射电子显微镜（TEM）、选区电子衍射（SAED）对纳米镍进行表征。利用傅立叶红外（FTIR）分析初步解释不同形貌纳米镍的形成机理。     

吐温和十二烷基硫酸钠作修饰剂对水热合成法制备纳米铜的影响

在一定温度下的水溶液中,以硫酸铜为前驱体,抗坏血酸(Vc)为还原剂,加入适量修饰剂,进行了粒径、形貌可控的纯铜纳米粒子的合成。通过X射线衍射分析(XRD)、透射电子显微镜观察(TEM)、选区电子衍射分析(SAED)和傅立叶红外光谱分析(FTIR)等手段对纳米铜进行了表征。制备过程中添加的修饰剂对铜粉颗粒的粒径大小、粒径分布、形貌和晶型结构的影响很大。分别探讨了单一修饰剂(吐温系列(Tween-20、Tween-40和Tween-80)和十二烷基硫酸钠(SDS))和复配修饰剂(SDS Tween-20、SDS Tween-40和SDS Tween-80)的影响作用,并初步解释了修饰剂的作用机理,将其归纳为静电效应和位阻效应。     

不同有机官能团对室温下纳米银形貌控制合成的影响

选择10种含有不同官能团的有机物为表面修饰剂,如聚乙烯吡咯烷酮、吐温-80、十二烷基硫酸钠、聚丙烯酸钠、聚乙二醇、山梨醇、十二烷基磺酸钠、聚乙烯醇、十二烷基苯磺酸钠和十六烷基三甲基溴化铵等,在室温下进行了平均粒径在2～131nm范围内纳米银颗粒的控制合成研究.有机修饰剂中含有的不同官能团对制得的纳米银形貌的影响主要取决于有机修饰剂的官能团特性和还原剂的还原能力.在不同还原条件下,含多醚键的聚乙二醇、吐温-80皆易于合成出平均粒径为几纳米、粒径分布窄、分散性好的纳米银.在弱还原剂条件下,十六烷基三甲基溴化铵诱导生成了三角形片状纳米银,但是在强还原剂存在条件下生成了粒状纳米银.粒径大于10m的纳米银晶体的生长是通过小颗粒的聚集与熔合而成,而不是经过小颗粒的溶解-沉积过程形成.     

玫瑰花状Bi2S3的制备与表征

以适量的月桂酸硫脲咪唑啉季铵盐（SUDEI）为表面活性剂，采用溶剂热法在N-N二甲基甲酰胺（DMF）中150℃反应12h，制备出了玫瑰花状的Bi2S3，并采用TEM、SEM观察其形貌；IR测试表面活性剂对Bi2S3的修饰作用；X射线衍射测试其晶体形态。讨论表面活性剂用量和不同溶剂对其形貌的影响，得出在DMF溶剂中，SUDEI用量为6g／L，反应时间为12h，得到玫瑰花状的Bi2S3。     

尺寸和形貌可控的纳米晶制备方法取得新进展

中国科学院长春应化所高分子物理与化学国家重点实验室姬相玲研究员领导的研究小组，近日成功地制备了球形、泪滴状、棒状、稻米状等多种形貌的二氧化锆纳米晶，该晶具有粒径分布窄、高结晶性和较少表面缺陷的特点，是高质量的纳米晶。这些尺寸可控、形态各异的纳米晶易溶于溶剂，可望用于燃料电池电解质、热阻隔涂层、电光材料、气体传感器、抗腐蚀及催化剂等。相应成果已申请专利，并已发表于J．Am．Chem．Soc．。     

Y2O3：Eu^3＋纳米晶的制备及其光学性能研究

以NaOH,Y（NO3）3·6H2O和Eu（NO3）3．6H2O为前驱体,通过添加络合剂PEG-2000,采用水热法,成功地合成了Y2O3：Eu^3＋纳米棒和纳米管,并采用先进的测试手段对其结构和性能进行了表征与测试。探讨了Y2O3：Eu^3＋纳米棒和纳米管的生长机制,同时研究了Y2O3：Eu^3＋纳米晶的光致发光性能。研究结果表明,水热温度、反应时间、NaOH的添加量和PEG-2000对产物形貌有着非常重要的影响,所制备的材料具有Eu^3＋的特征红光发射,并在Eu^3＋的掺杂量为5％（摩尔分数）时样品发光最好。     

表面修饰Cu纳米微粒的制备及摩擦学性能(英文)

利用两相萃取法合成了二辛基胺二硫代氨基甲酸(DTC8)表面修饰铜纳米微粒;采用X射线衍射仪、透射电子显微镜、红外光谱仪表征了铜纳米颗粒的尺寸、形貌和结构,采用四球摩擦磨损试验机评价了纳米铜添加剂在液体石蜡中的摩擦学性能,并采用扫描电子显微镜观察了磨斑形貌。结果表明:DTC8修饰铜纳米微粒的粒径较小,粒径分布较窄。与此同时,表面修饰纳米铜作为润滑油添加剂具有优异的抗磨性能,这可能是由于熔点低且易变形的纳米铜可填充磨损表面微坑而起到自修复作用所致。     

多形性SrSO_4纳米粉体的制备与生长机制

采用化学沉淀法制备出具有不同形貌(片状、柱状和等轴状等)的纳米SrSO_4粉体.采用扫描电镜和X射线衍射仪等对粉体的结构、形貌及生长机制进行了研究.片状SrSO_4粉体厚度约100 nm,片长约200 nm;柱状粉体横向长度为80～150 nm,纵向长度为700～800 nm;等轴状粉体粒径约80 nm.衍射强度对比表明,低能面(002)与(210)晶面相对生长的快慢导致了片状和柱状SrSO_4晶体的形成;而反应物浓度的降低、EDTA的络合以及PEG的分散等环境因素的改变降低了晶体生长驱动力,导致球状SrSO_4晶体的形成.     

含萃取剂修饰的纳米硫化铅有机流体的制备与表征

用溶剂萃取沉淀法直接在有机溶剂中合成了含萃取剂Cyanex 301修饰的PbS纳米粒子的有机流体,用IR、UV、TEM和XRD等表征了粒子的结构与形貌.结果表明,所合成的粒子由Cyanex 301修饰层和PbS纳米粒子构成,萃取剂和PbS粒子之间存在S→PbS的键合作用,表面修饰层的存在有效地阻止了纳米粒子的团聚,平均粒径20 nm.纳米粒子在汽油中的负载量可达10 g.L-1以上.     

多功能表面纳米针布阵材料的研究

通过定向电结晶方法制备了具有纳米针布阵结构的镍基纳米材料,所获得的纳米镍针直径一般为50～200 nm,高为150～500 nm.实验结果表明纳米针布阵结构的尺寸、形状等可通过结晶调整剂浓度以及电结晶时间等对纳米针布阵材料的结构分析证明镍基纳米针在(111)晶面上有较强的织构现象,说明镍基纳米针布阵结构的形成是由于晶体优先在(111)面上外延生长所至.另外,本文还就这种材料在电子方面的应用等进行了探讨.     

Preparation and characterization of Y3Al5O12:Ce and Y2O3:Eu phosphors powders by combustion process

A nickel hydroxide, Ni(OH)₂, was prepared by microwave-assisted heating technique from nickel nitrate aqueous solution and sodium hydroxide (assigned as PM). Then, the as-prepared PM was oxidized by liquid oxidation with sodium hypochlorite (assigned as PMO). Further, pure nanocrystalline nickel oxide (NiO) particles were obtained from the as-prepared PMO by calcination at 300, 400, 500, 600, 650 and 700 °C (labeled as C300, C400, C500, C600, C650 and C700, respectively). The as-prepared powders (PM and PMO) and the NiO nanoparticles were characterized by X-ray diffraction (XRD), infrared spectroscopy (IR), temperature-programmed reduction (TPR) and scanning electron microscope (SEM). The results indicated that the particle size of nickel oxide was controlled by the calcined temperature. The average crystal size of the NiO nanoparticles ranges from about 5 to 35 nm at 300–700 °C. Mechanism of nickel oxide nanocrystallite growth during thermal treatment was investigated.     

十二烷基硫酸钠调控合成梭形银纳米粒子

在十二烷基硫酸钠(SDS)溶液中,用柠檬酸(CA)还原硝酸银合成梭形银纳米粒子.紫外-可见光谱(Uv-vis)和透射电镜(TEM)实验结果表明,在固定SDS/CA质量比为50:50条件下,所制备的银粒子两头尖,中间宽,呈梭形结构.梭形银粒子的形成主要是SDS在不同晶面的吸附使得晶面的生长速率不同所致.SDS在梭形银粒子的形成过程中不是起模板作用,而是作为吸附剂和分散剂.     

Influence of surfactants on co-precipitation synthesis of strontium ferrite

Strontium ferrite (SrFe₁₂O₁₉) particles were prepared by co-precipitation method. The ferrite precursors were produced from aqueous mixtures of ferric chloride and strontium nitrate by co-precipitation, using 3 mol/L sodium hydroxide aqueous solutions as precipitant. Three surfactants sodium dodecyl sulfate (SDS), polyethylene glycol 6000 (PEG-6000), cetyltrimethylammonium bromide (CTAB), were applied and the influence of surfactants on the properties of the strontium ferrite particles was studied. The ferrite precursors were first precalcined in a muffle furnace at 400 °C and then mixed with KCl and NaCl using a planetary milling machine in order to lower the calcination temperature. Subsequently the mixtures were calcined at various temperatures. Structure and magnetic properties of the particles were characterized by X-ray powder diffraction, transmission electron microscopy and vibrating sample magnetometer. In this paper, effects of Fe³⁺/Sr²⁺ mole ratio were first verified and annealing temperatures were then discussed. The results show the strontium ferrite phase begins to form at 650 °C and complete at 800 °C after calcination, and the particles prepared using CTAB exhibit the best properties with respect to particle size and dispersibility.     

表面活性剂对镀Ti金刚石-Ni复合电沉积行为的影响

研究了阴离子表面活性剂十二烷基硫酸钠(SDS,sodium dodecyl sulfate)和阳离子表面活性剂十六烷基三甲基溴化铵(CTAB,cetyl trimethyl ammonium bromide)对镀Ti金刚石-Ni复合电沉积的影响,并结合循环伏安、交流阻抗等电化学方法研究了镀Ti金刚石-Ni镀液中Ni电沉积过程。结果表明:与未镀覆金刚石相比,镀Ti金刚石与Ni层浸润性得到提高。浓度为0.05 g/L的SDS对Ni电结晶过程有抑制作用,而浓度为0.05 g/L的CTAB能促进Ni~(2+)离子转移并加快Ni的电沉积过程。SDS和CTAB都能促进电沉积过程中氢气的析出并细化Ni镀层,同时减少镀层针孔和凹痕。     

直流电弧等离子体制备NiO包覆Ni纳米颗粒

采用直流电弧等离子体技术制备NiO包覆Ni纳米颗粒,对初产物经过钝化处理得到有氧化膜保护的NiO包覆Ni纳米颗粒.采用高分辨透射电子显微镜(HRTEM)、X射线衍射(XRD)、透射电子显微镜(TEM)、选区电子衍射(SAED)、热重和差示扫描量热分析仪(TGA/DSC)以及傅里叶变换红外光谱 (FTIR)等手段对试样的成分、表面组成、形貌、晶体结构、粒度、红外吸收性能和氧化特性进行了分析.结果表明:经过表面钝化处理的NiO包覆Ni纳米颗粒具有明显的核-壳结构,内核为纳米Ni,外壳为NiO氧化物;颗粒呈球形,粒度均匀,分散性良好,粒径分布在20～70 nm范围,平均粒径为44 nm,壳层氧化膜的厚度为5～8 nm;壳核结构可防止纳米Ni颗粒的进一步氧化和团聚,且使红外吸收峰发生蓝移.     

Understanding of the shape-controlled synthesis of strip shape diamond under high pressure and high temperature conditions

We present the shape-controlled synthesis of strip shape diamond with stretched crystal faces along {100} or {111} direction and larger length-to-radius ratio than the conventional diamond in the designed NiFe-C system at high pressures and high temperatures (HPHT). A series of synthetic experimental results on the strip shape diamonds were obtained at different pressures and temperatures. Under the constant pressure condition, the morphology of the strip shape diamond varied with the increase of temperature obviously. Fourier transform infrared (FTIR) micro spectroscopy and Raman spectroscopy revealed that the various locations of crystal face have different nitrogen impurity concentration, and internal strain and defects in these strip shape crystals. According to these results, it can be concluded that the difference of growth rates at various crystal faces results in different crystal morphologies. Based on the growth characteristics, we suggest that composition segregation of the metal film around the growing crystal induces the formation of strip shape diamond.     

Effects of different functional group-containing organics on morphology-controlled synthesis of silver nanoparticles at room temperature

Silver nanoparticles with average particles sizes ranging from 2 to 131nm were manipulatively synthesized starting from silver nitrate using different functional group-containing organic modifiers at room temperature. The effects of the organic modifiers on the morphology of the resulting silver nanoparticles were strongly dependent on the intrinsic properties of the functional groups and the reducibility of the reductant. Numerous ether bonds （-0-）present in polyethylene glycol and Tween-80 were beneficial to the formation of silver nanoparticles with particle sizes of several nanometers in a narrow size distribution in both weak and strong reducing environments. Cetyltrimethylammonium bromide induced the formation of nanosized silver triangle plates in a weak reducing environment. The crystal growth of the silver nanoparticles with particle sizes of more than lOnm was postulated through an adhesion process of small-sized particles followed by a subsequent coalescence process under the present reaction conditions.     

合成金刚石用水雾化触媒粉末Fe70Ni30性能的研究

我国近年普遍采用水雾化粉末触媒Fe70 Ni30合成金刚石,本文对这种粉末形貌、成分、粒度分布、氧含量、相组成等作了分析研究.结果表明:粉末呈不规则状;粒度呈正态分布,D50= 22.9 μm;粉末杂质含量很低:初始粉氧含量为0.2％(质量分数),将触媒粉和石墨粉混合(质量比3:7)压成合成柱,在1000℃,真空10-...