液相还原法制备纳米镍粉

为优化纳米镍粉的液相还原法制备工艺,本文以硫酸镍为主盐,水合肼为还原剂,水浴75 ℃条件下,选取产物纯度、产物粒径、反应速率等关键指标开展工艺优化试验,分别研究了NaOH加入量、溶剂种类、有无分散剂,反应物摩尔比,加料顺序五个变量对于镍粉制备的影响.采用XRD和TEM对产物镍粉进行了表征.结果表明,NaOH的加入量影响产物组成,溶剂种类影响产物粒径大小,分散剂对产物的团聚状态有影响,反应物摩尔比以及加料顺序影响体系的反应速率.最终获得如下的优化工艺：NaOH的加入量在0.015~0.02 mol,乙醇和乙二醇做反应溶剂,加入分散剂PVP,反应物摩尔比为4: 1以及采用氢氧化钠与水合肼混合后再向混合溶液中加入硫酸镍溶液的顺序可以获得较为纯净、粒径较小、分散性好的球形纳米镍粉,并且有较快的反应速率.     

液相还原两步法合成纳米铜的工艺研究

目的研究液相还原步法制备铜纳米颗粒过程中,工艺参数对铜纳米颗粒形貌尺寸的影响。方法在水体系下,先用葡萄糖将铜离子预还原为氧化亚铜,再使用次亚磷酸钠将氧化亚铜还原成纳米铜颗粒。分别改变反应过程中的PVP添加量、次亚磷酸钠的浓度以及加热温度,用场发射扫描电镜对所得的产物进行形貌观察。结果 PVP添加量与次亚磷酸钠浓度的提高,都使得铜纳米颗粒的尺寸逐渐减小,并且过量的PVP会造成铜纳米颗粒的团聚;然而随着温度的提高,铜纳米颗粒的尺寸先减小再增大。结论实验的最佳工艺参数为:PVP添加量为2 g,次亚磷酸钠浓度为1.2 mol/L,反应温度为60℃。此条件下所制备出的铜纳米颗粒分散性好、尺寸分布均匀,粒径为400 nm左右。     

1,2丙二醇液相还原法制备纳米镍粉的研究

采用有机醇液相还原工艺,用1,2丙二醇作还原剂,制备了晶粒尺寸小于50nm,具有面心立方晶体结构的纳米镍粉,运用XRD,TEM和SAED微观分析手段,研究了还原体系,中间相和NaOH浓度等因素对制备纳米粉的影响,结果表明：与乙醇相比,采用丙二醇作还原剂可获得粒径更小的纳米粉,且可明显缩短反应时间,对醇－水体系和醇溶液两种反应条件下的还原反应的分析表明,反应历程不同,纳米镍粉的纯度和粒度也不同。     

聚乙烯吡咯烷酮对羟基磷灰石结晶和形貌的影响

采用化学均相沉淀法,在水热条件下以Ca(NO3)2.4H2O和(NH4)2HPO4为原料,合成了具有特殊形貌的羟基磷灰石(HA)微球。在合成过程中加入聚乙烯吡咯烷酮(PVP)为模板剂,研究了PVP的加入和浓度对HA晶体形貌和粒径的影响。结果表明,PVP的加入改变了HA晶体的生长方式,颗粒是由针片状HA晶体组成的微球;HA颗粒的形貌和粒径可以通过调节PVP浓度来控制,当PVP浓度从0%(质量分数,下同)增加到12%时,HA颗粒的形貌逐渐由不规则的絮状团聚物转变为规整的微球,组成微球的结构单元也随PVP浓度的变化有所不同。     

以氢氧化铜为前躯体制备单分散球形氧化亚铜粉末

在不加任何添加剂和高反应物浓度的条件下,于碱性体系中以Cu(OH)2为前躯体,用葡萄糖还原制备了粒径为0.9-2.0μm的单分散球形氧化亚铜粉末。考察了反应温度和反应物(NaOH、葡萄糖、CuSO4)浓度等因素对Cu2O粉末形貌和粒径的影响。利用扫描电镜和X射线衍射分析对Cu2O粉末进行了表征。并根据晶体成核生长理论初步讨论了上述条件对Cu2O粉末形貌和粒径的影响。     

超顺磁性Fe3O4纳米颗粒的多元醇法制备及其在磁共振造影剂中的应用

利用高温多元醇方法制备了核心粒径为5～10nm的超顺磁性Fe3O4纳米颗粒,并且样品在水溶液中具有良好分散性。系统研究了修饰剂的种类和用量,反应温度,反应时间等生长条件对颗粒的尺寸、水中分散性及磁性能的影响。研究表明：选用带有强极性基团的修饰剂如HOOC-PEG-COOH、PAA、PVP,增加修饰剂的用量,提高反应温度和延长反应时间,可以增大颗粒的尺寸、改善它们的分散性、窄化粒径分布。磁性能研究表明所得样品在室温下都具有超顺磁性,并且尺寸越大,饱和磁化强度越大。磁共振实验表明样品对细胞具有很好的造影效果,其中PVP修饰的样品造影效果最好。     

超声辅助电火花放电制备微纳米镍颗粒中超声功率对颗粒粒径的影响

超声辅助电火花放电是一种绿色环保、易于控制的制备微纳米金属粉末的方法.为研究超声功率对微纳米金属粉末粒径分布的影响,本工作通过COMSOL仿真软件模拟声压在工作液中随时间的变化趋势,得出不同换能器功率下工作液中的最大声压值.利用测量得到的最大声压值与工作液理论空化阈值的比较确定了换能器的功率值,通过理论计算得到了不同超声功率对粒径的影响范围.最后采用实验室自制设备制备镍粉,通过SEM观测制备的镍粉的形貌,采用激光粒度分析仪分析镍粉的粒径分布,验证了理论分析结果.结果表明:超声的空化与振动效应能够破碎火花放电产生的汽化和熔融金属液滴;工作液中的空化泡破裂所产生的冲击波使小粒径的镍粉颗粒发生碰撞,动能转换成热能,产生的高温使镍颗粒烧结形成金属烧结颈,使多个小颗粒团聚成不规则的大颗粒.     

溶液还原法制备镍粉体的条件分析

以NiSO4·6H2O为氧化剂,水合肼为还原剂,NaOH为pH调节剂,十二烷基硫酸钠和PVP为分散剂,用溶液还原法制备了平均粒径约1.0μm、粒度分布范围窄、纯度高、多角形的镍粉.讨论了反应温度、pH值、水合肼加入量以及分散剂等因素对反应机理和镍粉体粒度的影响.     

燃烧合成二氧化硅纳米颗粒形成机理的实验研究

为了研究纳米颗粒在火焰中的形成机理,基于电子低压撞击器建立燃烧法合成纳米颗粒的在线表征系统。在扩散火焰中通过氧化六甲基二硅氧烷蒸气制备二氧化硅纳米颗粒;使用该表征系统研究火焰底部、中部和上部的颗粒的粒子数浓度和粒径的关系,提出燃烧法合成纳米颗粒的可能的形成机理。结果表明:火焰区域可以分为化学反应区、凝并区和聚集区。颗粒历经化学反应、成核、凝并、团聚而形成最终颗粒。     

自动连续丝电爆法制备纳米镍粉

研制一种自动连续丝电爆法制备纳米金属粉体的装置,在初始充电电压为5~9 k V时进行电爆实验,并对制得的纳米镍粉进行表征。结果表明:该装置可实现自动连续的电爆过程,制得的纳米镍体呈青灰色;粒径较小时,颗粒近似为正方体形,粒径较大时,颗粒为球形或类球形;增大初始充电电压可有效减小纳米镍粉颗粒粒径的分布范围;初始充电电压大于7 k V时,可制得平均粒径小于30 nm且粒径分布均匀的纳米镍粉。     

NiO包覆Ni纳米颗粒的制备及其氧化特性研究

通过对直流电弧等离子体制备的Ni纳米颗粒钝化处理得到NiO包覆Ni纳米颗粒。并对试样的组成成分、形貌、晶体结构、粒度和氧化特性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)和选区电子衍射(SAED)、热重和差示扫描量热分析仪(TGA/DSC)等手段进行分析。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20~70nm范围内,平均粒径为44nm,壳层氧化膜的厚度为5~8nm。壳核结构防止了纳米Ni颗粒的进一步氧化和团聚。     

Presence of intrinsic defects and transition from diamagnetic to ferromagnetic state in Co<Superscript>2+</Superscript> ions doped ZnO nanoparticles

In this paper, we report the structural, morphological and magnetic properties of pure and Co²⁺ doped ZnO nanoparticles synthesized using sol–gel auto combustion method. The prepared nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area diffraction pattern (SAED), Fourier transform infrared spectroscopy (FTIR) and photoluminescence spectroscopy. The analysis of XRD pattern shows the single phase nature with a hexagonal wurtzite structure for the prepared nanoparticles. The average crystallite sizes of the prepared nanoparticles were found in the range 18–19 nm. SEM images showed that pure and Co²⁺ doped nanoparticles have different morphology. The shape of the prepared nanoparticles is approximately hexagonal shown by TEM image. SAED pattern also confirms the wurtzite structure with single crystalline nature. FTIR spectra showed the characteristic vibrations frequency band of Zn–O. Photo luminescence spectrum showed that two emission peaks, which are ascribed to near band edge transitions and broadened intensive green emission associated with oxygen-vacancy defects. The magnetic properties were measured by vibrating sample magnetometer (VSM) and superconducting quantum interference device with field dependant magnetization at 300 K and temperature dependant magnetization from 0 to 300 K. From VSM analysis, pure ZnO nanoparticles show diamagnetic behavior while Co²⁺ doped ZnO nanoparticles revealed ferromagnetic behaviour at room temperature. The significant changes in M–H loop from diamagnetic behavior to ferromagnetic behavior are due to the intrinsic defects such as oxygen vacancies (Vo) and zinc vacancies (Vz_n). The RTFM has been presented in terms of vacancies in the frame of bound magnetic polaron model.     

Synthesis and Characterization of Fucan-Coated Cobalt Ferrite Nanoparticles

This work presents some results of the synthesis and structural, microstructural, and magnetic characterization of fucan coated cobalt ferrite nanoparticles prepared by using a modified coprecipitation method. Aqueous suspensions of magnetic particles were prepared by coprecipitation of Fe(III) and Co(II) in the presence of NaOH, acid oleic and fucan polymer. The samples were characterized by X-ray diffraction (XRD), electron scanning microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), accelerated surface area, and porosimetry (ASAP/BET-Brunauer-Emmet-Teller) determination and magnetization measurements. Our results reveal that both uncoated and fucan polysaccharide coated CoFe₂O₄ nanoparticles were successfully obtained. The nanoparticles present sizes between 7 to 20 nm and saturation magnetization of the order of 40 emu/g. The nanoparticles thus obtained are suitable for future applications as a solid support for enzymes immobilization and other biotechnology applications.     

化学还原法制备六方B-C-N化合物

采用氰尿酰氯和三溴化硼为原料, 金属钠为还原剂, 通过化学还原法在450℃合成了B-C-N化合物. 利用X射线衍射(XRD), 透射电子显微镜(TEM), 选区电子衍射(SAED), 电子能量损失谱(EELS)和傅立叶变换红外光谱(FTIR)对合成的样品进行了表征. 分析结果表明, 所合成的B-C-N化合物具有六方多晶结构, 其成分为B_0.5C_0.07N_0.43.     

Extracellular synthesis of silver nanoparticles using the leaf extract of Coleus amboinicus Lour.

In the present investigation, Coleus amboinicus Lour. leaf extract-mediated green chemistry approach for the synthesis of silver nanoparticles was described. The nanoparticles were characterized by ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). The influence of leaf extract on the control of size and shape of silver nanoparticles is reported. Upon an increase in the concentration of leaf extract, there was a shift in the shape of nanoparticles from anisotrophic nanostructures like triangle, decahedral and hexagonal to isotrophic spherical nanoparticles. Crystalline nature of fcc structured nanoparticles was confirmed by XRD spectrum with peaks corresponding to (1 1 1), (2 0 0), (2 2 0) and (3 1 1) planes and bright circular spots in the selected-area electron diffraction (SAED). Such environment friendly and sustainable methods are non-toxic, cheap and alternative to hazardous chemical procedures.     

Poly(vinylpyrrolidone) coated iron nanoparticles in polar aprotic solvent

Poly(vinylpyrrolidone) (PVP) coated iron nanoparticles which show well-defined core-shell structures have been successfully synthesized in a polar aprotic solvent. In this approach, PVP was employed not as capping agent, but as coating polymer directly applied to the metallic (iron) core nanoparticles. The morphologies, structures, compositions and magnetic properties of the products were investigated by transmission electron microscopy (TEM), X-ray powder diffraction (XRD), energy dispersive X-ray spectroscopy (EDXS), SQUID magnetometry and FTIR spectroscopy.     

Synthesis, characterization and magnetic properties of NiS1+x nanocrystals from [bis(salicylidene)nickel(II)] as new precursor

[Bis(salicylidene)nickel(II)] was used as a precursor to prepare nickel sulfides nanoparticles of average size 20 nm by a chemical process in oleylamine. The products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible spectroscopy (UV-vis) and photoluminescence (PL) spectroscopy. Magnetization measurement indicates that both of the α-NiS and Ni₃S₄ nanoparticles show pramagnetism due to the size effect.     

Green synthesis of biocompatible gold nanoparticles using Fagopyrum esculentum leaf extract

This report describes the use of ethnolic extract of Fagopyrum esculentum leaves for the synthesis of gold nanoparticles. UV-visible spectroscopy analysis indicated the successful formation of gold nanoparticles. The synthesized nanoparticles were characterized by transmission electron microscopy (TEM), high resolution TEM (HRTEM) and were found to be spherical, hexagonal and triangular in shape with an average size of 8.3 nm. The crystalline nature of the gold nanoparticles was confirmed from X-ray diffraction (XRD) and selected-area electron diffraction (SAED) patterns. Fourier transform infrared (FT-IR) and energy-dispersive X-ray analysis (EDX) suggested the presence of organic biomolecules on the surface of the gold nanoparticles. Cytotoxicity tests against human HeLa, MCF-7 and IMR-32 cancer cell lines revealed that the gold nanoparticles were non-toxic and thus have potential for use in various biomedical applications.     

Large-scale and shape-controlled synthesis and characterization of nanorod-like nickel powders under microwave radiation

The nanorod-like nickel powders were fabricated via hydrothermal liquid phase reduction route under microwave irradiation with hydrazine hydrate as a reducing agent as well as polyvinyl alcohol as a dispersant and/or structure directing agent. The morphology and structure of as-prepared products could be easily tuned by adjusting process parameters such as pH value and microwave irradiation time. The resulting materials were characterized by X-ray diffraction (XRD), scanning electron microscope, transmission electron microscopy and selected-area electron diffraction (SAED). The results demonstrated that pure nickel powders with face-centered cubic (fcc) structure were prepared at relatively mild condition and no characteristic peaks of nickel oxide in the XRD pattern were found. The phenomenon of lattice expansion for Ni powders was explained in details according to the XRD theory. As-prepared Ni sample was of obvious shape anisotropy with length diameter ratio of 5. Magnetic measurements shown that the magnetic properties of nanorod-like (fcc) Ni powders were quite different from those of hexagonal closed-packed (hcp) Ni nanoparticles. Furthermore, it had more strong ferromagnetic properties than that of Ni powders both bulk and nanoparticles.     

Magnetic hollow mesoporous silica nanospheres: facile fabrication and ultrafast immobilization of enzymes

Hollow mesoporous silica nanospheres with large pore size of around 11 nm have been synthesized by a structural difference based selective etching strategy, and the highly dispersed hydrophobic Fe3O4 nanoparticles with a particle size of 5 nm were then impregnated into hollow cores of nanospheres through these large pores by a vacuum impregnation technique. The structural characteristics of obtained magnetic composites were characterized by X-ray diffraction (XRD), Fourier Transform Infrared (FTIR), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Selected Area Electron Diffraction (SAED), Ultraviolet-visible (UV-Vis) and Vibrating Sample Magnetometer (VSM). The results show that the obtained Fe3O4-hollow mesoporous silica composites exhibit superparamagnetic property with saturation magnetization value of 4.17 emu/g. Furthermore, the obtained supports show ultrafast immobilization of hemoglobin and the immobilized enzymes are not denatured, indicating that the superparamagnetic hollow mesoporous silica spheres are excellent support for immobilization of enzymes with magnetic recycling property.