Preparation and characterization of Ni nanopowders prepared by anodic arc plasma

Ni nanopowders were successfully prepared in large quantities by anodic arc discharged plasma method with homemade experimental apparatus in inert gas. The particle size, microstructure and morphology of the particles were characterized via X-ray diffractometry (XRD), transmission electron microscopy (TEM) and the corresponding selected area electron diffractometry(SAED). The specific surface area and pore parameters were investigated by nitrogen sorption isotherms at 77 K with Brunauer-Emmett-Teller(BET) equation and Barrett-Joyner-Halenda (BJH) method. The chemical compositions were determined by X-ray energy dispersive spectrometry(XEDS) and element analysis. The experimental results indicate that this method is convenient and effective, and the nanopowders with uniform size, higher purity, weakly agglomerated and spherical chain shape are gotten. The crystal structure of the samples is FCC structure as the bulk materials, the particle size distribution ranges from 20 to 70 nm, and the average particle size is about 46 nm obtained by TEM and confirmed by XRD and BET results. The specific surface area is 14.23 m^2/g, specific pore volume is 0.09 cm^3/g and average pore diameter is 23 nm.     

阳极弧等离子体制备镍纳米粉的性能表征

采用阳极弧放电等离子体方法成功制备了高纯镍纳米粉末;利用X射线衍射（XRD）、透射电子显微镜（TEM）和选区电子衍射（SAED）、BET吸附法测试手段对试样的成分、形貌、晶体结构、比表面积、粒度及其分布进行性能表征,并采用元素分析仪测定C,H,N含量,采用X射线能量色散分析谱仪（EDS）测定试样所含的元素及其相对含量,用红外吸收光谱（FT-1R）对结构组成进行定性分析.实验结果表明：本法所制备的镍纳米粉末的晶体结构与相应的块体材料基本相同,为fcc结构的晶态,平均粒径为47 nm,粒度范围分布在20 nm～70 nm,呈规则的球形链状分布,比表面积为14.23 m2/g,试样纯度高且具有很强吸附性.     

Preparation and particle size characterization of Cu nanoparticles prepared by anodic arc plasma

1. Introduction Metal nanoparticles exhibit novel physical and chemical properties owing to the small size effect, surface effect, quantum size effect, and quanta tun-nel effect [1-4]. In recent years, the research and de-velopment for metal nanoparticles have attracted significant interest and is still the subject of intense investigation owing to their intriguing properties and various potential applications [5-7]. Because the properties depend strongly on the details of particle size, speci…     

Preparation and particle size characterization of Cu nanopartides prepared by anodic arc plasma

Copper nanoparticles were successfully prepared in large scale by means of anodic arc discharging plasma method in inert atmosphere. The particle size, specific surface area, crystal structure, and morphology of the samples were characterized by X-ray diffraction （XRD）, BET equation, transmission electron microscopy （TEM）, and the corresponding selected area electron diffraction （SAED）. The experimental results indicate that the crystal structure of the samples is fcc structure the same as that of the bulk materials. The specific surface area is 11 m^2/g, the particle size distribution is 30 to 90 nm, and the average particle size is about 67 nm obtained from TEM and confirmed from XRD and BET results. The nanoparticles with uniform size, high purity, narrow size distribution and spherical shape can be prepared by this convenient and effective method.     

Growth mechanism of Cu nanopowders prepared by anodic arc plasma

1 Introduction In recent years, the research and development for metal nanopowders has attracted significant interest and it is still the subject of intense investigation owing to their intriguing properties and extensive prospects [1-5]. Metal nanopowder…     

等离子体制备银纳米粉末的研究

采用阳极弧放电等离子体制备银纳米粉末，并利用X射线衍射(XRD)、透射电子显微镜(TEM)、X射线能谱仪(XEDS)和BET吸附等测试手段对样品的成分、形貌、晶体结构、粒度及其分布、比表面积等进行性能表征。结果表明：本法所制备的银纳米粉末纯度高，分散性好，呈类球形均匀分布；晶体结构与相应的块体材料基本相同，为fcc结构，其平均粒径为24nm，粒径范围在10～50nm，比表面积为23．81m^2／g。     

多元醇还原制取球形钴粉

以自制 Co(OH) 2 为原料 ,乙二醇为溶剂和还原剂 ,制得了分散性很好的球形超细钴粉。研究了单位体积乙二醇中 Co(OH) 2 加入量对钴粉的粒径和形貌的影响。用SEM、XRD、BET和激光粒度分析仪测试粉体的粒子形貌、晶体结构、比表面积和粒度分布。测试结果表明多元醇还原的钴粉为球形 ,以面心立方晶体为主 ,还有微量的简单六方 ;钴粉粒度分布较窄 ,平均粒径为 0 .88μm,比表面积为 3 .46m2 /g,钴含量 >99.5 %。     

阳极弧等离子体制备镍纳米粉

采用自行研制的实验装置，用阳极弧放电等离子体方法制备了高纯镍纳米粉末。利用X射线衍射(XRD)、透射电子显微镜(TEM)和相应选区电子衍射(ED)、BET吸附等对样品的成分、形貌、晶体结构、晶格常数、粒度及其分布、比表面积进行了分析。建立了关于金属超微粒产生过程的近似模型，分析了纳米粉的形成和生长机制，并对整个工艺过程影响纳米粉性能的各种工艺参数进行了理论探讨。结果表明：所制得的镍纳米粉纯度高，晶格结构与相应的致密体相同，为fcc相结构，平均粒径为47nm，粒径范围在20～70nm，比表面积为14．23m^2／g，呈规则的球形链状分布，并发现纳米晶体的晶格常数发生膨胀。     

煅烧对离心雾化制备羟基磷灰石微球结构和性能的影响

在较低温度下对离心喷雾干燥所制备的羟基磷灰石微球进行煅烧,并利用X射线衍射仪、扫描电子显微镜、傅里叶红外光谱仪、比表面积分析仪以及激光粒度分析仪等分析手段,研究了煅烧对羟基磷灰石微球的相组成、微观结构以及比表面积、孔体积和粒度等性能的影响。结果表明,经400℃煅烧,微球比表面积、孔体积及其粒度均明显增大;随煅烧温度升高,比表面积和孔体积均略有降低。     

Preparation and characterization of CuO-CoO-MnO/SiO2 nanocomposite aerogels as catalyst carriers

CuO-CoO-MnO/SiO₂ nanocomposite aerogels were prepared by using tetraethyl orthosilicate (TEOS) as Si source, and aqueous solution of Cu, Co and Mn acetates as the precursors via sol-gel process and ethanol supercritical drying technique. The gelatination mechanism was investigated by nuclear magnetic resonance (NMR) and X-ray photoelectron spectroscopy (XPS). The microstructure and composition of the CuO-CoO-MnO/SiO₂ nanocomposite aerogels were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron dispersive spectroscopy (EDS) and XPS. The specific surface area, pore size and pore size distribution of the nanocomposite aerogels were determined by the Brunauer-Emmett-Teller (BET) method. The products were analyzed by gas chromatography (GC). The results show that the CuO-CoO-MnO/SiO₂ nanocomposite aerogels are porous, with a particle size distribution of 10–150 nm, a pore size distribution of 2–16 nm, an average pore size of 7.68 nm, and a specific surface area of 664.4–695.8 m²/g. The molar fraction of transition metals in the nanocomposite aerogels is 0.71%-13.77%. This kind of structure is favorable not only to increase the loading of catalysts, but also to make full use of the effect of transition metal oxides as cocatalysts; CuO-CoO-MnO/SiO₂ nanocomposite aerogels can be used as a novel catalyst carrier in the safer and environment-friendly synthesis of diphenyl carbonate and other fields of catalysis.     

Preparation, characterization and electrochemical properties of mesoporous LiFe0.99Mo0.01PO4/C

A mesoporous LiFe0.99Mo0.01PO4/C composite was synthesized by the sol-gel method using (NH4)2MoO4 as a doping starting material. The formation of conductive carbon, metal doping and mesopores was achieved simultaneously in the prepared material. The characterizations of crystal structures and microstructures were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), extended X-ray-absorption free-structure (EXAFS) and X-ray-absorption near-structure spectroscopy (XANES), while the surface area was determined using N2 adsorption techniques. Cyclic voltammetry (CV) and charge-discharge cycling performance were used to characterize its electrochemical properties. The sample possessed uniformly distributed mesopores with an average pore size of 4 nm and the specific surface area was about 69.368 m2/g. The results show that the reversible capacity of mesoporous LiFe0.99Mo0.01PO4/C is about 160 mAh/g at 0.1C, 135 mAh/g at 1C and 90 mAh/g at 5C, respectively. The capacity fading is neglectable.     

溶胶-凝胶法有序介孔氧化硅薄膜的蒸发诱导自组装制备

以表面活性剂CTAB为模板,将TEOS与APTES以一定的比例混合,自组装共聚合成出有序介孔氧化硅薄膜,并采用XRD、FTIR、TEM、TGA及N2吸附等手段对PMO薄膜进行了表征,结果表明,当APTES/(TEOS APTES)比例为0.10时,介孔薄膜有序性最好,平均孔径为2.16 nm,比表面积达到1060 m2/g,孔容积达到0.76 cm3/g.     

Preparation and Characterization of Carbon Microfiber Through Shear Pulverization Using Pan-Mill Equipment

Carbon microfiber was prepared through shear pulverization using the self-designed pan-mill type equipment at ambient temperature from short carbon fiber (CF). The effects of shear stress on structure transformations, particles size, microfiber morphology, surface functional groups and crystalline properties during pulverization were studied by laser diffraction particle size analyzer, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), x-ray photoelectron spectroscopy (XPS) and wide-angle x-ray diffraction (WAXD), respectively. SEM analysis indicated that CF was milled into microfiber due to the strong shear and squeezing force. The average particle size of carbon microfiber was reduced to 12.7 μm and specific surface area was increased to 0.6 m²/g after 40 milling cycles. FT-IR and XPS analyses showed that the oxygen-containing groups increased after shear pulverization, and WAXD results illustrated that shear stress offered by mill discs had an obvious damage on the crystal structure of CF, leading to a decrease of crystallinity. Thermal analysis showed that carbon microfiber exhibited good thermal stability. The pan-milling shear pulverization technique is an environment-friendly and efficient method for preparing carbon microfiber.     

WO3-TiO2复合空心球的制备及其光催化性能

以钛酸四正丁酯和偏钨酸铵为原料,采用水热-模板法制备复合WO3-TiO2光催化剂。利用X射线衍射(XRD)、扫描电子显微镜(SEM)、比表面积(BET)和紫外-可见漫反射(UV-Vis DRS)等手段对催化剂的结构和光学性能进行表征。结果表明:WO3-TiO2复合半导体中的TiO2为锐钛矿晶型,焙烧后的WO3-TiO2呈中空球形结构,粒径在320 nm左右,且粒径分布均匀,其比表面积和平均孔径分别为40.95 m2/g和16.91 nm,WO3-TiO2复合半导体的紫外-可见吸收边带较TiO2的红移约50 nm,并在400~500 nm处有吸收。光降解甲基橙(MO)实验显示:经过80 min光照后,WO3-TiO2复合半导体在紫外和可见光下对甲基橙的降解率分别为99.2%和81%,而TiO2的仅为64%和25%,且在紫外和可见光下WO3-TiO2复合半导体的表观速率常数分别是TiO2的3.2和4.9倍左右。     

Preparation of mesoporous titania particles using ionic liquid dissolving starch as templates

A mesoporous titania photocatalyst was prepared via calcining the solution of ionic liquid (1-methyl-3-butyl imidazolium bromide, [BMIM]Br) containing tetrabutyl titanate (TBT) and starch. The microstructure of the prepared mesoporous titania was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and N₂ adsorption/desorption isotherm. The results indicate that the resulting mesoporous titania has a grain size of about 13.9 nm, a special surface area of 106 m²/g, and a pore volume of 0.22 cm³/g, and the pore size can be adjusted by the concentration of starch in ionic liquid. The photocatalytic activity of mesoporous titania in the degradation of methyl orange solution was determined. The effect of the specific surface area of mesoporous titania on the photocatalytic activity was also studied. The prepared mesoporous titania exhibits a high catalytic activity.     

Characterization of nanosized Tb–MCM-41 synthesized by the sol–gel-assisted self-assembly method

The nanosized luminescent Tb–MCM-41 (1:10) is synthesized by means of sol–gel-assisted self-assembly under basic conditions at room temperature. The results of ²⁹Si-MAS NMR and XRD prove that Tb³⁺ doped Si–O framework. The HRTEM image shows that the regular uniform particles with a diameter of 10 nm possess ultralarge pore with 2.0 nm, which is consistent with the result of N₂ adsorption. The BET surface area and porosity of Tb–MCM-41 (1:10) are 1127 m²/g and 0.84 cm³/g, respectively. The patterns of selected-area electron diffraction and XRD of Tb–MCM-41 (1:10) show an Fm3m space group in the cubic. FT-IR results show that the peaks near 970 cm⁻¹ are assigned to the deformation vibration of silanol group. The as-products are calcined at 800 °C and the mesoporous materials possess enormous specific areas and large porosity, it shows that the mesoporous materials are ultrastable.     

Surface properties of modified nanosized silica and their influence on human serum albumin immobilization

Silica powders with different surface functional groups were synthesized using the sol-gel method. The introduction of functional groups on the surface of silica was confirmed by IR spectroscopy. Surface physical parameters of silica particles (specific surface area, pore size, pore shape and volume) were obtained using BET. We have studied the adsorption capacity of human serum albumin on synthesized powders. Using atomic-force microscopy, we determined the size of silica particles with adsorbed protein. The influence of silica particle surface properties on the amount of adsorbed protein is speculated.     

Synthesis, Characterization, and Optimization of Co2SnO4 Nanoparticles via Co-precipitation Method

Nano-structured pure Co₂SnO₄ powders have been synthesized using the co-precipitation method in the presence of oleic acid (OA) as a capping agent. The Taguchi L₄ statistical design was used to investigate the effect of the main parameters (i.e., OA concentration, calcination time, and calcination temperature) on Co₂SnO₄ formation, crystallite size, and morphology. Co₂SnO₄ particles were characterized by powder x-ray diffraction (XRD), energy-dispersive x-ray spectroscopy, scanning electron microscopy (SEM), Fourier transform of infrared spectroscopy (FT-IR), dynamic light scattering (DLS), and Brunauer-Emmett-Teller (BET) surface area measurements. The formation of small and well-crystalline particles, on the order of 41.12-90.60 nm in crystal size, has been determined from XRD patterns and confirmed by SEM and DLS. The specific surface area was measured by a BET method to be 25.43 m²/g. The particle size of the product was observed by DLS to be in the range of 40-105 nm. The results indicated that calcination temperature has the most significant effect on the produced cobalt stannate crystal size.     

碳包覆氧化镍纳米颗粒制备与电化学性能研究

采用直流电弧放电等离子体技术制备了核壳结构碳包覆氧化镍纳米颗粒,并采用X射线衍射、高分辨透射电子显微镜、X射线能量色散分析谱仪和表面物理吸附仪等测试技术对样品的微观结构进行研究。并利用循环伏安法、恒电流充放电以及交流阻抗等技术研究其作为超级电容器电极材料的电化学性能。结果表明:直流电弧等离子体技术制备的碳包覆氧化镍纳米颗粒具有典型的核壳结构,内核为面心立方结构的氧化镍纳米颗粒,外壳为碳层。颗粒形貌主要为立方体结构,粒度均匀,分散性良好,粒径分布在30～70 nm范围,平均粒径为50 nm,外壳碳层的厚度为5 nm。碳包覆氧化镍纳米颗粒具有较高的比容量和良好的电化学活性。     

Electrochemical Performance of Li4Ti5O12 Synthesized by a PVP Combustion Assisted Sol-gel Method

Li4Ti5O12 samples were synthesized via a PVP (polyvinylpyrrolidone) assisted gel-combustion method by varying the calcination temperature. The effect of different roasting temperatures on the structure, the morphology, and the electrochemical performance of the Li4Ti5O12 material was analyzed. The cycle performance, the structure and the morphology of the prepared material were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and charge/discharge test system. The results show that the Li4Ti5O12 powder has a single-phase spinel structure with uniform particles size. The average particle size is 500 nm. The Li4Ti5O12 material synthesized at 800 oC for 8 h possesses excellent performance, and its first discharge capacity is 167.4 mAh/g