有机盐制备的Fe3O4-葡聚糖纳米粒子的磁性能及表征

利用葡糖酸铁(C12H22FeO14·2H2O)和柠檬酸铁(C6H5O7Fe·5H2O)参与的化学共沉积法制备出单分散核心氧化铁的平均粒径为4.1nm,葡聚糖厚度约为11nm,总体平均粒径为26nm的Fe3O4葡聚糖复合纳米粒子.研究结果表明,复合粒子Fe3O4葡聚糖具有超顺磁性.制备过程中没有N2保护,得到的Fe3O4无机粒子的晶体结构几乎没有发生变化,证明了有机盐的抗氧化性,合成的Fe3O4葡聚糖复合纳米粒子具有较好的磁性能.其在室温下(300K)的饱和磁化强度为52emu/g,低温下(5K)的饱和磁化强度为63emu/g.并利用TEM、XRD、DLS和VSM(振动样品磁强计)等手段对其粒结构、形态、粒径和磁性能进行了表征.     

H2O2氧化法制备Fe3O4纳米颗粒及与共沉淀法制备该样品的比较

在近中性条件下,利用H2O2氧化Fe(OH)2胶体成功制备了Fe3O4纳米颗粒.分别利用透射电镜(TEM),x射线衍射仪(XRD),振动样品磁强计(VSM)和超导量子干涉仪(SQUID)对样品的形貌,结构,宏观磁性进行了表征和测量.TEM图像表明样品为球形颗粒,直径大小约18nm,且分布较均匀.XRD结果表明样品为立方尖晶石结构.穆斯堡尔谱测量表明样品室温下对应两套六线谱,样品的晶体结构存在缺陷,内磁场略小于块体Fe3O4的值.宏观磁测量表明样品的饱和磁化强度可达67×10-3A·m2/g,在20 K出现了Verwey转变.选择该法制备的Fe3O4纳米颗粒与共沉淀法得到的样品作了磁性比较.宏观磁测量表明共沉淀法制备的样品在外磁场为1T时仍未饱和,磁化强度仅为46×10-3A·m2/g,在178K出现了超顺磁转变温度,且在测量温度范围内没有发现Verwey转变.     

CoFe2O4纳米颗粒的结构、磁性以及离子迁移

聚乙烯醇(PVA)溶胶凝胶法制备出CoFe2O4纳米微粉,用X 射线衍射研究了铁氧体纳米颗粒的结构.测量了CoFe2O4纳米颗粒80-873 K的变温穆斯堡尔谱,发现纳米颗粒的磁转变温度范围为793-813 K,比块体材料的磁性转变温度要低.CoFe2O4纳米颗粒的德拜温度θA=674 K,θB=243 K,比块体材料要小.CoFe2O4纳米颗粒超精细场Hf随温度的变化符合T3/2+T5/2定理.当温度较高时,平均同质异能移IS随温度的升高而减小,并呈线性关系.     

竹节状α-Fe2O3纳米棒的制备、表征和性能研究

以硝酸铁为铁源,氨水为沉淀剂,聚乙二醇(PEG)为分散剂,采用共沉淀法制备氢氧化铁前驱体,然后将获得的前驱体在450℃、氮气保护下热处理2 h,最后利用透射电镜、X射线衍射、拉曼光谱和近边X射线精细结构光谱(NEXAFs)表征样品的形貌和结构,并使用HH-50型振动样品磁强计测量样品在室温下的磁学行为.透射电镜结果显示,获得的样品由氧化铁纳米颗粒和竹节状氧化铁纳米棒组成,纳米颗粒的粒径范围为50～100 nin,纳米棒的直径大约为10 nin.XRD表征显示样品中氧化铁纳米棒和纳米颗粒为赤铁矿型α-Fe2O3;光谱实验结果证实了样品中氧化铁纳米颗粒和纳米棒的结构是α-Fe2O3;磁学性能测试表明获得的样品表现为典型铁磁性材料的磁滞回线,其饱和磁感应强度约为64.65 emu·g-1,矫顽力的大小约为15.13 Oe.     

Yb3+/Er3+共掺(MLaFn)x(M=0,K;n=3,4;x=1,1.5)纳米材料的控制合成及其上转换发光性质

采用水热与溶剂热结合的方法,在乙二醇-正己醇体系中,通过调节KF与RE(RE=La,Yb,Er)的量比、反应温度和反应时间实现了由LaF_3(六角相)到KLaF_4(立方相、六角相)晶型的控制合成。借助透射电子显微镜(TEM)和X射线粉末衍射(XRD)对样品的结构和微观形貌进行表征。结果表明,当KF/RE比例为2. 25时,制备的样品为片状的六角相LaF_3纳米颗粒;当KF/RE比例为3. 00时,得到具有近似球形的立方相KLaF_4纳米颗粒;当KF/RE比例为4. 25时,得到了六角相(KLaF_4)_(1. 5)纳米颗粒。上转换发射光谱显示:所有的样品在近红外光(980 nm)激发下,均有3个明显的发射峰,在522 nm、544 nm处分别对应于Er~(3+)的~4S_(3/2),~2H_(11/2)→~4I_(15/2)能级跃迁,655 nm处属于Er~(3+)的~4F_(9/2)→~4I_(15/2)能级跃迁。     

SnO2:Eu3+纳米晶的水热法制备及发光性能

采用水热法制备了Eu3+掺杂SnO2纳米发光粉,样品在不同温度下热处理得到不同粒径尺寸的纳米颗粒.利用X射线衍射(XRD)与光致发光(PL)谱对样品进行表征.XRD分析表明:SnO2:Eu3+样品均为纯相金红石结构.PL测量表明:水热法直接制备的样品的激发谱由Eu3+的f-f本征激发峰组成,而经过热处理后样品的激发谱由O2--Eu3+电荷迁移带和Eu3+的f-f本征激发组成;样品的发光强度与颗粒大小有密切关系.     

用水热法合成掺杂Pr~(3+)的NiPr_xFe_(2-x)O_4纳米颗粒及其表征

采用水热法制备了掺杂Pr3+的NiPrx Fe2-x O4(x=0.0,0.01,0.025,0.05,0.075,0.1,0.15)纳米颗粒.实验结果表明制备的样品是立方体结构的纳米颗粒,当掺杂量为0x≤0.1时Pr3+能成功掺杂到NiFe2O4尖晶石晶格内,但掺杂量x0.1(x=0.15)时会出现杂峰.随着掺杂量从0增加到0.1,样品的平均晶粒尺寸从47nm减小到18nm,饱和磁化强度从55A·m2/kg单调减小至37A·m2/kg,矫顽力从4.7×103 A/m减小到3.4×103 A/m.饱和磁化强度减少的原因主要是由于室温下无磁性的Pr3+代替NiFe2O4中的Fe3+造成的.     

离子交换树脂法制备纳米ZnS

以Zn(NO3)2·6H2O为锌源,Na2S为硫源,采用强碱性阴离子交换树脂法制备了纳米ZnS,并对形成的ZnS纳米粒子进行了XRD、TEM表征.XRD表征计算结果表明样品约为粒径6-10nm的小颗粒,TEM表征结果可观察到样品为由6-10nm的小颗粒团聚而成的50-80nm的大颗粒组成的.     

磁控溅射法制备金团簇纳米颗粒及性能表征

 采用磁控溅射法制备金团簇纳米颗粒，用透射电镜(TEM)、X射线衍射(XRD)、紫外可见光分光光度计(UV-Vis)和X射线光电子能谱(XPS)等分析手段对其表征，研究了金团簇纳米颗粒的形貌、颗粒度、结构、光吸收性质及物质成份。研究结果表明：制备的金团簇纳米颗粒呈球形，平均粒径在10 nm左右，粒径分布均匀，无团聚、氧化现象，颗粒的结构为面心立方。在519 nm处出现团簇颗粒的表面等离子共振吸收峰，测试得到Au(4f_7/2)和Au(4f_5/2)电子的结合能分别为83.3 eV和86.9 eV，并且没有出现金的氧化产物。     

水浴法制备ZnO纳米棒及其场发射性能

用硝酸锌(Zn(NO3)2·6H2O)与六亚甲基四胺(C6H12N4)以等浓度配制成反应溶液,通过水浴法制备出了形貌可控的棒状ZnO纳米结构,讨论了不同反应浓度及衬底对ZnO表面形貌的影响.样品的XRD和扫描电子显微镜分析结果表明,所得产物均为六方纤锌矿结构,在有晶种层的衬底上制备出的ZnO纳米棒沿(001)方向并垂直于衬底表面生长.随着反应浓度的增加,ZnO纳米棒的直径增大,长径比减小.样品的场发射性能测试表明,反应溶液浓度为0.005 mol/L,以铜膜为晶种层的硅衬底上制备出的场发射阴极具有较好的场发射性能.     

Preparation of CdO nanoparticles by mechanochemical reaction

CdO nanoparticles of 43 nm in crystal size were successfully synthesized by the mechanochemical reaction (CdCl₂ + Na₂CO₃) with NaCl as a diluent and subsequent thermal treatment at 700°C for 2 h. The samples were characterized by differential thermal analysis (DTA), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and transmission electron microscopy (TEM). Effect of calcination temperature on the crystal size of CdO nanoparticles was primarily investigated. The apparent activation energy of CdO nanoparticle formation during thermal treatment was calculated to be 12.2 kJ/mol.     

Sonochemical syntheses of a new nano-plate cadmium(II) coordination polymer as a precursor for the synthesis of cadmium(II) oxide nanoparticles

Nanoplates of the three-dimensional coordination polymer, {[Cd(3)(3-pyc)(4)(N(3))(2)(H(2)O)](n) (1), 3-pyc(-)=pyridine-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Cadmium(II) oxide nanoparticles were prepared from thermal decomposition in oleic acid and direct calcination of compound 1 at different temperatures. The thermal stability of nano-sized compound 1 was studied by thermal gravimetric (TG) and differential thermal analyses (DTA). Results show that the size and morphology of the CdO nanoparticles are dependent upon the particles size of compound 1 and the thermolysis temperature. A decrease in the particle size of compound 1 leads to a decrease in the particle size of the CdO, while an increase in the processing temperature leads to an increase in the particle size of the produced cadmium(II) oxide nano-particles.     

包覆镍铁氧体纳米粒子的空心玻璃微珠复合材料的制备与电磁性能研究

"用高分子凝胶法制备了包覆镍铁氧体纳米粒子的空心玻璃微珠复合材料．玻璃微珠含量为25%、50%和75%的复合粉的结构、表面形貌和电磁性能分别用X射线衍射仪、扫描电镜、能谱仪、红外光谱和HP8510网络分析仪来表征．结果表明,复合粉由镍铁氧体、石英和莫来石相组成．随着微珠含量的增加,镍铁氧体衍射峰强度迅速降低,莫来石衍射峰强度迅速增强．当温度达到800 ℃时,纯尖晶石结构的镍铁氧体在玻璃微珠表面生成．当玻璃微珠含量为50%时可获得均一、连续的镍铁氧体涂层．大部分镍铁氧体粒子的尺寸小于80 nm．玻璃微珠含量     

不同压制压力下NiFe2O4纳米固体的ESR研究

 以反滴共沉定法制备了NiFe₂O₄纳米微粉，并在不同压力下将其压制成纳成米固体，然后用XRD谱和ESR谱研究了NiFe₂O₄纳米固体结构和界百状态随压制压力的变化。实验结果表明，NiFe₂O₄纳米固体的结构在高压下没有明显的变化，但其ESR谱的共振线宽和g因子值随着压力升高均表示出先逐渐增大至最大值，然手缓慢下降的规律。这种变化可以归因于纳米固体内部界面离子间的磁相互作用在压力的下所发生和变化。这引起实验结果境示，对于NiFe₂O₄纳米固体而言，最佳的成型压力是4.5 GPa，在此压力下，NiFe₂O₄纳米粒子既可以被压制成致密的纳米固体，又能够保留下它们的纳米结构和纳米性质。     

Synthesis of ZnFe2O4 nanocrystallites by mechanochemical reaction

Mechanochemical reaction of ZnO and α-Fe₂O₃ in a planetary mill formed an amorphous precursor, which was subsequently heated to successfully produce zinc ferrite (ZnFe₂O₄) nanocrystallites. The amorphous precursor and nanocrystallites were characterized by differential thermal analysis (DTA), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and transmission electron microscopy (TEM). Calcination of the precursor powder at 600 °C led to the formation of ZnFe₂O₄ nanocrystallites of about 22 nm in crystal size, and most of particle was about 10-50 nm in diameter. Effect of calcination temperature on the crystal size of the nanoparticles was investigated. The mechanism of nanocrystallite growth was primarily investigated. The activation energy of ZnFe₂O₄ nanocrystallite formation during thermal treatment was calculated to be 18.5 kJ/mol.     

Formation of ZnO,MgO and NiO Nanoparticles from Aqueous Droplets in Flame Reactor

Nanoparticles of ZnO, MgO and NiO were produced from droplets of aqueous salt solution in the flame spray pyrolysis reactor. Conventional spray pyrolysis, in which electrical furnace reactor is used, is reported to produce nanoparticles only from acetate precursor. If the reactor pressure is low (60torr), nitrate salt precursor is also known to produce nanoparticles. In this paper, we report that nanoparticles are produced from nitrate as well as acetate salt precursor solution when propane–oxygen diffusion flame is used to decompose aqueous aerosol droplets. At low flame temperature, however, nanoparticles are not formed and the particle morphology is similar to the morphology produced by the conventional spray pyrolysis. At high flame temperature, nanoparticles are formed, regardless of the salt type. Nanoparticles are formed at lower flame temperature from acetate salts than from nitrate salts. All nanoparticle prepared in this work were fully crystallized and the size measured from transmission electron microscopy images was 30nm. This size agreed well with the particle size calculated from X-ray diffraction and specific surface area data.     

费-托合成制清洁燃料用担载纳米钴基催化剂制备中热处理对其结构和催化性能的影响

" 应用浸渍法在不同的焙烧条件(90~500 ℃)制备了一系列Al2O3担载钴基催化剂(质量含量为15%);采用XRD、XPS、程序升温还原对其进行了结构表征和分析,考察其在一氧化碳选择加氢制备清洁燃料用长链烷烃的反应中的催化性能．XPS结果表明,对于在90~200 ℃焙烧的催化剂,仍可观察到未完全分解的硝酸钴的存在;对于在200~500 ℃焙烧的几个催化剂可观察到Co3O4的物相．对于经过几种热处理制备的氧化铝担载的四个纳米钴基催化剂(200~500 ℃热处理),XRD和XPS结果表明四个样品中主要是9     

A simple thermal decomposition synthesis, magnetic properties, and cytotoxicity of La0.7Sr0.3MnO3 nanoparticles

This study reports the new and simple synthesis of magnetic La_0.7Sr_0.3MnO₃ (LSMO) nanoparticles by thermal decomposition method using acetate salts of La, Sr and Mn as starting materials. To obtain the LSMO nanoparticles, thermal decomposition of the precursor is carried out at the temperatures of 600, 700, 800, 900, and 1000°C for 6 hours. The synthesized LSMO nanoparticles were characterized by XRD, FT-IR, TEM and SEM. Structural characterization shows that the prepared particles consisted of two phases of LaMnO₃ (LMO) and LSMO with crystallite sizes ranging from 18 to 55 nm. All the prepared samples have a perovskite structure which changes from cubic to rhombohedral with the increase in the thermal decomposition temperature. Basic magnetic characteristics such as saturation magnetization (M _S) and coercive field (H _C) are evaluated by sample vibrating magnetometry at room temperature (20°C). The samples show soft ferromagnetic behavior with M _S values of ∼9–55 emu/g and H _C values of ∼8–37 Oe, depending on the crystallite size and thermal decomposition temperature. The relationship between the crystallite size and the magnetic properties is presented and discussed. The cytotoxicity of synthesized LSMO nanoparticles was also evaluated with NIH 3T3 cells and the result showed that the synthesized nanoparticles were not toxic to the cells as determined from cell viability in response to the liquid extraction of LSMO nanoparticles.     

CoFe2O4 nanocrystalline powders prepared by citrate-gel methods: Synthesis, structure and magnetic properties

Nanocrystalline CoFe₂O₄ powders were prepared by decomposition of metal ion citrate precursors. Four samples were synthesized from precursor solutions having different pH values in the range <1–7.0. The powders were characterized by X-ray Diffraction, Thermogravimetry, Differential Thermal Analysis, N₂ physisorption and Transmission Electron Microscopy. Magnetic properties were explored by a SQUID magnetometer. Three out of the four samples, coming from solutions of pH 2, 4 and 7, were produced by an autocombustion reaction and are very similar as regards average size of the nanoparticles (about 20 nm), their morphology and the magnetic properties, while the fourth sample was produced by a slower thermal decomposition and is composed of smaller nanoparticles (about 10 nm).     

Sonochemical synthesis and characterization of new seven coordinated zinc,cadmium and mercury nitrate complexes: New precursors for nanostructure metal oxides

The nitrate complexes of group 12 elements with a tridentate Schiff base ligand (L = (E)-N1-((E)-3- phenylallylidene)-N2-(2-((E)-((E)-3-phenylallylidene) amino)ethyl) ethane-1,2-diamine) were synthesized via sonochemical process and characterized by various physical and chemical methods. The structural analysis of the zinc nitrate complex by single crystal X-ray diffraction analysis shows that the central atom is seven-coordinated by three nitrogen atoms from the Schiff base ligand as well as four oxygen atoms from two different nitrate anions. The geometry around the metal center can be described as a distorted pentagonal bipyramid. The crystal packing analysis of zinc nitrate complex indicates that the intermolecular interactions related to nitrate groups plays the essential role in the orientation of supramolecular structure. Hirshfeld surfaces (HS) and their corresponding fingerprint plots (FP) have been also used for further investigation of crystal structure of zinc nitrate complex. Furthermore thermal analyses (TG/DTG) of three nanostructure complexes were carried out and discussed. Finally, direct thermolysis of zinc and cadmium nitrate complexes in air atmosphere led to the production of zinc and cadmium oxide nanoparticles.