静电纺丝法制备磁性Fe_3O_4纳米管（英文）

利用静电纺丝法制备复合纤维前躯体,将前躯体烧结、还原后成功得到了Fe3O4纳米管。研究了电纺工艺参数(PVA浓度、电压、接收距离)对复合纤维前躯体的影响。采用XRD、SEM、TEM等手段对纳米管的物相、形貌进行表征,同时通过改变烧结工艺研究了Fe3O4纳米管的形成机理,并且研究了Fe3O4纳米管的磁性能。结果表明:纳米管均匀、连续,外径和内径分别大约为100和50 nm;Fe3O4纳米管的磁饱和强度、矫顽力和剩磁强度分别为54.2 A·m2/kg,215×79.6 A/m和12.8 A·m2/kg。     

Fabrication of Magnetic Fe3O4 Nanotubes by Electrospinning

利用静电纺丝法制备复合纤维前躯体,将前躯体烧结、还原后成功得到了Fe3O4纳米管。研究了电纺工艺参数(PVA浓度、电压、接收距离)对复合纤维前躯体的影响。采用XRD、SEM、TEM等手段对纳米管的物相、形貌进行表征,同时通过改变烧结工艺研究了Fe3O4纳米管的形成机理,并且研究了Fe3O4纳米管的磁性能。结果表明:纳米管均匀、连续,外径和内径分别大约为100和50 nm;Fe3O4纳米管的磁饱和强度、矫顽力和剩磁强度分别为54.2 A·m2/kg,215×79.6 A/m和12.8 A·m2/kg。     

纳米NixZn1-xFe2O4颗粒的制备及其磁性能

采用水热法制备了不同镍锌比的纳米NixZn1-xFe2O4粉体.采用X射线衍射、透射电镜(TEM)、振动样品磁强计(VSM)等方法对制备的样品进行了表征,物相分析结果表明,在200℃水热5 h可以得到纯的纳米NiFe2O4粉体,在200℃水热5 h制备的Ni0.5Zn0.5Fe2O4中含有γ-Fe2O3,在220℃水热5 h可以得到纯Ni0.5Zn0.5Fe2O4纳米粉体.水热温度为220℃时制备的ZnFe2O4中仍然存在γ-Fe2O3.TEM结果表明,NixZn1-xFe2O4粒子为球形,粒径为10～20nm.磁滞回线结果表明纳米NixZn1-xFe2O4具有较好的磁性能,其中Ni0.5Zn0.5Fe2O4纳米粒子具有最大的饱和磁化强度(Ms),ZnFe2O4具有最大的矫顽力(Hc)值.     

原位一步法合成Ag/Fe2O3磁性核壳纳米粒子

采用原位法在低温下一步合成Ag/Fe2O3磁性核壳纳米粒子,并采用XRD,TEM和UV光谱研究了Ag-Fe2O3核壳纳米复合材料的结构。结果表明,纳米银粒子表面被Fe2O3层包覆,Ag核的平均粒径大约为35nm,Fe2O3壳层平均厚度约为7.5nm或15nm,形成了核壳结构的电磁复合纳米粒子。在室温下,饱和磁化强度达到0.98(A·m2)·kg-1,矫顽力8.48×103A/m;Ag/Fe2O3核壳粒子的导电率达到0.62S/cm。通过此法可以比较容易的控制核和壳的尺寸以及复合粒子的单分散性,并得到较高的产率,在催化剂、医药、光电等领域有着广阔的应用前景。     

均相沉淀模板法制备纳米Y2O3空心球研究

以粒径约150 nm的碳球为模板,通过均相沉淀法制备出Y(OH)3/碳球复合微球,煅烧除去碳球模板,得到粒径约300 nm的纳米Y2O3空心球。通过傅里叶红外光谱(FT-IR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射(XRD)和热失重分析(TG)以及X射线光电子能谱(XPS)等测试手段表征复合微球和纳米Y2O3空心球的形貌和结构。结果表明:空心球由立方晶系纳米Y2O3构成,粒径约为300 nm,壳厚度约为20 nm。     

微波加热碳热还原铁酸锌的动力学及热力学

研究550-950°C下微波加热配碳还原焙烧分解铁酸锌生成ZnO和Fe3O4/FeO的工艺及机理。利用HSC热力学软件对铁酸锌分解的热力学温度进行计算,并利用碳气化控制、化学控制及扩散控制模型研究样品中铁酸锌分解的动力学行为。分析微波功率、反应温度、配碳比和时间对铁酸锌分解率的影响。结果表明：在微波加热温度750°C,C/ZnFe2O4质量比为1：3,粒径74~89μm,微波功率1.2 kW的条件下,被还原的铁酸锌样品经过浸出后,Zn的回收率可以高达97.93%。通过采用不同的动力学模型对分解动力学进行测试。结果表明：碳气化控制机制是良好的机制。碳气化反应的活化能为38.21 kJ/mol。     

MCr2O4(M=Co, Zn)纳米晶的合成及磁性

通过配合物热分解法制备MCr2O4(M=Co,Zn)纳米晶,并对其物相、表面微结构和磁性进行表征。结果表明,产物为直径40 nm左右的球形粒子,具有立方晶系尖晶石结构。磁滞回线表明,CoCr2O4在低温下表现出明显的亚铁磁性和较强的交换偏置场,矫顽力和交换偏置场分别为Hc=6.05×105A/m和He=1.93×104A/m,饱和磁化强度Ms和剩余磁化强度Mr分别为19.86和12.63 A.m2/kg,这可用CoCr2O4纳米晶的表面结构缺陷导致表面原子的磁结构自旋无序来解释。     

氨水添加方式对硅油基磁流体性能的影响

采用化学共沉淀法制备纳米Fe_3O_4磁颗粒,用油酸钠作表面活性剂对其进行表面改性,用硅油作为载液制备出硅油基磁流体。重点研究了氨水的不同添加顺序及氨水的不同添加速度对磁流体性能的影响,通过磁性能测试、观察磁流体静置后的沉降现象以及透射电镜对磁流体进行表征,结果表明先加氨水再加油酸钠制备的磁流体分散稳定性好,其饱和磁化强度为11.4(A·m~2)/kg,进一步研究了以10 mL/min速度滴加氨水再加油酸钠,得到的磁流体分散稳定性较好,其饱和磁化强度为14.3(A·m~2)/kg。     

硅油基镝铁氧体磁流体研制及表征

用化学共沉淀法制备了硅油基镝铁氧体磁流体。用TEM观测了磁粒子形貌及粒径大小;用VSM测定磁流体饱和磁化强度并绘制磁滞回线,证实了磁流体具有良好的超顺磁性;用XRD分析了镝铁氧体磁粒子为反尖晶石结构。实验表明：制备工艺条件一定,以平均粒径为13.6 nm的镝铁氧体磁粒子做基体材料,制备的硅油基磁流体具有较强的稳定性和饱和磁化强度,实验测得透光率、饱和磁化强度分别达3.4%、1328.4 Gs。     

磁性荧光复合纳米颗粒的合成、表征及应用

首先通过共价键合法制备了羧甲基壳聚糖修饰(CMCS)的Fe3O4-CMCH复合纳米颗粒,然后与谷胱甘肽修饰的Cd Te@Zn S QDs通过酰胺缩合反应连接,并在此复合纳米颗粒表面再修饰一层CMCS,最终制备出以CMCS为基质的磁性荧光复合纳米颗粒。利用XRD、TEM、SEM、FT-IR、UV-vis、VSM和荧光光谱等方法对产物性能进行了表征与分析。结果表明:磁性荧光复合微球具有良好的单分散性,平均粒径为170±5 nm;且具有良好的磁性能和发光性能,饱和磁化强度为37.25 Am2/kg;当加入CMCS的浓度为6×10-10 mol/L时,复合纳米颗粒的荧光强度最强;在模拟人体的生理环境下检测,复合纳米颗粒显示出良好的缓释性能。     

Effect of heat treatment on the magnetic properties of nanocrystalline spinel Li–Ni ferrite prepared by a simple soft chemistry route

A simple soft chemistry route was developed to synthesize nanocrystalline Li–Ni ferrite (Li_0.25Ni_0.5Fe_2.25O₄). The as-prepared ferrite samples were characterized by X-ray diffractometer (XRD), transmission electron microscope (TEM) and vibrating sample magnetometer (VSM). The effects of the annealing temperature on the particle sizes and magnetic properties of the synthesized Li–Ni ferrites were investigated. The results indicated that the ferrite samples obtained by this method had the single-phase spinel structure. Particle sizes estimated from Scherrer's formula increased with the annealing temperature. The magnetic properties of the ferrite samples showed strong dependence on the annealing temperature. The coercivity initially increased and then decreased with increasing annealing temperature whereas the saturation magnetization continuously increased.     

Synthesis and magnetic properties of CoPt nanoparticles

CoPt nanoparticles were prepared by simultaneous thermally reducing Co(CH3COO)2 and Pt(acac)2 in oleylamine with a small quantity of oleic acid. The composition of the particles was controlled by changing the amount of the reactants. Transmission electronic microscopy reveals that Co 48 Pt 52 particles with an average diameter of 8.4 nm are steadily dispersed in octane in the presence of oleylamine and oleic acid. Selected area electron diffraction indicates that the as-prepared particles have a face center cubic structure. Magnetic properties of these particles measured by a vibrate sample magnetometer yield a coercivity of 1.194×104 A·m-1 and a saturation magnetization of 5.3 emu·g-1 . After annealing at 650 ℃ for 2 h under the flowing Ar, the coercivity increases to 9.552×104 A·m-1 according to partly phase transformation from face center cubic structure to face center tetragonal structure for the nanoparticles.     

“点击”化学法聚合物包覆纳米二氧化硅的研究

目的为了提高纳米二氧化硅与树脂的相容性,采用"点击"化学法研究表面接枝聚合物。方法利用普通自由基聚合制备的聚(甲基丙烯酸甲酯-马来酸酐)和聚(甲基丙烯酸甲酯-甲基丙烯酸缩水甘油酯),分别与丙炔醇和叠氮钠反应从而在分子链上引入多个炔基和叠氮基,然后与叠氮基改性的纳米二氧化硅粒子进行"点击"化学反应实现纳米二氧化硅包覆改性,并通过热重分析、红外光谱分析以及扫描电镜进行结构表征。结果聚合物接枝到了纳米二氧化硅表面,包覆第一层聚合物后,二氧化硅分散性明显提高;包覆第二层聚合物后,分散性有所下降。结论通过在纳米二氧化硅表面包覆聚合物,可以明显提高其分散性能。     

Properties of nanocrystalline copper prepared by vacuum-warm-compaction method

Nanocrystalline Cu with average grain size of 22.8-25.3 nm was prepared by vacuum-warm-compaction method. Scanning electronic microscope, HMV-2 type microhardness tester, X-ray diffractometer, and 6157 type electrometer were used to determine the microstructure, microhardness and electrical resistivity of as-prepared nanocrystalline Cu, respectively. The results show that the microhardness of nanocrystalline Cu increases with larger pressure, longer duration of pressure or higher temperature. The highest microhardness of nanocrystalline Cu is 3.8 GPa, which is 7 times higher than that of coarse-grained copper. The electrical resistivity of as-prepared specimens is (1.2-1.4)×10-7 Ω·m at temperature 233-293 K, which is 5-6 times higher than that of the coarse-grained copper.     

均一亚微米级氧化铈抛光粉的制备

为得到均一的亚微米级二氧化铈（CeO₂）抛光粉,以六水合硝酸铈（Ce(NO₃)₃·6H₂O）为原料,以醇－水混合溶液为溶剂,采用溶剂热法合成CeO₂。改变Ce3+浓度和醇-水体积比,利用X射线衍射仪（XRD）、激光粒度分布仪、扫描电子显微镜（SEM）对CeO₂的物相组成和形貌特征进行表征,分析CeO₂粒子的形成过程。将合成的CeO₂用于6H-SiC晶片Si面的化学机械抛光（chemical mechanical polishing,CMP）,利用原子力显微镜（atomic force microscopy, AFM）和电子天平得出CeO₂的抛光性能。结果表明:Ce3+浓度为0.10 mol/L,醇－水体积比为3∶1时合成的CeO₂的形貌规则、晶粒尺寸适中且粒度分布均匀。采用其抛光后,晶片表面粗糙度R_a为0.243 nm,材料去除速率d_MRR为287 nm/h。合成的CeO₂适用于化学机械抛光。      

Synthesis of ferromagnetic nickel ferrite nanofibers via electrospinning with iron acetate as an iron precursor

We report the synthesis of nickel ferrite nanofibers via an elecrospinning technique particularly using iron (II) acetate as an iron precursor. Nanofibers of a single-phase nickel ferrite with a uniform diameter of ??90 nm were successfully synthesized by adopting a properly prepared solution and calcination condition. Individual nickel ferrite nanofibers synthesized by electrospinning were made up of nanograins of ??20 nm in diameter. In addition, the hysteresis observed in a magnetization measurement confirmed their ferromagnetism, supporting their potential use in magnetic devices. These results demonstrate that the use of iron (II) acetate as an iron precursor is another way to synthesize ferromagnetic nickel ferrite nanofibers.     

Folate-conjugated Fe3O4 nanoparticles for in vivo tumor labeling

Highly biocompatible superparamagnetic Fe₃O₄ nanoparticles were synthesized by amide of folic acid (FA) ligands and the NH₂-group onto the surface of Fe₃O₄ nanoparticles. The as-synthesized folate-conjugated Fe₃O₄ nanoparticles were characterized by X-ray diffraction diffractometer, transmission electron microscope, FT-IR spectrometer, vibrating sample magnetometer, and dynamic light scattering instrument. The in vivo labeling effect of folate-conjugated Fe₃O₄ nanoparticles on the hepatoma cells was investigated in tumor-bearing rat. The results demonstrate that the as-prepared nanoparticles have cubic structure of Fe₃O₄ with a particle size of about 8 nm and hydrated diameter of 25.7 nm at a saturation magnetization of 51 A·m²/kg. These nanoparticles possess good physiological stability, low cytotoxicity on human skin fibroblasts and negligible effect on Wistar rats at the concentration as high as 3 mg/kg body mass. The folate-conjugated Fe₃O₄ nanoparticles could be effectively mediated into the human hepatoma Bel 7402 cells through the binding of folate and folic acid receptor, enhancing the signal contrast of tumor tissue and surrounding normal tissue in MRI imaging. It is in favor of the tumor cells labeling, tracing, magnetic resonance imaging (MRI) target detection and magnetic hyperthermia.     

嵌段共聚物模板法制备CoFe2O4纳米有序点阵列

嵌段共聚物PS-b-PMMA经离心涂膜,在丙酮蒸汽熏蒸条件下发生微相分离自组装,选择性刻蚀后制备了具有有序阵列纳米孔洞的嵌段共聚物模板。然后使用溶胶凝胶法在嵌段共聚物模板上沉积CoFe2O4前驱体,通过热处理去除交联的聚苯乙烯以及使CoFe2O4结晶化,从而制备了CoFe2O4纳米点阵列。扫描电子显微镜(SEM)、振动样品磁强计(VSM)、X射线衍射仪(XRD)被用于研究嵌段共聚物模板以及CoFe2O4磁性纳米点阵列的形貌、结构与磁性能。结果显示制备的CoFe2O4纳米点阵列中的纳米点为反尖晶石型CoFe2O4相,直径15~20nm左右、点间距100nm左右。同时,VSM测试显示CoFe2O4纳米点阵列呈铁磁性,矫顽力约为1350×79.6A/m,无明显磁性各向异性。     

高密度煤油基磁性液体的制备及其性能表征

采用化学共沉淀法,通过改变Fe₃O₄纳米颗粒的生长温度、包覆环境pH、清洗、分散方式等工艺参数进行对比试验,得出Fe₃O₄纳米颗粒在生长阶段、包覆阶段、分散阶段的最佳参数条件,优化以往的制备工艺,使油酸包覆的磁性颗粒在煤油中的分散稳定性得到提高。通过XRD、TEM、VSM等对样品进行表征,并使用旋转流变仪对所制煤油基磁性液体的流变性能进行分析。结果表明,改性后的Fe₃O₄纳米颗粒平均粒径约为14nm,呈现较为规则的球形,饱和磁化强度为60 (A·m²)·kg^-1,可制备出质量分数可达60%的高密度煤油基磁性液体,与普通磁液相比,以此制备工艺得的高密度煤油基磁性液体在饱和磁化强度、抗氧化性等方面皆有较大提升,拥有更高的应用价值。     

Fabrication and magnetic force microscopy (MFM) observation of nano scale ferromagnetic nanodot arrays

A novel electron beam lithography technique was utilized to fabricate nano scale magnetic dots array with high periodicity. C₆₀ film (fullerine) was used as an electron beam sensitive resist for electron beam patterning carried out under a high accelerating voltage of 200 kV in a transmission electron microscope with a scanning mode. 50 nm sized permalloy (Py) nanodot arrays were successfully fabricated using the method followed by ion-milling. An array of Co nanodots having a size of 100×70 nm was alternatively prepared by liftoff instead of ion milling so as to prevent surface damage by ion milling. Lift-off does not yield any surface roughness, which is important for device fabrication. Magnetic force microscopy (MFM) observations were carried out on the fabricated Co nanodot arrays. A single domain state could be realized in patterned Co nanodots. MFM tip induced magnetization effects were also clearly demonstrated in the array of Co nanodots.