掺杂对棒状纳米SrFe_(12)O_(19)形貌和性能的影响

以FeCl2为原料,利用化学沉淀法制备了针状纳米α-FeOOH中间体,并通过柠檬酸法在针状纳米α-FeOOH表面包裹锶的柠檬酸配合物,煅烧后形成的棒状纳米SrFe12O19并分别在共沉淀和溶胶-凝胶2个不同过程中对纳米SrFe12O19进行镧掺杂。采用XRD,TEM和振动样品磁强计(VSM)对SrFe12O19及掺杂锶铁氧体的结构、形貌及磁性能进行了表征。结果表明:沉淀法和柠檬酸法相结合后制得的针状前驱体于900℃煅烧后可制得平均直径为40nm,长径比为15～20的棒状纳米SrFe12O19。在沉淀过程中对前驱体进行掺杂后制得的SrLaxFe12-xO19较同温度时在溶胶-凝胶过程中进行掺杂制得样品的长径比有所增加,进而使得SrLaxFe12-xO19的各向异性变大,磁性能增加,且在沉淀过程中掺杂镧后,样品的矫顽力和饱和磁化强度达到最大值时,x值明显大于溶胶-凝胶过程中进行掺杂制得的棒状SrLaxFe12-xO19。利用共沉淀法掺杂后,当x=0.15时制备的样品的矫顽力最大为6179.1Oe,此时样品的饱和磁化强度和剩余磁化强度分别65.7和38.4emu·g-1。当x=0.2时制备的样品的饱和磁化强度达到最大值为67.3emu·g-1,样品的矫顽力为5852.7Oe。     

钡铁氧体微管的制备及镧掺杂对其性能的影响

以Ba(NO₃)₂和Fe(NO₃)₃为原料与不同比例的柠檬酸在水溶液中形成溶胶,把溶胶滴于脱脂棉模板上,水分挥发后在脱脂棉表面形成凝胶,于马弗炉中850 ℃煅烧2 h后制得了BaFe₁₂O₁₉微管,并在最佳柠檬酸用量时对BaFe₁₂O₁₉微管进行掺杂制得了BaLa_xFe_12-xO₁₉(x=0～0.3)微管。利用X射线衍射(XRD)﹑扫描电子显微镜(SEM)﹑透射电子显微镜(TEM)对样品的物相﹑形貌和粒径进行表征,并利用振荡样品磁强计(VSM)对样品进行磁性能研究。结果表明：借助脱脂棉模板,采用溶胶凝胶法制备了外径在8～13 μm之间,壁厚在0.5～2 μm之间的BaFe₁₂O₁₉微管,柠檬酸的加入使得微管出现破裂,随着柠檬酸用量的增加,BaFe₁₂O₁₉微管的矫顽力和饱和磁化强度先提高后下降,随着La掺入量的增加BaFe₁₂O₁₉微管的矫顽力、饱和磁化强度以及剩余磁化强度都先增加后减小,但饱和磁化强度和剩余磁化强度的最大值滞后于矫顽力的最大值,当柠檬酸与金属离子的物质的量之比为1∶1,x为0.05时850 ℃煅烧后制得了矫顽力、饱和磁化强度和剩余磁化强度分别为6 153.6 Oe,61.1和36.1 emu·g^-1的BaLa_xFe_12-xO₁₉微管。并就柠檬酸和La掺杂对微管的形成和磁性能的影响原理做了系统的研究。     

形貌可控纳米SrFe_(12)O_(19)的制备及其磁性能

以FeCl3为原料,NaOH作为沉淀剂,通过化学沉淀法,制备出球状的Fe(OH)3中间体,同时以FeCl2为原料,采用化学沉淀法,分别使用NH3·H2O、Na2CO3和NaOH作为沉淀剂制得了不同形貌的中间体,利用柠檬酸法在中间体表面包裹锶的柠檬酸络合物,煅烧后分别制得了球形、纺锤体及棒状的纳米SrFe12O19.利用X射线衍射(XRD)和透射电镜(TEM)等测试手段对不同形貌的纳米SrFe12O19进行表征,并利用振动样品磁强计(VSM)对磁性能进行研究.结果表明:在用化学沉淀-柠檬酸法制备SrFe12O19的过程中,铁盐的种类以及沉淀剂的碱性对中间体的物相和SrFe12O19的形貌有着至关重要的影响.当原料为Fe3+时,制得了球形的纳米SrFe12O19;当原料为Fe2+时,利用碱性不同的沉淀剂可制得不同形貌的纳米SrFe12O19.随着沉淀剂碱性的增加,所得SrFe12O19的长径比增加,形貌各向异性增加.SrFe12O19的矫顽力(Hc)主要取决于粒子的各向异性,各向异性越大,矫顽力越大,饱和磁化强度(Ms)随着样品的各向异性的增加也有所增加,以FeCl2为原料,NaOH作为沉淀剂时制得的棒状SrFe12O19的矫顽力和饱和磁化强度最大分别为458.2kA·m-1和64.2A·m2·kg-1.     

溶胶-凝胶自燃烧合成法制备纳米锶铁氧体及红外光谱研究

采用溶胶-凝胶与自燃烧相结合的技术,制备了纳米锶铁氧体,并对不同煅烧温度及时间所得样品的红外吸收光谱进行了分析,对锶铁氧体的形成过程有了更进一步的认识,得出锶铁氧体的较佳生成条件．结果得出：经柠檬酸溶胶凝胶法制得的干凝胶粉,自燃烧后,在850℃的条件下煅烧1h,能得到单一相的SrFe12O19纳米粉末．     

针状纳米SrFe12O19的溶胶-凝胶法制备及磁性研究

采用柠檬酸-EDTA的联合络合溶胶-凝胶法制得了针状纳米锶铁氧体磁性微粒。利用XRD对样品的物相进行分析,利用TEM对样品形貌和粒径进行表征,并利用振荡样品磁强计(VSM)对样品进行了磁性能研究。结果表明,相对于柠檬酸法制备的纯锶铁氧体微粒,EDTA加入后制备的SrFe₁₂O₁₉微粒仍保持六方磁铅石型结构,但是粒径减小,形貌向一维发展,且内禀矫顽力H_c显著提高。并直接对凝胶加热,使其发生自蔓延燃烧,省去了凝胶的干燥过程,制备周期缩短1/4以上,同时自蔓延燃烧使SrFe₁₂O₁₉的内禀矫顽力提高10%左右,通过洗涤前驱体使得SrFe₁₂O₁₉纯度得到提高,进而使比剩余磁化强度和比饱和磁化强度提高20%左右,最终制得了粒径为30 nm,长径比为5∶1,内禀矫顽力、比饱和磁化强度与比剩余磁化强度分别为6 446.9 Oe、68.9 emu·g^-1和40.2 emu·g^-1的针状纳米SrFe₁₂O₁₉。     

La-Co共掺杂的M型锶铁氧体纳米纤维的制备和磁性能

以聚乙烯吡咯烷酮(PVP)和金属盐为原料,采用静电纺丝、溶胶-凝胶技术以及随后的热处理工艺,制备了La、Co共掺杂的M型锶铁氧体Sr1-xLaxFe12-xCoxO19(x=0.12)(SLFC)纳米纤维.利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和超导量子干涉仪(SQUID)技术对纳米纤维样品的结构、形貌和磁学性能进行了观测,系统地研究了不同温度下样品的磁性能变化.结果表明:经过950°C焙烧2h后,得到纯相的M型锶铁氧体纳米纤维,纤维呈竹节状结构,直径约55nm;室温下测得矫顽力(Hc)为498.53kA·m-1,饱和磁化强度(Ms)为70.76A·m2·kg-1,剩磁(Mr)为36.35A·m2·kg-1,这比未掺杂SrFe12O19(SF)时纳米纤维的磁性能有明显的改善,并且与在相同温度下制得的相应纳米粉体样品相比,磁性能明显提高.     

Sm3+含量对BaSmxFe12-xO19 (x≤0.4)铁氧体纳米纤维结构和磁性能的影响

以金属盐和柠檬酸为原料,采用溶胶-凝胶法制备直径在1μm以内的BaSmxFe12-xO19(x≤0.4)铁氧体纳米纤维。采用FTIR、SEM、EDS、XRD和VSM对BaSmxFe12-xO19(x≤0.4)铁氧体纳米纤维进行表征。结果表明,经950℃烧结后,BaSmxFe12-xO19(x≤0.4)铁氧体已成相,且其微观结构和磁性能受掺杂离子浓度的影响。随着Sm3+含量的增加,饱和磁化强度呈先减小后增大的趋势,而矫顽力随Sm3+含量增加而逐渐增大,由x=0时的348.8 kA.m-1增大到x=0.4时的427.5 kA.m-1。与之相对应,在液氮(77 K)条件下,纤维的饱和磁化强度有显著的提高,而矫顽力则明显下降,这主要是由于纳米晶的表面自旋提高造成的。     

微球形氧化铝的制备及其表征研究

采用油柱成型法制备了一种核壳结构磁性氧化铝球,结果表明以球状Fe3O4为磁核合成的Fe3O4/Si O2/γ-Al2O3磁性球在500°C煅烧下,表面光滑,粒径分布为100~300μm,比表面积为200m2/g,平均孔径为16.8nm,孔容为0.77cm3/g,比饱和磁化强度较高(15.1emu/g),矫顽力和剩磁较低。     

热处理条件对BaSm0.3Fe11.7O19铁氧体纤维结构演化和磁性能的影响

以金属盐和柠檬酸为原料,采用溶胶凝胶法成功制备1μm以下具有较大长径比的纳米晶BaSm0.3Fe11.7O19 铁氧体纤维。采用热重-差热分析(TG-DSC)、X射线衍射仪(XRD)、场发射扫描电镜(FE-SEM)和振动样品磁强计(VSM)对前躯体纤维及其焙烧产物进行了表征。实验结果表明,750℃焙烧1小时,BaSm0.3Fe11.7O19铁氧体相已基本形成,随着焙烧温度的升高和保温时间的延长,BaSm0.3Fe11.7O19晶粒尺寸逐渐增大,纤维表面越发粗糙,片状结构越发明显。同时,纤维的饱和磁化强度(Ms)随晶粒尺寸的增加而增大,而矫顽力(Hc)则呈现先增大后减小的趋势,在晶粒尺寸为58.4 nm附近达到最大值459.2 kA/m,这表明Sm0.3Fe11.7O19纤维的临界单畴尺寸在60nm左右。对低温(77K)和室温(300K)样品的磁性能比较发现,磁性能存在明显的差异,这主要与纳米晶的表面自旋有关。     

双锥状纳米晶TiO2微管的制备及其光催化性能

本文采用模板法与溶胶-凝胶法结合,以脱脂棉为模板制备出了TiO2中空微管光催化材料.利用红外光谱(FTIR)、扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)对其在不同煅烧温度下产物的表面形貌及晶型进行了表征.以甲基橙的脱色降解为模式反应,考察了宏观形貌及煅烧温度对TiO2光催化性能的影响.结果表明:以脱脂棉为模板制得的TiO2中空微管直径3～8μm、壁厚0.5～1μm,TiO2晶体直径为30～80 nm,长径比约为5:1,呈双锥状结构,微管样品在酸性条件下30min内对甲基橙催化降解效率提高了约16%～40%.     

Structure and magnetic properties of CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> ferrites synthesized by sol–gel and microwave calcination

CoFe₂O₄ ferrites were synthesized sol–gel with cobalt chloride, ferric chloride and citric acid as the main raw material. X-ray diffraction, vibrating sample magnetometer and simultaneous thermal analysis were applied to character the structure and magnetic properties of traditional and microwave calcined samples. The samples with pH 5 and molar ratio of citric acid to metal nitrate 1–1.2 showed the optimal structure and magnetic properties. Microwave calcination reduces the synthesis time from 2 h for conventional calcination to 15–30 min. The saturation magnetization (σ _s ) for sample microwave-calcined at 550 °C for 30 min reaches to 75.89 emu/g, much higher than that of conventional-calcined samples.     

Nanocrystalline SrCexFe12?xO19 (x?=?0.00, 0.02, 0.04, 0.06, 0.08) microfibers by sol–gel method

The SrCe_xFe_12?xO₁₉ (x????0.08) ferrite microfibers were prepared via sol?Cgel method from starting reagents of metal nitrate salts and citric acid. The obtained microfibers were characterized by TG-DSC, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). The XRD patterns show that the main phase is M-type strontium hexaferrite without other impurity phases when calcined at 750?°C for 1?h, and the Ce³⁺ ions doping has not resulted in crystal structural changes of the Sr ferrite magnetoplumbite type structure. The SEM and TEM images indicate that samples with different calcination temperature and various values of x possess the diameters of below 10???m and homogeneous hexagonal plate-like morphology. The VSM results show that saturation magnetization (Ms) gradually increases with increase of calcination temperature while decreases with increase of addition of Ce³⁺ ions, and coercive force (Hc) reveals an increase at first and then decreases with increase of calcination temperature and Ce³⁺ ions content.     

溶剂热法合成花朵状钴磁性粉体及表征

采用一种简单的溶剂热法成功的合成了花朵状的钴磁性粉体。通过X射线粉末衍射(XRD),扫描电子显微镜(SEM)等对样品进行物相与形貌的表征。结果表明样品为六排堆积(hcp)和面心立方结构(fcc)混合结构的钴单质,形貌为由很多个厚度约为50～150 nm的菱形花瓣构成的花朵状结构,每个花朵的尺寸约为2μm左右。采用振动样品磁强计(VSM)测试了样品的磁性能,测试表明样品在室温下表现出铁磁性,饱和磁化强度(Ms)为140 emu.g-1,剩磁(Mr)为9.4 emu.g-1,矫顽力(Hc)为280 Oe。     

Fabrication and properties of Mn0.5Zn0.5Fe2O4 nanofibers

Zn-doped α-FeOOH nanofiber was synthesized by coprecipitation method. Then the α-FeOOH was enwraped by the complex of the Mn²⁺ and citric acid. The morphology of α-FeOOH did not transform after the calcination process and Mn_0.5Zn_0.5Fe₂O₄ nanofiber was successfully prepared. The phase, morphology, particle diameter and the magnetic properties of samples were studied by X-ray diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). The results indicated that Mn_0.5Zn_0.5Fe₂O₄ nanofibers with an aspect ratio over 40 and a diameter of 20 nm were prepared. Compared with the amorphous Mn_0.5Zn_0.5Fe₂O₄, the anisotropy of the Mn_0.5Zn_0.5Fe₂O₄ nanofiber increased, resulting in the higher coercivity and magnetization of the obtained sample. With an increase in the calcination temperature, the diameter and the saturation magnetization of the sample increased, while the aspect ratio and coercivity decreased. The coercivity of the sample obtained at 700 °C was maximal (up to 185.4 Oe). The saturation magnetization of the sample obtained at 900 °C was maximal (up to 65.3 emu/g). The use of citric acid method prevented the presence of Mn(OH)₂, resulting in the decrease of the calcination temperature.     

核壳结构磁性镁铝复合氧化物亚微米粒子的制备与表征

首先采用溶剂热法制备粒径均匀分散性良好的Fe3O4亚微米粒子,在对其包覆上一层碳膜进行表面修饰后,采用共沉淀法将硝酸根插层LDHs包覆到磁性粒子的表面,然后500℃焙烧2 h得到磁性镁铝复合氧化物亚微米粒子。这种磁性镁铝复合氧化物亚微米粒子具有以镁铝复合氧化物为壳层,Fe3O4为核的核壳结构,其中壳层厚度为20 nm左右,对其进行二次包覆后壳层厚度可达到50 nm左右,并可以方便的通过重复包覆焙烧过程进行调节,从而实现磁性镁铝复合氧化物亚微米粒子的控制制备。同时,磁性镁铝复合氧化物亚微米粒子具有较强的磁性,其比饱和磁化强度为23.3 emu·g-1,对其进行二次包覆并焙烧后为20.1 emu·g-1。     

Self-assembly of Fe3O4 nanocrystal-clusters into cauliflower-like architectures: Synthesis and characterization

Large-scale cauliflower-like Fe₃O₄ architectures consist of well-assembled magnetite nanocrystal clusters have been synthesized by a simple solvothermal process. The as-synthesized Fe₃O₄ samples were characterized by XRD, XPS, FT-IR, SEM, TEM, etc. The results show that the samples exhibit cauliflower-like hierarchical microstructures. The influences of synthesis parameters on the morphology of the samples were experimentally investigated. Magnetic properties of the Fe₃O₄ cauliflower-like hierarchical microstructures have been detected by VSM at room temperature, showing a relatively low saturation magnetization of 65 emu/g and an enhanced coercive force of 247 Oe.     

Facile method for synthesis of hollow porous magnetic microspheres with controllable structure

Hollow porous magnetic microspheres with strong magnetization and controllable structure were prepared via a facile electrostatic self-assembly of the positively charged Fe(3)O(4) nanoparticles onto the surface of the negatively charged poly(N,N'-methylenebisacrylamide-co-methacrylic acid) (P(MBAAm-co-MAA)) microspheres with subsequent removal of the polymer core through calcination at high temperature. The shell thickness was facilely tuned through the ratio between Fe(3)O(4) and polymer, and the void space was conveniently changed through the size of polymer microspheres. The hollow magnetic microspheres possessed high saturation magnetization value (51.38 emu/g) and porous structure with high specific surface area (108.04 m(2)/g). Based on these properties, the drug loading and release behaviors were investigated, which indicated that the hollow magnetic microspheres exhibited a controlled release process.     

Combined laser and magnetic field treatment of YFeO<Subscript>3</Subscript>—containing films grown by spray-pyrolysis

Thin films (50–1200 nm) of YFeO₃ were deposited on fused silica substrates by spray-pyrolysis using ethylene glycol solution of Y-Fe(III) citric complexes. The films were post deposition annealed at 750°C in static air for 2 h. Films obtained in this way were afterwards irradiated by a burst mode operated Nd-YAG laser (pulse energy 650 mJ, pulse duration 700 μs, energy density 110 mJ/cm²). The laser’s onset was synchronized with that of a magnetic field pulse of nearly square shape (magnetic induction 0.5 T, pulse duration 900 μs). The samples were placed normally to the direction of the magnetic field. The treatment does not affect the phase composition of the film but significantly increases the crystallite sizes of the phases presenting in the sample. The saturation magnetization of the films decreases as a result of the laser and magnetic field treatment and the coercive force increases by 50%.     

Synthesis of Barium Ferrite Ultrafine Particles by Coprecipitation in the Presence of Polyacrylic Acid

The barium ferrite ultrafine particles were synthesized by coprecipitation in an aqueous solution with polyacrylic acid (PAA) as a protective agent. Thermal analysis by TGA/DTA showed that the precursor could yield barium ferrite after calcination above 700 degrees C for 2 h. By analyses of the XRD and electron diffraction pattern, the formation of pure barium ferrite was confirmed and the appropriate molar ratio of Ba/Fe in aqueous solution was determined to be 1/11. The TEM measurements indicated that the average diameter of the precursor was 4.5 nm, and the diameters of the particles calcined at 700 and 800 degrees C were 23-34 and 49-82 nm, respectively. The magnetic properties characterized by a SQUID magnetometer showed that the barium ferrite ultrafine particles calcined at 700-800 degrees C had a saturation magnetization of 36.9-60.8 emu/g, a remanent magnetization of 19.0-31.0 emu/g, a coercivity of 117.3-221.8 Oe, and a squareness ratio of 0.51. The magnetization was also observed to increase with a decrease of temperature at 5-400 K. These magnetic properties all reflected the nature of ultrafine particles and also were influenced by the morphology and microstructure of final products. Copyright 2001 Academic Press.