Structure analysis and magnetic properties of nano-sized Nb(x)Ni(y)Zn1-x-yFe2O4 powders formed by combustion synthesis and mechanical milling

Nano-sized Nb(x)Ni(y)Zn1-x-yFe2O4 ferrites with average particle size of less than 100 nm were prepared by using self-propagating high-temperature synthesis and mechanical ball milling. Average ferrites size of the SHS products were less than about 100 nm after 20 minutes mechanical milling. The average combustion temperatures and the combustion propagating rates were in the ranges of 1145 to 1543 K and 4.1 to 7.2 mm/s, respectively. Rietveld refinement of the pattern converged to good agreement (chi2 = 4.87). Final product of SHS was Nb0.13Ni0.41Zn0.46Fe2O4 with Fd3m structure and the lattice parameter of 0.83623 nm. Maximum magnetization (Ms), residual magnetization (Mr), coercive force (iHc) and susceptibility of the Nb0.013Ni0.41Zn0.46Fe2O4 ferrites formed at the oxygen pressure of 0.25 MPa were 12.30 Wb/m2 Kg, 1.57 Wb/m2 Kg, 6321 A/m, and 0.02 m3/Kg, respectively. Niobium addition to nickel-zinc ferrites resulted in increasing Ms, Mr and iMc about 59%, 78% and 387%, respectively. Neutron diffractometry revealed that the variation of magnetic properties was related to non-stoichiometric number and oxygen position of the niobium-nickel-zinc ferrites due to the competitive reduction reaction among niobium, nickel and zinc oxides.     

微波多元醇法制备单分散Ni1-xZnxFe2O4/MWCNTs与磁性能

以多壁碳纳米管(MWCNTs)为模板,三乙二醇(TREG)为溶剂,采用微波多元醇法制备MWC-NTs负载组成可控的Ni1-xZnxFe2O4(x=0.4、0.5、0.6)纳米复合材料Ni1-xZnxFe2O4/MWCNTs。其结构和形貌通过XRD、SEM、TEM和EDX进行表征,用VSM测试样品的磁性,并探讨了微波功率、微波时间对镍锌铁氧体负载的影响。结果表明立方系尖晶石结构的单分散Ni1-xZnxFe2O4磁性纳米粒子均匀负载在碳纳米管表面,平均粒径约为6nm;其磁性能与镍锌铁氧体的组成有关,随着Zn含量的增加,饱和磁化强度(Ms)先增大后减小,当x=0.5时Ms达到最大值。矫顽力(Hc)都比较小,在室温下表现为超顺磁性。     

One-dimensional SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers and enhancement magnetic property

SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers of diameters about 100 nm with mass ratio 1:1 have been prepared by the electrospinning and calcination process. The SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrites are formed after calcined at 700 degrees C for 2 hours. The composite ferrite nanofibers are fabricated from nanosized Ni(0.5)Zn(0.5)Fe2O4 and SrFe12O19 ferrite grains with a uniform phase distribution. The ferrite grain size increases from about 11 to 36 nm for Ni(0.5)Zn(0.5)Fe12O4 and 24 to 56 nm for SrFe12O19 with the calcination temperature increasing from 700 to 1100 degrees C. With the ferrite grain size increasing, the coercivity (Hc) and remanence (Mr) for the SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers initially increase, reaching a maximum value of 118.4 kA/m and 31.5 Am2/kg at the grain size about 40 nm (SrFe12O19) and 24 nm (Ni(0.5)Zn(0.5)Fe2O4) respectively, and then show a reduction tendency with a further increase of the ferrite grain size. The specific saturation magnetization (Msh) of 63.2 Am2/kg for the SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers obtained at 900 degrees C for 2 hours locates between that for the single SrFe12O19 ferrite (48.5 Am2/kg) and the single Ni(0.5)Zn(0.5)Fe2O4 ferrite (69.3 Am2/kg). In particular, the Mr value 31.5 Am2/kg for the SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers is much higher than that for the individual SrFe12O19 (25.9 Am2/kg) and Ni(0.5)Zn(0.5)Fe2O4 ferrite (11.2 Am2/kg). These enhanced magnetic properties for the composite ferrite nanofibers can be attributed to the exchange-coupling interaction in the composite.     

自蔓延高温合成Ni-Zn铁氧体的研究

采用SHS方法合成Ni0.35Zn0.65Fe2O4铁氧体 ,取代了传统铁氧体工艺耗能、耗时的预烧环节。以XRD、SEM、阻抗分析仪等对铁氧体的微观结构、磁性能进行表征,并与传统工艺对比,获得了性能优良的铁氧体。     

Electronic structure studies of nanoferrite Cu(x)Co(1-x)Fe2O4 by X-ray absorption spectroscopy

Pure and mixed cobalt copper ferrites are of great interest due to their widespread application in electronics and medicine. We report on the electronic structure of a nanoferrite Cu(x)Co(1-x)Fe2O4 (0.0 < or = x < or = 1.0) system studied by X-ray absorption spectroscopy. These magnetic nanoferrites (average crystallite size approximately 31-43 nm) were synthesized by an auto combustion method and are characterized by high resolution X-ray diffraction and near edge X-ray absorption fine structure measurements at the O K and Co, Cu, and Fe L-edges. The O K-edge spectra suggest that there is a strong hybridization between O 2p and 3d electrons of Co, Cu and Fe cations and Fe L3,2-edge spectra indicate that Fe ions coexist in mixed valence states (Fe3+ and Fe2+) at tetrahedral and octahedral sites of the spinel structure. Copper and cobalt ions are distributed in the divalent state in octahedral sites of the spinel structure. The origin of high saturation magnetization and coercivity in cobalt-copper ferrites are explained in light of these results.     

静电纺丝法制备的Co0.6Ni0.3Cu0.1Fe2O4和Co0.6Ni0.3Zn0.1Fe2O4纳米纤维的结构及磁性能

采用静电纺丝技术制备出表面光滑、直径均匀的Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4/PVP和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4/PVP纳米纤维前驱丝,经500~900℃煅烧后得到Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维。用TG-DSC、XRD、SEM及VSM现代测试分析手段对Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的结构、形貌及磁学性能进行测试表征。结果表明:在空气气氛中经500~900℃煅烧后可得到纯尖晶石相、结晶度良好的纳米纤维或短纤维;当温度为700℃时,Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的形貌细长而光滑且直径相对均匀,大约为80nm;此时Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4纳米纤维则保有较高的剩磁比(M_r/M_s)及矫顽力,分别为0.56和1 088.87Oe。在500℃、600℃、700℃、800℃、900℃煅烧后,Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的饱和磁化强度分别比Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4纳米纤维增大了14.5%、7%、16%、10.7%、8%,而矫顽力则分别降低了38%、51%、50%、46%、46.7%。两种纳米纤维的饱和磁化强度及矫顽力存在差异,为CoNi铁氧体在电磁方面的应用提供了很好的参考。     

High-temperature thermoelectric properties of Na(Co0.91, Ni0.09)2O4 fabricated by solution combustion method for power generation

High-quality nano-sized Na(Co0.91Ni0.09)2O4 powders, i.e., 27 nm in average size, were synthesized by the solution combustion route. The magnitude of the electrical conductivity, the Seebeck coefficient, and the power factor for Na(Co0.91Ni0.09)2O4 depended strongly on the fuel used and followed the order of aspartic acid > glutamic acid > alanine > glycine. The order of the thermoelectric characteristics was consistent with that of the density of Na(Co0.91Ni0.09)2O4. The maximal power factor (1.06 x 10(-3) Wm(-1) K(-2)) was achieved for aspartic acid-processed Na(Co0.91 Ni0.09)2O4 twice-sintered at 800 degrees C. We believe that the solution combustion route was highly effective for fabricating high-efficiency thermoelectric materials.     

Thermoelectric properties of nanocrystalline Ca(3-x)Cu(x)Co4O9 (0 < or = x < or = 0.32) for power generation

We successfully synthesized nano-sized Ca(3-x)Cu(x)Co4O9 (0 < or = x < or = 0.32) powders by solution combustion process. Plate-like grains and porous structure were observed in the sintered Ca(3-x)Cu(x)Co4O9 ceramics. The sintered Ca(3-x)Cu(x)Co4O9 showed a monoclinic symmetry. The electrical conductivity of the Ca(3-x)Cu(x)Co4O9 increased with increasing temperature, indicative of a semiconducting behavior. The added Cu led to a significant increase in the electrical conductivity. The Seebeck coefficient of the Cu-added Ca(3-x)Cu(x)Co4O9 was much higher than that of the Cu-free Ca3Co4O9. The highest power factor (9.99 x 10(-4) Wm(-1)K-2) was obtained for Ca2.76Cu0.24Co4O9 at 800 degrees C.     

Synthesis of ferrites obtained from heavy metal solutions using wet method

Wet method was employed to the treatment of heavy metal-contaminated wastewater, and Zn(x)Fe(3-x)O(4), Ni(x)Fe(3-x)O(4) and Cr(x)Fe(3-x)O(4) (0Cr(3+) and the influence of the three ions on sample thermostability is Zn(2+)>Ni(2+)>Cr(3+).     

Structure, morphology and magnetic properties of Mg((x))Zn((1 - x))Fe2O4 ferrites prepared by polyol and aqueous co-precipitation methods: a low-toxicity alternative to Ni((x))Zn((1 - x))Fe2O4 ferrites

The synthesis and properties of Mg((x))Zn((1 - x))Fe(2)O(4) spinel ferrites as a low-toxicity alternative to the technologically significant Ni((x))Zn((1 - x))Fe(2)O(4) ferrites are reported. Ferrite nanoparticles have been formed through both the polyol and aqueous co-precipitation methods that can be readily adapted to industrial scale synthesis to satisfy the demand of a variety of commercial applications. The structure, morphology and magnetic properties of Mg((x))Zn((1 - x))Fe(2)O(4) were studied as a function of composition and particle size. Scanning electron microscopy images show particles synthesised by the aqueous co-precipitation method possess a broad size distribution (i.e. ～ 80-120 nm) with an average diameter of the order of 100 nm ± 20 nm and could be produced in high process yields of up to 25 g l(-1). In contrast, particles synthesised by the polyol-based co-precipitation method possess a narrower size distribution with an average diameter in the 30 nm ± 5 nm range but are limited to smaller yields of ～ 6 g l(-1). Furthermore, the polyol synthesis method was shown to control average particle size by varying the length of the glycol surfactant chain. Particles prepared by both methods are compared with respect to their phase purity, crystal structure, morphology, magnetic properties and microwave properties.     

Influence of Zn^2＋ or Cu^2＋ on Reduction and Recalcination Behavior of Fe2TiO5

Fe2O3, TiO2, CuO and ZnO powders were mixed according to the formula of （1-x）TiO2 xCuO-Fe2O3 or （1-x）TiO2 xZnO-Fe2O3 （x=0, 0.2 0.4, 0.6, 0.8, 1）, and well ball-milled with H2O for 3 h to ensure homogeneity of the powdered solids, then fired at 1200℃ for 4 h. The fired samples were reduced at 500℃ with hydrogen gas. The reduced samples were subjected to recalcination at 500℃ in CO2 atmosphere. Both of fired, reduced and calcined samples were characterized by X-ray diffraction, vibrating sample magnetometry, reflected light microscopy and scanning electron microscopy. Different phases were formed after firing of Cu^＋2 or Zn^2＋ substituted Fe2TiO5. Magnetization （Bs） of the formed phases after firing are very low corresponding to diluted magnetic semiconductors （DMS） and increases with increasing the substituted cations （Cu^＋2 or Zn^2＋）. The reduction of the fired samples enhanced the Bs values whereas the reducibility increases with increasing the Cu^＋2 or Zn^2＋ content. Samples show different tendency toward CO2 decomposition which is very important for environmental minimization for CO2.     

Preparation and Characterization of Some Ferrites from CuO-ZnO-Fe_2O_3 Mixtures

The ferrites of Cuo-ZnO-Fe2o3 solid solution series near the molar ratio of ZnxCu1-x were prepared by direct heating of their coprecipitated hydroxides using NH4OH as precipitating agent where x=0.0, 0.2, 0.5, 0.8 and 1.0. Additional amounts of Cu and Zn sulphates were added to compensate the loss during the coprecipitation of the hydroxides. The ferritized samples were characterized by chemical analysis, XRD. DTA, TGA and SEM. XRD of both Zn0.2Cu0.8Fe2O4 and Zn0.5Cu0.5 Fe2O4 that indicates the formation of a heterogeneous ferrite material of ZnFe2O4 and CuFe2O4 mixed with variable amounts of α-Fe2O3. Zn and Cu ferrites were observed only in Zn0.8Cu0.2Fe2O4.From TGA-time relation, the activation energy of the different transformation phases were calculated. It is found that, the activation energy of ZnFe2O4 is slightly equal to 3/2 of that for CuFe2O4. Dielectric measurements show that the electrical behaviour depends on the ordering and disordering of the phases.     

La掺杂纳米晶Ni-Zn铁氧体的制备及电磁性能

采用高分子凝胶法制备了Ni0.5Zn0.5LaxFe2-xO4（x=0,0.02,0.05和0.08）纳米晶铁氧体.采用X射线衍射仪（XRD）、透射电镜（TEM）和HP8510网络分析仪分别对其结构、形貌和电磁性能进行了研究.结果表明,当x=0,0.02和0.05时,所得粉体为纯立方晶系尖晶石结构.Ni0.5Zn0.5Fe2O4粉体平均粒径为70nm.随着La离子掺杂量的增加,红外光谱中550cm-1处吸收峰向高波数移动,420cm-1处吸收峰向低波数移动.La离子的掺杂对Ni-Zn铁氧体的电磁性能有一定的影响.在X波段,与Ni0.5Zn0.5Fe2O4铁氧体相比,掺杂La的Ni-Zn铁氧体的tanδm值降低,tanδε值升高.Ni0.5Zn0.5La0.02Fe1.98O4铁氧体的tanδε平均值为0.616.     

Co替代对纳米晶Ni0.4CoxZn0.6-xFe2O4结构和电磁性能的影响

采用聚丙烯酰胺凝胶法制备了尖晶石型纳米晶Ni0.4CoxZn0.6-xFe2O4(x=0、0.2、0.4),同时考察了铁氧体的电磁性能.由X射线衍射(XRD)可知,随着x的增大,Ni0.4CoxZn0.6-xFe2O4的晶格常数从0.838 4 nm减小到0.835 7 nm.透射电镜(TEM)结果表明,Ni0.4Zn0.6Fe2O4铁氧体粒子的平均直径约为20 nm.Ni0.4CoxZn0.6-xFe2O4在8.2～12.4 GHz的测试频率范围内具有介电损耗和磁损耗.在频率为9.0 GHz时,Ni0.4CoxZn0.6-xFe2O4(x=0.4)复介电常数虚部的最大值达到19.6.随着X值的增加,复数磁导率虚部的共振吸收峰向高频移动.制备的复合物可以被广泛地用于抑制电磁辐射和吸收雷达波等领域.     

晶化温度对纳米镍锌铁氧体吸波性能的影响

本文通过水热法制备纳米Ni0.6Zn0.4Fe_2O_4,研究了晶化温度对样品纯度、粒度、形貌及电磁波吸收性能的影响。结果表明:当晶化温度为160℃时,粒子形貌不规则,并未完全形成Ni0.6Zn0.4Fe_2O_4;纯相Ni0.6Zn0.4Fe_2O_4的形成温度为180℃,粒子呈类球形结构,分布均匀,平均粒径约为20~25nm;但温度高于180℃时,尖晶石结构不稳定性增加,有杂相α-Fe2O3生成,粒子明显增大,团聚严重。晶化温度180℃,晶化时间8h制得的纯相纳米Ni0.6Zn0.4Fe_2O_4吸波性能最好,损耗因子在3.5GHz处达到最大值为1.08。利用共振损耗理论对纳米镍锌铁氧体的吸波机理进行分析,通过Helmholtz方程推导出纳米镍锌铁氧体本征振动频率的计算公式。     

Effects of Cu-doping on the magnetic state of Zn(0.9-x)Fe0.1Cu(x)O

Magnetization measurements were performed on a series of Zn(0.9-x)Fe0.1Cu(x)O samples (0 < x approximately 0.1) prepared using solid state reaction and sol-gel methods. Although Cu is nonmagnetic, we found that increasing Cu content increases the saturation magnetization and enhances the hysteresis losses. Curie behavior of the susceptibility at high temperature indicates the presence of ferromagnetic exchange interaction. Moreover, we found that the exchange interaction and the molecular field coefficient are both ferromagnetic and greatly enhanced with Cu-doping; however, the Arrott-Belov-Kouvel plot did not reveal the presence of spontaneous magnetization down to 4.2 K.     

Electronic structure and magnetic properties of the Ni0.2Cd0.3Fe(2.5-x)A1(x)O4 (0 < or = x < or = 0.4) ferrite nanoparticles

The structural, magnetic, and electronic structural properties of Ni0.2Cd0.3Fe(2.5-x)Al(x)O4 ferrite nanoparticles were studied via X-ray diffraction (XRD), transmission electron microscopy (TEM), DC magnetization, and near-edge X-ray absorption fine-structure spectroscopy (NEXAFS) measurements. Nanoparticles of Ni0.2Cd0.3Fe(2.5x)Al(x)O4 (0 < or = x < or = 0.4) ferrite were synthesized using the sol-gel method. The XRD and TEM measurements showed that all the samples had a single-phase nature with a cubic structure, and had nanocrystalline behavior. From the XRD and TEM analysis, it was found that the particle size increases with Al doping. The DC magnetization measurements revealed that the blocking temperature increases with increased Al doping. It was observed that the magnetic moment decreases with Al doping, which may be due to the dilution of the sublattice by the doping of the Al ions. The NEXAFS measurements performed at room temperature indicated that Fe exists in a mixed-valence state.     

气泡液膜法-水热反应制备纳米Ni_(0.6)Zn_(0.4)Fe_2O_4铁氧体

采用气泡液膜法,将Zn2+,Ni2+和Fe3+与OH-在液膜中进行共沉淀反应,制得了Ni0.6Zn0.4Fe2O4铁氧体的前躯体,用元素分析、EDS、TEM、FT-IR、XRD和VSM方法进行表征。结果表明,前躯体中Ni、Zn和Fe元素组成较精确地保持了原料溶液中Zn2+,Ni2+和Fe3+的配料摩尔比并纳米级均匀分布。前躯体组成是0.6Ni(OH)2.0.4Zn(OH)2.2Fe(OH)3复合物,粒径为1～3nm的球状纳米粒子。前躯体于240℃水热反应4h,制得纳米Ni0.6Zn0.4Fe2O4铁氧体,其Ms=73.669emu/g,Mr=1.1035emu/g,Hc=8.896Gs,密度d=5.554g/cm3,再于800℃烧结1h,制得固结铁氧体的Ms=82.136emu/g。     

气泡液膜法制备Ni_(0.7)Zn_(0.3)Fe_2O_4铁氧体的前驱体纳米粒子

采用新颖的气泡液膜法,将Zn2+、Ni2+和Fe3+与OH-的共沉淀反应在气泡液膜中完成,制备了Ni0.7Zn0.3Fe2O4铁氧体前驱体纳米粒子,经元素分析、FT-IR、XRD和SEM等表征。实验结果表明,前驱体较精确地保持了原料溶液中Zn2+、Ni2+和Fe3+的配料摩尔比。前驱体分别经300、400、500、600、700或800℃烧结,制得Ni0.7Zn0.3Fe2O4铁氧体,用XRD和VSM表征。结果表明,在700℃烧结制得的Ni0.7Zn0.3Fe2O4铁氧体的粒径为26.92nm,磁饱和磁化强度sσ=64.22A.m2/kg,剩余磁化强度rσ=14.25A.m2/kg,内秉矫顽力jHc=16kA/m。将这种Ni-Zn铁氧体分散到合成油中,制成耐高温磁性液体。     

Ni_(0.5)Zn_(0.5)Fe_2O_4铁氧体的制备及其电磁损耗性能

以Zn(NO3)2.6H2O、Ni(NO3)2.6H2O和Fe(NO3)3.9H2O及柠檬酸为原料,采用溶胶-凝胶法制备前驱体,在1 200℃下煅烧3 h合成ZnFe2O4和Ni0.5Zn0.5Fe2O4铁氧体粉体。利用差热分析、X射线衍射、扫描电镜、透射电镜和红外光谱等测试手段对产物进行分析和表征。结果表明:ZnFe2O4和Ni0.5Zn0.5Fe2O4属于立方晶系尖晶石结构,结晶完整,晶粒大小在100 nm左右。在0.2~1.8 GHz的频率下对产品进行了电磁损耗性能测试,发现Ni0.5Zn0.5Fe2O4具有较好的电磁损耗特性。