自燃/球磨法制备NiZn系铁氧体

以金属硝酸盐和柠檬酸为原料,用溶胶凝胶自燃烧法制备NiZn系铁氧体前驱体粉末(Ni0.4Zn0.6Fe2O4,Ni0.2Zn0.6Cu0.2Fe2O4,Ni0.33Zn0.59Cu0.11Fe1.97O4(Bi2O3)0.002和Ni0.33Zn0.59Cu0.11 Fe1.97O4(Bi2O3)0.002(MnO2)0.02),然后经30小时高能球磨,从X-ray衍射谱中发现前驱体粉末虽然基本上是尖晶石结构,但是还有一些杂相,经过球磨,杂相明显减少,结构更加完整,颗粒减小.前驱体粉末Ni0.33Zn0.59Cu0.11Fe1.97O4(Bi2O3)0.002经30小时球磨后,在空气中退火,退火温度分别为400℃,600℃,800℃,900℃,1000℃.用X-ray衍射谱分析其物相,发现在800℃退火得到单相的尖晶石结构,无杂相.该样品的最佳退火温度低于1000℃.用振动样品磁强计分别测量制备态和退火态样品粉末的磁性,可以看出,随退火温度的升高,比饱和磁化强度σs逐渐增大,矫顽力Hc逐渐减小,当900℃退火后,比饱和磁化强度已接近块状NiZn系铁氧体.1000℃退火后,上述四种样品中Ni0.4Zn0.6Fe2O4具有最高的比饱和磁化强度σs=65.09emu/g.本文为NiZn铁氧体的低温烧结提供了有用的实验数据.     

Sol-gel法制备NiZnCu铁氧体性能的研究

采用溶胶-凝胶自燃法制备了Ni0.4Zn0.4Cu0.2Fe2O4铁氧体,使用HP4191A阻抗分析仪测试了材料高频磁谱;结合快速热处理(RTP)工艺制备了Ni0.4Zn0.4Cu0.2Fe2O4磁性薄膜,使用AFM、XRD、AGM系统地研究了制备工艺对薄膜样品表面形貌、晶相结构和准静态磁性的影响。测试结果表明:Ni0.4Zn0.4Cu0.2Fe2O4可适用于射频领域,截止频率fr在1GHz以上,1GHz处起始磁导率μ′=5.3,μ″=3.45;sol-gel法制备磁性薄膜最佳晶化温度为600℃左右,在此温度下制备的薄膜晶粒大小为13nm左右,饱和磁化强度Ms=2.29×105A/m,矫顽力Hc=1.24×103A/m。     

自蔓延高温合成镍铜锌铁氧体粉体研究

采用自蔓延高温合成(SHS)工艺制备了Ni0.25Cu0.25Zn0.5Fe1.96O3.94粉体,将铁氧体粉体分别在800、850、900℃进行热处理,以XRD、SEM、TG-DSC、振动样品磁强计(VSM)等手段分别对产物的物相、微观结构和磁性能进行研究.结果表明,SHS制备的NiCuZn铁氧体粉体经900℃热处理后可以转变成单一的尖晶石相,所得铁氧体粉体结构完整,矫顽力达到最小值,Hc=5 753.417 1A/m,同时饱和磁化强度达到最大值,Ms=68.34 emu/g.     

Co含量对Zn0.6CoxFe2.4-xO4结构与磁性的影响

采用溶胶-凝胶方法制备纳米尺度钴锌铁氧体Zn0.6CoxFe2.4-xO4(x=0～0.30)颗粒,利用X射线衍射仪(XRD)分析晶体结构和相变过程,利用振动样品磁强计(VSM)对其磁性进行测量和分析.实验结果表明,钴锌铁氧体Zn0.6Co0.15Fe2.25O4在800℃时生成单一尖晶石相锌钴铁氧体,在550～800℃温度区间出现R-Fe2O3过渡相.随钴含量的增加,Zn0.6CoxFe2.4-xO4的比饱和磁化强度先增后减,x=0.075～0.15比饱和磁化强度较高;Zn0.6CoxFe2.4-xO4在1300℃时x=0.075的矫顽力为47163.6A/m,x≥0.15时矫顽力在1200℃附近随温度缓慢上升,在1200～1300℃之间为平台状态,并且随钴含量的增加,矫顽力略有升高.在x=0.10附近,可同时获得较高的比饱和磁化强度和较高的矫顽力.     

锌掺杂钴铁氧体:硬磁→软磁

采用共沉淀法制备了不同Zn2+掺杂量的Co1-xZnxFe2O4,研究了Zn2+掺杂量对其结构和磁性的影响。X射线衍射测试表明Co1-xZnxFe2O4成相良好,结晶随烧结温度增加而愈加完善。经400℃热处理2h的Co0.7Zn0.3Fe2O4晶粒尺寸由谢乐公式计算为8.57nm。利用振动样品磁强计研究其静态磁性,结果表明,Zn2+掺杂量对Co1-xZnxFe2O4磁性有显著影响,Zn2+含量越高矫顽力越低,同时饱和磁化强度越大,当x=0.3时,矫顽力仅为1352.82A/m,磁化强度为42A.m2/kg,实现了CoFe2O4从硬磁性到软磁性的转变,可作为潜在的高频软磁材料。     

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。     

(1-x)CaTiO_3/xNi_(0.5)Zn_(0.5)Fe_2O_4复合材料的制备及其性能

采用固相反应法合成了(1-x)CaTiO3/xNi0.5Zn0.5Fe2O4(0≤x≤1.0)复合材料,并研究了复合材料的物相、微观结构、介电性能和磁性能。结果表明:样品中仅含有钙钛矿型CaTiO3和尖晶石型Ni0.5Zn0.5Fe2O4。1260℃保温3h,样品相对密度达到98.91%,颗粒尺寸约为2μm。样品介电常数随Ni0.5Zn0.5Fe2O4含量(x)增加而增大。当x=0.7、测试频率为103 Hz时,样品介电常数(εr)和介电损耗(tanδ)分别为2629.18和1.74。(1-x)CaTiO3/xNi0.5Zn0.5Fe2O4复合材料显示磁性。其中x=0.7时,样品饱和磁化强度(Ms)达到49.07A·m2/kg;这归因于Ni0.5Zn0.5Fe2O4具有优异的磁性能。     

溶胶凝胶法合成镍铜锌铁氧体纳米晶磁性研究

用溶胶-凝胶制备了系列Ni0.2Cu0.2Zn0.6Fe2O4铁氧体微粉.借助于TG-DTA、XRD、SEM、VSM技术,对干凝胶的热分解过程、产物的物相、微观结构和磁性能进行研究.结果表明,Ni0.2Cu0.2Zn0.6Fe2O4铁氧体微粉经800℃烧结后可以转变成尖晶石相.磁滞回线表明,Ni0.2Cu0.2Zn0.6Fe2O4在低温和室温都出现了交换偏置场,这可以用纳米晶的表面的掺杂和结构缺陷导致表面原子的磁结构自旋无序来解释.     

化学计量比和热处理条件对钡铁氧体磁性能的影响

讨论了溶胶-凝胶法制备钡铁氧体材料的过程中,主要工艺参数,即烧结温度、烧结时间、Fe/Ba比率对产物组成及磁性能的影响.研究结果表明,增加烧结时间和烧结温度有利于提高产物的饱和磁化强度(Ms),但对矫顽力(Hci)的影响甚微;Fe/Ba比率的变化主要影响产物组成中主相BaFe12O19和杂质相BaFe2O4的比率,进而影响产物的磁性能.     

低温烧结工艺对Bi-CVG铁氧体微结构及磁性能的影响

以氧化物Y2O3、Fe2O3、Bi2O3、V2O5、CaCO3为原料,采用固相反应法制备了Y1.05Bi0.75Ca1.2Fe4.4V0.6O12(Bi-CVG)铁氧体材料。通过XRD、SEM和MATS等方法考察了不同烧结温度、保温时间对产物体积密度、晶体结构、形貌和磁性能的影响。结果表明,选择适当的保温时间可以有效提高铁氧体的密度;烧结温度对相稳定性和磁性能影响显著。当烧结条件为1100℃与6h时,所制备的Bi-CVG样品属于体心立方晶系,且粒度大小分布比较均匀,结构致密。该样品磁性能良好,平均晶粒尺寸约为2μm,密度为5.20g/cm3;主要磁特性为剩磁Br=24.57mT,矫顽力Hc=764.4A/m,饱和磁化强度4πMs=343.2×10-4T。     

燃烧合成Co（Ti）-Al2O3金属陶瓷的组织与性能

利用低放热Al-TiO2反应体系部分取代高放热Al-CoO反应体系,并加入适量的稀释剂Al2O3吸收反应热量,通过热爆燃烧合成结合致密化工艺制备了铁磁性Co(Ti)-Al2O3金属陶瓷。研究表明,Co(Ti)-Al2O3金属陶瓷中随着Al-TiO2体系的增加,燃烧反应温度降低,金属相尺寸减小,分布更均匀,同时在金属相与基体之间形成过渡区域,提高了界面结合。Co(Ti)-Al2O3复合材料的饱和磁化强度随着金属Co含量增加而增加,最高可达到37.2849Am2/kg,而矫顽力在3997.6～5615.4A/m范围内变化,介于软磁体和硬磁体之间。     

Magnetic measurements of martensitic transformation in austenitic stainless steel after room temperature rolling

In order to investigate the detection of martensite phase in deformed austenitic stainless steel, magnetic properties were examined by means of super conducting quantum interface device (SQUID) and vibrating sample magnetometer (VSM) techniques. Stainless steel specimens were rolled at room temperature with 15 to 55% reduction in thickness. Results indicate that the magnetic properties of stainless steel were sensitive to percent reduction in thickness and micro structural condition of stainless steel. It was found that saturation magnetization, amount of martensite and hardness increased whereas, coercive force and remanence ratio decreased with increasing percent reduction in thickness. The saturation magnetization depends mainly on amount of martensite, while the coercive force and remanence depends mostly on shape and distribution of martensite phase.     

Magnetic properties of Ni-Zn ferrite powders formed by self-propagating high temperature synthesis reaction

The ferrite compositions of Ni_xZn_xFe₂O₄ were synthesized by self-propagating high temperature synthesis reaction with various contents of iron, iron oxide, nickel oxide and zinc oxide at oxygen partial pressures varying between 0.05 to 5.0 MPa. The oxygen pressure promoted the combustion reaction, while the compacting pressure retarded the reaction. The rate equation of ferrite formation is shown to be v = 14.5 exp (T_c1380 - 1) P _O2 ^0.2 . Phase identification of the final products by X-ray diffraction (XRD) revealed that the enhanced combustion reaction with oxygen pressure and iron content in the reactants resulted in increasing the spinel content in the combustion product. As the oxygen pressure changed from 0.1 to 5 MPa, the coercive force and residual magnetization decreased by about 73% and 66%, respectively, whereas, the maximum magnetization, susceptibility and Curie temperature increased by about 70%, 60%, and 32%, respectively. The improved magnetic properties are accounted for by the enhanced iron oxidation at a given combustion condition. Compared to the magnetic properties and productivity of the Ni-Zn ferrites prepared by wet chemical method, the self-propagating high temperature synthesis method at high oxygen pressure is one of the useful methods to fabricate improved ferrite powders.     

Self-propagating high temperature synthesis and magnetic properties of Ni0.35Zn0.65Fe2O4 powders

Ni-Zn ferrite powders were synthesized by self-propagating high temperature synthesis (SHS) method. X-ray diffraction, TEM and vibrating sample magnetometry (VSM) were used to characterize the phase composition, microstructure and magnetic properties of the combustion products. The effect of the combustion temperature (T _c), the major parameter of the SHS process, on particle size, phase composition and magnetic properties of the products was also studied. The results showed that particle size grew with the increasing combustion temperature. The maximum saturation magnetization,M _s, increased with combustion temperature indicating the growth of grain size and high degree of ferritization, while residual magnetization,M _r, and coercive force,H _c, decreased. Compared with other methods, Ni_0.35Zn_0.65Fe₂O₄ ferrite powders with improved magnetic properties can be obtained by SHS at 1000°C.     

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.     

Influence of cerium content on the structure and magnetic behavior of Co-Fe-Cu-Ce permanent magnets

As part of a continuing program to understand and optimize the magnetic behavior of Co-Fe-Cu-Ce permanent magnet alloys, we have made studies on the alloy system Co3.5Fe0.5CuCexwith x in the range 0.8 to 1.2. An alloy of x = 1 had previously been studied in detail and found to have good permanent magnet properties. In the present work, it was found that when x > 1, the coercive force was increased while both the Curie temperature and saturation magnetization were decreased. However when x < 1, the coercive force tends to decrease while the Curie temperature and saturation magnetization increase. The increase in coercive force with increase in cerium content can be accounted for largely by the decrease in saturation magnetization. These results are in accord with a domain wall pinning mechanism. Scanning electron microscopy studies have shown that a major second phase in the low cerium alloys is low in copper as compared with the matrix. On the contrary, the copper content of the second phase in the high cerium alloys is larger than that in the matrix.     

合成条件对纳米锌铁氧体形貌与性能的影响

采用多元醇法制备ZnFe_2O_4纳米颗粒,研究回流时间、升温速率和回流温度对产物尺寸、形貌和磁性能的影响。通过X射线衍射仪(XRD),透射电子显微镜(TEM),傅里叶红外光谱和振动样品磁强计对样品的结构、形貌和磁性能进行表征。结果表明:制备的ZnFe_2O_4纳米颗粒分散性较好,尺寸较均一。随着回流时间的延长和回流温度的升高,ZnFe_2O_4颗粒粒径增大。回流温度为270℃时,制备的ZnFe_2O_4饱和磁化强度为35.09A·m~2/kg,剩磁较小,矫顽力为4.2kA/m,表现出亚铁磁性。     

Solvothermal preparation of cobalt nanorods

Cobalt nanorods have been prepared through solvothermal process with hydrazine hydrate and dimethylglyoxime (DMG) as reducing and morphology directing agents. The phase structure, morphology and magnetic properties of the as-prepared product were extensively characterized by X-ray diffraction, transmission electron microscopy and superconducting quantum interference device magnetometer. X-ray diffraction pattern revealed that the as-synthesized product was cobalt with face-centered cubic structure. Transmission electron microscopy observation showed that the as-prepared product composed of rod-like shape with size around 10 nm. The presence of DMG molecules on the surface of Co nanostructures was confirmed by the FTIR spectra. Magnetic measurements revealed that the nanorod exhibit ferromagnetic behavior at 300 K. The coercive force value of cobalt nanorods is 340 Oe at 300 K. Compared with bulk cobalt, the nanorods exhibit significant increase in coercive force as a reflection of shape anisotropy. The saturation magnetization value of Co nano rod is 150 emu/g at room temperature.     

Structural & Magnetic Characterizations of NiLiZn Nanoferrites Synthesized by Co-precipitation Method

Synthesis of Ni0.5LixZn(0.5-x)Fe2O4 nanoparticles with x=0, 0.1, 0.2, 0.3, 0.4 and 0.5 were realized via co-precipitation method. X-ray diffraction (XRD) and vibrating sample magnetometer (VSM) measurements were performed on the samples to determine the characteristics of the crystal structures and the magnetic properties of the samples, respectively. The spinel phase structures of the samples were confirmed by XRD analysis. Patterns of decreased lattice parameter and increased crystallite size values were observed by increasing the Li concentration at longer synthesis reaction periods. Similarly, for the magnetic properties, both the saturation magnetization (Ms) and coercivity (Hc) were found to vary with increasing patterns at higher Li doping levels and longer synthesis reaction periods. The results and mechanisms concerned were discussed.     

Sol–gel autocombustion synthesis of Co–Ni alloy powder

Sol–gel autocombustion is confirmed to be an efficient method in the synthesis of Co–Ni alloy powder. Addition of adequate amount of ethanol can make the reduction reaction thorough and increase the purity of the samples. X-ray diffraction measurement indicates that the obtained samples consist of a single phase with bcc structure. Transmission electron microscopy study shows the grain size is about 10 nm. The magnetic measurements show that the samples are a soft magnetic material with the coercive field smaller than 100 Oe and the saturation magnetization about 95% of the theoretical value.