A device for measuring the concentration and dispersion quality ofmagnetic particle suspensions

A technique, called rheomagnetic measurement, for studying the concentration and orientation of magnetic particles through inductance measurement is presented. The particles are oriented in a predominantly extensional flow field, and, because they are magnetic, their orientation can be detected with a weak magnetic sensing field. Because flocs of magnetic particles orient differently in a flow field than primary particles do, this method can be useful in obtaining information about the particle flocculation aspect of dispersion quality. A magnetic sensing field can also be used to detect the particle concentration in a quiescent flow. Experimental data on the effects of particle concentration and milling for rod-like γ-Fe₂O₃ and plate-like Ba-ferrite suspensions are discussed. The results for Ba-ferrite magnetic markedly contrast with those for the rod-like magnetic particles but showed similarity with those for rod-like γ-Fe₂O₃     

High performances boron doped γ-Fe2O3particles prepared from oxalic precursors

γ-Fe₂O₃ particles (L≈0.15 to 0.2 μm, L/D≈2 to 5) with coercivity up to 400 Oe have been prepared from oxalic precursors. To preserve the particle form, the oxalates were doped with boron. The effects due to this element was studied during the different thermal treatments which effect the pseudomorphous transformation of oxalate particles into spinel ferrite. ESCA spectroscopy, and X-ray measurements could point out the presence of a Fe₃BO₅ phase at the surface of γ-Fe₂O₃ particles. In spite of the important mass losses (H₂O, CO, CO₂) and the important crystallographic structure modifications occurring during the transformation of oxalate into magnetic oxide, γ-Fe₂O ₃ particles obtained by this method have very good textural characteristics. Boron-doped γ-Fe₂O₃ particles were used to make 3.5-in diskettes with standard formulation. In these conditions, media properties were comparable to trading diskettes properties     

Effect of polymer adsorbed layer on magnetic particle dispersion

Experimental and theoretical investigations of dispersion properties of magnetic particles (acicular γ-Fe₂O₃ ) with an adsorbed epoxy-resin layer are presented. The adsorbed polymer amount was 20-110 mg/g and the adsorbed layer thickness was 6-22 nm, depending on the preparation conditions. Dispersion of γ-Fe ₂O₃ particles was evaluated by the sedimentation rate and surface roughness of the coated film. It was clarified that dispersion was improved with increasing adsorption, increasing solvent/epoxy-resin solubility, and decreasing γ-Fe₂O ₃ particle size. Interaction energy, consisting of magnetic attraction, van der Waals attraction, and steric repulsion of the adsorbed layer between two cylindrical magnetic particles, was calculated. The interaction energy curves, which vary with the distance between two particles, had primary minimum, maximum, and secondary minimum. The maximum energy and the secondary minimum energy were strongly related to dispersion stability. Experimental results are explained by the energy curve shapes     

CoFe2与CoFe2O4质量比及MgO稀释对CoFe2@CoFe2O4磁性的影响

采用金属有机盐热分解方法制备了MgO包覆的CoFe₂O₄纳米粒子（CoFe₂O₄@MgO）,然后将CoFe₂O₄@MgO在H₂中还原,接着在空气中氧化制备了一组CoFe₂@CoFe₂O₄@MgO样品;用盐酸溶液溶解CoFe₂@CoFe₂O₄@MgO中的MgO获得另一组样品（CoFe₂@CoF₂O₄）。测量并绘制了CoFe₂@CoFe₂O₄@MgO和CoFe₂@CoF₂O₄的磁化强度随外磁场及温度变化的关系曲线。随着氧化温度升高,CoFe₂@CoFe₂O₄@MgO和CoFe₂@CoF₂O₄的矫顽力H_c、饱和磁化强度M_s、剩磁比M_r/M_s及磁有序状态发生显著变化,这些变化强烈依赖于磁性粒子的各向异性及粒子间的偶极相互作用。     

Thermomagnetic study of surface cobalt modified iron oxideparticles derived from oxalic precursors

The cobalt modification of pure γ-Fe₂O₃ acicular particles by the so-called epitaxial process has been applied to γ-Fe₂O₃ particles, derived from oxalic precursors. Six elaboration parameters have been taken into account for the slurry heat treatment: cable content, pH, time, temperature, gas flowing into the solution, and surface activation. A thermomagnetic study including in situ annealing treatments and magnetic measurements at various temperatures in the range 20-380°C has been carried out. The results are compared with those of commercial surface-cobalt-modified pigments     

二次化学共沉淀法制备片状钡铁氧体的形成历程及磁性能研究

采用二次化学共沉淀法制备出六角或近六角片状BaFe₁₂O₁₉,其颗粒径向尺寸和径厚比分别为0.4-2μm和4-20。通过XRD、FTIR、TG/DTA及SEM/EDS分析技术研究了片状BaFe₁₂O₁₉的形成历程。结果表明:前驱体为非晶态BaCO₃、低结晶态Fe（OH）₃和晶态α-Fe₂O₃包覆原料BaFe₁₂O₁₉复合物;前驱体在焙烧过程中经过Fe（OH）₃脱水、BaCO₃分解反应、中间相α-Fe₂O₃和BaO反应得到终产物BaFe₁₂O₁₉。基于形成历程,六角片状BaFe₁₂O₁₉较原料BaFe₁₂O₁₉表现出显著提高的颗粒径向尺寸和径厚比、较高的纯度和略低的结晶有序程度,进而表现出明显提高的矫顽力、略低的饱和磁化强度和剩余磁化强度。     

Calorimetric characterization of magnetic pigment surfaces

One of the most direct and sensitive ways of studying pigment surface properties is to measure the enthalpy changes which accompany the immersion of pigments in liquids. Different wetting liquids were used to test for H donor and H acceptor properties as well as to probe the polarity of the pigments' surfaces. The measurements were performed in an isoperibol batch calorimeter. Results are presented for γ-Fe ₂O₃, CrO₂, Co-modified γ-Fe₂ O₃, and barium ferrite pigments. It is found that Co-modified γ-Fe₂O₃ pigments are very polar, whereas CrO₂ pigments have low polarities: H donor and H acceptor properties are less pronounced. It is found that barium ferrite pigments act very much like γ-Fe₂O₃ pigments. It is shown that the effects of surface treatment can clearly be monitored by calorimetry     

不同晶型Fe2O3催化H2O2湿法脱硝的实验研究

研究了以α-Fe₂O₃、β-Fe₂O₃和γ-Fe₂O₃为催化剂的类Fenton试剂溶液氧化吸收NO的过程,分析了3种Fe₂O₃的晶相结构和表面性质对NO脱除效率的影响机理。脱硝性能测试结果表明：γ-Fe₂O₃的活性最好,在H₂O₂浓度为1.5 mol/L、催化剂浓度为20 mmol/L、pH值为5以及反应温度为55℃等条件下,γ-Fe₂O₃的脱硝率可达87.5%。机理研究表明：3种Fe₂O₃催化H₂O₂分解湿法脱除NO的反应发生在催化剂表面,反应过程中存在氧化还原循环,H₂O₂催化分解的主要产物是·OH。活性差异分析结果表明：Fe₂O₃的晶相结构和表面性质对NO的脱除效果具有显著的影响,γ-Fe₂O₃的活性最高是由于比表面积大、分散性高和表面的Fe²⁺含量更多,而β-Fe₂O₃的活性高于α-Fe₂O₃是由于表面的氧空位含量更多。     

Magnetic properties of acicular BaFe12O19particles prepared by microwave plasma sintering

Acicular α-FeOOH particles coated with barium ions were irradiated with microwaves under an oxygen pressure of 20 torr to prepare fine BaFe₁₂O₁₉ particles by a plasma reaction. The fine acicular particles has an aspect ratio of about 13 and a magnetization of 43.5 emu/g and contained small amounts of α-Fe₂O₃ and BaFe₂O₄. The particles were mixed with a binder, and the resulting mixture was formed into a coating under a magnetic field of 7 kOe applied vertically to the surface of the film. The squareness ratio in the direction perpendicular to the surface of the coating film was 0.83 without any correction for the demagnetizing field. Transmission electron microscopy (TEM) showed that the long axes of the BaFe₁₂O₁₉ particles all were aligned parallel to the film base. The cross-sections of the particles were rectangular when observed by TEM. It follows that the easy axes of the particles are perpendicular to their long axes     

-Fe2O3 thin films prepared by metalorganic deposition (MOD) from Fe(III) 2-ethylhexanoate

-Fe₂O₃ thin films were prepared by metalorganic deposition (MOD) using Fe(III) 2-ethylhexanoate as the metalorganic precursor. A series of experiments were conducted on the metalorganic spin-coated films and their correspondingly annealed samples by employing experimental techniques ranging from thermal gravimetric analysis, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscopy (SEM) to optical property characterization. In this way a better understanding has been achieved regarding the decomposition process of the metalorganic precursor, the solid state -Fe₂O₃ film formation and crystallization process, and the relationship between the structure and the optical properties of the prepared films. The conclusions of our experiments are the following. The decomposition of Fe(III) 2-ethylhexanoate is a multistep process that is characterized by distinct transition temperatures and thermogravimetric loss rates. Amorphous -Fe₂O₃ film is formed at an annealing temperature of around 460°C, further annealing at higher temperatures induces the amorphous-to-crystalline phase transition and grain growth. FTIR, XRD and SEM data for structural characterization are correlated and in good agreement. A new FTIR absorption band, peaking at 1085 cm^-1, is assigned to the vibration of crystalline Fe-O mode, therefore this peak is useful in monitoring the amorphous-to-crystalline phase transition of -Fe₂O₃ material. Instead of columnar structure in physical vapour deposition-prepared films a granular structure is typical of MOD prepared films, the grain size is much larger near the surface of the film than near the substrate. Optical characterization shows that the refractive index and extinction coefficient of the -Fe₂O₃ thin films increase with the increase of annealing temperatures. The potential interesting applications of the MOD-prepared -Fe₂O₃ thin films include gas sensor materials, photoelectrodes and storage media.     

带状γ-Fe2O3/ZnO异质结光催化剂光催化降解四环素

针对传统ZnO光催化活性不高的问题,采用Zn(CH₃COO)₂和FeCl₃作为ZnO和Fe₂O₃的前驱体,水热条件下采用“一锅法”制备带状γ-Fe₂O₃/ZnO异质结光催化剂,采用XRD、BET比表面积测量仪、TEM、紫外-可见漫反射、电子顺磁共振(EPR)等对其晶体化学结构进行表征。在可见光光源下,探究了不同γ-Fe₂O₃负载量时γ-Fe₂O₃/ZnO异质结光催化剂对四环素的光催化降解的效果。研究表明,ZnO负载γ-Fe₂O₃后比表面积和光照吸收显著改善,禁带宽度有所减小,可见光光照120 min,n(Zn)∶n(Fe) (原子比)为20∶1的γ-Fe₂O₃/ZnO异质结光催化剂对四环素的降解率高达97.2%,多次重复使用后四环素的降解率保持在95%以上。      

Hydrothermal processings to produce magnetic particulates

α-Fe₂O₃, γ-Fe₂O₃ , and α-FeOOH powders were used as starting materials to prepare barium hexaferrite hydrothermally. Since strontium hexaferrite and lanthanum-doped calcium hexaferrite have coercivities similar to that of barium ferrite, the hydrothermal synthesis of strontium hexaferrite and lanthanum-doped calcium hexaferrite were also explored. The reaction products obtained with the various starting materials are described. Electron micrographs showed that α-Fe₂O₃, γ-Fe₂O₃, or α-FeOOH dissolved in the solution first, and then barium hexaferrite nucleated and grew from the solution     

Si3N4/FePd/Si3N4薄膜的晶体结构和磁性能研究

采用磁控溅射的方法制备了Si₃N₄/FePd/Si₃N₄三层膜, 研究了非磁性材料Si₃N₄作为插入层对磁记录FePd薄膜结构与磁性能的影响。结果表明, 热处理后Si₃N₄分布在FePd纳米颗粒之间, 抑制了FePd晶粒的生长, 与纯FePd薄膜相比, Si₃N₄/FePd/Si₃N₄薄膜的颗粒明显得到细化; 通过添加Si₃N₄层, FePd薄膜的晶体学参数c/a从0.960减小到0.946, 表明Si₃N₄可以有效促进FePd薄膜的有序化进程, 同时提升了矫顽力和剩磁比, 分别提高到249 kA/m、0.86; 随着600℃退火时间的进一步延长, 添加Si₃N₄的薄膜磁性没有迅速下降, 在较宽的热处理时间范围内磁性能保持在比较高的水平, 提高了抗热影响的能力。Si₃N₄作为插入层对FePd薄膜的磁性能具有较大的提升作用, 这对磁记录薄膜的发展具有重要意义。     

Development of high-quality ceramic powders for Sr0.9Ca0.1Zn2-W type hexagonal ferrite for permanentmagnet devices

Fine ceramic powders of Sr_0.9Ca_0.1Zn₂ Fe₁₆O₂₇ (Sr_0.9Ca_0.1Zn ₂-W) ferrite, of almost single domain grain size ~1 μm, have been synthesized successfully by sintering for a few hours a mixture of SrCO₃, CaCO₃, ZnO, and α-Fe₂ O₃ in stoichiometric amounts at an effectively low temperature (T_s) of ~1100°C. Carbon dioxide evolves in the reaction Sr(Ca)CO₃+2ZnO+8 α-Fe₂D₃ &lrarr2;Sr(Ca)Zn₂Fe₁₆O₂+C₂ , making fine pores in the sample, which prevent large grain growth of the material and result in a very loose powder. The small ⩽10% substitution of Sr by Ca activates the reaction, but preserves the crystallization of the small-sized grains. This yields magnetic properties useful for most permanent magnet applications, with a promisingly high coercivity H_c~3650 Oe and saturation magnetization M_s~65 emu/g. A considerably better saturation magnetization M_s~85 emu/g can be obtained by sintering the samples at higher T_s~1300°C, but that results in a rather very low coercivity H_c~105 Oe     

Recording Resolution and Writability for (Co-Pt)-SiO2/Co-SiO 2 Hard/Soft-Stacked Granular Perpendicular Media

The magnetic properties and recording performance of hard/soft stacked media consisting of a magnetically hard 9-nm-thick (Co-Pt)-SiO ₂ layer underneath a thin (2-3 nm) soft granular layer were studied. Experimental results indicated that an increase in the mean value of saturation magnetization of the soft layer langM_s ^softrang was very effective at improving the recording resolution D₅₀ due to an increase in the slope of magnetization curve alpha. The use of a Co-SiO₂ layer, which has the highest langM_s ^softrang in the present study, resulted in the highest D₅₀ value. It is likely that the increase in alpha was mainly caused by the demagnetization field in grains due to the difference between langM _s ^softrang and the mean value of saturation magnetization of the hard layer, langM_s ^hardrang. Moreover, it was successfully demonstrated that the magnetization reversal of (Co-Pt)-SiO₂/Co-SiO₂ stacked media changed systematically as theoretically predicted on reducing the interfacial exchange coupling by using NiFeCr-SiO₂ or Pt-SiO₂ interlayers. The reduction of remanence coercivity H_r was achieved by controlling the thickness and film composition of the interlayer, moreover, a high-langM_s ^softrang enhanced the H_r reduction. The H_r reduction improved recording writability without degrading D₅₀, the signal to medium noise ratio SN_mR and thermal stability     

Preparation and magnetic properties of barium ferrite fineparticles by the coprecipitation salt-catalysis method

The authors describe catalytic action by NaCl in the reaction between α-Fe₂O₃ and BaCO₃ and the development of a new process for manufacturing barium ferrite fine particles. Pure α-FeOOH and reagent-grade BaCO₃ are mixed and heated at temperatures from 300 to 800°C with and without NaCl. The BaCO₃ and α-Fe₂O₃ powders which are formed during heating react and change to barium ferrite at temperatures 100°C lower than NaCl than without it. A hematite defect structure is maintained up to a relatively high temperature due to the presence of the salt, which promotes the formation of barium ferrite. The manufacturing process involves mixing an aqueous solution of metallic chlorides with a mixture of NaOH and Na ₂CO₃. This alkaline coprecipitate slurry is then neutralized by HCl solution, filtered, and dried. The dried powder, containing salts produced by the reaction, is heated at 840°C. After the salts are dissolved in water, barium ferrite fine particles are obtained     

Aging effect on coercivity of iron oxide thin films

Changes in magnetic properties for Fe_3-x□_x O₄ (x: oxidation degree) thin films made by reactive sputtering and subsequent heat treatments have been examined under room temperature aging and constant temperature annealing. Aging causes variations in coercivity of insufficiently oxidized films which have a specific resistance of less than 1×10¹ Ω·cm, while the coercivity of γ-Fe₂O₃ (x=1/3) did not change. This phenomenon did not depend on additive elements or preparation method. Other magnetic properties such as saturation magnetization, residual magnetization, squareness ratio and coercive squareness, were not affected by aging for any Fe_3-x □_xO₄ composition. The activation energy for a coercivity change is 0.72-0.95 eV near room temperature for films with a specific resistance below 1×10¹ Ω·cm. It was confirmed that only the coercivity varied at 20°C, while both coercivity and the degree of oxidation changed with annealing at 100°C     

络合法制备均匀γ-Fe2O3纳米颗粒@多层石墨烯复合材料研究

采用水热反应中的金属离子络合一步制备均匀超细磁性γ-Fe₂O₃纳米颗粒@多层石墨烯复合材料, 无需对石墨烯进行氧化处理。采用超声法制备多层石墨烯作为基片, 制备方法简单, 石墨烯表面的含氧官能团少。以FeCl₂为反应物, 以DMF(N, N二甲基甲酰胺)和水混合液作为溶剂, 其中DMF能起到络合金属离子的作用。实验研究了乙酸钠、反应温度及填充度对制备产物的影响。采用X射线衍射(XRD)、X射线光电子能谱(XPS)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)对复合材料进行微结构分析, 采用振动样品磁强计(VSM)测试了复合材料的磁性能。研究结果表明: 利用亚铁离子与DMF形成的络合物与碳环的π-π吸附作用可以在多层石墨烯表面生成铁氧化物。通过控制亚铁离子的氧化速度和氧化铁的生长速度, 在多层石墨烯表面获得了尺寸小于10 nm的均匀γ-Fe₂O₃纳米颗粒, 复合材料具有良好的磁性能。     

Topotactic conversions of γ-FeOOH and comparative transformation methods of iron oxides in magnetic spinels

The DTA of a natural, well crystallized lepidocrocite sample containing small amounts of goethite, quartz and manganese shows that the conversion of γ-FeOOH to -Fe₂O₃ (through the γ-Fe₂O₃ metastable phase) occurs at 440°C, whereas in pure, synthetic γ-FeOOH the exothermic peak appears at ˜ 500°. Quartz (1.4% SiO₂) is not affected, nor does it hamper the transformation of FeOOH into magnetic spinels, when the sample is reacted with glycerol at reflux temperature followed by hydrolysis of the resulting solid (iron alkoxide) by boiling H₂O. Starting γ-FeOOH and final solid products are characterized by XRD and IR spectroscopy. This reaction is also discussed comparatively with the solid state transformations of iron oxides into magnetic materials by a combination of heating and grinding-pressing cycles of disks containing alkali halides as diluting agents.     

模板法制备多孔核/壳结构的Fe2O3/Al纳米铝热薄膜

通过聚苯乙烯(PS)胶晶球模板法制备出三维有序大孔(3DOM)α-Fe₂O₃薄膜骨架, 再利用磁控溅射将Al沉积到3DOM α-Fe₂O₃骨架上得到核/壳结构的Fe₂O₃/Al纳米铝热复合薄膜。扫描电镜(SEM)测试结果表明: 纳米Al均匀地附着在α-Fe₂O₃骨架表面, 骨架孔结构由原先的近圆形转变为Al沉积后的类菱形, 孔壁的厚度从32 nm增加到100 nm; 采用X射线能谱(EDS)对Fe₂O₃/Al纳米铝热薄膜的元素含量进行了分析; 由差示扫描量热法(DSC)分析显示铝热薄膜在490℃开始反应, 经历固-固和固-液两个反应阶段, 总放热量达到1374.7 J/g; 使用激光点火器对铝热薄膜进行点火, 薄膜飞溅出火花并伴有明亮刺眼的亮光, 整个发火时间达2.6 ms, 显示其能被点火并发生自蔓延反应, 可作为一种理想的点火材料。