球形尖晶石型钴铁氧体:合成方法及其影响因素

实现了在低温、常压条件下由含铁水滑石微晶到球形尖晶石型铁氧体的合成。结果表明,所合成的铁氧体系平均粒径为1.0μm的规整球。进一步研究发现,铁氧体微球的成型过程受到很多因素影响,例如,球型铁氧体磁性粒子的大小随着晶化过程中溶液的酸碱度的升高而变大;同时外加磁场的存在不但会使球型铁氧体磁性粒子的粒径变大,而且也会使晶化产物的粒子形貌更加趋于规整。另外,还对不同组成的尖晶石型铁氧体微球的形成进行横向比较时发现,合成初期的化合物投料组成对终产物形貌的影响是巨大的,随着投料组成中Fe2+含量的增加,转化过程变得容易,且在投料金属离子组成nCo2+∶nFe2+∶nFe3+为1∶1∶1时,所得的球型铁氧体磁性粒子的粒径最大。相同条件下不同组成的铁氧体微球粒径差异明显,MgFe2O4不能形成球形颗粒,NiFe2O4和CoFe2O4可以形成球形颗粒,其中CoFe2O4形成的颗粒粒径最大。     

空心锌铬铁氧体/二氧化钛复合物的制备及去污性能

以葡萄糖溶液为原料,通过水热法制备了分散性良好的碳微球;以碳微球为模板,应用化学沉淀法和热处理技术除去碳核获得空心铬锌铁氧体;用钛酸四丁酯作为钛源,在空心铁氧体表面包覆二氧化钛制备了锌铬铁氧体/二氧化钛二元复合物.采用现代分析技术表征了制备样品的微观结构、形貌和电磁性能,并对其吸附和降解染料废水的性能进行了研究.结果表明,Zn Cr_(0.25)Fe_(1.75)O_4对染料废水具有较好的去污效果,对甲基橙和罗丹明B的去污效率分别为87%和83%;TiO_2对铁氧体的包覆能提高复合物对染料废水的光催化降解性能,其中m_(T/ZCF)=0.3的ZnCr_(0.25)Fe_(1.75)O_4/TiO_2复合物的去污效果最佳,几乎与纯二氧化钛相仿.     

二氧化钛纳米棒在空心微球表面的定向生长

通过表面预处理和水热法开展了用二氧化钛包覆空心微球的研究, 用扫描电子显微镜(SEM)和X射线衍射仪(XRD)等表征了所得产品, 并探索了各种反应参数对产物形貌和结构的调控作用. 实验结果表明, 空心微球的表面溶胶-凝胶预处理至关重要. 采用表面溶胶-凝胶技术预处理空心微球表面, 然后在一定条件下进行水热反应, 我们在空心微球表面上成功地包覆了垂直于微球表面并紧密排列的锐钛矿型二氧化钛纳米棒. 该材料质轻、耐腐蚀, 有望成为一种新型光催化剂, 应用于治理水体表面的大面积污染.     

多孔氧化铜空心微球的一步法制备及其光催化性能

采用一步法成功制备出多孔氧化铜空心微球,用SEM、XRD和FTIR对制得的样品进行了表征。研究发现,碳源、反应温度、反应时间、CuSO4浓度等实验条件在多孔微球的制备过程中起着重要作用。在实验结果的基础上,提出了多孔氧化铜空心微球的形成机理。制备的多孔氧化铜空心微球的比表面积为409 m2.g-1,平均孔径为3.15 nm,总孔体积为0.256 cm3.g-1,这种空心微球具有量子尺寸效应并对罗丹明B有较高的光催化性能。     

纳米镍钴铁氧体空心微球的制备与性能

以乙二醇为溶剂,氯化铁、氯化钴、氯化镍和醋酸铵为反应试剂,采用溶剂热法制备纳米Ni_xCo_1-xFe₂O₄(x=0、0.3、0.5、0.7、1)铁氧体空心微球,研究镍含量对铁氧体空心球的磁性与吸波性能的影响。借助X-射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、振动样品磁强计(VSM)和网络分析仪对试样的物相组成、微观形貌和电磁特性进行表征。结果表明制备的镍钴铁氧体为尖晶石结构,且形貌为空心球,粒径在200 nm左右。当x=0时,镍钴铁氧体空心球饱和磁化强度最大为81.7 emu·g^-1,反射损耗在1 658.8 MHz有最小值为-16.9 dB。     

纳米镍钴铁氧体空心微球的制备与性能

以乙二醇为溶剂,氯化铁、氯化钴、氯化镍和醋酸铵为反应试剂,采用溶剂热法制备纳米Ni_xCo_1-xFe₂O₄(x=0、0.3、0.5、0.7、1)铁氧体空心微球,研究镍含量对铁氧体空心球的磁性与吸波性能的影响。借助X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、振动样品磁强计(VSM)和网络分析仪对试样的物相组成、微观形貌和电磁特性进行表征。结果表明制备的镍钴铁氧体为尖晶石结构,且形貌为空心球,粒径在200nm左右。当x=0时,镍钴铁氧体空心球饱和磁化强度最大为81.7emu·g^-1,反射损耗在1658.8MHz有最小值为-16.9dB。     

酵母模板合成CuO空心微球及其催化性能研究

以酵母作为生物模板合成了氧化铜空心微球。X-射线粉末衍射、电子扫描电镜、氮气吸附-脱附、紫外-可见光漫反射光谱对产品的物化结构和性能进行了表征。电子扫描电镜分析表明氧化铜产物具有空心结构,粒径为2.2-2.9μm。X射线粉末衍射表明CuO空心微球具有很好的单斜晶型结构。氮气吸附-脱附表明CuO空心微球的比表面积是8.15 m2/g,壳体表面具有多孔性,中孔尺寸分布在2.0-35.4 nm。紫外-可见光漫反射光谱证实产物的能隙是1.38 ev。傅里叶红外、热重-差热以及X射线能谱分析监控了合成过程中组分及化学键的变化,据此提出了空心氧化铜的合成机理。进一步利用差热分析,研究了空心氧化铜催化热分解高氯酸铵的反应,证实了该空心氧化铜产品具有很高的催化活性。     

二苯基二甲氧基硅烷单体制备空心微胶囊的模板合成方法研究

制备了直径在700～1500 nm范围内的空心聚硅氧烷微球. 在O/W型聚二苯基硅氧烷微乳模板核上, 加入一定比例的二苯基二甲氧基硅烷(D型官能团)和甲基三甲氧基硅烷(T型官能团)的有机硅单体, 使之围绕在模板核表面聚合交联形成核壳结构的聚硅氧烷微胶囊, 利用合适溶剂溶解透析的方法去除模板核得到空心微胶囊. 通过TEM和AFM测定考察, 讨论了体系的各反应条件对空心微球的形态结构和大小分布的影响.     

Au@ZrO_2空心纳米微球的制备及其催化性质

以Stober法合成了不同粒径的SiO_2微球。以这些SiO_2微球为硬模板,通过ZrOCl_2前驱体吸附和水解制备得到了ZrO_2@SiO_2复合物,然后用HF溶解去除二氧化硅模板剂,制备得到ZrO_2空心球。以ZrO_2空心球为载体,采用沉积-沉淀法(DP)合成了Au@ZrO_2纳米空心微球。考察了Au@ZrO_2纳米空心微球在对硝基苯胺还原反应中的催化性能。研究结果表明,所合成的SiO_2微球粒径大小均一、形状规则、分散性好;ZrO_2空心微球大小及比表面积可以通过硬模板SiO_2微球粒径进行有效控制;与Au@ZrO_2实心微球相比,Au@ZrO_2空心微球在对硝基苯胺还原反应中表现出良好的催化性能,当反应温度为45℃、反应7 min时,对硝基苯胺能够完全转化为对苯二胺。     

单分散空心SiO2纳米微球的合成与表征

聚乙烯吡咯烷酮(PVP)功能化的聚苯乙烯(PS)粒子在SiO2包覆的同时被乙醇/氨水介质溶解, 得到了单分散空心SiO2纳米微球. 该空心SiO2纳米微球的尺寸和形态可以通过PVP, NH4OH和正硅酸乙酯(TEOS)的用量来调节. PVP用量增加导致PS粒子变小, 从而得到较小的空心SiO2纳米微球; NH4OH用量增加, 空心SiO2纳米微球表面变得粗糙; TEOS用量增加, 空心SiO2纳米微球的壳层厚度增加. 包覆(溶解)温度是控制空心SiO2纳米微球形成的最有效手段. 在70 ℃的包覆(溶解)温度下可以获得全部空心的SiO2纳米微球.     

静电纺丝法制备铁酸锌中空纤维及其磁学性能

以锌盐、铁盐和聚乙烯吡咯烷酮(PVP)为原料,通过静电纺丝法先制备PVP/硝酸盐复合纤维,这些复合纤维以5℃·min-1的升温速率加热到500℃并保温3h,最终得到铁酸锌(ZnFe2O4)中空纤维.通过X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)以及振动样品磁强计(VSM)等分析手段对中空纤维的晶体结构、形貌和磁学性能进行了研究.结果显示,ZnFe2O4中空纤维属于尖晶石结构,高温处理后仍能保持一维结构,纤维直径在200-400nm之间,纤维壁由大小为25nm的颗粒堆积而成.室温磁化结果显示制备的ZnFe2O4中空纤维具有超顺磁性,在10kOe的磁化强度为2.03emu·g-1.     

Novel preparation and properties of magnesioferrite nanoparticles

Nano-magnetic magnesium ferrite particles were synthesized by a simple and cost-effective method using different ratios between Mg/Fe precursors and fuel. Significant effects of these ratios on the crystalline phases, crystallite size, particle size, lattice constant, morphological and magnetic properties of the as-synthesized nano-particles have been investigated. Phase evolution, morphological and magnetic characteristics were determined by XRD, SEM, EDX and VSM techniques. The results obtained revealed that the as-prepared Mg ferrite nano-particles have the nanometer size and partially inverse spinel structure. Nano-structured magnesium ferrite spinel has been synthesized with various cyrystallite sizes ranging from 8 to 66 nm. Room temperature magnetization results showed that the magnetic properties of Mg ferrite nano-particles depend upon their size and crystallinity. The saturation magnetization for the sample having the highest crystallite size was 32.85 emu/g.     

Structure and morphology of spinel MFe2O4 (M=Fe, Co, Ni) nanoparticles chemically synthesized from heterometallic complexes

We synthesized magnetic spinel ferrites from trimetallic single-source precursors. Fe(II), Co(II), and Ni(II) ferrite nanoparticles in the range of 9-25 nm were synthesized by solvothermal decomposition of trimetallic acetate complex precursors in benzyl ether in the presence of oleic acid and oleylamine, using 1,2-dodecanediol as the reducing agent. For comparison, spinel ferrite nanoparticles were synthesized by stoichiometric mixtures of metal acetate or acetylacetonate salts. The nanoparticles (NP) were characterized by TEM, DLS, powder XRD, and Raman spectroscopy; and their magnetic properties were characterized by ZFC-FC and M(H) measurements. The ferrite-NP were more homogeneous and had a narrower size distribution when trimetallic complexes were used as precursors. As a consequence, the magnetic properties of these ferrite-NP are closer to the aimed room temperature superparamagnetic behavior, than are those of other ferrites obtained by a mixture of salts.     

Hollow single-crystal spinel nanocubes: the case of zinc cobalt oxide grown by a unique Kirkendall effect

Small hollow nanocubes of the ternary spinel Zn x Co 1- x Co 2O 4 of ca. 18 nm dimension were prepared via a facile hydrothermal route. A growth mechanism is suggested in which solid single-crystal Co 3O 4 nanocubes are gradually converted to hollow single-crystal Zn x Co 1- x Co 2O 4 nanocubes with preservation of the spinel framework through differential diffusion of Zn (2+) and Co (2+) ions. With the cation exchange, the chemical composition and thus physical properties can be tailored.     

Long-Term Colloidally Stable Aqueous Dispersions of ≤5 nm Spinel Ferrite Nanoparticles

Applications in biomedicine and ferrofluids, for instance, require long-term colloidally stable, concentrated aqueous dispersions of magnetic, biocompatible nanoparticles. Iron oxide and related spinel ferrite nanoparticles stabilized with organic molecules allow fine-tuning of magnetic properties via cation substitution and water-dispersibility. Here, we synthesize≤5 nm iron oxide and spinel ferrite nanoparticles, capped with citrate, betaine and phosphocholine, in a one-pot strategy. We present a robust approach combining elemental (CHN) and thermal gravimetric analysis (TGA) to quantify the ratio of residual solvent molecules and organic stabilizers on the particle surface, being of particular accuracy for ligands with heteroatoms compared to the solvent. SAXS experiments demonstrate the long-term colloidal stability of our aqueous iron oxide and spinel ferrite nanoparticle dispersions for at least 3 months. By the use of SAXS we approved directly the colloidal stability of the nanoparticle dispersions for high concentrations up to 100 g L⁻¹.     

镝掺杂铁氧体纳米晶的制备、表征和磁性

采用化学共沉淀法制备出了镝掺杂铁氧体纳米晶, 利用透射电子显微镜(TEM)、X射线衍射仪(XRD)、傅立叶红外光谱仪(FTIR)、古埃磁天平、振动样品磁强计(VSM)、X射线能谱仪(EDX)等仪器对产物进行了表征, 研究了Dy^3＋掺杂量对铁氧体纳米晶的结构、磁性和粒度的影响. 结果表明: 适量稀土元素镝离子的掺杂可以提高尖晶石型铁氧体的磁性、降低矫顽力, 当n(Fe^3＋)∶n(Dy^3＋)＝14∶1时其磁性最强. Dy^3＋替代或充填进入了尖晶石晶格, 且主要占据B位. 掺杂了镝的铁氧体磁性纳米粒子粒度变小, 且分布更集中、均匀, 当Dy^3＋加入量为n(Fe^3＋)∶n(Dy^3＋)＝14∶1时铁氧体纳米粒子的平均粒径由掺杂前的14 nm降低到到8 nm. 这种具有超顺磁性的软磁铁氧体纳米晶可应用于纳米磁液领域.     

Preparation of Magnesium,Cobalt and Nickel Ferrite Nanoparticles from Metal Oxides using Deep Eutectic Solvents

Natural deep eutectic solvents (DESs) dissolve simple metal oxides and are used as a reaction medium to synthesize spinel‐type ferrite nanoparticles MFe₂O₄ (M=Mg, Zn, Co, Ni). The best results for phase‐pure spinel ferrites are obtained with the DES consisting of choline chloride (ChCl) and maleic acid. By employing DESs, the reactions proceed at much lower temperatures than usual for the respective solid‐phase reactions of the metal oxides and at the same temperatures as synthesis with comparable calcination processes using metal salts. The method therefore reduces the overall required energy for the nanoparticle synthesis. Thermogravimetric analysis shows that the thermolysis process of the eutectic melts in air occurs in one major step. The phase‐pure spinel‐type ferrite particles are thoroughly characterized by X‐ray diffraction, diffuse‐reflectance UV/Vis spectroscopy, and scanning electron microscopy. The properties of the obtained nanoparticles are shown to be comparable to those obtained by other methods, illustrating the potential of natural DESs for processing metal oxides.     

Preparation and Electromagnetic Properties of Composites of Hollow Glass Microspheres Coated with NiFe2O4 Nanoparticles

"The composites of hollow glass microspheres coated with NiFe2O4 nanoparticles were prepared using polyacrylamide gel method. The structural characteristics, morphology and electromagnetic properties of the composite powders with different weight percent of glass microspheres (15%, 40%, and 65%) were obtained by X-ray diffraction, scanning electron microscope, infrared spectroscopy and HP8510 network analyzer. The results indicated that the phase structure of composite powders was the mixtures of nickel ferrite, quartz, and mullite. The peak intensity for nickel ferrite decreased rapidly and for mullite increased remarkably with the increasing amount of microspheres. A pure spinel structure of NiFe2O4 formed on the glass microspheres at 600 oC. A uniform and continuous NiFe2O4-coating was obtained when the content of microspheres was 40%. A great amount of NiFe2O4 particle size is less than 80 nm. The composite with a content of 40% microspheres exhibits better dielectric and magnetic loss properties which are useful to absorb more electromagnetic wave. It can be a kind of good and light electromagnetic wave absorbing material in the X-band."     

On the consequences of mechanical activation of zinc and nickel ferrites

Mechanical activation of zinc and nickel ferrites was shown to affect their physicochemical properties. For example, the temperature of magnetic transition of activated zinc ferrite sharply increased, while that of activated nickel ferrite decreased. Variation in the magnetic properties of ferrites is not due to their reversal degree, but is caused by transfer of cation from tetrahedral- to the vacant octahedral-sites in the spinel structure. The cations are randomly distributed on the octahedral-sites producing new exchange-bound pairs. The disordering of the anion and cation sublattices, leading eventually to the X-ray-amorphous structure, is thought to be due to the plastic deformations in the course of mechanical activation.     

A review on photodegradation of organic pollutants using spinel oxide

Spinel oxide has produced rapid improvement in various applications such as catalysis, sensors, batteries, degradation of dyes, drug delivery, and so on. In the current age, most of the researches are engrossed on spinel oxides for their photocatalytic activity because proficient exclusion of organic contaminants from wastewater has become a hot research topic by considering the environment. Photocatalytic degradation of organic contaminants is advantageous over conventional wastewater treatment technique like desalination, adsorption, and reverse osmosis. The current review demonstrates the photocatalytic activity of aluminate, ferrite spinel oxides, and modified spinel oxide for the removal of organic pollutants. This article comprises the structure, process of synthesis of spinel oxide, properties, photocatalytic activity, and reaction mechanism of degradation. In the end, future research needed to enhance the photocatalytic activity is discussed.