Sol-gel法制备CoxFe3-xO4薄膜的结构磁性及温度特性

采用溶胶一凝胶旋转包覆法在SiO2衬底上制备了CoxFe3-xO4(x=0.2～0.8)钴铁氧体薄膜.样品的磁性、结构及表面形貌分别采用振动样品磁强计(VSM)、X射线衍射仪(XRD)和原子力显微镜(AFM)进行测量与分析,并对Co0.8Fe2.2O4薄膜进行了高温结构和磁性原位测量.室温测量结果表明,随Co2 含量增加,样品中的尖晶石相衍射峰逐渐增强,至x=0.8时样品形成单一的尖晶石结构,同时获得较高的磁性,矫顽力达到1.56×105A/m,并且薄膜的晶粒得到细化.高温原位测量结果表明,在500 ℃高温下样品的线膨胀系数为1.3×10-5K-1,表明Co0.8Fe2.2O4薄膜结构具有良好的热稳定性.     

Co元素对Al-10Si-1.5Fe合金显微组织和力学性能的影响

在Al-10Si-1.5Fe合金中添加不同含量的钴元素,研究了钴元素对合金中富铁相的影响。研究表明,钴元素可以有效使针状富铁相组织变质,且随着钴含量的增加,针状β相逐渐转变成小块状的α-Al_(15)(Fe,Co)_3Si_2相结构,在Co/Fe物质的量比为1.5时,针状Fe相基本消失,含Fe相平均长度达到最小值(15.4μm),细化效果最好,且其抗拉强度达到最大值(152.7 MPa),断后延伸率最大值为1.58%,相比未添加Co的原始合金分别提高了66.8%和61.2%。随着钴元素的过量加入,小块状富(Fe,Co)金属间化合物发生团聚,且有白色丝状富Co相Al_3Co析出,导致合金性能下降。由此可见,在基体中添加Co,Co会与含Fe化合物中的Fe元素发生置换反应,形成多种不同的金属间化合物,同时不同的Co含量也会对金属间化合物的形貌产生影响。     

喷射共沉淀法制备纳米铁酸钴及气敏性能表征

尖晶石结构的复合氧化物已经成为一类重要的气体敏感材料.本文采用喷射共沉淀法制备了纳米铁酸钴,使用TG-DTA、XRD和TEM分析了结构特征.研究了纳米铁酸钴的气敏特性并探讨了气敏机理.     

表相掺杂Co的球形LiMn2O4制备及其电化学性能

通过CoSO4与LiOH溶液的沉淀反应,在球形Mn2O3前驱体表面包覆Co(OH)2,再与Li2CO3混合后于750℃下高温烧结20h,得到表相掺杂Co的尖晶石锰酸锂正极材料.SEM和XRD结果表明,合成样品为球形,表面粗糙,属于单一的立方晶系尖晶石结构,无其它杂相产生.与纯相LiMn2O4相比,表相掺杂Co的正极材料在室温和55℃时的循环比容量和电化学性能均得到一定提高.     

Li1+xCoyMn2-x-yO4的结构及电化学性能研究

利用溶液相合成技术把钴掺入到主尖晶石相中制得掺钴尖晶石相材料。所合成的材料具有颗粒分布均匀及结晶性能好等特点。利用X射线粉末衍射仪、傅里叶变换红外分光光度计及扫描电子显微镜对所合成掺杂锂材料的结构性能进行表征。研究表明掺杂钴可提高材料的结构稳定性能，减少锰在电解液中溶解，减少锂离子在材料中迁移电阻。电化学性能测试结果表明所合成掺钴材料Li1.03Co0.05Mn1.92O4具有较好的初始容量及循环稳定性能。     

Li1+xCoyMn2-x-yO4的结构及电化学性能研究

利用溶液相合成技术把钴掺入到主尖晶石相中制得掺钴尖晶石相材料.所合成的材料具有颗粒分布均匀及结晶性能好等特点.利用X射线粉末衍射仪、傅里叶变换红外分光光度计及扫描电子显微镜对所合成掺杂锂材料的结构性能进行表征.研究表明掺杂钴可提高材料的结构稳定性能,减少锰在电解液中溶解,减少锂离子在材料中迁移电阻.电化学性能测试结果表明所合成掺钴材料Li_1.03Co_0.05Mn_1.92O₄具有较好的初始容量及循环稳定性能.     

液相包裹法制备Pb(Mg1/3Nb2/3)O3-CoFe2O4磁电耦合材料

以无机盐Nb2O5、Mg(NO3)2、Pb(NO3)4、Co(NO3)2、Fe2(NO3)3为原料,柠檬酸和EDTA为络合剂,分别制备了Nb5+、Mg2+、Pb2+、Co2+、Fe3+等离子的络合溶液。采用络合法制备了铌酸镁-铁酸钴先驱体(MgNb2O6-CoFe2O4,简称MN-CFO)。此先驱体在1000℃煅烧1h后,得到纯净的MgNb2O6-CoFe2O4固溶体。采用液相包裹法制备了铌镁酸铅-铁酸钴(Pb(Mg1/3Nb2/3)O3-CoFe2O4)先驱体,在1000℃煅烧1h,Pb(Mg1/3Nb2/3)O3-CoFe2O4先驱体分解为具有铁电相Pb(Mg1/3Nb2/3)O3和铁磁相CoFe2O4的复相组织。研究了10%过量的PbO对煅烧过程中烧绿石相向铁电相的转变作用,并在700℃煅烧5h条件下制备了不含烧绿石相的Pb(Mg1/3Nb2/3)O3-CoFe2O4固溶体。     

钴铁氧体纳米管阵列制备及其磁学性能(英文)

为了研究一维钴铁氧体纳米管阵列的磁学性质,应用氧化铝模板具有的约束作用和毛细管作用,结合溶胶凝胶技术合成了钴铁氧体纳米管阵列.在140℃条件下,通过包含Fe(AO)3和Co(AO)2(物质的量之比为2∶1)的柠檬酸和乙二醇混合溶液(物质的量之比为1∶4)酯化反应得到溶胶.将氧化铝模板浸入溶胶几次后取出,取出充满溶胶的氧化铝模板,在大气气氛中,以0.6℃/min～5℃/min的升温速度将样品由室温升温至500℃,保温8 h.结果表明,在控制Fe3+离子浓度的条件下也可以合成钴铁氧体纳米线(Fe3+离子浓度大于1 mol/L)和"竹节"型纳米管(Fe3+离子浓度介于0.5 mol/L～1.0 mol/L),但重点进行了其纳米管阵列(Fe3+离子浓度小于0.5 mol/L)合成和磁学性能测试.透射电子显微镜(TEM)、高分辨电镜(HRTEM)的观察以及粉末X光衍射(XRD)测试结果表明纳米管组成为多晶结构.纳米管的直径取决于氧化铝模板的孔径,大约为200 nm,其长度约几个微米.应用样品振动磁强计对样品磁性进行了表征,结果表明纳米管阵列未表现出方向特性,矫顽力随着升温速率的降低而升高,在0.6℃/min的升温速率时,矫顽力达到最高的1 445 kOe,简单讨论了其形成原因.     

混合导体氧化物SrFeCo0.5Oy粉末的微波合成与表征

采用微波加热方法与常规高温固相法合成了Sr-Fe-Co-O系混合导体陶瓷氧化物粉末.利用XRD,TEM/EDX及SEM等测试方法分析与表征粉体.用微波加热合成的粉体颗粒尺寸分布均匀,一次颗粒尺寸较小,结晶度也好于用常规加热合成的粉体.微波加热合成粉体的结晶相结构是钙钛矿结构Sr(Fe,Co)1.5Oy相,并有少量的正交结构相和尖晶石(Co,Fe)3O4相;高温固相法合成粉末由Sr4(Fe,Co)6O13±δ相及少量的Sr(Fe1-xCox)O3-δ相和CoO相组成.     

Co掺杂改性尖晶石型Li_(1.035)Mn_(1.965)O_4的合成及其电化学性能（英文）

采用湿化学–后续热处理技术,合成了掺钴尖晶石锰酸锂材料。X射线衍射(XRD)分析结果表明,钴的掺入没有改变材料的Fd3m结构。扫描电子显微镜(SEM)分析表明,所合成的材料颗粒均匀,形貌规整,粒径分布较窄。透射电子显微镜(TEM)结果表明,Li1.035Co0.035Mn1.930O4具有完好的结晶态。充放电测试结果表明,在室温下钴掺杂能够提高材料的电性能。当产物为Li1.035Co0.035Mn1.930O4时,其电性能达到最优:以0.5C充放电,首次放电容量为113 mAh/g,经过100次循环后容量保持率为93.8%,经过4C放电后仍然能够保持0.5C放电容量的76.1%;而未掺钴的Li1.035Mn1.965O4经过4C放电容量仅保持0.5C放电容量的64.8%。电化学阻抗测试结果表明,钴离子的掺杂能够提高锰酸锂材料的锂离子扩散速率。     

Preparation and Characterization of Fe3O4 Magnetic Nano-particles by 60Co γ-ray Irradiation

By using a new method, ^60Co γ-ray irradiation, Fe3O4 magnetic nano-particles were successfully synthesized at room temperature under ambient pressure. The structure, morphology and magnetic properties of these nanoparticles were characterized by X-ray diffraction （XRD）, transmission electron microscope （TEM） and vibrating sample magnetometer （VSM）, respectively. The radiation formation mechanism was also discussed. The results show that the absorbed dose can greatly influence the structure, morphology and magnetic properties of the products. XRD and TEM studies show that the product prepared by γ-ray irradiation （10 kGy） is pure FesO4 phase and the mean diameter of these nano-particles is about 21 nm. The Fe3O4 nano-particles synthesized by γ-ray irradiation （10 kGy） are mainly in small cubic shape and the size uniformity of these particles is good.     

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.     

Ni doped Fe3O4 magnetic nanoparticles

In this work, the effect of nickel doping on the structural and magnetic properties of Fe3O4 nanoparticles is analysed. Ni(x)Fe(3-x)O4 nanoparticles (x = 0, 0.04, 0.06 and 0.11) were obtained by chemical co-precipitation method, starting from a mixture of FeCl2 x 4H2O and Ni(AcO)2 x 4H2O salts. The analysis of the structure and composition of the synthesized nanoparticles confirms their nanometer size (main sizes around 10 nm) and the inclusion of the Ni atoms in the characteristic spinel structure of the magnetite Fe3O4 phase. In order to characterize in detail the structure of the samples, X-ray absorption (XANES) measurements were performed on the Ni and Fe K-edges. The results indicate the oxidation of the Ni atoms to the 2+ state and the location of the Ni2+ cations in the Fe2+ octahedral sites. With respect to the magnetic properties, the samples display the characteristic superparamagnetic behaviour, with anhysteretic magnetic response at room temperature. The estimated magnetic moment confirms the partial substitution of the Fe2+ cations by Ni2+ atoms in the octahedral sites of the spinel structure.     

Mn和Fe掺杂对尖晶石氧化物Co2MnO4结构和磁性的影响

以金属盐及柠檬酸为原料, 采用溶胶-凝胶法制备了尖晶石氧化物Co_2-xMn_1+xO₄和Co_2-xFe_xMnO₄系列, 通过XRD、FT-IR及PPMS等手段研究了Co₂MnO₄及系列掺杂样品的成相、结构、磁性等特征。结果表明, Co_2-xMn_1+xO₄系列在x<0.6时, 呈单相立方结构, 晶格常数和磁性随着Mn掺杂量的增加而增大, x≥0.6时逐渐向四方结构转化, 磁性下降, 并呈现磁化强度不易饱和的特征; Co_2-xFe_xMnO₄系列样品在x<1.75成分范围内均可保持立方结构, 且晶格常数和磁性都随着x增大而提高。这些变化主要是由于掺杂原子尺度及磁矩均大于原有元素, 掺杂后样品内部的磁性相互作用有所增强。     

Anomalous electrical properties of nanocrystalline Ni–Zn ferrite

Nanocrystalline powders of Ni–Zn ferrite (NZFO) having the chemical formula Ni _x Zn_1−x Fe₂O₄, where x varies as 1, 0.8, 0.6, 0.4, 0.2, and 0, were synthesized by chemical co-precipitation technique. The samples synthesized were characterized by X-ray diffraction (XRD) technique at several stages. As prepared samples at room temperature show absence of Bragg peak indicating that there was no crystalline phase formation of ferrite. The XRD pattern of the samples sintered at 400 °C clearly showed the characteristic Bragg peaks of spinel cubic structure. XRD patterns were further analyzed to calculate the lattice constant, porosity, and jump length of charge carriers. Electrical dc resistivity measurements were carried out with respect to temperature using two probe method. NZFO samples showed abnormal electrical behavior at room temperature. Also abnormal electrical behavior with increase in temperature in the range 600–800 K was observed. Variation of dielectric constant and loss tangent with frequency were studied at room temperature. The electrical and dielectric behavior of the Ni–Zn samples is discussed in the light of literature.     

Preparation, electrocatalytic and photocatalytic performances of nanoscaled CuO/Co3O4 composite oxides

Cu-Co composite oxides with different Cu/Co atomic ratios were prepared by the calcination of the precursors synthesized via a co-precipitation method. The samples were characterized by XRD, SEM and TEM, respectively. The XRD analysis revealed that only spinel structure of Cu-Co composite oxide was confirmed with lower Cu/Co ratio (<1:2). The sizes and morphologies of samples are controlled significantly by the Cu/Co atomic ratios. The electrocatalytic activity for p-nitrophenol reduction in a basic solution with the samples decorated on glassy carbon (GC) electrodes was tested by cyclic voltammetry (CV). The results showed that the sample with Cu/Co ratio of 2:8 exhibited the highest catalytic activity for p-nitrophenol reduction. The photocatalytic performances of the samples for the degradation of methyl orange under irradiation of visible light were investigated. The samples with Cu/Co ratios from 5:5 to 10:0 all showed better photocatalytic activities for methyl orange degradation, but the sample with Cu/Co ratio of 9:1 exhibited much higher catalytic activity. The catalyst with Cu/Co ratio of 9:1 also exhibited excellent repeatability for the catalytic degradation of methyl orange.     

富锂正极材料Li1+x[Ni0.36Mn0.64]1-xO2的制备及电化学性能研究

采用氢氧化物共沉淀-高温固相焙烧法合成了富锂正极材料Li1+x[Ni0.36Mn0.64]1-xO2(x=0.12,0.15,0.18,0.2)。采用XRD表征其结构,SEM表征其形貌,恒电流充放电和循环伏安测试其电化学性能。其中,XRD结果表明各样品都具有α-NaFeO2型层状结构。结果表明:室温下以30mA/g的电流密度,在4.6~2.75V的电压范围内充放电,x=0.15的首次放电比容量为237.9mAh/g,经50次循环后容量保持率为98%。研究发现,层状富锂镍锰正极材料中的Li2MnO3组分在充放电过程中会逐渐向尖晶石相转变,这是容量衰减的主要原因。     

Hydrothermal synthesis and magnetic properties of CoxFe1−x/CoyLazFe3−y−zO4 composites

A series of iron–cobalt alloy and cobalt–ferrite composites doped with La³⁺ (Co_xFe_1−x/Co_yLa_zFe_3−y−zO₄) in which the Fe–Co alloy has either a bcc or a fcc structure and the oxide is a spinel phase, have been synthesized by using the disproportionation of Fe (OH)₂ and the reduction of Co (II) by Fe⁰ in a concentrated and hot KOH solution. when x ≤ 0.1, the structures of the Fe_xCo_1−x alloy and cobalt–ferrite are fcc structure; and when x ≥ 0.25, the structures of the Fe_xCo_1−x alloy is bcc structure. The fcc structure of alloy is favored for [KOH] close to 9 N, Co(II)/Fe(II) ratios between 0.5 and 0.9 and short reaction time of synthesis. And the bcc structure of the alloy is favored for [KOH] close to 1 N, Co(II)/Fe(II) ratios between 0.1 and 0.5 and long reaction time of synthesis. A low [KOH] favors nucleation leading to octahedral of 1 μm. And [KOH] of 9–12 N favors particle growth. The metal occurs in square particles of 100–150 nm included within the spinel. Powder X-ray diffraction (XRD), thermal gravity analysis (TGA) and different thermal analysis (DTA), scanning electron microscope (SEM), transmission electron micrograph (TEM) and vibrating sample magnetometer (VSM) were employed characterize the crystallite sizes, structure, morphology and magnetic properties of the composites. And the effect of the Co(II)/Fe (II) ratio (0 ≤ Co/Fe ≤ 1), concentration of KOH, reaction time and substitution Fe³⁺ ions by La³⁺ ions on structure, magnetic properties of the composites were investigated.     

锰锌铁氧体的低温合成及表征

采用溶胶-凝胶自燃烧法在低温下一步合成了纯相尖晶石结构的锰锌铁氧体(Mn0.5Zn0.5Fe2O4)纳米颗粒。其结构、形貌和热分解过程分别采用X射线衍射仪(XRD)、扫描电镜(SEM)和TG-DSC分析仪进行了表征。结果表明:在pH=7.0、柠檬酸与金属离子摩尔比为1∶1和柠檬酸的浓度为0.7mol/L的条件下,金属的硝酸盐和柠檬酸形成的干凝胶可通过自燃烧过程一步合成出平均粒径约为60nm的纯相Mn0.5Zn0.5Fe2O4铁氧体纳米颗粒。经过400℃煅烧后,颗粒粒径增大,衍射峰变窄,强度增加,晶型更趋于完整。     

Oleic-acid-coated CoFe2O4 nanoparticles synthesized by co-precipitation and hydrothermal synthesis

Oleic-acid-coated CoFe₂O₄ nanoparticles were synthesized by co-precipitation and hydrothermal synthesis. The coprecipitation of the nanoparticles was achieved by the rapid addition of a strong base to an aqueous solution of cations in the presence of the oleic acid surfactant, or without this additive. The nanoparticles were also synthesized by a hydrothermal treatment of suspensions of the precipitates, coprecipitated at room temperature in the presence of the oleic acid, or without it. The influence of the synthesis conditions, such as the valence state of the iron cation in the starting aqueous solution, the temperature of the treatment and the presence of oleic acid, on the particles size was systematically studied. X-ray powder diffractometry (XRD) and transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDS) revealed that, although spinel forms at room temperature, a substantial amount of Co was incorporated within the secondary, feroxyhyte-like phase when the iron cation was in the 2+ state. In contrast, when iron was in the 3+ state, the spinel forms at elevated temperatures of approximately 60 °C. The presence of the oleic acid further increased the formation temperature for the stoichiometric spinel. Moreover, the oleic acid impeded the particles’ growth and enabled the preparation of colloidal suspensions of the nanoparticles in non-polar organic solvents. The nanoparticles’ size was successfully controlled by the temperature of the synthesis in the region where superparamagnetism dominates to the region where mono-domain ferrimagnetism dominates the magnetic properties.