不同磁场下水热制备CoFe2O4纳米颗粒及其磁性能的研究

以Co(NO3)2·6H2O,Fe(NO3)3·9H2O,NaOH为原料,在不同外加磁场条件下进行水热处理,分别制备了颗粒尺寸为几纳米到20 nm的CoFe2O4纳米颗粒,通过XRD,TEM和振动样品磁强计对其晶体形貌和宏观磁性能进行表征.结果表明,采用水热法制备的CoFe2O4可获得纯度较高晶粒生长完整的CoFe2O4磁性纳米微粒,稳恒磁场条件对晶格常数,磁性能有较大的影响.当稳恒磁场在一定范围内时,随着稳恒磁场的增加,磁性颗粒的粒径增大,样品室温下的饱和磁化强度逐渐增大.但是当稳恒磁场超出一定范围时,随着稳恒磁场的减小,磁性颗粒的粒径减小,样品室温下的饱和磁化强度逐渐减小.     

单分散BaFe12-xCuxO19纳米颗粒磁性能及穆斯堡尔谱分析

采用水热法制备BaFe12-xCuxO19(x=0、0.2、0.4、0.6、0.8)钡铁氧体,探讨Cu2掺杂量对纳米BaFe12O19微观结构以及磁性能的影响.穆斯堡尔光谱分析结果显示,Cu2可以定量可控的掺入到BaFe12O19的晶格中.利用X射线衍射仪(XRD)和扫描电镜(SEM)对不同掺杂量的样品进行表征,结果表明,800 ℃热处理可以明显提高BaFe12O19纳米颗粒的结晶性,并随着Cu2掺入量的增多BaFe12O19的晶粒尺寸逐渐增大.从磁测量分析结果可以得知,适当掺入Cu2可以降低BaFe12O19的矫顽力与饱和磁化强度,使得BaFe12O19纳米颗粒开始从硬磁性能向软磁性能转变.     

B位四价Sn4+, Zr4+取代对Ba(Zn1/3Nb2/3)O3系统微观结构的影响

采用传统的固相陶瓷烧结工艺,利用四价正离子Sn4+、Zr4+取代Ba(Zn1/3Nb2/3)O3陶瓷的B位Zn2+、Nb5+,研究其对Ba(Zn1/3Nb2/3)O3系统微观结构的影响.四价Sn4+、Zr4+取代B位Zn2+、Nb5+可以形成固溶体,系统的主晶相仍为立方相.系统晶格常数a随着Sn4+取代量的增加而呈线性增大,相同Sn4+取代量下随着烧结温度的增加,晶格常数a增大.BaZrO3(BZ)的加入可减少第二相的生成.Sn4+、Zr4+均可改善系统烧结特性,加快致密化形成.     

水热法制备Ti1-xFexO2稀磁半导体

本论文采用水热法制备Fe掺TiO2稀磁半导体Ti1-xFexO2(x=0-0.04),并对其形貌、结构及磁性能进行表征.X射线衍射分析结果表明,掺杂Fe离子后产物为TiO2锐钛矿结构,其晶体晶格常数随掺人铁离子含量的增加而略有增大.透射电镜和x射线能谱测试结果表明,样品形貌规整,平均粒径约为20 nm.利用振动样品磁强计对其磁性能进行测量,结果表明样品在室温条件下存在铁磁性.     

对比不同离子的掺杂对镍锌铁氧体电磁损耗性能的影响

应用水热法掺杂Co2+、Mn2+和Cu2+到纳米镍锌铁氧体粉末中.并利用XRD、TEM和VNA对其进行表征和分析,研究了掺杂不同金属离子对样品粒度、形貌、电磁损耗性能及吸收性能的影响.结果表明:镍锌钴铁氧体结晶更加完全,晶粒结构更加完整,出现团聚现象,晶粒排列相比其他更加致密.并且晶格常数由0.8352 nm增加到0.8404 nm,改变吸收峰的位置,增加吸收器的带宽,改善材料在低频率区间内的的吸波性能.Mn2+的掺杂相比镍锌钴铁氧体吸波性能下降,吸波效果减弱.Cu2+的掺杂没有影响纳米镍锌铁氧体电磁损耗的吸波频段.     

镍锌铁氧体Ni(1-x)ZnxFe2O4中锌含量对其微观结构以及磁电性能的影响

用传统的固相法制备镍锌铁氧体Ni(1-x)ZnxFe2O4(x=0～1.0).样品在1150～1250℃不同温度烧结,得到了纯相的尖晶石结构铁氧体,深入并详细研究了陶瓷样品的结构、微观结构、磁性能以及电性能.研究发现,居里温度随锌含量的增加呈线性增大;磁导率以及饱和磁化强度随着锌含量的增加先增大后减小;矫顽力在不同烧结温度表现出不同的性能特征,在1200℃烧结的样品的矫顽力随着锌的增多先逐渐增大,然后又逐渐减小,而在1250℃烧结的样品的矫顽力随着锌的增加整体逐渐减小;部分样品的介电性能出现了德拜迟豫现象.     

Zn含量对NiCuZn旋磁铁氧体的显微结构、磁性能和介电性能的影响

采用氧化物陶瓷工艺制备了Ni0.6533-xCu0.1005 Zn0.2613+xFe1.9899O4(x=0,0.0402,0.0804,0.1206)微波铁氧体,研究了不同Zn含量对NiCuZn铁氧体的显微结构、磁性能和介电性能的影响.结果表明:ZnO具有明显的助熔作用,NiCuZn铁氧体的平均晶粒尺寸与饱和磁化强度随着Zn含量的增多逐渐增大,而矫顽力和居里温度则逐渐减小.样品的剩余磁感应强度随着温度的升高而不断降低,且Zn含量越多,其下降速率越大.当x=0.0804时,室温下NiCuZn铁氧体具有最高的剩余磁感应强度356 mT,且其温度稳定性也较好.此外,x在0～0.1206范围内,铁氧体的电阻率、介电常数和介电损耗角正切变化不大.     

微波烧结制备高性能锶铁氧体永磁材料的研究

以工业锶铁氧体磁瓦生坯为对象,分别考察了工业隧道窑烧结、间歇微波烧结和连续微波烧结等工艺过程制备M型锶铁氧体永磁材料.微波烧结试验发现:采用间歇工艺可制备出具有磁铅石型结构的锶铁氧体磁瓦,烧结周期为3h,且在1100℃烧结时获得最佳磁性能为:Br=396.0 mT,Hcj=342.9 kA/m,(BH)max=28.23 kJ/m3.其性能优于推板式隧道窑在室温～1230℃,烧结周期20～24 h所烧结的产品.连续微波烧结条件为:1000℃,2h,同样获得磁铅石型结构的锶铁氧体磁瓦,其性能为:Br=363.8 mT,Hcj=363.0kA/m,(BH)max=25.76 kJ/m3.由此可见,针对湿法成型锶铁氧体永磁材料,采用微波烧结工艺不仅能够获得所期望的结构与性能,而且能够显著降低温度和缩短烧结周期.     

CeO2对CaTiO3陶瓷烧结性能以及微观结构的影响

以CaO和TiO2为原料,采用固相反应烧结法合成钛酸钙陶瓷.以CeO2为添加剂,重点研究CeO2掺杂对合成钛酸钙陶瓷烧结性能及微观结构的影响.利用XRD、SEM、EDS等手段对试样的物相组成、显微形貌以及元素分布进行表征.通过X'pert High score Plus软件研究CeO2添加量和煅烧温度对合成钛酸钙的相组成、晶胞参数、缺陷反应的影响.结果表明:随着CeO2加入量的增大,Ce4+与Ti4+及Ce3+与Ca2+之间发生取代,致使钛酸钙的晶体结构发生畸变,晶格常数以及晶胞体积出现了先增大后减小的趋势.CaTiO3结构中取代位置的改变,是造成晶胞体积呈非线性变化趋势的原因.形成的结构缺陷加速了固相烧结反应,钛酸钙晶粒由发育不完全的台阶状转变为规则的多边形.过量的CeO2会抑制晶粒的生长,减小晶粒尺寸.随着煅烧温度的升高,结构中热缺陷浓度增大,促进了钛酸钙的烧结.     

热处理工艺对室温制备ZnO:Al薄膜结构与光电性能的影响

采用室温溅射加后续退火工艺制备了ZnO∶ Al透明导电薄膜.研究了热处理工艺对薄膜微观结构和光电性能的影响.研究表明:退火有助于减小Al~(3+)对Zn~(2+)的取代造成的晶格畸变,消除应力,促进晶粒长大,有效提高电子浓度和迁移率,降低电阻率;当溅射功率为80 W、退火温度为320 ℃时,薄膜的电阻率可低至8.6×10~(-4) Ω·cm;退火气氛对薄膜的导电性能有较大影响,真空退火可使吸附氧脱附,大大降低薄膜的方块电阻.而退火温度和退火气氛均对ZnO∶ Al薄膜的透光率没有明显影响,薄膜的透光率在86;以上.     

Effect of Sintering Temperature on Thermoelectric Power of Mixed Lithium?Zinc Ferrites

Thermoelectric power of polycrystalline lithium-zinc ferrites having the compositional formula Li_0.5−x/2Zn_xFe_2.0−x/2O₄ (where × = 0.2, 0.4, 0.6, 0.8, and 1.0), sintered at 1200, 1250 and, 1300°C has been investigated over the temperature range 300 to 450 K by the probe method. The Seebeck coefficient (Q) is found to decrease with increasing sintering temperature, whereas the carrier concentration (n) and the charge carrier mobility (μ) are found to increase with increasing sintering temperature. Among all the mixed lithium-zinc ferrites, the one having a zinc content of 0.6 mole has a minimum value of Seebeck coefficient and maximum value of charge carrier concentration.     

Al掺杂ZnO多晶的热电输运性质研究

采用固相反应法制备了六方纤锌矿结构Zn1-xAlxO(0≤x≤0.03)系列多晶,探究了Al掺杂对ZnO多晶的微观形貌和热电输运性质的影响.结果表明,Al掺杂促使ZnO晶粒长大联结,晶界减少,x＞0.003时出现在晶界分布的ZnAl2O4尖晶石相.掺杂后样品由ZnO的半导体行为转变为电阻率显著下降的金属行为,且x=0.003有最小的室温电阻率～1.7 mΩ·cm,主要由于掺杂使样品载流子浓度和迁移率显著提高,x=0.003时载流子浓度和迁移率为最高,分别为1.05×1021 cm-3和20 cm2/V·s;300 ～900 K下掺杂样品热电势的绝对值和功率因子均随温度升高而增大,x =0.003时有最大的室温功率因子～0.4mW/m·K2.综合得到ZnO中Al掺杂的饱和固溶度x≈0.003.     

Magnetic properties of nanoparticles glass–ceramic rich with copper ions

The current study aimed at the assessment of CuO gradual addition on the crystallization behavior and magnetic properties of ferromagnetic glass ceramic in the system Fe₂O₃·CaO·ZnO·SiO₂. Ferromagnetic glass–ceramics with a high quantity of magnetite were designed to be crystallized in the system Fe₂O₃·CaO·ZnO·SiO₂. The influences of gradual addition of CuO and melting temperature on the sequence of crystallization and magnetic properties were studied. The X-ray diffraction patterns showed the presence of nanometric magnetite crystals in a glassy matrix after direct cooling from the melt without any additional heat treatments. Increasing the melting temperature resulted in an increase in the magnetite crystallization. The addition of up to 20 g CuO/100 g batch composition revealed a decreasing effects in both endo- and exothermic values, whereas, the same values were inversely increased with increasing the CuO addition to 30 g. In general, increasing the CuO amounts greatly enhanced the crystallization of magnetite. A significant amount of delaffosite (CuFeO₂) was unexpectedly detected and increased by increasing both the added amount of CuO and the treatment temperature. The XRD results detected some traces of cuprite (Cu₂O) in the samples of high CuO content. The TEM results reflected the precipitation of nano-magnetite crystals in the 2–10 nm size range. Magnetic hysteresis cycles were analyzed using a vibrating sample magnetometer with a maximum applied field of 20 kOe at room temperature in quasi-static conditions. From the obtained hysteresis loops, the saturation magnetization (Ms), remanence magnetization (Mr) and coercivity (Hc) were determined.     

The influence of hafnia and impurities (CaO/SiO2) on the microstructure and magnetic properties of Mn–Zn ferrites

The study investigates the effects of hafnia (0.2, 0.4 and 0.6 wt%) along with impurities such as 0.02 wt% SiO₂ and 0.04 wt% CaO on the microstructure and magnetic properties of Mn–Zn ferrites. The specimens have been prepared by the conventional mixed oxide method. It has been revealed that the substitution of hafnium into Mn–Zn ferrites enhances the grain growth. Measurements of initial permeability, resistivity and power loss have been related to the microstructure of sintered ferrites in particular to grain size, porosity and grain boundary phases. The present paper gives a summary that optimum properties could be achieved with additive level of 0.4 wt% HfO₂.     

烧结对低功耗掺杂MnZn铁氧体性能的影响

烧结是功率铁氧体研制过程中极为重要的一个环节.文中详细分析了不同烧结温度对样品微结构的影响,以及烧结温度对不同掺杂的低功耗MnZn铁氧体材料磁性能以及功耗的影响.结果表明,样品烧结温度过低,样品中晶粒大小悬殊,气孔分散于晶粒和晶界内部,导致其磁导率降低,矫顽力增大,功耗上升;同时,过高的温度将使晶粒异常长大,导致某些杂质局部熔融而使晶界变形,从而降低了铁氧体的性能.     

Topology and symmetry analysis of rare earth borocarbides structural family,analogy to hexaferrites and relation to properties

The topology and symmetry analysis was applied to a series of rare earth borocarbide compounds, which have been gaining increasing interest due to their magnetic and thermoelectric properties. Using principles of OD theory, the crystal structures were deconvoluted into L(1) (B₁₂ icosahedra and C‐B‐C chain) layers and L(2) (rare earth and B₆ octahedral) layers. The arrangement of B₁₂ icosahedra in the L(1) layer is equal to close packed spheres, however, symmetry of the B₁₂ block lowers symmetry of the resulting layer from P 6/mmm to P 3m1. Both layers, L(1) and L(2) possess symmetry P 3m1 and the conjugation of L(1) with L(2) layers occurs in accordance with the symmetry elements. No disorder may appear here because of equal symmetry of single layers and layer pairs and it is not a classical OD family. Only the increasing of the amount of one type of layers, namely L(1), provides the structural variations. Close analogy to the hexagonal ferrites family has been found. Topology and symmetry analysis reveals principles in the building up of the structural family, gives an insight into the particular order‐disorder formation mechanism/criteria of these homologous borocarbide compounds and as the result relation to the properties (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

不同退火温度对钡铁氧体薄膜磁性的影响

M型钡铁氧体(BaFe₁₂O₁₉, BaM)是一种单轴磁晶各向异性的六角晶系硬磁材料,由于其具有很强的各向异性场,因此在自偏置微波器件领域具有广阔的应用前景。本文采用常温射频磁控溅射法在(000l)取向的蓝宝石衬底上沉积了厚度约为130 nm的BaFe₁₂O₁₉非晶薄膜,然后分别在850 ℃、900 ℃、950 ℃、1 000 ℃对其空气退火处理3 h,得到BaM晶体薄膜样品。采用X射线衍射仪对薄膜样品进行物相及晶体生长取向鉴别,采用扫描探针显微镜和扫描电子显微镜对薄膜样品的粗糙度和表面形貌进行测量和观察,采用振动样品磁强计对样品进行了静态磁性能测试。实验结果表明,退火后的薄膜样品的主晶相为BaM,且具有(000l)取向择优生长,其微观组织结构都表现为C轴垂直于膜面的颗粒状结构。退火温度为900 ℃时所得样品的各项性能达到最佳,其表面粗糙度为2.8 nm,矩形比为0.84,饱和磁化强度为247 emu/cm³,矫顽力为1 528 Oe。     

溶胶-凝胶自燃烧法制备Ba(NiMg)0.2AlxFe11.4-xO19的结构与磁性能

以柠檬酸为络合剂,利用溶胶-凝胶自燃烧法制备了Ni、Mg、Al掺杂的M型钡铁氧体粉体(Ba(NiMg)0.2AlxFe11.4-xO19,x=0~0.4),利用X射线衍射仪、透射电子显微镜、综合物性测量系统等对样品结构与室温磁性能进行研究.结果表明,样品的物相组成与Al掺杂量有密切关系,当Al掺杂量x超过0.2时,产物中出现杂相α-Fe2O3,且杂相α-Fe2O3的含量随x值的增大而增加.在10kOe的外加磁场下,样品的饱和磁化强度(Ms)随x值的增大而降低,矫顽力(Hc)则随x值的增大先增大后减小,当x=0.2时,矫顽力达到最大值5644Oe,对应的饱和磁化强度为46emu/g.     

Sr掺杂对Ca3Co4O9基材料热电性能的影响

采用溶胶-凝胶法,结合常压烧结工艺制备了Ca3-xSrxCo4O9(x=0～0.5)热电陶瓷材料,并对材料的热电性能进行了测试。结果表明,Sr掺杂对Ca3Co4O9基材料的热电性能有较大影响。随着掺杂量的增加,电导率逐渐增大,Seebeck系数略有减小。Sr掺杂能显著降低热导率,而且随着掺杂量的增加,热导率的下降幅度逐渐增大。Sr掺杂显著改善Ca3Co4O9材料的热电性能,当掺杂量为0.5时获得最佳热电性能,573 K时Z值达1.07×10-4 K-1。     

Structural and morphological studies on Mn substituted ZnO nanometer‐sized crystals

Mn substituted ZnO nanocrystals synthesized by a co‐precipitation method. X‐ray diffraction (XRD) studies confirms the presence of wurtzite (hexagonal) crystal structure similar to un doped ZnO, suggesting that doped Mn ions go at the regular Zn sites. The lattice parameters a and c are increasing with increasing Mn content. The unit cell volume increases with increasing Mn concentration, indicating the homogeneous substitution of Mn²⁺ for the Zn²⁺. The lattice distortion parameter (ε_v) is evaluated from XRD data and found that it enhances as Mn content increases. Transmission electron microscopy photographs show that the size of the ZnO crystals is in the range of 20‐50 nm. The SAED pattern confirms the hexagonal and crystalline nature of the samples which are in agreement with X‐ray analysis. The chemical groups of the samples have been identified by FTIR studies (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)