La0.8Sr0.2CoxFe1-xO3型氧扩散障层材料的制备及结构性能研究

采用共沉淀-凝胶方法制备La0.8Sr0.2CoxFe1-xO3(x=1.0、0、0.3)氧扩散障碍层材料的前驱体,分别用X射线衍射分析、透射电镜、扫描电镜和交流阻抗谱仪对三种不同粉体及其陶瓷结构和性能进行研究.结果表明:在870℃下焙烧制备的La0.8Sr0.2CoxFe1-xO3(x=1.0、0、0.3)粉末具有钙钛矿相结构,无硬团聚,颗粒大小在20～60 nm.此粉末经冷等静压250MPa成型后,在1120℃下烧结6h,La0.8Sr0.2CoO3和La0.8Sr0.2FeO3混合导体的电导率在10—1S/cm数量级,而La0.8Sr0.2Co0.3Fe0.7O3导电率最高达100 S/cm数量级.三种陶瓷都是电子电导远大于离子电导的混合导体,电导率最高值在200～300℃范围,偏向低温.     

Ln0.6Sr0.4 FeO3-δ(Ln=La、Nd、Ce)阴极材料的制备与表征

以甘氨酸-硝酸盐水溶液为前驱体合成了Sr掺杂的稀土铁酸盐Ln0.6Sr0.4FeO3-δ(Ln=La、Nd、Ce)粉体.对制备过程的化学键变化、样品的热稳定性、物相形成过程及导电性进行了表征.结果表明,甘氨酸-硝酸盐合成法成相温度低于1000℃.坯体烧结较粉状样品更有利于钙钛矿物相的形成,La0.6Sr0.4FeO3-δ及Nd0.6Sr0.4FeO3-δ坯体1000℃煅烧2h即可形成近乎单一的钙钛矿相(ABO3);Ce0.6 Sr0.4 FeO3-δ是CeO2立方萤石相和产物钙钛矿相共存,两相难分主次.合成样品低温下的导电行为符合小极化子导电机制;1200℃烧结的La0.6Sr0.4FeO3-δ样品在测试全温度范围内(450～800℃)电导率超过100S/cm,Nd0.6Sr0.4FeO3-δ在中温区(600～800℃)电导率＞60S/cm;Ce0.6Sr0.4FeO3-δ样品的电导率不理想.     

中空ZnCo2O4纳米线的合成及其电化学性能分析

运用微乳液法,以醋酸盐为原料,草酸为沉淀剂,CTAB为表面活性剂,乙二醇为单一溶剂首先合成前驱体ZnCo2(C2O4)3纳米线,然后用ZnCo2(C2O4)3纳米线作为牺牲模板经过煅烧合成多孔的ZnCo2O4纳米线。用FT-IR、XRD、SEM、TEM和电化学性能测试,研究得到的产物的形貌结构和电化学性能。结果表明:合成了具有一维结构的尖晶石结构的ZnCo2O4纳米线,由于具有较大的比表面积和多孔性,更有利于锂离子的嵌入与脱出,其初始放电比容量达1841mAh.g-1,25次循环后容量还能达到765mAh.g-1,整体的库伦效率维持在100%左右,循环性能良好。     

La1-xSrxFeO3纳米微粉的微结构与磁性

为了研究La1-x Srx FeO3纳米微粉的成分及颗粒尺寸对其微结构及磁学性能的影响,采用溶胶-凝胶法制备了不同颗粒尺寸、不同Sr含量的钙钛矿型La1-x Srx FeO3(x=0～0.3)纳米微粉,采用X射线衍射和振动样品磁强计对其结构与磁性进行了分析.分析表明,所制样品均具有正交钙钛矿结构;对于颗粒尺寸相近、Sr含量不同的样品,随Sr含量增加,晶格收缩;在具有不同颗粒尺寸的La1-xSrx FeO3(x=0.3)纳米微粉中,随着颗粒尺寸的减小,晶格膨胀;La1-x Srx FeO3(x=0～0.3)纳米微粒具有弱铁磁性,Sr含量的增加导致自发磁化强度下降,且随着颗粒尺寸的减小,La1-x Srx FeO3(x=0.3)纳米微粉的自发磁化强度增大;由Sr的替代以及颗粒尺寸减小引起的结构变化导致磁性的变化.     

La0.7Sr0.3FeO3纳米晶薄膜的制备及FET式气敏元件的研制

采用溶胶凝胶工艺,合成出纳米晶La07Sr03FeO3薄膜,薄膜为钙铁矿结构,平均粒径在40nm左右。利用该薄膜采用平面工艺制作出微米尺寸、室温工作的La07Sr0.3FeO3纳米薄膜栅OSFET式气敏元件,并对其气敏性能进行了测试,发现器件的漏电流在乙醇气体中zk大,在氮氧化物中降低。     

La0.3Sr0.7Fe0.7Cu0.2Mo0.1O3-δ钙钛矿超细陶瓷粉体制备与催化性能研究

采用溶胶低温燃烧法制备了单一组成的La0.3Sr0.7Fe0.7Cu0.2Mo0.1O3-δ(LSFCM)超细钙钛矿陶瓷粉体。用XRD,SEM以及TA等方法对粉体的物相、形貌、粒度以及导电性能等进行了表征。考察了LSFCM陶瓷粉体对甲烷部分氧化(POM)制备合成气的催化活性与稳定性。结果表明:溶胶燃烧粉末经800℃下煅烧4h可得到平均粒径小于35nm的立方钙钛矿结构LSFCM陶瓷粉体,相对密度为96.7%的LSFCM烧结体在空气气氛600℃温度下电导率达到26.27S·cm-1,在950℃、CH4/O2比为1.5~2.0时,甲烷转化率及一氧化碳与氢气选择性均达到90.0%以上;反应43h后虽产生少量积炭,但仍能保持钙钛矿结构,表明LSFCM粉体对甲烷部分氧化制合成气反应具有良好的催化活性和稳定性。     

负载磷钼杂多酸/La0.7Ca0.3Fe0.25Co0.75O3/聚吡咯的制备及光催化性能研究

采用甘氨酸-硝酸盐燃烧法成功制备了La0.7Ca0.3Fe0.25Co0.75O3钙钛矿型复合氧化物,以(NH4)2S2O8为氧化剂,运用化学氧化法合成La0.7Ca0.3Fe0.25Co0.75O3/聚吡咯薄膜,然后通过静电自组装方法制备了一种新的表面负载修饰型复合光催化剂La0.7Ca0.3Fe0.25Co0.75O3/PPy/PMO12。采用XRD、SEM、FT-IR对催化剂的物化结构进行了表征。光催化性能测试是以亚甲基蓝染料的水溶液为降解目标,结果表明,PMo12的负载修饰改进了La0.7Ca0.3-Fe0.25Co0.75O3/PPy光催化剂的催化活性。     

中温固体电解质LaGaO3的制备

分别采用固相反应法、凝胶燃烧法分别制备了镓酸镧基固体电解质粉体(La0．9Sr0.1Ga0．8Mg0．2O3-δ)．讨论了煅烧温度对粉体物相的影响,比较了两种方法所制备粉体的特点．X射线衍射分析表明．固相反应法制备需经1250℃下预烧15h,1500℃下煅烧24h．得到La0．9Sr0.1Ga0．8Mg0．2O3-δ粉体颗粒尺寸在1μm,而凝胶燃烧法仅需在1400℃煅烧10h可以合成La0．9Sr0.1Ga0．8Mg0．2O3-δ粉体,粉体颗粒尺寸150nm。     

阴极材料Ba0.5Sr0.5Co0.8Fe0.2O3-σ合成工艺优化

为了在较低温度下合成具有高纯度的阴极材料Ba0.5Sr0.5Co0.8Fe0.2O3-σ(BSCF),采用X射线、扫描电镜以及能谱分析等方法,研究了共沉淀合成法中溶液pH值和煅烧温度等工艺条件对产物的相结构、组成成分和颗粒形貌的影响.结果表明,pH值的升高使前驱体由草酸盐沉淀向氢氧化物沉淀转化,在pH=10条件下,前驱体1100℃煅烧2 h后形成了单一的立方型钙钛矿型结构,比在pH=6条件下的前驱体煅烧温度降低了约100℃,而且成分配比更为准确.研究认为前躯体溶液的pH值对煅烧产物的组成和形貌影响至关重要,这主要是由于pH值的不同改变了前驱体的组成和颗粒形貌造成的.     

钙钛矿型La0.9Sr0.1NiO3催化剂的合成条件及其可见光催化活性的研究

采用溶胶-凝胶法制备了钙钛矿型La0.9Sr0.1NiO3复合氧化物光催化剂,通过TG-DTA、XRD、可见光催化性能等对合成产物的热分解过程、物相结构和可见光催化活性进行了研究;采用单因素实验探究了合成工艺条件(柠檬酸用量、pH值、煅烧温度、煅烧时间)对合成产物的物相结构和可见光催化性能的影响。结果表明,在柠檬酸用量与金属离子的总量比为1∶1,pH=1.5,400℃预处理4h,700℃煅烧4h时可制备出单一相的六方晶系的La0.9-Sr0.1NiO3晶体;在500 W氙灯的照射下,当La0.9Sr0.1NiO3催化剂用量为1.20g/500mL时,在180min内对13.2mg/L的甲基橙溶液的脱色率达到62.1%。     

Synthesis,characterization and formaldehyde gas sensitivity of La0.7Sr0.3FeO3 nanoparticles assembled nanowires

La_0.7Sr_0.3FeO₃ nanoparticles assembled nanowires were synthesized by a hydrothermal method assisted with cetyltrimethylammonium bromide (CTAB). The hydrothermal temperature was 180 °C and the annealed temperature was 700 °C. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to characterize the morphology, composition and structural properties of the materials. The results showed that the La_0.7Sr_0.3FeO₃ nanoparticles assembled nanowires had a high aspect ratio (the largest aspect ratio >100); the size of the nanoparticles was about 20 nm and the diameter of the nanowires was about 100–150 nm. The growth mechanism of La_0.7Sr_0.3FeO₃ nanowires was discussed. Gas sensors were fabricated by using La_0.7Sr_0.3FeO₃ nanowires. Formaldehyde gas sensing properties were carried out in the concentration range of 0.1–100 ppm at the optimum operating temperature of 280 °C. The response and recovery times to 20 ppm formaldehyde of the sensor were 110 s and 50 s, respectively. The gas sensing mechanism of La_0.7Sr_0.3FeO₃ nanowires was investigated.     

Exchange coupling and exchange bias in La0.7Sr0.3MnO3-SrRuO3 superlattices

La(0.7)Sr(0.3)MnO(3)-SrRuO(3) superlattices with and without nanometrically thin SrTiO(3), BaTiO(3) and Ba(0.7)Sr(0.3)TiO(3) interlayers were grown by pulsed laser deposition. Transmission electron microscopy studies showed coherent growth of La(0.7)Sr(0.3)MnO(3), SrRuO(3) and SrTiO(3) layers with atomically sharp interfaces, even if individual layers were as thin as one or two unit cells. In contrast, misfit dislocations and unit cell high interfacial steps were observed at the interfaces between BaTiO(3) and one of the ferromagnetic layers. The presence of the interlayers as well as these extended defects had a significant influence on the magnetic properties of the superlattices, especially on the antiferromagnetic interlayer exchange coupling between the La(0.7)Sr(0.3)MnO(3) and SrRuO(3) layers and the exchange biasing. Surprisingly, exchange biasing was found to increase with decreasing strength of the antiferromagnetic interlayer exchange coupling. This was explained by different magnetization reversal mechanisms acting in the regimes of strong and weak interlayer exchange coupling.     

纳米晶La_(1-x)Sr_xFeO_3薄膜的制备与表征

采用Sol－gel工艺在石英玻璃和硅衬底上成功地制备了纳米晶La1-xSrxFeO3（x=0～0．4）系列薄膜，薄膜为钙钛矿结构，平均粒度在30nm左右。XPS结果表明，随着Sr含量的增大薄膜表面吸附氧含量增大。     

Microwave assisted hydrothermal synthesis and magnetocaloric properties of La0.67Sr0.33MnO3 manganite

We report microwave assisted hydrothermal synthesis and magnetocaloric properties of La0.67Sr0.33MnO3 manganite. The synthesized La0.67Sr0.33MnO3 nanoparticles was characterized using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS) and magnetization measurements. The XRD results indicated that La0.67Sr0.33MnO3 nanoparticles have polycrystalline nature with monoclinic structure. FE-SEM results suggested that La0.67Sr0.33MnO3 nanoparticles are assembled into rod like morphology. Magnetization measurements show that La0.67Sr0.33MnO3 nanoparticles exhibit transition temperature (Tc) above room temperature. The maximum magnetic entropy change (deltaS(M))max was found to be 0.52 J/kg K near Tc approximately 325 K at applied magnetc field of 20 kOe. This compound may considered as potential material for magnetic refrigeration near room temperature.     

微波辅助Sol-gel法制备La0.7Ca0.3CrO3-δ超细粉体及其烧结性能的研究

铬酸镧是最有希望的固体氧化物燃料电池陶瓷连接材料,但存在空气中烧结活性差、中温电导率低等缺陷。利用微波辅助Sol-gel工艺成功制备了La0.7Ca0.3CrO3-δ高活性超细粉体,粉体粒径分布集中,900℃煅烧后的粉体在1400℃空气中烧结4h获得了高达96.3%的相对密度。烧结体具有优良的电导性能,850℃达到63.6S/cm,远高于文献报道值,完全能够满足中温燃料电池(IT-SOFCs)的使用要求。     

CeO_2掺杂对La_(0.7)Ca_(0.3)CrO_(3-δ)低温烧结及电导性能的影响

LaCrO3基固体氧化物燃料电池(SOFC)连接材料存在难以在空气中致密化烧结、中温电导率差等缺陷。本文利用自燃烧工艺(auto-ignition process)制备La0.7Ca0.3CrO3-δ高活性粉体,掺入2%～8%(质量分数)CeO2作为烧结助剂,在1 400℃空气气氛下烧结获得了95.4%以上的高致密度,并且随着CeO2掺杂量的增加晶粒逐渐细化;掺入2%CeO2时La0.7Ca0.3CrO3-δ烧结样品的电导率最高,在空气中850℃达到52.7Scm-1,500℃时也能达到41.9Scm-1,约为同等条件下未掺杂La0.7Ca0.3CrO3-δ电导率的2.5倍,完全能够满足中温固体氧化物燃料电池连接材料的使用要求。     

A precursor nanowire templated route to CdS nanowires

We report the synthesis of the Cd-cysteine precursor nanowires using CdCl₂·2.5H₂O, L-cysteine and ethanolamine in the solvent of water at room temperature. The average diameter and lengths of Cd-cysteine precursor nanowires are 200 nm and several hundred microns, respectively. The precursor nanowires are used as the source materials for cadmium and sulfur and the template for the subsequent preparation of CdS nanowires using ethylene glycol as the solvent by a solvothermal method at 200 °C. The formation process of CdS nanowires is discussed. The samples are characterized using X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy and Fourier transform infrared spectroscopy.     

Grain boundary analysis and secondary phases in LaCoO3-based perovskites

Secondary phases and grain boundaries in LaCoO₃ and La_0.7Sr_0.3CoO_3−δ ceramics have been studied by transmission electron microscopy. Both materials contained small amounts of grains of a secondary phase; the face centered cubic spinel structure Co₃O₄, located at triple junctions. These grains were agglomerates of several smaller grains. High resolution electron microscopy combined with annular dark field scanning transmission electron microscopy and electron energy loss spectroscopy were used to analyze the grain boundaries. In LaCoO₃, the grain boundaries were sharp with stable compositions of La, Co and O across the boundaries. In La_0.7Sr_0.3CoO_3−δ, a 1–2 nm thick intergranular layer between the grains was observed. This layer was rich in O and Co and deficient in Sr and La, compared to the nominal composition of the material.     

Preparation and characterization of SiC nanowires and nanoparticles from filter paper by sol–gel and carbothermal reduction processing

The carbothermal reduction of SiO₂ gel containing filter paper (as carbon precursors) in argon was used to prepare SiC nanowires and nanoparticles. The resulting SiC ceramic, as well as the conversion mechanism of carbon/silica composites to SiC nanowires and nanoparticles, have been investigated by scanning electron microscopy (SEM), Transmission electron microscopy (TEM), x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TG) techniques. XRD and IR studies show that the materials, obtained from reaction at 1550 °C for 1 h in static argon atmosphere, are β-SiC. SEM and TEM reveal that SiC nanowires is single crystal wires with diameters ranging from 50–200 nm and their lengths over several tens of microns. According to thermodynamic analysis, SiC nanowires and SiC nanoparticles in the resulting SiC ceramic are formed by gas-gas reaction of SiO (g) and CO (g).     

Synthesis and characterization of pure and doped (Na, Ca, Sr) nanograined LaMnO3 magnetoresistive ceramics

Pure and Na, Ca, and Sr doped lanthanum manganites (LaMnO3, La0.85Na0.15MnO3, La0.7Ca0.3 MnO3, La0.7Sr0.3MnO3) were prepared in form of bulk nano-structured materials through a two-step process. Nanometric powders were synthesized by the Pechini method and subsequently densified by Spark Plasma Sintering at 1273 K for 5 minutes under a pressure of 140 MPa. The method allowed the preparation of single phase manganites with a theoretical density above 98% together with a very limited growth of the grain size. Grain sizes below 70 nm were obtained for all materials except La0.85Na0.15MnO3 which showed a much larger grain size. Curie temperatures (Tc) and magnetoresistivity properties of the samples were measured by a Superconducting Quantum Interference Device (SQUID). The decrease in the resistivity below Tc occurred in a much wider range of temperature compared to ceramics having micron-size grains.