La_(0.67)Ca_(0.33-x)Ba_xMnO_3的电输运性质反常及磁电阻温度稳定性

用固相反应法制备La_(0.67)Ca_(0.33-x)Ba_xMn O_3(x=0,0.10,0.15,0.20,0.25)系列样品,烧结温度为1200℃。通过X射线衍射(XRD)图谱,扫描电子显微镜(SEM)照片、零场和加场下的电阻率-温度(ρ-T)曲线,磁电阻-温度(MR-T)曲线,研究Ba~(2+)替代Ca~(2+)的La_(0.67)Ca_(0.33-x)Ba_xMnO_3的电输运性质及磁电阻温度稳定性。结果表明:随Ba~(2+)替代量的改变晶体结构发生变化,x=0的样品为立方结构,x=0.10的样品为正交结构,x=0.15,0.20,0.30的样品为六方结构。x=0.10样品的电输运性质出现反常,它的电阻率不仅比未掺Ba的La_(0.67)Ca_(0.33)Mn O_3高出60倍,也比高掺Ba样品的电阻率高出几倍,随Ba~(2+)替代量的增加电阻率逐渐下降,用掺Ba引起的晶格结构变化及Mn O_6八面体畸变进行解释;高掺Ba样品实现了室温附近磁电阻温度稳定性,x=0.15的样品在187~246 K温区磁电阻为(8.91±0.42)%,x=0.20的样品在230~290 K温区磁电阻为(6.07±0.32)%,x=0.25的样品在320 K以下直至50 K温区磁电阻均大于14%。在0.8 T磁场下在室温附近产生磁电阻的温度稳定性有利于MR效应的实际应用。磁电阻温度稳定性机制是,钙钛矿的磁电阻是体相内双交换作用产生的本征磁电阻与界面自旋相关散射或自旋极化隧穿产生的低场磁电阻的叠加,制备样品时控制烧结温度(1200℃),尽量提高低场磁电阻,两种磁电阻叠加产生磁电阻温度稳定性。     

La_(0.80)Sr_(0.05)Na_(0.15)MnO_3/xCuO复合体电输运机制及磁电阻的温度稳定性

用固相反应法制备了La0.80Sr0.05Na0.15MnO3/xCuO(x=0,0.05,0.10,0.15,0.20,0.30)二相复合体系,通过X射线衍射(XRD)图谱、电阻率-温度(ρ-T)曲线、ρ-T拟合曲线、磁电阻-温度(MR-T)曲线,研究了样品的电输运机制及磁电阻的温度稳定性。结果表明,在低温类金属区,电输运机制是自旋电子受单磁子散射作用,用ρ-T2拟合得很好;在较高温区MR-T曲线出现"压峰效应",是因为界面效应产生的非本征磁电阻占优势,本征磁电阻与非本征磁电阻迭加产生的磁电阻随温度变化不大;特别是x=0.05的样品,0.8 T磁场下在240 K~320K温区,磁电阻保持(9.9±0.4)%基本不随温度变化,在室温附近△T=80 K温区磁电阻的温度稳定性很好。     

CuO复合对La0.80Sr0.05K0.15MnO3电输运和磁电阻的影响

用固相反应法制备了(1-x)La0.80Sr0.05K0.15MnO3/xCuO(x=0.00,0.04,0.08,0.10,0.20,0.30)二相复合体。通过X射线衍射图谱、扫描电子显微镜照片检测结构,表明形成完好的钙钛矿相和CuO相,CuO分布在钙钛矿颗粒之间,形成对钙钛颗粒的包覆。通过测量零场和加场下的电阻率-温度曲线以及磁电阻-温度曲线,研究电输运性质及磁电阻效应,结果表明,CuO复合对La0.80Sr0.05K0.15MnO3电输运和磁电阻效应影响很大。在高温区出现磁电阻峰,表现出本征磁电阻特征,在低温区随温度降低磁电阻持续增大,表现出由界面引起的隧穿磁电阻特征,总的磁电阻是本征磁电阻与隧穿磁电阻的迭加,在中间温区出现磁电阻的温度稳定性。     

改善钙钛矿材料室温下磁电阻效应的有效途径

将Ag2O与La0.67Ca0.25Sr0.08MnO3均匀混合经高温烧结后形成La0.67Ca0.25Sr0.08MnO3/xAg两相复合体系。随Ag掺入量的增加,样品的电阻率明显下降,磁化强度有小量下降,TC及电阻率的峰值温度TP没有明显变化。304K温度下,从x=0.25样品中得到最大磁电阻效应,磁电阻比约为41%,分别是La0.67Ca0.25Sr0.08MnO3和La0.67Sr0.33MnO3样品的1.6及10倍。磁电阻的本征效应和传导电子在界面处的自旋相关散射作用是产生室温下增强磁电阻效应的主要原因。结果说明,利用离子的掺杂效应调整居里温度到室温附近,再结合金属/钙钛矿复合体系界面属性丰富的特性来制备庞磁电阻材料是提高室温磁电阻有效的途径,这对应用研究具有十分重要的意义。     

La2/3Ca1/3MnO3/xTiO2复合磁性材料的磁电特性研究

采用溶胶-凝胶法制备La2/3Ca1/3MnO3纳米级磁性颗粒和TiO2胶体,按一定比例制成La2/3Ca1/3MnO3/xTiO2(其中x取0、0.1、0.2、0.3、0.4)复合磁电阻材料。用XRD谱确定样品的晶体结构。采用振动样品磁强计测量了样品的磁滞回线和场冷却磁化强度随温度的变化行为;采用标准四引线法测量样品在恒定磁场下的电阻率随温度的变化。实验测量结果表明体系的磁化强度、剩磁、矫顽力随TiO2含量的变化具有相似的规律,具有室温的居里温度;并且当磁场强度小于0.4T时,磁电阻与磁场平方成正比关系;当大于0.6T时,磁电阻与磁场成线性关系。     

非化学计量(La0.6Dy0.1Sr0.3)1-xMnO3的电输运及MR温度稳定性机制研究

用固相反应法制备了非化学计量的(La0.6Dy0.1Sr0.3)1-xMnO3(x=0.00,0.10,0.20,0.30,0.35)系列样品,通过XRD、ρ-T曲线、MR-T曲线,研究电输运及磁电阻(MR)温度稳定性的机制。XRD检测表明,非化学计量的(La0.6Dy0.1Sr0.3)1-xMnO3在1200℃下烧结24 h,实际形成了La0.6Dy0.1Sr0.3MnO3钙钛矿相和Mn2O3相组成的二相复合体材料。电输运性质均表现出绝缘体-金属相变,ρ-T曲线高温区出现尖峰,较低温区出现"肩峰",是钙钛矿体相内双交换作用和晶界处电子自旋极化隧穿引起的电阻率共同作用的结果。MR-T表现出,在高温区出现磁电阻峰,在低温区随温度降低磁电阻持续增大,表现出低场磁电阻特征,在中间温区出现磁电阻的温度稳定性,用La0.6Dy0.1Sr0.3MnO3钙钛矿颗粒体相产生的本征磁电阻与颗粒界面效应产生的隧穿磁电阻的叠加给出解释。x=0.30的样品,0.8 T磁场下,在258 K～198 K温区,产生的磁电阻为(6.3±0.2)%。     

La2/3(Ca60Ba40)1/3MnO3的磁电阻与磁化强度及其相关性

用固相反应法制备了La2/3(Ca60Ba40)1/3MnO3多晶材料,测量了77K～320K范围内的磁化曲线及在77K～350K范围内0～1.0T外磁场下的电阻率。结果表明低场磁电阻与高场磁电阻随外磁场的变化与磁化强度(M2)的变化存在着一定相关性,采用ρ(M)∝1-M2及低温隧穿磁电阻效应和逾渗模型解释了实验结果。     

(1-x)La0.6Dy0.1Sr0.3MnO3/0.5x(Sb2O3)复合体系的电输运性质及低场磁电阻效应

用固相反应法制备了(1 -x)La0.6Dy0.1Sr0.3MnO3/0.5x( Sb2 O3)系列样品,通过电阻率-温度(ρ-T)曲线以及ρ-T拟合曲线,研究了样品的电输运性质,电输运机制及低场磁电阻效应.结果表明:所有样品在高温区表现为绝缘体导电,在低温区表现为金属导电,产生绝缘体-金属相变;在金属导电区主要是单磁子散射起作用,可以用公式ρ=ρ0+AT拟合;所有样品在整个温区随温度降低MR持续增大,表现出低场磁电阻特征,复合样品的磁电阻(MR)与纯的La0.6Dy0.1Sr0.3 MnO3的MR相比,在低温区减小,在高温区增大,对x=0.15的样品在高温区的MR大幅度提高,当B=0.2 T,T=300 K时,MR达7.79％,比纯La0.6Dy0.1 Sr0.3 MnO3的MR增大2.6倍,有利于MR的实际应用.     

YAG:Ce3+荧光粉制备技术的研究进展

综述了白光LED用YAG:Ce3+黄色荧光粉多种制备技术的新进展,包括固相反应法、溶胶-凝胶法、喷雾干干燥法、燃烧法、共沉淀法、共沉淀-熔盐法等,并对这些方法的优缺点进行了综合比较,展望了该领域的发展前景及研究趋势.     

La_(0.5)Sm_(0.2)Sr_(0.3)MnO_3/Ag_x二相复合体的结构及磁电阻

用固相反应法制备La0.5Sm0.2Sr0.3MnO3/(Ag2O)x/2(x=0.00,0.04,0.08,0.25,0.30)样品,通过X射线衍射谱线(XRD),扫描电子显微镜(SEM)照片及SEM能谱(EDS),ρ-T曲线,研究样品的输运行为及磁电阻效应。结果表明:少量掺杂时Ag全部挥发。掺杂量较多时,挥发后多余的Ag主要以金属态包覆在母体颗粒的表面,使体系形成两相复合体。掺Ag为30%摩尔比时,样品的电阻率较低掺杂样品的电阻率降低一个数量级,在300K、0.5T磁场下,磁电阻明显增强,达到9.4%,这与颗粒母体界面结构的改善有关,也与材料电阻率的降低有关。     

钛酸锶钡陶瓷的制备及介电性能

采用固相法和溶胶凝胶法制备钛酸锶钡(BaxSr1 xTiO3,BST)粉末,用X射线分析仪(XRD)和扫描电镜(SEM)分析2种方法制备的BST粉末的物相组成和显微形貌。固相法和溶胶凝胶法所得粉末制备的压坯分别在1 400℃和1 300℃烧结2 h得到BST陶瓷,用密度分析仪、扫描电镜(SEM)和阻抗分析仪对BST陶瓷的密度、断口显微形貌和介电性能进行分析,研究不同Ba/Sr比例和2种不同粉末颗粒尺寸对BST陶瓷介电性能的影响。结果表明:室温下,BaxSr1 xTiO3(x=0.5,0.6)为立方相,BaxSr1 xTiO3(x=0.7,0.8)为四方相;固相法粉末制备的BaxSr1 xTiO3(x=0.5,0.6,0.7,0.8)陶瓷的密度、颗粒尺寸和介电常数峰值均随Ba含量的增加而增加,居里温度随Ba含量的增加呈线性增加,线性拟合得到Tc=221.6+354x,BST陶瓷的介电常数随频率的增加而降低;与固相法粉末制备的BST陶瓷相比,溶胶凝胶法粉末制备的BaxSr1 xTiO3(x=0.5,0.6)陶瓷密度较高,但同时出现介电峰弥散,介电常数和介电损耗较低。     

柠檬酸盐溶胶—凝胶法合成Li1＋2xZn1—xPO4及其离子导电性

采用柠檬酸盐溶胶-凝胶法制备了组成为Li     

Synthesis of Long Afterglow Phosphor CaAl2Si2O8:Eu2+, Dy3+ via Sol-Gel Technique and Its Optical Properties

The long afterglow phosphor CaAl2Si2O8:Eu2 , Dy3 was prepared by a sol-gel method. The sol-gel process and the structure of the phosphor were investigated by means of X-ray diffraction analysis (XRD). It is found that the single anorthite phase formed at about 1000 ℃, which is 300 ℃ lower than that required for the conventional solid state reaction. The obtained phosphor powders are easier to grind than those of solid state method and the partical size of phosphor has a relative narrow distribution of 200 to 500 nm. The photoluminescence and afterglow properties of the phosphor were also characterized. An obvious blue shift occurs in the excitation and emission spectra of phosphors obtained by sol-gel and solid state reaction methods. The change of the fluorescence spectra can be attributed to the sharp decrease of the crystalline grain size of the phosphor resulted from the sol-gel technique.     

Effect of sintering temperature on morphology and arc erosion properties of La-Ni-O ceramic and its composites

Ceramic LaNiO3 samples were prepared by solid state reaction method at different sintering temperatures. It was found that the resultant was not ABO3 perovskite single phase but dual phase La2NiO4 and NiO, and the percentage of the two phases varied with sintering temperature. Ceramics sintered at 1400 ℃ were well crystallized and the phase ratio of La2NiO4 was the maximum. The surface morphology observed by scanning electron microscopy (SEM) indicated that the grains of the ceramics sintered at 1400 ℃ were uniform and compact, which were in agreement with the properties of high density and low electrical resistivity of the samples. X-ray diffraction (XRD) patterns of ceramics before and after arc erosion indicated their high structural stability, which resulted in the good arc erosion resistance properties for silver-based electrical contact materials. The contact materials prepared with the ceramic sintered at 1400 ℃ exhibited better mass transition and arc erosion resisting properties.     

SrAl2O4 :Eu2+, Dy3+ Long Afterglow Phosphors Prepared by Chemical Coprecipitation Method

SrAl2 O4: Eu2 , Dy3 long afterglow phosphors were prepared by chemical coprecipitation method. Ammonium carbonate and ammonium hydrogen carbonate were used as the precipitants. The preparation of the SrAl2 O4: Eu2 ,Dy3 precursor was completed at room temperature by controlling the concentration of the metal-salt solution, pH value of the system, etc. The phosphors were prepared by sintering the precursor at 1000 ～ 1200 ℃ in a weak reducing atmosphere for 2 h. The XRD, SEM, excitation spectra, emission spectra and afterglow decay of the samples were tested and the optimal synthesis conditions of the SrAl2O4: Eu2 , Dy3 long afterglow phosphors prepared by precipitation method were determined. The phosphor which had good luminescent properties is prepared and its persistent time can reach more than 1600 min. In the coprecipitation process, a small amount of glucose operates to refe the luminescent powders. The particle size of the phosphor can be less than 1 μm. The sintering temperature of the sample prepared by the coprecipitation method is much lower than that of the one prepared by the high temperature solid state method.Compared with the high temperature solid state method, a clear blue shift occurs in the excitation and emission spectra of the samples.     

Catalytic combustion study of soot on Ce0.7Zr0.3O2 solid solution

The Ce0.7Zr0.3O2 solid solution and CeO2 were prepared using the sol-gel method. The phase structure, crystallite sizes and the reducibility of the catalysts were characterized by XRD and H2-TPR techniques. XRD results indicated that Zr^4＋ had replaced part of Ce^4＋ to form a fluorite-like solid solution, which was favorable to obtain ultrafine nanoparticles. The ratio of main HE consumption for Ce0.7Zr0.3O2：CeO2 was 4.4：1.0, implying that the solid solution could improve the reducibility compared to the single CeO2. The Ce0.7Zr0.3O2 solid solution catalyst showed a sharp combustion peak at 397 ℃, which was 200 ℃ lower than that of the single soot. The good catalytic activity of the Ce0.7Zr0.3O2 was attributed to the formation of nano-CeO2-based solid solution, which enhanced the reducibility and then improved the combustion activity. As Ce0.7Zr0.3O2 could be easily reduced to Ce0.7Zr0.3O2-x meanwhile, after oxygenation, the Ce0.7Zr0.3O2.x was recovered to Ce0.7Zr0.3O2 completely. A catalytic combustion reaction mechanism was proposed： the Ce0.7Zr0.3O2 was reduced to Ce0.7Zr0.3O2-x by the reaction with carbon and then it was recovered to Ce0.7Zr0.3O2-x by the interaction with O2.     

低温燃烧法制备Ce_(0.8)Sm_(0.2)O_(1.9)电解质固溶体及其烧结性能的研究

采用柠檬酸–硝酸盐低温燃烧合成法,以Ce(NO_3)_3·6H_2O为氧化剂,柠檬酸为还原剂,制备Sm_2O_3掺杂的Ce_(0.8)Sm_(0.2)O_(1.9)(SDC)超细粉体,利用XRD、TG-DSC、FT-IR、SEM及FESEM等手段对制备样品的晶相结构、热分解过程、微观形貌以及团聚情况进行研究.结果表明:柠檬酸与硝酸盐组成的干凝胶自蔓延燃烧点火温度为270.0℃;粉体经600℃焙烧2 h后,形成了单一立方萤石型结构的固溶体,平均晶粒度为18.80 nm.粉体的结晶性能完善,分散性能良好,粒子间仅有微弱的软团聚.将素坯在1 250℃烧结2 h,即可得到相对密度为95.5%的陶瓷烧结体.     

烧结温度对LiNi0.8Co0.15Al0.05O2结构和电化学性能的影响

采用共沉淀法+高温固相法,首次在740~820℃制备了一系列LiNi_0.8Co_0.15Al_0.05O₂正极材料,探讨温度变化对材料结构性能的影响.通过X射线分析仪、扫描电镜、电化学工作站、电池充放电测试系统表征材料性能.结果显示在780℃烧结出的材料有纯的六方晶相、层状结构优异,在2.75~4.2 V、0.1 C倍率获得188.11 mAh/g,0.5 C循环100次后容量稳定率为88.55 %,高于其他温度制备的材料; 经过不同倍率放电后,780℃烧结出的材料不可逆容量损失远低于其他温度制备的材料.      

溶胶-原位凝胶法制备金刚石/LZAS系陶瓷结合剂砂轮的结构与性能

以硝酸盐溶液、磷酸铵溶液、Si O2溶胶和金刚石颗粒制成混合料浆,经快速凝胶及干燥后,在850℃/1.5 h条件下烧结,得到金刚石/陶瓷结合剂复合体,通过对其微观结构以及表面粗糙度、抗弯强度和孔隙率等性能进行表征,研究混合料浆中的固相含量对金刚石/复合氧化物陶瓷复合体结构与性能的影响。结果表明:Si O2-Al2O3-Zn O-Na2O-Li2O-P2O5复合氧化物陶瓷结合剂的晶化程度高,晶型完整;随料浆中固含量增加,金刚石/陶瓷复合体的孔隙率先降低后升高,而抗弯强度则先升高后降低,当固含量(体积分数)为60%时,砂轮的孔隙率和抗弯强度分别达到最小值(26.2%)和最大值(69 MPa)。与传统粉末压制法制备的金刚石/复合陶瓷结合剂砂轮相比,采用溶胶-凝胶原位法制备的砂轮,结构均匀,抗弯强度和孔隙率分别提高约40.5%和34.8%,磨削加工的硬质合金工件表面无较深划痕,工件表面粗糙度为0.049μm。     

SiO_2∶Eu~(3+)的制备与发光性能研究

以三氧化二铕和正硅酸乙酯为原材料,利用溶胶-凝胶法、高温机械力化学法合成了SiO_2∶Eu~(3+)粉体.用X射线衍射(XRD)、扫描电镜(SEM)表征了材料的结构和形貌,采用激发光谱、发射光谱对荧光粉体的发光性能进行了测量.结果说明:溶胶-凝胶法、高温机械力化学法合成样品的发光性能随着热处理温度的增加先增强后减弱,分别在900℃和600℃达到最好,粉体平均粒度分别为2μm与1μm.与溶胶-凝胶法比较,高温机械力化学法的制备温度降低了300℃.且利用高温机械力化学法制备的样品的发光性能要好于溶胶-凝胶法制备的样品.