Mn1-xZnxFe2O4 (0≤x≤1)纳米粉体的模板辅助溶胶凝胶法制备及其磁性能研究

通过模板辅助溶胶-凝胶法制备了一系列的Mn_1-xZn_xFe₂O₄(0≤x≤1,步长为0.2)纳米粉体。利用XRD和VSM对材料的物相和磁性能进行了表征,主要研究了Mn_1-xZn_xFe₂O₄分子式中Zn含量的变化对样品的微观结构和磁性能的影响。实验结果表明,具有不同Zn含量的Mn_1-xZn_xFe₂O₄样品均为尖晶石结构;随着Zn含量的增加,样品的晶面间距d、平均晶粒尺寸D、饱和磁化强度M_s和居里温度T_c都呈现出下降的趋势,而样品的矫顽力H_c则呈现出先升高后降低的趋势。分析认为,M_s的下降可以用Yafet-Kittel倾角理论解释,T_c的降低归因于晶格中反铁磁性耦合的降低,而H_c的变化则主要是由于材料的磁晶各向异性常数K₁的变化引起的。     

钙钛矿型La1-xSrxCoO3-δ粉体的制备及其在银基电接触材料中的应用

采用溶胶-凝胶法和粉末冶金工艺分别制备了颗粒状和网孔状La_0.5Sr_0.5CoO_3-δ(LSCO)粉体及其Ag-LSCO电接触复合材料。优化了溶液pH,溶胶预处理温度等工艺对LSCO粉体微结构的影响,并考察成型压力,烧结温度等对Ag-LSCO材料电学、力学性能的影响研究。采用扫描电镜、X-射线衍射仪、D60K数字金属电导率测量仪和HVS-1000型数显显微硬度计等对LSCO粉体及Ag-LSCO电接触材料进行了微观形貌、物相结构、电导率与硬度等性能表征。结果表明：以柠檬酸为单一胶凝剂,当pH为9.5,在700℃烧结8h可获得颗粒状LSCO_p粉体;而以柠檬酸和EDTA为复合胶凝剂时,于前驱体溶液pH=9.5,溶胶预处理温度200℃,烧结温度700℃,8h条件下合成网孔块体结构的LSCO_w粉体。经成型压力及烧结制度的优化结果可知,成型压力(1100MPa)、烧结温度900℃,6h 为制备Ag/LSCO_w电接触材料的最佳工艺参数。相比于Ag-LSCO_p电接触复合材料,Ag-LSCO_w表现出更低的电阻率(2.5μΩcm)。     

溶胶-凝胶法制备La1-xSrxMnO3及其电磁性能研究

采用溶胶凝胶法,制备了La_1-xSr_xMnO₃(LSMO)纳米微粉。探究了Sr^₂₊的掺杂量对LSMO晶体结构、磁学性质、电磁特性和微波吸收性能的影响。结果表明,随Sr^₂₊含量的升高,样品的晶格常数和Mn-O-Mn键角增大,平均晶粒尺寸逐渐下降,样品出现从反铁磁性向铁磁性的转变,复介电常数呈先增大后减小的趋势。在2~18GHz内,x=0的样品在厚度为2mm时有最佳吸波效果,反射率小于-10dB对应的有效吸波频段为12.5~18GHz;Sr^₂₊的掺杂可使吸波频段有效的向低频移动,在X波段内,x=0.2的样品在厚度为2.3mm时的有效带宽达2.6GHz,证明LSMO是一种性能优异的介电损耗型吸波材料。     

NiMoO4/g-C3N4的制备及电化学性能研究

超级电容器具有比电容高、循环寿命长和绿色无污染的特点,其优异的电化学性能备受关注。本文水热合成了NiMoO₄/g-C₃N₄复合粉体,并将粉体涂覆在泡沫镍上制备了NiMoO₄/g-C₃N₄电极材料。结果表明,NiMoO₄/g-C₃N₄粉体形貌主要为NiMoO₄纳米棒和团状g-C₃N₄,且NiMoO₄纳米棒生长在g-C₃N₄纳米片上。在NiMoO₄中加入30at%的g-C₃N₄能降低电容体系的等效串联电阻和扩散阻抗,有利于氧化还原反应的进行。相比于其他g-C₃N₄含量的电极材料,g-C₃N₄含量为30at%的NiMoO₄/g-C₃N₄电极材料具有更高的比电容(584.3F/g)和更好的倍率特性。     

废旧锂离子电池中Li, Fe和V的回收及xLiFePO4-yLi3V2(PO4)3的制备

由于LiFePO_4和Li_3V_2(PO_4)_3材料的特征相近,制备方法类似,提供了一种从废旧LiFePO_4和Li_3V_2(PO_4)_3混合电池中回收Li、Fe和V,再制备xLiFePO_4-yLi_3V_2(PO_4)_3的方法。在空气气氛中600℃热处理1h后,去除粘结剂PVDF使活性物质与集流体分离。调节Li、Fe、V和P摩尔比,球磨、锻烧,配制不同比例的xLiFePO_4-yLi_3V_2(PO_4)_3(x:y=5:1,7:1,9:1)复合电极材料。表征了其形貌、结构和电化学性能,结果表明,回收制备的复合材料将同时具备LiFePO_4和Li_3V_2(PO_4)_3两种材料的电化学性能,能显著改善LiFePO_4的倍率性能。     

Cr3+掺杂LiNi0.5Mn1.5O4材料的制备及性能研究

采用高温固相法合成了Cr₃₊掺杂的LiNi_0.5Mn_1.5O₄正极材料,研究了掺杂量对材料物理性能和电化学性能的影响。利用XRD、SEM对材料的结构和形貌进行了表征,结果显示样品具有棱边清晰的尖晶石形貌。讨论了不同Cr₃₊掺杂量对LiCr_xNi_0.5-0.5xMn_1.5-0.5xO₄(x=0,0.05,0.1,0.15,0.2)正极材料性能的影响。充放电测试、循环伏安和交流阻抗测试结果表明：当Cr₃₊的掺杂量为x=0.1时(LiCr_0.1Ni_0.45Mn_1.45O₄)正极材料的性能最好,0.1C、0.5C、1C、2C及5C的首次放电比容量依次为131.54mAh g_-1、126.84mAh g_-1、121.28mAh g_-1、116.49mAh g_-1和96.82mAh g_-1,1C倍率下循环50次,容量保持率仍为96.5%。     

水热法制备C3N4/CuGaO2 复合物及其气敏性能

采用简单水热法合成了一系列C₃N₄/CuGaO₂复合材料。采用XRD、SEM、TEM和XPS对制备的样品进行了表征。研究了一系列C₃N₄/CuGaO₂复合材料的气敏性能。结果表明,基于C₃N₄/CuGaO₂-0.3复合材料（C₃N₄与CuGaO₂的摩尔比为0.3:1）的气体传感器对甲苯的传感性能优于CuGaO₂传感器。相比较于CuGaO₂传感器的工作温度（140 ℃）,C₃N₄/CuGaO₂-0.3复合材料传感器的最佳工作温度仅为25 ℃,对100 μL/L甲苯气体的响应达到28,检出限低至0.01 μL/L。对100 μL/L甲苯气体的响应时间和恢复时间分别为114.2和27.4 s。此外,用于检测甲苯的C₃N₄/CuGaO₂-0.3复合材料传感器还具有优异的长期稳定性、良好的重复性和优异的抗湿性能。     

过锂量对富锂锰基正极材料Li1.2xNi0.1Co0.2Mn0.5O2结构与电化学性能的影响

采用流变相法合成得到Li_(1.2+x)Ni_(0.1)Co_(0.2)Mn_(0.05)O_2(x=0, 0.036, 0.060, 0.096),探讨过锂量对结构和电化学性能的影响。X射线衍射(XRD)对样品进行结构分析证明所有样品具有典型的α-NaFeO_2结构和较小的阳离子混排度。扫描电镜(SEM)对样品进行表征证明不同过锂量的材料,颗粒相对均匀,表面光滑。电化学性能测试结果表明:最佳过锂量为x=0.036时,正极材料Li_(1.236)Ni_(0.1)Co_(0.2)Mn_(0.5)O_2在0.05C、2～4.8V测试条件下进行电化学性能测试,25和55℃下该材料初始放电容量分别为215.3和297.1 mAh·g-1,首次库伦效率分别为66.6%和84.6%,0.2 C下循环50次后容量保持率分别为89.0%和87.8%,且x=0.036时该材料具有最佳的倍率性能。     

Ni2Cr(BO3)O2涂层的制备及其红外发射性能

通过喷雾造粒和高温焙烧制备Ni_2Cr(BO_3)O_2粉末后利用等离子喷涂得到一种高红外发射涂层,并研究了该种涂层的红外发射性能。SEM观察涂层的表面、断面形貌,发现涂层与基体结合紧密、无脱落;XRD对焙烧后的粉末物相组成进行了表征,主要以Ni_2Cr(BO_3)O_2为主。对涂层红外波段发射率的测试表明,在0.76~2.5μm波段的发射率为0.896、2.5~14μm波段发射率为0.925,具有优异的红外发射性能。Ni_2Cr(BO_3)O_2晶胞内的畸变、非对称性以及电子转移跃迁是导致Ni_2Cr(BO_3)O_2这种材料具有高红外发射率的主要原因。Ni_2Cr(BO_3)O_2涂层能够经受37次"900℃~水冷"热震循环。该种涂层由于其高红外发射性能、优异的耐热震性能和热稳定性能而具有较高的实用价值。     

锆盐原料不同对LiZr2(PO4)3锂离子固体电解质结构及性能的影响

以不同的锆盐为原料,采用固相法及液相法制备LiZr_2(PO_4)_3锂离子固体电解质,通过无压烧结的方式制备得到固体电解质片,并通过X射线衍射(XRD),扫描电子显微镜(SEM),电化学交流阻抗(EIS)对LiZr_2(PO_4)_3锂离子固态电解质进行表征,通过测试结果对比分析,研究锆盐原料的不同对LiZr_2(PO_4)_3锂离子固态电解质结构及性能的影响。结果表明:当以醋酸锆为锆盐原料时,合成的LiZr_2(PO_4)_3以高电导率的菱方相于室温下稳定存在,而其他3种锆盐作原料时合成的LiZr_2(PO_4)_3室温下以三斜相存在。制备的菱方相LiZr_2(PO_4)_3电解质样品片室温锂离子总电导率最大,为2.25×10~(-5) S/cm,且激活能值最小,为0.28 eV。     

固相-水热法制备LiFePO4-Li3V2（PO4）3复合材料及其电化学性能（英文）

分别采用固相-水热法和球磨法制备磷酸亚铁锂-磷酸钒锂复合正极材料(LiFePO4-Li3V2(PO4)3)。电化学性能测试表明,LiFePO4-Li3V2(PO4)3复合正极材料的电化学性能远远高于 LiFePO4和 Li3V2(PO4)3单独作为正极材料的性能,并且以固相-水热法制备的复合材料性能优于以球磨法制得的复合材料。研究发现 LiFePO4-Li3V2(PO4)3复合材料有 4 个氧化还原峰,相当于 LiFePO4 和 Li3V2(PO4)3 氧化还原峰的叠加。采用固相-水热法制备的LiFePO4-Li3V2(PO4)3 复合材料形貌较为规则,且有新相物质产生,这是导致其电化学性能较好的原因。     

Structural and electrical properties of Gd(Ni1/2Zr1/2)O3

The Gd(Ni_1/2Zr_1/2)O₃ (GNZ) ceramic is synthesized by the solid-state reaction technique. The X-ray diffraction pattern of the sample shows monoclinic phase at room temperature. The dielectric dispersion of the material is investigated in the temperature range from 303 K to 673 K and in the frequency range from 100 Hz to 1 MHz. The relaxation peak is observed in the frequency dependence of the loss tangent. The relaxation time at different temperatures is found to obey Arrhenius law having activation energy of 1.1 eV which indicates the hopping of ions at the lattice site and may be responsible for the dielectric relaxation of GNZ. The scaling behaviour of loss tangent suggests that the relaxation mechanism is temperature independent. The frequency dependent conductivity spectra follow the power law. In the impedance formalism, the Cole-Cole model is used to study the relaxation mechanism of GNZ.     

LaSrCuO4粉体微结构对Ag/LSCO电接触材料性能的影响

以硝酸镧、硝酸铜、硝酸锶等为原料,分别采用固相法、溶胶-凝胶法和共沉淀法合成了不规则颗粒状(LSCO_g)、介孔状(LSCOm)和片层状(LSCOl)的LaSrCuO_4(LSCO)粉体。采用高能球磨并结合初压-初烧-热压工艺制备出Ag/LSCO电接触材料。利用X射线衍射(XRD)、扫描电镜(SEM)、金属电导率仪、维氏硬度计和电寿命试验机等对粉体形貌及电接触材料的物理和电学性能进行了表征。结果表明:与Ag/LSCO_(m)、Ag/LSCO_l材料相比,Ag/LSCO_(g)电接触材料表现出更加优异的物理性能,其电阻率为2.37μΩ·cm,硬度为800MPa,密度为9.32g/cm~3;但电学性能差异较小,其在AC220V12A开断状态下的燃弧能量为400 mJ、燃弧时间为23 ms,关合状态下的燃弧能量为1500 mJ,燃弧时间为68ms。Ag/LSCO电接触材料的主要失效形式是液滴喷溅,微裂纹和孔洞。     

Preparation and characteristic of spherical Li3V2(PO4)3

Spherical Li₃V₂(PO₄)₃ was synthesized by using N₂H₄ as reducer. The products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that single-phase, spherical and well-dispersed Li₃V₂(PO₄)₃ has been successfully synthesized in our experimental process. Electrochemical behaviors have been characterized by charge/discharge measurements. The initial discharge capacities of Li₃V₂(PO₄)₃ were 123 mAh g⁻¹ in the voltage range of 3.0–4.3 V and 132 mAh g⁻¹ in the voltage range of 3.0–4.8 V.     

Synthesis and phosphorescence properties of Mn, La and Ho in MgAl2Si2O8

Mn⁴⁺, La³⁺ and Ho³⁺ doped MgAl₂Si₂O₈-based phosphors were first synthesized by solid state reaction. They were characterized by thermogravimetry (TG), differential thermal analysis (DTA), X-ray powder diffraction (XRD), photoluminescence (PL) and scanning electron microscopy (SEM). The phosphors were obtained at about 1300 °C. They showed broad red and fuchsia-pink emission bands in the range of 610-715 nm and had a different maximum intensity when activated by UV illumination. Such a fuchsia-pink emission can be attributed to the intrinsic d-d transitions of Mn⁴⁺.     

Effects of precipitator on the morphological, structural and electrochemical characteristics of Li[Ni1/3Co1/3Mn1/3]O2 prepared via carbonate coprecipitation

Three precipitators, i.e. Na₂CO₃, (NH₄)₂CO₃ and NH₄HCO₃, are employed to prepare Li[Ni_1/3Co_1/3Mn_1/3]O₂ via the carbonate coprecipitation method. The effects of precipitator on the morphological, structural and electrochemical characteristics of the prepared samples are studied. The sample prepared by using Na₂CO₃ as precipitator has irregular particle shape and nonuniform particle size, while the sample prepared by using (NH₄)₂CO₃ as precipitator has spherical particle shape and uniform particle size. Among all the samples, the one prepared with (NH₄)₂CO₃ exhibits the best hexagonal layered structure, which results in its highest discharge capacity and best cycling performance. Therefore, precipitator plays an important role in the coprecipitation reaction and makes a great impact on the characteristics of Li[Ni_1/3Co_1/3Mn_1/3]O₂.     

Effect of the impurity LixNi1−xO on the electrochemical properties of 5 V cathode material LiNi0.5Mn1.5O4

The formation of impurity Li_xNi_1−xO when synthesizing spinel LiNi_0.5Mn_1.5O₄ using solid state reaction method, and its influence on the electrochemical properties of product LiNi_0.5Mn_1.5O₄ were studied. The secondary phase Li_xNi_1−xO emerges at high temperature due to oxygen deficiency for LiNi_0.5Mn_1.5O₄ and partial reduction of Mn⁴⁺ to Mn³⁺ in LiNi_0.5Mn_1.5O₄. Annealing process can diminish oxygen deficiency and inhibit impurity Li_xNi_1−xO. The impurity reduces the specific capacity of product, but it does not have obvious negative effect on cycle performance of product. The capacity of LiNi_0.5Mn_1.5O₄ that contains Li_xNi_1−xO can deliver about 120 mAh g⁻¹.