室温固相法制备纳米Fe_2O_3的工艺研究

以FeCl3·6H2O和NaOH为原料,Tw een-80为分散剂,在室温下通过固相反应制备前驱物,然后煅烧前驱物制得纳米氧化铁。研究了表面活性剂的用量、前驱物的煅烧温度、煅烧时间对产物的影响。利用XRD对制备的纳米氧化物进行表征。结果表明,制备的产物为纳米α-Fe2O3。表面活性剂Tween-80可使产物的产率明显提高,粒径减小;随煅烧温度的提高,煅烧时间的延长,产物的粒径先减小,再增大。煅烧温度500℃,煅烧时间2h,制得的α-Fe2O3的平均粒径为21nm。     

纳米α—Fe2O3制备工艺的研究

用微乳液法制备纳米α-Fe2O3,研究不同反应温度和煅烧温度对其晶型结构和形貌的影响,并用x射线衍射仪（XRD）对其进行表征、用扫描电子显微镜（SEM）观察其形貌。结果表明,当煅烧温度大于600℃时,所得样品均为α-Fe2O3,随着反应温度和煅烧温度的增加,α-Fe2O3粒子的粒径逐渐增大,表面呈现蓬松多孔状,而且出现少量团聚现象。     

纳米CuO的室温固相制备工艺研究

采用室温固相制备前驱物再热处理和室温一步固相法两种方法制备纳米CuO.室温固相制备前驱物再热处理的方法以Cu（CH3COO）2·2H2O和H2C2O4·2H2O为原料,通过室温固相反应制备前驱物,再对前驱物进行热处理制备产物,研究了研磨时间、热处理温度及时间对产物的影响;室温一步固相法以CuCl2·2H2O和NaOH为原料,以PEG-400为表面活性剂,通过室温固相反应制备产物,研究了PEG-400用量对产物的影响.通过XRD对产物进行表征.结果表明：室温制备前驱物再热处理的方法制备的纳米CuO产率高,平均粒径小,最好的制备工艺为：对反应物研磨30min,将得到的前驱物在350℃热处理1h,得到的纳米CuO平均粒径为27.06nm,产率为93.16％.     

化学沉淀法制备纳米α-Fe_2O_3及其气敏性能研究

以Fe(NO3)3.9H2O和Na2CO3为起始物,采用化学沉淀法制备了纳米级α-Fe2O3粉体材料.采用XRD、TG-DTA和TEM等技术对产物的晶型、晶粒大小及形貌进行了表征.结果表明,沉淀法所制备的α-Fe2O3粉体材料为分散均匀的球形颗粒,平均粒径大小约40 nm.气敏性能测试结果表明该材料具有可观的气敏性能,对H2S气体表现出较高的灵敏度及良好的选择性,且对乙醇气体的灵敏度明显高于市售样品.在对所制备的α-Fe2O3纳米材料的结构及气敏性能进行系统研究的基础上,初步讨论了其对还原性气体的敏感机理.     

化学沉淀法制备纳米α-Fe2O3及其气敏性能研究

以Fe(NO3)3.9H2O和Na2CO3为起始物,采用化学沉淀法制备了纳米级α-Fe2O3粉体材料.采用XRD、TG-DTA和TEM等技术对产物的晶型、晶粒大小及形貌进行了表征.结果表明,沉淀法所制备的α-Fe2O3粉体材料为分散均匀的球形颗粒,平均粒径大小约40 nm.气敏性能测试结果表明该材料具有可观的气敏性能,对H2S气体表现出较高的灵敏度及良好的选择性,且对乙醇气体的灵敏度明显高于市售样品.在对所制备的α-Fe2O3纳米材料的结构及气敏性能进行系统研究的基础上,初步讨论了其对还原性气体的敏感机理.     

模板调控固相α-Fe2O3的制备及吸附催化性能研究

以甲基橙为矿化模板调控固相合成α-Fe2O3前驱体,经500℃煅烧得到α-Fe2O3纳米粒子,通过XRD及TEM对物相和形貌进行表征,对比研究了有无模板调控α-Fe2O3吸附甲基橙前后的吸附、光催化脱色性能。结果表明:模板调控所制备α-Fe2O3的结晶度降低,且出现大量的介孔,在添加量为0.1g、温度为20℃、pH=5、初始浓度为9mg/L甲基橙时最大吸附容量为1.88mg/g,吸附平衡时间为7h,分别比没有模板调控制备的α-Fe2O3提高了9.04%和缩短了22.2%;对于初始浓度为5mg/L甲基橙,两者的最大光催化脱色率分别为93.21%和89.59%。     

α-Fe2O3/Fe3O4纳米复合材料的相变化及室温磁性质

为研究纳米α—Fe2O3和Fe3O4在受热过程中的物相变化过程和磁学性质,采用燃烧合成方法制备了含α—Fe2O3和Fe3O4不同尺寸的纳米复合材料．用XRD、TEM、穆斯堡尔谱和振动样品磁强计,表征纳米复合材料相变化过程中的性质．结果表明,低于450℃煅烧的复合材料样品中含有一定量的超顺磁相,该相影响着此温度以下煅烧得到的纳米复合材料的磁性质,晶粒尺寸在该温度附近也具有临界现象;复合材料中存在的超顺磁相是超细颗粒尺寸α—Fe2O3和Fe3O4的贡献;当复合材料中的超顺磁相消失后,随煅烧温度提高在复合材料中α-Fe2O3的质量分数不断增加,而Fe3O4的质量分数不断降低直至消失．     

纳米ZrO2/Al2O3复合陶瓷粉体的制备及XRD分析

以醋酸锆、硝酸铝为原料,柠檬酸作为络合剂,采用溶胶-凝胶法获得前驱体,将前驱体在空气中热分解,制备了纳米ZrO2/A l2O3复合陶瓷粉体.采用XRD考察了合成产物的结构和纯度,分析了制备过程中原料初始浓度及前驱体热分解温度对最终产物的影响.结果表明,初始浓度为0.6mol/L,热分解温度为1 200℃时,ZrO2/A l2O3复合陶瓷粉体的粒径为30~41nm.     

焙烧温度对S2O8^2-／Al2O3-Fe2O3固体酸催化性能的影响

制备S2O8^2-／Al2O3-Fe2O3型固体酸催化剂,用于催化乙酸和正丁醇合成乙酸正丁酯,采用TG／DSC、IR、SEM、XRD等对其结构和性能进行了表征,并研究了焙烧温度对其催化性能的影响。结果表明,不同焙烧温度对S2O8^2-／Al2O3-Fe2O3系列催化剂的结构和性能均产生一定的影响;随着焙烧温度的升高,酯化率呈先增加后降低的趋势,其中500℃焙烧的催化剂具有最佳的催化活性,其酯化率达到90．78％。     

α-Fe_2O_3的可控合成及机理研究

本文以FeCl3·6H2O和CTAB为主要原料,采用传统水热法制备出球状和立方体α-Fe2O3颗粒.研究了不同因素对产物形貌的影响;并对形成机理进行了探索;XRD分析表明产物的结晶性好,纯度很高;SEM表明产物的分散性好,颗粒尺寸分布均一,并且反应温度和FeCl3浓度对产物的形貌影响很大.结果表明:当T=120℃,CTAB浓度为0.04M,FeCl3浓度为0.05M时得到了立方体α-Fe2O3,当T=160℃,CTAB浓度为0.04 M,FeCl3浓度为0.02M时得到了球状α-Fe2O3.     

Ba3La2Ti2Ta2O15: A new microwave dielectric of A5B4O15-type cation-deficient perovskites

The synthesis, structure and properties of a new A5B4O15-type cation-deficient perovskite Ba3La2Ti2Ta2O15 were discribed. The compound was prepared by the conventional solid-state reaction route. The phase and structure of the ceramics were characterized by X-ray diffraction （XRD）, scanning electron microscopy （SEM）. The results reveal that the compound is successfully synthesized. The compound crystallizes in the trigonal system with unit cell parameter a=5.6730（2） A, c=11.6511（2） A, V=324.93（1） A^3 and Z=1. The microwave dielectric properties of the ceramic are studied using a network analyzer, and it shows a high dielectric constant of 45.1, a high quality factors with Q×fof21 029 GHz, and a positive τf of 5.3 ppm℃^-1.     

低介Ba(Al0.98Co0.02)2Si2O8-Ba5Si8O21基LTCC微波介质陶瓷的研究

采用传统固相反应法,按摩尔比合成0.7Ba(Al_0.98Co_0.02)₂Si₂O₈?0.3Ba₅Si₈O₂₁(BACS-BS)基陶瓷,分析Li₂O-B₂O₃(1wt%)(L-B)烧结助剂对其烧结特性、相组成和微波介电性能的影响,探讨0.7BACS-0.3BS+1wt%(L-B)陶瓷理论与实验介电常数(ε_r)的差异。结果表明:添加1wt%(L-B)烧结助剂能有效降低0.7BACS-0.3BS基陶瓷的烧结温度(950 ℃),但严重影响其微波介电性能;在950℃烧结的0.7Ba(Al_0.98Co_0.02)₂Si₂O₈-0.3Ba₅Si₈O₂₁+1wt%(Li₂O-B₂O₃)陶瓷具有较好的微波介电性能,其ε_r=7.56, Q×f=13 976 GHz, τ_f=?6.32 ppm/℃;0.7BACS-0.3BS+1wt%(L-B)复合陶瓷与Ag电极有很好的化学相容性,这为其在LTCC技术的应用奠定了良好的基础。     

Electrical conductivity of （Na3AlF6-40%K3AlF6）-AlF3-Al2O3 melts

The effects of contents of AlF3 and Al2O3, and temperature on electrical conductivity of （Na3AlF6-40%K3AlF6）- AlF3-Al2O3 were studied by continuously varying cell censtant （CVCC） technique. The results show that the conductivities of melts increase with the increase of temperature, but by different extents. Every increasing 10 ℃ results in an increase of 1.85 × 10^-2, 1.86× 10^-2, 1.89 × 10^-2 and 2.20 × 10^-2 S/cm in conductivity for the （Na3AlF6-40%K3AlF6）-AlF3 melts containing 0%, 20%, 24%, and 30% AlF3, respectively. An increase of every 10 ℃ in temperature results an increase about 1.89× 10^-2, 1.94 × 10^-2, 1.95 × 10^-2, 1.99× 10^-2 and 2.10× 10^-2 S/cm for （Na3AlF6-40%K3AlF6）-AlF3-Al2O3 melts containing 0%, 1%, 2%, 3% and 4% Al2O3, respectively. The activation energy of conductance was calculated based on Arrhenius equation. Every increasing 1% of AlF3 results in a decrease of 0.019 and 0.020 S/cm in conductivity for （Na3AlF6-40%K3AlF6）-AlF3 melts at 900 and 1 000 ℃, respectively. Every increase of 1% Al2O3 results in a decrease of 0.07 S/cm in conductivity for （Na3AlF6-40%K3AlF6）-AlF3-Al2O3 melts. The activation energy of conductance increases with the increase in content of AlF3 and Al2O3.     

Preparation and electrical-magnetic properties of Co0.6Cu0.16Ni0.24Fe2O4/MWCNTs composites

Co0.6Cu0.16Ni0.24Fe2O4/multi-walled carbon nanotube nanocomposites (CCNF/MWCNTs) were synthesized by solution filling method.The phase structure,thermal stability,morphology and electrical-magnetic properties of the samples were characterized by means of modern testing technology.The effect of iron concentration,filling time,sintering temperature on their electrical and magnetic performance was discussed.The results indicated that conductivity was related to the content of MWCNTs,while the magnetism correlated with the volume fraction of the filled CCNF in the composites.When the optimal condition satisfied the filling time of 18 h,ferric concentration of 0.25 mol L-1 and sintering temperature of 350°C,the prepared composite had the best magnetic loss performance,and its minimum reflection loss reached-22.47 dB on 9.76 GHz,the available bandwidth was beyond 2.0 GHz.Hence,the obtained composite can be used as advancing absorption and shielding material due to its favorable microwave absorbing property.     

Ca0.9Ce0.1Ti0.8Al0.2SiO5在水热作用下的化学稳定性

通过固相法合成掺铈榍石固溶体(Ca0.9 Ce0.1Ti0.8Al0.2SiO5),采用PCT粉末浸泡试验法,借助X射线衍射(XRD)、扫描电镜(SEM)、电感耦合等离子体发射光谱(ICP-OES)等分析测试手段,研究掺铈榍石固溶体在热液作用下的稳定性.实验结果表明,掺铈榍石固化体在不同条件下(温度150～ 200℃,0.476～1.554 MPa,pH值5～9),都具有良好的稳定性.随着浸泡时间的增加,各元素的归一化浸出率逐渐降低并保持在较低水平.     

Synthesis and characterization of Mg3(PO4)2-coated Li1.05Ni1/3Mn1/3Co1/3O2 cathode material for Li-ion battery

Mg₃(PO₄)₂-coated Li_1.05Ni_1/3Mn_1/3Co_1/3O₂ cathode materials were synthesized via co-precipitation method. The morphology, structure, electrochemical performance and thermal stability were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), cyclic voltammetry(CV), electrochemical impedance spectroscopy(EIS), charge/discharge cycling and differential scanning calorimeter (DSC). SEM analysis shows that Mg₃(PO₄)₂-coating changes the morphologies of their particles and increases the grains size. XRD and CV results show that Mg₃(PO₄)₂-coating powder is homogeneous and has better layered structure than the bare one. Mg₃(PO₄)₂-coating improved high rate discharge capacity and cycle-life performance. The reason why the cycling performance of Mg₃(PO₄)₂-coated sample at 55 °C was better than that of room temperature was the increasing of lithium-ion diffusion rate and charge transfer rate with temperature rising. Mg₃(PO₄)₂-coating improved the cathode thermal stability, and the result was consistent with thermal abuse tests using Li-ion cells: the Mg₃(PO₄)₂ coated Li_1.05Ni_1/3Mn_1/3Co_1/3O₂ cathode did not exhibit thermal runaway with smoke and explosion, in contrast to the cells containing the bare Li_1.05Ni_1/3Mn_1/3Co_1/3O₂. Funded by the National Natural Science Foundation of China (No. 20273047)     

Modification of LiCo1/3Ni1/3Mn1/3O2 cathode material by CeO2-coating

LiCo_1/3Ni_1/3Mn_1/3O₂ was coated by a layer of 1.0 wt% CeO₂ via sol-gel method. The bared and coated LiMn_1/3Co_1/3Ni_1/3O₂ was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammogram (CV) and galvanotactic charge-discharge test. The results show that the coating layer has no effect on the crystal structure, only coating on the surface; the 1.0 wt% CeO₂-coated LiCo_1/3Ni_1/3Mn_1/3O₂ exhibits better discharge capacity and cycling performance than the bared LiCo_1/3Ni_1/3Mn_1/3O₂. The discharge capacity of 1.0 wt% CeO₂-coated cathode is 182.5 mAh·g⁻¹ at a current density of 20 mA·g⁻¹, in contrast to 165.8 mAh·g⁻¹of the bared sample. The discharge capacity retention of 1.0 wt% CeO₂-coated sample after 12 cycles reaches 93.2%, in comparison with 86.6% of the bared sample. CV results show that the CeO₂ coating could suppress phase transitions and prevent the surface of cathode material from direct contact with the electrolyte, thus enhance the electrochemical performance of the coated material.     

Electrolysis expansion performance of semigraphitic cathode in [K3AlF6/Na3AlF6]-AlF3-Al2O3 bath system

The electrolysis expansion of semigraphitic cathode in [K₃AlF₆/Na₃AlF₆]-AlF₃-Al₂O₃ bath system was tested by self-made modified Rapoport apparatus. A mathematical model was introduced to discuss the effects of α _CR (cryolite ratio) and β _KR (elpasolite content divided by the total amount of elpasolite and sodium cryolite) on performance of cathode electrolysis expansion. The results show that K and Na (potassium and sodium) penetrate into the cathode together and have an obvious influence on the performance of cathode electrolysis expansion. The electrolysis expansion and K/Na penetration rate increase with the increase of α _CR. When α _CR=1.9 and β _KR=0.5, the electrolysis expansion is the highest, which is 3.95%; and when α _CR=1.4 and β _KR=0.1, the electrolysis expansion is the lowest, which is 1.28%. But the effect of β _KR is correlative with α _CR. When α _CR=1.6 and 1.9, with the increase of β _KR, the electrolysis expansion and K/Na penetration rate increase. However, when α _CR=1.4, the electrolysis expansion and K/Na penetration rate firstly increase and then decrease with the increase of β _KR. Foundation item: Project (2005CB623703) supported by the Major State Basic Research and Development Program of China; Project (2008AA030502) supported by the National High-Tech Research and Development Program of China     

Characteristics of LiCoO2, LiMn2O4 and LiNi0.45Co0.1Mn0.45O2 as cathodes of lithium ion batteries

LiNi_0.45Co_0.10Mn_0.45O₂ was synthesized from Li₂CO₃ and a triple oxide of nickel, cobalt and manganese at 950 °C in air. The structures and characteristics of LiNi_0.45Co_0.10Mn_0.45O₂, LiCoO₂ and LiMn₂O₄ were investigated by XRD, SEM and electrochemical measurements. The results show that LiNi_0.45Co_0.10Mn_0.45O₂ has a layered structure with hexagonal lattice. The commercial LiCoO₂ has sphere-like appearance and smooth surfaces, while the LiMn₂O₄ and LiNi_0.45Co_0.10Mn_0.45O₂ consist of cornered and uneven particles. LiNi_0.45Co_0.10Mn_0.45O₂ has a large discharge capacity of 140.9 mA · h/g in practical lithium ion battery, which is 33.4% and 2.8% above that of LiMn₂O₄ and LiCoO₂, respectively. LiCoO₂ and LiMn₂O₄ have higher discharge voltage and better rate-capability than LiNi_0.45Co_0.10Mn_0.45O₂. All the three cathodes have excellent cycling performance with capacity retention of above 89.3% at the 250th cycle. Batteries with LiMn₂O₄ or LiNi_0.45Co_0.10Mn_0.45O₂ cathodes show better safety performance under abusive conditions than those with LiCoO₂ cathodes. Foundation item: Project(50302016) supported by the National Natural Science Foundation of China; Project(2005037698) supported by the Postdoctoral Science Foundation of China     

Molar heat capacities of La2Mo2O9 and La1.9Sr0.1MO209-δ

The molar heat capacities of La2Mo209 and La1.9Sr0.1MO209-δ were obtained using the differential scanning calorimetry （DSC） technique in a temperature range from 298 to 1473 K. The DSC curve of La2Mo209 showed an endothermal peak around 834 K corresponding to a first-order monoclinic-cubic phase transition, and the enthalpy change accompanying this phase transition is 5.99 kJ/mol. No evident endothermal peak existed in the DSC curve of La1.9Sr0.1MO209-δ, but a broad thermal anomaly existed in its heat capacity curve at around 832 K. In addition, the heat capacity values of La2Mo209 and La1.9Sr0.1MO209-δ began to decrease at 1196 and 1330 K, respectively. The non-transitional heat capacity values of La2Mo209 and La1.9Sr0.1MO209-δ were formulated using multiple regression analysis in two temperature ranges.