低压制备纳米Sb_2O_3粉的研究

用低压蒸发普通 Sb2 O3的方法制备出了纳米 Sb2 O3,分析了生成 Sb2 O3的热力学条件 ,对抑制 Sb2 O3的分解做了详细的理论分析 ,确定了制备纳米 Sb2 O3的温度条件和压力条件 ,证明在一定的氧分压情况下 Sb2 O3是不会分解的 ,测定了 Sb2 O3的粒度和粒度分布 ,探讨了生产可行性     

纳米Sb2O3/云母阻燃微粉的制备及其阻燃机理

以三氯化锑和片状云母为原料,通过醇解、水解反应,表面活性剂处理,制备了纳米Sb2O3/云母阻燃微粉.用TEM表征了纳米Sb2O3/云母的形貌及其在云母表面的组装行为,利用XRD研究了不同煅烧温度对氧化锑形态的影响,利用燃烧法研究了纳米Sb2O3/云母复合微粒的阻燃性能,探讨了阻燃机理.结果表明,当云母的质量分数为5%,煅烧温度为400℃时,制备的纳米Sb2O3/云母纯度较高,阻燃性能优异;Sb2O3均匀地组装在云母上,在组装过程中不易团聚,Sb2O3的平均粒径约为5 nm.纳米Sb2O3/云母和氯化石蜡协同体系的阻燃机理包括自由基捕获机理和物理作用.在高温下纳米Sb2O3与氯化石蜡分解产生的氯化氢反应生成SbCl3,SbCl3在燃烧区内发生分解, 可捕获气相中维持聚合物燃烧链式反应的活泼自由基,使得链反应终止.物理作用包括隔热、隔氧、降低燃烧反应温度等.     

纳米二氧化钛导电粉制备研究

采用化学共沉淀方法,以掺杂Sb的SnO2(ATO)包覆纳米二氧化钛,制备纳米二氧化钛导电粉.研究制备条件对纳米二氧化钛体积电阻率的影响,利用SEM、XRD和XRF分析产物的表面形貌、成分与含量.实验得出较佳的制备条件为:反应温度70～80℃,SnCl4·5H2O的质量分数为60%,SbCl3的质量分数为6%,pH值为2,加料时间2.5 h,煅烧时间2 h,煅烧温度600℃.     

水热法制备Sb_2Se_3纳米晶

以酒石酸锑钾(K(SbO)C4H4O6.1/2H2O)和硒粉作为锑源和硒源,自制的2-十一烷基-1-二硫脲乙基咪唑啉季铵盐(SUDEI)为表面活性剂,150℃水热反应24 h,得到不同形貌的Sb2Se3纳米晶。通过透射电镜(TEM)、X射线衍射(XRD)、X射线光电子能谱仪(XPS)对Sb2Se3纳米晶进行了表征。讨论了反应条件对Sb2Se3纳米晶形貌的影响。     

微乳液法制备纳米ZnO粉体

采用双微乳液混合法制备纳米ZnO粉末．通过实验从nH2O／nAEO3 AEO9、反应物浓度、老化温度及时间、前驱体煅烧温度及时间等方面讨论影响产物的粒径，确定了制备纳米ZnO粉末的较理想的工艺条件．经XRD，TEM和激光粒度仪等检测表征，产物为球形六角晶系结构，平均粒径27nm，粒径尺寸分布范围较窄，99％颗粒达纳米级．     

硫化铋纳米晶的水热合成及表征

在低温水热条件下,以BiCl3、Na2S2O3（或Na2S、硫脲）为反应物,制备了硫化铋（Bi2S3）纳米晶.用X射线粉末衍射（XRD）、扫描电镜（SEM）及纳米粒度测定仪对样品的结构及形貌进行了表征分析.结果表明,所得样品为正交晶系的Bi2S3纳米晶,形貌主要为纳米棒;同时硫源、反应温度及反应时间会影响样品的粒径.     

掺杂纳米Al2O3的石墨/Cu基复合材料性能研究

利用均相沉淀法制备了含石墨粉的纳米Al2O3，采用模压成型法制备了含有纳米Al2O3的铜质石墨复合材料，并研究了此复合材料的性能与纳米Al2O3质量分数的关系．根据实验结果分析了实验现象的原因，并由此得出：当纳米Al2O3的质量分数为4％时，其铜质石墨复合材料性能最佳。     

Ni/MgO-Al_2O_3催化剂的制备及在CO_2重整CH_4反应中的应用

采用溶胶-凝胶法制备了纳米催化剂的载体复合氧化物MgO-Al2O3,然后采用浸渍法制备出纳米Ni//MgO-Al2O3催化剂,并将其应用在CO2重整CH4反应中,结果表明,在适宜的反应条件下,纳米Ni//MgO-Al2O3催化剂具有很好的活性和稳定性.     

ZnO-Sb2O3-P2O5系统玻璃的制备与性能

用熔体冷却方法制备了xSb2O3-(70-x)P2O5-30ZnO(x=0~40mol)和xSb2O3-(65-x)ZnO-35P2O5(x=0~40mol)系统无铅易熔玻璃,研究了ZnO-Sb2O3-P2O系统玻璃的形成区。采用热膨胀仪和红外光谱仪等对ZnO-Sb2O3-P2O5系统玻璃的结构及性能进行了研究和分析。结果表明,在ZnOSb2O3-P2O5系统玻璃中,Sb2O3参与网络结构。随着Sb2O3含量的增加,玻璃的软化点降低,密度和化学稳定性增加。在Sb2O3摩尔分数为35%左右时,系统玻璃的结构和性能比较优异。     

水热法和溶胶-凝胶法制备Mn_(0.8)Zn_(0.2)Fe_2O_4纳米磁性粒子及其结构表征

通过水热法和Sol-Gel法制备了Mn0.8Zn0.2Fe2O4纳米磁性粒子,利用X射线衍射(XRD)、扫描电镜(TEM)以及ICP元素分析对Mn0.8Zn0.2Fe2O4纳米粒子的晶型和形貌进行了表征,讨论了反应方法和反应条件对纳米粒度和结构的影响。结果表明,水热法和Sol-Gel法制备的纳米粒子均为尖晶石型结构,但前者纯度很高,平均粒径为11 nm,而后者含有氧化物杂相,平均粒径为45 nm,通过对比显示出水热法在此反应中的优越性。     

SnO2及SnO2／Fe2O3复合微米材料的合成及表征

本文首先以SnCl2·2H2O为主要原料,无水乙醇为溶剂,利用溶剂热法于180℃反应24h得到了SnO2微球;再以所制备的SnO2微球为前驱体,FeCl3·6H2O为主要原料,通过水热法得到SnO2／Fe2O3复合材料．利用X射线粉末衍射仪（XRD）和扫描电子显微镜（SEM）对所得产物进行了表征．结果表明：所得的SnO2为四方锡石型,形貌为微球,平均直径约为2．0μm;复合后得到的SnO2／Fe2O3微球平均直径约为2．5μm．其中,Fe2O3为六方赤铁矿型,在复合物的表面以小颗粒的形式存在,尺寸约为200nm．另外,也对SnO3与SnO2／Fe2O3微球的形成过程进行了讨论．     

Temperature dependence on reaction of CaCO3 and SO2 in O2/CO2 coal combustion

The temperature dependence on the reaction of desulfurization reagent CaCO₃ and SO₂ in O₂/CO₂ coal combustion was investigated by thermogravimetric analysis, X-ray diffraction measurement and pore structure analysis. The results show that the conversion of the reaction of CaCO₃ and SO₂ in air is higher at 500–1 100 °C and lower at 1 200 °C compared with that in O₂/CO₂ atmosphere. The conversion can be increased by increasing the concentration of SO₂, which causes the inhibition of CaSO₄ decomposition and shifting of the reaction equilibrium toward the products. XRD analysis of the product shows that the reaction mechanism of CaCO₃ and SO₂ differs with temperature in O₂/CO₂ atmosphere, i.e. CaCO₃ directly reacts with SO₂ at 500 °C and CaO from CaCO₃ decomposition reacts with SO₂ at 1 000 °C. The pore analysis of the products indicates that the maximum specific surface area of the products accounts for the highest conversion at 1 100 °C in O₂/CO₂ atmosphere. The results reveal that the effect of the atmosphere on the conversion is temperature dependence.     

Preparation of TiO2 photocatalyst loaded with V2O5 for O2 evolution

TiO₂ photocatalysts loaded with V₂O₅ were prepared via a modified hydrolysis process, and characterized by X-ray diffraction, transmission electron microscopy, Raman spectra and diffuse reflectance UV-Vis spectra measurements. The photocatalytic activity of V₂O₅/TiO₂ was investigated by employing splitting of water for O₂ evolution. The results indicate that V₂O₅ loading can pronouncedly improve the photocatalytic activity of TiO₂ with Fe³⁺ as an electron acceptor under UV or visible light irradiation. The optimum mass fraction of the loaded V₂O₅ is 8%, and the largest speed of O₂ evolution for 8%V₂O₅ (mass fraction) loaded TiO₂ catalyst is 118.2 μmol/(L·h) under UV irradiation, and 83.7 μmol/(L·h) under visible light irradiation.     

Bi2O3和Fe2O3掺杂对BaTiO3陶瓷显微结构的影响

利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线能量色散谱(EDAX)等结构分析技术,研究了施主(Bi     

Dielectric properties of Pb (Zn1/3 Nb2/3) O3?PbZrO3?PbTiO3 solid solution near morphotropic phase boundary

The dielectric properties of Pb(Zn_1/3Nb_2/3) O₃-PbZrO₃−PbTiO₃ (PZN-PZ-PT) system near the rhombohedral/tetragonal morphotropic phase boundary (MPB) are carefully studied in this paper. It is found that, for all samples, the curves around the temperatures of dielectric permittivity peak show the characteristics of diffuse phase transition. The change in PbZrO₃/PbTiO₃ ratio has much influence on the dielectric properties of the samples. The extent of diffuse phase transition increases with the increasing Zr/Ti ratio. The samples in rhombohedral region have typical diffuse phase transition in the temperature range measured. However, for the samples with tetragonal symmetry, a spontaneous normal ferroelectric-relaxor phase transition exists at temperature lower than that of permittivity peak. This normal ferroelectric-relaxor phase transition is confirmed by the experiment of thermally driven current. The analysis of TEM reveals that the samples in tetragonal region show a 90% macrodomain structure, while the samples in rhombohedral region have the configuration of microdomain structure.     

三氧化二铝是导致建筑物火灾的严重隐患

建筑物供电线路中的铜线与铝线连接处常常生成一种灰白物质－－三氧化二铝,极易引发建筑物火灾。着重介绍和分析这种灰白物质的成分、生成原因、危害以及防止其生成的主要措施。     

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     

Modification of nano-TiO2 by Al2O3 in-situ coating

A novel technology of in-situ coating Al₂O₃ on the surface of H₄TiO₄ was developed to prevent the aggregation of nano-TiO₂ powders and improve the dispersibility and thermal stability in the way of forming a uniform coating layer. The heterogeneous nucleation was conducted to prepare the precursor of nano-TiO₂ and then Al₂O₃ was coated on the surface of precursor. The effects of Al₂O₃ in-situ coating on the properties of nano-TiO₂ were investigated. The results show that H₄TiO₄ can be dispersed well under alkaline condition (pH 8.5) and the heterogeneous nucleation can be controlled easily. The optimized uniform coating layer is obtained by adding 5% (mass fraction) and 10% of Al₂O₃ and the aggregation of nano-TiO₂ powders is effectively inhibited and the dispersibility is obviously improved. The crystal sizes of TiO₂ powders are 12.3, 11.4 and 8.7 nm after coating 0,5% and 10% of Al₂O₃ respectively. Al₂O₃ on the surface of particulates in amorphous phase could increase the thermal stability of nano-particles after calcined at 550 °C. Foundation item: Project(04GK2007) supported by Hunan Industrial Key Project of Science and Technology     

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     

Inducing effect of Pb(Zr0.4Ti0.6)O3 thin film derived by different processes in BiFeO3/Pb(Zr0.4Ti0.6)O3 multilayer capacitor at room temperature

BiFeO₃/PZT multilayer capacitor was prepared on Pt(100)/Ti/SiO₂/Si(100) substrate. PZT buffer layer was derived by MOCVD method (label: PZT₁) and sputtering method (label: PZT₂) respectively. XRD analysis indicated that high (110) orientation of BFO in the BFO/PZT₁ structure was achieved. SEM analysis indicated a better microstructure in the BFO/PZT₁ structure compared with BFO/PZT₂. The remnant polarization of the BFO/PZT₁ was 82.5 μ C/cm² at an applied voltage of 8 V, compared with that of 25.2 μC/cm² in the BFO/PZT₂ structure. The BFO/PZT₁ multilayer exhibited little polarization fatigue (<1.5%) upon 1×10¹⁰ switching cycles, at an applied voltage of 4 V. The leakage current density was about 2×10₋₇ A/cm² at an applied voltage 4 V, in the BFO/PZT₁ capacitor. All the results indicated that PZT can act as an inducing layer to the BFO and the MOCVD derived PZT has more inducing effect to the BFO thin film at room temperature. Supported by the National Natural Science Foundation of China (Grant No. 60601003), Ying Tong Education Foundation (Grant No. 101063), and International Cooperation Project from Ministry of Science and Technology of China (Grant No. 2008DFA12000)