Preparation of TiO(2) Nanocrystallite Powders Coated with 9 mol% ZnO for Cosmetic Applications in Sunscreens

The preparation of TiO(2) nanocrystallite powders coated with and without 9 mol% ZnO has been studied for cosmetic applications in sunscreens by a co-precipitation process using TiCl(4) and Zn(NO(3))(2)·6H(2)O as starting materials. XRD results show that the phases of anatase TiO(2) and rutile TiO(2) coexist for precursor powders without added ZnO (T-0Z) and calcined at 523 to 973 K for 2 h. When the T-0Z precursor powders are calcined at 1273 K for 2 h, only the rutile TiO(2) appears. In addition, when the TiO(2) precursor powders contain 9 mol% ZnO (T-9Z) are calcined at 873 to 973 K for 2 h, the crystallized samples are composed of the major phase of rutile TiO(2) and the minor phases of anatase TiO(2) and Zn(2)Ti(3)O(8). The analyses of UV/VIS/NIR spectra reveal that the absorption of the T-9Z precursor powders after being calcined has a red-shift effect in the UV range with increasing calcination temperature. Therefore, the TiO(2) nanocrystallite powders coated with 9 mol% ZnO can be used as the attenuate agent in the UV-A region for cosmetic applications in sunscreens.     

微乳液结合Sol-Gel法制备纳米ZnTiO3及其表征

将溶胶-凝胶法与微乳液化学剪裁法相结合,以钛酸丁酯和氯化锌制备凝胶,在OP-10-SDS/正丁醇/环己烷/水复配微乳体系中进行化学剪裁制备前驱物,再经煅烧制备了组成单一的球状纳米ZnTiO3粉体,通过XRD、TEM、SEM、TG-DSC等方法对产物进行了表征,并讨论了凝胶的陈化时间、煅烧温度和煅烧时间对纳米ZnTiO3的组成、粒径和形貌的影响,提出了纳米ZnTiO3可能的形成机理。结果表明,在700℃煅烧2h制备的纳米ZnTiO3平均粒径为35nm,粒径分布比较均匀,基本呈单分散;适当延长陈化时间会减少ZnO及TiO2杂质;随着煅烧时间的延长,ZnTiO3晶体粒径开始增大;煅烧温度过高会使六方相ZnTiO3分解为立方相的Zn2TiO4和金红石型TiO2。     

微乳液结合Sol-Gel法制备纳米ZnTiO_3及其表征

将溶胶-凝胶法与微乳液化学剪裁法相结合,以钛酸丁酯和氯化锌制备凝胶,在OP-10-SDS/正丁醇/环己烷/水复配微乳体系中进行化学剪裁制备前驱物,再经煅烧制备了组成单一的球状纳米ZnTiO3粉体,通过XRD、TEM、SEM、TG-DSC等方法对产物进行了表征,并讨论了凝胶的陈化时间、煅烧温度和煅烧时间对纳米ZnTiO3的组成、粒径和形貌的影响,提出了纳米ZnTiO3可能的形成机理。结果表明,在700℃煅烧2h制备的纳米ZnTiO3平均粒径为35nm,粒径分布比较均匀,基本呈单分散;适当延长陈化时间会减少ZnO及TiO2杂质;随着煅烧时间的延长,ZnTiO3晶体粒径开始增大;煅烧温度过高会使六方相ZnTiO3分解为立方相的Zn2TiO4和金红石型TiO2。     

Preparation and scintillating properties of sol-gel eu, tb co-doped lu(2)o(3) nanopowders

Nanocrystalline Eu(3+), Tb(3+) co-doped Lu(2)O(3) powders with a maximum size of 25.5 nm were prepared by the sol-gel process, using lutetium, europium and terbium nitrates as precursors, and ethanol as a solvent. Differential thermal analysis (DTA) and infrared spectroscopy (IR) were used to study the chemical changes during the xerogel annealing. After the sol evaporation at 100 °C, the formed gel was annealed from 300 to 900 °C for 30 min under a rich O(2) atmosphere, and the yielded product was analyzed by X-ray diffraction (XRD) to characterize the microstructural behavior and confirm the crystalline structure. The results showed that Lu(2)O(3) nanopowders start to crystallize at 400 °C and that the crystallite size increases along with the annealing temperature. A transmission electron microscopy (TEM) study of samples annealed at 700 and 900 °C was carried out in order to analyze the microstructure, as well as the size, of crystallites. Finally, in regard to scintillating properties, Eu(3+) dopant (5 mol%), Tb(3+) codoped Lu(2)O(3) exhibited a typical red emission at 611 nm (D(°)→(7)F(2)), furthermore, the effect of Tb(3+) molar content (0.01, 0.015 and 0.02% mol) on the Eu(3+) radioluminiscence was analyzed and it was found that the higher emission intensity corresponds to the lower Tb(3+) content.     

锂离子电池负极材料钛酸锂的制备与研究

以四氯化钛、氢氧化锂为原料,采用模板法,获得前躯体（Li1.81H0.19）Ti2O5·0.262 5TiO2,再通过煅烧,得到纳米钛酸锂（Li4Ti5O12）。最佳制备工艺条件为：模板∶钛（摩尔比）为4∶1,700℃煅烧1 h。采用TEM电镜观测的粒度达到10~100 nm,XRD拟合粒径5~30 nm,比表面积达100~600 m2/g。     

纯六方相钛酸锌粉体的制备与表征

本文以钛酸四丁酯、冰醋酸、盐酸、六水合硝酸锌为主要原料,采用溶胶-凝胶法,以去离子水作为溶剂制备出具有钛铁矿结构的纯六方相ZnTiO3粉体,并利用TG/DTA,XRD,FE-SEM和FT-IR对其组织结构和形貌进行了研究。实验结果表明:前驱体干凝胶在550℃热处理4h可制得纯六方相ZnTiO3,且六方相稳定存在的温度范围相对较宽,从550℃到900℃。当温度升高到950℃后,六方相ZnTiO3将分解为立方相Zn2TiO4和金红石相TiO2。在550℃热处理制得的ZnTiO3粉体粒径约为50nm。     

共沉淀法制备Bi3.25La0.75Ti3O12纳米粉体

用硝酸铋、硝酸镧和钛酸四丁酯为原料，硝酸、无水乙醇和去离子水为溶剂，氨水为沉淀剂，采用共沉淀法合成了单相铋层状钙钛矿结构Bi3.25La0．75Ti3O12(BLT)纳米粉体。用DTA／TG和XRD研究了BLT前驱体的热行为和晶相转化过程，用场致发射扫描电子显微镜观察了BLT粉体的颗粒形貌和大小的变化。结果表明：共沉淀前驱体溶液的配制过程中，硝酸铋水解生成的硝酸氧铋不利于层状钙钛矿结构BLT相的合成。利用浓度较高的硝酸作溶剂，可以防止硝酸铋的水解，采用氨基共沉淀法直接合成出了单一相的BLT纳米粉体，在煅烧过程中，未出现Bi2Ti2O3焦绿石相。700℃煅烧2h合成的BLT粉体颗粒不大于100nm，颗粒间结合疏松，具有良好的分散性。     

Photopyroelectric Spectroscopic Studies of ZnO-MnO(2)-Co(3)O(4)-V(2)O(5) Ceramics

Photopyroelectric (PPE) spectroscopy is a nondestructive tool that is used to study the optical properties of the ceramics (ZnO + 0.4MnO(2) + 0.4Co(3)O(4) + xV(2)O(5)), x = 0-1 mol%. Wavelength of incident light, modulated at 10 Hz, was in the range of 300-800 nm. PPE spectrum with reference to the doping level and sintering temperature is discussed. Optical energy band-gap (E(g)) was 2.11 eV for 0.3 mol% V(2)O(5) at a sintering temperature of 1025 °C as determined from the plot (ρhυ)(2)versushυ. With a further increase in V(2)O(5), the value of E(g) was found to be 2.59 eV. Steepness factor 'σ(A)' and 'σ(B)', which characterize the slope of exponential optical absorption, is discussed with reference to the variation of E(g). XRD, SEM and EDAX are also used for characterization of the ceramic. For this ceramic, the maximum relative density and grain size was observed to be 91.8% and 9.5 μm, respectively.     

Use of a Reflectance Spectroscopy Accessory for Optical Characterization of ZnO-Bi(2)O(3)-TiO(2) Ceramics

The optical band-gap energy (E(g)) is an important feature of semiconductors which determines their applications in optoelectronics. Therefore, it is necessary to investigate the electronic states of ceramic ZnO and the effect of doped impurities under different processing conditions. E(g) of the ceramic ZnO + xBi(2)O(3) + xTiO(2), where x = 0.5 mol%, was determined using a UV-Vis spectrophotometer attached to a Reflectance Spectroscopy Accessory for powdered samples. The samples was prepared using the solid-state route and sintered at temperatures from 1140 to 1260 °C for 45 and 90 minutes. E(g) was observed to decrease with an increase of sintering temperature. XRD analysis indicated hexagonal ZnO and few small peaks of intergranular layers of secondary phases. The relative density of the sintered ceramics decreased and the average grain size increased with the increase of sintering temperature.     

掺N纳米ZnO/TiO_2复合粉体的光催化性能

以Ti(SO4)2和Zn(NO3)2为原料,CO(NH2)2为沉淀剂,采用均匀沉淀法制备了掺N和不同质量分数ZnO掺杂的纳米TiO2复合粉体,通过XRD、XPS、TEM等进行了表征,并以甲基橙水溶液为底物,测定了其光催化性能。结果表明,掺杂产生了Ti—O—Zn和Ti—O—N键,使复合粉体的激发波段从紫外光波段扩展到可见光波段,催化活性大大提高,其中w(ZnO)=2%时,复合粉体太阳光催化性能最高,太阳光照射6 h,甲基橙降解率达到98.4%,重复使用6次后,降解率仍达到94.2%。     

固相反应法制备纳米ZnO及其晶粒生长动力学

以乙酸锌和草酸为原料,采用低热固相化学反应法制备纳米氧化锌的前体,通过微波和马弗炉两种焙烧方式焙烧制备得到纳米氧化锌,考察了焙烧温度和时间对纳米氧化锌粒径的影响。使用透射电镜、热重-差热、傅里叶变换红外光谱仪和X射线衍射仪对前体和纳米ZnO进行表征;采用晶粒生长动力学唯象理论计算得出纳米氧化锌在这两种焙烧方式下的晶粒生长动力学规律。结果表明,前体为ZnC2O4?2H2O,随着焙烧温度的提高,纳米氧化锌晶粒迅速长大,在相同焙烧温度和时间下,微波焙烧氧化锌的晶粒尺寸要明显大于常规焙烧方式。微波焙烧和常规焙烧下氧化锌的晶粒生长平均动力学指数分别是6.114和6.858,晶粒生长的平均活化能分别为70.67 kJ/mol和52.13 kJ/mol。     

ZnO粉体的固相法合成及微波介电性能

采用固相反应法制备了ZnO前驱体,在不同煅烧温度和保温时间分解得到ZnO粉体.用扫描电镜和X射线衍射仪表征合成粉体.采用矢量网络分析仪测试ZnO粉体在8.2～12.4 GHz的微波介电性能.结果表明:在不同煅烧温度和保温时间,前驱体均分解生成ZnO粉体.低温时,得到的样品颗粒大小均匀一致;随着温度的升高,颗粒逐渐长大,但均匀性变差.保温时间对样品颗粒大小的影响不明显.样品介电常数的实部(ε')和虚部(ε')随温度的升高先增大后减小,700℃时,达到最大;而随保温时间的增加,ε'和ε'的变化不显著.对产生介电损耗的机理进行了讨论,并提出改善介电性能的途径.     

复合锌镍铁氧体纳米粉体材料的制备实验

以硫酸盐为原料，添加NaOH溶液和NaHCO3粉末，先制备碱式碳酸盐前驱体，350℃空气中焙烧1 h后，制备出复合锌镍铁氧体纳米晶体. 经XRD和TEM分析，粒径约为30 nm，粒度较均匀. 通过改变原料中锌盐与镍盐的配比，制备出Zn0.9Ni0.1Fe2O4, Zn0.8Ni0.2Fe2O4, Zn0.7Ni0.3Fe2O4, Zn0.6Ni0.4Fe2O4和Zn0.5Ni0.5Fe2O4 五种纳米粉.     

二氧化硫脲为硫源制备硫掺杂二氧化钛及其光催化活性

以钛酸四丁酯为TiO2的前驱物,二氧化硫脲为掺杂硫的源物质,采用溶胶-凝胶法制备了掺硫改性的TiO2光催化剂。采用XRD对制备的掺硫二氧化钛结构进行了表征,探讨了溶胶-凝胶制备工艺、硫掺杂量及催化剂煅烧温度对该催化剂光催化活性的影响。结果表明,掺硫改性的TiO2经600℃煅烧后光催化活性有了明显提高,且硫的掺杂有一个最佳值,即二氧化硫脲的掺杂质量百分数为4%。经掺硫改性后的TiO2在可见光区具备更强的光催化活性,在波长不低于400nm的可见光作用下,对亚甲基蓝的4 h降解率最高可达89.5%。     

Structural and Physical Properties of Nd-Doped Pb(Zr0.52Ti0.48)O3 Ceramics

Lead zirconate titanate (PZT) ceramics (Zr/Ti = 52/48) have been modified with different quantities of neodymium oxide (Nd₂O₃). The preparation was carried out via the solid-state-reaction route. The samples were calcined and sintered at 850°C and 1200°C, respectively. The structural evolution and the microstructure were investigated using an X-ray diffractometer (XRD) and a scanning electron microscope (SEM), respectively. The physical properties such as dielectric constants, piezoelectric coefficients, density etc. were also studied.     

Hydrothermal synthesis of BaTiO3 from different Ti-precursors and microstructural and electrical properties of sintered samples with submicrometric grain size

Barium titanate submicrometric particles were synthesized at 180 °C in a closed PTFE-lined stainless steel reactor with continuous stirring. Precursors used for titanium were Degussa P25 TiO₂ or titanium isopropoxide (TIP). Barium hydroxide (Ba(OH)₂) was added in a Ba/Ti = 1.1 molar ratio and KOH was used as mineralizer. The obtained powders were characterized by XRD and Raman spectroscopy. Powders were uniaxially pressed into discs and sintered at 1250 °C. The resulting microstructures were characterized by XRD, SEM, and Raman spectroscopy. Electrical measurements were carried out in order to characterize the ferroelectric behavior. The Ti precursor determined the sample density and grain size distribution and, consequently, the electrical response.     

ZnO微／纳米纤维的静电纺丝及其表征

以聚乙烯吡咯烷酮(PVP)为络合剂与醋酸锌[Zn(CH3COO)2]反应制得前驱体溶液,用静电纺丝法制备了PVP／Zn(CH3COO)2纤维,经煅烧得到具有微孔结构的氧化锌(ZnO)微／纳米纤维。对所制备纤维分别采用差热-热重分析、红外光谱分析、X射线衍射分析、扫描电镜等手段进行了表征。结果表明: PVP/Zn(CH3COO)纤维表面光滑,直径约300-700 nm,经700℃煅烧后,可得到ZnO微／纳米纤维。     

Synthesis of nano-crystalline Ce0.9Gd0.1O1.95 electrolyte by novel sol–gel thermolysis process for IT-SOFCs

In the present work, nano-crystalline Ce_0.9Gd_0.1O_1.95 (GDC) powder has been successfully prepared by a novel sol–gel thermolysis method using a unique combination of urea and PVA. The gel precursor obtained during the process was calcined at 400 and 600 °C for 2 h. A range of analyzing techniques including XRD, TGA, BET, SEM, EDS and TEM were employed to characterize the physical and chemical properties of obtained powders. GDC gel precursors calcined at 400 and 600 °C were found to have an average crystallite size of 10 and 19 nm, respectively. From the result of XRD patterns, we found that well-crystalline cubic fluorite structure GDC was obtained by calcining the precursor gel at 400 and 600 °C. It has been also found that the sintered samples with lower temperature calcined powder showed better sinterability as well as higher ionic conductivity of 2.21 × 10⁻² S cm⁻¹ at 700 °C in air.     

Preparation and characterization of a ZnO powder with the hexagonal plate particles

Zinc oxide precursors were obtained by the reaction of excess urea with 0.05-0.30 M ZnSO₄ in boiling aqueous solution. The precursors precipitated were dried at 100 °C for 2 h to yield powdery products and these products were calcined at 1000 °C for 2 h to yield zinc oxide powders. Differential thermal analysis (DTA) and thermal gravimetric analysis (TGA) curves of the air-dried precursor precipitates show that the suitable temperatures for dehydration of crystal water, of ligand water and of dehydroxylation are 76, 290, and 866 °C, respectively. From the scanning electron microscopy (SEM) photographs and particle size distribution (PSD) curves, the average sizes of the hexagonal plate particles in precursor and ZnO powders are found to be 55 and 35 μm, respectively. X-ray diffraction (XRD) data were evaluated by Scherrer equation for the estimation of the average crystal size of the precursor (11 nm) and ZnO (45 nm). The specific surface area and specific micro-mesopore volume of the ZnO powders are so small as to fall into the experimental error limits. It was concluded that all the measured quantities are not affected considerably by the Zn²⁺ concentration.     

TiO2/ZnO Supported on Sepiolite: Preparation,Structural Characterization,and Photocatalytic Degradation of Flumequine Antibiotic in Aqueous Solution

In this study, TiO₂, ZnO, TiO₂/ZnO (Ti/Zn), and TiO₂/ZnO/Sep (Ti/Zn/Sep) catalysts have been synthesized using sol–gel and chemical precipitation method. Their photocatalytic performances have been compared using Flumequine (FLQ) antibiotic. X-ray diffraction (XRD), Fourier transform infrared spectra (FTIR), scanning electron microscopy (SEM), N₂-adsorption, and the determination of a zero point charge has been used to characterize the synthesized catalysts. The degradation studies showed that the catalytic efficiency of Ti/Zn/Sep is higher than that for other catalysts. The operational parameters such as pH, initial FLQ concentration, and catalyst dosage were evaluated. UV–vis and high-resolution mass spectroscopy (HRMS) analyses were used to determine the degradation efficiency and products. ZnO played a major role in the FLQ degradation process, and sepiolite contributed to adsorption of FLQ on the catalyst surface enormously. The catalysts exhibited 11%, 23%, 63%, and 85% degradation efficiency for ZnO, TiO₂, Ti/Zn, and Ti/Zn/Sep in the decomposition of FLQ, respectively.