凹凸棒负载纳米TiO2的制备、表征及其光催化性能研究

TiO2光催化剂的固定化研究对其大规模工业化应用具有重要的实际意义.通过在TiO2溶胶中浸渍的方法,制备了天然粘土矿石凹凸棒负载的TiO2光催化剂.并采用TEM、XRD等分析手段对TiO2纳米管的形貌和晶相进行了表征.对比了负载后的光催化剂在制备方法、热处理温度、光催化剂的投加量及其模拟废水溶液不同时对其光催化剂性能的影响,并且验证了该光催化剂的可重复利用性.     

自悬浮定向流法制备纳米Fe微粒的粒度控制

采用自悬浮定向流技术制备了金属Fe纳米微粒,对样品平均粒度进行TEM等测试分析,研究了主要制备工艺条件对微粒粒径的影响。结果表明,自悬浮定向流技术可用以制备出不同粒度的金属Fe纳米微粒,其平均粒径随熔球温度的降低和冷却气体流速的增大而减小;在1500℃左右时,微粒平均粒径随冷却惰性气体Ar压强的增大而减小,而在1600℃时,气体压强对微粒平均粒径的影响不再具有规律性。     

High-efficiency mechanochemical synthesis of Strontium carbonate nanopowder from Celestite

In this study, the conversion of Celestite to SrCO₃ was studied by wet mechanochemical synthesis in a high-energy ball mill and treatment with Na₂CO₃. For this purpose, solid strontium carbonate and soluble Na₂SO₄ were obtained after wet milling of Celestite powder and sodium carbonate. The solid phase was washed with water at room temperature by filter pressing. X-Ray diffraction patterns showed that the SrCO₃ nanopowder was synthesized and conversion boosted with increasing the milling time up to 8 hours Also, Rietveld refinement analysis was used to calculate the fraction of SrCO₃ as well as structural properties of synthesized samples. It was found that initial Celestite could be converted to strontium carbonate with a purity more than 98% using high-energy milling without simultaneous heating. The optimum milling time was determined as 4 hours resulting in formation of nanopowders with an average particle size around 90 nm. Field Emission Scanning Electron Microscopy (FE-SEM), clearly showed the nanoscale structure of the synthesized powders.     

Dy纳米粉含量对烧结Nd-Fe-B磁体的影响

为了改善烧结Nd-Fe-B磁体的磁性能和力学性能,采用二元合金法添加Dy纳米粉制备了高性能Nd-Fe-B磁体.利用扫描电子显微镜、X射线衍射仪、粒度分布仪、磁滞回线测试仪与维氏硬度仪对烧结Nd-Fe-B磁体的形貌、微观结构、化学成分、磁性能和力学性能进行了分析.结果表明,随着Dy元素质量分数的增加,磁体矫顽力大幅提高,剩磁和最大磁能积略有下降.相比未添加Dy元素的磁体,当Dy元素质量分数为0.8%时,磁体矫顽力提高了5.4%,剩磁和最大磁能积分别下降了1.3%和1.5%,维氏硬度提高了7.1%,此时磁体的综合磁性能最优.     

钛酸钡纳米粉的低温合成研究

结合溶胶．凝胶法和水热法的优点，将溶胶处理引入水热法中，采用改进的水热法在低温条件下合成了纯钙钛矿结构钛酸钡纳米粉，并与水热法合成产物进行了适当的比较。通过XRD，TEM，X射线荧光光谱(XRF)，微分扫描式量热法(DSC)以及热重分析(TGA)分析了BaTiO3粉的结构和组成，并初步探讨了溶胶处理的作用。结果表明，采用乙酰丙酮改性的钛酸四丁酯作为Ti源，可有效降低BaTiO3纳米粉的水热合成温度；与常用水热法相比，采用改进的水热法合成BaTiO3纳米粉的温度更低。溶胶处理过程有利于水热合成温度的降低。     

Preparation of highly dispersed antimony-doped tin oxide nanopowders by azeotropic drying with isoamyl acetate

Antimony-doped tin hydroxide colloid precipitates were prepared by hydrolysis of SnCl4·5H2O and SbCl3 ethanol solutions. Isoamyl acetate was selected as azeotropic drying solvent and was compared with the most commonly used n-butanol solvent on treating precipitate for low hard agglomeration precursor powders. The FT-IR, BET, XRD, and TEM results of the precursor powders and calcinated antimony-doped tin oxide powders were recorded. The results demonstrate that isoamyl acetate is an excellent azeotropic drying solvent that can effectively prevent the agglomeration of particles and greatly improve the fluffiness of the obtained dried powders. After these precursor powders are calcined, antimony-doped tin oxide nanopowders with tetragonal futile structure and high dispersivity can be obtained.     

纳米Cu粉对Nd_2Fe_(14)B磁性材料性能的影响

为了提高磁性材料的耐腐蚀性和力学性能,采用二元合金法制备了Nd2Fe14B磁性材料.利用X射线衍射仪、扫描电子显微镜、粒度分布仪和磁性材料测试设备分别对样品进行了性能检测.结果表明,添加纳米Cu粉后,Nd2Fe14B磁性材料的性能得到了明显的改善.当纳米Cu粉的质量分数为0.25%时,样品的剩磁、矫顽力、磁能积均得到了不同程度的提高;样品的晶界十分清晰,晶粒尺寸趋于均匀化;样品的耐腐蚀性能得到了明显的改善,且样品在0.005 mol/L的H2SO4溶液中腐蚀96 h后的质量损失仅为0.021 7 g/cm3.     

缓冲溶液法制备钴酸锶钐阴极材料及其性能

以硝酸盐为前驱体,NH3·H2O-NH4HCO3为沉淀剂,用缓冲溶液法制得了Sm1-xSrxCoO3复合沉淀物,将其在800～1 000℃不同温度煅烧5 h.用X射线衍射、透射电镜对煅烧产物的相组成和微观形貌进行了测定.所制备的(Sm1-xSrxCoO3)粉体模压成形后,在1 000～1 200℃进行烧结.用Archimedes排水法测定了烧结体的密度和孔隙率.用扫描电镜对烧结体的微观结构进行了观测.用直流四端子法测定了烧结样品的电导率.实验结果表明:缓冲溶液法所获得的沉淀物在800℃煅烧形成了具有钙钛矿结构的Sm1-xSrxCoO3粉体,其粒度均匀细小,形状规则.在一定的烧结温度,Sm1-xSrxCoO3烧结体具有多孔结构.随着烧结温度的增加,烧结体密度增大,孔隙率和孔径减小.Sr的掺入,使Sm1-xSrxCoO3烧结体的电导率明显高于未掺杂的SmCoO3.在500～800℃,Sm1-xSrxCoO3材料的电导率随温度的增高而降低.在500℃,样品Sm0.6Sr0.4CoO3的电导率可达2 700 S·cm-1.     

均匀沉淀法制备纳米氧化镁粉体的试验研究

以六水氯化镁和尿素为原料,以聚乙二醇辛基苯基醚为分散剂,采用均匀沉淀法制备出颗粒直径约为20～30 nm的氧化镁粉体.通过四因素三水平正交试验确定了液相反应条件对纳米氧化镁晶粒直径的影响程度和最佳液相合成条件.结果表明,影响纳米氧化镁晶粒直径的液相反应因素主次顺序依次为:反应物(六水氯化镁)浓度、反应时间、反应物配比(尿素和六水氯化镁的物质的量比)及反应温度.以纳米氧化镁粉体晶粒直径为控制指标的最佳液相反应条件为:反应物浓度1.5 mol/L,反应时间3 h,反应物配比5:1,反应温度99℃.     

Eu掺杂TiO_2纳米晶光致发光影响因素

为了寻找Ti O2∶Eu3+纳米晶的最佳制备工艺条件,采用溶胶-凝胶法制备了Ti O2∶Eu3+纳米晶,研究了Eu3+掺杂浓度、退火温度、Al3+的掺入等工艺参数对Ti O2∶Eu3+纳米晶发射光谱的影响.利用PL、PLE对样品进行了表征.结果表明用468 nm激发光源激发Ti O2∶Eu3+纳米晶时,样品显示出强红光发射,对应于Eu3+粒子的5D0→7F2超灵敏跃迁;且荧光强度随着Eu3+掺杂浓度和退火温度的升高先增强后减弱;700℃退火的样品红光发射强度达到最强,Eu3+的最佳掺杂浓度为0.8%mol;Al3+的掺入可以提高Eu3+的红光发射强度,采用钛酸正四丁脂∶异丙醇∶冰乙酸∶水=1∶4∶4∶2制备出的Ti O2:Eu3+纳米晶的红光发射光谱最强.