层状纳米羟基磷灰石的结晶性能及形成机理

在前期利用模板剂法制备层状纳米羟基磷灰石（nano-hydroxyapatite,n-HA）的基础上,利用透射电子显微镜、X射线衍射和Fourier变换红外光谱等研究并讨论工艺参数对材料结晶性能影响以及形成机理。结果表明：反应24h后,HA晶体形成且层状结构清晰;在碱性条件下,生成的产物主要是n-HA,酸性条件下则生成CaHPO4;乙醇与水的质量比为2.0时,纳米晶体形状、大小相对均一。工艺参数的变化会影响表面活性剂的堆积参数,沿着表面活性剂模板生长的羟基磷灰石颗粒有不同的微观结构及形貌。     

曲拉通X-100微乳模板中碳酸钙-环糊精复合材料的合成研究

在非离子表面活性剂曲拉通X-100微乳模板中利用复分解反应法合成了碳酸钙-环糊精纳米复合材料。设计反应温度、反应时间、反应物浓度、环糊精浓度四因素三水平正交实验,探求得到文石、球霰石晶型的最佳工艺方法。合成产物的无机物结晶类型、有机物的成分以及晶体形貌利用X射线衍射、红外光谱、透射电子显微镜测试表征。某些反应条件下得到的复合材料具有贝壳珍珠层“砖－泥”式层状结构,本文讨论了此类结构的生成机理。     

调控表面活性剂浓度制备单分散SBA-15介孔材料

采用溶胶-凝胶水热法,调控反应参数和反应工艺制备SBA-15介孔材料。通过扫描电镜、透射电镜、X射线衍射以及氮气吸附-脱附分析表征表明,在一定范围,随着表面活性剂浓度增加,介孔材料SBA-15形貌出现由球形、陀螺形到米粒状的变化,介观有序度提高。在反应物料P123与Si物质的量比为0.012时,介孔材料的物性常数如晶面间距、比表面积、孔体积和最可几孔径较小。采用静态陈化-水热法研究不同表面活性剂浓度对介孔材料形貌演变的影响,为有效调控SBA-15介孔材料形貌提供必要依据。     

表面活性剂对氧化锌纳米棒形貌的影响与机理

分别以PEG400和PVA124为表面活性剂辅助水热法合成了氧化锌(ZnO)纳米棒.X射线衍射分析显示:产物为结晶良好的六角结构ZnO晶体,PEG400为表面活性剂制得的ZnO比PVA124为表面活性剂时的结晶性好.用透射电镜和选区电子衍射研究了不同表面活性剂对ZnO纳米棒形貌和结晶性的影响,解释了PEG400和PVA124对ZnO形貌影响的机理,并对ZnO的生长机制进行了初步探讨.     

TiO2中空纤维的制备及光催化性能

采用模板法制备了不同温度的TiO2中空纤维光催化材料,并利用X射线衍射、扫描电镜对其晶型及表面形貌进行了表征.以亚甲基蓝(MB)的脱色降解为模式反应,考察了温度对TiO2中空纤维光催化性能的影响.     

反应温度对ZnO粉体材料形貌与尺度的影响

利用水热法,以NaOH为沉淀剂,CTAB为表面活性剂,在较低温度下合成了ZnO粉体材料。用X射线衍射(XRD)、扫描电子显微镜(SEM)及粒度仪对样品的纯度、形貌和粒度进行了表征。实验结果表明:温度对产物的形貌和尺度具有重要的影响,温度越低,产物的尺度越大,得到由片组装而成的类球状结构;随着温度的升高,粒度减小,产物的组装方式发生了变化,形成了类雪花状结构,并且有棒状结构出现;除此之外,对形貌的形成机理进行了分析。     

水热反应条件对纳米钼酸银形貌的影响

以钼酸铵和硝酸银为原料,采用一步水热法制备了不同形貌的纳米钼酸银(Ag_2Mo_2O_7),探究了反应温度、反应时间、Ag NO_3浓度和表面活性剂聚乙烯吡咯烷酮(PVP)对产物结构及形貌的影响。利用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)对纳米钼酸银的物相和形貌进行了表征。结果表明,通过改变水热反应条件可以得到纳米线、纳米棒、纳米片等不同形貌的钼酸银,其中反应温度和表面活性剂PVP对纳米钼酸银的形貌影响显著。     

微乳液法制备BaF_2纳米粉体

采用CTAB/正戊醇/正辛烷/水反相微乳液体系,制备了BaF2纳米粉体.研究了微乳液体系中(水与表面活性剂的摩尔比)对BaF2尺寸和形貌的影响.用扫描电子显微镜、X射线衍射仪表征样品的形貌和结构.结果表明:所得产物粒径为80nm～800nm.     

表面活性剂浓度对介孔光催化材料的影响

利用溶胶-凝胶技术,用表面活性剂F127和钛酸异丙酯、硝酸铈、氧氯化锆制备前驱体溶胶,老化后通过煅烧去除表面活性剂形成介孔光催化材料ZrO_2-CeO_2-TiO_2。通过N2吸附脱附、红外光谱、X射线衍射、透射电子显微镜等表征发现表面活性剂浓度的变化对介孔材料的结构和性能均有影响,随浓度增加,比表面积逐渐增大,晶型由无定型变为锐钛矿型,介孔有序度增加,在反应物料F127浓度为6 mmol/L时,介孔材料的晶型、有序度最好,光催化性能最高。     

机械力化学法制备LiNi0.5Mn1.5O4粉体的研究

以Li2CO3,MnO2和Ni(OH)2·H2O为原料,采用机械力化学法制备锂离子层状结构正极材料LiNi0.5Mn1.5O4,采用X射线衍射,扫描电镜对其结构和形貌进行了表征.结果表明粉磨6 h可制备能在较低温度下发生固相反应的前驱体;前驱体于800℃煅烧6 h制备得到具有α-NaFeO2型层状有序结构的单相LiNi0.5Mn1.5O4.样品的首次放电容量为80 mAh·g-1.     

Controllable synthesis of ZnO nanostructures on the Si substrate by a hydrothermal route

In this paper, controllable synthesis of various ZnO nanostructures was achieved via a simple and cost-effective hydrothermal process on the Si substrate. The morphology evolution of the ZnO nanostructures was well monitored by tuning hydrothermal growth parameters, such as the seed layer, solution concentration, reaction temperature, and surfactant. X-ray diffraction and photoluminescence measurements reveal that crystal quality and optical properties crucially depend on the morphology of the ZnO nanostructures. The ease of synthesis and convenience to tune morphology and optical properties bring this approach great potential for nanoscale applications.     

表面活性剂存在下四氯化硅水解制备二氧化硅

多晶硅生产中主要副产物四氯化硅副产量大、腐蚀性强、难以安全处理。笔者以四氯化硅为原料,在表面活性剂存在下制备二氧化硅。研究了物料比例、反应温度、加料速率等因素对产品比表面及产率的影响,采用红外光谱仪、X射线衍射仪、比表面积测定仪和扫描电子显微镜对晶体结构、比表面积、产品的形貌进行了表征。结果表明,采用质量浓度0.5 g/L的十二烷基苯磺酸钠(SDBS)溶液为反应底物、四氯化硅加入量为1.5 mol/L(底物)、反应温度为45℃、加料速率为0.35 mol/h,反应混合物具有较好的过滤性能,并可得到粒径分布窄的二氧化硅产品,产品收率可达80%。     

DC-field-induced synthesis of ZnO nanowhiskers in water-in-oil microemulsions

ZnO nanowhiskers were successfully fabricated using DC-field induced water-in-oil microemulsions method. Phase structure, morphology and microstructure of the product were investigated by X-ray diffraction and transmission electron microscopy. Parameters in preparation process such as electric field intensity and surfactant were discussed and the product formation mechanism was studied. XRD and TEM results showed that the obtained ZnO particle was hexagonal wurtzite-type with 1-3 nm in diameter and 20-70 nm in length, and morphology of the particles was shown to be correlated not only with the electric field intensity but also with the surfactant. There was a threshold when the electric field intensity was 80 V/mm. The morphology of the particles was basically spherical before the threshold, while L/D increased with the raise of electric field intensity. ZnO nanowhiskers were obtained under mixed surfactants but spherical particles were got with a single surfactant.     

Fabrication and properties of degradable poly(amino acid)/nano hydroxyapatite bioactive composite

Poly(amino acid)/nano hydroxyapatite (PAA/n-HA) bioactive composite was prepared by in situ melting polymerization. The composition, structure and morphology as well as glass transition temperature (T_g), dynamic mechanical properties of the PAA/n-HA composite were characterized by infrared spectrometer, X-ray diffractometer, X-ray photoelectron spectroscopy, scanning electron microscope, differential scanning calorimeter, and dynamic mechanical analyzer. The results indicated that the n-HA particles were uniformly distributed into PAA matrix and some interactions were found at the interface between PAA and n-HA, and the crystallinity of PAA in the composite decreased with the increase of n-HA content. The T_g and storage modulus of the composite increased with increasing n-HA content, demonstrating that the n-HA content had obvious effects on the crystallization kinetic parameters and thermo properties of the PAA/n-HA composite. In addition, the n-HA amount had evident effects on the degradation of the PAA/n-HA composite in phosphate buffered saline (PBS), and the weight loss ratio of the composite decreased with the increase with n-HA content. The pH value of the medium was stable around 7.40 after the composite immersion into PBS for 8 weeks. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Study on the surface-modification of nano-hydroxyapatite with lignin and the corresponding nanocomposite with poly (lactide-co-glycolide)

To obtain nano-hydroxyapatite/poly(lactide-co-glycolide) (n-HA/PLGA) nanocomposite with superior mechanical properties, here, lignin was chosen to surface-modify for n-HA through co-precipitation method. The different reaction conditions of reaction time, phosphorus source, and the lignin addition amount were studied by fourier transformation infrared spectra, X-ray diffraction, the intuitionistic dispersion experiment, transmission electron microscope and thermal gravimetric analysis. The reaction mechanism and the best appropriate reaction condition were obtained. More importantly, the results of electromechanical universal tester, scanning electron microscope, differential scanning calorimetric analyzer, polarized optical microscopy and dynamic mechanical analysis confirmed that the obtained n-HA could greatly increase the mechanical strength of PLGA, owing to the excellent dispersion and promotion crystallization effect. Moreover, in vitro cell culture experimental results indicated that the n-HA surface-modified by lignin was favorable to improve the cell biocompatibility of PLGA. The study suggested that the introduction of lignin was a novel method to acquire a highly dispersed n-HA, which would provide a new idea to achieve the n-HA/PLGA nanocomposite as bone materials in future, and it would pave the way towards a new application of lignin in biomedical field.     

空心钛酸钡的制备及其形成机理

以二氧化钛（TiO₂）和八水合氢氧化钡[Ba（OH）₂·8H₂O]为原料,采用水热合成法,成功制备出具有四方相晶型和空心形貌结构的钛酸钡粉体。利用透射式电子显微镜（TEM）和X射线衍射（XRD）对样品的形貌结构和晶型做了表征,通过研究反应过程中钛酸钡粉体的结构和晶型随时间的变化过程,对空心钛酸钡的形成机理做了详细的探讨,并考察了不同反应温度和钡浓度对钛酸钡粉体结晶和生长的影响。研究结果表明：反应温度和钡浓度会影响钛酸钡粉体的晶型和形貌,并以此提出了一种空心钛酸钡的形成机理;当反应温度为180 ℃、钡浓度为3.0 mmol/L时,能获得粒径分布均匀的四方相晶型的空心钛酸钡粉体。     

多孔球形羟基磷灰石生物材料的制备

研究了一种作为药物载体的多孔球形羟基磷灰石生物材料的制备工艺。采用微乳液法先制得多孔球形碳酸钙,并以此为模板与磷酸氢二钠在一定条件下反应制备出直径约10μm的多孔球形羟基磷灰石。通过X射线衍射,扫描电子显微镜等手段对制备的羟基磷灰石的结构、组成和形貌进行表征,考察了不同反应温度、表面活性剂浓度、反应时间对多孔球形貌的影响,并对反应机理进行了初步探讨。结果表明,当制备多孔球形碳酸钙模板的温度为25℃、吐温-80浓度为3％且碳酸钙与磷酸氢二钠反应时间为30h时,得到的羟基磷灰石为5-10μm、分散性好的球形晶体。     

SnO2/ZnO复合中空纤维材料的制备及其光催化性能

采用天然棉花为模板制备了具有高光催化活性的SnO2/ZnO复合中空纤维光催化材料;利用X-射线衍射(XRD)、扫描电子显微镜(SEM)技术对其相结构和形貌进行了表征;以亚甲基蓝(MB)的脱色降解为模型反应,考察了Sn4+和Zn2+物质的量比为0.1∶1时煅烧温度对其催化性能的影响。实验结果表明:制备的样品为复制了棉花纤维模板形貌、具有中空结构的SnO2和ZnO半导体复合材料(SnO2/ZnO);煅烧温度对材料SnO2/ZnO的结晶度、晶粒大小﹑表面微结构和催化性能等有显著影响;650℃左右所得样品在太阳光下的催化活性最好,1 h可使MB溶液的脱色降解率达100%;该材料易于离心分离,具有良好的催化活性和重复使用性能。     

The pillaring effect of the 1,2-dimethyl-3(benzyl ethyl iso-butyl POSS) imidazolium cation in polymer/montmorillonite nanocomposites

A polyhedral oligomeric silsesquioxane (POSS) tethered imidazolium surfactant was used to exchange montmorillonite for the preparation of polymer nanocomposites in polystyrene, poly(ethylene-co-vinyl acetate), and polyamide-6 using a melt blending technique. Simultaneous temperature resolved small angle X-ray scattering and wide angle X-ray diffraction was used to monitor the surfactant stability and phase behavior of the polyamide-6 nanocomposites. Good thermal stability of the surfactant was in agreement with thermogravimetric analysis. Transmission electron microscopy revealed a mixed intercalated/exfoliated structure, with the presence of small tactoids exhibiting gallery spacings greater than 3.8 nm in all three polymers. Fluorescently tagged organically exchanged montomorillonite was used to assess the quality of nanoparticle dispersion. Exchanging the montmorillonite with lower loadings of the POSS surfactant slightly increased the size of clay tactoids, but did not significantly alter the gallery spacing or overall dispersion. The results suggest that the bulky and rigid structure of POSS, as well as its tendency to aggregate into ordered crystals, form a bilayer structure in the clay galleries and prevent montmorillonite from completely exfoliating, even in polyamide-6.