Template synthesis of 3-D bimodal ordered porous silica

A dual template synthesis combined with a modified bulk sol-gel process was used to prepare the three dimensional bimodal ordered porous silica, in which the macropore wall is mesoporous and both the pores are interconnected. The macropores were replicated from the template of the dried polystyrene colloidal crystal after being removed by calcination at high temperature, whislt the mesopores were achieved by burning off the surfactant in the gel. The ordered morphologies and interconnection of both the macropores and the mesopores were evidenced by the characterizations with SEM and TEM attached with electron diffraction. Nitrogen adsorption results also confirmed the interconnectivity, sizes and their distribution of the two sorts of pores. The effect of surfactant concentration and calcination conditions on mesopore size and its distribution was also investigated.     

Synthesis of 3-D ordered macroporous silicate using the template formed from monodispersed polystyrene latex

Based on the template formed from monodispersed polystyrene (PS) latex, a modified fast sol-gel process was employed to synthesize a three-dimensional (3-D) ordered macroporous silica material after removing the template by calcination at high temperature. It was indicated that there existed highly ordered packed pores within the whole silica material by SEM morphology observation. It was also found that the pores were interconnected. The pore size could be controlled mainly by varying the particle size of the latex ranging from 10¹ to 10² nm. The formation process of the ordered pores was also preliminarily discussed.     

三维大孔氮化碳材料的制备及其血液相容性

以粒径640 nm的单分散二氧化硅胶体晶体为模板,由四氯化碳和乙二胺回流加热制备出氮化碳的前驱物;将其填入模板的缝隙中,在氮气中热处理,形成氮化碳/二氧化硅的复合物;用氢氟酸除去二氧化硅模板,制备出三维大孔氮化碳材料. 通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射 (XRD)、选区电子衍射(SAED)、元素分析、红外光谱(FT-IR)、X射线光电子能谱(XPS),对其形貌结构、元素组成、键合状态进行了形貌和结构的表征. 采用部分凝血活酶时间(APTT)、凝血酶原时间(PT)和凝血酶时间(TT)对其体外抗凝血活性作了初步的评价,发现制备的大孔氮化碳对血液不会造成促凝,说明其可能成为一种新的血液相容性材料.     

Preparation and characterization of three-dimen-sionally ordered macroporous polystyrene via atom-transfer radical polymerization

Three-dimensionally ordered macroporous polystyrene(3DOM PS) with pore size of 350 nm was fabricated using Cp2Co/Ethyl 2-bromoisobutyrate(EBiB) catalytic system by ATRP.The resulting polymers were detected by FT-IR,1H-NMR,SEM,and GPC.The microstructure of 3DOM PS was confirmed by FT-IR and 1H-NMR.SEM micrographs show that both silica spheres within the templates and pores in the 3DOM polystyrene are arranged in highly ordered fashion,and the shrinkage of the pores in the 3DOM PS is 24%.GPC curves show that the 3DOM PS possesses slightly lower Mn and narrow MWD compared with bulk one.This result indicats that living polymerization is different from non-living polymerizationin in the confined space.     

复合模板剂制备有序介孔氧化铝

采用溶胶-凝胶法以异丙醇铝为铝源,乙醇为溶剂,非离子表面活性剂TritonX-100和三嵌段共聚物P123为复合模板剂,制备了有序介孔氧化铝。用PSD、XRD、TEM等测试技术对样品进行了结构表征,实验结果表明,合成的有序介孔氧化铝比表面积大于500m²/g,孔容超过1.0cm³/g,孔径分布窄（2～12nm）,形成的蠕虫状孔道具有一定的有序性,与采用单一模板剂P123制得的介孔氧化铝相比具有比表面积大,孔分布窄,有序性好的优点。最佳模板剂配比为 n(TritonX-100)∶n(P123)=3∶1。     

Preparation of three-dimensionally ordered macroporous perovskite materials

In this paper,we use La0.8Sr0.2MnO3 and La0.7Ca0.2Sr0.1MnO3 as examples to demonstrate a preparation method for threedimensionally ordered macroporous(3DOM) perovskite thermochromic materials.Polystyrene spheres with an average diameter of 220 nm were self-assembled into a three-dimensionally ordered colloidal crystal template.A mixed metal nitrate solution prepared using La(NO3) 3·6H2O,Ca(NO3) 2·4H2O,Sr(NO3) 2,Mn(CH3COO) 2·4H2O and an ethanol precursor was used to fill the interstitial voids of the polystyrene colloidal crystal templates.3DOM La0.8Sr0.2MnO3 and La0.7Ca0.2Sr0.1MnO3 materials were then obtained after the sphere templates were removed via drying and calcination.The results show that the framework of the 3DOM materials can have different thicknesses and pore shrinkage rates by varying the filling times.In addition,the Curie temperatures of the 3DOM and bulk La0.8Sr0.2MnO3 materials can be varied by altering the preparation method.     

高骨架填充率的SiO2有序大孔材料的制备

以SiO2有序大孔材料制备作为研究对象,系统考察了胶晶模板法中影响前驱物填充率的诸因素,包括填充方法、填充时间和填充次数.研究表明,直接浸渍法易导致大孔结构的收缩、脱落和表面覆盖.本文提出的在模板表面添加盖片再填充的方法有效解决了上述问题.当填充时间为5 min、填充次数为两次时,SiO2有序大孔材料的骨架填充率较高.扫描显微镜(SEM)和分光光度计的表征结果证实,实验成功制备了填充率高达22.53%的大面积SiO2有序大孔材料.     

中空二氧化硅微球的制备及其在超声成像中的应用研究

具有空心结构的纳米/微米二氧化硅微球由于其独特的性质,受到了广泛的关注,成为国内外科学家的研究热点.简要总结了中空二氧化硅微球的制备方法,对其在超声成像领域的研究进展进行了介绍,并对该领域的发展前景做出了展望,为其进一步研究提供了参考.     

Preparation and characterization of three-dimensionally ordered macroporous polystyrene <Emphasis Type=Italic>via</Emphasis> atom-transfer radical polymerization

Three-dimensionally ordered macroporous polystyrene （3DOM PS） with pore size of 350 nm was fab- ricated using Cp2Co/Ethyl 2-bromoisobutyrate （EBiB） catalytic system by ATRP. The resulting polymers were detected by FT-IR, 1H-NMR, SEM, and GPC. The microstructure of 3DOM PS was confirmed by FT-IR and 1H-NMR. SEM micrographs show that both silica spheres within the templates and pores in the 3DOM polystyrene are arranged in highly ordered fashion, and the shrinkage of the pores in the 3DOM PS is 24%. GPC curves show that the 3DOM PS possesses slightly lower Mn and narrow MWD compared with bulk one. This result indicats that living polymerization is different from non-living polymerizationin in the confined space.     

Synthesis of carbon nanotube arrays using ethanol in porous anodic aluminum oxide template

Carbon nanotube (CNT) arrays confined by porous anodic aluminum oxide (AAO) template were synthesized using ethanol as reactant carbon source at low pressure. Images by scanning electron microscope (SEM) and low magnification transmission electron microscopy (TEM) show that these CNTs have highly uniform outer diameter and length, absolutely controlled by the diameter and depth of nano-channel arrays of the AAO. High resolution transmission electron microscopy (HRTEM) imaging indicates that the graphitization of the CNT walls is better than the results reported on this kind of template-based CNT arrays, although it is not so good as that of multiwalled carbon nanotubes (MWCNTs) synthesized by catalysis. CNTs synthesized using acetylene as reactant gas show much less graphitization than those prepared using ethanol by comparing the results of HRTEM and Raman spectroscopy. The etchingeffects of decomposed OH radicals on the amorphous carbon and the roughness of AAO nano-channel arrays on the CNTs growth were employed to explain the graphitization and growth of the CNTs.     

聚合物微球支载手性磺酰二胺的合成研究

以苯甲醛为原料,经安息香缩合、氧化、成环、还原、手性拆分、磺酰化反应制备含有双键的手性磺酰二胺分子,与苯乙烯和二乙烯基苯共聚制备聚苯乙烯支载手性磺酰二胺微球,总产率8.1％.用IR,1H NMR,13C NMR及元素分析对其结构进行表征,波谱解析结果与化合物结构相符.     

磺酸基键合硅胶的制备及其酸催化性能研究

以氯丙基氯硅烷和苯基氯硅烷为偶联剂对硅胶进行表面改性,进一步磺化得到以磺酸基为活性中心的固体酸,磺化剂分别为硫酸和亚硫酸铵。以BET、红外光谱、总有机碳对固体酸及其前驱体进行了表征并测定了固体酸酸密度;利用总有机碳计算前驱体的键合量,苯基、氯丙基硅胶键合量分别为1.40mmol/g,1.95mmol/g;以这两种前驱体制得的固体酸酸密度分别为0.32mmol/g,0.26mmol/g;BET数据表明键合反应发生后苯基磺酸和丙基磺酸样品的比表面积由521m2/g降至406m2/g,432m2/g。将制得固体酸应用于乙酸丁酯的合成,经五次使用仍保持较高转化率。     

利用廉价硅酸盐为硅源合成微米级球形介孔二氧化硅

利用廉价的硅酸盐为二氧化硅前驱体,以非离子和阳离子表面活性剂为混合模板剂合成微米级的介孔二氧化硅,控制非离子和阳离子表面活性剂的量可以得到分散性较好的介孔二氧化硅球,并用SEM,XRD以及N2吸附-脱附,对所得介孔二氧化硅材料的宏观形貌和微观结构进行了表征。讨论了2种表面活性剂的比例对介孔二氧化硅形貌的影响,并用混合模板机理解释了球形介孔材料形成的原因。     

六方介孔硅基分子筛SBA-3合成条件的优化与表征

采用X射线衍射、N2 吸附脱附、热重热差分析方法 ,考察了合成物体系中表面活性剂与硅源的量之比、反应温度、晶化时间、酸度及共溶剂等反应条件对SBA - 3硅基介孔分子筛合成过程中结晶度、比表面积及热稳定性的影响 ,并筛选出较佳的反应条件。结果表明 ,以正硅酸乙酯为硅源 ,十六烷基三甲基溴化铵为结构模板剂时 ,表面活性剂与硅源的量之比在 0 .12～ 1.2时 ,均可得到六方相介孔材料。最佳合成条件 :较强酸性介质 (pH值为 - 0 .6 )、反应温度为 0℃、晶化时间为 2 4h。对共溶剂的考察发现 ,三甲基苯有较好的扩孔性能 ,其加入量与表面活性剂的加入量之比为1时 ,能合成出比表面积高达 12 0 0m2 / g、晶形较好的SBA 3介孔材料。     

纳米孔硅气凝胶/聚苯乙烯核壳材料合成制备

为获得纳米孔超级绝热复合材料,采用硅烷偶联剂对原位生成的纳米孔硅气凝胶进行表面处理,通过分散聚合工艺制备出聚苯乙烯接枝包覆硅气凝胶的纳米核壳结构复合材料。通过电子显微镜(TEM)对上述纳米样品进行了表征,并就体系组分、引发剂、聚合参数和分散工艺的影响进行了讨论。结果表明:体系组分中对转化率影响最大的是硅气凝胶与苯乙烯的质量比;以有机类偶氮二异丁腈(AIBN)为引发剂,经独特的超声工艺处理,获得包覆率达70%的核壳结构复合材料。     

溶胶—凝胶模板法制备有序Mn3O4纳米线阵列

通过模板法制备的一维金属氧化物纳米结构在材料科学领域具有潜在的应用前景。以醋酸锰为前驱体,利用多孔阳极氧化铝膜(anodic aluminum oxide,AAO)为模板,通过溶胶—凝胶法成功制备出Mn3O4纳米线阵列。利用扫描电子显微镜(SEM)、X射线衍射(XRD)、热重分析技术等手段分析合成条件与产物的结构、形貌之间的关系。结果表明,所得产物为四方尖晶石结构,纳米线直径约80 nm,长度约几微米。通过测试产物的磁滞回线,发现其在常温下呈顺磁性。     

Synthesis of ordered Si nanowire arrays in porous anodic aluminum oxide templates

Highly ordered polycrystalline Si nanowire arrays were synthesized in porous anodic aluminum oxide (AAO) templates by the chemical vapor deposition (CVD) method. The morphological structure, the crystal character of Si nanowire arrays and the individual nanowire were analyzed by the transmission electron microscopy (TEM), scanning electron microscopy (SEM), atom force microscopy (AFM) and the X-ray diffraction spectrum (XRD), respectively. It is shown that most fabricated silicon nanowires (SiNWs) tend to be assembled parallelly in bundles and constructed with highly orientated arrays. This method provides a simple and low cost fabricating craftwork and the diameters and lengths of SiNWs can be controlled, the large area Si nanowire arrays can be achieved easily under such a way. The curling and twisting SiNWs are fewer than those by other synthesis methods.     

银改性六方介孔硅的合成及其抗菌性能研究

采用溶胶凝胶法合成了银改性六方介孔硅(AgHMS)抗菌材料,以X射线衍射(XRD)、红外(FTIR)、固体紫外漫反射(UVVis)、环境扫描(ESEM)、电子能谱(EDS)、热重(TGDTA)及N2的吸附脱附技术对材料结构和特性进行了分析,通过浊度值测定法考察了材料的抗菌性能。结果表明：AgHMS具有较好的热稳定性,银在材料中以骨架和非骨架态两种形式存在并且分散均匀。银的引入会导致六方介孔硅(HMS)载体材料的结晶度、介孔有序度、比表面积及平均孔径等的变化,模板剂及脱模温度对Si-O的红外吸收峰峰位及强度也有显著影响。抗菌实验表明：银改性六方介孔材料具有优良的抗菌性能,对金黄色葡萄球菌、芽孢杆菌、大肠杆菌及枯草杆菌的抗菌性能依次增强。抗菌剂质量浓度为0.20 mg/L时对枯草杆菌的生长可起到抑制作用;当其质量浓度为1.00 mg/L,12 h后即可实现对枯草杆菌的彻底杀灭。     

硅溶胶在固井水泥浆中的应用性能研究

对比分析了添加硅溶胶前后固井水泥浆性能的变化,以此获得硅溶胶的作用特点,为硅溶胶的推广应用提供理论依据和实验基础.结果表明,水灰比为0.44时,添加1.0%的硅溶胶就能明显改善浆体的稳定性;水灰比为0.75时,添加4.0%的硅溶胶可得到1.60 g/cm3的低密度水泥浆.随后利用ATR-IR、XRD、DSC-TG、SEM等手段分析水泥水化产物,结果表明:硅溶胶具有火山灰的作用,添加量为1.0%时已具有较明显的促凝、增加抗压强度及降低渗透率的作用;同时,它还具有一定的防高温衰退作用,在127℃单独添加1.0%的硅溶胶或在165℃将1.0%的硅溶胶与15.0%的硅粉混合使用,养护3 d后均没有明显的水泥石强度衰退发生.