核壳结构Au@SiO2的可控制备及应用于SERS检测多环芳烃

以金纳米粒子为内核,硅酸钠为硅源,采用自组装法制备了Au@SiO₂核-壳结构,考察了不同反应时间对核壳结构的影响。以4-巯基苯甲酸(4-MBA)为探针分子测试不同厚度Au@SiO₂核壳的表面增强拉曼散射光谱(SERS)性能。通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)和紫外分光光度计对核壳结构进行表征。结果表明,采用自组装法制备的Au@SiO₂核壳结构粒径均一、稳定性好、壳层厚度可控且对多环芳烃(PAHs)具有吸附能力。将Au@SiO₂核壳结构用于嵌二萘的SERS检测,检出限低至0.1μg/mL。制备的Au@SiO₂核壳结构可以进一步应用于痕量物质的检测。     

Sb2S3纳米粒子修饰ZnO纳米片微纳分级结构的光电化学性能

采用恒电位方法,选择氯化钾和乙二胺(EDA)为添加剂,在氧化铟锡(ITO)导电玻璃上制备了高度有序的ZnO纳米片阵列,通过二次电沉积得到了ZnO纳米片上生长纳米棒的微纳分级结构.利用化学浴沉积法在ZnO基底上沉积Sb₂S₃纳米粒子制备出了Sb₂S₃/ZnO纳米片壳核结构和Sb₂S₃/ZnO微纳分级壳核结构.利用扫描电子显微镜(SEM)、X射线衍射(XRD)、紫外-可见(UV-Vis)吸收光谱、瞬态光电流等对其形貌、结构组成和光电化学性能进行了表征和分析.结果表明, Sb₂S₃/ZnO纳米片上生长纳米棒分级壳核结构的光电流明显高于Sb₂S₃/ZnO纳米片壳核结构.在Sb₂S₃/ZnO纳米片壳核结构和Sb₂S₃/ZnO微纳分级壳核结构的基础上旋涂一层P3HT薄膜形成P3HT/Sb₂S₃/ZnO复合结构,以上述复合结构薄膜为光活性层组装成杂化太阳电池,其中, P3HT/Sb₂S₃/ZnO分级壳核结构杂化太阳电池的能量转换效率最高,达到了0.81%.     

SiO2@Fe2O3核-壳结构催化剂的制备及表征

采用优化的Stöber法制备了平均粒径为230 nm的单分散球形SiO₂颗粒,并以此为内核,通过水解沉积法制备了不同壳层厚度的核-壳结构SiO₂@Fe₂O₃催化剂。采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、N₂物理吸附和X射线衍射分析(XRD)等手段对催化剂进行表征,探讨了不同制备条件对SiO₂@Fe₂O₃催化剂形貌的影响。结果表明,通过水解沉积法制备的SiO₂@Fe₂O₃催化剂具有明显的核-壳结构,并且保持了原始SiO₂核的球形形貌,Fe₂O₃纳米粒子通过-OH的氢键作用连接在SiO₂表面,形成了2~10 nm厚的Fe₂O₃均匀连续包覆层。     

金纳米壳球体的制备及其潜在的生物学应用

利用分子自组装和胶体还原化学制备出具有核-壳结构的金纳米壳球体Au@SiO₂; 通过透射电子显微镜(TEM)、X射线光电子能谱 (XPS)和紫外-可见分光光度计对Au@SiO₂的制备过程及其在全血中的光学特性进行了研究. 结果表明, 通过改变复合颗粒Au-APTES-SiO₂的浓度, 可以得到具有合理核-壳比例的Au@SiO₂, 其等离激元共振峰位于光谱的近红外区, 这使得具有红外消光特性的金纳米壳球体具有潜在的生物学应用价值.     

Zn-MOF模板法制备ZnO/C/SNTs及其药物缓释性能

采用超声法一步合成了SiO₂包覆金属-有机骨架[Zn₆(OH)₃(BTC)₃(H₂O)₃] ·7H₂O(Zn-MOF, BTC=1,3,5-均苯三羧酸根)纳米晶, 在N₂保护下, 热解Zn-MOF@SiO₂获得了ZnO/C/SNTs复合物, 进而与布洛芬(HIBU)反应合成药物组装体Zn(IBU)₂/C/SNTs. 通过透射电子显微镜(TEM)、 傅里叶变换红外光谱仪(FTIR)、 高分辨透射电子显微镜(HRTEM)和X射线衍射仪(XRD)对样品的结构和形貌进行表征. 结果显示, Zn-MOF@SiO₂呈棒状, 具有清晰的核/壳结构, 形貌单一, 分散性良好. 煅烧后SNTs结构稳定, 形貌基本不变. 载药实验表明, 药物组装体的载药量为752 mg/g, 并具有良好的pH响应性能.     

手性聚苯胺/二氧化硅核/壳复合物的合成及应用

以苯胺为单体,右旋樟脑磺酸为手性掺杂剂制备了手性聚苯胺[(+)-PANI];以(+)-PANI为核,表面包覆二氧化硅外壳,得到手性聚苯胺/二氧化硅核/壳复合物[(+)-PANI@SiO_2].采用比旋度([α]t D)、紫外-可见光谱(UV-Vis)及圆二色谱(CD)等表征光学活性,结果表明,(+)-PANI及(+)-PANI@SiO_2均具有手性;红外光谱(IR)表明,二氧化硅已经包覆于(+)-PANI表面;扫描电子显微镜(SEM)结果表明,(+)-PANI@SiO_2为核/壳结构.将(+)-PANI和(+)-PANI@SiO_2分别用于丙氨酸对映体选择性结晶,L-丙氨酸均优先结晶,且(+)-PANI@SiO_2手性识别能力更强.以光学活性聚苯胺为核,无机二氧化硅为壳的核/壳复合物在手性识别领域具有潜在的应用价值.     

Ag/mSiO2空心微球的制备及SERS标记性能

以聚苯乙烯微球为模板, 经过原位还原和种子生长过程在聚苯乙烯微球表面包覆银(Ag)纳米粒子; 以正硅酸乙酯为硅源, 在十六烷基三甲基溴化铵的导向下实现介孔二氧化硅(mSiO₂)可控包覆, 去除模板得到Ag/mSiO₂空心微球. 透射电子显微镜(TEM)和氮气吸附-脱附分析结果表明, SiO₂壳层厚度约为20 nm, 介孔孔径为2.1 nm, 孔道分布均匀. 进一步利用虹吸作用使对巯基苯胺(4-ATP)分子进入微球内与Ag粒子结合, 构建表面增强拉曼散射(SERS)标记材料. SERS测试结果表明, 该标记材料检测限达到10^-7 mol/L, SERS增强因子达到3.7×10⁵.     

中空碳球负载TiO2纳米颗粒用于增强光催化抗菌性能

以聚吡咯包覆聚苯乙烯核壳结构衍生的中空碳球(hollow carbon spheres,HCS)为载体,乙酰丙酮钛(TOAC)为钛源,通过湿化学法和可控热解法制备了HCS负载纳米二氧化钛(HCS@TiO₂)复合材料。通过粉末X射线衍射、紫外可见光谱、X射线光电子能谱、热重分析、扫描电子显微镜、透射电子显微镜、光致发光光谱和Mott-Schottky曲线对HCS@TiO₂的晶态结构、微观形貌、光学性能等进行表征,并通过调控TiO₂的负载量和热解温度对HCS@TiO₂复合材料进行了结构优化。在模拟太阳光照射条件下,以大肠杆菌(E. coli)和金黄色葡萄球菌(S. aureus)为实验对象,研究了不同TiO₂负载量的HCS@TiO₂复合材料及TiO₂和HCS对照样品的光催化抗菌性能,以及光照时间对抗菌性能的影响。结果表明,当TOAC与HCS质量比为15∶1、热解温度为650℃时,最优化的HCS@TiO₂-15复合材料...     

中空多壳层CoFe2O4的制备及锂离子电池性能研究

以二元金属氧化物CoFe₂O₄为研究对象,通过次序模板法制备了CoFe₂O₄中空多壳层结构(HoMS)材料;对其形貌、结构进行了表征;考察了壳层结构与电化学性能之间的关系.电化学测试结果表明,双壳层-核CoFe₂O₄中空球具有最高的放电比容量(1354.4 mA·h/g)、优异的倍率性能和循环稳定性,其独特的结构优势和最优的空腔体积占有率使其在多次循环过程中能始终保持结构和电化学性质的稳定.     

新型核壳结构纳米催化剂的三效催化活性及热稳定性

从Pd纳米粒子出发制备了具有核壳结构的新型纳米Pd@SiO₂/Ce_0.4Zr_0.6O₂三效催化剂及作为参比的Pd/Ce_0.4Zr_0.6O₂催化剂, 采用X射线衍射、 透射电子显微镜、 氢气程序升温还原和氮气低温吸附-脱附等技术对催化剂的物化性质进行了表征, 研究了Pd@SiO₂/Ce_0.4Zr_0.6O₂和Pd/Ce_0.4Zr_0.6O₂催化剂的三效反应催化活性和热稳定性. 结果表明, SiO₂壳层可以抑制Pd粒子的团聚, 同时还能抑制Pd物种的再分散, 减少Pd的流失. 具有核壳结构的纳米Pd@SiO₂/Ce_0.4Zr_0.6O₂催化剂具有更好的三效催化活性和更高的热稳定性.     

共缩聚法制备有序介孔氧化硅纳米螺旋纤维

在传统球状介孔氧化硅合成工作的基础上,以正硅酸乙(TEOS)和γ-巯丙基三甲氧基硅烷(MPTMS)为硅源,在水体系下利用共缩聚法一步合成出具有介孔分子筛结构特征的纳米纤维,并通过扫描电子显微镜(SEM)、小角X射线衍(XRD)、透射电子显微镜(TEM)和氮气吸附-脱附实验对样品进行了表征与分析.     

均匀共沉淀法制备BaTiO3 -Nix Zn1-x Fe2 O4 核-壳粒子及其性能

以尿素为沉淀剂, 在无后续热处理的情况下, 采用均匀共沉淀法制备了BaTiO3-NixZn1-xFe2O4核-壳粒子. 采用透射电子显微镜(TEM)、 X射线衍射仪(XRD)、 能谱仪(EDS)及振动样品磁强计(VSM)对BaTiO3-NixZn1-xFe2O4核-壳粒子的形貌、 结构、 成分和磁性能进行了表征. 结果表明, 制备的核-壳结构粒子中NixZn1-xFe2O4壳层在BaTiO3颗粒的表面包覆完整. 通过控制共沉淀中NiCl2·6H2O与ZnCl2的摩尔比可以调控BaTiO3-NixZn1-xFe2O4核-壳粒子的磁性; 加入的NiCl2·6H2O与ZnCl2摩尔比为7∶3时制得的核-壳粒子具有较好的磁性能, 其饱和磁化强度和矫顽力分别为26.999 A·m2/kg和902.787 A/m.     

羧基化核壳磁性纳米Fe3O4吸附剂的制备及对Cu2+吸附性能

在以共沉淀法制备的磁性纳米Fe3O4粒子(Magnetic nanoparticles, MNP)表面进行了化学修饰, 制备了一种新型富含羧基功能团的核壳磁性纳米吸附剂(Carboxylic functionalized Fe3O4 magnetic nanoparticles, CMNP). 利用透射电子显微镜(TEM)、 X射线衍射仪(XRD)、 X射线能量色散谱(EDS)、 振动样品磁强计(VSM)、 傅里叶变换红外光谱(FIIR)和热重分析仪(TGA)对CMNP的形貌、 结构、 化学组成和磁性能进行了表征, 并考察了吸附剂对Cu2+的吸附性能, 研究了溶液pH值、 吸附时间和Cu2+初始浓度对吸附性能的影响. 结果表明, 羧基化核壳磁性纳米Fe3O4颗粒的平均粒径为15 nm, 具有良好的超顺磁性, 饱和磁化强度为41.84 A·m2/kg, 在10 min中内可达到吸附平衡, 在pH=7.0时吸附量最高, 吸附等温数据符合Langmuir模型, 饱和吸附量qm= 43.48 mg/g.     

Sonochemical Processes and Formation of Gold Nanoparticles within Pores of Mesoporous Silica

Mesoporous silica with gold nanoparticles inside its pores was prepared by the soaking and ultrasound-induced reduction method. This new composite was characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), and high-resolution transmission electron microscopy (HRTEM) techniques. The results showed that nearly spherical-shaped gold nanoparticles, with mean size in diameter of 5.2 nm, are located in the pores, most of which are less than 6 nm in diameter. The ultrasonic irradiation time dependence of optical absorption for the soaked porous solid sample, as suggested by the variation in absorbance at 310 and 544 nm, indicated the reduction of Au (III) ions, and the nucleation and aggregation of gold nanoparticles within pores of mesoporous silica. Additionally, the reaction rates estimated phenomenologically by the absorbance decay at 310 nm for both the porous sample and the corresponding soaking solution presented the enhancement of the sonochemical reduction rate of Au (III) ions within pores of mesoporous silica. It is assumed that the extensive liquid-solid interfacial zones in the pores, due to the high specific surface areas and great porosity of the mesoporous solid, are the major regions where the efficient sonochemical reduction induced by the cavitation takes place. Copyright 2001 Academic Press.     

Hematite template route to hollow-type silica spheres

Hollow-type silica spheres with controlled cavity size were prepared from Fe₂O₃-SiO₂ core-shell composite particles by selective leaching of the iron oxide core materials using acidic solution. The spherical Fe₂O₃ core particles with a diameter range of 20-400 nm were first prepared by the hydrolysis reaction of iron salts. Next, the Fe₂O₃-SiO₂ core-shell particles were prepared by the deposition of a SiO₂ layer onto the surface of Fe₂O₃ particles using a two-step coating process, consisting of a primary coating with sodium silicate solution and a subsequent coating by controlled hydrolysis of tetraethoxysilicate (TEOS). The Fe₂O₃ core was then removed by dissolving with acidic solution, giving rise to hollow-type silica particles. Scanning electron microscopy clearly revealed that the cavity size was closely related to the initial size of the core Fe₂O₃ particle. According to the cross-sectional view obtained by transmission electron microscopy, the silica shell thickness was about 10 nm. The porous texture of the hollow-type silica particles was further characterized by nitrogen adsorption-desorption isotherm measurements.     

银纳米颗粒负载阶层多孔二氧化硅块体的制备及表征

以溶胶-凝胶伴随相分离法制备的阶层多孔二氧化硅作为载体,3-氨丙基三乙氧基硅烷(APTES)为改性剂,乙醇为还原剂,在阶层多孔二氧化硅固体骨架上进行银纳米颗粒均匀负载.利用扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、汞压、N2吸附/脱附、X射线光电子能谱(XPS)等测试技术对银纳米颗粒负载阶层多孔二氧化硅进行了表征,探讨了APTES表面改性、乙醇还原机理以及银纳米颗粒负载块体的孔结构特征变化规律.结果表明:APTES表面改性将氨基接枝于阶层骨架上,氨基与银离子形成银氨离子,银氨离子经乙醇还原后将平均粒径约16 nm的银纳米颗粒成功负载于二氧化硅的大孔及介孔内部;负载后的阶层多孔块体的大孔骨架未受到破坏,但其比表面积由418 m2·g-1下降到254m2·g-1,两次还原负载能提高银纳米颗粒的负载量.     

Silicon dioxide hollow microspheres with porous composite structure: synthesis and characterization

In this paper, a strategy for hollow porous silica microspheres with ideally flower structure is presented. SiO(2)/PAM hybrid composite microspheres with porous were synthesized by the reaction that the porous polyacrylamide (PAM) micro-gels immersed in tetraethoxysilane (TEOS) anhydrous alcohol solution and water in a moist atmosphere, with ammonium hydroxide as a catalyst. The SiO(2) hollow microspheres with porous were obtained after calcination of the composite microspheres at 550 °C for 4 h. The morphology, composition, and crystalline structure of the microspheres were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermo-gravimetric analysis (TGA), Fourier transform infrared spectroscopy (FI-IR), and X-ray diffraction (XRD), N(2) absorption analysis, respectively. The results indicated that the obtained hollow porous SiO(2) microspheres were a perfect flower structure.     

PMMA纳米球的制备及其银膜包覆技术

采用无皂乳液聚合法制备了单分散、直径为170 nm左右的聚甲基丙烯酸甲酯(PMMA)纳米球, 然后利用3-甲基丙烯酰氧基丙基三甲氧基硅烷(MATS)和3-巯丙基三甲氧基硅烷(MPTMS)对PMMA纳米球进行表面改性, 在其表面包覆一层均匀的巯基, 通过巯基与银离子之间的相互作用, 使银在PMMA纳米球表面成核长大, 从而合成PMMA/Ag纳米球壳粒子. 通过扫描电子显微镜、投射电子显微镜和紫外-可见吸收光谱测试技术对产物性能进行了表征, 研究结果表明, 制备的PMMA/Ag纳米球壳粒子的分散性好、包覆均匀.     

Preparation and characterization of composites built of poly(N-benzophenoyl methacrylamide-co-N-hydroxyethyl acrylamide) cores and silica raspberry-like shells with dual orthogonal functionality

The design and fabrication of novel poly(N-benzophenoyl methacrylamide-co-N-hydroxyethyl acrylamide)@SiO(2) composites are reported herein. These core-shell composites demonstrate orthogonal functionality, composed of photoreactive cores, containing a benzophenone (BPh) moiety and silica (SiO(2)) shells, enabling the utilization of the free hydroxyl groups via silane-based chemistry. The co-polymer cores, which are 1.28μm in diameter, are first obtained by dispersion polymerization of photoreactive (N-benzophenoyl methacrylamide) (polyBPMA) and N-Hydroxyethyl acrylamide (HEAA). Next, silica seeds with a 42nm diameter are deposited onto the surfaces as a result of the hydrolysis and the condensation of tetraethyl orthosilicate (TEOS) in a basic condition. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), FT-infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), UV-spectrophotometry, X-ray photoelectron spectroscopy (XPS), and ζ-potential measurements were used to characterize the composites. The morphology and surface smoothness of the deposited silica nanoparticles (NPs) were found to strongly depend on a number of parameters such as the pH value of the medium, TEOS concentration, and the temperature.