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1.
采用微波辅助水热法制备介孔分子筛MCM-41,并用浸渍法将左氧氟沙(LVFX)组装在MCM-41均一的六方形孔道中,制备出新型载药复合物LVFX/MCM-41.用粉末X射线衍射(XRD)、低温氮吸附、傅里叶变换红外光谱(FTIR)及差热-热重(TGA-DTA)分析对MCM-41以及LVFX/MCM-41复合物进行表征,合成的介孔分子筛MCM-41的孔径为2.382 nm,比表面积为1 015 m2·g-1.对MCM-41、LVFX/MCM-41、LVFX(固态)及LVFX(溶液)的荧光光谱研究结果显示,LVFX/MCM-41的荧光光谱比组装前发生明显红移,表明MCM-41孔道内表面的羟基和LVFX形成氢键,羟基上的电子云向LVFX分子上的吸电子基团转移;同时MCM-41和LVFX之间形成新环,使电子云能在更大的环上移动,药物分子的共轭体系扩大,荧光光谱峰红移.MCM-41与左氧氟沙星之间强的相互作用为研发以MCM-41为载体的新型释药系统提供了理论依据.  相似文献   

2.
将稀土有机配合物Eu(BA)3组装进介孔MCM-41中,得到有机-无机杂化介孔材料Eu(BA)3-MCM-41。采用XRD、IR、激发、发射光谱等测试方法对其结构和性能进行了分析。结果表明,组装体保持了有序的介孔骨架结构,由组装体IR谱图中波数3451cm-1吸收峰的消失及970cm-1吸收峰强度的降低可知,介孔中Eu(BA)3的引入使得配合物自身含有的结晶水、MCM-41中的吸附水和羟基数目减少,由于Eu(BA)3与—OH在介孔孔道中成键使羟基减少,降低了Eu3 的发光猝灭效应,提高了Eu3 的发光效率。组装体中主客体之间存在较强的相互作用,MCM-41的存在使Eu(BA)3对激发光有更强吸收,且使Eu(BA)3-MCM-41的发光强度较Eu(BA)3有显著的提高。  相似文献   

3.
在室温下,以掺Yb3+的MCM-41作为主体,"热处理"后的Tb(aspirin)3phen作为发光客体,将其进行组装,通过XRD和N2-吸附脱附和IR对组装体的结构和物理性质进行了研究.利用激发和发射光谱分析了组装体的光致发光性能和主客体关系.采用了一种新型的掺杂方法"直接焙烧法",用以避免在试样合成中掺杂离子的损失.在Yb/MCM-41和Tb(aspirin)3phen-Yb/MCM-41的XRD谱图中同时在20=2.6时出现了(100)晶面衍射峰,表明试样为规则有序,六方结构的MCM-41材料.Tb(aspirin)3phen进入Yb/MCM-41孔道后,无机骨架的有序性进一步增加.相对于MCM-41,Yb/MCM-41在IR谱图中波数963cm-1的谱带减弱,表明Yb3+已经进入无机骨架.另外,波数1 384 cm-1的吸收谱带也能提供组装体Tb(as-pirin)3phen-MCM-41中成键的特征信息.PL测试结果表明,Tb(aspirin)3phen在240~375 nm区间的宽激发吸收分别归属于配体aspirin羰基n→π跃迁,苯环,π→π跃迁和phen的杂菲基团吸收.对客体Tb(aspirin)3phen进行热处理,能增强Tb(aspirin)3phen在MCM-41孔道中的发光效率,并且当基质MCM-41硅骨架掺杂Yb3+后,组装体的发光强度进一步增强,当Yb/Si=7.579×10-3时,发光强度最高.  相似文献   

4.
以硅酸钠(NaSiO3·9H2O)为硅源,三甲基十六烷基溴化铵(CTAB)为模板剂在碱性条件下水热合成介孔分子筛MCM-41,然后以其为主体,采用锌盐浸渍-灼烧的方法.在介孔分子筛MCM-41上负载了氧化锌(ZnO)纳米微粒,并通过扫描电子显微镜,红外光谱(1R).紫外可见吸收光谱(UV-Vis),N2-吸附脱附和荧光光谱等手段对产品进行了系列表征.结果表明,分子筛平均直径约为1.7μm,对不同温度下灼烧后得到的ZnO/MCM-41组装体的光谱性质进行研究表明介孔分子筛MCM-41的尺寸所限,制备出的ZnO粒子粒径小于2 nm.量子尺寸效应使得ZnO/MCM-41组装体中的ZnO纳米粒子的紫外可见吸收光谱及荧光光谱均发生蓝移.通过红外光谱分析得知ZnO负载到MCM-41上并没有改变介孔分子筛原有的骨架结构.  相似文献   

5.
罗丹明6G/MCM-41纳米复合物的发光蓝移   总被引:3,自引:0,他引:3  
介孔分子筛MCM-41具有规则排列的纳米量级的孔道,可以作为宿主封装其他材料。利用这一性质,将激光染料罗丹明6G分子封装在介孔分子筛MCM-41中形成了纳米复合物。用透射电镜、小角度X射线衍射和荧光光谱等方法对纳米复合物的性质进行了分析。用波长为480nm的光对纳米复合物进行激发,得到的发光峰为531nm。与无限稀罗丹明6G乙醇溶液的发光峰相比,这一发光峰有15nm的蓝移和明显的宽化。我们认为当罗丹明6G分子封装在MCM-41的介孔中时,罗丹明6G分子与介孔分子筛孔道表面分子之间存在较强的相互作用(包括氢键、静电吸引等),导致电子云被局域在具有较强吸引力的分子筛表面原子周围。引起激发态能量升高,发光峰蓝移。  相似文献   

6.
以水热法制备了纳米微粒MCM-41分子筛,通过离子交换法将Cd(II)交换到分子筛中,然后采用硫代乙酰胺作硫化氢前驱体对(MCM-41)-Cd进行硫化,制备出主-客体复合材料(MCM-41)-CdS.化学分析表明,客体成功地组装到分子筛中.粉末X射线衍射结果表明,组装过程并未破坏所制备的主-客体材料中分子筛的骨架,分子筛骨架完整且结晶度仍然很高.红外光谱表明所制备材料骨架保持完好.低温N2吸附-解吸附研究表明,相对于MCM-41分子筛主体所制备的复合材料孔体积、孔尺寸及比表面积降低,表明客体在分子筛孔道内组装成功.制备的主-客体复合材料固体扩散漫反射吸收光谱相对于CdS体相呈现某些蓝移,说明客体处于分子筛孔道内,也表明分子筛主体对纳米硫化镉客体表现出明显的立体限域效应.(纳米MCM-41)-CdS及(微米MCM-41)-CdS样品呈现明显发光.  相似文献   

7.
胡冰  洪广言  甘树才  孔丽 《发光学报》2009,30(5):601-605
采用高温固相反应合成了Y1-x-yEuxGdyTaO4荧光体,经过XRD证明产物为纯相的M'型YTaO4结构。通过对样品的光谱测试表明,TaO3-4将吸收的能量传递给Eu3+,起着一定的敏化作用。掺入少量Gd3+对YTaO4 : Eu的发光有一定的增强作用。用147 nm的真空紫外光激发样品时,样品具有较强的荧光发射,其主发射峰位于612 nm,具有较好的色纯度。  相似文献   

8.
尹伟  张迈生  康北笙 《发光学报》2001,22(3):232-236
本文在超声波条件下以三甲基十六烷基溴化铵为模板剂,正硅酸乙酯为硅源合成了纳米级(10-40nm)的介孔分子筛(MCM-41),其筛孔直径在2.7nm左右,选择Eu(Phen)4为客体,纳米级介孔分子筛为主体,在无水乙醇中进行分子组装,制备具有强发光性能的超分子纳米材料MCM-41-Eu(Phen),采用HRTEM,TEM,XRD,TG,IR和荧光光谱检测手段对产物进行了表征。  相似文献   

9.
以光动力治疗药物玫瑰红( Rose Bengal,RB)与孔径为2.7nm的介孔二氧化硅MCM-41为主体材料进行结构组装,制备了具有生物光敏功能的介孔复合载体.对介孔复合载体的性质进行了表征,通过紫外吸收和荧光光谱对玫瑰红RB在介孔孔道内的光学性质进行了分析.由于介孔道表面与RB的相互作用,不同结构和性质的内孔道中的...  相似文献   

10.
采用连续嫁接方法对纯硅MCM-41孔道表面分别进行一次和两次TiO2修饰,并进行了硫酸根促进,制备了具有规整介孔结构的硫酸根促进型复合金属氧化物ST/MCM-41和d-ST/MCM-41;同时制备了经一次钛修饰但未经硫酸根促进的样品T/MCM-41作为对比. 利用XRD、氮吸附-脱附、元素分析、拉曼光谱和红外光谱等表征手段,对所制样品的结构和表面酸性进行考察;利用假性紫罗兰酮环化这一典型的酸催化反应对其催化活性进行评价,并与工业应用的大孔磺酸树脂Amberlyst-15进行催化性能比较. 表征结果显示,纯  相似文献   

11.
Nanosized materials loaded with organic dyes are of interest with respect to novel optical applications. The optical properties of malachite green (MG) in MCM-41 are considerably influenced by the limited nanoporous channels of nanometer MCM-41. Nanometer MCM-41 was synthesized by tetraethyl orthosilicate (TEOS) as the source of silica and cetyltrimethylammonium bromide (CTMAB) as the template. The liquid-phase grafting method has been employed for incorporation of the malachite green molecules into the channels of nanometer MCM-41. A comparative study has been carried out on the adsorption of the malachite green into modified MCM-41 and unmodified MCM-41. The modified MCM-41 was synthesized using a silylation reagent, trimethychlorosilane (TMSCl), which functionalized the surface of nanometer MCM-41 for proper host-guest interaction. The prepared (nanometer MCM-41)-MG samples have been studied by powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, low-temperature nitrogen adsorption-desorption technique at 77 K, Raman spectra and luminescence studies. In the prepared (nanometer MCM-41)-MG composite materials, the frameworks of the host molecular sieve were kept intact and the MG located inside the pores of MCM-41. Compared with the MG, it is found that the prepared composite materials perform a considerable luminescence. The excitation and emission spectra of MG in both modified MCM-41 and unmodified MCM-41 were examined to explore the structural effects on the optical properties of MG. The results of luminescence spectra indicated that the MG molecules existed in monomer form within MCM-41. However, the luminescent intensity of MG incorporated in the modified MCM-41 are higher than that of MG encapsulated in unmodified MCM-41, which may be due to the anchored methyl groups on the channels of the nanometer MCM-41 and the strong host-guest interactions. The steric effect from the pore size of the host materials is significant. Raman spectra firmly demonstrated the stable form obtained after the MG incorporation into the nanometer MCM-41. Therefore, nanometer MCM-41 appears to have a good potential for its use as a support for dyes and the (nanometer MCM-41)-MG composite materials may give a wide optical application.  相似文献   

12.
Vanadium polyoxometalate (PVMo) supported on mesoporous MCM-41, MCM-41-NH(2), as efficient and heterogeneous catalysts, with large surface area, for hydrocarbon oxidation with hydrogen peroxide is reported. Oxidation of the alkenes and alkanes gave product selectivities, which are similar to those observed for corresponding homogeneous catalyst. PVMo-MCM was prepared by introduction of PVMo into the mesoporous molecule sieves of MCM-41 by impregnation and adsorption techniques. The samples were characterized by X-ray diffraction (XRD), thermal gravimetric-differential thermal analysis (TG-DTA), FT-IR, scanning electron microscopy (SEM), UV-Vis and cyclic voltametry (CV). Ultrasonic irradiation has a particular effect on MCM-41 structural uniformity and reduced the reaction times and improved the product yields. In addition, the solid catalysts could be recovered and reused several times without loss of its activity.  相似文献   

13.
The synthesis and characterization of photoactive hybrid materials based on [Ru(bpy)3]2+ physically adsorbed within the channels of mesoporous MCM-41 silica nanoparticles is presented. A set of photoactive mesostructured hybrids with different guest loading has been prepared and characterized by X-ray diffraction, High Resolution Transmission Electron Microscopy, volumetric analyses, Diffuse Reflectance UV-Vis and Photoluminescence spectroscopies and lifetime measurements. The hybrids synthesis and the washing procedures, performed to investigate the host-guest interaction and the stability of the complex within the mesopores, didn??t affect the integrity of the structure and morphology of MCM-41 nanoparticles. The dispersion of [Ru(bpy)3]2+ within the channels varied depending on the loading value and this is reflected in the different and peculiar photoluminescence features of the resulting hybrid materials. Photoluminescence spectroscopy evidenced that the use of MCM-41 nanoparticles ensures a better dispersion of the complex within the mesopores, if compared with traditional MCM-41. Further studies are in progress to investigate the interesting and promising features exhibited by such photoactive systems for advanced applications of electrochemiluminescence in optoelectronics and diagnostics.  相似文献   

14.
In this paper, a novel luminescent organic-inorganic hybrid material containing covalently bonded ternary europium complex in mesoporous silica MCM-41 has been successfully prepared by co-condensation of tetrethoxysilane (TEOS) and the modified ligand 2-phenyl-1H-imidazo[4,5-f][1,10]phen-3-(triethoxysilyl)propylcarbamate (PIP-Si) in the presence of cetyltrimethylammonium bromide (CTAB) surfactant as template. PIP-Si containing 1,10-phenanthroline covalently grafted to 3-(triethoxysilyl)propyl isocyanate is used not only as a precursor but also as the second ligand for Eu(TTA)3·2H2O (TTA: 2-thenoyltrifluoroacetate) complex to prepare a novel functionalized mesoporous material. The resulted mesoporous composite materials, which demonstrate strong characteristic emission lines of Eu3+5D0-7FJ (J=0, 1, 2, 3, 4), were characterized by Fourier transform infrared (FT-IR), small-angle X-ray diffraction, excited-state decay analysis. Emission intensity of the Eu(III) complex covalently linked to MCM-41 (Eu-MCM-41) increases with the increasing irradiation time, demonstrating better photostability compared with both pure Eu(III) complex and physically incorporated sample.  相似文献   

15.
Strong visible photoluminescence of TEEDPS-modified silica MCM-41 materials   总被引:1,自引:0,他引:1  
The photoluminescence (PL) of mesoporous silica MCM-41 modified with triethoxy-3-ethylenediaminepropyl-silane (TEEDPS) has been investigated using UV-Vis fluorescence and absorption spectroscopy methods and thermogravimetry. Results suggest that the TEEDPS-modified MCM-41 has a greatly enhanced (by 20 times) PL intensity at 420 nm relative to that of TEEDPS, and this enhanced PL still remains even after post heat treatment at 180 °C under vacuum (yielding a sample MTV). Meanwhile, a strong PL band at 450 nm appeared in the sample MTV when excited at 380 nm. The TEEDPS-modified material could be partly oxidized at 180 °C in air (yielding a sample MTA); therefore obvious absorption was found up to about 600 nm. The interaction between this absorption and the vacancy-related emission resulted in the maximum of the emission bands of the sample MTA at around 515 nm when excited at 440 nm. PACS 78.55.Mb; 78.55.Hx; 79.60.Jv; 78.40.Ha  相似文献   

16.
Using cetyltrimethyl ammonium bromide (CTAB) as the template and sodium silicate as the silicon source, the MCM-41 mesoporous molecular sieves with Eu incorporated in the framework were synthesized under microwave irradiation condition and the influence of the Si/Eu molar ratio on the crystalline structure, textural properties and the long-range ordering of the resulting sample was investigated by various physicochemical techniques such as X-ray diffraction (XRD), transmission electron microscope (TEM), diffuse reflectance ultraviolet-visible spectroscopy (UV-vis), thermal gravimetric-differential scanning calorimeter (TG-DSC) and N2 physical adsorption. The results of N2 adsorption and XRD reveal that the synthesized sample has the ordered hexagonal mesoporous structure. UV-vis spectra provide the strong evidences that most of europium ions were incorporated into the framework of the MCM-41 sample. The crystalline structure, textural properties and mesoporous ordering of the resultant mesoporous materials are related to the amount of europium incorporation. Small amount europium incorporated into the silica-based MCM-41 does not strongly modify the structure of mesoporous molecular sieve. An increase of the Eu content in sample led to reduction of the specific surface area and the deterioration of the long-range ordering.  相似文献   

17.
Co (Ni or Cu)-MCM-41 mesoporous molecular sieves with different amount of metal were synthesized by using cetyltrimethyl ammonium bromide as a template and by a novel microwave irradiation method. These samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and N2 physical adsorption. The experimental results show that Co (Ni or Cu)-MCM-41 mesoporous molecular sieves were successfully synthesized. When the as-synthesized samples were calcined at 550 °C for 10 h, the template was effectively removed. Under microwave irradiation condition, Co-MCM-41 mesoporous molecular sieves have specific surface areas in a range of 745.7-1188.8 m2/g and average pore sizes in a range of 2.46-2.75 nm; Ni-MCM-41 mesoporous molecular sieves have specific surface areas in a range of 625.8-1161.3 m2/g and average pore sizes of ca. 2.7 nm; Cu-MCM-41 mesoporous molecular sieves have specific surface areas in a range of 601.6-1142.9 m2/g and average pore sizes in a range of 2.46-2.76 nm. On the other hand, with increasing the introduced metal amount, the specific surface area and pore volume of the synthesized Co (Ni or Cu)-MCM-41 mesoporous molecular sieves became small, and the mesoporous ordering of the samples became poor. Under the comparable synthesis conditions, the synthesized Co-MCM-41 mesoporous molecular sieve has a bigger specific surface area and a more uniform pore distribution as compared with the synthesized Ni-MCM-41and Cu-MCM-41 mesoporous molecular sieves.  相似文献   

18.
Highly ordered mesoporous material MCM-41 was synthesized from tetraethylorthosilicate (TEOS) as Si source and cetyltrimethylammonium bromide (CTAB) as template. Well-dispersed NiO nanoparticles were introduced into the highly ordered mesoporous MCM-41 by chemical precipitation method to prepare the highly ordered mesoporous NiO/MCM-41 composite. X-ray diffraction (XRD) analysis, transmission electron microscopy (TEM) and high-resolution TEM (HRTEM), and nitrogen adsorption–desorption measurement were used to examine the morphology and the microstructure of the obtained composite. The morphological study clearly revealed that the synthesized NiO/MCM-41 composite has a highly ordered mesoporous structure with a specific surface area of 435.9 m2 g−1. A possible formation mechanism is preliminary proposed for the formation of the nanostructure. The adsorption performance of NiO/MCM-41 composite as an adsorbent was further demonstrated in the removal azo dyes of methyl orange (MO), Congo red (CR), methylene blue (MB) and rhodaming B (RB) under visible light irradiation and dark, respectively. The kinetics and mechanism of removal methylene blue were studied. The results show that NiO/MCM-41 composite has a good removal capacity for organic pollutant MB from the wastewater under the room temperature. Compared with MCM-41 and NiO nanoparticles, 54.2% and 100% higher removal rate were obtained by the NiO/MCM-41 composite.  相似文献   

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