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1.
In this study we report the synthesis of a new class of materials called hybrid periodic mesoporous organosilicas (HPMOs). By coupling a silsesquioxane precursor through at least two chemical linkages to the mesopore walls of a pre‐existing periodic mesoporous silica (PMS) or periodic mesoporous organosilica (PMO). Many of the problems of a conventional PMO material can be avoided while ensuring efficient use of the bridging organic functional groups of the silsesquioxane. We demonstrate this concept for PMS by anchoring various silsesquioxanes, such as ethene and ethane silsesquioxanes, to the mesopore walls of the PMS. The addition of anchored silsesquioxane monolayers and multilayers to the mesopore walls also allows for the strict control of the diameter of the mesopore as well as the mesopore wall thickness in the final HPMO material. Additionally it is shown that having the silsesquioxane located solely on the surface of the mesopores in HPMOs gives increased chemical accessibility of the organic bridge‐bonded moiety when compared with their PMO counterparts containing the bridge‐bonded organic both on the surface and within the pore walls. 相似文献
2.
Using surfactant‐assisted synthesis, aluminas with hierarchical nanopores are produced. The hierarchical structures are composed of mesopores of 4 nm diameter, and macropores with diameters of about 300 nm. The structures were found to be stable to the thermal removal of the surfactant. Synthesis factors affecting the appearance of the hierarchically structured alumina material are presented. A potential mechanism for the formation of the uniquely structured aluminas is proposed. 相似文献
3.
A. Prim E. Pellicer E. Rossinyol F. Peiró A. Cornet J. R. Morante 《Advanced functional materials》2007,17(15):2957-2963
A mesoporous CaO‐loaded In2O3 material (with Ca/In2O3 ratios ranging from 2.5 to 8.5 at %) has been synthesized and used as resistive gas sensor for the detection of CO2. A nanostructured In2O3 matrix has been obtained by hard template route from the SBA‐15 silica template. Additive presence does not distort the lattice of In2O3, which crystallizes in the Ia3 cubic space group. It has been proved by XRD, HRTEM, Raman and XPS measurements that samples contain not only CaO but also CaCO3 in calcite phase as a consequence of CaO carbonation. Pure In2O3 based sensors are low sensitive to CO2, whereas those containing the additive show an important response in the 300–5000 ppm range of gas concentrations. As seen by DRIFTS, the electrical response arises from the interaction between CO32– and CO2, yielding bicarbonates products. The reaction is water‐assisted, so that hydration of the sensing material ensures sensor reliability whilst its dehydration would inhibit sensor response. The use of CaCO3 instead of CaO does not cause significant differences in electrical and DRIFTS data, which corroborates the important role played by carbonate species in the sensing mechanism. 相似文献
4.
J‐H. Yim J‐B. Seon H‐D. Jeong L.&#x;S. Pu M.&#x;R. Baklanov D.&#x;W. Gidley 《Advanced functional materials》2004,14(3):277-282
Porous cyclic silsesquioxane (CSSQ) thin films containing nanopores (～ 2 nm) with low dielectric constant (k < 2.2), have been prepared by using various kinds of cyclodextrin (CD) derivatives as porogenic materials. The pore structure, including average pore size and interconnectivity, can be controlled by changing the functional groups of the cyclodextrin derivatives. The pore structure is found to be strongly related to the affinity of the functional groups between CD molecules. The electrical and mechanical properties of the porous thin films were monitored in order to determine the relationship between the pore structure and film properties. The mechanical properties of porous low‐k thin films (total porosity ～ 30 %) prepared with CD derivatives are found to be correlated with the pore interconnection length. The longer the deduced interconnection length in the thin film, the worse the mechanical properties (such as hardness and modulus) of the thin film, even though the porogen‐induced pore diameters are very small (～ 2 nm). 相似文献
5.
E. Rossinyol A. Prim E. Pellicer J. Arbiol F. Hernández‐Ramírez F. Peiró A. Cornet J. R. Morante L. A. Solovyov B. Tian T. Bo D. Zhao 《Advanced functional materials》2007,17(11):1801-1806
SBA‐15 (2D hexagonal structure) and KIT‐6 (3D cubic structure) silica materials are used as templates for the synthesis of two different crystalline mesoporous WO3 replicas usable as NO2 gas sensors. High‐resolution transmission electron microscopy (HRTEM) studies reveal that single‐crystal hexagonal rings set up the atomic morphology of the WO3 KIT‐6 replica, whereas the SBA‐15 replica is composed of randomly oriented nanoparticles. A model capable of explaining the KIT‐6 replica mesostructure is described. A small amount of chromium is added to the WO3 matrix in order to enhance sensor response. It is demonstrated that chromium does not form clusters, but well‐distributed centers. Pure WO3 KIT‐6 replica displays a higher response rate as well as a lower response time to NO2 gas than the SBA‐15 replica. This behavior is explained by taking into account that the KIT‐6 replica has a higher surface area as demonstrated by Brunauer–Emmett–Teller analyses and its mesostructure is fully maintained after the screen‐printing step involved in sensors preparation. The presence of chromium in the material results in a shorter response time and improved sensor response to the lowest NO2 concentrations tested. Electrical differences related to mesostructure are reduced as a result of additive introduction. 相似文献
6.
B. Tan S. M. Vyas H.‐J. Lehmler B. L. Knutson S. E. Rankin 《Advanced functional materials》2007,17(14):2500-2508
A new partially fluorinated cationic surfactant, 1‐(10‐perfluorooctyldecyl)pyridinium bromide monohydrate, is synthesized and used as the template for mesoporous ceramic and inorganic–organic hybrid particles. Several hydrolyzed alkoxide precursors are shown to co‐assemble with this surfactant to form hollow vesicle‐like particles, and the effect of changing the alkoxide chemical structure on the formation of these particles is examined. Tetramethoxysilane produces cubic or columnar particles without hollow cavities, but all other tetra‐n‐alkoxysilanes tested up to the n‐butoxide produce hollow particles. As the alkoxide length increases, the shell structure changes from multilayered (with Si(OC2H5)4) to a single thin layer (with Si(OC3H7)4) to a single thick layer (with Si(OC4H9)4). The stability of the fluorocarbon bilayers allows similar vesicular structures to be obtained in organic–inorganic hybrids prepared with bridged alkoxysilanes. Ethylene‐bridged silanes display similar structures to tetraalkoxysilanes. However, the hollow structures appear to partially collapse when the bridging chain is too long (octylene) and no hollow particles are formed with bis(trialkoxysilylpropyl)amines. 相似文献
7.
J.&#x;P.&#x;K. Reynhardt Y. Yang A. Sayari H. Alper 《Advanced functional materials》2005,15(10):1641-1646
Polyamidoamine dendrimers up to the fourth generation have been grown with unprecedentedly high loading within the channels of pore‐expanded (10.6 nm) MCM‐41 silica. In‐depth characterization using nitrogen adsorption, solid‐state NMR, FTIR, thermogravimetry, and elemental analysis showed that the dendrimers grow inside the channels with an average yield better than 99 %. The pore size and structure of the support have been found to be determining factors as to how much dendrimer growth can be achieved. 相似文献
8.
C. Boissire M. Kümmel M. Persin A. Larbot E. Prouzet 《Advanced functional materials》2001,11(2):129-135
Among the mesoporous silica micellar templated structures (MTSs), MSU‐X silica, obtained through an N0I0 assembly between non‐ionic polyethyleneoxide‐based surfactants (N0) and silica neutral inorganic precursors (I0), exhibits a regular ordered structure with a 3D wormhole porous framework and an easily controlled pore size. These materials have been tested for applications requiring both a narrow mesopore size distribution and isotropic properties. A specific double‐step synthesis that we developed recently for MSU‐X materials has allowed us to prepare mesoporous silica particles with the required shape, size, and properties. Both the particles’ synthesis and comparative HPLC separation tests with a commercial ungrafted silica HPLC powder of identical shape and size are reported. 相似文献
9.
Z.&#x;Y. Wu H.&#x;J. Wang T.&#x;T. Zhuang L.&#x;B. Sun Y.&#x;M. Wang J.&#x;H. Zhu 《Advanced functional materials》2008,18(1):82-94
Aluminum‐containing plugged mesoporous silica has been successfully prepared in an aqueous solution that contains triblock copolymer templates, nitrates, and silica sources but without using mineral acid. The acidity of the solution can be finely tuned from pH 1.4 to 2.8 according to the amount of the introduced aluminum species which ranged from an Al/Si molar ratio of 0.25/1 to 4.0/1. The aluminum nitrate additive in the starting mixture, along with the weak acidity produced by the nitrates, contributes to the formation of plugged hexagonal structures and the introduction of different amounts of aluminum species into the mesostructure. Characterization by X‐ray diffraction, transmission electron microscopy, and N2 sorption measurements show that the Al‐containing plugged silicas possess well‐ordered hexagonal mesostructures with high surface areas (700–860 m2 g–1), large pore volume (0.77–1.05 cm3 g–1) and, more importantly, combined micropores and/or small mesopores in the cylindrical channels. Inductively coupled plasma–atomic emission spectrometry results show that 0.7–3.0 wt % aluminum can be introduced into the final samples. 27Al MAS NMR results display that about 43–60% aluminum species are incorporated into the skeleton of the Al‐containing silicas and the amount of the framework aluminum increases as the initial added nitrates rises. Scanning electron microscopy images reveal that the directly synthesized Al‐containing plugged silica has a similar morphology to that of traditional SBA‐15. Furthermore, the Al‐containing plugged samples have excellent performances in the adsorption and the catalytic decomposition of isopropyl alcohol and nitrosamine. Finally, the direct synthesis method is used to produce plugged mesoporous silicas that contain other metals such as chromium and copper, and the resultant samples also show good catalytic activities. 相似文献
10.
A new type of mechanically improved rubbery epoxy composite is demonstrated based on the use of a mesocellular silica foam, denoted MSU‐F, as the reinforcement agent. The silica exhibits a surface area of 540 m2 g–1, a cell size of 26.5 nm (14.9 nm window size) and a pore volume of 2.2 cm3 g–1. Most notably, the silica foam particles readily disperse in the epoxy matrix without the need for an organic surface modifier or dispersing agent. Relative to the pristine polymer, the tensile modulus, strength, strain‐at‐break, and toughness for the mesocomposites are systematically enhanced at relatively low silica loading over the range 1–9 wt %. Moreover, all of these benefits are realized without a sacrifice in thermal stability or optical transparency of the polymer. The results demonstrate that silica in mesocellular foam form can provide polymer reinforcement far beyond the level realized for non‐porous silica or silica with small mesopores at the same weight loading. 相似文献
11.
A mesocellular silica–carbon nanocomposite foam (MSCF) is designed for the immobilization and biosensing of proteins. The as‐prepared MSCF has a highly ordered mesostructure, good biocompatibility, favorable conductivity and hydrophilicity, large surface area, and a narrow pore‐size distribution, as verified by transmission electron microscopy (TEM), IR spectroscopy, electrochemical impedance spectroscopy (EIS), nitrogen adsorption–desorption isotherms, pore size distribution plots, and water contact angle measurements. Using glucose oxidase (GOD) as a model, the MSCF is tested for immobilization of redox proteins and the design of electrochemical biosensors. GOD molecules immobilized in the mesopores of the MSCF show direct electrochemistry with a fast electron transfer rate (14.0 ± 1.7 s–1) and good electrochemical performance. Based on a decrease of the electrocatalytic response of the reduced form of GOD to dissolved oxygen, the proposed biosensor exhibits a linear response to glucose concentrations ranging from 50 μM to 5.0 mM with a detection limit of 34 μM at an applied potential of –0.4 V. The biosensor shows good stability and selectivity and is able to exclude interference from ascorbic acid (AA) and uric acid (UA) species that always coexist with glucose in real samples. The nanocomposite foam provides a good matrix for protein immobilization and biosensor preparation. 相似文献
12.
Hydrothermally stable thioether‐bridged mesoporous materials have been synthesized by one‐step co‐condensation of 1,4‐bis(triethoxysily)propane tetrasulfide (TESPTS) with tetramethoxysilane (TMOS) using cetyltrimethylammonimum bromide (CTAB) as the surfactant in basic conditions. The ordered mesoporous materials can be formed with a wide range of thioether concentrations in the mesoporous framework, as is seen by X‐ray diffraction (XRD) characterization. The results of N2 sorption and transmission electron microscopy (TEM) reveal that the materials synthesized with TESPTS/TMOS molar ratios in the range 1:8–1:3 have extensive structural defect holes in the nanochannels. All materials exhibit enhanced hydrothermal stability, which is in proportion to the concentration of thioether bridging in the mesoporous framework. The thioether‐functionalized mesoporous materials are efficient adsorbents for removing Hg2+ and phenol from waste water. The Hg2+‐adsorption capacity of the material can be as high as 1500 mg g–1. 相似文献
13.
M. Alvaro C. Aprile H. Garcia C.&#x;J. Gmez‐García 《Advanced functional materials》2006,16(12):1543-1548
Magnetite nanoparticles modified covalently with triethoxysilane having a quaternary dicetyl ammonium ion are used together with tetraethylorthosilicate as building blocks to prepare a mesoporous material. Cetyltrimethylammonium bromide is used as a structure‐directing agent under conditions typically used for mesoporous MCM‐41 silicas. The resulting mesoporous material (MAG‐MCM‐41), containing up to 15 wt % of magnetite is characterized by transmission electron microscopy (TEM), isothermal gas adsorption, and X‐ray diffraction. In contrast to siliceous MCM‐41, mesoporous MAG‐MCM‐41 exhibits a remarkable hydrothermal stability. The magnetic properties of MAG‐MCM‐41 are characterized by DC and AC magnetic susceptibility, and by isothermal hysteresis cycles, confirming the long‐range magnetic ordering above 400 K. As evidenced by atomic force microscopy and TEM, the ability to respond to magnetic fields is used to orient films of MAG‐MCM‐41 with the channels perpendicular to a support. 相似文献
14.
Y. Cohen K. Landskron N. Ttreault S. Fournier‐Bidoz B. Hatton G.&#x;A. Ozin 《Advanced functional materials》2005,15(4):593-602
The synthesis and characterization of a novel silicon–silica nanocomposite material are reported. A self‐assembly method allows the encapsulation of silicon nanoclusters within the channels of a periodic mesoporous silica thin film. The result is the formation of a silicon–silica nanocomposite film with bright, room‐temperature photoluminescence in the visible range, and a nanosecond luminescence lifetime. The properties of the nanocomposite material have been studied by several analytical techniques, which collectively show the existence within the channels of non‐diamondoid‐structure‐type silicon nanoclusters with various hydrogenated silicon sites. It is estimated that the silicon nanoclusters in the silica mesoporous films occupy up to 39 % of the accessible pore volume. The nanocomposite film shows improved resistance to air oxidation compared to crystalline silicon. The high loading and chemical stability to oxidation under ambient conditions are important advantages in terms of the development of silicon‐based light‐emitting diodes from this class of materials. 相似文献
15.
T. Brezesinski A. Fischer K.‐i. Iimura C. Sanchez D. Grosso M. Antonietti B.&#x;M. Smarsly 《Advanced functional materials》2006,16(11):1433-1440
Crack‐free, mesoporous SnO2 films with highly crystalline pore walls are obtained by evaporation‐induced self‐assembly using a novel amphiphilic block‐copolymer template (“KLE” type, poly(ethylene‐co‐butylene)‐block‐poly(ethylene oxide)), which leads to well‐defined arrays of contracted spherical mesopores by suitable heat‐treatment procedures. Because of the improved templating properties of these polymers, a facile heat‐treatment procedure can be applied whilst keeping the mesoscopic order intact up to 600–650 °C. The formation mechanism and the mesostructural evolution are investigated by various state‐of‐the‐art techniques, particularly by a specially constructed 2D small‐angle X‐ray scattering setup. It is found that the main benefit from the polymers is the formation of an ordered mesostructure under the drastic conditions of using molecular Sn precursors (SnCl4), taking advantage of the large segregation strength of these amphiphiles. Furthermore, it is found that the crystallization mechanism is different from other mesostructured metal oxides such as TiO2. In the case of SnO2, a significant degree of crystallization (induced by heat treatment) already starts at quite low temperatures, 250–300 °C. Therefore, this study provides a better understanding of the general parameters governing the preparation of mesoporous metal oxides films with crystalline pore walls. 相似文献
16.
A series of manganese oxide‐loaded SBA‐15 (MnSBA‐xh, x = 1, 2, 3, 4, 5, 6; h: hour(s)) mesoporous materials are synthesized via a facile, in‐situ reduction method with a surfactant template. The composite materials are characterized using Fourier‐transform infrared spectroscopy, X‐ray diffraction, N2 sorption isotherms, X‐ray photoelectron spectroscopy (XPS), transmission electron microscopy, energy‐dispersive spectroscopy, and CO oxidation catalysis. The results show that a high content of manganese (an atomic ratio of Mn/Si from 0.12 up to approximately 1) could be loaded into the channels of SBA‐15 when treated with an aqueous solution of potassium permanganate, while retaining the ordered mesostructure and large surface area of SBA‐15. Increasing the manganese oxide content results in a gradual decrease in the specific surface area, pore size, and pore volume. XPS spectra are employed to confirm the redox reaction between KMnO4 and the surfactant. CO‐conversion tests on the calcined MnSBA‐2h sample (MnSBA‐2h‐cal) shows that it has a repeatable, and relatively high, catalytic activity. 相似文献
17.
Nanometer‐sized surfactant‐templated materials are prepared in the form of stable suspensions of colloidal mesoporous silica (CMS) consisting of discrete, nonaggregated particles with dimensions smaller than 200 nm. A high‐yield synthesis procedure is reported based on a cationic surfactant and low water content that additionally enables the adjustment of the size range of the individual particles between 50 and 100 nm. Particularly, the use of the base triethanolamine (TEA) and the specific reaction conditions result in long‐lived suspensions. Dynamic light scattering reveals narrow particle size distributions in these suspensions. Smooth spherical particles with pores growing from the center to the periphery are observed by using transmission electron microscopy, suggesting a seed‐growth mechanism. The template molecules could be extracted from the nanoscale mesoporous particles via sonication in acidic media. The resulting nanoparticles give rise to type IV adsorption isotherms revealing typical mesopores and additional textural porosity. High surface areas of over 1000 m2 g–1 and large pore volumes of up to 1 mL g–1 are obtained for these extracted samples. 相似文献
18.
Extended porous silica films with thicknesses in the range of 60 to 130 μm and pores on both the meso‐ and macroscale have been prepared by simultaneously using porous membrane templates and amphiphilic supramolecular aggregates as porogens. The macropore size is determined by the cellulose acetate or polyamide membrane structure and the mesopores by the chosen ethylene‐oxide‐based molecular self‐assembly (block copolymer or non‐ionic surfactants). Both the template and the porogen are removed during an annealing step leaving the amorphous silica material with a porous structure that results from sol–gel chemistry occurring in the aqueous domains of the amphiphilic liquid‐crystalline phases and casting of the initial template membrane. The surface area and total pore volume of the inorganic films vary from 473 to 856 m2 g–1, and 0.50 to 0.73 cm3 g–1, respectively, depending on the choice of template and porogen. The combined benefits of both macro‐ and mesopores can potentially be obtained in one film. Such materials are envisaged to have applications in areas of large molecule (biomolecule) separation and catalysis. Enhanced gas and liquid flow rates through such membranes, due to the presence of the larger pores, also makes them attractive as supports for other catalytic materials. 相似文献
19.
W.‐H. Zhang X.‐B. Lu J.‐H. Xiu Z.‐L. Hua L.‐X. Zhang M. Robertson J.‐L. Shi D.‐S. Yan J.&#x;D. Holmes 《Advanced functional materials》2004,14(6):544-552
Direct synthesis (co‐condensation reaction) and post‐synthesis reaction (grafting) are combined for the first time to efficiently fabricate bifunctionalized ordered mesoporous materials (OMMs). Ethylenediamine‐containing OMMs (ED‐MCM‐41) were first synthesized via direct synthesis and then further modified by the phenyl (PH) group in a supercritical fluid (SCF) medium via grafting reaction, resulting in OMMs with ED and PH groups (PH‐ED‐MCM‐41). X‐ray diffraction (XRD) patterns, N2 sorption properties, transmission electron microscopy (TEM), 29Si and 13C magic angle spinning (MAS) NMR, chemical analysis, and hydrothermal treatment were used to characterize the bifunctionalized materials. Experiments show that bifunctionalized OMMs can be efficiently prepared by modifying the directly synthesized monofunctionalized OMMs via grafting reaction in a supercritical fluid medium. Both functional groups are distributed uniformly at the surfaces. The advantage of bifunctionalized OMMs over monofunctionalized OMMs was illustrated by introducing thiol groups into ED‐MCM‐41 materials and the subsequent formation of CdS nanocrystals inside thiol‐ and ED‐functionalized MCM‐41 (HS‐ED‐MC‐41). Because of the variety of the functional groups that can be introduced into OMMs by direct synthesis or post‐synthesis reaction, it is expected that the present strategy could provide a generally applicable approach to the design of OMMs with two functional groups. 相似文献
20.
Wenru Zhao Hangrong Chen Yongsheng Li Liang Li Meidong Lang Jianlin Shi 《Advanced functional materials》2008,18(18):2780-2788
A novel kind of rattle‐type hollow magnetic mesoporous sphere (HMMS) with Fe3O4 particles encapsulated in the cores of mesoporous silica microspheres has been successfully fabricated by sol–gel reactions on hematite particles followed by cavity generation with hydrothermal treatment and H2 reduction. Such a structure has the merits of both enhanced drug‐loading capacity and a significant magnetization strength. The prepared HMMSs realize a relatively high storage capacity up to 302 mg g?1 when ibuprofen is used as a model drug, and the IBU–HMMS system has a sustained‐release property, which follows a Fick's law. 相似文献