有序介孔材料的制备与应用
摘要
多孔分子筛由于具有可控的纳米孔道结构，大的比表面积，耐酸耐碱等特殊的物理化学性质，在工业生产和实际生活中得到了广泛的应用。随着科技的进步和研究工作的深入，不断拓展有序介孔材料的应用范围，从最初的分离、催化和吸附等方面的应用扩展到电子元器件、光学材料、生物材料等其它方面的应用。多孔分子筛的成功应用不仅与其内在孔道结构有关，同时与其形貌、颗粒尺寸、客体分子在孔道中的组装效率及催化、分离过程中的传质过程密切相关。因此，在制备分子筛材料时，如何控制其宏观形貌成为该领域内研究的一个重要方向：如将分子筛制成膜状、球状和大块等。近年来分子筛的功能化研究为其开拓了更加广阔的应用前景。本文利用水热合成的方法制备了不同类型的分子筛，并考察各种合成条件对不同类型分子筛在介电材料、湿敏材料与手性分离材料方向应用的影响。取得的研究成果列举如下：
1采用UV光照的方法脱除纳米微孔/介孔材料合成时所用的模板剂。即室温下将事先合成的材料放在臭氧发生的、中压Hg光栅灯产生的短波紫外灯（λ=184~257nm）下照射。这种方法被用于MCM-41介孔材料、Silicalite-1分子筛、A型分子筛和Y型分子筛模板剂的脱除中。材料在UV光照前后的结构和有机物含量分别用XRD、FT-IR、BET和SEM进行表征。并以高温焙烧后的样品作为对比，进行了相应的结构表征。 XRD表明UV光照或高温焙烧后的样品都保留对应原粉的骨架结构。FT-IR表明高温焙烧可彻底脱除所有微孔/介孔材料的模板剂，但UV光照只能彻底脱除MCM-41介孔材料和Silicalite-1分子筛中的模板剂，A型分子筛和Y型分子筛中仍残留少量模板剂。SEM照片显示，UV光照后的微孔/介孔材料仍然保持很好的分散状态，没有出现纳米颗粒的聚集现象。将UV光照的方法同样用于Silicalite-1薄膜模板剂的脱除。结果表明，UV光照只需6h即可彻底脱除Silicalite-1薄膜中的模板剂，而高温焙烧所需时间超过3天。同时UV光照后的Silicalite-1薄膜致密、连续，没有裂缝和洞眼。与传统的高温焙烧方法相比，UV光照法是一种省时、低能耗的脱除分子筛薄膜模板剂，制备高质量分子筛薄膜的有效方法。
以正硅酸乙酯为硅源，四丙基氢氧化铵(TPAOH)为模板剂和碱源，采取水热晶化技术，通过原位法在硅晶片表面制备出纯二氧化硅透明分子筛薄膜；与传统高温焙烧法相比，采用紫外光解法脱除分子筛薄膜孔道内的模板剂，更易制备出具有低介电性能的氧化硅分子筛薄膜。以正硅酸乙酯（TEOS）和甲基三乙氧基硅烷（MeSi(OEt)_3）为混合硅源，十六烷基三甲基溴化铵(CTAB)为模板剂，采取旋涂技术，在硅晶片表面制备出二氧化硅透明薄膜，再经过正硅酸乙酯（TEOS）蒸气孔壁强化后采用线性升温焙烧法脱除薄膜孔道内的模板剂，制备出具有超低介电性能的氧化硅分子筛薄膜。采用FT-IR、XRD和SEM对样品进行了结构表征,并采用椭偏仪测量了薄膜的介电常数，纳米硬度计测量薄膜的弹性模量。氧化硅分子筛薄膜在24℃相对湿度80%的条件下静置360h后，介电常数维持在1.8，弹性模量大于6GP，很好的满足了在超大规模集成电路中应用的要求。
2采用水热合成方法在酸性条件下合成出有序介孔材料SBA-15。主要研究了晶化温度和搅拌速度等条件对有序介孔材料SBA-15孔结构及形貌的影响。合成试样的孔径尺寸单一，孔道呈六方排列，具有良好的长程有序结构，是典型的有序介孔SBA-15结构材料。通过优化实验方案，成功制备出具有规整微观形貌的新型SBA-15材料，其最大孔径为12.7nm，热稳定性优良。研究结果表明：在合成SBA-15时，晶化温度和搅拌速度对非离子型表面活性剂在水溶液中形成棒状胶束的临界胶束浓度(CMC)产生影响，可以导致CMC降低，促使棒状胶束形成六方有序排列。有序介孔材料SBA-15具有大的比表面积和孔体积、孔径均一且在纳米尺寸上连续可调的孔径和形貌、表面基团富有硅羟基易于与空气中的水分键合、二氧化硅无生理毒性等一系列优点，首次把有序硅基介孔材料SBA-15作为具有灵敏度高、选择性好、成本低、装置简单、易于集成化、易于实现现场连续检测优点的石英晶体微天平（QCM）质量型传感器的湿敏材料来制备新型的湿度传感器。研究结果表明：开发出的湿度传感器具有湿度量程大（可在1%-100%RH范围内检测）、灵敏度高（可达69.5Hz/%RH）、湿滞小（湿度为52.9%以下几乎无湿滞）、装置简单、耐高温、耐溶剂、成本低、有利于环保、易于集成化、易于实现现场连续检测等优点。MCM-41传感器随湿度变化的频率变化关系证实了介孔材料具有很好的湿敏特性，可以作为石英晶体微天平湿度传感器的备选材料。且涂覆MCM-41的石英晶体微天平传感器在湿度很高(＞90%RH)和很低(﹤20%RH)的情况下仍然能够起振，相比于那些涂覆其它材料在高湿和低湿条件下不能起振的传感器来说，是很好的改进。
3以手性药物左旋萘普生(S-naproxen)为模板分子，四乙烯基吡啶(4-VPy)为功能单体，采用分子印迹法，以介孔材料SBA-15为载体合成了能选择性识别S-naproxen的分子印迹聚合物微球。扫描电镜及BET分析结果表明，所合成的分子印迹聚合物微球具有粒径均匀、孔径分布窄、比表面积大等特点；同时扫描电镜、X射线衍射和红外光谱分析结果表明载体表面形成了分子印迹聚合物层，Scatchard分析表明分子印迹聚合物在自组装过程中存在两类结合位点，聚合物高亲和力和低亲和力结合位点的最大表观结合容量分别为Qmax_1=2.504μmol/g，Qmax_2=16.680μmol/g;分子印迹聚合物的热力学研究表明，吸附过程可以自发进行。
Zeolite has been used in industrial production and real life widely because ofthetunable pore size, larger surface area (up to1500m2/g), acid and alkali resistant andother special physical and chemical characteristics. With the progress of science andtechnology, people greatly expand the application range of zeolites, from the initialseparation, catalysis and adsorption to the electronic components, optical materials,biological materials and other applications. In recent years the functionalized zeolite hasbeen used in other field. Zeolite membrane, spheres and block have been synthesized.Therefore our research work focused on the synthesis of different condensed matter zeolitematerials, and examine various factors of different zeolites in condensed matter dielectricmaterial moisture sensitive material and material direction of the chiral separationapplications.
This paper describes an application of UV radiation near room temperature conditionsfor the removal of the template in the synthesis of micro/mesoporous materials, such asmesoporous MCM-41, Silicalite-1, zeolite LTA etc. The UV radiation relies on the exposureof the sample to short-wavelength ultraviolet(UV) radiation in air and the ozoneenvironment generated by a medium pressure mercury lamp(184-257nm). The structuresand organic contents of the micro/mesoporous materials before and after UV radiation weredetermined using a combination of XRD, FT-IR, BET, carbon analysis and SEM. XRDpatterns showed that the framework structure was kept after UV radiation or thermallycalcinations. Before and after calcination the sample made similar characterization forcomparison. FT-IR data showed the complete removal of the template in micro/mesoporousmaterials. But it is only useful for the complete removal of the template of mesoporousMCM-41and Silicalite-1nanoparticle, while there was a trace of residual template inzeolite LTA and zeolite Y nanoparticles. The SEM images showed micro/mesoporousnanoparticles UV treated have no obvious aggregation.The UV radiation is also efficient forthe complete removal of the template in the preparation of Silicalite-1thin film only after6h exposure time, while the thermally calcination process is more than3days. The SEMimages reveal the formation of a continuous thin film from displaying densely packedcrystals and there is not any significant cracks or pin holls. Compared with conventionalthermally calcination, the method provides an efficient and economical approach for thepreparation of high quality zeolite thin films free of template. Organic-functionalizedmesoporous silica films (Me-MCM-TEOS) have been produced using co-condensation ofmethyltrimethoxyslane and tetraethyl orthosilicate (TEOS), and a TEOS vapor treatmentbefore the removal of surfactant by spin-coating method. The materials have beencharacterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR)and Field emission scanning electron microscope (FE-SEM). Dielectric constant k isdetermined using Ellipsometer, and elastic modulus (Young’s modulus, E) and hardness ofthe films are measured by a Nano Indenter XP. XRD patterns and FT-IR spectra show that the methylsilated mesoporous films (Me-MCM-TEOS-CAL) have densified mesochannelwalls and an increased hydrophobic property by the TEOS vapor treatment. The k value isas low as1.78even in80%-relative-humidity environments for seven days. Mechanicalstrength is also high enough to withstand the stresses that occur during the chemicalmechanical polishing (CMP) and wire bonding process (E>6.0GPa). TEOS vapor treatedmesoporous silica films without the addition of methyl groups (MCM-TEOS) are alsosynthesized for a comparison.
Mesoporous silica SBA-15was prepared through a hydrothermal treatment in acidmedia. The as-synthesized samples show the uniform pore size and long-distance orderedarrangement of hexagonal structure, which is typically ordered mesoporous structure.Through the optimal experiments, SBA-15products with uniform morphology of hexagonallamelliform were obtained. The biggest pore size is mainly centered on12.7nm. Theas-made SBA-15possesses of good thermal stability. The mesoporous silica SBA-15wasdeposited on the quartz crystal micro-balances (QCMs) to construct highly stable andsensitive humidity sensors. The humidity sensing characteristics of the sensors wereinvestigated by measuring the resonant frequency shift of QCMs due to the additional massloading caused by adsorption of water. The results showed that the sensors had highsensitivity, good stability, short response/recovery time, well reproducibility and narrowhysteresis.Improved humidity sensors based on quartz crystal micro-balance coated withmesoporous silica MCM-41thin film were fabricated. XRD, BET, TEM and SEM wereemployed to characterize sensing films so as to study the effects of its pore structure on thehumidity sensing properties. The results reveal that sensitivity over a wide humidity rangeand especially for low humidity conditions. The high sensitivity, well reproducibility, shortresponse and recovery times obtained were ascribed to the ordered pore arrays and highsurface area of the MCM-41films. This study has significance in tailoring the moisturesensitivity in the design of diverse sensors for practical applications. Herein, not only anovel and low-cost humidity sensor material was exploited, but also a new application areafor mesoporous materials was opened up.
Molecularly imprinted composite materials (MICMs) selectiveto S-naproxen wereprepared onthe surface of mesoporous silica sphere (SBA-15) by a surface imprintingtechnique with S-naproxenas the template and42vinylpyridine as the functional monomer.As observed by SEMandpore structure analysis, the microspheres coated with thesynthesized molecularlyimprintedpolymers have a uniform particle size, narrowsizedistributionandhighspecific surfacearea. The polymer layer on SBA-15can be determinedby SEM, XRD and FT-IR spectroscopy. Scatchard analysis shows that two kinds ofrecognition sites are formed on the MICMS with the apparent binding capacities of2.504μmol/g and16.680mol/g, respectively. Based on anisothermalbindingthermodynamicinvestigation, the absorption to template is found to be spontaneous.
1采用UV光照的方法脱除纳米微孔/介孔材料合成时所用的模板剂。即室温下将事先合成的材料放在臭氧发生的、中压Hg光栅灯产生的短波紫外灯（λ=184~257nm）下照射。这种方法被用于MCM-41介孔材料、Silicalite-1分子筛、A型分子筛和Y型分子筛模板剂的脱除中。材料在UV光照前后的结构和有机物含量分别用XRD、FT-IR、BET和SEM进行表征。并以高温焙烧后的样品作为对比，进行了相应的结构表征。 XRD表明UV光照或高温焙烧后的样品都保留对应原粉的骨架结构。FT-IR表明高温焙烧可彻底脱除所有微孔/介孔材料的模板剂，但UV光照只能彻底脱除MCM-41介孔材料和Silicalite-1分子筛中的模板剂，A型分子筛和Y型分子筛中仍残留少量模板剂。SEM照片显示，UV光照后的微孔/介孔材料仍然保持很好的分散状态，没有出现纳米颗粒的聚集现象。将UV光照的方法同样用于Silicalite-1薄膜模板剂的脱除。结果表明，UV光照只需6h即可彻底脱除Silicalite-1薄膜中的模板剂，而高温焙烧所需时间超过3天。同时UV光照后的Silicalite-1薄膜致密、连续，没有裂缝和洞眼。与传统的高温焙烧方法相比，UV光照法是一种省时、低能耗的脱除分子筛薄膜模板剂，制备高质量分子筛薄膜的有效方法。
以正硅酸乙酯为硅源，四丙基氢氧化铵(TPAOH)为模板剂和碱源，采取水热晶化技术，通过原位法在硅晶片表面制备出纯二氧化硅透明分子筛薄膜；与传统高温焙烧法相比，采用紫外光解法脱除分子筛薄膜孔道内的模板剂，更易制备出具有低介电性能的氧化硅分子筛薄膜。以正硅酸乙酯（TEOS）和甲基三乙氧基硅烷（MeSi(OEt)_3）为混合硅源，十六烷基三甲基溴化铵(CTAB)为模板剂，采取旋涂技术，在硅晶片表面制备出二氧化硅透明薄膜，再经过正硅酸乙酯（TEOS）蒸气孔壁强化后采用线性升温焙烧法脱除薄膜孔道内的模板剂，制备出具有超低介电性能的氧化硅分子筛薄膜。采用FT-IR、XRD和SEM对样品进行了结构表征,并采用椭偏仪测量了薄膜的介电常数，纳米硬度计测量薄膜的弹性模量。氧化硅分子筛薄膜在24℃相对湿度80%的条件下静置360h后，介电常数维持在1.8，弹性模量大于6GP，很好的满足了在超大规模集成电路中应用的要求。
2采用水热合成方法在酸性条件下合成出有序介孔材料SBA-15。主要研究了晶化温度和搅拌速度等条件对有序介孔材料SBA-15孔结构及形貌的影响。合成试样的孔径尺寸单一，孔道呈六方排列，具有良好的长程有序结构，是典型的有序介孔SBA-15结构材料。通过优化实验方案，成功制备出具有规整微观形貌的新型SBA-15材料，其最大孔径为12.7nm，热稳定性优良。研究结果表明：在合成SBA-15时，晶化温度和搅拌速度对非离子型表面活性剂在水溶液中形成棒状胶束的临界胶束浓度(CMC)产生影响，可以导致CMC降低，促使棒状胶束形成六方有序排列。有序介孔材料SBA-15具有大的比表面积和孔体积、孔径均一且在纳米尺寸上连续可调的孔径和形貌、表面基团富有硅羟基易于与空气中的水分键合、二氧化硅无生理毒性等一系列优点，首次把有序硅基介孔材料SBA-15作为具有灵敏度高、选择性好、成本低、装置简单、易于集成化、易于实现现场连续检测优点的石英晶体微天平（QCM）质量型传感器的湿敏材料来制备新型的湿度传感器。研究结果表明：开发出的湿度传感器具有湿度量程大（可在1%-100%RH范围内检测）、灵敏度高（可达69.5Hz/%RH）、湿滞小（湿度为52.9%以下几乎无湿滞）、装置简单、耐高温、耐溶剂、成本低、有利于环保、易于集成化、易于实现现场连续检测等优点。MCM-41传感器随湿度变化的频率变化关系证实了介孔材料具有很好的湿敏特性，可以作为石英晶体微天平湿度传感器的备选材料。且涂覆MCM-41的石英晶体微天平传感器在湿度很高(＞90%RH)和很低(﹤20%RH)的情况下仍然能够起振，相比于那些涂覆其它材料在高湿和低湿条件下不能起振的传感器来说，是很好的改进。
3以手性药物左旋萘普生(S-naproxen)为模板分子，四乙烯基吡啶(4-VPy)为功能单体，采用分子印迹法，以介孔材料SBA-15为载体合成了能选择性识别S-naproxen的分子印迹聚合物微球。扫描电镜及BET分析结果表明，所合成的分子印迹聚合物微球具有粒径均匀、孔径分布窄、比表面积大等特点；同时扫描电镜、X射线衍射和红外光谱分析结果表明载体表面形成了分子印迹聚合物层，Scatchard分析表明分子印迹聚合物在自组装过程中存在两类结合位点，聚合物高亲和力和低亲和力结合位点的最大表观结合容量分别为Qmax_1=2.504μmol/g，Qmax_2=16.680μmol/g;分子印迹聚合物的热力学研究表明，吸附过程可以自发进行。
Zeolite has been used in industrial production and real life widely because ofthetunable pore size, larger surface area (up to1500m2/g), acid and alkali resistant andother special physical and chemical characteristics. With the progress of science andtechnology, people greatly expand the application range of zeolites, from the initialseparation, catalysis and adsorption to the electronic components, optical materials,biological materials and other applications. In recent years the functionalized zeolite hasbeen used in other field. Zeolite membrane, spheres and block have been synthesized.Therefore our research work focused on the synthesis of different condensed matter zeolitematerials, and examine various factors of different zeolites in condensed matter dielectricmaterial moisture sensitive material and material direction of the chiral separationapplications.
This paper describes an application of UV radiation near room temperature conditionsfor the removal of the template in the synthesis of micro/mesoporous materials, such asmesoporous MCM-41, Silicalite-1, zeolite LTA etc. The UV radiation relies on the exposureof the sample to short-wavelength ultraviolet(UV) radiation in air and the ozoneenvironment generated by a medium pressure mercury lamp(184-257nm). The structuresand organic contents of the micro/mesoporous materials before and after UV radiation weredetermined using a combination of XRD, FT-IR, BET, carbon analysis and SEM. XRDpatterns showed that the framework structure was kept after UV radiation or thermallycalcinations. Before and after calcination the sample made similar characterization forcomparison. FT-IR data showed the complete removal of the template in micro/mesoporousmaterials. But it is only useful for the complete removal of the template of mesoporousMCM-41and Silicalite-1nanoparticle, while there was a trace of residual template inzeolite LTA and zeolite Y nanoparticles. The SEM images showed micro/mesoporousnanoparticles UV treated have no obvious aggregation.The UV radiation is also efficient forthe complete removal of the template in the preparation of Silicalite-1thin film only after6h exposure time, while the thermally calcination process is more than3days. The SEMimages reveal the formation of a continuous thin film from displaying densely packedcrystals and there is not any significant cracks or pin holls. Compared with conventionalthermally calcination, the method provides an efficient and economical approach for thepreparation of high quality zeolite thin films free of template. Organic-functionalizedmesoporous silica films (Me-MCM-TEOS) have been produced using co-condensation ofmethyltrimethoxyslane and tetraethyl orthosilicate (TEOS), and a TEOS vapor treatmentbefore the removal of surfactant by spin-coating method. The materials have beencharacterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR)and Field emission scanning electron microscope (FE-SEM). Dielectric constant k isdetermined using Ellipsometer, and elastic modulus (Young’s modulus, E) and hardness ofthe films are measured by a Nano Indenter XP. XRD patterns and FT-IR spectra show that the methylsilated mesoporous films (Me-MCM-TEOS-CAL) have densified mesochannelwalls and an increased hydrophobic property by the TEOS vapor treatment. The k value isas low as1.78even in80%-relative-humidity environments for seven days. Mechanicalstrength is also high enough to withstand the stresses that occur during the chemicalmechanical polishing (CMP) and wire bonding process (E>6.0GPa). TEOS vapor treatedmesoporous silica films without the addition of methyl groups (MCM-TEOS) are alsosynthesized for a comparison.
Mesoporous silica SBA-15was prepared through a hydrothermal treatment in acidmedia. The as-synthesized samples show the uniform pore size and long-distance orderedarrangement of hexagonal structure, which is typically ordered mesoporous structure.Through the optimal experiments, SBA-15products with uniform morphology of hexagonallamelliform were obtained. The biggest pore size is mainly centered on12.7nm. Theas-made SBA-15possesses of good thermal stability. The mesoporous silica SBA-15wasdeposited on the quartz crystal micro-balances (QCMs) to construct highly stable andsensitive humidity sensors. The humidity sensing characteristics of the sensors wereinvestigated by measuring the resonant frequency shift of QCMs due to the additional massloading caused by adsorption of water. The results showed that the sensors had highsensitivity, good stability, short response/recovery time, well reproducibility and narrowhysteresis.Improved humidity sensors based on quartz crystal micro-balance coated withmesoporous silica MCM-41thin film were fabricated. XRD, BET, TEM and SEM wereemployed to characterize sensing films so as to study the effects of its pore structure on thehumidity sensing properties. The results reveal that sensitivity over a wide humidity rangeand especially for low humidity conditions. The high sensitivity, well reproducibility, shortresponse and recovery times obtained were ascribed to the ordered pore arrays and highsurface area of the MCM-41films. This study has significance in tailoring the moisturesensitivity in the design of diverse sensors for practical applications. Herein, not only anovel and low-cost humidity sensor material was exploited, but also a new application areafor mesoporous materials was opened up.
Molecularly imprinted composite materials (MICMs) selectiveto S-naproxen wereprepared onthe surface of mesoporous silica sphere (SBA-15) by a surface imprintingtechnique with S-naproxenas the template and42vinylpyridine as the functional monomer.As observed by SEMandpore structure analysis, the microspheres coated with thesynthesized molecularlyimprintedpolymers have a uniform particle size, narrowsizedistributionandhighspecific surfacearea. The polymer layer on SBA-15can be determinedby SEM, XRD and FT-IR spectroscopy. Scatchard analysis shows that two kinds ofrecognition sites are formed on the MICMS with the apparent binding capacities of2.504μmol/g and16.680mol/g, respectively. Based on anisothermalbindingthermodynamicinvestigation, the absorption to template is found to be spontaneous.
引文
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