新型囊泡及泡沫材料的制备与表征
摘要
多孔材料在吸附、缓释、催化、分离等领域具有重要的应用价值,因而引起了研究者的广泛兴趣。嵌段共聚物可以自组装为不同的超分子结构,例如囊泡和不同的液晶相结构。利用不同的液晶相为模板(liquid crystal templating,LCT),可直接制备或者协同组装出有序的介孔材料。Hubert等利用离子型表面活性剂,首先提出利用表面活性剂预先形成的有机囊泡作为模板(vesicle templating,VT)制备无机氧化硅单层囊泡材料的方法。相对目前大量的关于液晶模板制备介孔材料的文献报道而言,“囊泡模板”的合成概念并未得到人们的重视,而利用嵌段共聚物作为“囊泡模板”来合成无机单层囊泡的工作亦未见报道。
本论文以非离子型表面活性剂为模板,以正硅酸甲酯为硅源,提出了“协同囊泡模板”(cooperative vesicle templating,CVT)制备大孔容无机纳米单层囊泡材料的“绿色”新路线,。通过改变反应的pH值、反应温度、无机盐及其浓度,以及硅源的量来合成不同结构的多孔材料,并实现LCT与CVT的调变。通过对材料进行进一步的功能化,合成了具有不同组成和性能的二氧化硅复合材料,并在应用方面进行了一些初步的探索。
第二章中,我们利用商业化非离子型表面活性剂作为模板,在近中性,无需添加有机膨胀剂的条件下,制备出具有超大孔容(＞3cm~3 g~(-1))和超大孔径的新型二氧化硅囊泡、泡沫材料。在固定缓冲溶液pH值不变时,随着反应温度的提高,观察到从管状胶束→单层囊泡→纳米泡沫的结构转化。提出了通过嵌段共聚物协同囊泡模板(CVT)方法来合成氧化硅囊泡、泡沫的新方法。与文献中合成氧化硅囊泡的方法相比,本章使用的方法,更加方便,产率更高。和其它多孔材料相比,我们制备的纳米泡沫(Nano foam)对大分子量的蛋白有更好的吸附能力。
第三章中,我们提出一种“超级自组装”的方法,即利用自组装的囊泡为结构单元进一步“超级”组装成大孔有序氧化硅泡沫材料(macroporous orderedsiliceous foams,MOSFs),首次实现了直接利用表面活性剂分子自组装制备孔径高达100 nm的有序大孔材料。成功地利用电子断层扫描(electron tomography,ET)技术确定了MOSFs具有与蜂巢类似的结构,采用自然界中最有效利用空间的堆积方法构成。MOSFs的形成过程受到反应时间,水热处理和离子强度等多重因素的影响。随着实验过程中离子强度的增大,产物的结构经历一个囊泡→聚集的囊泡→MOSFs→无序堆积的复杂囊泡的结构转变,同时材料的孔径也呈逐渐增大的趋势。
第四章中,我们详细考察了反应温度、溶液pH、无机盐的种类和浓度,以及硅源的量等多种实验条件对传统液晶模板(liquid crystal templating,LCT)与CVT路线的调变。结果表明,当其它条件保持不变时,随着合成温度的升高,在较小的温度范围内(≈25℃),实现了从二维六方(介孔孔径为10nm)到MOSFs(孔径为110nm)的结构转变,材料的孔径膨胀了10倍。在HCl反应体系中(pH=2-7),观察到随着反应pH的增大,产物的结构也会实现从二维六方(pH＜3)到囊泡(pH=3-4)的转变,而pH过高(pH＞4)则无法得到有序结构。在pH=4的HCl体系中加入无机盐,随着离子强度的增大,亦可诱导从囊泡→泡沫→MOSFs的结构变化。在缓冲体系中加入相同离子强度、不同组成的无机盐,考察不同阳离子和阴离子对产物的影响。研究发现阴离子对材料的结构起决定作用,阳离子(Ca~(2+)、Mg~(2+)等)可通过与表面活性剂的螯合等作用,对囊泡的墙壁产生影响。调变硅源和结构导向剂的比例,也发现随着硅源量的增加产物从最初的分散囊泡→MOSFs→具有介孔墙壁的囊泡的转变过程。上述结果对设计合成具有不同结构的多孔材料具有较好的良好的理论指导价值。
第五章中,我们通过简单的共沉淀方法成功地合成出了硅钛摩尔比不同的硅钛复合材料。随着硅钛摩尔比的变化实现了从泡沫到介观有序结构的转变。当硅钛摩尔比≥10时,二氧化钛物种可很好地分散在二氧化硅骨架中。初步研究结果表明,具有较大比表面积和孔容的硅钛复合材料,在磷酸化肽段富集分离方面有较好的应用前景。
Porous materials have attracted considerable attention in the areas such as separation of large molecules,biosensors,catalysis,adsorption,microelectronics, optics,and fabrication of novel nano-objects because of their uniform and adjustable properties.Generally,porous materials are fabricated by the template approach.By utilizing a liquid-crystal templating(LCT) method organized mesostructured inorganic materials can be directly or cooperatively assembled.Hubert firstly reported the vesicle templating(VT) synthesis of unilamellar silica vesicles by directly coating the pre-formed unilamellar vesicles of ionic surfactants.Although the phase behavior of block copolymers has been extensively studied,the block-copolymer VT method to synthesize inorganic unilamellar vesicular structure has not been reported. Furthermore,a large-scale,high-yield,cheap synthesis of unilamellar vesicles with sub-micrometer diameters and ultrahigh pore volumes is currently a challenge in both block-copolymer and hybrid material studies.
Macroporous materials with large pore size of＞50 nm have been extensively studied and exhibited significant applications in different areas.However,ordered macroporous materials are usually synthesized by means of emulsion,microemulsion, or colloidal sphere templating methods.For future applications of functional and economic macroporous materials,it is important to search a facile and green approach to fabricate ordered macroporous materials without adding any organic solvents or hard templates to produce large pores.
The current contribution concerns the synthesis of unilamellar siliceous vesicles and nanofoams with large pore diameters and high pore volumes by employing commercial triblock copolymer as templates in the absence of organic cosolvents.A new cooperative vesicle templating(CVT) approach is proposed.Novel inorganic siliceous materials with various morphologies and hierarchical pore structures are obtained by varying the reaction temperature,pH,inorganic salts and ionic strength. The transformation between the LCT and CVT approaches is revealed.
In chapter 2,we report the synthesis of unilamellar siliceous vesicles and nanofoams with ultrahigh pore volumes(＞3 cm~3g~(-1)) by using EO_(20)PO_(70)EO_(20)(P123) as a template in near neutral aqueous solutions.At controlled pH,a structural transformation from tubules to unilamellar vesicles then to nanofoams is observed by increasing the reaction temperature.It is proposed that the siliceous vesicles are synthesized via a co-operative block-copolymer vesicle templating approach,while the siliceous nanofoams are obtained by the fusion of vesicles at increased ionic strength.Compared to literature methods to synthesize siliceous vesicles and foams, our method is convenient,cheap,and produces a high yield.Siliceous nanofoams synthesized by using our approach show superior bioimmobilization capacity over other porous materials for biomolecules with large molecular weight.
In chapter 3,macroporous ordered siliceous foams(MOSFs) with cage sizes on the order of～110 nm have been successfully synthesized via a facile and green approach.The synthesis is carried out under mild condition in the absence of organic cosolvent,similar to the biosilica formation process in the slightly acidic environment in silica deposition vesicles(SDV) in diatoms.The fusion of soft unilamellar composite vesicles with relatively uniform size finally results in MOSFs,and the electron tomography(ET) characterization shows that MOSFs have well ordered and defined honeycomb structures at the macroscale,which is energetically beneficial. The formation of MOSFs is influenced by the reaction time,the hydrothermal treatment process,the reaction pH,and the concentration of sodium sulfate(Na_2SO_4) during the synthesis.When the concentration of Na_2SO_4 is adjusted between 0.1 and 0.45 M when the other reaction conditions are not changed,a structural transition from vesicles to tightly aggregated vesicles and then MOSFs and finally large compound vesicles(LCV) has been observed.
In chapter 4,the influences of reaction temperature,pH,different inorganic salts and the amount of the silica source have been carefully investigated,and the transformation between the LCT and CVT approaches has been revealed.In buffer solution at pH=5.0,a limited variation of temperature from 15 to 35℃leads to a structural evolution from ordered hexagonal mesostructure with a pore size of 10 nm to MOSFs with the pore size of～110 nm,inducing a pore expansion of～10 times. Under acidic conditions(pH=2-7 HCI solution),a structural transformation from ordered hexagonal mesostructure(pH＜3) to vesicles(pH=3-4) is also observed.With increasing ion strength,a structural transformation from vesicle to tightly aggregated vesicle and then MOSFs can be achieved.When different types of salts with the same ion strength are used,it is found that not only the anions,but also the cations have great influence on the final structures.Finally,by increasing the molar ratio of silica precursor to the organic template,a continuous structural transformation from vesicles to MOSFs and finally to vesicles with mesoporous walls can be achieved.
In chapter 5,TiO_2-SiO_2 porous materials with tunable Si/Ti molar ratio(R) have been successfully prepared through a one-pot method under a near neutral condition. With decreasing Si/Ti R,a phase transition from a macroporous foam-like structure to mesostructure is observed.The resultant TiO_2-SiO_2 porous materials possess large surface areas and high pore volumes.In addition,the titania species are homogenously dispersed in silica matrix when Si/Ti R≥10.Our preliminary results show that such functional porous materials have good performance in the enrichment of phosphopeptides for proteomic research.
本论文以非离子型表面活性剂为模板,以正硅酸甲酯为硅源,提出了“协同囊泡模板”(cooperative vesicle templating,CVT)制备大孔容无机纳米单层囊泡材料的“绿色”新路线,。通过改变反应的pH值、反应温度、无机盐及其浓度,以及硅源的量来合成不同结构的多孔材料,并实现LCT与CVT的调变。通过对材料进行进一步的功能化,合成了具有不同组成和性能的二氧化硅复合材料,并在应用方面进行了一些初步的探索。
第二章中,我们利用商业化非离子型表面活性剂作为模板,在近中性,无需添加有机膨胀剂的条件下,制备出具有超大孔容(＞3cm~3 g~(-1))和超大孔径的新型二氧化硅囊泡、泡沫材料。在固定缓冲溶液pH值不变时,随着反应温度的提高,观察到从管状胶束→单层囊泡→纳米泡沫的结构转化。提出了通过嵌段共聚物协同囊泡模板(CVT)方法来合成氧化硅囊泡、泡沫的新方法。与文献中合成氧化硅囊泡的方法相比,本章使用的方法,更加方便,产率更高。和其它多孔材料相比,我们制备的纳米泡沫(Nano foam)对大分子量的蛋白有更好的吸附能力。
第三章中,我们提出一种“超级自组装”的方法,即利用自组装的囊泡为结构单元进一步“超级”组装成大孔有序氧化硅泡沫材料(macroporous orderedsiliceous foams,MOSFs),首次实现了直接利用表面活性剂分子自组装制备孔径高达100 nm的有序大孔材料。成功地利用电子断层扫描(electron tomography,ET)技术确定了MOSFs具有与蜂巢类似的结构,采用自然界中最有效利用空间的堆积方法构成。MOSFs的形成过程受到反应时间,水热处理和离子强度等多重因素的影响。随着实验过程中离子强度的增大,产物的结构经历一个囊泡→聚集的囊泡→MOSFs→无序堆积的复杂囊泡的结构转变,同时材料的孔径也呈逐渐增大的趋势。
第四章中,我们详细考察了反应温度、溶液pH、无机盐的种类和浓度,以及硅源的量等多种实验条件对传统液晶模板(liquid crystal templating,LCT)与CVT路线的调变。结果表明,当其它条件保持不变时,随着合成温度的升高,在较小的温度范围内(≈25℃),实现了从二维六方(介孔孔径为10nm)到MOSFs(孔径为110nm)的结构转变,材料的孔径膨胀了10倍。在HCl反应体系中(pH=2-7),观察到随着反应pH的增大,产物的结构也会实现从二维六方(pH＜3)到囊泡(pH=3-4)的转变,而pH过高(pH＞4)则无法得到有序结构。在pH=4的HCl体系中加入无机盐,随着离子强度的增大,亦可诱导从囊泡→泡沫→MOSFs的结构变化。在缓冲体系中加入相同离子强度、不同组成的无机盐,考察不同阳离子和阴离子对产物的影响。研究发现阴离子对材料的结构起决定作用,阳离子(Ca~(2+)、Mg~(2+)等)可通过与表面活性剂的螯合等作用,对囊泡的墙壁产生影响。调变硅源和结构导向剂的比例,也发现随着硅源量的增加产物从最初的分散囊泡→MOSFs→具有介孔墙壁的囊泡的转变过程。上述结果对设计合成具有不同结构的多孔材料具有较好的良好的理论指导价值。
第五章中,我们通过简单的共沉淀方法成功地合成出了硅钛摩尔比不同的硅钛复合材料。随着硅钛摩尔比的变化实现了从泡沫到介观有序结构的转变。当硅钛摩尔比≥10时,二氧化钛物种可很好地分散在二氧化硅骨架中。初步研究结果表明,具有较大比表面积和孔容的硅钛复合材料,在磷酸化肽段富集分离方面有较好的应用前景。
Porous materials have attracted considerable attention in the areas such as separation of large molecules,biosensors,catalysis,adsorption,microelectronics, optics,and fabrication of novel nano-objects because of their uniform and adjustable properties.Generally,porous materials are fabricated by the template approach.By utilizing a liquid-crystal templating(LCT) method organized mesostructured inorganic materials can be directly or cooperatively assembled.Hubert firstly reported the vesicle templating(VT) synthesis of unilamellar silica vesicles by directly coating the pre-formed unilamellar vesicles of ionic surfactants.Although the phase behavior of block copolymers has been extensively studied,the block-copolymer VT method to synthesize inorganic unilamellar vesicular structure has not been reported. Furthermore,a large-scale,high-yield,cheap synthesis of unilamellar vesicles with sub-micrometer diameters and ultrahigh pore volumes is currently a challenge in both block-copolymer and hybrid material studies.
Macroporous materials with large pore size of＞50 nm have been extensively studied and exhibited significant applications in different areas.However,ordered macroporous materials are usually synthesized by means of emulsion,microemulsion, or colloidal sphere templating methods.For future applications of functional and economic macroporous materials,it is important to search a facile and green approach to fabricate ordered macroporous materials without adding any organic solvents or hard templates to produce large pores.
The current contribution concerns the synthesis of unilamellar siliceous vesicles and nanofoams with large pore diameters and high pore volumes by employing commercial triblock copolymer as templates in the absence of organic cosolvents.A new cooperative vesicle templating(CVT) approach is proposed.Novel inorganic siliceous materials with various morphologies and hierarchical pore structures are obtained by varying the reaction temperature,pH,inorganic salts and ionic strength. The transformation between the LCT and CVT approaches is revealed.
In chapter 2,we report the synthesis of unilamellar siliceous vesicles and nanofoams with ultrahigh pore volumes(＞3 cm~3g~(-1)) by using EO_(20)PO_(70)EO_(20)(P123) as a template in near neutral aqueous solutions.At controlled pH,a structural transformation from tubules to unilamellar vesicles then to nanofoams is observed by increasing the reaction temperature.It is proposed that the siliceous vesicles are synthesized via a co-operative block-copolymer vesicle templating approach,while the siliceous nanofoams are obtained by the fusion of vesicles at increased ionic strength.Compared to literature methods to synthesize siliceous vesicles and foams, our method is convenient,cheap,and produces a high yield.Siliceous nanofoams synthesized by using our approach show superior bioimmobilization capacity over other porous materials for biomolecules with large molecular weight.
In chapter 3,macroporous ordered siliceous foams(MOSFs) with cage sizes on the order of～110 nm have been successfully synthesized via a facile and green approach.The synthesis is carried out under mild condition in the absence of organic cosolvent,similar to the biosilica formation process in the slightly acidic environment in silica deposition vesicles(SDV) in diatoms.The fusion of soft unilamellar composite vesicles with relatively uniform size finally results in MOSFs,and the electron tomography(ET) characterization shows that MOSFs have well ordered and defined honeycomb structures at the macroscale,which is energetically beneficial. The formation of MOSFs is influenced by the reaction time,the hydrothermal treatment process,the reaction pH,and the concentration of sodium sulfate(Na_2SO_4) during the synthesis.When the concentration of Na_2SO_4 is adjusted between 0.1 and 0.45 M when the other reaction conditions are not changed,a structural transition from vesicles to tightly aggregated vesicles and then MOSFs and finally large compound vesicles(LCV) has been observed.
In chapter 4,the influences of reaction temperature,pH,different inorganic salts and the amount of the silica source have been carefully investigated,and the transformation between the LCT and CVT approaches has been revealed.In buffer solution at pH=5.0,a limited variation of temperature from 15 to 35℃leads to a structural evolution from ordered hexagonal mesostructure with a pore size of 10 nm to MOSFs with the pore size of～110 nm,inducing a pore expansion of～10 times. Under acidic conditions(pH=2-7 HCI solution),a structural transformation from ordered hexagonal mesostructure(pH＜3) to vesicles(pH=3-4) is also observed.With increasing ion strength,a structural transformation from vesicle to tightly aggregated vesicle and then MOSFs can be achieved.When different types of salts with the same ion strength are used,it is found that not only the anions,but also the cations have great influence on the final structures.Finally,by increasing the molar ratio of silica precursor to the organic template,a continuous structural transformation from vesicles to MOSFs and finally to vesicles with mesoporous walls can be achieved.
In chapter 5,TiO_2-SiO_2 porous materials with tunable Si/Ti molar ratio(R) have been successfully prepared through a one-pot method under a near neutral condition. With decreasing Si/Ti R,a phase transition from a macroporous foam-like structure to mesostructure is observed.The resultant TiO_2-SiO_2 porous materials possess large surface areas and high pore volumes.In addition,the titania species are homogenously dispersed in silica matrix when Si/Ti R≥10.Our preliminary results show that such functional porous materials have good performance in the enrichment of phosphopeptides for proteomic research.
引文
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