智能聚电解质刷复合纳米粒子的制备和表征
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摘要
智能材料正越来越多地吸引研究者的目光,并已成为材料科学的研究热点。智能纳米粒子,作为智能材料的一个重要分支,在可控催化、药物控释、传感器、微纳米驱动等方面有着广泛的应用前景。另外,还有一类被称为Janus的纳米粒子因形状或结构的各向异性而具有特殊的自组装和刺激响应能力,是另一种具有很大应用潜力的智能纳米材料。
本文在聚丙烯酸(PAA)球形聚电解质刷(SPB)的基础上合成了多种智能纳米微球,包括温度/pH双响应型球形聚电解质刷、有机/无机杂化二氧化硅复合微球和二氧化硅空心微球；首次利用Pickering乳液法结合光乳液聚合方法在聚合物纳米粒子表面接枝了非球形聚电解质刷,得到各向异性(Janus)纳米粒子；另外,通过不同的合成路线还制备了聚合物/二氧化硅Janus微球和聚合物/四氧化三铁磁性Janus微球。本文还利用原子力显微镜(AFM)研究了球形刷和Janus刷的形貌以及在不同性质的基底表面的自组装行为。具体内容如下：
1.通过光乳液聚合将N-异丙基丙烯酰胺(NIPA)和丙烯酸(AA)共聚接枝到PS核表面,制得同时对pH和温度具有响应的双功能球形聚合物刷(BSPB)。动态光散射(DLS)对BSPB的pH和温度响应行为的观察表明,以共聚方式结合的NIPA和AA杂化刷与均聚的PAA刷相比从酸性到碱性的pH响应发生一定的滞后。另外,本文用原子力显微镜(AFM)在气相和液相中原位观察了双功能球形刷的形貌,并通过定性分析,发现其表面粘附力在pH值=3时达到最低,并随pH值增加有增大的趋势。
2.以PAA球形聚电解质刷为模板,合成了核直径在100nm左右近单分散的SPB/二氧化硅核-壳型微球和空心微球。通过与聚乙烯基吡咯烷酮(PVP)中性刷对比,证明以PAA阴离子球形聚电解质刷作为模板更适合原位沉积二氧化硅。同时发现PAA刷厚度、金属盐浓度和体系温度对二氧化硅的沉积都有显著影响。DLS的数据证明,在用溶剂除去聚合物核后的空心微球仍具有pH值响应的能力,并且核-壳结构微球和空心微球在水相中均具有良好的再分散能力。
3.通过Pickering乳液法制备了PS/PAA和PS/SiO2Janus微球。具体合成路线包括：1)制备得到Pickering乳液后,PS核一部分嵌入石蜡固体表面,紫外光引发水溶性单体AA接枝到PS核暴露部分的表面,得到非对称的Janus PAA(?)；2)同样先制备Pickering乳液,然后通过湿法腐蚀对吸附在石蜡表面的PS/SiO2(?)球进行不对称腐蚀,得到Janus SiO2复合微球；3)利用苯乙烯单体对Pickering乳液中的PS/SiO2微球进行非对称溶胀和种子乳液聚合制备得到Janus SiO2复合微球。对Pickering乳液的制备进行了研究,考察了PS核的浓度和体系搅拌的速度对Pickering乳液的影响。在用AFM表征Janus刷时,先用硫醇季铵盐对AFM镀金探针改性,同时让PAA刷在低温下干燥并保留少量水分,最后促使成像过程中探针与刷子因强相互作用而发生不规律共振,使得刷子部分与PS核部分的图像形成较大反差,呈现出Janus刷各向异性的形貌特征。
4.用共沉淀法先制备得到粒径10nm左右的Fe304纳米粒子,然后在细乳液聚合过程中Fe3O4纳米粒子与聚合物之间因相分离而形成一半为Fe304一半为聚苯乙烯的粒径100nm左右的PS/Fe3O4磁性Janus微球。然后用苯乙烯单体对微球进行溶胀并进行种子乳液聚合得到200nm和450nm左右的磁性Janus微球；选用200nm的PS/Fe3O4磁性Janus微球为模板,分别结合光乳液聚合方法和阴影-气相沉积法制备了PAA@PS/Fe3O4磁性Janus刷和Pd@PS/Fe3O4磁性Janus微球。利用DLS观察磁性Janus刷的水力学直径随pH值的变化；考察了磁性Janus刷和磁性Janus微球的饱和磁化强度；用高分辨电镜表征了磁性Janus微球的形貌。研究了外加磁场下镀钯磁性Janus微球在石蜡(液)/水(液)界面中的自组装形态。
5.研究了基底的表面极性、表面电荷、沉积温度和球形刷浓度等对球形刷在固体表面自组装的影响；用AFM观察了Janus刷在基底表面的自组装,发现依据不同的基底表面性质Janus刷呈现不同的取向。
Smart materials have increasingly attracted the attention of researchers, and became the hotspot of materials science research. Smart nanoparticles is an important branch of smart materials has been broad applied in controlled catalysis, controlled drug delivery, sensors, micro-drivers, etc. In addition, there are a class of nanoparticles are anisotropic in shape or surface functionality with special self-assembly and stimulus-response capability, known as the Janus nanoparticles, which are also smart nano-materials showing a great potential applications.
A series type of smart nanoparticles has been synthesized based on spherical polyelectrolyte brushes (SPB) in this article, including temperature/pH double-responsive nano spherical polyelectrolyte brushes, SPB/silica composite microspheres; With an assistant of Pickering emulsion method, pH-responsive anisotropy polyelectrolyte brushes were prepared through grafting nonsperical poly (acrylic acid)(PAA) brushes onto nano-sized core surfaces by photo-emulsion polymerization, and the morphology, stimulate-response and self-assembly of the microspheres were characterized by atomic force microscopy (AFM); more over, polyer/silica and magnetic-responsive Janus composite microspheres were also synthesized. Details are listed as follows:
1. Isopropylacrylamide (NIPA) and acrylic acid (AA) copolymer were grafted onto the PS core surface by the light emulsion polymerization to obtain a pH and temperature bifunctional spherical polymer brush (BSPB). The dynamic light scattering (DLS) studies showed that the pH-responsive behavior of BSPB occurs lag compared to the homopolymer poly (acrylic acid)(PAA) brush. In addition, we used AFM to observe the morphology of BSPB in the gas and liquid, and to qualitatively analyze its surface adhesion by force curves. It was found that the surface adhesion responses to the pH value that increasing with increases of pH, and show low-sticky in pH value=3.
2. Using PAA SPB as a template, SPB/silica core-shell and hollow microspheres was synthesized with a diameter ca.100nm. Compared to neutral brush polyvinylpyrrolidone (PVP), PAA anionic spherical polyelectrolyte brush is a more ideal template for in situ deposition of silica. The effect of the PAA brushes thickness, the salt concentration and temperature on silica deposition were discussed in the thesis. The DLS data proved that the hollow microspheres still have pH-response, and core-shell and hollow structure microspheres with good dispersion properties in water.
3. PAA Janus polyelectrolyte and PS/SiO2Janus microspheres were prepared by Pickering emulsion method. Specific synthesis strategies include:1) After formation of Pickering emulsions, PS core embedded into paraffin wax surface, and the exposed part of the surface grafted PAA brush under UV irradiation to obtain non-spherical PAA brushes;2) PS/SiO2microspheres Janus nanoparticles were fabricated by asymmetric wet-etching based on Pickering emulsion;3) in the Pickering emulsion, styrene monomer asymmetrical swelled the PS/SiO2microspheres and then polymerized to obtain asymmetric SiO2shell structure. The effects of concentration and system stirring speed on Pickering emulsions were investigated. AFM probe modification and PAA brush incomplete drying was used to make a sharp contrast with the PS core in AFM images.
4. Iron oxide nanoparticles of10nm were made by coprecipitation method. Magnetic Janus microspheres of100nm with a half of Fe3O4and a half of polystyrene were synthesized through phase separation by miniemulsion. Furtherly,200nm and450nm PS/Fe3O4magnetic Janus microspheres were prepared by seed emulsion polymerization. Using200nm PS/Fe3O4magnetic Janus microspheres as a template, respectively, PAA@PS/Fe3O4magnetic Janus brush and Pd@PS/Fe3O4magnetic Janus microspheres were prepared by photo-emulsion polymerization and the shadow vapor deposition. The thicknesses of Magnetic Janus brushes changed with pH as observed by DLS; The saturation magnetization and morphology of the magnetic Janus microspheres and brushes were investigated. The self-assembly of Janus microspheres controlled by an external magnetic field was observed.
5. The polarity and surface charge of the substrate surface, the deposition temperature and the concentration of spherical brushes which influenced the self-assembly of spherical brush were discussed in this thesis; AFM was used to observe the orientation of Janus brush upon different surface.
本文在聚丙烯酸(PAA)球形聚电解质刷(SPB)的基础上合成了多种智能纳米微球,包括温度/pH双响应型球形聚电解质刷、有机/无机杂化二氧化硅复合微球和二氧化硅空心微球；首次利用Pickering乳液法结合光乳液聚合方法在聚合物纳米粒子表面接枝了非球形聚电解质刷,得到各向异性(Janus)纳米粒子；另外,通过不同的合成路线还制备了聚合物/二氧化硅Janus微球和聚合物/四氧化三铁磁性Janus微球。本文还利用原子力显微镜(AFM)研究了球形刷和Janus刷的形貌以及在不同性质的基底表面的自组装行为。具体内容如下：
1.通过光乳液聚合将N-异丙基丙烯酰胺(NIPA)和丙烯酸(AA)共聚接枝到PS核表面,制得同时对pH和温度具有响应的双功能球形聚合物刷(BSPB)。动态光散射(DLS)对BSPB的pH和温度响应行为的观察表明,以共聚方式结合的NIPA和AA杂化刷与均聚的PAA刷相比从酸性到碱性的pH响应发生一定的滞后。另外,本文用原子力显微镜(AFM)在气相和液相中原位观察了双功能球形刷的形貌,并通过定性分析,发现其表面粘附力在pH值=3时达到最低,并随pH值增加有增大的趋势。
2.以PAA球形聚电解质刷为模板,合成了核直径在100nm左右近单分散的SPB/二氧化硅核-壳型微球和空心微球。通过与聚乙烯基吡咯烷酮(PVP)中性刷对比,证明以PAA阴离子球形聚电解质刷作为模板更适合原位沉积二氧化硅。同时发现PAA刷厚度、金属盐浓度和体系温度对二氧化硅的沉积都有显著影响。DLS的数据证明,在用溶剂除去聚合物核后的空心微球仍具有pH值响应的能力,并且核-壳结构微球和空心微球在水相中均具有良好的再分散能力。
3.通过Pickering乳液法制备了PS/PAA和PS/SiO2Janus微球。具体合成路线包括：1)制备得到Pickering乳液后,PS核一部分嵌入石蜡固体表面,紫外光引发水溶性单体AA接枝到PS核暴露部分的表面,得到非对称的Janus PAA(?)；2)同样先制备Pickering乳液,然后通过湿法腐蚀对吸附在石蜡表面的PS/SiO2(?)球进行不对称腐蚀,得到Janus SiO2复合微球；3)利用苯乙烯单体对Pickering乳液中的PS/SiO2微球进行非对称溶胀和种子乳液聚合制备得到Janus SiO2复合微球。对Pickering乳液的制备进行了研究,考察了PS核的浓度和体系搅拌的速度对Pickering乳液的影响。在用AFM表征Janus刷时,先用硫醇季铵盐对AFM镀金探针改性,同时让PAA刷在低温下干燥并保留少量水分,最后促使成像过程中探针与刷子因强相互作用而发生不规律共振,使得刷子部分与PS核部分的图像形成较大反差,呈现出Janus刷各向异性的形貌特征。
4.用共沉淀法先制备得到粒径10nm左右的Fe304纳米粒子,然后在细乳液聚合过程中Fe3O4纳米粒子与聚合物之间因相分离而形成一半为Fe304一半为聚苯乙烯的粒径100nm左右的PS/Fe3O4磁性Janus微球。然后用苯乙烯单体对微球进行溶胀并进行种子乳液聚合得到200nm和450nm左右的磁性Janus微球；选用200nm的PS/Fe3O4磁性Janus微球为模板,分别结合光乳液聚合方法和阴影-气相沉积法制备了PAA@PS/Fe3O4磁性Janus刷和Pd@PS/Fe3O4磁性Janus微球。利用DLS观察磁性Janus刷的水力学直径随pH值的变化；考察了磁性Janus刷和磁性Janus微球的饱和磁化强度；用高分辨电镜表征了磁性Janus微球的形貌。研究了外加磁场下镀钯磁性Janus微球在石蜡(液)/水(液)界面中的自组装形态。
5.研究了基底的表面极性、表面电荷、沉积温度和球形刷浓度等对球形刷在固体表面自组装的影响；用AFM观察了Janus刷在基底表面的自组装,发现依据不同的基底表面性质Janus刷呈现不同的取向。
Smart materials have increasingly attracted the attention of researchers, and became the hotspot of materials science research. Smart nanoparticles is an important branch of smart materials has been broad applied in controlled catalysis, controlled drug delivery, sensors, micro-drivers, etc. In addition, there are a class of nanoparticles are anisotropic in shape or surface functionality with special self-assembly and stimulus-response capability, known as the Janus nanoparticles, which are also smart nano-materials showing a great potential applications.
A series type of smart nanoparticles has been synthesized based on spherical polyelectrolyte brushes (SPB) in this article, including temperature/pH double-responsive nano spherical polyelectrolyte brushes, SPB/silica composite microspheres; With an assistant of Pickering emulsion method, pH-responsive anisotropy polyelectrolyte brushes were prepared through grafting nonsperical poly (acrylic acid)(PAA) brushes onto nano-sized core surfaces by photo-emulsion polymerization, and the morphology, stimulate-response and self-assembly of the microspheres were characterized by atomic force microscopy (AFM); more over, polyer/silica and magnetic-responsive Janus composite microspheres were also synthesized. Details are listed as follows:
1. Isopropylacrylamide (NIPA) and acrylic acid (AA) copolymer were grafted onto the PS core surface by the light emulsion polymerization to obtain a pH and temperature bifunctional spherical polymer brush (BSPB). The dynamic light scattering (DLS) studies showed that the pH-responsive behavior of BSPB occurs lag compared to the homopolymer poly (acrylic acid)(PAA) brush. In addition, we used AFM to observe the morphology of BSPB in the gas and liquid, and to qualitatively analyze its surface adhesion by force curves. It was found that the surface adhesion responses to the pH value that increasing with increases of pH, and show low-sticky in pH value=3.
2. Using PAA SPB as a template, SPB/silica core-shell and hollow microspheres was synthesized with a diameter ca.100nm. Compared to neutral brush polyvinylpyrrolidone (PVP), PAA anionic spherical polyelectrolyte brush is a more ideal template for in situ deposition of silica. The effect of the PAA brushes thickness, the salt concentration and temperature on silica deposition were discussed in the thesis. The DLS data proved that the hollow microspheres still have pH-response, and core-shell and hollow structure microspheres with good dispersion properties in water.
3. PAA Janus polyelectrolyte and PS/SiO2Janus microspheres were prepared by Pickering emulsion method. Specific synthesis strategies include:1) After formation of Pickering emulsions, PS core embedded into paraffin wax surface, and the exposed part of the surface grafted PAA brush under UV irradiation to obtain non-spherical PAA brushes;2) PS/SiO2microspheres Janus nanoparticles were fabricated by asymmetric wet-etching based on Pickering emulsion;3) in the Pickering emulsion, styrene monomer asymmetrical swelled the PS/SiO2microspheres and then polymerized to obtain asymmetric SiO2shell structure. The effects of concentration and system stirring speed on Pickering emulsions were investigated. AFM probe modification and PAA brush incomplete drying was used to make a sharp contrast with the PS core in AFM images.
4. Iron oxide nanoparticles of10nm were made by coprecipitation method. Magnetic Janus microspheres of100nm with a half of Fe3O4and a half of polystyrene were synthesized through phase separation by miniemulsion. Furtherly,200nm and450nm PS/Fe3O4magnetic Janus microspheres were prepared by seed emulsion polymerization. Using200nm PS/Fe3O4magnetic Janus microspheres as a template, respectively, PAA@PS/Fe3O4magnetic Janus brush and Pd@PS/Fe3O4magnetic Janus microspheres were prepared by photo-emulsion polymerization and the shadow vapor deposition. The thicknesses of Magnetic Janus brushes changed with pH as observed by DLS; The saturation magnetization and morphology of the magnetic Janus microspheres and brushes were investigated. The self-assembly of Janus microspheres controlled by an external magnetic field was observed.
5. The polarity and surface charge of the substrate surface, the deposition temperature and the concentration of spherical brushes which influenced the self-assembly of spherical brush were discussed in this thesis; AFM was used to observe the orientation of Janus brush upon different surface.
引文
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