无机纳米晶体与天然纤维素物质复合材料的制备及性质研究
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摘要
随着科学技术尤其是纳米技术的飞速发展,人们越来越多地发现即使组成完全相同的物质,当其处于不同的尺度时,将会具有截然不同的独特性质。例如,半导体纳米晶体具有大块半导体材料所不具有的优异光学性能,金属纳米颗粒与大块金属相比也在诸如催化等众多领域显示出了巨大的应用潜力。正是如此,如何更好更高效地利用这些处于微观纳米尺度的无机晶体成为了近些年来新型材料领域的研究重点。天然纤维素物质作为一种廉价易得并且具有良好生物相容性的材料在制备新型复合材料领域显示出了其特有的优势。
本文利用不同的组装或生长技术,在天然纤维素物质上固定上多种无机纳米晶体,包括量子点,金属纳米颗粒,碳酸钙晶体,从而使这些无机纳米晶体从难以直接利用且不稳定的分散液状态转变成为多维乃至宏观大块的新型复合材料,扩展了这些具有优异性能的无机纳米晶体的实际应用价值。主要内容如下：
(1)纤维素/CdSe量子点复合发光材料：首先利用钛酸四丁酯在纤维素基底上沉积二氧化钛凝胶薄膜,再将硬脂酸利用羧基与钛的配位作用沉积在其表面,最后通过合成得到的三辛基氧化膦与十六烷基胺包裹的CdSe量子点表面烷基与硬脂酸烷基链之间的疏水作用,制备得到纤维素/CdSe量子点复合发光材料。扫描电子显微镜的结果表明纤维素原有的三维复杂层次性结构没有任何破坏。透射电子显微镜中能够看到在纤维素的纳米纤维上均匀地分布有CdSe量子点颗粒。紫外-可见和荧光光谱表征表明了此复合材料很好地继承了CdSe量子点的优异光学性能,并且在荧光显微镜下能够用肉眼观察到明显的绿色荧光。不仅如此,通过把原本不稳定的分散液状态的CdSe量子点组装到纤维素表面,不仅得到了宏观大块的发光复合材料,并且此材料的优异发光性质能够维持长达数月之久。
(2)一步水热法制备纤维素/ZnS:Mn量子点复合发光材料：在水热反应釜中加入纤维素,ZnS:Mn量子点的前体物质和聚乙烯亚胺,在180℃下反应8h,利用一步水热法成功地制备了纤维素/ZnS:Mn量子点复合材料。透射电子显微镜的表征有力地证明了对不含有纤维素基底的ZnS:Mn量子点来说,聚乙烯亚胺的加入能够很好地改善其分散性。同时,由于聚乙烯亚胺与纤维素材料之间的氢键相互作用作用,ZnS:Mn量子点能够更加均匀的组装在纤维素的纤维之上,而不需要其他额外的修饰。X射线光电子能谱也进一步地佐证了ZnS:Mn量子点在纤维素表面的组装。同样的,此纤维素/ZnS:Mn量子点复合材料在荧光显微镜下能够观察到稳定且明显的荧光现象。
(3)纤维素／双金属纳米颗粒复合催化材料：利用表面溶胶-凝胶法在纤维素表面沉积上二氧化钛凝胶薄膜,再利用层层自组装的方法,将带有不同电性的聚电解质和预先合成的五种不同组成的双金属纳米颗粒通过静电作用组装到纤维素表面,制备得到了纤维素／双金属纳米颗粒复合材料。扫描电子显微镜的表明了利用此方法得到的五种不同组成的复合材料保留了原始纤维素的三维复杂层次性结构。透射电子显微镜中能够明显地看到Cu-Ag, Cu-Au, Fe-Ag, Fe-Au以及Au-Ag双金属纳米颗粒均匀地分布在纤维素的纤维之上。紫外-可见光谱上能够观察到金属纳米颗粒对应的特征表面等离子体共振吸收峰。此五种纤维素／双金属纳米颗粒复合材料都对硼氢化钠还原对硝基苯分表现出了很高的催化活性,反应原料液三次过滤经过此复合材料后,转化率均能够高达95%以上,并且由于纤维素基底的优势,产物的分离和催化剂的循环再利用都明显简单快捷的多。
(4)纤维素／文石型碳酸钙晶体复合超疏水材料：利用表面溶胶-凝胶法在纤维素表面沉积上二氧化钛凝胶薄膜,将其放在氯化钙溶液中吸附钙离子,再放在碳酸钠溶液中使其表面沉积上碳酸钙的小晶核,最后放进50℃的含有多种离子的地热水中进行碳酸钙晶体的生长。经过48h后,在修饰有二氧化钛凝胶薄膜的纤维素表面生长上了高相纯度的针状文石型碳酸钙晶体。通过对不同晶体生长时间的样品的表征发现,高相纯度的文石晶体的形成经历了方解石型晶体的溶解和再结晶过程。当在地热水中生长时间超过24h后,最稳定的方解石晶体逐渐溶解,并且由于二氧化钛凝胶膜与地热水中镁离子等的作用,再结晶形成了针状的文石晶体。此纤维素／文石型碳酸钙晶体复合材料再经过低表面能的硬脂酸钠修饰过后,对水的接触角能够达到153°,是一种具有很好生物相容性的超疏水材料。
With the rapid development of modern technology, lots of researchers found that the mirco-and nano-scaled materials have unique properties compared with bulk materials even with the same composition. For example, semiconductor nanocrystals have very different optoelectronic properties such as size-tuned fluorescence which benefits from the rather small size in the nanoscale. Noble metallic nanoparticles show great potentials in catalysts. However, bulk noble metals are known to be extremely inert. As a result, making better use of these inorganic nanocrystals has become a focus in the field of fabricating new functional composite materials.
Herein, several kinds of inorganic nanocrystals like quantum dots, bimetallic nanoparticles and calcium carbonate were assembled or directly grown on natural cellulose substrates. After the appropriate treatments, the original unstable inorganic nanocrystals had been immobilized on the polymer substrates to generate multi-dimensional functional composite materials. The extraordinary properties of the inorganic nanocrystals were reserved. And because of the existence of the polymer substrates the practical applications of the composite materials have also been extended. The details are described as follows.
(1) Bulk luminescent cellulose/CdSe QDs composite material:Each cellulose nanofiber of the filter paper was firstly coated with nanometrethick titania film by means of the surface sol-gel process, followed by alternative deposition of self-assembled layers of stearic acid (SA) and TOPO/HDA capped CdSe nanoparticles, giving a filter paper/titania/SA/(CdSe/SA) composite luminescent sheet possessing stable and well-defined green fluorescence. SEM and TEM observations showed that the resulting luminescent sheet retained the hierarchical structures and morphologies of the initial cellulose substance; meanwhile, the CdSe nanoparticles were anchored on the nanofiber surfaces within SA thin layers through the hydrophobic interaction between the alkyl chains of the surface ligands of CdSe nanoparticles and SA molecules. UV-vis and photoluminescence spectra indicated that the resulting luminescent sheet showed similar characteristic absorption and emission properties as those of the original CdSe nanoparticles. The luminescent property of this composite material can be kept for over months.
(2) One-step fabrication of cellulose/ZnS:Mn QDs composite material:A bulk piece of cellulose/ZnS:Mn QDs composite material has been generated through a facile one-step hydrothermal method. TEM results show that the employment of PEI improves the dispersibility of the virginal ZnS:Mn QDs. With the help of hydrogen interaction between PEI and cellulose substances, there was no need of extra modification of the filter paper. XPS results further comfirm the success of immobilization of the ZnS:Mn QDs onto cellulose substrate. The ZnS:Mn QDs were found to be uniformly immobilized on the fibers of the filter paper, which gives the obtained bulk composite material stable and well-defined luminescent property.
(3) Catalytic cellulose/bimetallic nanoparticels composite materials:Employing titanium (IV) n-butoxide as precursor, ultrathin titania gel films were deposited on cellulose nanofiber in bulk filter paper by the surface sol-gel process. Five kinds of bimetallic nanoparticles (BNPs) were synthesized by the reduction of NaBH4and sodium citrate. These BNPs were immobilized onto the fibers of the titania-modified filter paper through the electrostatic interaction between the positively charged poly(diallyldimethylammonium chloride)(PDDA) and negatively charged BNPs. The electron microscopes results revealed that the fabricated bulk composite materials inherited the original three-dimensional morphology of the initial filter paper. Moreover, these five kinds of composite materials showed good efficient catalytic activities on the reduction of4-nitrophenol by NaBH4by means of simply filtration three times of the feed solution through the BNPs-related composite materials. The catalytic activities maintained even after ten cycles of the three-time filtration, which indicated the stability and reusability of the BNPs-related composite materials.
(4) Cellulose/aragonite crystals composite material:Employing titanium (IV) n-butoxide as precursor, ultrathin titania gel films were deposited on cellulose nanofiber in bulk filter paper by the surface sol-gel process. After prenucleation with calcium carbonate nanoparticles, the titania-modified filter paper was put into classic geothermal water for the growth of needle-like aragonite calcium carbonate crystals, and the needle-like calcium carbonate crystals were guaranteed to be pure aragonite. The mechanism of the formation of the pure aragonite crystals is that the calcium carbonate crystals may undergo a dissolution and recrystallization process. After the surface modification with a monolayer of sodium stearate, this composite material was endowed with a superhydrophobic property showing a water contact angle of153°.
本文利用不同的组装或生长技术,在天然纤维素物质上固定上多种无机纳米晶体,包括量子点,金属纳米颗粒,碳酸钙晶体,从而使这些无机纳米晶体从难以直接利用且不稳定的分散液状态转变成为多维乃至宏观大块的新型复合材料,扩展了这些具有优异性能的无机纳米晶体的实际应用价值。主要内容如下：
(1)纤维素/CdSe量子点复合发光材料：首先利用钛酸四丁酯在纤维素基底上沉积二氧化钛凝胶薄膜,再将硬脂酸利用羧基与钛的配位作用沉积在其表面,最后通过合成得到的三辛基氧化膦与十六烷基胺包裹的CdSe量子点表面烷基与硬脂酸烷基链之间的疏水作用,制备得到纤维素/CdSe量子点复合发光材料。扫描电子显微镜的结果表明纤维素原有的三维复杂层次性结构没有任何破坏。透射电子显微镜中能够看到在纤维素的纳米纤维上均匀地分布有CdSe量子点颗粒。紫外-可见和荧光光谱表征表明了此复合材料很好地继承了CdSe量子点的优异光学性能,并且在荧光显微镜下能够用肉眼观察到明显的绿色荧光。不仅如此,通过把原本不稳定的分散液状态的CdSe量子点组装到纤维素表面,不仅得到了宏观大块的发光复合材料,并且此材料的优异发光性质能够维持长达数月之久。
(2)一步水热法制备纤维素/ZnS:Mn量子点复合发光材料：在水热反应釜中加入纤维素,ZnS:Mn量子点的前体物质和聚乙烯亚胺,在180℃下反应8h,利用一步水热法成功地制备了纤维素/ZnS:Mn量子点复合材料。透射电子显微镜的表征有力地证明了对不含有纤维素基底的ZnS:Mn量子点来说,聚乙烯亚胺的加入能够很好地改善其分散性。同时,由于聚乙烯亚胺与纤维素材料之间的氢键相互作用作用,ZnS:Mn量子点能够更加均匀的组装在纤维素的纤维之上,而不需要其他额外的修饰。X射线光电子能谱也进一步地佐证了ZnS:Mn量子点在纤维素表面的组装。同样的,此纤维素/ZnS:Mn量子点复合材料在荧光显微镜下能够观察到稳定且明显的荧光现象。
(3)纤维素／双金属纳米颗粒复合催化材料：利用表面溶胶-凝胶法在纤维素表面沉积上二氧化钛凝胶薄膜,再利用层层自组装的方法,将带有不同电性的聚电解质和预先合成的五种不同组成的双金属纳米颗粒通过静电作用组装到纤维素表面,制备得到了纤维素／双金属纳米颗粒复合材料。扫描电子显微镜的表明了利用此方法得到的五种不同组成的复合材料保留了原始纤维素的三维复杂层次性结构。透射电子显微镜中能够明显地看到Cu-Ag, Cu-Au, Fe-Ag, Fe-Au以及Au-Ag双金属纳米颗粒均匀地分布在纤维素的纤维之上。紫外-可见光谱上能够观察到金属纳米颗粒对应的特征表面等离子体共振吸收峰。此五种纤维素／双金属纳米颗粒复合材料都对硼氢化钠还原对硝基苯分表现出了很高的催化活性,反应原料液三次过滤经过此复合材料后,转化率均能够高达95%以上,并且由于纤维素基底的优势,产物的分离和催化剂的循环再利用都明显简单快捷的多。
(4)纤维素／文石型碳酸钙晶体复合超疏水材料：利用表面溶胶-凝胶法在纤维素表面沉积上二氧化钛凝胶薄膜,将其放在氯化钙溶液中吸附钙离子,再放在碳酸钠溶液中使其表面沉积上碳酸钙的小晶核,最后放进50℃的含有多种离子的地热水中进行碳酸钙晶体的生长。经过48h后,在修饰有二氧化钛凝胶薄膜的纤维素表面生长上了高相纯度的针状文石型碳酸钙晶体。通过对不同晶体生长时间的样品的表征发现,高相纯度的文石晶体的形成经历了方解石型晶体的溶解和再结晶过程。当在地热水中生长时间超过24h后,最稳定的方解石晶体逐渐溶解,并且由于二氧化钛凝胶膜与地热水中镁离子等的作用,再结晶形成了针状的文石晶体。此纤维素／文石型碳酸钙晶体复合材料再经过低表面能的硬脂酸钠修饰过后,对水的接触角能够达到153°,是一种具有很好生物相容性的超疏水材料。
With the rapid development of modern technology, lots of researchers found that the mirco-and nano-scaled materials have unique properties compared with bulk materials even with the same composition. For example, semiconductor nanocrystals have very different optoelectronic properties such as size-tuned fluorescence which benefits from the rather small size in the nanoscale. Noble metallic nanoparticles show great potentials in catalysts. However, bulk noble metals are known to be extremely inert. As a result, making better use of these inorganic nanocrystals has become a focus in the field of fabricating new functional composite materials.
Herein, several kinds of inorganic nanocrystals like quantum dots, bimetallic nanoparticles and calcium carbonate were assembled or directly grown on natural cellulose substrates. After the appropriate treatments, the original unstable inorganic nanocrystals had been immobilized on the polymer substrates to generate multi-dimensional functional composite materials. The extraordinary properties of the inorganic nanocrystals were reserved. And because of the existence of the polymer substrates the practical applications of the composite materials have also been extended. The details are described as follows.
(1) Bulk luminescent cellulose/CdSe QDs composite material:Each cellulose nanofiber of the filter paper was firstly coated with nanometrethick titania film by means of the surface sol-gel process, followed by alternative deposition of self-assembled layers of stearic acid (SA) and TOPO/HDA capped CdSe nanoparticles, giving a filter paper/titania/SA/(CdSe/SA) composite luminescent sheet possessing stable and well-defined green fluorescence. SEM and TEM observations showed that the resulting luminescent sheet retained the hierarchical structures and morphologies of the initial cellulose substance; meanwhile, the CdSe nanoparticles were anchored on the nanofiber surfaces within SA thin layers through the hydrophobic interaction between the alkyl chains of the surface ligands of CdSe nanoparticles and SA molecules. UV-vis and photoluminescence spectra indicated that the resulting luminescent sheet showed similar characteristic absorption and emission properties as those of the original CdSe nanoparticles. The luminescent property of this composite material can be kept for over months.
(2) One-step fabrication of cellulose/ZnS:Mn QDs composite material:A bulk piece of cellulose/ZnS:Mn QDs composite material has been generated through a facile one-step hydrothermal method. TEM results show that the employment of PEI improves the dispersibility of the virginal ZnS:Mn QDs. With the help of hydrogen interaction between PEI and cellulose substances, there was no need of extra modification of the filter paper. XPS results further comfirm the success of immobilization of the ZnS:Mn QDs onto cellulose substrate. The ZnS:Mn QDs were found to be uniformly immobilized on the fibers of the filter paper, which gives the obtained bulk composite material stable and well-defined luminescent property.
(3) Catalytic cellulose/bimetallic nanoparticels composite materials:Employing titanium (IV) n-butoxide as precursor, ultrathin titania gel films were deposited on cellulose nanofiber in bulk filter paper by the surface sol-gel process. Five kinds of bimetallic nanoparticles (BNPs) were synthesized by the reduction of NaBH4and sodium citrate. These BNPs were immobilized onto the fibers of the titania-modified filter paper through the electrostatic interaction between the positively charged poly(diallyldimethylammonium chloride)(PDDA) and negatively charged BNPs. The electron microscopes results revealed that the fabricated bulk composite materials inherited the original three-dimensional morphology of the initial filter paper. Moreover, these five kinds of composite materials showed good efficient catalytic activities on the reduction of4-nitrophenol by NaBH4by means of simply filtration three times of the feed solution through the BNPs-related composite materials. The catalytic activities maintained even after ten cycles of the three-time filtration, which indicated the stability and reusability of the BNPs-related composite materials.
(4) Cellulose/aragonite crystals composite material:Employing titanium (IV) n-butoxide as precursor, ultrathin titania gel films were deposited on cellulose nanofiber in bulk filter paper by the surface sol-gel process. After prenucleation with calcium carbonate nanoparticles, the titania-modified filter paper was put into classic geothermal water for the growth of needle-like aragonite calcium carbonate crystals, and the needle-like calcium carbonate crystals were guaranteed to be pure aragonite. The mechanism of the formation of the pure aragonite crystals is that the calcium carbonate crystals may undergo a dissolution and recrystallization process. After the surface modification with a monolayer of sodium stearate, this composite material was endowed with a superhydrophobic property showing a water contact angle of153°.
引文
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