基于微/纳米结构单元的有序组装制备仿生结构功能复合材料
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摘要
在纳米材料合成日趋成熟的背景下,如何使得这些具有新颖性质的纳米材料在实际应用中发挥作用是当前面临的挑战之一。目前,利用先进的组装技术,将微纳功能结构单元集合成具有多级微纳结构的宏观块材是纳米材料应用研究的重要方向。通过微纳结构功能单元有序的组装,这些纳米结构单元的新颖性质在宏观块材中不仅能够得到了保留,而且还通过各个结构单元之间的协同和复合展现出多重性质和特殊功能。另一方面,仿生微纳结构材料的研究表明,在宏观尺度的人工块材中设计和仿造生物的多级微纳结构能够优化和提高材料的整体性质。在多级微纳结构材料的设计和制备上,自然界给予了我们很多启发和模型。比如,具有“砖-泥”微纳层状结构的珍珠母层,骨骼的多级“纤维板层”结构,木材的“多孔”结构,开心果壳以及仙人掌刺的“带状复合板层”结构,海绵的“三维网络”结构,等等。
本论文将集中阐述基于仿生微纳结构模型和微纳结构单元的合成与组装制备多功能微纳结构复合材料。首先通过对生物材料的多级结构和组成单元的分析,寻找和设计合适的人工微纳结构组装单元;然后大量合成具有特殊形貌的微纳结构功能材料,如一维纤维状结构材料,二维片状或板状结构材料;最后利用先进的组装技术将合成得到的微纳结构单元与聚合物复合制得功能性的微纳结构复合薄膜和块材,并研究这些宏观材料优越的力学性质,特殊的光,电学性质,以及性质之间的协同和关联。所取得的主要研究结果总结如下:
1.成功制备了仿珍珠母层状结构的无机微纳板材-聚合物高强功能性杂化薄膜。在本工作中,我们以珍珠母层状结构为模型,首先大量合成了具有板状形貌的双层氢氧化物(LDHs)和沸石(zeolites),然后通过界面组装和旋涂层层组装的方法得到了一系列的以LDHs或zeolites微米板为无机组装单元的高强、透光的类珍珠母结构的功能性杂化薄膜。此类薄膜具有类似珍珠母的层状微结构,在抗拉伸方面表现优异,可以同天然贝壳媲美。更有趣的是,此类有机无机杂化薄膜非常透明,并且光学性质可以通过使用不同的板块状结构单元来调控。
2.利用天然粘土和生物大分子壳聚糖的自组装成功制备了仿珍珠母结构的有机无机杂化薄膜。此工作中,我们设计了一套粘土-壳聚糖杂化构筑单元自组装流程成功制备了具有珍珠母结构的有机无机生物纳米复合薄膜。所制得的薄膜拉伸强度可以达到100 MPa,具有良好的透光性,并且能在水中变得更加透明。更有意思的是,此类薄膜在抗火性上有良好表现,整体结构不会被破坏。另外,还通过原位生长法,在粘土-壳聚糖杂化纳米片表面修饰一层均匀的金纳米颗粒。然后再将修饰金纳米颗粒的二维杂化纳米结构组装成珍珠母层状结构的复合薄膜,在取得一定机械强度的基础上,扩展此类杂化薄膜的功能和应用。
3.围绕二维纳米结构的氧化石墨烯(GO)设计和制备了具有珍珠母层状结构的陶瓷-石墨烯功能性复合薄膜和块材。(1).以二氧化钛(TiO)和氧化石墨烯(GO)纳米片作为功能性结构单元,我们可以通过TiO纳米薄片光还原GO成为还原型石墨烯(RGO)直接在GO/聚二烯丙基二甲基铵(PDDA)/TiO层层组装复合薄膜上设计光导图案。首先,高质量的GO/PDDA/TiO复合膜通过层层组装技术在玻璃衬底上交替浸涂GO、PDDA和TiO纳米薄片而得到。然后将复合膜在装备刻有图样的铝箔为遮光板的条件下用300W的Xe灯照射适当的时间,在光照区域形成具有光导性质的图案。(2).以GO为模板,在其表面包覆一层介孔氧化硅的前驱物。然后将得到的GO-介孔氧化硅前驱物杂化纳米片粉末放入模具,经过热压得到还原型石墨烯(RGO)-介孔氧化硅纳米复合块材。制得的RGO-介孔氧化硅纳米复合块材具有介孔氧化硅连接RGO纳米片的层状微观结构,表现出轻质,高强和导电的多重性质。
4.以水热反应合成的Ag@聚乙烯醇(PVA)三维仿海绵网络为模板成功制备了宏观尺度的类海绵状弹性导体。由相互搭接的一维纳米材料组成的类似海绵体的三维网络材料,由于其多孔性,高比表面,轻质,和优越的机械性能,受到了材料学家的广泛关注。我们在以往合成Ag@PVA同轴微电缆的基础上,进一步改进实验,合成了自支撑的Ag@PVA同轴电缆的三维网络海绵结构。将Ag@PVA同轴电缆海绵体在惰性气氛下碳化,得到Ag-C纳米电缆和C纳米管组成的三维弹性导体。通过这种模板法制备得到的弹性导体表现出良好的弹性,高的导电性(导电率为1.28S·m~(-1)),和很好的压缩循环性。另外,硅树脂还能填充到制得的弹性导体网络中,形成具有更高弹性模量的导电复合块材。
5.作为大量有效合成特殊纳米结构材料的普适方法,以小分子胺为模板合成一系列规整形貌的有机-无机杂化纳米材料,并以纳米杂化材料为前驱物制备了功能性无机纳米结构材料的思路被进一步发展。我们合成了一类新颖的具有蓝色荧光的超长亚碲酸镉-多胺有机无机杂化纳米纤维,并研究了其热稳定性和酸稳定性;合成了平板状的肼-亚碲酸镉杂化微米晶,并以此为前驱物得到了多孔碲化镉和碲微晶;以(Cd2Se2)(pa)(pa=丙胺)有机-无机杂化材料作为前驱物,在油相中热解得到各种CdSe纳米结构,并研究了其中的结构演变和光学性质。这些功能性纳米结构材料有望作为仿生微纳结构材料的组装单元。
In the past decades, various nanostructured materials have been synthesized via mature techniques. However, the currently emerging challenge is that how to efficiently utilize these novel functional nanomaterials in practical fields. The assembly of functional nano-building blocks into macroscale bulk materials within hierarchical micro-/nano- structures via advantaged fabrication techniques is a feasile route to broaden the practical applications of nanostructured materials. By hierarchical assembly of nano-building blocks, the obtained bulk materials not only own the properties of nano-building blocks but also behave the synergetic properties and multifunctionalities due to the hierarchical organizations. One the other hand, the research on bio-inspired hierarchical structures indicates that mimicking the?biological hierarchical structure in artificial material can enhance and optimize the property and functionality. For the design and fabrication of hierarchical structures, nature offers us much inspiration and many models. For example, the“brick and mortar”structured nacre, the bone’s“nanofiber consisted plate”structure, wood’s“cellular”structure, the“nanobelt assembled plate”structure of pistachio’s shell and cactus’s spicule, sponges’s“three dimensional network”structure, and so on.
The present dissertation will focus on the fabrication of bio-inspired hierarchical structured functional composite materials based on the models of biomaterials and ordered assembly of artificially synthesized functional micro-/nano- building blocks. According to the components and structures analysis of biomaterials, we firstly searched and designed proper artificial building blocks. Then, we synthesized these artificial building blocks on large scale, such as one dimensional nano fibrious materials and two dimensional platelet-like or sheet-like nanomaterials. Finally, we assembled these artificial inorganic building blocks together with polymers to fabricate bio-inspired structural functional composite materials. The excellent mechanical propeties, special optical and electric properties, and their multifunctionalities have been studied. The main results can be summarized as follows:
1. Biologically inspired, strong, transparent, and functional layered double hydroxides (LDHs) or zeolites micro-bricks reinforced composite films have been successfully fabricated. In this work, according to the model of layered structure of nacre, we firstly synthesized the platelet-like LDHs or zeolites microcrystals on large scale. Then, by using these LDHs or zeoites platelet-like microcrystals as inorganic building blocks, a series of strong, transparent, functional nacre-like layered hybrid films were fabricated via interfacial assembly and layer by layer spin coating technique. The obtained hybrid films displayed nacre-like layered microstructures and behaved excellent tensile strength which is comparable to that of natural nacre. Interestingly, these hybrid films are transparent and their optical properties can be tuned by using different inorganic functional building blocks.
2. Artificial nacre-like chitosan-Montmorillonite (MTM) bionanocomposite films with amazing‘brick and mortar’microstructures have been fabricated based on using chitosan-MTM hybrid nanosheets as building blocks. In the designed fabrication procedure, we assembled hybrid building blocks with thin layer of chitosan coating on the MTM nanosheets to form chitosan-MTM bionanocomposite film via vacuum filtration or water evaporation. The obtained nacre-like films displayed higher performance in mechanical properties (Young’s modulus: 10 GPa, tensile strength: 100 MPa) compared with the film made by conventional method. Moreover, these hybrid films are transparent and fire-retardant. Addtionally, gold nanoparticles (Au NPs) can be modified on the surfaces of chitosan-MTM hybrid nanosheets via in situ growth method. The obtained chitosan-MTM-Au NPs hybrid building blocks can also been assembled to form nacre-like layer structured films with good tensile strength and novle optical properties expanding the applications of nacre-like chitosan-MTM hybrid films.
3. Based on the ultrafine two dimensional structure of graphene oxide, we designed and fabricated a series of nacre-like layer structured reduced graphene oxide-ceramic nanocomposite films and bulk bricks: (1) By using graphene oxide (GO) and titania oxide (TiO) nanosheets as functional building blocks, high quality (PDDA/GO/PDDA/TiO)20 hybrid films were fabricated on the glass substrate through alternatively LBL self-assembly with GO, TiO nanosheets, and PDDA. Then, the photoconductive pattern was fabricated by illuminating the hybrid film equipped with a pre-designed aluminum foil as the shadow mask through the photothermal and photocatalyic reduction; (2) The graphene oxide nanosheets were firstly coated with mesoporous silicon precursor to form the GO-mesoporous silicon precursor hybrid nanosheets. Then, these obtained GO-mesoporous silicon precursor hybrid nanosheets were hot pressed together to yield a bulk brick which consisted of lamellar RGO connected by mesoporous silicon. The bulk brick is light weight, robust, and conductive due to its hierarchial structures.
4. Elastomeric conductors composed of sponge-like three dimensional silver-carbon hybrid nanocable/carbon nanotube networks have been fabricated by using hydrothermal synthesized Ag@PVA nanocables networks as templates. Sponge-like materials, composed of interconnected one dimensional nanostructures, have attracted intensive attention of researchers due to their high porosity, high surface area, light-weight, and excellent mechanical strength. By carefully controlling the conditions of hydrothermal reaction, we firstly demonstrated that the silver@PVA nanocables can grow and interconnect each other to form the cylinder-shaped three dimensional networks. Through carbonization of silver@PVA nanocable networks, the conductive silver-carbon hybrid nanocable/nanotube sponges can be fabricated as elastomeric conductors, which show good compressive properties and high conductivties (1.28 S·m-1), and good reversibility. Moreover, these artificial sponges can also be used to fabricate the conductive nanocomposites due to their percolating three-dimensional network nanostrucutres.
5. As a feasible route to synthesize various nanostructured materials, the small organic amine templating synthesis of organic-inorganic hybrid nanostructured materials has been further developed. The obtained hybrid nanostructured materials can be also used as efficient precursors to synthesize functional inorganic nanomaterials. We synthesized a new kind of blue light emitting ultralong Cd(L)(TeO3) (L = ethylenediamine, diethylenetriamine) nanofibre bundles and studies their thermal and acidic stabilities; prepared uniform, well-defined, and platelet-like hydrazine-cadmium tellurite hybrid microcrystals and used them as precursors to yield porous cadmium telluride and tellurium architectures; synthesized the Cd2Se2(pa) hybrid materials and used them as a precursor to explore the“top-down”fabrication process of structural evolution from two dimensional layered structures to zero- or one- dimensional nanocrystals. These functional nanostructured materials are also promising to be used as building blocks in the fabrication of bio-inspired hierarchical structured materials.
本论文将集中阐述基于仿生微纳结构模型和微纳结构单元的合成与组装制备多功能微纳结构复合材料。首先通过对生物材料的多级结构和组成单元的分析,寻找和设计合适的人工微纳结构组装单元;然后大量合成具有特殊形貌的微纳结构功能材料,如一维纤维状结构材料,二维片状或板状结构材料;最后利用先进的组装技术将合成得到的微纳结构单元与聚合物复合制得功能性的微纳结构复合薄膜和块材,并研究这些宏观材料优越的力学性质,特殊的光,电学性质,以及性质之间的协同和关联。所取得的主要研究结果总结如下:
1.成功制备了仿珍珠母层状结构的无机微纳板材-聚合物高强功能性杂化薄膜。在本工作中,我们以珍珠母层状结构为模型,首先大量合成了具有板状形貌的双层氢氧化物(LDHs)和沸石(zeolites),然后通过界面组装和旋涂层层组装的方法得到了一系列的以LDHs或zeolites微米板为无机组装单元的高强、透光的类珍珠母结构的功能性杂化薄膜。此类薄膜具有类似珍珠母的层状微结构,在抗拉伸方面表现优异,可以同天然贝壳媲美。更有趣的是,此类有机无机杂化薄膜非常透明,并且光学性质可以通过使用不同的板块状结构单元来调控。
2.利用天然粘土和生物大分子壳聚糖的自组装成功制备了仿珍珠母结构的有机无机杂化薄膜。此工作中,我们设计了一套粘土-壳聚糖杂化构筑单元自组装流程成功制备了具有珍珠母结构的有机无机生物纳米复合薄膜。所制得的薄膜拉伸强度可以达到100 MPa,具有良好的透光性,并且能在水中变得更加透明。更有意思的是,此类薄膜在抗火性上有良好表现,整体结构不会被破坏。另外,还通过原位生长法,在粘土-壳聚糖杂化纳米片表面修饰一层均匀的金纳米颗粒。然后再将修饰金纳米颗粒的二维杂化纳米结构组装成珍珠母层状结构的复合薄膜,在取得一定机械强度的基础上,扩展此类杂化薄膜的功能和应用。
3.围绕二维纳米结构的氧化石墨烯(GO)设计和制备了具有珍珠母层状结构的陶瓷-石墨烯功能性复合薄膜和块材。(1).以二氧化钛(TiO)和氧化石墨烯(GO)纳米片作为功能性结构单元,我们可以通过TiO纳米薄片光还原GO成为还原型石墨烯(RGO)直接在GO/聚二烯丙基二甲基铵(PDDA)/TiO层层组装复合薄膜上设计光导图案。首先,高质量的GO/PDDA/TiO复合膜通过层层组装技术在玻璃衬底上交替浸涂GO、PDDA和TiO纳米薄片而得到。然后将复合膜在装备刻有图样的铝箔为遮光板的条件下用300W的Xe灯照射适当的时间,在光照区域形成具有光导性质的图案。(2).以GO为模板,在其表面包覆一层介孔氧化硅的前驱物。然后将得到的GO-介孔氧化硅前驱物杂化纳米片粉末放入模具,经过热压得到还原型石墨烯(RGO)-介孔氧化硅纳米复合块材。制得的RGO-介孔氧化硅纳米复合块材具有介孔氧化硅连接RGO纳米片的层状微观结构,表现出轻质,高强和导电的多重性质。
4.以水热反应合成的Ag@聚乙烯醇(PVA)三维仿海绵网络为模板成功制备了宏观尺度的类海绵状弹性导体。由相互搭接的一维纳米材料组成的类似海绵体的三维网络材料,由于其多孔性,高比表面,轻质,和优越的机械性能,受到了材料学家的广泛关注。我们在以往合成Ag@PVA同轴微电缆的基础上,进一步改进实验,合成了自支撑的Ag@PVA同轴电缆的三维网络海绵结构。将Ag@PVA同轴电缆海绵体在惰性气氛下碳化,得到Ag-C纳米电缆和C纳米管组成的三维弹性导体。通过这种模板法制备得到的弹性导体表现出良好的弹性,高的导电性(导电率为1.28S·m~(-1)),和很好的压缩循环性。另外,硅树脂还能填充到制得的弹性导体网络中,形成具有更高弹性模量的导电复合块材。
5.作为大量有效合成特殊纳米结构材料的普适方法,以小分子胺为模板合成一系列规整形貌的有机-无机杂化纳米材料,并以纳米杂化材料为前驱物制备了功能性无机纳米结构材料的思路被进一步发展。我们合成了一类新颖的具有蓝色荧光的超长亚碲酸镉-多胺有机无机杂化纳米纤维,并研究了其热稳定性和酸稳定性;合成了平板状的肼-亚碲酸镉杂化微米晶,并以此为前驱物得到了多孔碲化镉和碲微晶;以(Cd2Se2)(pa)(pa=丙胺)有机-无机杂化材料作为前驱物,在油相中热解得到各种CdSe纳米结构,并研究了其中的结构演变和光学性质。这些功能性纳米结构材料有望作为仿生微纳结构材料的组装单元。
In the past decades, various nanostructured materials have been synthesized via mature techniques. However, the currently emerging challenge is that how to efficiently utilize these novel functional nanomaterials in practical fields. The assembly of functional nano-building blocks into macroscale bulk materials within hierarchical micro-/nano- structures via advantaged fabrication techniques is a feasile route to broaden the practical applications of nanostructured materials. By hierarchical assembly of nano-building blocks, the obtained bulk materials not only own the properties of nano-building blocks but also behave the synergetic properties and multifunctionalities due to the hierarchical organizations. One the other hand, the research on bio-inspired hierarchical structures indicates that mimicking the?biological hierarchical structure in artificial material can enhance and optimize the property and functionality. For the design and fabrication of hierarchical structures, nature offers us much inspiration and many models. For example, the“brick and mortar”structured nacre, the bone’s“nanofiber consisted plate”structure, wood’s“cellular”structure, the“nanobelt assembled plate”structure of pistachio’s shell and cactus’s spicule, sponges’s“three dimensional network”structure, and so on.
The present dissertation will focus on the fabrication of bio-inspired hierarchical structured functional composite materials based on the models of biomaterials and ordered assembly of artificially synthesized functional micro-/nano- building blocks. According to the components and structures analysis of biomaterials, we firstly searched and designed proper artificial building blocks. Then, we synthesized these artificial building blocks on large scale, such as one dimensional nano fibrious materials and two dimensional platelet-like or sheet-like nanomaterials. Finally, we assembled these artificial inorganic building blocks together with polymers to fabricate bio-inspired structural functional composite materials. The excellent mechanical propeties, special optical and electric properties, and their multifunctionalities have been studied. The main results can be summarized as follows:
1. Biologically inspired, strong, transparent, and functional layered double hydroxides (LDHs) or zeolites micro-bricks reinforced composite films have been successfully fabricated. In this work, according to the model of layered structure of nacre, we firstly synthesized the platelet-like LDHs or zeolites microcrystals on large scale. Then, by using these LDHs or zeoites platelet-like microcrystals as inorganic building blocks, a series of strong, transparent, functional nacre-like layered hybrid films were fabricated via interfacial assembly and layer by layer spin coating technique. The obtained hybrid films displayed nacre-like layered microstructures and behaved excellent tensile strength which is comparable to that of natural nacre. Interestingly, these hybrid films are transparent and their optical properties can be tuned by using different inorganic functional building blocks.
2. Artificial nacre-like chitosan-Montmorillonite (MTM) bionanocomposite films with amazing‘brick and mortar’microstructures have been fabricated based on using chitosan-MTM hybrid nanosheets as building blocks. In the designed fabrication procedure, we assembled hybrid building blocks with thin layer of chitosan coating on the MTM nanosheets to form chitosan-MTM bionanocomposite film via vacuum filtration or water evaporation. The obtained nacre-like films displayed higher performance in mechanical properties (Young’s modulus: 10 GPa, tensile strength: 100 MPa) compared with the film made by conventional method. Moreover, these hybrid films are transparent and fire-retardant. Addtionally, gold nanoparticles (Au NPs) can be modified on the surfaces of chitosan-MTM hybrid nanosheets via in situ growth method. The obtained chitosan-MTM-Au NPs hybrid building blocks can also been assembled to form nacre-like layer structured films with good tensile strength and novle optical properties expanding the applications of nacre-like chitosan-MTM hybrid films.
3. Based on the ultrafine two dimensional structure of graphene oxide, we designed and fabricated a series of nacre-like layer structured reduced graphene oxide-ceramic nanocomposite films and bulk bricks: (1) By using graphene oxide (GO) and titania oxide (TiO) nanosheets as functional building blocks, high quality (PDDA/GO/PDDA/TiO)20 hybrid films were fabricated on the glass substrate through alternatively LBL self-assembly with GO, TiO nanosheets, and PDDA. Then, the photoconductive pattern was fabricated by illuminating the hybrid film equipped with a pre-designed aluminum foil as the shadow mask through the photothermal and photocatalyic reduction; (2) The graphene oxide nanosheets were firstly coated with mesoporous silicon precursor to form the GO-mesoporous silicon precursor hybrid nanosheets. Then, these obtained GO-mesoporous silicon precursor hybrid nanosheets were hot pressed together to yield a bulk brick which consisted of lamellar RGO connected by mesoporous silicon. The bulk brick is light weight, robust, and conductive due to its hierarchial structures.
4. Elastomeric conductors composed of sponge-like three dimensional silver-carbon hybrid nanocable/carbon nanotube networks have been fabricated by using hydrothermal synthesized Ag@PVA nanocables networks as templates. Sponge-like materials, composed of interconnected one dimensional nanostructures, have attracted intensive attention of researchers due to their high porosity, high surface area, light-weight, and excellent mechanical strength. By carefully controlling the conditions of hydrothermal reaction, we firstly demonstrated that the silver@PVA nanocables can grow and interconnect each other to form the cylinder-shaped three dimensional networks. Through carbonization of silver@PVA nanocable networks, the conductive silver-carbon hybrid nanocable/nanotube sponges can be fabricated as elastomeric conductors, which show good compressive properties and high conductivties (1.28 S·m-1), and good reversibility. Moreover, these artificial sponges can also be used to fabricate the conductive nanocomposites due to their percolating three-dimensional network nanostrucutres.
5. As a feasible route to synthesize various nanostructured materials, the small organic amine templating synthesis of organic-inorganic hybrid nanostructured materials has been further developed. The obtained hybrid nanostructured materials can be also used as efficient precursors to synthesize functional inorganic nanomaterials. We synthesized a new kind of blue light emitting ultralong Cd(L)(TeO3) (L = ethylenediamine, diethylenetriamine) nanofibre bundles and studies their thermal and acidic stabilities; prepared uniform, well-defined, and platelet-like hydrazine-cadmium tellurite hybrid microcrystals and used them as precursors to yield porous cadmium telluride and tellurium architectures; synthesized the Cd2Se2(pa) hybrid materials and used them as a precursor to explore the“top-down”fabrication process of structural evolution from two dimensional layered structures to zero- or one- dimensional nanocrystals. These functional nanostructured materials are also promising to be used as building blocks in the fabrication of bio-inspired hierarchical structured materials.
引文
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