功能性层状双氢氧化物/聚合物纳米复合材料的制备及性能研究
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摘要
本论文主要研究聚合物基功能性纳米复合材料的结构与性能关系,以功能性层状双氢氧化物(LDHs)为无机组分,通过熔融共混法、可控取向堆积法及原位生长法分别制备剥离型LDHs/聚合物纳米复合材料、具有高取向结构的LDHs/聚合物复合薄膜及具有三维复杂结构的LDHs取向薄膜,研究纳米粒子的功能性、分散形态及取向结构对纳米复合材料各项性能的影响。
LDHs为阴离子型层状粘土,具有形貌可控、结构可调、易分散等优异性能,可作为功能性纳米填料制备LDHs/聚合物纳米复合材料。随着科学进步和世界经济的发展,各使用领域对材料的性能提出了更高要求,而具有光、电、磁效应以及自阻燃等特性的功能性纳米复合材料将成为未来军工、航空航天、汽车、电力电子等行业的首选材料。
制备聚合物基功能性纳米复合材料的方法有多种,可分别从聚合物基体、纳米粒子及分散形态三个方面调控纳米复合材料的功能性。最直接的方法是利用功能性聚合物为基体,制备具有温敏、光敏、导电等性能的纳米复合材料；由于功能性聚合物种类少,使用领域较窄,因而以功能性聚合物为基体的纳米复合材料研究和应用均较少。而将具有功能性(如具有光、电、磁、热响应以及导电导热等性能)的无机纳米粒子均匀分散于聚合物基体中,赋予普通聚合物基纳米复合材料功能性,则将大幅提高通用聚合物材料的性能,提升其应用潜力,具有较高的研究和应用价值。另一种方式是通过调控成型加工条件或无机纳米粒子在聚合物基体中的分散形态,构建具有特殊结构的纳米复合材料(如静电纺丝纳米纤维、取向薄膜、微-纳米复合结构材料等),从而赋予纳米复合材料功能性(如超疏水、超阻隔、选择性吸附等性能)。
本论文的研究分三部分进行。首先通过尿素水解法制备尺寸为微米级的LDHs,将其作为铜离子的“绿色”载体,制备具有阻燃、抑烟性能的MgCuAl-LDH微米粒子,并表征其结构与形貌。将制备的功能性MgCuAl-LDH与聚氯乙烯(PVC)熔融共混,制备LDHs/PVC纳米复合材料,考察功能性MgCuAl-LDH对PVC热稳定性、热分解行为以及燃烧发烟性能的影响。MgCuAl-LDH不仅能发挥铜离子显著的抑烟效果,还能保留LDHs的离子交换性能及对PVC的热稳定效应。对MgCuAl-LDH离子交换改性,并将改性LDHs分散于PVC基体中,考察LDHs纳米片层在PVC基体中的分散形态,发现十二烷基磺酸根(DS-)插层的MgCuAl-LDH能在基体中剥离,形成剥离型LDH/PVC纳米复合材料,并考察LDHs分散形态对纳米复合材料性能的影响。
第二部分为具有高取向结构LDHs/聚合物复合薄膜的制备,以及复合薄膜结构、形貌、性能及溶液中LDHs纳米片层与阴离子共组装行为的研究。以不同尺寸大小的CoAl-LDH (6μm)和NiAl-LDH (500 nm)为模型,利用NO3-LDHs在甲酰胺体系中的全剥离,首先制备了单片层分散的CoAl-和NiAl-LDH/甲酰胺溶胶,AFM结果显示LDHs单片层厚度约为0.8 nm；通过真空抽滤法快速制备了具有高取向结构的CoAl-和NiAl-LDH薄膜,发现能将其转印至多种基体表面：考察了LDHs薄膜的结构与形貌,提出了不同尺寸大小的LDH纳米片层在堆积成膜时不同的堆积机理；在LDHs/甲酰胺体系中加入阴离子与聚合物,考察LDHs片层与阴离子在甲酰胺中的共组装行为,并得到了能在水中稳定分散的、表面呈电负性的LDHs/阴离子聚丙烯酰胺杂化粒子；通过调控LDHs/甲酰胺体系中阴离子的种类及数量,还能获得性能优异的功能性LDHs薄膜。
第三部分为原位生长法制备LDHs取向薄膜的结构与性能研究。利用水热法分别在云母片及表面亲水处理的Si02电纺纤维膜表面原位生长LDHs,结果发现原位生长的LDHs晶体均垂直于基体表面取向排列；通过改变水热反应体系中的离子浓度,可调控LDHs取向薄膜的疏密度及LDHs晶体尺寸大小；在微米级电纺纤维表面原位生长取向LDHs,构筑具有三维复杂结构的功能性薄膜,具有广阔的应用前景。
本论文的相关研究,为功能性LDHs/聚合物纳米复合材料的设计提供了理论基础,将有益于设计出具有更优异性能的聚合物基功能性纳米复合材料。
Layered double hydroxide (LDHs) is a class of anionic clay with layered structure, represented by the general formula [MⅡ1-xMⅢx(OH)2]x+[An-x/n·yH2O]x-. LDHs can be synthesized with tunable morphology, composition and dispersibility by simple control over the conditions of preparation. Therefore, LDHs with designed morphology and function can be used as functional nanofillers in LDHs/polymer nanocomposites. There are various methods that can be applied to fabricate polymer based functional nanocomposites. Basically it can be categorized into three groups: functional polymer based, functional nanofiller based and structure based functional nanocomposites. Using functional polymer as matix of nanocomposites is the most direct way to obtain thermo-and photo-responsive, electro-conductive nanocomposites. However, functional polymers are limited in a few kinds of polymers and application fileds. Thus functional polymer based functional nanocomposites are rarely studied. On the contrary, functional nanocomposites fabricated by homogeneous dispersion of functional nanofiller into common polymer matrices will significantly enhance properties of nanocomposites, endowing common polymers with funtions. The other methods of fabricating functional nanocomposites are to deliberately design the structure of nanocomposites, e.g. electrospun nanofibers, oriented thin films, nanocomposites with micro/nano hybrid structures, etc. As a result, nanocomposites with superhydrophobic surfaces, superbarrier effect, and selective adorption, and so on, can be formed.
This thesis is focused on the studies of relationship between structure and properties of nanocomposites. Inorganic funtional LDHs are selected as nanofillers to fabricate exfoliated LDH/polymer nanocomposites and highly oriented LDH/polymer hybrid films by melt compounding and controlled orientation method, respectively. Besides, in situ growth of LDHs on mica and electrospun SiO2 fiber gave vertically oriented LDHs thin films with 3D hybrid structure, which show versatile functions and properties. The functionality of LDHs, dispersion morphology of LDHs in matrices, structure and properties of nanocomposites were studied and discussed.
In the first part, microsized LDH crystals were syntheized via urea hydrolysis method and used as green carrier for copper ions to fabricate functional MgCuAl-LDH which will be a new class of environmental friendly thermal stabilizers with efficient smoke suppression effect and mechanical enhancement for poly(vinyl chloride) (PVC). MgCuAl-LDH/PVC nanocomposites were fabricated by melt compounding. The thermal stablility, degradation behavior and smoke properties of nanocomposites were studied and discussed. It is found that MgCuAl-LDH not only retains the smoke suppression effect of copper ions, but also keeps the properties of LDHs. After anion exchange, MgCuAl-DS-LDH can be delaminated in PVC, forming exfoliated LDH/PVC nanocomposites. The relationship between dispersion morphology and performance of nanocomposits were consequently discussed.
The second part is mainly the fabrication and characterization of highly oriented LDH/polymer hybrid films and related studies of coassemly of LDH nanosheets with anions or polymers in formamide. LDHs with different lateral size, CoAl-LDH (6μm) and NiAl-LDH (500 nm), were syntheized, anion exchanged and delaminated in formamide to form exfoliated LDH nanosheets/formamide colloidal dispersion. The thickness of LDH monolayer was characterized to be about 0.8 nm by AFM. After vacuum filtration of LDH/formamide colloidal dispersion, highly oriented LDH thin films on filter membrane can be transfer-printed onto different substrates, forming transparent, strong and flexible LDH thin films. The morphology and structure studies of LDH films reveal different stacking modes of CoAl-LDH and NiAl-LDH. Utilizing coassembly of positively charged LDH nanosheets with polymeric anions, negatively charged LDH nanohybrids can be obtained. By adding various types of anions into colloidal dispersion of LDHs and subsequent filtration, LDH thin films with tunable composition and nanostructure can be prepared easily. This facile filtration method will facilitate the fabrication of functional LDH thin films.
The third part is the studies of in situ growth of LDHs on surfaces of mica and electrospun SiO2 micro-fiber. LDHs crystals vertically oriented on surfaces of substrates and can be easily controlled by tuning the hydro-thermo conditions. The in situ growth of LDHs on electrospun SiO2 micro-fiber built functional oriented LDHs thin films with 3D hybrid structure which have numerous potential applications.
LDHs为阴离子型层状粘土,具有形貌可控、结构可调、易分散等优异性能,可作为功能性纳米填料制备LDHs/聚合物纳米复合材料。随着科学进步和世界经济的发展,各使用领域对材料的性能提出了更高要求,而具有光、电、磁效应以及自阻燃等特性的功能性纳米复合材料将成为未来军工、航空航天、汽车、电力电子等行业的首选材料。
制备聚合物基功能性纳米复合材料的方法有多种,可分别从聚合物基体、纳米粒子及分散形态三个方面调控纳米复合材料的功能性。最直接的方法是利用功能性聚合物为基体,制备具有温敏、光敏、导电等性能的纳米复合材料；由于功能性聚合物种类少,使用领域较窄,因而以功能性聚合物为基体的纳米复合材料研究和应用均较少。而将具有功能性(如具有光、电、磁、热响应以及导电导热等性能)的无机纳米粒子均匀分散于聚合物基体中,赋予普通聚合物基纳米复合材料功能性,则将大幅提高通用聚合物材料的性能,提升其应用潜力,具有较高的研究和应用价值。另一种方式是通过调控成型加工条件或无机纳米粒子在聚合物基体中的分散形态,构建具有特殊结构的纳米复合材料(如静电纺丝纳米纤维、取向薄膜、微-纳米复合结构材料等),从而赋予纳米复合材料功能性(如超疏水、超阻隔、选择性吸附等性能)。
本论文的研究分三部分进行。首先通过尿素水解法制备尺寸为微米级的LDHs,将其作为铜离子的“绿色”载体,制备具有阻燃、抑烟性能的MgCuAl-LDH微米粒子,并表征其结构与形貌。将制备的功能性MgCuAl-LDH与聚氯乙烯(PVC)熔融共混,制备LDHs/PVC纳米复合材料,考察功能性MgCuAl-LDH对PVC热稳定性、热分解行为以及燃烧发烟性能的影响。MgCuAl-LDH不仅能发挥铜离子显著的抑烟效果,还能保留LDHs的离子交换性能及对PVC的热稳定效应。对MgCuAl-LDH离子交换改性,并将改性LDHs分散于PVC基体中,考察LDHs纳米片层在PVC基体中的分散形态,发现十二烷基磺酸根(DS-)插层的MgCuAl-LDH能在基体中剥离,形成剥离型LDH/PVC纳米复合材料,并考察LDHs分散形态对纳米复合材料性能的影响。
第二部分为具有高取向结构LDHs/聚合物复合薄膜的制备,以及复合薄膜结构、形貌、性能及溶液中LDHs纳米片层与阴离子共组装行为的研究。以不同尺寸大小的CoAl-LDH (6μm)和NiAl-LDH (500 nm)为模型,利用NO3-LDHs在甲酰胺体系中的全剥离,首先制备了单片层分散的CoAl-和NiAl-LDH/甲酰胺溶胶,AFM结果显示LDHs单片层厚度约为0.8 nm；通过真空抽滤法快速制备了具有高取向结构的CoAl-和NiAl-LDH薄膜,发现能将其转印至多种基体表面：考察了LDHs薄膜的结构与形貌,提出了不同尺寸大小的LDH纳米片层在堆积成膜时不同的堆积机理；在LDHs/甲酰胺体系中加入阴离子与聚合物,考察LDHs片层与阴离子在甲酰胺中的共组装行为,并得到了能在水中稳定分散的、表面呈电负性的LDHs/阴离子聚丙烯酰胺杂化粒子；通过调控LDHs/甲酰胺体系中阴离子的种类及数量,还能获得性能优异的功能性LDHs薄膜。
第三部分为原位生长法制备LDHs取向薄膜的结构与性能研究。利用水热法分别在云母片及表面亲水处理的Si02电纺纤维膜表面原位生长LDHs,结果发现原位生长的LDHs晶体均垂直于基体表面取向排列；通过改变水热反应体系中的离子浓度,可调控LDHs取向薄膜的疏密度及LDHs晶体尺寸大小；在微米级电纺纤维表面原位生长取向LDHs,构筑具有三维复杂结构的功能性薄膜,具有广阔的应用前景。
本论文的相关研究,为功能性LDHs/聚合物纳米复合材料的设计提供了理论基础,将有益于设计出具有更优异性能的聚合物基功能性纳米复合材料。
Layered double hydroxide (LDHs) is a class of anionic clay with layered structure, represented by the general formula [MⅡ1-xMⅢx(OH)2]x+[An-x/n·yH2O]x-. LDHs can be synthesized with tunable morphology, composition and dispersibility by simple control over the conditions of preparation. Therefore, LDHs with designed morphology and function can be used as functional nanofillers in LDHs/polymer nanocomposites. There are various methods that can be applied to fabricate polymer based functional nanocomposites. Basically it can be categorized into three groups: functional polymer based, functional nanofiller based and structure based functional nanocomposites. Using functional polymer as matix of nanocomposites is the most direct way to obtain thermo-and photo-responsive, electro-conductive nanocomposites. However, functional polymers are limited in a few kinds of polymers and application fileds. Thus functional polymer based functional nanocomposites are rarely studied. On the contrary, functional nanocomposites fabricated by homogeneous dispersion of functional nanofiller into common polymer matrices will significantly enhance properties of nanocomposites, endowing common polymers with funtions. The other methods of fabricating functional nanocomposites are to deliberately design the structure of nanocomposites, e.g. electrospun nanofibers, oriented thin films, nanocomposites with micro/nano hybrid structures, etc. As a result, nanocomposites with superhydrophobic surfaces, superbarrier effect, and selective adorption, and so on, can be formed.
This thesis is focused on the studies of relationship between structure and properties of nanocomposites. Inorganic funtional LDHs are selected as nanofillers to fabricate exfoliated LDH/polymer nanocomposites and highly oriented LDH/polymer hybrid films by melt compounding and controlled orientation method, respectively. Besides, in situ growth of LDHs on mica and electrospun SiO2 fiber gave vertically oriented LDHs thin films with 3D hybrid structure, which show versatile functions and properties. The functionality of LDHs, dispersion morphology of LDHs in matrices, structure and properties of nanocomposites were studied and discussed.
In the first part, microsized LDH crystals were syntheized via urea hydrolysis method and used as green carrier for copper ions to fabricate functional MgCuAl-LDH which will be a new class of environmental friendly thermal stabilizers with efficient smoke suppression effect and mechanical enhancement for poly(vinyl chloride) (PVC). MgCuAl-LDH/PVC nanocomposites were fabricated by melt compounding. The thermal stablility, degradation behavior and smoke properties of nanocomposites were studied and discussed. It is found that MgCuAl-LDH not only retains the smoke suppression effect of copper ions, but also keeps the properties of LDHs. After anion exchange, MgCuAl-DS-LDH can be delaminated in PVC, forming exfoliated LDH/PVC nanocomposites. The relationship between dispersion morphology and performance of nanocomposits were consequently discussed.
The second part is mainly the fabrication and characterization of highly oriented LDH/polymer hybrid films and related studies of coassemly of LDH nanosheets with anions or polymers in formamide. LDHs with different lateral size, CoAl-LDH (6μm) and NiAl-LDH (500 nm), were syntheized, anion exchanged and delaminated in formamide to form exfoliated LDH nanosheets/formamide colloidal dispersion. The thickness of LDH monolayer was characterized to be about 0.8 nm by AFM. After vacuum filtration of LDH/formamide colloidal dispersion, highly oriented LDH thin films on filter membrane can be transfer-printed onto different substrates, forming transparent, strong and flexible LDH thin films. The morphology and structure studies of LDH films reveal different stacking modes of CoAl-LDH and NiAl-LDH. Utilizing coassembly of positively charged LDH nanosheets with polymeric anions, negatively charged LDH nanohybrids can be obtained. By adding various types of anions into colloidal dispersion of LDHs and subsequent filtration, LDH thin films with tunable composition and nanostructure can be prepared easily. This facile filtration method will facilitate the fabrication of functional LDH thin films.
The third part is the studies of in situ growth of LDHs on surfaces of mica and electrospun SiO2 micro-fiber. LDHs crystals vertically oriented on surfaces of substrates and can be easily controlled by tuning the hydro-thermo conditions. The in situ growth of LDHs on electrospun SiO2 micro-fiber built functional oriented LDHs thin films with 3D hybrid structure which have numerous potential applications.
引文
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