以配合物为模板在离子液中制备无机/有机纳米材料
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摘要
纳米材料是目前材料化学研究的热点，被认为是本世纪最有前途的学科之一。以金属配合物为前驱体，是制备无机／有机纳米材料的有效手段：一方面可以利用配合物的模板作用，诱导纳米粒子生长；另一方面在制备纳米的同时，利用其表面效应将有机配体修饰到纳米粒子表面，能够防止纳米粒子团聚。由于无机配合物在水和大部分有机溶剂中溶解性差，限制了其在纳米材料制备中的应用。离子液，又称低温熔融盐，是完全由离子组成，在室温下呈现液态的化合物。离子液作为一种优良溶剂，能够溶解大部分无机化合物、有机化合物和聚合物。在离子液中制备纳米材料能充分利用其良好的溶解性、软模板作用，且重现性好、操作简单。因此，近年来受到人们的广泛关注。
本文通过文献调研，以一定结构的配合物为原料，利用配合物的模板作用，在离子液中制备了具有一定规则形貌的ZnS，PbS和Ag纳米微粒，并在纳米粒子表面修饰了有机配体，有效的防止纳米粒子的团聚。主要研究内容如下：
(1)制备并表征了3-二茂铁基-2-丁烯酸锌(Zn(FCA)_2)配位聚合物，利用Zn(FCA)_2形成的1D链和离子液模板的共同作用制备了ZnS纳米微粒。讨论了球形和花生形纳米粒子的形成机理，从反应前后FCA基团红外光谱的变化解释了羧酸基团配位模式的改变，认为羧酸基团以双齿螯合的配位模式修饰在ZnS纳米微粒表面。
(2)设计合成了四(对溴苯基)卟啉锌(ZnT(p-Br)PP)，通过X。射线单晶衍射确定了其单晶结构。发现其具有很好的平面性，相邻分子间通过对溴苯基与卟啉环之间的边一面π-π作用形成层状结构。制备了片状的ZnT(p-Br)PP纳米微粒，通过XRD，TEM和SEM对其进行了表征。以ZnT(p-Br)PP为前驱体、离子液为溶剂，分别通过低温和高温两种方法制备了不同尺寸的棒状ZnS纳米微粒，讨论了棒状纳米粒子的形成机理。测试了其光学性质，所得ZnS样品在350nm左右出现荧光发射峰。
(3)利用离子液的模板作用，成功地制备了长方体形的PbS纳米晶，运用HRTEM确定出PbS纳米晶体的晶体结构和生长晶面。此外，合成、表征了具有良好光学性质的咔唑类羧酸及其Pb的配合物，并以Pb的配合物为前驱体在离子液中制备了粒径小于10 nm的硫化铅纳米粒子；测试了其不同反应时间的紫外一可见吸收光谱，比较了配体、Pb配合物及PbS纳米粒子荧光光谱，发现它们十分相似。由于PbS纳米微粒与修饰在微粒表面的配体的协同效应，使其最大发射波长蓝移了约40 nm，且半峰宽宽化了约20 nm。
(4)将3-二茂铁基-2-丁烯酸钠盐与银盐反应，利用所得配合物自身的氧化还原反应制备银纳米晶，同时将二茂铁配体修饰在银纳米晶的表面，通过紫外一可见吸收光谱和循环伏安法对其光、电性能进行了初步的研究。讨论了溶液的极性对于银纳米粒子尺寸和形貌的影响：随着溶液的极性变大，纳米粒子由球形逐渐向棒形转变，且尺寸随之增大。此外，利用三腔扩散的方法简便地合成了三角形和六边形银纳米晶。XRD表明银样品以(111)晶面为基本平面，具有较好的结晶性。
It is a versatile way that using coordination compounds both as precursor and template in the preparation and modification of nanomaterials. The novel structure of coordination compounds can give the effect on the growth of nanoparticles, and the ligands can cap surface to stabilize freshly formed nanoparticles. Thus organic-inorganic materials are obtained. However, inorganic coordination compounds usually are hardly dissolving in water andmost organic solvents, except ionic liquids (ILs). ILs are organic salts entirely composed of ions, which have low melting points. They are good solvents for a wide range of inorganic, organic, and polymer materials. Most recently, synthesis of nano- and microstructured inorganic materials in ILs has aroused more and more attention because of its effective soft template effect, reproducibility, and simple maneuverability. According to literatures, we synthesized ZnS, PbS, and Ag nanoparticles modified with ligands from coordination compounds in ILs. The main works are listed as follows:
(1) Zn(FCA)_2 (FCA = 3-Ferrocenyl-2-crotonic acid) coordination polymer has been synthesized and characterized. 1-D polymeric chain structure of Zn(FCA)_2 is excellent template for the synthesis of organized assemblies of ZnS nanoparticles by an ionic liquid-assisted templating. In this work, we illustrate the formation mechanism of ZnS nanoparticles with spherical and peanut-like shapes. We explain the change of coordination mode for the carboxylate groups form FCA ligand which is revealed by FT-IR spectra. And we think the carboxylate groups use the bidentate coordination mode modified on the surface of nanoparticles.
(2) ZnT(p-Br)PP (T(p-Br)PP = tetra(p-bromophenyl)porphyrin) has been designed and synthesized. The crystal structure of ZnT(p-Br)PP was obtained and discussed. It exhibited nice molecule planarity. ZnT(p-Br)PP organic nanoplates was synthesized and characterized by XRD, TEM and SEM. Using ZnT(p-Br)PP as precursor, nanorod ZnS with different sizes were prepared by two methods and their optical properties were studied (their fluorescence peaks appeared at approximately 350 nm). The formation mechanism of rod-like ZnS nanoparticles was illustrated.
(3) PbS nanocube has been successfully synthesized in an ionic liquid, which has soft template effect. HRTEM showed the cubic morphology of PbS, its crystallite morphology and the crystal orientation. Carbazole derivatives (L) and Pb coordination compound have been synthesized and characterized. PbS naocrystalline under 10 nm was obtained by using Pb coordination compound as precursor. The UV-vis spectra of PbS solution at different reaction stages were examined. The photoluminescence of L, PbL_2, and PbS nanoparticles were compared and they were similar. However, due to cooperative effect between L and PbS nanoparticles, the maximum fluorescence peak of PbS nanoparticles blue-shifted about 40 nm, and the FWHM broadened about 20 nm.
(4) Ag nanoparticles were synthesized by Ag coordination compound self-reduction method. The products were characterized by UV-vis spectra and cyclic voltammetry. The polarity of solution affects the size and shape of Ag nanoparticles: with increasing of the polarity of solution, the shape of Ag nanoparticles transformed from spherical to rodlike shape and their sizes increased. We also facilely synthesized triangular and hexagonal silver nanoplates in three-cavity-diffusion device at low temperature and ambient atmosphere. XRD showed they are single crystals, with the basal plane as (111) lattice plane.
本文通过文献调研，以一定结构的配合物为原料，利用配合物的模板作用，在离子液中制备了具有一定规则形貌的ZnS，PbS和Ag纳米微粒，并在纳米粒子表面修饰了有机配体，有效的防止纳米粒子的团聚。主要研究内容如下：
(1)制备并表征了3-二茂铁基-2-丁烯酸锌(Zn(FCA)_2)配位聚合物，利用Zn(FCA)_2形成的1D链和离子液模板的共同作用制备了ZnS纳米微粒。讨论了球形和花生形纳米粒子的形成机理，从反应前后FCA基团红外光谱的变化解释了羧酸基团配位模式的改变，认为羧酸基团以双齿螯合的配位模式修饰在ZnS纳米微粒表面。
(2)设计合成了四(对溴苯基)卟啉锌(ZnT(p-Br)PP)，通过X。射线单晶衍射确定了其单晶结构。发现其具有很好的平面性，相邻分子间通过对溴苯基与卟啉环之间的边一面π-π作用形成层状结构。制备了片状的ZnT(p-Br)PP纳米微粒，通过XRD，TEM和SEM对其进行了表征。以ZnT(p-Br)PP为前驱体、离子液为溶剂，分别通过低温和高温两种方法制备了不同尺寸的棒状ZnS纳米微粒，讨论了棒状纳米粒子的形成机理。测试了其光学性质，所得ZnS样品在350nm左右出现荧光发射峰。
(3)利用离子液的模板作用，成功地制备了长方体形的PbS纳米晶，运用HRTEM确定出PbS纳米晶体的晶体结构和生长晶面。此外，合成、表征了具有良好光学性质的咔唑类羧酸及其Pb的配合物，并以Pb的配合物为前驱体在离子液中制备了粒径小于10 nm的硫化铅纳米粒子；测试了其不同反应时间的紫外一可见吸收光谱，比较了配体、Pb配合物及PbS纳米粒子荧光光谱，发现它们十分相似。由于PbS纳米微粒与修饰在微粒表面的配体的协同效应，使其最大发射波长蓝移了约40 nm，且半峰宽宽化了约20 nm。
(4)将3-二茂铁基-2-丁烯酸钠盐与银盐反应，利用所得配合物自身的氧化还原反应制备银纳米晶，同时将二茂铁配体修饰在银纳米晶的表面，通过紫外一可见吸收光谱和循环伏安法对其光、电性能进行了初步的研究。讨论了溶液的极性对于银纳米粒子尺寸和形貌的影响：随着溶液的极性变大，纳米粒子由球形逐渐向棒形转变，且尺寸随之增大。此外，利用三腔扩散的方法简便地合成了三角形和六边形银纳米晶。XRD表明银样品以(111)晶面为基本平面，具有较好的结晶性。
It is a versatile way that using coordination compounds both as precursor and template in the preparation and modification of nanomaterials. The novel structure of coordination compounds can give the effect on the growth of nanoparticles, and the ligands can cap surface to stabilize freshly formed nanoparticles. Thus organic-inorganic materials are obtained. However, inorganic coordination compounds usually are hardly dissolving in water andmost organic solvents, except ionic liquids (ILs). ILs are organic salts entirely composed of ions, which have low melting points. They are good solvents for a wide range of inorganic, organic, and polymer materials. Most recently, synthesis of nano- and microstructured inorganic materials in ILs has aroused more and more attention because of its effective soft template effect, reproducibility, and simple maneuverability. According to literatures, we synthesized ZnS, PbS, and Ag nanoparticles modified with ligands from coordination compounds in ILs. The main works are listed as follows:
(1) Zn(FCA)_2 (FCA = 3-Ferrocenyl-2-crotonic acid) coordination polymer has been synthesized and characterized. 1-D polymeric chain structure of Zn(FCA)_2 is excellent template for the synthesis of organized assemblies of ZnS nanoparticles by an ionic liquid-assisted templating. In this work, we illustrate the formation mechanism of ZnS nanoparticles with spherical and peanut-like shapes. We explain the change of coordination mode for the carboxylate groups form FCA ligand which is revealed by FT-IR spectra. And we think the carboxylate groups use the bidentate coordination mode modified on the surface of nanoparticles.
(2) ZnT(p-Br)PP (T(p-Br)PP = tetra(p-bromophenyl)porphyrin) has been designed and synthesized. The crystal structure of ZnT(p-Br)PP was obtained and discussed. It exhibited nice molecule planarity. ZnT(p-Br)PP organic nanoplates was synthesized and characterized by XRD, TEM and SEM. Using ZnT(p-Br)PP as precursor, nanorod ZnS with different sizes were prepared by two methods and their optical properties were studied (their fluorescence peaks appeared at approximately 350 nm). The formation mechanism of rod-like ZnS nanoparticles was illustrated.
(3) PbS nanocube has been successfully synthesized in an ionic liquid, which has soft template effect. HRTEM showed the cubic morphology of PbS, its crystallite morphology and the crystal orientation. Carbazole derivatives (L) and Pb coordination compound have been synthesized and characterized. PbS naocrystalline under 10 nm was obtained by using Pb coordination compound as precursor. The UV-vis spectra of PbS solution at different reaction stages were examined. The photoluminescence of L, PbL_2, and PbS nanoparticles were compared and they were similar. However, due to cooperative effect between L and PbS nanoparticles, the maximum fluorescence peak of PbS nanoparticles blue-shifted about 40 nm, and the FWHM broadened about 20 nm.
(4) Ag nanoparticles were synthesized by Ag coordination compound self-reduction method. The products were characterized by UV-vis spectra and cyclic voltammetry. The polarity of solution affects the size and shape of Ag nanoparticles: with increasing of the polarity of solution, the shape of Ag nanoparticles transformed from spherical to rodlike shape and their sizes increased. We also facilely synthesized triangular and hexagonal silver nanoplates in three-cavity-diffusion device at low temperature and ambient atmosphere. XRD showed they are single crystals, with the basal plane as (111) lattice plane.
引文
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