有机添加剂辅助无机材料形貌控制合成
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摘要
生物体能够在生物大分子的精确控制下，通过生物矿化过程合成具有特殊形貌和功能的生物矿物。目前，仿生合成具有特定形貌、取向、组织、和多级结构的无机材料和无机-有机复合材料引起了人们普遍的关注。利用有机模板或者晶体生长调控剂，控制晶体的成核、生长、组装已被广泛地应用于仿生合成大量具有特定形态的无机材料。本文研究了有机添加剂辅助的一些无机材料形貌控制合成，内容包括7个部分。
第一部分和第二部分，我们研究了在苯乙烯-马来酸交替共聚物(PSMA)和十六烷基三甲基溴化铵(CTAB)的混合系统中，CaCO_3和PbS晶体的形貌控制合成。结果显示，PSMA-CTAB混合系统能够对CaCO_3和PbS的晶体形貌和纳米晶的组装进行有效地调控。在混合系统中，PSMA和CTAB的浓度对CaCO_3和PbS的结晶有非常显著的影响，在特定的PSMA和CTAB浓度下，我们合成了花生状的CaCO_3晶体和星形的PbS晶体，这些特殊形貌的形成机制与有机-无机界面作用的选择性有关，这种作用的选择性导致晶体沿着某些特定的方向优先生长。此外，在PSMA-CTAB混合系统中，我们还成功地合成了微米尺寸的CaCO_3空心球，我们认为这是高聚物-表面活性剂混合胶束模板作用的结果。
第三部分，我们在另外一个高聚物和表面活性剂的混合系统中研究了PbS的结晶行为，这个混合系统的组成是聚甲基丙烯酸(PMAA)和CTAB。我们发现，单独的有机添加剂PMAA或者CTAB对PbS的结晶均有不同程度的影响。PMAA-CTAB混合系统能诱导PbS纳米晶组装成球形和珊瑚状的聚集体，我们认为，这个组装过程可能是由于吸附在不同组装单元上的PMAA和CTAB之间的相互作用造成的。
第四部分，我们研究了PMAA存在下水热合成PbWO_4。PMAA浓度、[Pb~(2+)]／[WO_4~(2-)]摩尔比、pH值、以及陈化温度对PbWO_4晶体的形貌有明显的影响，在特定的实验条件下，PbWO_4可以形成形貌新颖的微米尺寸的针状结构，微米针的长度和光致发光强度可以通过改变水热反应温度来控制。我们提出了一个非经典结晶的机理，合理地解释了微米针的形成和相关的实验结果。
第五部分，我们通过CuSO_4和H_2C_2O_4的沉淀反应，合成了表面有孔、或者表面有花纹的草酸铜片状微米多晶。研究发现，晶体表面的孔、或者花纹，是在陈化过程中发生在片状晶体表面中心区域的溶蚀造成的。聚乙二醇(PEG)、介质酸度、陈化温度对草酸铜的溶蚀有影响，因而通过可以控制这些因素调控草酸铜多晶的形貌。
第六部分，在PMAA存在下，我们给出了一个室温合成空心结构金属钨酸盐和钼酸盐的简便方法，提出了“高聚物-金属离子原位模板”反应机理，合理地解释了空心结构的形成。另外，我们还给出了一个合成空心结构WO_3的方法，即利用预先合成的空心结构的BaWO_4或者SrWO_4作为前驱物，通过硝酸处理和高温煅烧，将BaWO_4或者SrWO_4转化为WO_3，在此过程中，前驱物原有的空心结构在产物WO_3中完好地保持下来。
最后一部分，我们在PMAA存在下，通过沉淀反应室温合成了微米和亚微米级的BaSO_4单分散颗粒。我们认为，BaSO_4单分散颗粒的形成同样遵循“高聚物-金属离子原位模板”反应机理。
Biological systems are able to generate crystalline materials with complex morphologies and specific functions via the processes of biomineralization and these processes are elaborately controlled by some biomacromolecules. Controlled synthesis of inorganic and inorganic/organic hybrid materials of specific morphology, orientation, organization, complex form, and hierarchical structure has drawn a lot of attention in materials science. The strategy of using organic templates or modifiers with complex functionalization patterns to control the nucleation, growth, and alignment of crystals has been widely adapted for the biomimetic synthesis of a variety of inorganic materials with complex forms. This dissertation focuses on the morphosynthesis of some inorganic materials assisted by organic additives, and contains seven parts.
In the first two parts, controlled synthesis of CaCO_3 and PbS was studied in a mixed systems of poly-(styrene-alt- maleic acid) (PSMA) and cetyltrimethylammonium bromide (CTAB), and the results showed that the mixed PSMA-CTAB system was a very effective crystal growth modifiers to direct the growth of CaCO_3 and PbS crystals to various morphologies. The concentrations of PSMA and CTAB in the mixed system exerted great influence on the crystal growth of CaCO_3 and PbS. Peanut-like CaCO_3 and star-like PbS crystals were synthesized, and the formation mechanism was related to the selective interaction between the organic-inorganic interfaces, which resulted in preferential growth along some specific crystallographic directions. Moreover, we successfully prepared micrometer sized CaCO_3 hollow spheres in the mixed PSMA-CTAB system, and the formation of hollow structured CaCO_3 was ascribed to the templating of polymer-surfactant mixed micelle.
In the third part, crystallization of PbS was studied in another polymer-surfactant mixed system: poly(methacrylic acid)-cetyltrimethylammonium bromide (PMAA-CTAB). We found that the presence of a single organic additive, i.e. PMAA or CTAB, could alter the crystal habit of PbS. Moreover, the PMAA-CTAB mixed system could induce self-assembly of PbS nanocrystals to spherical and coral-like aggregates by virtue of the interaction between the adsorbed PMAA and CTAB on different crystalline building blocks.
The hydrothermal synthesis of PbWO4 crystals in the presence of PMAA was studied in the forth part. The concentration of PMAA, [pb~(2+)]/[WO_4~(2-)] molar ratio (R), pH value, and ageing temperature exhibited great effect on the crystal morphology of PbWO_4. Novel needle-like PbWO_4 single crystals of micrometer size were prepared. The length and photoluminescence intensity of PbWO_4 microneedles increased with raising ageing temperature. A nonclassical crystallization mechanism was proposed to elucidate the formation of needle-like structure of PbWO4 and the related experimental results.
In the fifth part, we demonstrated the morphosynthesis of pitted or patterned copper oxalate polycrystalline tablets by a precipitation reaction between copper sulfate and oxalic acid solutions. The formation of the pit or pattern on the surfaces of the tablets could be due to the etching or partial dissolution at the central region of the tablets during ageing. Because the etching of copper oxalate depends on the coexisted poly(ethylene glycol) (PEG), acidity of the reaction mixture and ageing temperature, the morphology of copper oxalate could be facilely tailored by regulating these experimental parameters.
In the sixth part, we presented a facile route to hollow structured metal tungstate and molybdate particles via precipitation reactions at the ambient temperature in the presence of PMAA. A "polymer-M in situ template" reaction model was established to elucidate the formation of these hollow structures. Moreover, hollow structured WO_3 was achieved using the hollow structured SrWO_4 or BaWO4 particles as the precursors, which were treated by nitric acid and calcinations sequentially. In the procedure, BaWO_4 or SrWO_4 was turned to WO_3, whereas the original hollow structures of the precursors were perfectly maintained.
In the last part, micrometer and submicrometer sized monodispersed particles of polycrystalline BaSO_4 were produced by a simple precipitation reaction in the presence of PMAA at the ambient temperature. The "polymer-M in situ template" model was also available in explanation of formation process of such polycrystalline BaSO_4 particles.
第一部分和第二部分，我们研究了在苯乙烯-马来酸交替共聚物(PSMA)和十六烷基三甲基溴化铵(CTAB)的混合系统中，CaCO_3和PbS晶体的形貌控制合成。结果显示，PSMA-CTAB混合系统能够对CaCO_3和PbS的晶体形貌和纳米晶的组装进行有效地调控。在混合系统中，PSMA和CTAB的浓度对CaCO_3和PbS的结晶有非常显著的影响，在特定的PSMA和CTAB浓度下，我们合成了花生状的CaCO_3晶体和星形的PbS晶体，这些特殊形貌的形成机制与有机-无机界面作用的选择性有关，这种作用的选择性导致晶体沿着某些特定的方向优先生长。此外，在PSMA-CTAB混合系统中，我们还成功地合成了微米尺寸的CaCO_3空心球，我们认为这是高聚物-表面活性剂混合胶束模板作用的结果。
第三部分，我们在另外一个高聚物和表面活性剂的混合系统中研究了PbS的结晶行为，这个混合系统的组成是聚甲基丙烯酸(PMAA)和CTAB。我们发现，单独的有机添加剂PMAA或者CTAB对PbS的结晶均有不同程度的影响。PMAA-CTAB混合系统能诱导PbS纳米晶组装成球形和珊瑚状的聚集体，我们认为，这个组装过程可能是由于吸附在不同组装单元上的PMAA和CTAB之间的相互作用造成的。
第四部分，我们研究了PMAA存在下水热合成PbWO_4。PMAA浓度、[Pb~(2+)]／[WO_4~(2-)]摩尔比、pH值、以及陈化温度对PbWO_4晶体的形貌有明显的影响，在特定的实验条件下，PbWO_4可以形成形貌新颖的微米尺寸的针状结构，微米针的长度和光致发光强度可以通过改变水热反应温度来控制。我们提出了一个非经典结晶的机理，合理地解释了微米针的形成和相关的实验结果。
第五部分，我们通过CuSO_4和H_2C_2O_4的沉淀反应，合成了表面有孔、或者表面有花纹的草酸铜片状微米多晶。研究发现，晶体表面的孔、或者花纹，是在陈化过程中发生在片状晶体表面中心区域的溶蚀造成的。聚乙二醇(PEG)、介质酸度、陈化温度对草酸铜的溶蚀有影响，因而通过可以控制这些因素调控草酸铜多晶的形貌。
第六部分，在PMAA存在下，我们给出了一个室温合成空心结构金属钨酸盐和钼酸盐的简便方法，提出了“高聚物-金属离子原位模板”反应机理，合理地解释了空心结构的形成。另外，我们还给出了一个合成空心结构WO_3的方法，即利用预先合成的空心结构的BaWO_4或者SrWO_4作为前驱物，通过硝酸处理和高温煅烧，将BaWO_4或者SrWO_4转化为WO_3，在此过程中，前驱物原有的空心结构在产物WO_3中完好地保持下来。
最后一部分，我们在PMAA存在下，通过沉淀反应室温合成了微米和亚微米级的BaSO_4单分散颗粒。我们认为，BaSO_4单分散颗粒的形成同样遵循“高聚物-金属离子原位模板”反应机理。
Biological systems are able to generate crystalline materials with complex morphologies and specific functions via the processes of biomineralization and these processes are elaborately controlled by some biomacromolecules. Controlled synthesis of inorganic and inorganic/organic hybrid materials of specific morphology, orientation, organization, complex form, and hierarchical structure has drawn a lot of attention in materials science. The strategy of using organic templates or modifiers with complex functionalization patterns to control the nucleation, growth, and alignment of crystals has been widely adapted for the biomimetic synthesis of a variety of inorganic materials with complex forms. This dissertation focuses on the morphosynthesis of some inorganic materials assisted by organic additives, and contains seven parts.
In the first two parts, controlled synthesis of CaCO_3 and PbS was studied in a mixed systems of poly-(styrene-alt- maleic acid) (PSMA) and cetyltrimethylammonium bromide (CTAB), and the results showed that the mixed PSMA-CTAB system was a very effective crystal growth modifiers to direct the growth of CaCO_3 and PbS crystals to various morphologies. The concentrations of PSMA and CTAB in the mixed system exerted great influence on the crystal growth of CaCO_3 and PbS. Peanut-like CaCO_3 and star-like PbS crystals were synthesized, and the formation mechanism was related to the selective interaction between the organic-inorganic interfaces, which resulted in preferential growth along some specific crystallographic directions. Moreover, we successfully prepared micrometer sized CaCO_3 hollow spheres in the mixed PSMA-CTAB system, and the formation of hollow structured CaCO_3 was ascribed to the templating of polymer-surfactant mixed micelle.
In the third part, crystallization of PbS was studied in another polymer-surfactant mixed system: poly(methacrylic acid)-cetyltrimethylammonium bromide (PMAA-CTAB). We found that the presence of a single organic additive, i.e. PMAA or CTAB, could alter the crystal habit of PbS. Moreover, the PMAA-CTAB mixed system could induce self-assembly of PbS nanocrystals to spherical and coral-like aggregates by virtue of the interaction between the adsorbed PMAA and CTAB on different crystalline building blocks.
The hydrothermal synthesis of PbWO4 crystals in the presence of PMAA was studied in the forth part. The concentration of PMAA, [pb~(2+)]/[WO_4~(2-)] molar ratio (R), pH value, and ageing temperature exhibited great effect on the crystal morphology of PbWO_4. Novel needle-like PbWO_4 single crystals of micrometer size were prepared. The length and photoluminescence intensity of PbWO_4 microneedles increased with raising ageing temperature. A nonclassical crystallization mechanism was proposed to elucidate the formation of needle-like structure of PbWO4 and the related experimental results.
In the fifth part, we demonstrated the morphosynthesis of pitted or patterned copper oxalate polycrystalline tablets by a precipitation reaction between copper sulfate and oxalic acid solutions. The formation of the pit or pattern on the surfaces of the tablets could be due to the etching or partial dissolution at the central region of the tablets during ageing. Because the etching of copper oxalate depends on the coexisted poly(ethylene glycol) (PEG), acidity of the reaction mixture and ageing temperature, the morphology of copper oxalate could be facilely tailored by regulating these experimental parameters.
In the sixth part, we presented a facile route to hollow structured metal tungstate and molybdate particles via precipitation reactions at the ambient temperature in the presence of PMAA. A "polymer-M in situ template" reaction model was established to elucidate the formation of these hollow structures. Moreover, hollow structured WO_3 was achieved using the hollow structured SrWO_4 or BaWO4 particles as the precursors, which were treated by nitric acid and calcinations sequentially. In the procedure, BaWO_4 or SrWO_4 was turned to WO_3, whereas the original hollow structures of the precursors were perfectly maintained.
In the last part, micrometer and submicrometer sized monodispersed particles of polycrystalline BaSO_4 were produced by a simple precipitation reaction in the presence of PMAA at the ambient temperature. The "polymer-M in situ template" model was also available in explanation of formation process of such polycrystalline BaSO_4 particles.
引文
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