纳米粒子的制备及其与有序分子薄膜的组装
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摘要
纳米尺度组件的构筑与未来的纳米电子学和生物分子识别器件密切相关。将纳米粒子由材料转化为器件的过程中，必须将纳米粒子以某种方式固定或与其它基体复合起来，组装成预定二维结构的纳米有序薄膜。探索纳米有序薄膜的组装方法，研究纳米薄膜的特性与结构之间的关系，为纳米电子器件、微型光电材料等提供新的思路是当今纳米科技研究的前沿。
本论文的研究目标是制备有序的纳米粒子复合薄膜，研究重点着眼于薄膜的有序性或图案化，并在此基础上与纳米粒子进行组装，并对其结构特性进行了表征。采用共沉淀法制备Fe_3O_4纳米粒子，将所得的Fe_3O_4纳米粒子分散在水中形成Fe_3O_4溶胶，研究Fe_3O_4溶胶的稳定性。以花生酸为成膜物质，Fe_3O_4溶胶为亚相，通过LB膜技术进行组装制备有序的纳米粒子复合薄膜。将Gemini阳离子表面活性剂分子与十二烷基苯磺酸钠(SDBS)改性的Fe_3O_4溶胶进行组装，制备有序的纳米粒子复合薄膜。采用布儒斯特角显微镜(BAM)原位监测了亚相Fe_3O_4溶胶气液界面上花生酸分子和Gemini分子成膜过程中单分子膜区域形貌的动态变化，分析其成膜过程。以巯基丙酸作稳定剂，采用水相法制备CdSe纳米晶，通过静电自组装方法制备PDDA／CdSe多层自组装膜，探索自组装膜的光学特性。
本论文得到的主要结论如下：
采用共沉淀法制备了粒径约为10nm、分布均匀的Fe_3O_4纳米粒子。将所得粒子分散到高纯水中获得Fe_3O_4溶胶，其等电点约为pH=6.9，浓度为0.96×10~(-5)mol·L~(-1)。测定了花生酸在纯水亚相上和Fe_3O_4溶胶(pH=4)亚相气／液界面上的π-A曲线。当以Fe_3O_4溶胶作为亚相时，相对于纯水亚相而言，由于表面带正电荷的Fe_3O_4纳米粒子受到花生酸分子中阴离子基团-COO~-的静电作用而进入花生酸单分子层内，花生酸单分子所占的面积由0.22nm~2提高到0.28nm~2；花生酸单分子层崩溃压从62mN·m~(-1)上升到67mN·m~(-1)。
布儒斯特角显微镜观测花生酸单分子层在Fe_3O_4溶胶亚相上的成膜情况，结果表明当表面压较低时，花生酸两亲分子聚集形成岛状区域；当表面压增加至30mN·m~(-1)时，花生酸分子在Fe_3O_4溶胶亚相上形成完整的单分子膜；继续增大表面压，薄膜出现裂纹，单分子膜重叠，形成多层膜。选择表面压为30mN·m~(-1)时，利用花生酸分子与表面带正电的Fe_3O_4纳米粒子之间的相互静电作用，在花生酸单分子层内组装了分布较为均匀的Fe_3O_4纳米粒子。
SDBS改性后Fe_3O_4粒子之间的团聚现象明显减轻，平均粒径约为10nm。所得Fe_3O_4溶胶的浓度为1.30×10~(-5)mol·L~(-1)。分别以高纯水和改性后的Fe_3O_4溶胶为亚相测定了Gemini单分子层的π-A曲线，Fe_3O_4粒子进入Gemini单分子层使得其平均单分子面积由1.00nm~2增大到1.28nm~2，崩溃压由34mN·m~(-1)升高到40mN·m~(-1)，薄膜的稳定性增强。
pH=4时SDBS分散的Fe_3O_4粒子表面带负电荷，利用它与Gemini分子中阳离子基团的静电相互作用在气／液界面与Gemini分子进行了组装。当Gemini单分子层表面压较小时，所组装得到的复合单分子膜中Fe_3O_4纳米粒子分布不均，且形成大小不一的聚集体。当表面压逐渐增大时，气液界面上Gemini单分子层内的电荷密度增加，吸引更多的Fe_3O_4纳米粒子进入其中。当Gemini单分子层表面压为12mN·m~(-1)～15mN·m~(-1)时，由于Gemini分子特殊的分子结构在Fe_3O_4溶胶气液界面上形成聚集并规则地排列在一起形成六边形的区域，受到Gemini分子中带电基团的静电吸引，Fe_3O_4纳米粒子进入六边形区域内与Gemini分子组装形成复合单分子膜。当表面压为15mN·m~(-1)时组装得到的复合单分子膜上的Fe_3O_4纳米粒子排布相当均匀。
以巯基丙酸作稳定剂，通过水相法制备了高荧光强度的CdSe纳米晶。所得粒子呈球状、粒子大小分布均匀、粒径约为5nm。通过静电自组装方法在石英基片上成功制备了PDDA／CdSe多层自组装膜，薄膜的紫外-可见光谱、荧光光谱分析结果表明所得的多层自组装薄膜成膜质量良好，且具有很高的荧光光致发光性。
The building of nanoscaled subassembly is interrelated with the coming nanoelectronics and biomolecular recognition devices nearly. In the process of nanomaterial converting to devices, the nanoparticles must be immobiled or deposited onto some substrate slice to fabricate composite nano-films with prearranged two-dimensional (2D) structures. Having a knowledge of how to prepare nano-film using molecular assembly technique such as Langmuir-Blodgett (LB) film technique and self-assembly (SA) technique, and what is the relation between the properties and the structures in the obtained composite thin film contribute to provide novel approach to prepare nanoelectronics devices and micro-optical and electronic materials etc and is still the focus of the modern research of nanotechnology.
The aim in this paper is to prepare ordered assembled composite thin film and the emphasis of the research is to prepare well-arrayed two-dimensional thin film or nanopattern, then assembly them with nanoscaled particles to build ordered composite nano-film. Fe_3O_4 nanoparticles were first synthesized from cotrolled chemical coprecipitation of aqueous Fe~(3+) and Fe~(2+) ions and then they were dispersed into the high purity water to obtain Fe_3O_4 hydrosol. The resulted Fe_3O_4 hydrosols were assembled with arachidic acid (AA) to obtain ordered Fe_3O_4-AA composite monolayer using LB film technique. Also in this way we assembled Gemini surfactant monolayer with magnetite nanoparticles which were modified by sodium dodecyl benzene sulfonate (SDBS) at the air/liquid interface. Dynamic domains morphology of monolayer of arachidic acid and Gemini at the air/liquid interface of magnetite hydrosol have been studied by Brewster angle microscopy (BAM) .The CdSe nanocrystal was synthesized in aqueous phase, and then
multilayers of cationic polyelectrolyte Poly (diallyldimethylammonium chloride) (PDDA) and CdSe nanocrystal were deposited onto glass substrate using electrostatic self-assembly method (ESAM). The properties of the self-assembly PDDA/CdSe multilayer thin film was investigated by the means of UV-VIS spectra and photoluminescence spectra. The results in this paper are shown as follow:
The prepared nanoscaled Fe_3O_4 particles is of about 10 nm, and the concentration of the obtained magnetite hydrosol is 0.96×10~(-5) mol·L~(-1) and its isoelectric point is pH=6.9. The surface pressure-area per molecule isotherm (π-A isotherm) of AA chloroformic solution at the air/liquid interface of high purity water and Fe_3O_4 hydrosol (pH=4) were measured respectively. The results indicates that the mean molecular area of AA is about 0.22nm~2, and the collapse pressure of the monolayer is 62 mN·m~(-1) with the subphase of puried water. While the two value are 0.28 nm~2 and 67 mN·m~(-1) respectively at the air/liquid of magnetite hydrosol due to the significant interaction between the positively charged Fe_3O_4 nanoparticles and the negatively charged AA molecules on the surface, which results in the magnetite nanoparticles moving into AA monolayer through the electrostatic interaction.
Dynamic domains morphology of arachidic acid monolayer at the air/liquid interface of magnetite hydrosol have been researched by BAM. The results shows that AA molecules distribute randomly just as insular domain originally during the formation process of the monolayer, then they are shaped into a whole condensed monolayer at a surface pressure of 30mN·m~(-1). The monolayer cracks with the increased pressure, and then they overlap and form multilayer. Finally we assembled Fe_3O_4 in the whole condensed and ordered AA monolayer at a pressure of 30 mN·m~(-1) through the interaction of AA and magnetite molecules.
Magnetite nanoparticles of about 10 nm were synthesized by cotrolled chemical co- precipitations method in the presence of SDBS. As-surface modified magnetite nanoparticles were dispersed into the pure water and the resulted SDBS-Fe_3O_4 hydrosols whose surface are taking positive charge at pH=4 has a concentration of 1.30×10~(-5) mol·L~(-1). Theπ-A isotherm of Gemini surfactant chloroformic solution at the air/liquid interface of puried water and Fe_3O_4 hydrosol were measured respectively. The results indicates that the collapse pressure of the monolayer and the aera per molecule of Gemini are increased to 1.28 nm~2 and 40 mN·m~(-1) in contrast to the results of pure water as subphase which are 1.00 nm~2 and 34 mN·m~(-1) respectively because there is a significant interaction between the positively charged Fe_3O_4 nanoparticles and the negatively charged cationic ammonium groups of Gemini molecules on the surface, which result in the magnetite nanoparticles moving into Gemini monolayer through the electrostatic interaction. However, the shape of theπ-A isotherm of Gemini dislikes the results of AA in a degree because of the special structure of Gemini molecules.
Using magnetite hydrosols as subphase, we assembled Gemini surfactant monolayer with magnetite nanoparticles at the air/liquid interface. At the beginning, a low concentration of the Fe_3O_4 nanoparticles, randomly distributed on the Gemini monolayer. Aggregates of nanoparticles are apparent on the film, leading to larger irregular shapes. As the surface pressure increases, the surface concentration of the Gemini repeat unit increases, which leads to a higher negative surface charge and a stronger electrostatic interactions between the Fe_3O_4 nanoparticles and the monolayer, causing more of the positively charged nanoparticles to adhere to the monolayer at higher surface pressures. The attachment of the nanoparticles at the surface of the monolayer should make the collapse of the monolayer more difficult. Extraordinarily between the surface pressure of 12mN·m~(-1) and 15mN·m~(-1), Gemini molecules are likely to have a specific hexagonal configuration which attracted the magnetite nanoparticles into the aera forming a composite monolayer. While the Fe_3O_4 nanoparticles arrange well in the Gemini monolayer when the surface pressure is more than 15mN·m~(-1).
The nanocrystal CdSe quanta dots were synthesized in aqueous phase with the materials of CdCl_2·2H_2O, NaBH4 and selenium powder using 3-mercaptopropionic acid(MPA)as stabilization reagent. As-prepared CdSe particles has a narrow size distribution and an average sizes of about 5nm. With PDDA and the resulted nanocrystal CdSe hydrosol, we deposited multilayers of PDDA and CdSe nanocrystal onto pre-treated glass substrate using layer-by-layer electrostatic self-assembly method. The self-assembly PDDA/CdSe multilayer thin film was characterized by the means of UV-VIS spectra and photoluminescence spectra. The results indicates that the PDDA/CdSe multilayer has a good quality and shows very strong luminescence intensity.
本论文的研究目标是制备有序的纳米粒子复合薄膜，研究重点着眼于薄膜的有序性或图案化，并在此基础上与纳米粒子进行组装，并对其结构特性进行了表征。采用共沉淀法制备Fe_3O_4纳米粒子，将所得的Fe_3O_4纳米粒子分散在水中形成Fe_3O_4溶胶，研究Fe_3O_4溶胶的稳定性。以花生酸为成膜物质，Fe_3O_4溶胶为亚相，通过LB膜技术进行组装制备有序的纳米粒子复合薄膜。将Gemini阳离子表面活性剂分子与十二烷基苯磺酸钠(SDBS)改性的Fe_3O_4溶胶进行组装，制备有序的纳米粒子复合薄膜。采用布儒斯特角显微镜(BAM)原位监测了亚相Fe_3O_4溶胶气液界面上花生酸分子和Gemini分子成膜过程中单分子膜区域形貌的动态变化，分析其成膜过程。以巯基丙酸作稳定剂，采用水相法制备CdSe纳米晶，通过静电自组装方法制备PDDA／CdSe多层自组装膜，探索自组装膜的光学特性。
本论文得到的主要结论如下：
采用共沉淀法制备了粒径约为10nm、分布均匀的Fe_3O_4纳米粒子。将所得粒子分散到高纯水中获得Fe_3O_4溶胶，其等电点约为pH=6.9，浓度为0.96×10~(-5)mol·L~(-1)。测定了花生酸在纯水亚相上和Fe_3O_4溶胶(pH=4)亚相气／液界面上的π-A曲线。当以Fe_3O_4溶胶作为亚相时，相对于纯水亚相而言，由于表面带正电荷的Fe_3O_4纳米粒子受到花生酸分子中阴离子基团-COO~-的静电作用而进入花生酸单分子层内，花生酸单分子所占的面积由0.22nm~2提高到0.28nm~2；花生酸单分子层崩溃压从62mN·m~(-1)上升到67mN·m~(-1)。
布儒斯特角显微镜观测花生酸单分子层在Fe_3O_4溶胶亚相上的成膜情况，结果表明当表面压较低时，花生酸两亲分子聚集形成岛状区域；当表面压增加至30mN·m~(-1)时，花生酸分子在Fe_3O_4溶胶亚相上形成完整的单分子膜；继续增大表面压，薄膜出现裂纹，单分子膜重叠，形成多层膜。选择表面压为30mN·m~(-1)时，利用花生酸分子与表面带正电的Fe_3O_4纳米粒子之间的相互静电作用，在花生酸单分子层内组装了分布较为均匀的Fe_3O_4纳米粒子。
SDBS改性后Fe_3O_4粒子之间的团聚现象明显减轻，平均粒径约为10nm。所得Fe_3O_4溶胶的浓度为1.30×10~(-5)mol·L~(-1)。分别以高纯水和改性后的Fe_3O_4溶胶为亚相测定了Gemini单分子层的π-A曲线，Fe_3O_4粒子进入Gemini单分子层使得其平均单分子面积由1.00nm~2增大到1.28nm~2，崩溃压由34mN·m~(-1)升高到40mN·m~(-1)，薄膜的稳定性增强。
pH=4时SDBS分散的Fe_3O_4粒子表面带负电荷，利用它与Gemini分子中阳离子基团的静电相互作用在气／液界面与Gemini分子进行了组装。当Gemini单分子层表面压较小时，所组装得到的复合单分子膜中Fe_3O_4纳米粒子分布不均，且形成大小不一的聚集体。当表面压逐渐增大时，气液界面上Gemini单分子层内的电荷密度增加，吸引更多的Fe_3O_4纳米粒子进入其中。当Gemini单分子层表面压为12mN·m~(-1)～15mN·m~(-1)时，由于Gemini分子特殊的分子结构在Fe_3O_4溶胶气液界面上形成聚集并规则地排列在一起形成六边形的区域，受到Gemini分子中带电基团的静电吸引，Fe_3O_4纳米粒子进入六边形区域内与Gemini分子组装形成复合单分子膜。当表面压为15mN·m~(-1)时组装得到的复合单分子膜上的Fe_3O_4纳米粒子排布相当均匀。
以巯基丙酸作稳定剂，通过水相法制备了高荧光强度的CdSe纳米晶。所得粒子呈球状、粒子大小分布均匀、粒径约为5nm。通过静电自组装方法在石英基片上成功制备了PDDA／CdSe多层自组装膜，薄膜的紫外-可见光谱、荧光光谱分析结果表明所得的多层自组装薄膜成膜质量良好，且具有很高的荧光光致发光性。
The building of nanoscaled subassembly is interrelated with the coming nanoelectronics and biomolecular recognition devices nearly. In the process of nanomaterial converting to devices, the nanoparticles must be immobiled or deposited onto some substrate slice to fabricate composite nano-films with prearranged two-dimensional (2D) structures. Having a knowledge of how to prepare nano-film using molecular assembly technique such as Langmuir-Blodgett (LB) film technique and self-assembly (SA) technique, and what is the relation between the properties and the structures in the obtained composite thin film contribute to provide novel approach to prepare nanoelectronics devices and micro-optical and electronic materials etc and is still the focus of the modern research of nanotechnology.
The aim in this paper is to prepare ordered assembled composite thin film and the emphasis of the research is to prepare well-arrayed two-dimensional thin film or nanopattern, then assembly them with nanoscaled particles to build ordered composite nano-film. Fe_3O_4 nanoparticles were first synthesized from cotrolled chemical coprecipitation of aqueous Fe~(3+) and Fe~(2+) ions and then they were dispersed into the high purity water to obtain Fe_3O_4 hydrosol. The resulted Fe_3O_4 hydrosols were assembled with arachidic acid (AA) to obtain ordered Fe_3O_4-AA composite monolayer using LB film technique. Also in this way we assembled Gemini surfactant monolayer with magnetite nanoparticles which were modified by sodium dodecyl benzene sulfonate (SDBS) at the air/liquid interface. Dynamic domains morphology of monolayer of arachidic acid and Gemini at the air/liquid interface of magnetite hydrosol have been studied by Brewster angle microscopy (BAM) .The CdSe nanocrystal was synthesized in aqueous phase, and then
multilayers of cationic polyelectrolyte Poly (diallyldimethylammonium chloride) (PDDA) and CdSe nanocrystal were deposited onto glass substrate using electrostatic self-assembly method (ESAM). The properties of the self-assembly PDDA/CdSe multilayer thin film was investigated by the means of UV-VIS spectra and photoluminescence spectra. The results in this paper are shown as follow:
The prepared nanoscaled Fe_3O_4 particles is of about 10 nm, and the concentration of the obtained magnetite hydrosol is 0.96×10~(-5) mol·L~(-1) and its isoelectric point is pH=6.9. The surface pressure-area per molecule isotherm (π-A isotherm) of AA chloroformic solution at the air/liquid interface of high purity water and Fe_3O_4 hydrosol (pH=4) were measured respectively. The results indicates that the mean molecular area of AA is about 0.22nm~2, and the collapse pressure of the monolayer is 62 mN·m~(-1) with the subphase of puried water. While the two value are 0.28 nm~2 and 67 mN·m~(-1) respectively at the air/liquid of magnetite hydrosol due to the significant interaction between the positively charged Fe_3O_4 nanoparticles and the negatively charged AA molecules on the surface, which results in the magnetite nanoparticles moving into AA monolayer through the electrostatic interaction.
Dynamic domains morphology of arachidic acid monolayer at the air/liquid interface of magnetite hydrosol have been researched by BAM. The results shows that AA molecules distribute randomly just as insular domain originally during the formation process of the monolayer, then they are shaped into a whole condensed monolayer at a surface pressure of 30mN·m~(-1). The monolayer cracks with the increased pressure, and then they overlap and form multilayer. Finally we assembled Fe_3O_4 in the whole condensed and ordered AA monolayer at a pressure of 30 mN·m~(-1) through the interaction of AA and magnetite molecules.
Magnetite nanoparticles of about 10 nm were synthesized by cotrolled chemical co- precipitations method in the presence of SDBS. As-surface modified magnetite nanoparticles were dispersed into the pure water and the resulted SDBS-Fe_3O_4 hydrosols whose surface are taking positive charge at pH=4 has a concentration of 1.30×10~(-5) mol·L~(-1). Theπ-A isotherm of Gemini surfactant chloroformic solution at the air/liquid interface of puried water and Fe_3O_4 hydrosol were measured respectively. The results indicates that the collapse pressure of the monolayer and the aera per molecule of Gemini are increased to 1.28 nm~2 and 40 mN·m~(-1) in contrast to the results of pure water as subphase which are 1.00 nm~2 and 34 mN·m~(-1) respectively because there is a significant interaction between the positively charged Fe_3O_4 nanoparticles and the negatively charged cationic ammonium groups of Gemini molecules on the surface, which result in the magnetite nanoparticles moving into Gemini monolayer through the electrostatic interaction. However, the shape of theπ-A isotherm of Gemini dislikes the results of AA in a degree because of the special structure of Gemini molecules.
Using magnetite hydrosols as subphase, we assembled Gemini surfactant monolayer with magnetite nanoparticles at the air/liquid interface. At the beginning, a low concentration of the Fe_3O_4 nanoparticles, randomly distributed on the Gemini monolayer. Aggregates of nanoparticles are apparent on the film, leading to larger irregular shapes. As the surface pressure increases, the surface concentration of the Gemini repeat unit increases, which leads to a higher negative surface charge and a stronger electrostatic interactions between the Fe_3O_4 nanoparticles and the monolayer, causing more of the positively charged nanoparticles to adhere to the monolayer at higher surface pressures. The attachment of the nanoparticles at the surface of the monolayer should make the collapse of the monolayer more difficult. Extraordinarily between the surface pressure of 12mN·m~(-1) and 15mN·m~(-1), Gemini molecules are likely to have a specific hexagonal configuration which attracted the magnetite nanoparticles into the aera forming a composite monolayer. While the Fe_3O_4 nanoparticles arrange well in the Gemini monolayer when the surface pressure is more than 15mN·m~(-1).
The nanocrystal CdSe quanta dots were synthesized in aqueous phase with the materials of CdCl_2·2H_2O, NaBH4 and selenium powder using 3-mercaptopropionic acid(MPA)as stabilization reagent. As-prepared CdSe particles has a narrow size distribution and an average sizes of about 5nm. With PDDA and the resulted nanocrystal CdSe hydrosol, we deposited multilayers of PDDA and CdSe nanocrystal onto pre-treated glass substrate using layer-by-layer electrostatic self-assembly method. The self-assembly PDDA/CdSe multilayer thin film was characterized by the means of UV-VIS spectra and photoluminescence spectra. The results indicates that the PDDA/CdSe multilayer has a good quality and shows very strong luminescence intensity.
引文
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