界面扩散受限条件下晶体生长形态学研究
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摘要
作为一个历史问题,制备形貌可控的微型和纳米结构的晶体物质的能力是走向材料应用的关键一步。在平衡条件下形成的无机晶体,其形貌是由晶体表面能的相对顺序习惯确定。然而,通过改变晶体晶面能顺序得到令人印象深刻的结构则很少被报道。在实际晶体生长过程中,扩散效应通常在复杂的异构和分层架构的形成起着重要的作用。最新进展表明,通过控制在空气/液体,液体/液体或固体/液体界面的晶体的生长过程中扩散效益可以合成复杂的晶体结构。
液/液(L/L)界面是一个独特的环境,因为不连续的物理性质,化学性质,存在两种液体。液/液界面为各种材料的空心微粒的合成形成提供了一个理想的平台。,这一战略已经被证明在聚合物,无机和金属有机骨架胶囊的制备。然而,水溶性无机盐作为无机化合物的一大家族,如氯化物,亚硫酸盐和硫酸盐,通过界面合成复杂的晶体结构则较少的的报道。本实验成功的利用亚稳态水滴界面作为平台成功的取得了一系列的研究成果。具体研究内容如下：
(1)亚稳态水滴界面生长斗状氯化钠单晶及其组装空心微球。
氯化钠(NaCl),结晶化学的最经典的主题,一直是作为立方晶体的典型代表。同时,改变氯化钠的结晶习性获得令人印象深刻的结构未实现。在此,我们报告单晶NaCl斗状单晶和他们在亚稳水液滴界面的自组装空心微球。当氯化钠水溶液被注入到丙酮和环己烷的混合物,在快速搅拌的情况下,亚稳态水滴被短时间的稳定。随着丙酮扩散进入水相,氯化钠在水/环己烷-丙酮两相之间成核。同时,非极性的环己烷吸附在晶体的(001)面,阻止了晶体在此<001>方向的生长。然而,{001}面和{111)面的继续生长,并保持了原有的生长速度。有趣的是,我们成功的改变氯化钠晶体的生长习性,并以亚稳定水滴为模板生成了的斗状单晶和它们的自组装空心微球。该结果打开了一条新的途径来控制水溶性物种晶体的生长,了解在晶体的生长机理。
(2)亚稳态水滴界面生长四角锥斗状氯化钠八面体及其自组装空心微球。
人们在几世纪以前,在存在低浓度的添加剂时,发现晶体形态可以发生显着改变,其作用机理是由于添加剂可以吸附在特定晶面进而减小晶体在特定晶面的生长速率。如,在氯化钠水溶液中存在的尿素或甲酰胺,面心立方晶体氯化钠将形成八面体。因此,我们在的亚稳态水滴的界面研究的尿素对氯化钠的晶体形貌的影响。成功合成氯化钠四角锥斗状八面体形状的单晶以及自组装的空心微球。扫描电镜显示,微球大部分粒径范围为10-40微米,其是有几十个大小为2微米左右的四角锥斗状八面体氯化钠单晶组成。
(3)亚稳态水滴晶面生长立方晶系、正交晶系和六方晶系的水溶性无机盐单晶以及组装空心微球。
无机盐作为无机化合物中的重要成员,探讨各种不同晶系的无机盐晶体在新体系下生长情况具有重要的意义。我们选择了三种不同晶系的水溶性无机盐,立方晶系的溴化钾和NH4C1,正交晶系的(NH4)2SO4和正交晶系的亚硫酸钠作为例子,说明了该方法在生长立方晶系、正交晶系、正交晶系的水溶性无机盐漏斗状的单晶和他们的自组装空心微球的普适性。
As a historical subject, the ability to tailor the micro-and nanoscale architecture of crystalline substances is a critical step toward application. When inorganic crystals are formed under equilibrium conditions, their crystal habit is determined by the relative order of surface energies. However, the morphological evolution with crystal modifiers usually resulted in a limited variation of the intrinsic shape of crystal; the impressive structures/architectures have rarely been reported. There has been active research in the area exploring novel synthetic chemical methods for the synthesis of heterogeneous and hierarchical architectures with controllable sizes and shapes. Alternatively, during real crystal growth process, the diffusion effect usually plays an important role in the formation of complex heterogeneous and hierarchical architectures. Recent advances have demonstrated that it is possible to control the growth processes of complex heterogeneous and hierarchical architectures with interfacial growth at air/liquid, liquid/liquid or solid/liquid interfaces. Here, we report a unified approach to the synthesis of water-soluble salts crystal with stunning structure at the metastable liquid-liquid interface between the organic solvent and aqueous droplets. The metastable liquid-liquid interface of the two compatible liquids offered a platform for the controlled formation of water-soluble salts.
(1) Hopper-Like Single Crystals of Sodium Chloride Grown at Interface of Metastable Water Droplets
Sodium chloride (NaCl), the most classical topic in crystallization chemistry, has always been dedicated as the representative of regular cubic crystals. To change the growth habit of water-soluble salts for the production of impressive structures/architectures has not yet been achieved. Herein, we report the hopper-like single crystals of NaCl and KCl and their self-assembly at interface of metastable water microdroplets. When the undersaturated NaCl aqueous solution was introduced into the mixture of acetone and cyclohexane, the metastable water microdroplets were temporally formed under vigorously stirring. With the diffusion of acetone into the water phase, NaCl nucleated at the metastable interface of water/acetone-cyclohexane. Meanwhile, nonpolar cyclohexane adsorbed at the nuclei's (001) plane faced to the organic phase, preventing the growth at this<001> direction. However, the growths of other{001} planes and the{111} planes maintained the original growth rates. Interestingly, the changed growth habit and the water droplet template resulted in the hopper-like single crystals and their uniform arrangement in the form of hollow microspheres, respectively. The reported results open a new avenue to control the crystallization of water-soluble species and shed significant insights to understand the growth mechanism of nanocrystals in the natural and artificial systems.
(2) Pyramidic-Hopper-Like Single Crystals of Sodium Chloride Grown at Interface of Metastable Water Droplets
It has been found for over a century that the nucleation, growth, and morphology of crystals can significantly altered by the presence of low concentrations of additives. Additives can reduce crystal growth rate and alter morphology by binding to crystal faces and interfering with propagation steps. Interestingly, sodium chloride crystals form octahedrons in the presence of urea or formamide. Therefore, we have examined the interaction of urea with sodium chloride at the meteastable interface of water droplets. We synthesized microparticles of NaCl octahedron single crystal with hopper polyhedral shapes. SEM shows that the formation products are mainly composed of many hollow microspheres, most of which are in the size range10-40μm. The micro structure is in fact built by uniform octahedral NaCl single crystals and the size is about2μm. The products consist of tens of octahedrons single crystals.
(3) Hopper-Like Single Crystals of Water-soluble salts Grown at Interface of Metastable Water Droplets
Herein, we chose water-soluble salts with different crystal system, the cubic system of KBr and NH4Cl, the orthorhombic system of (NH4)2SO4and the hexagonal system of Na2SO3, as examples to demonstrate the effectiveness of this method in yielding sidewalls and hopper-like crystallites and their self-assembly into hollow microspheres.
液/液(L/L)界面是一个独特的环境,因为不连续的物理性质,化学性质,存在两种液体。液/液界面为各种材料的空心微粒的合成形成提供了一个理想的平台。,这一战略已经被证明在聚合物,无机和金属有机骨架胶囊的制备。然而,水溶性无机盐作为无机化合物的一大家族,如氯化物,亚硫酸盐和硫酸盐,通过界面合成复杂的晶体结构则较少的的报道。本实验成功的利用亚稳态水滴界面作为平台成功的取得了一系列的研究成果。具体研究内容如下：
(1)亚稳态水滴界面生长斗状氯化钠单晶及其组装空心微球。
氯化钠(NaCl),结晶化学的最经典的主题,一直是作为立方晶体的典型代表。同时,改变氯化钠的结晶习性获得令人印象深刻的结构未实现。在此,我们报告单晶NaCl斗状单晶和他们在亚稳水液滴界面的自组装空心微球。当氯化钠水溶液被注入到丙酮和环己烷的混合物,在快速搅拌的情况下,亚稳态水滴被短时间的稳定。随着丙酮扩散进入水相,氯化钠在水/环己烷-丙酮两相之间成核。同时,非极性的环己烷吸附在晶体的(001)面,阻止了晶体在此<001>方向的生长。然而,{001}面和{111)面的继续生长,并保持了原有的生长速度。有趣的是,我们成功的改变氯化钠晶体的生长习性,并以亚稳定水滴为模板生成了的斗状单晶和它们的自组装空心微球。该结果打开了一条新的途径来控制水溶性物种晶体的生长,了解在晶体的生长机理。
(2)亚稳态水滴界面生长四角锥斗状氯化钠八面体及其自组装空心微球。
人们在几世纪以前,在存在低浓度的添加剂时,发现晶体形态可以发生显着改变,其作用机理是由于添加剂可以吸附在特定晶面进而减小晶体在特定晶面的生长速率。如,在氯化钠水溶液中存在的尿素或甲酰胺,面心立方晶体氯化钠将形成八面体。因此,我们在的亚稳态水滴的界面研究的尿素对氯化钠的晶体形貌的影响。成功合成氯化钠四角锥斗状八面体形状的单晶以及自组装的空心微球。扫描电镜显示,微球大部分粒径范围为10-40微米,其是有几十个大小为2微米左右的四角锥斗状八面体氯化钠单晶组成。
(3)亚稳态水滴晶面生长立方晶系、正交晶系和六方晶系的水溶性无机盐单晶以及组装空心微球。
无机盐作为无机化合物中的重要成员,探讨各种不同晶系的无机盐晶体在新体系下生长情况具有重要的意义。我们选择了三种不同晶系的水溶性无机盐,立方晶系的溴化钾和NH4C1,正交晶系的(NH4)2SO4和正交晶系的亚硫酸钠作为例子,说明了该方法在生长立方晶系、正交晶系、正交晶系的水溶性无机盐漏斗状的单晶和他们的自组装空心微球的普适性。
As a historical subject, the ability to tailor the micro-and nanoscale architecture of crystalline substances is a critical step toward application. When inorganic crystals are formed under equilibrium conditions, their crystal habit is determined by the relative order of surface energies. However, the morphological evolution with crystal modifiers usually resulted in a limited variation of the intrinsic shape of crystal; the impressive structures/architectures have rarely been reported. There has been active research in the area exploring novel synthetic chemical methods for the synthesis of heterogeneous and hierarchical architectures with controllable sizes and shapes. Alternatively, during real crystal growth process, the diffusion effect usually plays an important role in the formation of complex heterogeneous and hierarchical architectures. Recent advances have demonstrated that it is possible to control the growth processes of complex heterogeneous and hierarchical architectures with interfacial growth at air/liquid, liquid/liquid or solid/liquid interfaces. Here, we report a unified approach to the synthesis of water-soluble salts crystal with stunning structure at the metastable liquid-liquid interface between the organic solvent and aqueous droplets. The metastable liquid-liquid interface of the two compatible liquids offered a platform for the controlled formation of water-soluble salts.
(1) Hopper-Like Single Crystals of Sodium Chloride Grown at Interface of Metastable Water Droplets
Sodium chloride (NaCl), the most classical topic in crystallization chemistry, has always been dedicated as the representative of regular cubic crystals. To change the growth habit of water-soluble salts for the production of impressive structures/architectures has not yet been achieved. Herein, we report the hopper-like single crystals of NaCl and KCl and their self-assembly at interface of metastable water microdroplets. When the undersaturated NaCl aqueous solution was introduced into the mixture of acetone and cyclohexane, the metastable water microdroplets were temporally formed under vigorously stirring. With the diffusion of acetone into the water phase, NaCl nucleated at the metastable interface of water/acetone-cyclohexane. Meanwhile, nonpolar cyclohexane adsorbed at the nuclei's (001) plane faced to the organic phase, preventing the growth at this<001> direction. However, the growths of other{001} planes and the{111} planes maintained the original growth rates. Interestingly, the changed growth habit and the water droplet template resulted in the hopper-like single crystals and their uniform arrangement in the form of hollow microspheres, respectively. The reported results open a new avenue to control the crystallization of water-soluble species and shed significant insights to understand the growth mechanism of nanocrystals in the natural and artificial systems.
(2) Pyramidic-Hopper-Like Single Crystals of Sodium Chloride Grown at Interface of Metastable Water Droplets
It has been found for over a century that the nucleation, growth, and morphology of crystals can significantly altered by the presence of low concentrations of additives. Additives can reduce crystal growth rate and alter morphology by binding to crystal faces and interfering with propagation steps. Interestingly, sodium chloride crystals form octahedrons in the presence of urea or formamide. Therefore, we have examined the interaction of urea with sodium chloride at the meteastable interface of water droplets. We synthesized microparticles of NaCl octahedron single crystal with hopper polyhedral shapes. SEM shows that the formation products are mainly composed of many hollow microspheres, most of which are in the size range10-40μm. The micro structure is in fact built by uniform octahedral NaCl single crystals and the size is about2μm. The products consist of tens of octahedrons single crystals.
(3) Hopper-Like Single Crystals of Water-soluble salts Grown at Interface of Metastable Water Droplets
Herein, we chose water-soluble salts with different crystal system, the cubic system of KBr and NH4Cl, the orthorhombic system of (NH4)2SO4and the hexagonal system of Na2SO3, as examples to demonstrate the effectiveness of this method in yielding sidewalls and hopper-like crystallites and their self-assembly into hollow microspheres.
引文
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