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Hydrothermal Synthesis of Euhedral Co3O4 Nanocrystals via Nutrient-Assisted Topotactic Transformation of the Layered Co(OH)2 Precursor under Anoxic Conditions: Insights into Intricate Routes Leading to Spinel Phase Development and Shape Perfection
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2020-11-11 , DOI: 10.1021/acs.cgd.0c01031 Joanna Gryboś 1 , Camillo Hudy 1 , Angelika Gryczynska 1 , Witold Piskorz 1 , Zbigniew Sojka 1
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2020-11-11 , DOI: 10.1021/acs.cgd.0c01031 Joanna Gryboś 1 , Camillo Hudy 1 , Angelika Gryczynska 1 , Witold Piskorz 1 , Zbigniew Sojka 1
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Euhedral cobalt spinel cubes, octahedra, and cuboctahedra with narrow size dispersions have been synthesized in a one-pot hydrothermal reaction, using cobalt(II) nitrate and sodium hydroxide at variable concentrations as the only reagents, while their ratio was kept constant at cCo2+/cOH– = 2.7. Three main reaction stages, including parent reactive template (PRT) formation, nutrient-mediated topotactic nucleation (NTN), and morphogenesis of nanocrystals (MNC), were distinguished. In the NTN step, the primary spinel grains development occurs with the [100] and [111] directions of the Co3O4 facets inheriting the [1–11] direction of the elongated PRT plates (formation of cubes) or the [001] direction of the hexagonal PRT plates (formation of octahedra). In an anoxic environment, the excess nitrate anions play a critical role as the Co2+ to Co3+ oxidants and oxygen donors required to attain the Co3O4 stoichiometry. The nucleated Co3O4 primary nanocrystals are spontaneously assembled into sub-micrometer spinel mesocrystals via imperfectly oriented attachments and then consolidated into euhedral bulk nanocrystals by a hydrothermal treatment (nanocubes) or via dissolution and reentrant recrystallization processes (octahedra and cuboctahedra).
中文翻译：
在缺氧条件下通过层状Co（OH）2前体的营养辅助全能转化水热合成Euhedral Co 3 O 4纳米晶体：导致尖晶石相发展和形状完善的复杂途径的见解
一锅水热反应中，使用硝酸钴（II）和氢氧化钠作为可变浓度的试剂，通过一锅法水热反应合成了具有窄尺寸分散体的正方钴尖晶石立方晶，八面体和立方八面体，而它们的比例在c Co下保持恒定2+ / c OH – = 2.7。区分了三个主要的反应阶段，包括母体反应模板（PRT）的形成，营养物介导的全能成核（NTN）和纳米晶体的形态发生（MNC）。在NTN步骤中，初始尖晶石晶粒的生长沿Co 3 O 4的[100]和[111]方向发生刻面继承了延长的PRT板的[1-11]方向（立方体的形成）或六角形PRT板的[001]方向（八面体的形成）。在缺氧环境中，过量的硝酸根阴离子起着实现Co 3 O 4化学计量所需的Co 2+到Co 3+氧化剂和氧供体的关键作用。有核的Co 3 O 4初生纳米晶体通过不完全定向的附着物自发组装为亚微米尖晶石中间晶体，然后通过水热处理（纳米晶）或通过溶解和折返重结晶过程（八面体和立方八面体）固结为正方体体纳米晶体。
更新日期：2020-12-02
中文翻译：
在缺氧条件下通过层状Co（OH）2前体的营养辅助全能转化水热合成Euhedral Co 3 O 4纳米晶体：导致尖晶石相发展和形状完善的复杂途径的见解
一锅水热反应中，使用硝酸钴（II）和氢氧化钠作为可变浓度的试剂，通过一锅法水热反应合成了具有窄尺寸分散体的正方钴尖晶石立方晶，八面体和立方八面体，而它们的比例在c Co下保持恒定2+ / c OH – = 2.7。区分了三个主要的反应阶段，包括母体反应模板（PRT）的形成，营养物介导的全能成核（NTN）和纳米晶体的形态发生（MNC）。在NTN步骤中，初始尖晶石晶粒的生长沿Co 3 O 4的[100]和[111]方向发生刻面继承了延长的PRT板的[1-11]方向（立方体的形成）或六角形PRT板的[001]方向（八面体的形成）。在缺氧环境中，过量的硝酸根阴离子起着实现Co 3 O 4化学计量所需的Co 2+到Co 3+氧化剂和氧供体的关键作用。有核的Co 3 O 4初生纳米晶体通过不完全定向的附着物自发组装为亚微米尖晶石中间晶体，然后通过水热处理（纳米晶）或通过溶解和折返重结晶过程（八面体和立方八面体）固结为正方体体纳米晶体。
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