纳米结构Ⅳ-Ⅵ族化合物的制备、表征及性能测试
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摘要
本论文的研究工作是以基于溶液反应的自下而上的方法来制备得到具有独特形貌结构以及优异性能的Ⅳ-Ⅵ族化合物。本文利用一步水热法制备得到超薄SnO2二维纳米薄片材料,通过多种测试手段对其进行表征,发现了其取向连接的生长机理,同时将这种具备超大比表面积的产物用于锂离子电池负极材料的测试,获得了非常优异的锂离子容量性能；同时发现这种超薄SnO2二维纳米薄片材料具有奇特的室温铁磁性的性质,并通过各种测试方法揭示这种室温铁磁性很可能来源于材料表面的Sn空位；利用一步水热法制备得到超薄SnS2二维纳米薄片材料,同时将这种产物用于光催化性能测试,获得了非常优异的降解有机染料的能力；利用改进的微乳液法首先制备得到单分散的GeO2纳米方块,通过后续的在表面附着Au颗粒以及伴随着同步的GeO2的溶解,得到非常均匀尺寸和形貌的Au纳米空心立方壳层,这在生物医学上具有非常重大的意义。本论文得到的主要结果如下：
(1)成功制备得到大量并且高纯的超薄SnO2二维纳米薄片材料,其中通过高分辨透射电镜和X射线衍射图谱精修以及原子力显微镜等测试手段可以测得我们的SnO2纳米薄片的最薄厚度约为2.1 nm。通过透射电镜和高分辨透射电镜对于不同反应时间的样品的观察可以发现我们制备得到的SnO2超薄纳米薄片材料是由初始生成的SnO2纳米颗粒通过“取向连接”的生长方式自组装而成。系统的对比实验还表明,只有在适当的反应时间、溶剂、添加剂、前驱体浓度以及冷却速率时才能生成非常完美的超薄SnO2纳米薄片。然而,即使在非常完美的超薄SnO2纳米薄片样品中,仍然不可避免地存在一定程度的非化学计量比。实际的实验参数与最佳参数值相差很大时更容易造成这种非化学计量比,从而导致生成Sn3O4或者SnO。这一发现能很好地帮助我们对锡氧化物进行更深入的研究。最后,我们还研究了这种超薄SnO2纳米薄片在作为锂离子电池负极材料时的性能,并与SnO2空心球以及纳米颗粒进行了比较。实验结果表明超薄SnO2纳米薄片的性能要远高于另外两种对比样品。这可能要归结于SnO2纳米薄片的超薄厚度以及独特的多孔状结构：纳米化的网络状结构提供了极短的离子扩散距离也即促成更快的相变反应；而内部多孔结构则可以很好的缓冲在充放电过程中由材料体积的巨大变化带来的应力应变。
(2)在制备得到的超薄SnO2纳米薄片中发现奇特的室温铁磁性的现象。其中,饱和磁感应强度为15.1memu/g,矫顽力为20 Oe。同时,通过第一性原理的计算发现,当材料表面存在Sn空位时,最外层O原子层中O原子的s和p轨道电子存在自旋极化现象,造成了这种室温铁磁性的产生。随后,我们系统地研究了这种超薄SnO2纳米薄片样品在不同气氛和温度下退火处理后的磁学性能。实验结果表明,在所有的样品中仍然存在着室温铁磁性的现象,并且所有的磁性样品中饱和磁感应强度都不与样品中的O空位数量成线性关系；相反地,假设材料表面的Sn空位是磁性的来源则可以更好地解释所有现象。这恰好与我们之前的第一性原理计算结果相符。同时,我们还发现,这种超薄SnO2纳米薄片的居里温度约为300℃,远高于室温,这对于新型自旋电子器件来说具有非常大的潜力。
(3)成功地制备得到了SnS2二维纳米薄片材料。产物纯度高,产量大,薄片厚度约为5 nm左右。其中我们详细地讨论了改变反应溶液中的溶剂极性对产物最终形貌的影响。此外,通过对比不同SnS2样品在光催化降解罗丹明B染料时的表现,详细探讨了不同形貌、不同结晶性的样品对最终光催化活性的影响。实验结果发现,六角片状的SnS2纳米薄片的光催化活性最好,甚至超过商用的TiO2(P25),这在未来的污水处理方面可能具有很大的意义。
(4)通过对GeO2表面功能化以及后续的沉淀-沉积反应来合成表面覆盖Au颗粒的GeO2复合物。其中,我们详细探讨了氯金酸的浓度对Au种的尺寸分布和分散程度的影响；并且发现,当氯金酸的浓度充足时有利于同质均匀并完美分散的Au颗粒的产生。随后,通过额外添加一定量的氯金酸使得另一部分Au颗粒被还原生长在之前形成的Au/GeO2复合物表面,同时伴随着GeO2核的同步溶解,致使形成Au立方空心壳层。整个方法非常简单方便,非常适于制备这种特殊结构的Au空心壳层。同时,这种产物的吸收光谱的共振峰在900 nm以上,使得它们在生物医学应用中具有非常大的前景。
In this thesis, our work mainly focused on the solution-based "bottom-up" method to synthesize special morphological and structured IV-VI compounds with excellent properties. The ultrathin SnO2 nanosheets were synthesized by one-pot hydrothermal method, after having been investigated by various measurements, the "Oriented Attachment" mechanism was used to illustrate the morphology evolution. By applying this material in lithium ion battery, higher lithium storage was obtained compared to the other counterparts. Besides, novel room-temperature ferromagnetism was found in the products of SnO2 nanosheets, which was proposed to be the result of surface Sn vacancies. The SnS2 nanosheets were fabricated using similar protocols, and these products features splendid photocatalytic capability towards organic pigments. Finally, we synthesized Au hollow cubic shells with uniform size and morphology using an improved microemulsion method and a subsequent deposition-precipitation process. The main results are summarized as follows.
(1) Successfully synthesized large-scale and highly pure ultrathin SnO2 nanosheets (NSs), with a minimum thickness in the regime of ca.2.1 nm as determined by HRTEM; and in good agreement with XRD refinements and AFM height profiles. Through TEM and HRTEM observations on time-dependent samples, we found that the as-prepared SnO2 NSs were assembled by "oriented attachment" of pre-formed SnO2 nanoparticles (NPs). Systematic trials showed that well-defined ultrathin SnO2 NSs could only be obtained under appropriate reaction time, solvent, additive, precursor concentration and cooling rate. A certain degree of nonstoichiometry appears inevitable in the well-defined SnO2 NSs sample. However, deviations from the optimal synthetic parameters give rise to severe nonstoichiometry in the products, resulting in the formation of Sn3O4 or SnO. This finding may open new accesses to the fundamental investigations of tin oxides as well as their inter-transition processes. Finally, we investigated the lithium-ion storage of the SnO2 NSs as compared to SnO2 hollow spheres and NPs. The results showed superior performance of SnO2 NSs sample over its two counterparts. This greatly enhanced Li-ion storage capability of SnO2 NSs is probably resulting from the ultrathin thicknesses and the unique porous structures:the nanometer-sized networks provide negligible diffusion times of ions thus faster phase transitions; while the "breathable" interior porous structure can effectively buffer the drastic volume changes during lithiation and delithiation reactions.
(2) Room-temperature ferromagnetism of ultrathin SnO2 nanosheets has been found experimentally with saturation magnetization and coercive force of about 15.1 memu/g and 20 Oe, respectively. First-principles calculations reveal that oxygen atoms at O-terminated surface in SnO2 sheet are spin polarized, resulting in magnetic moment of 1.6μB for pure SnO2 nanosheet while Sn atoms just beneath the O-terminated surface contribute only-0.082/μB Besides, we have systematically studied the magnetic behavior of post-annealed SnO2 NSs samples by treating at different temperatures from 200℃to 400℃and under O2 or Ar atmosphere. Room-temperature ferromagnetisms have been observed in all studied samples. It is found that the saturation magnetization of all the annealed samples do not feature mono-dependence on oxygen vacancies, whereas the Sn vacancy-related origin seems more plausible to account for variations in magnetization of samples studied. This finding is quite correspondent to first-principle calculation results from our previous work. Furthermore, the Curie temperature of SnO2 nanosheets was estimated to be around 350℃rendering it a very good option for next-generation of spintronics.
(3) Successfully synthesized SnS2 nanosheets with high purity and large production, the thicknesses of which are about 5 nm. Afterwards, we systematically studied the influences on the morphologies of final products brought by the polarity of the solvent. Furthermore, by comparing the performances of different SnS2 samples on the degradation of methylene blue, the effect of different morphologies and crystallinities were discussed in detail. The results enclosed that the hexagonal SnS2 nanosheets possessed better photocatalytic property compared to hierarchical SnS2 microspheres or even TiO2 (P25), which is meaningful in the water treatment.
(4) Successfully synthesized gold-coated GeO2 nanocubes by applying surface functionalization and deposition-precipitation methods. The effect of gold salt concentration on the size distribution and dispersion of gold nanoparticles are examined. It was found that homogeneous and well-dispersed gold nanoparticles on GeO2 nanocubes could be obtained only if gold salt is abundant to favor simultaneous, homogeneous nucleation of gold. Eventually, additional gold was reduced onto these attached "seed" particles accompanied by synchronous dissolution of GeO2 cores, resulting in gold hollow cubic shells. This is an easy, convenient and in-situ method for preparation of gold hollow cubic shells. The absorption spectra of obtained samples have been explained according to the structures of samples. Gold hollow cubic shells feature a plasmon resonance peak at above 900 nm, which makes it very attractive in biochemical applications.
(1)成功制备得到大量并且高纯的超薄SnO2二维纳米薄片材料,其中通过高分辨透射电镜和X射线衍射图谱精修以及原子力显微镜等测试手段可以测得我们的SnO2纳米薄片的最薄厚度约为2.1 nm。通过透射电镜和高分辨透射电镜对于不同反应时间的样品的观察可以发现我们制备得到的SnO2超薄纳米薄片材料是由初始生成的SnO2纳米颗粒通过“取向连接”的生长方式自组装而成。系统的对比实验还表明,只有在适当的反应时间、溶剂、添加剂、前驱体浓度以及冷却速率时才能生成非常完美的超薄SnO2纳米薄片。然而,即使在非常完美的超薄SnO2纳米薄片样品中,仍然不可避免地存在一定程度的非化学计量比。实际的实验参数与最佳参数值相差很大时更容易造成这种非化学计量比,从而导致生成Sn3O4或者SnO。这一发现能很好地帮助我们对锡氧化物进行更深入的研究。最后,我们还研究了这种超薄SnO2纳米薄片在作为锂离子电池负极材料时的性能,并与SnO2空心球以及纳米颗粒进行了比较。实验结果表明超薄SnO2纳米薄片的性能要远高于另外两种对比样品。这可能要归结于SnO2纳米薄片的超薄厚度以及独特的多孔状结构：纳米化的网络状结构提供了极短的离子扩散距离也即促成更快的相变反应；而内部多孔结构则可以很好的缓冲在充放电过程中由材料体积的巨大变化带来的应力应变。
(2)在制备得到的超薄SnO2纳米薄片中发现奇特的室温铁磁性的现象。其中,饱和磁感应强度为15.1memu/g,矫顽力为20 Oe。同时,通过第一性原理的计算发现,当材料表面存在Sn空位时,最外层O原子层中O原子的s和p轨道电子存在自旋极化现象,造成了这种室温铁磁性的产生。随后,我们系统地研究了这种超薄SnO2纳米薄片样品在不同气氛和温度下退火处理后的磁学性能。实验结果表明,在所有的样品中仍然存在着室温铁磁性的现象,并且所有的磁性样品中饱和磁感应强度都不与样品中的O空位数量成线性关系；相反地,假设材料表面的Sn空位是磁性的来源则可以更好地解释所有现象。这恰好与我们之前的第一性原理计算结果相符。同时,我们还发现,这种超薄SnO2纳米薄片的居里温度约为300℃,远高于室温,这对于新型自旋电子器件来说具有非常大的潜力。
(3)成功地制备得到了SnS2二维纳米薄片材料。产物纯度高,产量大,薄片厚度约为5 nm左右。其中我们详细地讨论了改变反应溶液中的溶剂极性对产物最终形貌的影响。此外,通过对比不同SnS2样品在光催化降解罗丹明B染料时的表现,详细探讨了不同形貌、不同结晶性的样品对最终光催化活性的影响。实验结果发现,六角片状的SnS2纳米薄片的光催化活性最好,甚至超过商用的TiO2(P25),这在未来的污水处理方面可能具有很大的意义。
(4)通过对GeO2表面功能化以及后续的沉淀-沉积反应来合成表面覆盖Au颗粒的GeO2复合物。其中,我们详细探讨了氯金酸的浓度对Au种的尺寸分布和分散程度的影响；并且发现,当氯金酸的浓度充足时有利于同质均匀并完美分散的Au颗粒的产生。随后,通过额外添加一定量的氯金酸使得另一部分Au颗粒被还原生长在之前形成的Au/GeO2复合物表面,同时伴随着GeO2核的同步溶解,致使形成Au立方空心壳层。整个方法非常简单方便,非常适于制备这种特殊结构的Au空心壳层。同时,这种产物的吸收光谱的共振峰在900 nm以上,使得它们在生物医学应用中具有非常大的前景。
In this thesis, our work mainly focused on the solution-based "bottom-up" method to synthesize special morphological and structured IV-VI compounds with excellent properties. The ultrathin SnO2 nanosheets were synthesized by one-pot hydrothermal method, after having been investigated by various measurements, the "Oriented Attachment" mechanism was used to illustrate the morphology evolution. By applying this material in lithium ion battery, higher lithium storage was obtained compared to the other counterparts. Besides, novel room-temperature ferromagnetism was found in the products of SnO2 nanosheets, which was proposed to be the result of surface Sn vacancies. The SnS2 nanosheets were fabricated using similar protocols, and these products features splendid photocatalytic capability towards organic pigments. Finally, we synthesized Au hollow cubic shells with uniform size and morphology using an improved microemulsion method and a subsequent deposition-precipitation process. The main results are summarized as follows.
(1) Successfully synthesized large-scale and highly pure ultrathin SnO2 nanosheets (NSs), with a minimum thickness in the regime of ca.2.1 nm as determined by HRTEM; and in good agreement with XRD refinements and AFM height profiles. Through TEM and HRTEM observations on time-dependent samples, we found that the as-prepared SnO2 NSs were assembled by "oriented attachment" of pre-formed SnO2 nanoparticles (NPs). Systematic trials showed that well-defined ultrathin SnO2 NSs could only be obtained under appropriate reaction time, solvent, additive, precursor concentration and cooling rate. A certain degree of nonstoichiometry appears inevitable in the well-defined SnO2 NSs sample. However, deviations from the optimal synthetic parameters give rise to severe nonstoichiometry in the products, resulting in the formation of Sn3O4 or SnO. This finding may open new accesses to the fundamental investigations of tin oxides as well as their inter-transition processes. Finally, we investigated the lithium-ion storage of the SnO2 NSs as compared to SnO2 hollow spheres and NPs. The results showed superior performance of SnO2 NSs sample over its two counterparts. This greatly enhanced Li-ion storage capability of SnO2 NSs is probably resulting from the ultrathin thicknesses and the unique porous structures:the nanometer-sized networks provide negligible diffusion times of ions thus faster phase transitions; while the "breathable" interior porous structure can effectively buffer the drastic volume changes during lithiation and delithiation reactions.
(2) Room-temperature ferromagnetism of ultrathin SnO2 nanosheets has been found experimentally with saturation magnetization and coercive force of about 15.1 memu/g and 20 Oe, respectively. First-principles calculations reveal that oxygen atoms at O-terminated surface in SnO2 sheet are spin polarized, resulting in magnetic moment of 1.6μB for pure SnO2 nanosheet while Sn atoms just beneath the O-terminated surface contribute only-0.082/μB Besides, we have systematically studied the magnetic behavior of post-annealed SnO2 NSs samples by treating at different temperatures from 200℃to 400℃and under O2 or Ar atmosphere. Room-temperature ferromagnetisms have been observed in all studied samples. It is found that the saturation magnetization of all the annealed samples do not feature mono-dependence on oxygen vacancies, whereas the Sn vacancy-related origin seems more plausible to account for variations in magnetization of samples studied. This finding is quite correspondent to first-principle calculation results from our previous work. Furthermore, the Curie temperature of SnO2 nanosheets was estimated to be around 350℃rendering it a very good option for next-generation of spintronics.
(3) Successfully synthesized SnS2 nanosheets with high purity and large production, the thicknesses of which are about 5 nm. Afterwards, we systematically studied the influences on the morphologies of final products brought by the polarity of the solvent. Furthermore, by comparing the performances of different SnS2 samples on the degradation of methylene blue, the effect of different morphologies and crystallinities were discussed in detail. The results enclosed that the hexagonal SnS2 nanosheets possessed better photocatalytic property compared to hierarchical SnS2 microspheres or even TiO2 (P25), which is meaningful in the water treatment.
(4) Successfully synthesized gold-coated GeO2 nanocubes by applying surface functionalization and deposition-precipitation methods. The effect of gold salt concentration on the size distribution and dispersion of gold nanoparticles are examined. It was found that homogeneous and well-dispersed gold nanoparticles on GeO2 nanocubes could be obtained only if gold salt is abundant to favor simultaneous, homogeneous nucleation of gold. Eventually, additional gold was reduced onto these attached "seed" particles accompanied by synchronous dissolution of GeO2 cores, resulting in gold hollow cubic shells. This is an easy, convenient and in-situ method for preparation of gold hollow cubic shells. The absorption spectra of obtained samples have been explained according to the structures of samples. Gold hollow cubic shells feature a plasmon resonance peak at above 900 nm, which makes it very attractive in biochemical applications.
引文
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