几种单分散硫族化物纳米晶与异质结构的制备及其性能研究
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摘要
胶体纳米晶,也被称为“人工原子”,其制备技术在过去的几十年中取得飞速的进步。这些纳米颗粒可以运用不同物质相互反应廉价且大量的合成,所得到的纳米颗粒的尺寸和形貌都非常均一规整。作为新颖的纳米结构之一,纳米异质结构是由两种或两种以上的物质组成的,其可以是半导体-半导体接触生长,也可以是半导体·金属相接触生长。这种异质结构因其具有多种组分,而各个组分具有不同的功能,因此具有多重功能,并且因异质界面的存在,这种结构有可能会产生一些新的性质。因其拥有这种独特的纳米结构特征,异质结纳米晶将会在不同领域获得重要的应用,如太阳能电池,高效催化剂,生物与医学探测器,以及新一代的光电转化装置等。因此,我们通过液相法合成了几种硫族化合物纳米异质结构。取得的研究结果如下：
1.发展了六方柱状硫化铜-硫化锌纳米异质结及复杂异质结构的可控合成方法。运用高温油相的方法,以CuI和[Zn(S2CNEt2)2]作为反应物分子前驱体,在油胺溶液中合成了六方柱状的Cu1.94S-ZnS(螺丝状)、Cu1.94S-ZnS-Cu1.94(哑铃状)、Cu1.94S-ZnS-Cu1.94S-ZnS-Cu1.94S(三明治状)纳米异质结构。研究了[Zn(S2CNEt2)2]用量、反应物浓度、反应时间对产物的影响。通过上述研究,我们提出了相关的反应机理。并且我们对于不同组分的以直接的光吸收性质进行了研究。由于ZnS与Cu1.94S的同时存在,该结构在紫外和近红外都有宽的吸收。这一研究结果为今后提供了一种合成类似硫族纳米异质结的新方法,为光电子器件(例如太阳能电池、光电传感器等)的发展提供了一种新颖的材料。运用类似的合成方法,在锰离子的协助下,我们还成功合成了哑铃状的Cu2S-CuS纳米异质结构。经研究发现,在锰离子的影响下,单斜相的Cu2S纳米晶体最终会转化为CuS纳米六方片结构。
2.首次于温和条件下合成了单分散三元化合物AgFeS2纳米晶及二聚体Ag2S-Fe7S8异质纳米结构。运用高温油相合成的方法,于150摄氏度在油胺体系中第一次合成了单分散的三元化合物AgFeS2纳米晶体,并且该纳米晶可在进一步加热条件下通过内在热转换反应形成二聚体Ag2S-Fe7S8异质结构纳米晶,这种方法可被推广用于制备其它类似结构的半导体纳米异质结。该三元化合物AgFeS2的带隙能为1.21eV,而且转化为异质结后会呈现出更加独特的磁学和光学性质,可以作为一种很好的吸光材料使得其在光电器件等领域具有潜在的应用价值。
3.一步法合成了具有不同晶相的Cu2S1-xSex固溶体纳米晶,并运用离子交换法成功将其转化为CdSxSe1-x和ZnSxSe1-x纳米六方片。运用高温油相的方法,以单质S和Se02作为反应物的硫源和硒源,用氯化亚铜作为铜源,在油胺和十八烯溶液中合成了不同晶相的Cu2S1-xSex纳米晶体。研究发现,当Cu2S1-xSex纳米晶体中x≠1时,形成的是六方晶相Cu2S2-xSex纳米六方片晶体；当x=1时,形成的是立方晶相的Cu2Se纳米三角形晶体。通过阳离子交换反应,可以分别制备纤锌矿CdSxSe1-x和ZnSxSe1-x纳米六方片和闪锌矿的CdSe和ZnSe纳米三角形结构。这一研究结果为以后制备类似的半导体纳米晶提供了一种新的合成思路。
4.发明了以多元硫族化合物纳米晶为前驱物制备金属纳米晶及金属硫化物纳米异质结构的新途径。首次发现了银离子和铋离子可从它们的硫族化合物纳米晶中被还原出来的现象；运用高温油相的方法,在三苯基膦的作用下,将银离子和铋离子从它们的硫族化合物中还原出来,形成单质银和铋的纳米晶体；利用这一反应原理,我们成功制备了Ag、Bi、Ag-NiS、Ag-ZnS、Ag-InS、Ag-FeS、Ag-Bi和Bi-Cu2S等多种纳米晶体和纳米异质结构。
Colloidal nanocrystals referred to as'artificial atoms'have been intensively developed during the past decades for being grown from many different materials and cheaply produced in fairly large amounts with uniform size and shape. As one particular interesting emerging class of colloidal nanostructures, heterostructured nanocrystals containing two or more chemically distinct components, i.e., semiconductor-semiconductor or semiconductor-metal, in one single nanostructure with multifunctional or new properties induced by the heterointerfaces will undoubtedly lead to revolutionary new applications of nanomaterials in various fields, such as photovoltaic devices, high-performance catalysis, biological and biomedical sensing, and a new generation of optoelectronic devices. Herein, we report solution-process for controlled synthesis of several chalcogenide nanomaterials and heterostructures. The detail can be summarized as follows:
1. We present a new colloidal route for the synthesis of hexagonal prism Cui94S-ZnS, Cu1.94S-ZnS-Cu1.94S and Cu1.94S-ZnS-Cu1.94S-ZnS-Cu1.94S heteronanostructures with screw-, dumbbell-, and sandwich-like shapes by using CuI and Zn(S2CNEt2)2as precursors in oleylamine. This colloid method may provide a new way for controlled growth of a family of metal chalcogenide heteronanostructures with interesting optical property or multifunctionalities for applications in optoelectronic devices, such as solar cells, and optical sensing. Using the similar method, we synthesized dumbbell like Cu2S-CuS heteronanostructures with Mn2+assistant. Under the influence of Mn2+, we find that the Cu2S nanocrystals can completely transform into CuS nanoplates finally.
2. Unique colloidal AgFeS2ternary nanocrystals can be synthesized at150℃for the first time in oleylamine solution. Interestingly, such ternary AgFeS2nanocrystals can further transform to Ag2S-Fe7Sg heterodimers by internal thermal reaction, which can be extended to synthesize other family of semiconductor heteronanostructures. These ternary AgFeS2nanocrystals with a band gap of1.21eV and their transformed Ag2S-Fe7S8heterodimers with different magnetic and optical property, which may have potential applications in photovoltaic devices as a promising light-absorbing material.
3. We report a facile bottom-up approach to prepare Cu2S1-xSex hexagonal nanoplates by a colloidal solution reaction in1-octadecene using CuCl, S and SeO2as precursors. Because of the high chemical stability of SeO2and its facile dissolution in1-octadecene at low temperature, this new synthetic approach does not require the use of a glove box. Furthermore, Cu2S1-xSex nanoplates can be sequentially converted to CdS1-xSex, and ZnS1-xSex nanocrystals by use of exchange reactions. It has been found that Cu2S1-xSex (x≠1) nanocrystals favor to form hexagonal structure, while Cu2Se nanocrystals favor to form cubic structure under the same experiment conditions. This approach provides a new route to access a family of other alloyed semiconducting nanocrystals.
4. We develop a new route for the synthesis of metals and metal-sulfides heterostructures with multiple sulfides as the precursors. Using the solution process, we find that triphenylphosphine can extract the Ag+and Bi3+from the nanostructural chalcogenides and reduce them to the zero-valent state for the first time. Using this reaction principle, we successively synthesized Ag, Bi, Ag-NiS, Ag-ZnS, Ag-InS, Ag-FeS, Ag-Bi, Bi-Cu2S nanostrucyures.
1.发展了六方柱状硫化铜-硫化锌纳米异质结及复杂异质结构的可控合成方法。运用高温油相的方法,以CuI和[Zn(S2CNEt2)2]作为反应物分子前驱体,在油胺溶液中合成了六方柱状的Cu1.94S-ZnS(螺丝状)、Cu1.94S-ZnS-Cu1.94(哑铃状)、Cu1.94S-ZnS-Cu1.94S-ZnS-Cu1.94S(三明治状)纳米异质结构。研究了[Zn(S2CNEt2)2]用量、反应物浓度、反应时间对产物的影响。通过上述研究,我们提出了相关的反应机理。并且我们对于不同组分的以直接的光吸收性质进行了研究。由于ZnS与Cu1.94S的同时存在,该结构在紫外和近红外都有宽的吸收。这一研究结果为今后提供了一种合成类似硫族纳米异质结的新方法,为光电子器件(例如太阳能电池、光电传感器等)的发展提供了一种新颖的材料。运用类似的合成方法,在锰离子的协助下,我们还成功合成了哑铃状的Cu2S-CuS纳米异质结构。经研究发现,在锰离子的影响下,单斜相的Cu2S纳米晶体最终会转化为CuS纳米六方片结构。
2.首次于温和条件下合成了单分散三元化合物AgFeS2纳米晶及二聚体Ag2S-Fe7S8异质纳米结构。运用高温油相合成的方法,于150摄氏度在油胺体系中第一次合成了单分散的三元化合物AgFeS2纳米晶体,并且该纳米晶可在进一步加热条件下通过内在热转换反应形成二聚体Ag2S-Fe7S8异质结构纳米晶,这种方法可被推广用于制备其它类似结构的半导体纳米异质结。该三元化合物AgFeS2的带隙能为1.21eV,而且转化为异质结后会呈现出更加独特的磁学和光学性质,可以作为一种很好的吸光材料使得其在光电器件等领域具有潜在的应用价值。
3.一步法合成了具有不同晶相的Cu2S1-xSex固溶体纳米晶,并运用离子交换法成功将其转化为CdSxSe1-x和ZnSxSe1-x纳米六方片。运用高温油相的方法,以单质S和Se02作为反应物的硫源和硒源,用氯化亚铜作为铜源,在油胺和十八烯溶液中合成了不同晶相的Cu2S1-xSex纳米晶体。研究发现,当Cu2S1-xSex纳米晶体中x≠1时,形成的是六方晶相Cu2S2-xSex纳米六方片晶体；当x=1时,形成的是立方晶相的Cu2Se纳米三角形晶体。通过阳离子交换反应,可以分别制备纤锌矿CdSxSe1-x和ZnSxSe1-x纳米六方片和闪锌矿的CdSe和ZnSe纳米三角形结构。这一研究结果为以后制备类似的半导体纳米晶提供了一种新的合成思路。
4.发明了以多元硫族化合物纳米晶为前驱物制备金属纳米晶及金属硫化物纳米异质结构的新途径。首次发现了银离子和铋离子可从它们的硫族化合物纳米晶中被还原出来的现象；运用高温油相的方法,在三苯基膦的作用下,将银离子和铋离子从它们的硫族化合物中还原出来,形成单质银和铋的纳米晶体；利用这一反应原理,我们成功制备了Ag、Bi、Ag-NiS、Ag-ZnS、Ag-InS、Ag-FeS、Ag-Bi和Bi-Cu2S等多种纳米晶体和纳米异质结构。
Colloidal nanocrystals referred to as'artificial atoms'have been intensively developed during the past decades for being grown from many different materials and cheaply produced in fairly large amounts with uniform size and shape. As one particular interesting emerging class of colloidal nanostructures, heterostructured nanocrystals containing two or more chemically distinct components, i.e., semiconductor-semiconductor or semiconductor-metal, in one single nanostructure with multifunctional or new properties induced by the heterointerfaces will undoubtedly lead to revolutionary new applications of nanomaterials in various fields, such as photovoltaic devices, high-performance catalysis, biological and biomedical sensing, and a new generation of optoelectronic devices. Herein, we report solution-process for controlled synthesis of several chalcogenide nanomaterials and heterostructures. The detail can be summarized as follows:
1. We present a new colloidal route for the synthesis of hexagonal prism Cui94S-ZnS, Cu1.94S-ZnS-Cu1.94S and Cu1.94S-ZnS-Cu1.94S-ZnS-Cu1.94S heteronanostructures with screw-, dumbbell-, and sandwich-like shapes by using CuI and Zn(S2CNEt2)2as precursors in oleylamine. This colloid method may provide a new way for controlled growth of a family of metal chalcogenide heteronanostructures with interesting optical property or multifunctionalities for applications in optoelectronic devices, such as solar cells, and optical sensing. Using the similar method, we synthesized dumbbell like Cu2S-CuS heteronanostructures with Mn2+assistant. Under the influence of Mn2+, we find that the Cu2S nanocrystals can completely transform into CuS nanoplates finally.
2. Unique colloidal AgFeS2ternary nanocrystals can be synthesized at150℃for the first time in oleylamine solution. Interestingly, such ternary AgFeS2nanocrystals can further transform to Ag2S-Fe7Sg heterodimers by internal thermal reaction, which can be extended to synthesize other family of semiconductor heteronanostructures. These ternary AgFeS2nanocrystals with a band gap of1.21eV and their transformed Ag2S-Fe7S8heterodimers with different magnetic and optical property, which may have potential applications in photovoltaic devices as a promising light-absorbing material.
3. We report a facile bottom-up approach to prepare Cu2S1-xSex hexagonal nanoplates by a colloidal solution reaction in1-octadecene using CuCl, S and SeO2as precursors. Because of the high chemical stability of SeO2and its facile dissolution in1-octadecene at low temperature, this new synthetic approach does not require the use of a glove box. Furthermore, Cu2S1-xSex nanoplates can be sequentially converted to CdS1-xSex, and ZnS1-xSex nanocrystals by use of exchange reactions. It has been found that Cu2S1-xSex (x≠1) nanocrystals favor to form hexagonal structure, while Cu2Se nanocrystals favor to form cubic structure under the same experiment conditions. This approach provides a new route to access a family of other alloyed semiconducting nanocrystals.
4. We develop a new route for the synthesis of metals and metal-sulfides heterostructures with multiple sulfides as the precursors. Using the solution process, we find that triphenylphosphine can extract the Ag+and Bi3+from the nanostructural chalcogenides and reduce them to the zero-valent state for the first time. Using this reaction principle, we successively synthesized Ag, Bi, Ag-NiS, Ag-ZnS, Ag-InS, Ag-FeS, Ag-Bi, Bi-Cu2S nanostrucyures.
引文
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