不同形貌的铌基和钨基纳米材料的合成与性能研究
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摘要
本论文系统地研究了溶剂热方法的合成条件、气—固反应的反应条件对制备纳米材料和改性纳米材料的影响,并用SEM、TEM、XRD、XPS、IR、Raman等技术对合成和改性的纳米材料进行了结构表征。具体做了以下几个方面的工作:
(1)以为NbCl_5原料,用溶剂热方法制备了不同长径比的Nb_2O_5纳米棒、三维Nb_2O_5纳米网和多边形Nb_2O_5纳米棒片,并研究了反应温度、反应时间、反应物浓度以及溶液pH值对合成反应的影响,实验表明235℃为最佳反应温度。用SEM、TEM、XRD对其结构进行了表征。得到长度约为300nm、500nm、800nm和1μm,直径约为50-80nm的Nb_2O_5纳米棒和具有三维结构特征的Nb_2O_5纳米树—一头逐渐变细的树干大约长1—2μm,直径约80—100nm,树枝相对较小,长约100—500nm,直径约40—80nm以及约100nm厚,直径为300-500nm的Nb_2O_5多边形纳米片。纳米棒和纳米片均由Nb_2O_5单晶组成。
(2)用一维Nb_2O_5纳米棒和三维Nb_2O_5纳米网作为模板与H_2S气体反应得到核壳结构的一维和三维Nb_2O_5/NbS_2纳米电缆,用Nb_2O_5多边形纳米片作为模板与H_2S气体反应得到NbS_2多边形纳米片。研究了反应温度、反应时间对合成一维、三维Nb_2O_5/NbS_2纳米电缆和NbS_2多边形纳米片的影响,实验表明适宜的反应温度时780℃。并用SEM、TEM、XRD对其结构进行了表征。Nb_2O_5纳米棒硫化后,得到由六方NbS_2包裹的正交Nb_2O_5一维和三维Nb_2O_5/NbS_2纳米电缆,硫化产物遗传了反应物的形貌。若反应3min,壳由2-5层NbS_2组成,约1.2-3nm厚;若反应6min,壳由4-10层NbS_2组成,约2.4-6nm厚。Nb_2O_5多边形纳米片硫化后,得到由六方NbS_2和正交Nb_2O_5混合相组成的多边形纳米片,NbS_2-Nb_2O_5多边形纳米片的厚度约为100nm,直径在300-500nm之间。
(3)用Nb_2O_5纳米棒作为模板与NH_3气体反应得到一维纳米棒;用多边形Nb_2O_5纳米片作为模板与NH_3气体反应得到多边形纳米片。讨论了反应温度、反应时间对合成一维氮化物纳米棒和多边形氮化物纳米片的影响。并用SEM、TEM、XRD对其结构进行了表征。氮化产物分别为一维Nb_(3.49)N_(4.56)O_(0.44)纳米棒和多边形Nb_(3.49)N_(4.56)O_(0.44)纳米片,均由Nb_(3.49)N_(4.56)O_(0.44)单晶组成,它们也遗传了反应物的几何形貌和尺寸大小。
(4)以WEl_6和FeCl_3为原料,用溶剂热方法制备了FeWO_4纳米花,用SEM、TEM、XRD、XPS、Raman和IR对其结构进行了表征,并研究了它们的磁性能。当改变WCl_6/FeCl_3的摩尔比值时,实现从长的、细的WO_3纳米线到短的、粗的纳米线束,到短的纳米线束和纳米片的混合物,到含有短的纳米线束的‘沙漠玫瑰'类结构,再到完全变成3-D纳米花的转变,最后完全变成纳米片。测定了3-D FeWO_4纳米花的光致发光性能。3-D FeWO_4纳米花的磁性测定结果表明,3-D FeWO_4纳米花在60K处发生反铁磁转变,但是块状FeWO_4的Neel温度为66K或者75K,比FeWO_4纳米花要高一些,可能是由于FeWO_4纳米花的小尺寸所致。
The effects of different synthysis conditions by solvothermal method on generation of nanomaterials,different reacting conditions by gas-solid reaction on modify of nanomaterials have been investigated in this work.The nanomaterials were charactered by SEM,TEM,XRD,IR,XPS and Raman techelonegies.These works as fellow:
(1) Novel orthorhombic Nb_2O_5 nanorods and polygonal Nb_2O_5 platelets have been generated by a simple solvothermal technique.The geometry evolution of the resultant Nb_2O_5 from amorphous nanoparticles to crystallized particles,from polygonal platelets to well-elongated nanorods has been studied in detail.The processing parameters,including the reaction temperatures,reaction time,concentration of the precursors,and pH values of the solution,that affect the shape and size of the nanorods have been investigated.The nanomaterials were charactered by SEM,TEM and XRD technologies.
(2) One-dimensional(1-D) NbS_2/Nb_2O_5 nanocables have been generated by a two-step process,a simple solvothermal technique for a Nb_2O_5 nanorod core and subsequent reaction with H_2S to form the NbS_2 shells at 800℃.Under optimal conversion conditions,the final geometry features of the sulfide-sheathed oxide nanocables are predetermined by the size and morphology of the Nb_2O_5 nanorods which grow along the equivalent crystallographic directions of[110]in the orthorhombic Nb_2O_5.Three-dimensional(3-D) Nb_2O_5/NbS_2 cabled networks have been synthesized via gas-solid reactions between the three-dimensional(3-D) Nb_2O_5 single crystalline nanostructures and H_2S gas.The nanostructures produced by 3 min sulphidization usually consist of 2-5 layers of lattice fringe.Those reacted for 6 min comprise 4-10 NbS_2 layers.
(3) The reactions of the Nb_2O_5 nanoplatelets with NH_3 or the reactions of the Nb_2O_5 nanorods with NH_3 lead to another two types of interesting structures:The Nb_(3.49)N_(4.56)O_(0.44) nanoplatelets and the Nb_(3.49)N_(4.56)O_(0.44) nanorods.The Nb_2O_5 nanoplatelets can be employed asprecursors for the creation of the Nb_(3.49)N_(4.56)O_(0.44) nanoplatelets and the Nb_(3.49)N_(4.56)O_(0.44) nanorods.By modifying the processing parameters,we have subsequently achieved nanoplatelets and nanorods with tuneable geometry identical to their parent oxide nanoplatelets,which is important for understanding nanostructure processing.
(4) we describe the first successful creation of 1-D Fe-doped tungsten oxide and ferberite nanowires by employing a simple solvothermal technique,and then uncover the interesting evolution secrets toward a class of complex and amazingly elegant 3-D flower-like structures made of 6-folded blades of ferberite.It is found that different Fe ions addition has a profound impact on the geometry and morphology of the products.The resulting nanostructures obtained under diverse Fe ions additions in respective chloride solvents demonstrate clearly the geometry evolution routes of these structures,from long and fine(bundled and ultra thin) WO_3 nanowires to short and heavily bundled nanowires, and to irregular mixture of short nanowires and nanoplatelets,then to 'desert rose' type structures accompanied with many nanoparticles,and eventually to completely converted 3-D nanoflowers,along with the increase of the Fe concentration.
(1)以为NbCl_5原料,用溶剂热方法制备了不同长径比的Nb_2O_5纳米棒、三维Nb_2O_5纳米网和多边形Nb_2O_5纳米棒片,并研究了反应温度、反应时间、反应物浓度以及溶液pH值对合成反应的影响,实验表明235℃为最佳反应温度。用SEM、TEM、XRD对其结构进行了表征。得到长度约为300nm、500nm、800nm和1μm,直径约为50-80nm的Nb_2O_5纳米棒和具有三维结构特征的Nb_2O_5纳米树—一头逐渐变细的树干大约长1—2μm,直径约80—100nm,树枝相对较小,长约100—500nm,直径约40—80nm以及约100nm厚,直径为300-500nm的Nb_2O_5多边形纳米片。纳米棒和纳米片均由Nb_2O_5单晶组成。
(2)用一维Nb_2O_5纳米棒和三维Nb_2O_5纳米网作为模板与H_2S气体反应得到核壳结构的一维和三维Nb_2O_5/NbS_2纳米电缆,用Nb_2O_5多边形纳米片作为模板与H_2S气体反应得到NbS_2多边形纳米片。研究了反应温度、反应时间对合成一维、三维Nb_2O_5/NbS_2纳米电缆和NbS_2多边形纳米片的影响,实验表明适宜的反应温度时780℃。并用SEM、TEM、XRD对其结构进行了表征。Nb_2O_5纳米棒硫化后,得到由六方NbS_2包裹的正交Nb_2O_5一维和三维Nb_2O_5/NbS_2纳米电缆,硫化产物遗传了反应物的形貌。若反应3min,壳由2-5层NbS_2组成,约1.2-3nm厚;若反应6min,壳由4-10层NbS_2组成,约2.4-6nm厚。Nb_2O_5多边形纳米片硫化后,得到由六方NbS_2和正交Nb_2O_5混合相组成的多边形纳米片,NbS_2-Nb_2O_5多边形纳米片的厚度约为100nm,直径在300-500nm之间。
(3)用Nb_2O_5纳米棒作为模板与NH_3气体反应得到一维纳米棒;用多边形Nb_2O_5纳米片作为模板与NH_3气体反应得到多边形纳米片。讨论了反应温度、反应时间对合成一维氮化物纳米棒和多边形氮化物纳米片的影响。并用SEM、TEM、XRD对其结构进行了表征。氮化产物分别为一维Nb_(3.49)N_(4.56)O_(0.44)纳米棒和多边形Nb_(3.49)N_(4.56)O_(0.44)纳米片,均由Nb_(3.49)N_(4.56)O_(0.44)单晶组成,它们也遗传了反应物的几何形貌和尺寸大小。
(4)以WEl_6和FeCl_3为原料,用溶剂热方法制备了FeWO_4纳米花,用SEM、TEM、XRD、XPS、Raman和IR对其结构进行了表征,并研究了它们的磁性能。当改变WCl_6/FeCl_3的摩尔比值时,实现从长的、细的WO_3纳米线到短的、粗的纳米线束,到短的纳米线束和纳米片的混合物,到含有短的纳米线束的‘沙漠玫瑰'类结构,再到完全变成3-D纳米花的转变,最后完全变成纳米片。测定了3-D FeWO_4纳米花的光致发光性能。3-D FeWO_4纳米花的磁性测定结果表明,3-D FeWO_4纳米花在60K处发生反铁磁转变,但是块状FeWO_4的Neel温度为66K或者75K,比FeWO_4纳米花要高一些,可能是由于FeWO_4纳米花的小尺寸所致。
The effects of different synthysis conditions by solvothermal method on generation of nanomaterials,different reacting conditions by gas-solid reaction on modify of nanomaterials have been investigated in this work.The nanomaterials were charactered by SEM,TEM,XRD,IR,XPS and Raman techelonegies.These works as fellow:
(1) Novel orthorhombic Nb_2O_5 nanorods and polygonal Nb_2O_5 platelets have been generated by a simple solvothermal technique.The geometry evolution of the resultant Nb_2O_5 from amorphous nanoparticles to crystallized particles,from polygonal platelets to well-elongated nanorods has been studied in detail.The processing parameters,including the reaction temperatures,reaction time,concentration of the precursors,and pH values of the solution,that affect the shape and size of the nanorods have been investigated.The nanomaterials were charactered by SEM,TEM and XRD technologies.
(2) One-dimensional(1-D) NbS_2/Nb_2O_5 nanocables have been generated by a two-step process,a simple solvothermal technique for a Nb_2O_5 nanorod core and subsequent reaction with H_2S to form the NbS_2 shells at 800℃.Under optimal conversion conditions,the final geometry features of the sulfide-sheathed oxide nanocables are predetermined by the size and morphology of the Nb_2O_5 nanorods which grow along the equivalent crystallographic directions of[110]in the orthorhombic Nb_2O_5.Three-dimensional(3-D) Nb_2O_5/NbS_2 cabled networks have been synthesized via gas-solid reactions between the three-dimensional(3-D) Nb_2O_5 single crystalline nanostructures and H_2S gas.The nanostructures produced by 3 min sulphidization usually consist of 2-5 layers of lattice fringe.Those reacted for 6 min comprise 4-10 NbS_2 layers.
(3) The reactions of the Nb_2O_5 nanoplatelets with NH_3 or the reactions of the Nb_2O_5 nanorods with NH_3 lead to another two types of interesting structures:The Nb_(3.49)N_(4.56)O_(0.44) nanoplatelets and the Nb_(3.49)N_(4.56)O_(0.44) nanorods.The Nb_2O_5 nanoplatelets can be employed asprecursors for the creation of the Nb_(3.49)N_(4.56)O_(0.44) nanoplatelets and the Nb_(3.49)N_(4.56)O_(0.44) nanorods.By modifying the processing parameters,we have subsequently achieved nanoplatelets and nanorods with tuneable geometry identical to their parent oxide nanoplatelets,which is important for understanding nanostructure processing.
(4) we describe the first successful creation of 1-D Fe-doped tungsten oxide and ferberite nanowires by employing a simple solvothermal technique,and then uncover the interesting evolution secrets toward a class of complex and amazingly elegant 3-D flower-like structures made of 6-folded blades of ferberite.It is found that different Fe ions addition has a profound impact on the geometry and morphology of the products.The resulting nanostructures obtained under diverse Fe ions additions in respective chloride solvents demonstrate clearly the geometry evolution routes of these structures,from long and fine(bundled and ultra thin) WO_3 nanowires to short and heavily bundled nanowires, and to irregular mixture of short nanowires and nanoplatelets,then to 'desert rose' type structures accompanied with many nanoparticles,and eventually to completely converted 3-D nanoflowers,along with the increase of the Fe concentration.
引文
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