SnO_2一维纳米材料的制备、表征以及特性研究
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摘要
本文采用新工艺和新方法制备了SnO_2纳米棒、Cd~(2+)掺杂SnO_2纳米棒和Zn~(2+)掺杂SnO_2纳米棒三种SnO_2一维纳米材料。对材料的制备工艺、材料合成、材料结构的表征、晶体生长机理等进行了探讨；与SnO_2纳米颗粒粉体和SnO_2(SiO_2)壳(核)结构纳米粒子两种零维纳米SnO_2材料相对照，对比研究了SnO_2一维纳米材料的红外吸收光学特性、氧化还原特性和气体敏感特性，制备出了具有高灵敏度和高选择性的几种新型气敏元件。论文取得了多项新颖的研究结果。
1、SnO_2纳米棒的新制备方法与表征
在微乳液法制备SnO_2一维纳米材料的基础上，发展了采用表面活性剂包裹下的室温固相还原反应合成单分散的前驱体粒子再在熔盐中生长SnO_2一维纳米材料的新工艺制备出了SnO_2纳米棒，获得了采用新方法制备SnO_2纳米棒的条件与工艺。
采用新方法制备SnO_2一维纳米材料，可获得直径为5nm～100nm，长度为几百纳米～10μm的单晶SnO_2纳米棒。SnO_2纳米棒Sn和O原子浓度比随着在熔盐中的晶体生长温度的高低而发生变化，生长温度越低，O原子缺位越严重；生长温度越高，SnO_2纳米棒中O原子缺位越少。
2、Cd~(2+)掺杂或Zn~(2+)掺杂SnO_2纳米棒新型一维纳米材料的合成与表征
采用微乳液法，在熔盐介质中生长制备了掺杂Cd~(2+)或掺杂Zn~(2+)的SnO_2纳米棒新型SnO_2一维纳米材料。通过XPS和XRF测量表明，在Cd~(2+)掺杂的SnO_2纳米棒晶体中CdO的含量约为3％，Zn~(2+)掺杂的SnO_2纳米棒晶体中ZnO的含量约为1.5％。SnO_2纳米棒的晶体结构是Cd~(2+)、Zn~(2+)代替部分Sn~(4+)构成替位式固溶体的晶体结构。这种掺杂的SnO_2一维纳米材料未见报导。
3、研究了SnO_2纳米棒在熔融盐中的晶体生长过程，提出了熔融盐中SnO_2一维纳米晶体生长机制的新见解
SnO_2纳米棒在熔融盐中的生长是一个从最初的SnO_2纳米颗粒前驱物，在一定生长温度形成细小纤维，纤维生长纳米棒成型，在较高的生长温度下纳米棒逐步长大、长粗，最终生长成为纳米棒。这一生长期过程的主要特点是在熔盐介质中同一种物质(SnO_2)从零维的纳米颗粒到一维的纳米棒的固态转变。
SnO_2纳米棒在熔融盐中的固态转变生长机制是：在熔融盐提供的液态环境中，单分散前驱体SnO_(2-δ)纳米颗粒在熔融盐中作热扩散，以熔融盐中的空洞线或隙缝线形成的位错线为“软模板”，单分散SnO_(2-δ)纳米颗粒中SnO发生歧化反应形成SnO_2，按气—液—固(VLS)晶体生长机制，以降低表面能为驱动力，沿着“软模板”按一定的晶面进行“自组装”取向生长，最终在熔融盐形成的封闭体系中生长成SnO_2一维纳米材料。SnO_2纳米棒在熔融盐中的固态转变生长机理是一种新的一维纳米材料的生长机制。这种SnO_2一维纳米材料生长机制尚未见报道。
4、对SnO_2一维纳米材料的红外吸收光谱特性进行了研究，发现SnO_2纳米棒、掺杂Cd~(2+)或掺杂Zn~(2+)的SnO_2纳米棒的奇异红外光谱演变现象
在400-1000cm~(-1)低波数范围，SnO_2纳米棒材料Sn-O振动带的特征红外吸收峰呈双峰形式，分别位于680.5cm~(-1)和475.2cm~(-1)的位置。SnO_2纳米棒Sn-O红外吸收特性与纳米棒直径大小密切相关，表现出明显的尺寸效应。随着SnO_2纳米棒直径的减小，吸收峰出现明显宽化；475.2 cm~(-1)位置的吸收峰，随着SnO_2纳米棒直径减小，吸收峰出现蓝移；680.5cm~(-1)位置的吸收峰，随着SnO_2纳米棒直径减小，吸收峰却出现了红移。这种红外收吸峰蓝移和红移并存的奇异光谱现象，在一维纳米材料中也是首次观察到。
在400-1000 cm~(-1)低波数范围的Sn-O的红外吸收振动带，Cd~(2+)掺杂和Zn~(2+)掺杂SnO_2纳米棒的红外吸收与SnO_2纳米棒的红外吸收相似，也是呈双红外吸收峰。但是随着SnO_2纳米棒直径的减小，吸收峰出现明显宽化外，其Sn-O红外吸收峰只出现红移现象。这种红移由Cd~(2+)、Zn~(2+)在SnO_2纳米棒晶体中形成的替位式晶体结构引起。
5、SnO_2一维纳米材料的氧化还原特性及新的还原反应热力学机理分析通过H_2-TPR研究表明，SnO_2纳米棒具有由表面吸附的活性氧导致的较好的表面活性和氧化还原性质。纯SnO_2纳米棒在320℃左右的低温下就可以使H_2发生缓慢氧化，纯SnO_2纳米棒的H_2还原反应机理是“表面脱氧反应+歧化反应”；Cd~(2+)掺杂和Zn~(2+)掺杂的SnO_2纳米棒的H_2还原反应与纯SnO_2纳米棒的H_2还原反应类似，但由于纳米CdO和ZnO的催化作用使H_2还原反应温度大大降低，并形成H_2消耗反应峰。掺杂Cd~(2+)和Zn~(2+)的SnO_2纳米棒的H_2还原反应机理是“脱氧反应+歧化反应+纳米催化还原反应+Cd~(2+)(或Zn~(2+))的还原反应”。
6、SnO_2纳米棒一维纳米材料的气敏特性及气敏机理探讨
首次以SnO_2纳米棒集群材料为气体敏感材料，设计制作了二种新型材料气体传感器：
(?)SnO_2一维纳米集群材料传感器
(?)SnO_2一维纳米集群材料+SnO_2纳米粉体混合材料传感器
两种新型传感器对乙醇(C_2H_5OH)气体具有很好的灵敏度和稳定性，并具有较好的恢复-响应特性。其中以掺杂Zn~(2+)的SnO_2纳米棒对乙醇气体的敏感性最好，纯SnO_2纳米棒次之，而掺杂Cd~(2+)的SnO_2纳米棒对乙醇气体的敏感性再次之。这种SnO_2一维纳米集群气敏材料的气敏特性及元件设计，还未见报道。
根据纳米SnO_2气敏材料偏离化学计量比及相关缺陷，材料的表面气体吸附特性，晶粒尺寸及比表面积大小，以及界面理论和导电通道理论，讨论了SnO_2一维纳米材料的气敏机理，提出了SnO_2一维纳米材料的气敏机理模型。用该气敏机理能很好地解释相关的实验结果。
Nanoscale one-dimensional (1-D) materials of SnO_2 nanorods, SnO_2 nanorods doped Cd~(2+) and SnO_2 nanorods doped Zn~(2+) were produced by a new method and technology of preparation. It was researched that the method and the technology of preparation, the structures, the growth mechanism of SnO_2 nanorods were studied. Comparing SnO_2 nanorods materials with SnO_2 nano-powders and SnO_2 nano-particles coating on SiO_2 ball prepared, the properties in infrared absorption spectra (IR), redox, gas sensitive of SnO_2 nanorods materials were studied. High sensitivity and high selectivity new gas sensors of SnO_2 nanorods materials were investigated too. Some new results were obtained in this paper. The results are as follows:
1. Preparation and characterizations of SnO_2 nanorods
A new synthesis method of SnO_2 nanorods developed based on the preparing way of SnO_2 nanorods via annealing the precursor powders, which were prepared by microemulsion system consisting of oil phase, water phase and surfactant. SnO_2 nanorods were produced via the growth in molten salt medium of precursors, which prepared applying by solid-state reaction coated surfactants at room temperature. It was obtained that the preparing techniques of SnO_2 precursors and SnO_2 nanorods.
It is found that SnO_2 nanorods prepared via the new synthesis method were single crystal materials. The diameter and length of the SnO_2 nanorods are in the range of 5nm to 100nm and several micrometers depended on the growth temperature and time. The atomic composition of Sn and O was calculated by using peak area sensitivity factors. The results showed that the atomic ratio of Sn/O was changed from 1:1 to 1:2. The deviation of composition from stoichiometry caused by oxygen vacancies was strongly affected by the growth temperature. Lower growth temperature, higher atomic ratio of Sn and O. Contradictorily, higher growth temperature, closer to the stoichiometry of atomic ratio of Sn and O.
2. Synthesis and characterizition of SnO_2 nanorods doped Cd~(2+) or Zn~(2+)
In molten salt medium, two kinds of SnO_2 nanorods doped Cd~(2+) or Zn~(2+) were obtained via annealing the precursors of SnO_2 powders doped Cd~(2+) or Zn~(2+), which were prepared by redox reaction in microemulsion system. The structure and chemical composition of SnO_2 nanorods doped Cd(2+) or Zn(2+) were characterized by means of XPS and XFS(X-ray fluorescence spectrometry). It is found that the content of CdO in SnO_2 nanorods materials doped Cd~(2+) is up to 3%, and the content of ZnO in SnO_2 nanorods materials doped Zn~(2+) is up to 1.5 %. The crystalline structure of SnO_2nanorods doped Cd~(2+) or Zn~(2+) is a substitutional solid solution crystalline, which was formed by Sn~(4+) replaced with Cd~(2+) or Zn~(2+). The work was not reported.
3. Growth processes and mechanism of SnO_2 nanorods in molten salt medium
The growth processes and mechanism of SnO_2 nanorods in molten salt medium were investigated. The growth of SnO_2 nanorods is a process of homogeneously dispersed particles of SnO_2 precursors growing into SnO_2 whiskers via self assembly, forming thin SnO_2 nanorods, and gradually growing up in molten salt medium. The main feature of this procedure is a solid transformation forming process of SnO_2 crystalline from nano-particles of 0-D to nanorods of 1-D in molten salt medium.
In molten salt, the growth mechanism of SnO_2 nanorods is that molten salt provide the liquid environment, in which dispersed particles of SnO_(2-δ) nano-crystal can diffuse along the dislocations in tubes. SnO_2 was formed by divergent reaction of SnO contained in SnO_(2-δ), and take the tube dislocations as "template" oriented growth via self assembly derived by decreasing the surface energy of homogeneously dispersed SnO_(2-δ) particles, and controlled by VLS growth mechanism. Eventually, SnO_(2-δ) particles grow into SnO_2 nanorods in the tube dislocations of molten salt. The growth mechanism of SnO_2 nanorods in molten salt medium is a new mechanism of 1-D nano-materials.
4. Study on infrared absorption characteristics of SnO_2 nanorods
The infrared absorption characteristics of SnO_2 nanorods with different diameters were investigated by infrared absorption spectra (IR). It is found that there existdouble peaks at 475.2cm~(-1) and 680.5cm~(-1) of the vibrational modes of Sn-O band in the low frequency range 400-1000 cm~(-1). The IR modes of Sn-O band depend on the diameter of SnO_2 nanorods closely. The smaller the diameter is, the wider the IR peaks become. The active IR mode at 475.2cm~(-1) shifts to high frequency(blue shift) in accordance with decrease of diameter of SnO_2 nanorods. On the other hand, the active IR mode at 680.5cm~(-1) shifts to low frequency(red shift) in accordance with decrease of diameter of SnO_2 nanorods. This novel phenomenon about the infrared absorption spectra of SnO_2 nanorods with different diameters was investigated for the first time.
Being similar to the infrared absorption spectra of SnO_2 nanorods, the infrared absorption spectra of SnO_2 nanorods doped Cd~(2+) or Zn~(2+) have double peaks of the vibrational modes of Sn-O band in the low frequency range 400-1000 cm~(-1), too. But the two active IR modes shift to low frequency(red shift) in accordance with decreasing of nanorods diameter at the same time. It is different from the infrared absorption spectra of SnO_2 nanorods due to the substitutional solid solution crystalline structure of SnO_2 nanorods doped Cd~(2+) or Zn~(2+).
5. Redox properties and new reaction thermodynamics mechanism of SnO_2 nanorods
The redox properties of SnO_2 nanorods materials were investigated by means of H_2-TPR. The results showed that the better redox properties of SnO_2 nanorods ascribed to higher oxidizing activity induced adsorbed oxygen on the surface of SnO_2 nanorods. The slow-reaction temperature of H_2 consumption was started at 320℃. The reaction mechanism of SnO_2 nanorods is in the employ of H_2 consumption reaction of the desorbed oxygen and the divergent reaction of SnO_2.
The redox properties of SnO_2 nanorods materials doped Cd~(2+) or Zn~(2+) were similar to redox properties of SnO_2 nanorods materials. But the started slow-reaction temperature of H_2 consumption were reduced in a large degree due to the catalytic effect of CdO or ZnO. The reaction was started at 270℃and the H_2 consumption peak was at 510℃in H_2-TPR profile of SnO_2 nanorods materials doped Cd~(2+). In the meanwhile, the reaction was started at 180℃and the H_2 consumption peak was at 420℃in H_2-TPR profile of SnO_2 nanorods materials doped Zn~(2+). The reaction mechanism submits to catalytic reaction of CdO or ZnO cooperated with H_2 consumption reaction of the desorbed oxygen, the divergent reaction of SnO_2 and reduction reaction of Cd~(2+) or Zn~(2+). This work of reaction mechanism was reported for the first time.
6. Research on gas sensing properties and new gas sensitive mechanism of SnO_2 1-D nano-materials.
Two kinds of gas sensor have been desired with new gas-sensing materials based on SnO_2 nanorods and mixture materials of SnO_2 nanorods with SnO_2 nano-powders for the first time. It was discovered that sensors exhibited higher sensitivity, better selectivity, better stability, and better response and reversion to ethanol (C_2H_5OH). Sensors based on SnO_2 nanorods materials doped Zn~(2+) illustrated the best sensitivity to ethanol and sensors based on SnO_2 nanorods materials was inferior to it. Sensitivity to ethanol of the sensors based on SnO_2 nanorods materials doped Cd~(2+) followed them. The work was not still reported.
The gas sensitive mechanism of SnO_2 nanorods was put forward according to structure characteristics of SnO_2 nanorods gas sensitive materials with deviated from stoichiometry, to adsorption properties and interface principle, to grain size and surface-to-volume ratios associated with 1-D nanostructures, and to the tunnel of electrical conductivity theory. Relative experiment results of the gas sensing properties of SnO_2 nanorods materials can be explain very well with using the mechanism pattern.
1、SnO_2纳米棒的新制备方法与表征
在微乳液法制备SnO_2一维纳米材料的基础上，发展了采用表面活性剂包裹下的室温固相还原反应合成单分散的前驱体粒子再在熔盐中生长SnO_2一维纳米材料的新工艺制备出了SnO_2纳米棒，获得了采用新方法制备SnO_2纳米棒的条件与工艺。
采用新方法制备SnO_2一维纳米材料，可获得直径为5nm～100nm，长度为几百纳米～10μm的单晶SnO_2纳米棒。SnO_2纳米棒Sn和O原子浓度比随着在熔盐中的晶体生长温度的高低而发生变化，生长温度越低，O原子缺位越严重；生长温度越高，SnO_2纳米棒中O原子缺位越少。
2、Cd~(2+)掺杂或Zn~(2+)掺杂SnO_2纳米棒新型一维纳米材料的合成与表征
采用微乳液法，在熔盐介质中生长制备了掺杂Cd~(2+)或掺杂Zn~(2+)的SnO_2纳米棒新型SnO_2一维纳米材料。通过XPS和XRF测量表明，在Cd~(2+)掺杂的SnO_2纳米棒晶体中CdO的含量约为3％，Zn~(2+)掺杂的SnO_2纳米棒晶体中ZnO的含量约为1.5％。SnO_2纳米棒的晶体结构是Cd~(2+)、Zn~(2+)代替部分Sn~(4+)构成替位式固溶体的晶体结构。这种掺杂的SnO_2一维纳米材料未见报导。
3、研究了SnO_2纳米棒在熔融盐中的晶体生长过程，提出了熔融盐中SnO_2一维纳米晶体生长机制的新见解
SnO_2纳米棒在熔融盐中的生长是一个从最初的SnO_2纳米颗粒前驱物，在一定生长温度形成细小纤维，纤维生长纳米棒成型，在较高的生长温度下纳米棒逐步长大、长粗，最终生长成为纳米棒。这一生长期过程的主要特点是在熔盐介质中同一种物质(SnO_2)从零维的纳米颗粒到一维的纳米棒的固态转变。
SnO_2纳米棒在熔融盐中的固态转变生长机制是：在熔融盐提供的液态环境中，单分散前驱体SnO_(2-δ)纳米颗粒在熔融盐中作热扩散，以熔融盐中的空洞线或隙缝线形成的位错线为“软模板”，单分散SnO_(2-δ)纳米颗粒中SnO发生歧化反应形成SnO_2，按气—液—固(VLS)晶体生长机制，以降低表面能为驱动力，沿着“软模板”按一定的晶面进行“自组装”取向生长，最终在熔融盐形成的封闭体系中生长成SnO_2一维纳米材料。SnO_2纳米棒在熔融盐中的固态转变生长机理是一种新的一维纳米材料的生长机制。这种SnO_2一维纳米材料生长机制尚未见报道。
4、对SnO_2一维纳米材料的红外吸收光谱特性进行了研究，发现SnO_2纳米棒、掺杂Cd~(2+)或掺杂Zn~(2+)的SnO_2纳米棒的奇异红外光谱演变现象
在400-1000cm~(-1)低波数范围，SnO_2纳米棒材料Sn-O振动带的特征红外吸收峰呈双峰形式，分别位于680.5cm~(-1)和475.2cm~(-1)的位置。SnO_2纳米棒Sn-O红外吸收特性与纳米棒直径大小密切相关，表现出明显的尺寸效应。随着SnO_2纳米棒直径的减小，吸收峰出现明显宽化；475.2 cm~(-1)位置的吸收峰，随着SnO_2纳米棒直径减小，吸收峰出现蓝移；680.5cm~(-1)位置的吸收峰，随着SnO_2纳米棒直径减小，吸收峰却出现了红移。这种红外收吸峰蓝移和红移并存的奇异光谱现象，在一维纳米材料中也是首次观察到。
在400-1000 cm~(-1)低波数范围的Sn-O的红外吸收振动带，Cd~(2+)掺杂和Zn~(2+)掺杂SnO_2纳米棒的红外吸收与SnO_2纳米棒的红外吸收相似，也是呈双红外吸收峰。但是随着SnO_2纳米棒直径的减小，吸收峰出现明显宽化外，其Sn-O红外吸收峰只出现红移现象。这种红移由Cd~(2+)、Zn~(2+)在SnO_2纳米棒晶体中形成的替位式晶体结构引起。
5、SnO_2一维纳米材料的氧化还原特性及新的还原反应热力学机理分析通过H_2-TPR研究表明，SnO_2纳米棒具有由表面吸附的活性氧导致的较好的表面活性和氧化还原性质。纯SnO_2纳米棒在320℃左右的低温下就可以使H_2发生缓慢氧化，纯SnO_2纳米棒的H_2还原反应机理是“表面脱氧反应+歧化反应”；Cd~(2+)掺杂和Zn~(2+)掺杂的SnO_2纳米棒的H_2还原反应与纯SnO_2纳米棒的H_2还原反应类似，但由于纳米CdO和ZnO的催化作用使H_2还原反应温度大大降低，并形成H_2消耗反应峰。掺杂Cd~(2+)和Zn~(2+)的SnO_2纳米棒的H_2还原反应机理是“脱氧反应+歧化反应+纳米催化还原反应+Cd~(2+)(或Zn~(2+))的还原反应”。
6、SnO_2纳米棒一维纳米材料的气敏特性及气敏机理探讨
首次以SnO_2纳米棒集群材料为气体敏感材料，设计制作了二种新型材料气体传感器：
(?)SnO_2一维纳米集群材料传感器
(?)SnO_2一维纳米集群材料+SnO_2纳米粉体混合材料传感器
两种新型传感器对乙醇(C_2H_5OH)气体具有很好的灵敏度和稳定性，并具有较好的恢复-响应特性。其中以掺杂Zn~(2+)的SnO_2纳米棒对乙醇气体的敏感性最好，纯SnO_2纳米棒次之，而掺杂Cd~(2+)的SnO_2纳米棒对乙醇气体的敏感性再次之。这种SnO_2一维纳米集群气敏材料的气敏特性及元件设计，还未见报道。
根据纳米SnO_2气敏材料偏离化学计量比及相关缺陷，材料的表面气体吸附特性，晶粒尺寸及比表面积大小，以及界面理论和导电通道理论，讨论了SnO_2一维纳米材料的气敏机理，提出了SnO_2一维纳米材料的气敏机理模型。用该气敏机理能很好地解释相关的实验结果。
Nanoscale one-dimensional (1-D) materials of SnO_2 nanorods, SnO_2 nanorods doped Cd~(2+) and SnO_2 nanorods doped Zn~(2+) were produced by a new method and technology of preparation. It was researched that the method and the technology of preparation, the structures, the growth mechanism of SnO_2 nanorods were studied. Comparing SnO_2 nanorods materials with SnO_2 nano-powders and SnO_2 nano-particles coating on SiO_2 ball prepared, the properties in infrared absorption spectra (IR), redox, gas sensitive of SnO_2 nanorods materials were studied. High sensitivity and high selectivity new gas sensors of SnO_2 nanorods materials were investigated too. Some new results were obtained in this paper. The results are as follows:
1. Preparation and characterizations of SnO_2 nanorods
A new synthesis method of SnO_2 nanorods developed based on the preparing way of SnO_2 nanorods via annealing the precursor powders, which were prepared by microemulsion system consisting of oil phase, water phase and surfactant. SnO_2 nanorods were produced via the growth in molten salt medium of precursors, which prepared applying by solid-state reaction coated surfactants at room temperature. It was obtained that the preparing techniques of SnO_2 precursors and SnO_2 nanorods.
It is found that SnO_2 nanorods prepared via the new synthesis method were single crystal materials. The diameter and length of the SnO_2 nanorods are in the range of 5nm to 100nm and several micrometers depended on the growth temperature and time. The atomic composition of Sn and O was calculated by using peak area sensitivity factors. The results showed that the atomic ratio of Sn/O was changed from 1:1 to 1:2. The deviation of composition from stoichiometry caused by oxygen vacancies was strongly affected by the growth temperature. Lower growth temperature, higher atomic ratio of Sn and O. Contradictorily, higher growth temperature, closer to the stoichiometry of atomic ratio of Sn and O.
2. Synthesis and characterizition of SnO_2 nanorods doped Cd~(2+) or Zn~(2+)
In molten salt medium, two kinds of SnO_2 nanorods doped Cd~(2+) or Zn~(2+) were obtained via annealing the precursors of SnO_2 powders doped Cd~(2+) or Zn~(2+), which were prepared by redox reaction in microemulsion system. The structure and chemical composition of SnO_2 nanorods doped Cd(2+) or Zn(2+) were characterized by means of XPS and XFS(X-ray fluorescence spectrometry). It is found that the content of CdO in SnO_2 nanorods materials doped Cd~(2+) is up to 3%, and the content of ZnO in SnO_2 nanorods materials doped Zn~(2+) is up to 1.5 %. The crystalline structure of SnO_2nanorods doped Cd~(2+) or Zn~(2+) is a substitutional solid solution crystalline, which was formed by Sn~(4+) replaced with Cd~(2+) or Zn~(2+). The work was not reported.
3. Growth processes and mechanism of SnO_2 nanorods in molten salt medium
The growth processes and mechanism of SnO_2 nanorods in molten salt medium were investigated. The growth of SnO_2 nanorods is a process of homogeneously dispersed particles of SnO_2 precursors growing into SnO_2 whiskers via self assembly, forming thin SnO_2 nanorods, and gradually growing up in molten salt medium. The main feature of this procedure is a solid transformation forming process of SnO_2 crystalline from nano-particles of 0-D to nanorods of 1-D in molten salt medium.
In molten salt, the growth mechanism of SnO_2 nanorods is that molten salt provide the liquid environment, in which dispersed particles of SnO_(2-δ) nano-crystal can diffuse along the dislocations in tubes. SnO_2 was formed by divergent reaction of SnO contained in SnO_(2-δ), and take the tube dislocations as "template" oriented growth via self assembly derived by decreasing the surface energy of homogeneously dispersed SnO_(2-δ) particles, and controlled by VLS growth mechanism. Eventually, SnO_(2-δ) particles grow into SnO_2 nanorods in the tube dislocations of molten salt. The growth mechanism of SnO_2 nanorods in molten salt medium is a new mechanism of 1-D nano-materials.
4. Study on infrared absorption characteristics of SnO_2 nanorods
The infrared absorption characteristics of SnO_2 nanorods with different diameters were investigated by infrared absorption spectra (IR). It is found that there existdouble peaks at 475.2cm~(-1) and 680.5cm~(-1) of the vibrational modes of Sn-O band in the low frequency range 400-1000 cm~(-1). The IR modes of Sn-O band depend on the diameter of SnO_2 nanorods closely. The smaller the diameter is, the wider the IR peaks become. The active IR mode at 475.2cm~(-1) shifts to high frequency(blue shift) in accordance with decrease of diameter of SnO_2 nanorods. On the other hand, the active IR mode at 680.5cm~(-1) shifts to low frequency(red shift) in accordance with decrease of diameter of SnO_2 nanorods. This novel phenomenon about the infrared absorption spectra of SnO_2 nanorods with different diameters was investigated for the first time.
Being similar to the infrared absorption spectra of SnO_2 nanorods, the infrared absorption spectra of SnO_2 nanorods doped Cd~(2+) or Zn~(2+) have double peaks of the vibrational modes of Sn-O band in the low frequency range 400-1000 cm~(-1), too. But the two active IR modes shift to low frequency(red shift) in accordance with decreasing of nanorods diameter at the same time. It is different from the infrared absorption spectra of SnO_2 nanorods due to the substitutional solid solution crystalline structure of SnO_2 nanorods doped Cd~(2+) or Zn~(2+).
5. Redox properties and new reaction thermodynamics mechanism of SnO_2 nanorods
The redox properties of SnO_2 nanorods materials were investigated by means of H_2-TPR. The results showed that the better redox properties of SnO_2 nanorods ascribed to higher oxidizing activity induced adsorbed oxygen on the surface of SnO_2 nanorods. The slow-reaction temperature of H_2 consumption was started at 320℃. The reaction mechanism of SnO_2 nanorods is in the employ of H_2 consumption reaction of the desorbed oxygen and the divergent reaction of SnO_2.
The redox properties of SnO_2 nanorods materials doped Cd~(2+) or Zn~(2+) were similar to redox properties of SnO_2 nanorods materials. But the started slow-reaction temperature of H_2 consumption were reduced in a large degree due to the catalytic effect of CdO or ZnO. The reaction was started at 270℃and the H_2 consumption peak was at 510℃in H_2-TPR profile of SnO_2 nanorods materials doped Cd~(2+). In the meanwhile, the reaction was started at 180℃and the H_2 consumption peak was at 420℃in H_2-TPR profile of SnO_2 nanorods materials doped Zn~(2+). The reaction mechanism submits to catalytic reaction of CdO or ZnO cooperated with H_2 consumption reaction of the desorbed oxygen, the divergent reaction of SnO_2 and reduction reaction of Cd~(2+) or Zn~(2+). This work of reaction mechanism was reported for the first time.
6. Research on gas sensing properties and new gas sensitive mechanism of SnO_2 1-D nano-materials.
Two kinds of gas sensor have been desired with new gas-sensing materials based on SnO_2 nanorods and mixture materials of SnO_2 nanorods with SnO_2 nano-powders for the first time. It was discovered that sensors exhibited higher sensitivity, better selectivity, better stability, and better response and reversion to ethanol (C_2H_5OH). Sensors based on SnO_2 nanorods materials doped Zn~(2+) illustrated the best sensitivity to ethanol and sensors based on SnO_2 nanorods materials was inferior to it. Sensitivity to ethanol of the sensors based on SnO_2 nanorods materials doped Cd~(2+) followed them. The work was not still reported.
The gas sensitive mechanism of SnO_2 nanorods was put forward according to structure characteristics of SnO_2 nanorods gas sensitive materials with deviated from stoichiometry, to adsorption properties and interface principle, to grain size and surface-to-volume ratios associated with 1-D nanostructures, and to the tunnel of electrical conductivity theory. Relative experiment results of the gas sensing properties of SnO_2 nanorods materials can be explain very well with using the mechanism pattern.
引文
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