镍和氧化镍纳米晶的控制生长及应用研究
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摘要
传感器技术是当今世界发展最为快速的高新技术之一，也是现代工程技术进步的一个重要标志；电导型纳米传感器现已在航空航天、军事国防、信息科技、矿山机械、食品安全、家庭安全、生物监测、农业监视、医学、环境等诸多领域获得广泛的应用和发展。NiO拥有稳定的理化性能，被认为是构筑微型传感器的理想候选材料之一，其最为重要的应用就是电导型气敏传感器。本论文主要研究了Ni和NiO纳米晶（纳米线、树枝晶、纳米锥）的可控生长，并将NiO纳米线和Zn掺杂的NiO树枝晶应用于微型气敏传感器，利用NiO的纳米效应来提高气敏传感器对气体分子的快速吸附，利用Zn掺杂来改善传感器对气体分子的快速解吸附特性；同时，通过去除Ni纳米锥表面的气体分子极大地改善了其场电子发射性能，为新型场电子发射器的开发提供了新的思路。具体研究进展如下：
（1）通过磁场辅助肼还原法制得了高纯的Ni纳米线，在空气中380℃以下具有很高的化学稳定性，矫顽力Hc（257.6Oe）高于体相材料；同时，实验发现通过改变溶液中的Ni~(2+)离子浓度、反应温度、NaOH浓度、溶剂种类、外加磁场强度、反应时间、N_2H_4·H_2O浓度可以很好地控制Ni纳米线的表面形貌、微结构、长径比；根据大量的实验得出了Ni纳米线的生长机制，发现通过外加磁场和反应参数能够很好地将Ni晶核组装成不同形貌的纳米结构；此外，我们开发了批量Ni纳米线的制备装置。
（2）通过高温氧化法将磁场组装的超长Ni纳米线阵列转化为NiO纳米线阵列，发现氧化温度越低，NiO纳米线的平均晶粒尺寸越小，带隙值越大；根据不同温度和时间的高温氧化实验提出了NiO纳米线的形成机理；随后利用lift-off工艺将NiO纳米线阵列组装成气敏传感器，发现其对NH_3均具有很好的响应、恢复性能，优异的重复性和选择性；此外，我们还发现平均晶粒尺寸越小的NiO纳米线传感器灵敏度越大，这是因为其表面活性点较多，能够吸附更多的NH_3分子。
（3）通过电解法制得了分层、对称、高度有序的Ni树枝晶，研究发现Ni树枝晶主要由主干、第二分支、第三分支组成，第二分支与主干之间的角度约为70o，第三分支与第二分支之间的角度约为60o，树枝晶的主干和分支的直径分别为280nm和210nm，主干和分支的平均长度分别为10μm和1.5μm；根据一系列不同时间反应产物的形貌，分析了Ni树枝晶的生长过程，提出了Ni树枝晶可能的生长机制；实验还得出了电解法制备Ni树枝晶的最佳工艺参数。
（4）通过电解的途径和随后的高温氧化法制得了Zn掺杂的NiO树枝晶，SEM测试得知树枝晶的主干长度在6-10μm，分支长度在1-3μm；HRTEM分析显示，Zn掺入之后，NiO晶格条纹有加宽的趋势，这是因为较大的Zn原子替代了NiO晶格中较小的Ni原子所致；同时发现Zn在NiO树枝晶中的溶解极限低于7%；随后将掺杂的树枝晶组装成微传感器并测试其对NH_3的气敏性能，发现Zn的掺入致使传感器的响应速度提高了5-8倍，恢复速度提高了30-50倍；最后探讨了Zn掺杂NiO树枝晶传感器的气敏机理。
（5）通过水热法在Ni箔基底上可控生长了Ni纳米锥阵列，锥底直径范围为50-450nm，锥的高度范围为50-200nm，锥的顶部直径在10nm左右，锥的顶角约40o；同时探讨了Ni纳米锥的生长机制以及反应参数对锥体结构的影响；随后我们用Ni纳米锥作为阴极，镀有ITO玻璃作为阳极，测试了其场电子发射性能，发现真空环境下的残余气体分子对Ni纳米锥场电子发射性能有较大的影响，针对这种问题我们提出了两种改善Ni纳米锥场电子发射性能的方案。
Sensor technology is one of the most rapidly developing high-tech, which is animportant symbol of the development of modern science and technology. Conductancenano-sensors are being widely applied in aerospace, national defense, informationtechnology, mining machinery, food security, homeland security, biological detection,monitoring of agriculture, medical, environments, and so on. NiO has stable physical andchemical properties, which are considered to be one of the ideal materials for buildingminiature sensors, and the conductance nano-sensor is the most important application ofNiO. In our work, we synthesized the Ni and NiO nanocrystals (nanowires, dendriticcrystals and nanocones), and exploited the NiO nanowire and Zn doped NiO dendriticcrystal as the sensing materials, to fabricate the gas sensor based on the networks of NiOnanocrystals. NiO nanometer effect makes the fast adsorption of gas molecules, and Zndoping makes the fast desorption of gas molecules in gas sensors. Meanwhile, we greatlyimproved the field electron emission properties of Ni nanocone arrays via the removal ofgas molecules on the nanocones’ surface, which provide a new idea of field electronemitters. Specific research progresses are as follows:
(1) Ni nanowires with large aspect ratio have been prepared via a hydrazine hydratereduction method under assistance of magnetic fields, which have the high stability in air,and the coercivity (Hc,257.6) of nanowires is higher than that of the bulk materials.Meanwhile, we find that the surface morphology, microstructure and aspect ratio of Ninanowires can be controlled through adjusting the Ni~(2+)concentration, reaction temperature, NaOH concentration, solution species, intensity of the applied magnetic field, reaction timeand N_2H_4·H_2O concentration. The growth mechanism of Ni nanowires was proposedaccording to lots of experiments, which illustrate that the different morphology ofnanocrystals can be assembled with Ni nuclei via external magnetic field and optimalreaction parameters. In addition, we developed a batch Ni nanowires preparation device,which mainly comprises five large institutions (the reaction chamber, the compensationloop part, thermostatic temperature control part, a magnetic field generator, gas protectingpart).
(2) Transformation from Ni nanowire arrays to NiO semiconducting nanowire arrayscan achieved via in situ high temperature oxidation method. It was found that the lower theoxidation temperature is, the smaller the average grain size of the NiO nanowries is, thelarger the bad gap energy is. The forming mechanism of NiO nanowires was providedaccording to the different temperature and time experiments. And then, we assembled theas-synthesized NiO nanowires into the gas sensor using the lift-off technology, and findthat this sensor have the fast response, rapid recovery, outstanding reproducibility andexcellent selectivity. In addition, we find that the sensitivity of sensor gradually increaseswith the decrease of average grain size of NiO nanowires due to the smaller grains havingmore grain boundaries, which are considered as the active sites to adsorb more gasmolecules.
(3) Symmetric Ni dendritic crystals, which consist of a long main trunk and highlyordered secondary and tertiary branches, have been successfully synthesized via a simpleand inexpensive electrolytic process in ethylene glycol solution. The length of the maintrunk is about10μm, and that of each branch is about1.5μm with a width of210nm.Microstructure characterization indicates that the angles between the central trunk and allthe secondary branches in dendritic structure are almost the same at about70o, and theangles between the secondary branches and tertiary branches are about60o. A possible growth mechanism of magnetic pure metal dendritic crystals was proposed afterinvestigating four different stages during the electrolytic process. Meanwhile, we obtainedthe optimal parameters of preparation of Ni dendritic crystals: NiCl2concentration is0.010mol/L, electrolytic voltage is50V, electrolytic temperature is60oC, and electrolytic timeis more than5h.
(4) Zn-doped NiO dendritic crystals have been successfully synthesized via anelectrolytic approach combined with subsequent high temperature oxidation. The trunkshave lengths in the range6–10μm with diameters varying from190nm to200nm, and thebranches have lengths in the range1–3μm with diameters varying from150nm to180nm.Microstructure characterization indicated that the solubility limit of zinc ions in the NiOlattice sites was lower than7mol%. We systematically investigated the gas sensingproperties of the Zn-doped NiO sensors for NH_3gas detection at room temperature. Thesensor with doped NiO dendritic crystals gave5–8times faster responses and30–50timesfaster recovery speeds than the sensor with pristine NiO dendritic crystals, which isimportant for the practical application of this NiO sensor. Lastly, a possible gas sensingmechanism of NiO dendritic crystal sensors was discussed.
(5) We present the fabrication of Ni nanocone arrays on Ni foil substrate as well asgas exposure field electron emission experiments using them as cold electron cathodes.The Ni nanocones have base diameters ranging from50to450nm and heights rangingfrom50to200nm. The tip diameter of the nanocones is about10nm and the apex angle ofnanocone is about40o. Field electron emission measurements indicated that the as-grownNi nanocone array is an excellent field emitter exhibiting low turn-on field, high currentdensity, and large field enhancement factor due to sharper tips and better contact with theNi substrate. Meanwhile, we find that adsorbed gas molecules greatly hindered the fieldelectron emission performance of the Ni nanocone array. Repeated applying voltage or‘vacuum J–E annealing’ could significantly improve field emission properties and stability, which is attributed to desorption of the adsorbed gas molecules through Joule heating.
（1）通过磁场辅助肼还原法制得了高纯的Ni纳米线，在空气中380℃以下具有很高的化学稳定性，矫顽力Hc（257.6Oe）高于体相材料；同时，实验发现通过改变溶液中的Ni~(2+)离子浓度、反应温度、NaOH浓度、溶剂种类、外加磁场强度、反应时间、N_2H_4·H_2O浓度可以很好地控制Ni纳米线的表面形貌、微结构、长径比；根据大量的实验得出了Ni纳米线的生长机制，发现通过外加磁场和反应参数能够很好地将Ni晶核组装成不同形貌的纳米结构；此外，我们开发了批量Ni纳米线的制备装置。
（2）通过高温氧化法将磁场组装的超长Ni纳米线阵列转化为NiO纳米线阵列，发现氧化温度越低，NiO纳米线的平均晶粒尺寸越小，带隙值越大；根据不同温度和时间的高温氧化实验提出了NiO纳米线的形成机理；随后利用lift-off工艺将NiO纳米线阵列组装成气敏传感器，发现其对NH_3均具有很好的响应、恢复性能，优异的重复性和选择性；此外，我们还发现平均晶粒尺寸越小的NiO纳米线传感器灵敏度越大，这是因为其表面活性点较多，能够吸附更多的NH_3分子。
（3）通过电解法制得了分层、对称、高度有序的Ni树枝晶，研究发现Ni树枝晶主要由主干、第二分支、第三分支组成，第二分支与主干之间的角度约为70o，第三分支与第二分支之间的角度约为60o，树枝晶的主干和分支的直径分别为280nm和210nm，主干和分支的平均长度分别为10μm和1.5μm；根据一系列不同时间反应产物的形貌，分析了Ni树枝晶的生长过程，提出了Ni树枝晶可能的生长机制；实验还得出了电解法制备Ni树枝晶的最佳工艺参数。
（4）通过电解的途径和随后的高温氧化法制得了Zn掺杂的NiO树枝晶，SEM测试得知树枝晶的主干长度在6-10μm，分支长度在1-3μm；HRTEM分析显示，Zn掺入之后，NiO晶格条纹有加宽的趋势，这是因为较大的Zn原子替代了NiO晶格中较小的Ni原子所致；同时发现Zn在NiO树枝晶中的溶解极限低于7%；随后将掺杂的树枝晶组装成微传感器并测试其对NH_3的气敏性能，发现Zn的掺入致使传感器的响应速度提高了5-8倍，恢复速度提高了30-50倍；最后探讨了Zn掺杂NiO树枝晶传感器的气敏机理。
（5）通过水热法在Ni箔基底上可控生长了Ni纳米锥阵列，锥底直径范围为50-450nm，锥的高度范围为50-200nm，锥的顶部直径在10nm左右，锥的顶角约40o；同时探讨了Ni纳米锥的生长机制以及反应参数对锥体结构的影响；随后我们用Ni纳米锥作为阴极，镀有ITO玻璃作为阳极，测试了其场电子发射性能，发现真空环境下的残余气体分子对Ni纳米锥场电子发射性能有较大的影响，针对这种问题我们提出了两种改善Ni纳米锥场电子发射性能的方案。
Sensor technology is one of the most rapidly developing high-tech, which is animportant symbol of the development of modern science and technology. Conductancenano-sensors are being widely applied in aerospace, national defense, informationtechnology, mining machinery, food security, homeland security, biological detection,monitoring of agriculture, medical, environments, and so on. NiO has stable physical andchemical properties, which are considered to be one of the ideal materials for buildingminiature sensors, and the conductance nano-sensor is the most important application ofNiO. In our work, we synthesized the Ni and NiO nanocrystals (nanowires, dendriticcrystals and nanocones), and exploited the NiO nanowire and Zn doped NiO dendriticcrystal as the sensing materials, to fabricate the gas sensor based on the networks of NiOnanocrystals. NiO nanometer effect makes the fast adsorption of gas molecules, and Zndoping makes the fast desorption of gas molecules in gas sensors. Meanwhile, we greatlyimproved the field electron emission properties of Ni nanocone arrays via the removal ofgas molecules on the nanocones’ surface, which provide a new idea of field electronemitters. Specific research progresses are as follows:
(1) Ni nanowires with large aspect ratio have been prepared via a hydrazine hydratereduction method under assistance of magnetic fields, which have the high stability in air,and the coercivity (Hc,257.6) of nanowires is higher than that of the bulk materials.Meanwhile, we find that the surface morphology, microstructure and aspect ratio of Ninanowires can be controlled through adjusting the Ni~(2+)concentration, reaction temperature, NaOH concentration, solution species, intensity of the applied magnetic field, reaction timeand N_2H_4·H_2O concentration. The growth mechanism of Ni nanowires was proposedaccording to lots of experiments, which illustrate that the different morphology ofnanocrystals can be assembled with Ni nuclei via external magnetic field and optimalreaction parameters. In addition, we developed a batch Ni nanowires preparation device,which mainly comprises five large institutions (the reaction chamber, the compensationloop part, thermostatic temperature control part, a magnetic field generator, gas protectingpart).
(2) Transformation from Ni nanowire arrays to NiO semiconducting nanowire arrayscan achieved via in situ high temperature oxidation method. It was found that the lower theoxidation temperature is, the smaller the average grain size of the NiO nanowries is, thelarger the bad gap energy is. The forming mechanism of NiO nanowires was providedaccording to the different temperature and time experiments. And then, we assembled theas-synthesized NiO nanowires into the gas sensor using the lift-off technology, and findthat this sensor have the fast response, rapid recovery, outstanding reproducibility andexcellent selectivity. In addition, we find that the sensitivity of sensor gradually increaseswith the decrease of average grain size of NiO nanowires due to the smaller grains havingmore grain boundaries, which are considered as the active sites to adsorb more gasmolecules.
(3) Symmetric Ni dendritic crystals, which consist of a long main trunk and highlyordered secondary and tertiary branches, have been successfully synthesized via a simpleand inexpensive electrolytic process in ethylene glycol solution. The length of the maintrunk is about10μm, and that of each branch is about1.5μm with a width of210nm.Microstructure characterization indicates that the angles between the central trunk and allthe secondary branches in dendritic structure are almost the same at about70o, and theangles between the secondary branches and tertiary branches are about60o. A possible growth mechanism of magnetic pure metal dendritic crystals was proposed afterinvestigating four different stages during the electrolytic process. Meanwhile, we obtainedthe optimal parameters of preparation of Ni dendritic crystals: NiCl2concentration is0.010mol/L, electrolytic voltage is50V, electrolytic temperature is60oC, and electrolytic timeis more than5h.
(4) Zn-doped NiO dendritic crystals have been successfully synthesized via anelectrolytic approach combined with subsequent high temperature oxidation. The trunkshave lengths in the range6–10μm with diameters varying from190nm to200nm, and thebranches have lengths in the range1–3μm with diameters varying from150nm to180nm.Microstructure characterization indicated that the solubility limit of zinc ions in the NiOlattice sites was lower than7mol%. We systematically investigated the gas sensingproperties of the Zn-doped NiO sensors for NH_3gas detection at room temperature. Thesensor with doped NiO dendritic crystals gave5–8times faster responses and30–50timesfaster recovery speeds than the sensor with pristine NiO dendritic crystals, which isimportant for the practical application of this NiO sensor. Lastly, a possible gas sensingmechanism of NiO dendritic crystal sensors was discussed.
(5) We present the fabrication of Ni nanocone arrays on Ni foil substrate as well asgas exposure field electron emission experiments using them as cold electron cathodes.The Ni nanocones have base diameters ranging from50to450nm and heights rangingfrom50to200nm. The tip diameter of the nanocones is about10nm and the apex angle ofnanocone is about40o. Field electron emission measurements indicated that the as-grownNi nanocone array is an excellent field emitter exhibiting low turn-on field, high currentdensity, and large field enhancement factor due to sharper tips and better contact with theNi substrate. Meanwhile, we find that adsorbed gas molecules greatly hindered the fieldelectron emission performance of the Ni nanocone array. Repeated applying voltage or‘vacuum J–E annealing’ could significantly improve field emission properties and stability, which is attributed to desorption of the adsorbed gas molecules through Joule heating.
引文
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