受限空间内一维纳米材料的制备与生长机理研究
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摘要
对能满足21世纪要求且具有分子级性能材料的探索,引导了一维纳米结构的发展。几乎每种传统材料都有一种一维纳米材料的匹配物。一维纳米材料在纳米电子学、设备和系统、纳米复合材料、可替代能源和国家安全上都具有深远的影响。本论文紧跟时代要求,成功制备了具有集成图案的一维纳米材料阵列,如一维聚合物纳米材料、一维金属纳米材料,开拓了同轴金属纳米电缆和多层金属纳米材料体系,研究了这些一维纳米材料的制备,并探讨了在受限空间内一维纳米材料的生长机理,这一领域的系统性研究尚未见报道。
本论文掌握了采用紫外光刻蚀技术制备纳米或微米图案的工艺。在众多的图案化制备技术中,紫外光刻技术被认为是一种制备大面图案、经济、易操作的技术。在紫外光刻技术中有五个主要步骤：涂胶、前烘、曝光、后烘和显影。对每一个步骤都做了详尽的分析和实验,最终找到了一个最适宜的工艺条件,在多孔氧化铝(AAO)模板的表面上成功制备了不同图案、不同尺寸的大面积、规整图案。
首次以图案化模板为二次模板,通过物理浸润的方法,如溶液浸润法和熔体浸润法,成功制备了多种图案化的聚合物纳米管和纳米线阵列结构,如常规分子量的PS、PA6、PA66、PA11、ABS、PMMA等六种聚合物。微观形貌测试结果表明,两种方法都能获得结构完整的纳米管和纳米线结构,其直径与模板孔径相吻合。在溶液法中,纳米管壁厚随着溶液浓度的增加而增厚,当溶液浓度达到一定值时,制得纳米线结构,溶剂不同则溶液浓度不同,如以三氯甲烷为溶剂配制聚苯乙烯(PS)溶液,溶液浓度为10.0 wt%,则得到PS纳米线；以甲酸为溶剂配制聚酰胺6(PA6)溶液,溶液浓度为8.0 wt%,则可制得PA66纳米线。熔体法制备时,纳米管的壁厚与熔融温度有关,一般地,熔融温度越高,纳米管的壁厚越薄,反之,越厚。
首次用高分辨电子透射电镜观察到了低结晶度聚合物(PS)和高结晶聚合物(PA6)纳米管的结晶现象,突破了以模型研究聚合物纳米管结晶的范畴。在纳米管外壁的部分区域观察到结晶条纹,其它区域为无定形区。通过与本体聚合物的X射线衍射对比,发现聚合物纳米管的X射线衍射图谱有较大的改变,这表明在受限空间内纳米管在形成过程中,有晶相转变现象发生,而PA6则发生了明显的转变,在本体中主要存在α晶相,而在纳米管中则转变成γ晶相。
研究了金属纳米材料的制备及其性质。采用电化学沉积方法制备了非磁性金属纳米线体系(以Cu为代表),研究发现,纳米线随着沉积时间的延长而增长,但不成正比关系。高分辨与电子衍射花样显示Cu纳米线具有单晶结构；生长方向沿[220],首次观察到纳米线的断裂方向,分别沿着(202)和(022)两个晶面的方向断裂,断裂端呈规则的圆锥型；在外力作用下,Cu纳米线还显示出与块体材料相似的性质：柔韧性。
同时,研究了磁性金属纳米材料(以Ni,Co,Fe为代表)的制备及磁性能。经过一系列的实验,通过高分辨透射电镜表征,首次观察到磁性纳米管的形成过程,发现在沉积时间低于15min,得到的全部是纳米管,高于40mmin得到的全部是纳米线,由此可知先生成纳米管,再形成纳米线。通过磁性测试发现磁性金属纳米管具有一定的磁性,在轴方向上易被磁化,却拥有较低的矫顽力。
研究了Cu/Ni核/壳结构的同轴纳米电缆的制备方法和磁性。通过两步电沉积方法(先沉积Ni纳米管,再在Ni纳米管中沉积Cu纳米线)和一步共沉积方法(电解质溶液中既含有Ni离子也含有Cu离子),均能制备Cu/Ni核/壳结构的同轴纳米电缆结构。与Ni纳米管磁性能相比,Cu/Ni核/壳结构的同轴纳米电缆剩余磁化强度明显大于Ni纳米管的剩余磁化强度。
开拓了Cu-Ni嵌段纳米线新体系。透射电镜照片显示了嵌段纳米线的竹节状结构,电子衍射花样显示界面处的物质具有单晶结构,与Ni纳米层的多晶结构不相符,对此,解释了可能的形成原因,是由于原子掺杂所致。
首次提出了聚合物在受限空间内形成机理：bamboo-like和cylinder-shaped两种形成方式,并给予了充分的解释。根据此现象,首次提出了AAO模板对聚合物纳米管的形成具有诱导效应,可以导致聚合物在受限空间内成核时发生晶型和结晶度的改变,影响分子链的排列。同时,首次提出了磁性金属纳米管的形成机理：brick-stacked wirelike growth生长机理。
The quest for materials with molecular scale properties that can satisfy the demands of the 21st century has led to the development of one dimensional nanostructures, ODNS. Nearly, every class of traditional material has an ODNS counterpart. ODNS has a profound impact in nanoelectronics, nanodevices and systems, nanocomposite materials, alternative energy resources and national security. In the thesis, one dimensional nanomaterials arrays, such as polymer nanomaterials and metal nanomaterials, with integrated patterns have been successfully fabricated. Meanwhile, we developed new nanomaterials systems including metal coaxial nanocable and metal multilayer nanomaterials. However, only few systemic research works concerning the fabrication and growth mechanism in restricted spaces have been reported.
Fabrication of nano- or micro- patterns with photolithographic technique has been marstered. Among those techniques, photolithography has been regarded as one of the most successful techniques in large-scale microfabrication, and the method is effective, low-cost and simple implementation. There are main 5 steps:coating, soft bake, exposure, hard bake and developing. The best experimental conditions have been found by systemic analysis and experiment. High-ordered large area patterns with different scales and patterns have been fabricated on the side of porous anodic aluminum oxide (AAO) templates.
Patterned AAO template were used as a second template firstly to fabricate various patterned polymer (such ascommen molecular weight PS, PA6, PA66, PA11, ABS, PMMA) nanotube and nanowire arrays by polymer solution wetting and melt wetting templates. The diameters of the polymer nanotubes and nanowires are consistent with the pore diameters of the templates. The wall of the nanotubes increases with the solution concentration in solution wetting template. When the solution concentration reaches a certain value, nanowires are obtained. The concentration are different with the solvents, for example, trichloromethane was used as solvent in PS solution, and the concentration was 10.0 wt%, and PS nanowires were obtained. Whereas, if formic acid was used as solvent in PA6 solution, and the concentration was 8.0 wt%, then PA6 nanowires were obtained. With melt wetting templates, the wall of nanotubes is depended on the melt temperature. Generally, the more the melt temperature is, the thinner the wall of the nanotubes is, or, thicker.
The crystallization phenomena of the low crystallinity PS and high crytallinity PA6 have been observed by high reolution transition electron microscope (HRTEM) firstly. The crystalline lattice fringes exist in some regions, while most regions show an amorphous nature. Compared with X-ray diffraction (XRD) patterns of the bulk polyer, the XRD patterns of polymer nanotubes are very different. It is proved that crystal phase have changed during the nanotubes growing in the restricted spaces. And, it was found that there is a crystal transformation from the a-form in bulk to theγ-form of PA6 in nanotubes.
Fabrication and properties of metal nanomaterials were studied. Cu nanowires were prepared by the electrodeposition. The length of the Cu nanowires increases with the deposition time. HRTEM image and select area electron diffraction pattern show that the Cu nanowires have single crystal structure. The growth orientation is along [220] direction, and the broken orientation was obsvered firstly, it is along (202) and (022) directions, respectively. Regular cones were formed at the broken end of nanowires. Bent nanowires were also observed, this means that the copper nanowires have good mechanical properties when applied external force.
In the meantime, ferromagnetic nanomaterials, such as Ni, Co and Fe, were studied on fabrication and magnetic property firstly. The process of the nanotube growth was observed by the HRTEM after a series of experiments. The deposition time is less than 15 min, nanotubes are obtained. While the deposition time is more than 40 min, nanowires are obtained. Come to the conclusion, the nanotubes are obtanined first, then nanowires. It was found that the nanotubes are magnetized along the long axis more, but have lower coercivity.
Fabrication and magnetic property of Cu/Ni core/shell coaxial nanocables were investigated. There are two methods to obtain nanocables:the first method, Ni nanotubes were deposited first, and then deposited Cu naniwires in the obtained Ni nanotubes. The second method is codeposition. Compared with the magnetic property of Ni nanotubes, the remanent magnetization of the Cu/Ni nanocalbe is lager than that of Ni nanotubes.
The new Cu-Ni block nanowire system was developed. TEM images show that the block nanowires have bamboo-like structure. SAED pattern at the interfaces between Ni and Cu layer shows where the matter possesses single crystal structure which is not consistent with polycrystal structure of Ni layer. The reasons for the formation may be caused by the atomic doping.
Two growth mechanisms including bamboo-like and cylinder-shaped growth mechanism for the polymer nanotube forming in the restricted spaces were put forward firstly. According to the experimental results, the induction effect of the AAO templates for the polymer nanotubes formation was raised firstly. The induction effect can cause changes for crystal form and crystallinity, and affect molecular chains arrangement. For the magnetic metal nanotube formation, the Brick-Stacked Wirelike Growth (BSWG) mechanism was first proposed.
本论文掌握了采用紫外光刻蚀技术制备纳米或微米图案的工艺。在众多的图案化制备技术中,紫外光刻技术被认为是一种制备大面图案、经济、易操作的技术。在紫外光刻技术中有五个主要步骤：涂胶、前烘、曝光、后烘和显影。对每一个步骤都做了详尽的分析和实验,最终找到了一个最适宜的工艺条件,在多孔氧化铝(AAO)模板的表面上成功制备了不同图案、不同尺寸的大面积、规整图案。
首次以图案化模板为二次模板,通过物理浸润的方法,如溶液浸润法和熔体浸润法,成功制备了多种图案化的聚合物纳米管和纳米线阵列结构,如常规分子量的PS、PA6、PA66、PA11、ABS、PMMA等六种聚合物。微观形貌测试结果表明,两种方法都能获得结构完整的纳米管和纳米线结构,其直径与模板孔径相吻合。在溶液法中,纳米管壁厚随着溶液浓度的增加而增厚,当溶液浓度达到一定值时,制得纳米线结构,溶剂不同则溶液浓度不同,如以三氯甲烷为溶剂配制聚苯乙烯(PS)溶液,溶液浓度为10.0 wt%,则得到PS纳米线；以甲酸为溶剂配制聚酰胺6(PA6)溶液,溶液浓度为8.0 wt%,则可制得PA66纳米线。熔体法制备时,纳米管的壁厚与熔融温度有关,一般地,熔融温度越高,纳米管的壁厚越薄,反之,越厚。
首次用高分辨电子透射电镜观察到了低结晶度聚合物(PS)和高结晶聚合物(PA6)纳米管的结晶现象,突破了以模型研究聚合物纳米管结晶的范畴。在纳米管外壁的部分区域观察到结晶条纹,其它区域为无定形区。通过与本体聚合物的X射线衍射对比,发现聚合物纳米管的X射线衍射图谱有较大的改变,这表明在受限空间内纳米管在形成过程中,有晶相转变现象发生,而PA6则发生了明显的转变,在本体中主要存在α晶相,而在纳米管中则转变成γ晶相。
研究了金属纳米材料的制备及其性质。采用电化学沉积方法制备了非磁性金属纳米线体系(以Cu为代表),研究发现,纳米线随着沉积时间的延长而增长,但不成正比关系。高分辨与电子衍射花样显示Cu纳米线具有单晶结构；生长方向沿[220],首次观察到纳米线的断裂方向,分别沿着(202)和(022)两个晶面的方向断裂,断裂端呈规则的圆锥型；在外力作用下,Cu纳米线还显示出与块体材料相似的性质：柔韧性。
同时,研究了磁性金属纳米材料(以Ni,Co,Fe为代表)的制备及磁性能。经过一系列的实验,通过高分辨透射电镜表征,首次观察到磁性纳米管的形成过程,发现在沉积时间低于15min,得到的全部是纳米管,高于40mmin得到的全部是纳米线,由此可知先生成纳米管,再形成纳米线。通过磁性测试发现磁性金属纳米管具有一定的磁性,在轴方向上易被磁化,却拥有较低的矫顽力。
研究了Cu/Ni核/壳结构的同轴纳米电缆的制备方法和磁性。通过两步电沉积方法(先沉积Ni纳米管,再在Ni纳米管中沉积Cu纳米线)和一步共沉积方法(电解质溶液中既含有Ni离子也含有Cu离子),均能制备Cu/Ni核/壳结构的同轴纳米电缆结构。与Ni纳米管磁性能相比,Cu/Ni核/壳结构的同轴纳米电缆剩余磁化强度明显大于Ni纳米管的剩余磁化强度。
开拓了Cu-Ni嵌段纳米线新体系。透射电镜照片显示了嵌段纳米线的竹节状结构,电子衍射花样显示界面处的物质具有单晶结构,与Ni纳米层的多晶结构不相符,对此,解释了可能的形成原因,是由于原子掺杂所致。
首次提出了聚合物在受限空间内形成机理：bamboo-like和cylinder-shaped两种形成方式,并给予了充分的解释。根据此现象,首次提出了AAO模板对聚合物纳米管的形成具有诱导效应,可以导致聚合物在受限空间内成核时发生晶型和结晶度的改变,影响分子链的排列。同时,首次提出了磁性金属纳米管的形成机理：brick-stacked wirelike growth生长机理。
The quest for materials with molecular scale properties that can satisfy the demands of the 21st century has led to the development of one dimensional nanostructures, ODNS. Nearly, every class of traditional material has an ODNS counterpart. ODNS has a profound impact in nanoelectronics, nanodevices and systems, nanocomposite materials, alternative energy resources and national security. In the thesis, one dimensional nanomaterials arrays, such as polymer nanomaterials and metal nanomaterials, with integrated patterns have been successfully fabricated. Meanwhile, we developed new nanomaterials systems including metal coaxial nanocable and metal multilayer nanomaterials. However, only few systemic research works concerning the fabrication and growth mechanism in restricted spaces have been reported.
Fabrication of nano- or micro- patterns with photolithographic technique has been marstered. Among those techniques, photolithography has been regarded as one of the most successful techniques in large-scale microfabrication, and the method is effective, low-cost and simple implementation. There are main 5 steps:coating, soft bake, exposure, hard bake and developing. The best experimental conditions have been found by systemic analysis and experiment. High-ordered large area patterns with different scales and patterns have been fabricated on the side of porous anodic aluminum oxide (AAO) templates.
Patterned AAO template were used as a second template firstly to fabricate various patterned polymer (such ascommen molecular weight PS, PA6, PA66, PA11, ABS, PMMA) nanotube and nanowire arrays by polymer solution wetting and melt wetting templates. The diameters of the polymer nanotubes and nanowires are consistent with the pore diameters of the templates. The wall of the nanotubes increases with the solution concentration in solution wetting template. When the solution concentration reaches a certain value, nanowires are obtained. The concentration are different with the solvents, for example, trichloromethane was used as solvent in PS solution, and the concentration was 10.0 wt%, and PS nanowires were obtained. Whereas, if formic acid was used as solvent in PA6 solution, and the concentration was 8.0 wt%, then PA6 nanowires were obtained. With melt wetting templates, the wall of nanotubes is depended on the melt temperature. Generally, the more the melt temperature is, the thinner the wall of the nanotubes is, or, thicker.
The crystallization phenomena of the low crystallinity PS and high crytallinity PA6 have been observed by high reolution transition electron microscope (HRTEM) firstly. The crystalline lattice fringes exist in some regions, while most regions show an amorphous nature. Compared with X-ray diffraction (XRD) patterns of the bulk polyer, the XRD patterns of polymer nanotubes are very different. It is proved that crystal phase have changed during the nanotubes growing in the restricted spaces. And, it was found that there is a crystal transformation from the a-form in bulk to theγ-form of PA6 in nanotubes.
Fabrication and properties of metal nanomaterials were studied. Cu nanowires were prepared by the electrodeposition. The length of the Cu nanowires increases with the deposition time. HRTEM image and select area electron diffraction pattern show that the Cu nanowires have single crystal structure. The growth orientation is along [220] direction, and the broken orientation was obsvered firstly, it is along (202) and (022) directions, respectively. Regular cones were formed at the broken end of nanowires. Bent nanowires were also observed, this means that the copper nanowires have good mechanical properties when applied external force.
In the meantime, ferromagnetic nanomaterials, such as Ni, Co and Fe, were studied on fabrication and magnetic property firstly. The process of the nanotube growth was observed by the HRTEM after a series of experiments. The deposition time is less than 15 min, nanotubes are obtained. While the deposition time is more than 40 min, nanowires are obtained. Come to the conclusion, the nanotubes are obtanined first, then nanowires. It was found that the nanotubes are magnetized along the long axis more, but have lower coercivity.
Fabrication and magnetic property of Cu/Ni core/shell coaxial nanocables were investigated. There are two methods to obtain nanocables:the first method, Ni nanotubes were deposited first, and then deposited Cu naniwires in the obtained Ni nanotubes. The second method is codeposition. Compared with the magnetic property of Ni nanotubes, the remanent magnetization of the Cu/Ni nanocalbe is lager than that of Ni nanotubes.
The new Cu-Ni block nanowire system was developed. TEM images show that the block nanowires have bamboo-like structure. SAED pattern at the interfaces between Ni and Cu layer shows where the matter possesses single crystal structure which is not consistent with polycrystal structure of Ni layer. The reasons for the formation may be caused by the atomic doping.
Two growth mechanisms including bamboo-like and cylinder-shaped growth mechanism for the polymer nanotube forming in the restricted spaces were put forward firstly. According to the experimental results, the induction effect of the AAO templates for the polymer nanotubes formation was raised firstly. The induction effect can cause changes for crystal form and crystallinity, and affect molecular chains arrangement. For the magnetic metal nanotube formation, the Brick-Stacked Wirelike Growth (BSWG) mechanism was first proposed.
引文
了受限空间为纳米结构带来的某些效应。
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3.首次用HRTEM观察到结晶度较低的PS纳米管结晶的现象,观察到少量区域有明显的衍射条纹,XRD分析亦证明了PS纳米管结晶现象,并根据布拉格方程计算出了晶面间距,与HRTEM显示的条纹间距相吻合。
4.首次用HRTEM观察到结晶度较高的PA6纳米管结晶的现象,并通过傅立叶变换,得到了典型的晶体衍射圆环。XRD分析表明,在AAO模板纳米孔的诱导作用下得到的PA6纳米管的晶型由本体的主要晶型α型转变为γ晶型,DSC曲线也证明了这一事实。
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1.采用电沉积与AAO模板相结合的方法,成功制备了高度有序的图案化金属Cu纳米线阵列,并研究了纳米线长与沉积时间的关系：线长随着沉积时间的延长而增长；高分辨与电子衍射花样显示Cu纳米线具有单晶结构；生长方向沿[220],而断裂方向则沿着(202)和(022)两个晶面的方向断裂,断裂端呈规则的圆锥型；在外力作用下,Cu纳米线还显示出与块体材料相似的性质：柔韧性。
2.采用电沉积与AAO模板相结合的方法,制备了Ni纳米管和纳米线阵列。研究了在不同电沉积参数下能得到不同的微观结构,实验证明,电压低于-1.0V,沉积时间少于15 min,则得到Ni纳米管阵列；时间高于40 min,则得到Ni纳米线阵列。同时,研究了更小尺寸的Ni纳米结构,同样可以得出上述结论。同样,也制备了Co和Fe纳米管阵列。并对这些磁性纳米管进行了磁性测试,发现磁性金属纳米管具有一定的磁性,沿纳米管长轴方向易被磁化。3.本工作通过系统研究,发现磁性金属可以通过控制电沉积参数制备纳米管阵列或纳米线阵列,而非磁性金属铜却得不到纳米管阵列。
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3.采用电沉积法制备了Cu-Ni嵌段纳米线阵列,在Cu纳米层和Ni纳米层界面处,电子衍射图片显示两种单晶结构的物质的掺杂,与Ni纳米层的多晶结构不相符,对此,解释了形成原因。通过TEM照片可以观察到AAO纳米隧道的微观结构可以影响Cu-Ni纳米线的形貌。
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3.首次用HRTEM观察到结晶度较低的PS纳米管结晶的现象,观察到少量区域有明显的衍射条纹,XRD分析亦证明了PS纳米管结晶现象,并根据布拉格方程计算出了晶面间距,与HRTEM显示的条纹间距相吻合。
4.首次用HRTEM观察到结晶度较高的PA6纳米管结晶的现象,并通过傅立叶变换,得到了典型的晶体衍射圆环。XRD分析表明,在AAO模板纳米孔的诱导作用下得到的PA6纳米管的晶型由本体的主要晶型α型转变为γ晶型,DSC曲线也证明了这一事实。
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1.采用电沉积与AAO模板相结合的方法,成功制备了高度有序的图案化金属Cu纳米线阵列,并研究了纳米线长与沉积时间的关系：线长随着沉积时间的延长而增长；高分辨与电子衍射花样显示Cu纳米线具有单晶结构；生长方向沿[220],而断裂方向则沿着(202)和(022)两个晶面的方向断裂,断裂端呈规则的圆锥型；在外力作用下,Cu纳米线还显示出与块体材料相似的性质：柔韧性。
2.采用电沉积与AAO模板相结合的方法,制备了Ni纳米管和纳米线阵列。研究了在不同电沉积参数下能得到不同的微观结构,实验证明,电压低于-1.0V,沉积时间少于15 min,则得到Ni纳米管阵列；时间高于40 min,则得到Ni纳米线阵列。同时,研究了更小尺寸的Ni纳米结构,同样可以得出上述结论。同样,也制备了Co和Fe纳米管阵列。并对这些磁性纳米管进行了磁性测试,发现磁性金属纳米管具有一定的磁性,沿纳米管长轴方向易被磁化。3.本工作通过系统研究,发现磁性金属可以通过控制电沉积参数制备纳米管阵列或纳米线阵列,而非磁性金属铜却得不到纳米管阵列。
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3.采用电沉积法制备了Cu-Ni嵌段纳米线阵列,在Cu纳米层和Ni纳米层界面处,电子衍射图片显示两种单晶结构的物质的掺杂,与Ni纳米层的多晶结构不相符,对此,解释了形成原因。通过TEM照片可以观察到AAO纳米隧道的微观结构可以影响Cu-Ni纳米线的形貌。
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