Synthesis of copper nanowires and its application in flexible electronic devices
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摘要:
目的 本文通过查阅近几年来相关文献，总结了纳米铜线常用的制备工艺、纯化手段、抗氧化方法和性能之间的密切联系，为本领域的研究者快速了解纳米铜线的尺寸形貌、电学性能、应用现状及面临的挑战提供便捷的窗口，并启发出新的思路或研究方向。 方法 运用分析、比较、整理、归纳等方法，系统介绍了近几年纳米铜线常用的制备方法和纯化手段，并从纳米铜线的尺寸形貌、产率和纯度等方面分析了其各自的优缺点；针对纳米铜线易氧化的问题，列举了常用的包覆材料和包覆工艺；总结了纳米铜线在柔性电子器件的应用领域及其效果。 结果 从所参考的文献来看：① 纳米铜线常用的制备方法主要包括模板法、气相沉积法、静电纺丝技术和化学液相法。根据模板自身不同的特点，模板法可以分为软模板法和硬模板法，利用硬模板法合成的纳米铜线的分散性好，按照所需的大小选择合适的模板尺寸，大小均一，但结构单一，模板难去除、价格昂贵、产率低。利用软模板制备纳米材料时，模板形态多样，不需要复杂的设备，但结构稳定性差，导致模板效率不高。气相沉积法根据气相中间产物的形成过程的差异，分为物理气相沉积法和化学气相沉积法，物理沉积法得到的纳米线结晶度较高，但形貌难以控制，并且反应条件较苛刻，能耗高，而化学气相沉积法合成纳米材料具有操作方便、工艺简单、生产成本低等优点，但产物的成分复杂、易团聚、直径分布不均匀。静电纺丝技术制备纳米铜线具有设备简单、操作方便，纺丝便宜，制备周期短，纳米铜线的形貌和尺寸可控，高长径比等优点，但是需要高温去除静电纺丝溶液中的聚合物，对衬底要求较高，因此不适用于不耐高温的柔性基底。利用化学液相法制备纳米铜线时，能够通过优化反应条件调控纳米铜线的生长速率和形貌，成本较低、制备简单，接近工业化生产，适用于大规模生产，成为当前制备纳米铜线主流的方法。② 针对纳米铜线制备过程形成其他形状的副产物及在空气中氧化，导致基于纳米铜线的电子器件功能降低的问题。通过水-疏水有机溶剂体系、摇动—旋转技术，能够有效地将纳米线和纳米颗粒分离开，获得高纯度的纳米线。另外，利用冰醋酸、热退火以及激光烧结等方法，可以去除纳米铜线表面的有机物和氧化物，提高纳米铜线基柔性电子器件的导电率和透射率。③ 为了降低纳米铜线在空气中的腐蚀倾向，提高其应用价值，在纳米铜线表面沉积金、银、镍等惰性金属，包覆石墨烯、石墨烯衍生物和碳纳米管等碳基材料以及聚吡咯、聚多巴胺、聚二甲基硅氧烷等有机聚合物，能够有效减少其与氧气接触，改善纳米铜线的抗氧化性和抗腐蚀性。④ 纳米铜线及其复合材料与纸基、聚氨酯、聚对苯二甲酸乙二酯等柔性基底组装成柔性电子器件，其良好的导电性和透光性成为柔性透明电极、能量存储/转化和柔性传感器等领域理想的选择。 结论 纳米铜线的高导电性、优异的光电特性、耐屈挠性和低成本等优点，有望成为一维纳米银线或纳米金线的替代品，应用于柔性电子领域。随着高产率、绿色环保和低成本制备工艺的开发以及抗氧化处理技术的日益成熟，纳米铜线及其柔性电子器件将会具有更广阔的应用前景。 Abstract: Copper nanowires not only have excellent electrical conductivity comparable to silver, but also have good light transmittance and flexural resistance due to the size effect at the nanoscale. In addition, it is far cheaper than gold and silver, hence it is an ideal electrode material for preparing flexible electronic devices. The synthesis methods of copper nanowires were systematically reviewed, such as template method, vapor deposition method, electrospinning technology, and chemical liquid phase method. Purification technologies based on water-hydrophobic organic solvent system and acid treatment for copper nanowires were introduced. Various cladding materials with core-shell structure and corresponding cladding technologies used to improve the oxidation resistance and stability of copper nanowires were listed, including inert metals, carbon-based materials, and organic polymer materials. The application status of flexible electronic devices integrating high-quality copper nanowires (or their composites) with flexible substrates (paper-based, polyurethane, and polyethylene terephthalate, etc.) in the fields of flexible transparent electrodes, energy storage/conversion, and flexible sensors were concluded. Finally, the challenges faced in practical application were prospected. -
图 1 采用水热法制得纳米铜线(CuNWs) (a)及微观形貌((b)~(d))[37]；(e) 反应前的溶液照片；(f) 在80°C生长1 h后的溶液照片[38]；((g)~(j))Xia等制备的CuNWs微观形貌[41]
Figure 1. Copper nanowires (CuNWs) obtained by hydrothermal method (a) and its micromorphologies ((b)-(d))[37]; (e) Photographs of the solution before reaction for synthesizing CuNWs; (f) Photographs of the solution after reaction for 1 h at 80°C[38]; ((g)-(j)) Morphology of CuNWs prepared by Xia et al[41]
图 3 ((a)~(c)) Cu@Au NWs的形貌；(d) 电生理传感器的示意图；((e), (f)) 安装在目标皮肤上的EMG和ECG传感器的实物照片；((g), (h)) CuNWs氧化前后传感器采集到的EMG、ECG信号变化[64]
Figure 3. ((a)-(c)) Microstructure of Cu@Au NWs; (d) Schematic of the electrophysiology sensor; ((e), (f)) EMG and ECG sensor mounted on the target skin; ((g), (h)) EMG, ECG signal change collected using Cu NWs-based sensor before and after the oxidation[64]
图 4 (a) RCC电极的制造工艺示意图；(b) RCC电极的柔性透明电容触摸板的结构；((c)~(g)) RCC电极电容式触摸传感器的性能测试：(c) “ON”和“OFF”触摸信号；(d) 连续触摸和相应的信号输出；连续触摸力在不同弯曲半径条件下产生的输出触摸信号：(e)平面；(f) 15 mm；(g) 5 mm[94]
Figure 4. (a) Schematic of the fabrication process for the RCC electrode; (b) Structure of flexible transparent capacitive touch plate based on RCC electrode, performance tests of the RCC-electrode-based capacitive touch sensor; (c) “ON” and “OFF” touch signal; (d) A successive touch and corresponding signal output; Successive touch forces generate different output touch signals at the different bending radius conditions: (e) Flat; (f) 15 mm; (g) 5 mm[94]
图 5 (a) Cu RGO NWs仿生棘突微结构压阻传感器的制造过程；(b) Cu RGO NWs仿生棘突微结构压阻传感器的工作机制，表皮仿生Cu RGO NW-SMPS用于实时监测人体运动和微妙生理信号的信号反馈：(c)手腕弯曲；(d)二头肌屈曲；(e)颈部扭转；(f)颈动脉搏动；(g)咽喉吞咽；(h)手指按压；(i)快速敲击；(j)手指弯曲；(k)膝盖弯曲-释放循环；(l)行走[113]
Figure 5. (a) Schematics of the epidermis-bioinspired Cu RGO NW-SMPS; (b) Mechanism revelation of the bioinspired spinosum microstructured piezoresistive sensor with Cu RGONWs, wearable applications of the epidermis-bioinspired Cu RGONW-SMPS for real-time monitoring of human motions and subtle physiological signals feedback in the form of current change: (c) Wrist bending; (d) Bicep flexion; (e) Neck torsion; (f) Carotid artery pulse; (g) Throat swallowing; (h) Finger pressing; (i) Quick tapping; (j) Finger bending; (k) Knee bending-release cycle; (l) Walking[113]
表 1 化学液相法制备的纳米铜线的尺寸
Table 1. Dimension of copper nanowires fabricated by chemical liquid phase method
Number Solvent Cu source Reductant Capping agent Diameter
/nmLength
/μmReference 1 H2O CuCl2 L-AA ODA 35 100 [10] 2 H2O CuCl2 C6H12O6 HDA 25-35 50-60 [46] 3 H2O CuCl2 C6H12O6 OLA/
OA65 70 [44] 4 NaOH(aq) Cu(NO3)2 N2H4 EDA 35 200 [47] 5 H2O CuCl2 C6H12O6 DDA 18 200 [48] 6 H2O Cu(OH)2 C6H12O6 DETA 37 17 [49] 7 H2O CuCl2 ODA ODA 30-100 Several millimeters [42] 8 EG Cu(NO3)2 – PVP/
CTAC60 40 [50] 9 OLA/
C18H36CuCl2,
Cu(acac)2OLA OLA 30-35 35-45 [51] 10 H2O CuCl2 C6H12O6/
KBrODA 20-40 Hundreds of micrometers [52] Notes: L-AA—L-ascorbic acid; ODA—Octadecylamine; HDA—Hexadecylamine; OLA—Oleylamine; OA—Oleic acid; PVP—Polyvinylpyrrolidone; CTAC—Cetyltrimethylammonium chloride; EG—Ethylene glycol; EDA—Ethylenediamine; DDA—Dodecylamine; C18H36—Octotene; DETA—Diethylenetriamine; N2H4—Hydrazine hydrate; Cu(acac)2—Copper(Ⅱ) acetylpyruvate. 
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