CN106939413A - 一种锌纳米线阵列电极制备方法 - Google Patents
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Abstract
本发明涉及一种锌纳米线阵列电极的制备方法，属于纳米材料制备与微纳阵列电极设计领域。本发明提出的锌纳米线阵列电极的制备方法是通过球磨将含锌化合物与碳材料混合均匀；而后利用惰性气体将管式炉高温区的锌蒸气带到低温区的基片上形成规则排列的锌纳米线阵列。该方法无需精密仪器控制、无需昂贵原料，锌纳米线阵列致密均匀，长度与直径可通过反应时间控制；电极基底的沉积面积可控且基底也可更换，易于批量化生产，也可制备面积较大的阵列电极再切割成预定的尺寸使用。因此，该方法具有工艺简单、易规模化等优点且制备的锌纳米线阵列电极规则均匀致密，特别适合用于分析检测、柔性储能器件、太阳能电池和传感器等。
Description
技术领域
本发明涉及一种锌纳米线阵列电极的制备方法，属于纳米材料制备与微纳阵列电极设计领域。
背景技术
纳米阵列是以纳米颗粒、纳米线、纳米管为基本单元，采用物理和化学等方法在二维或三维空间构筑的纳米体系。而纳米阵列电极则是多个纳米电极的集合体，制备电极的材料一般包括金属、半导体、高聚物和碳纳米管等，由于纳米阵列电极上的材料具有高度取向性，且电极上的材料尺寸均在纳米尺度，因此该电极除具有一般纳米材料的性质外，它的量子效应、界面效应、小尺寸效应等突出，具有比无序的纳米材料更加优异的性能。此外，纳米阵列电极还可以通过电、磁、光等外场实现对其性能的控制，从而使其成为设计微纳电子元器件的基础。纳米阵列电极的发展对于电化学分析、微型生物传感器、电催化和高能化学电源等领域的发展具有十分重要的意义，并且也显示出了广阔的应用前景。如今人们通过研究，实现了纳米阵列电极的设计与组装，并有效的控制其组成、结构和性能，已相继设计出如圆盘状、井状、截锥形、球形和半球形等多种形状的纳米阵列电极；制备纳米阵列电极的方法也较多，一般有模板法、光/化学刻蚀法、自组装法、气相沉积法等。锌作为一种高导电金属，具有特殊的物化性质，以其作为纳米阵列电极在传感、能源存储、催化、传感等领域将会有广阔的应用空间。然而锌的化学性质较为活泼，且锌金属的晶相结构为六边形，锌纳米线一般沿着±[001]方向生长而产生扭曲，因此获得规则锌纳米线阵列的电极比较困难。例如，Yan将氧化锌和石墨混合，并在反应过程中采用了比较危险的氨气辅助还原制备了锌纳米线(J.Appl.Phys.，2003，93，4807)。Chen采用硼还原氧化锌制备了无序的纳米线，其中硼较昂贵且还原温度高达1050℃(Mater.Lett.，2007，61，144)。Wang以阳极氧化铝为模板基于电化学沉积获得了锌的纳米线，消除阳极氧化铝模板将是一个比较繁琐的过程，并且锌纳米线的表面有氧化锌，影响电极的导电性(NanoLett.，2005，5，1247)。上述工作虽然制备了锌的纳米线，但均未获得规则锌纳米线的阵列电极，如今以锌纳米线构成阵列电极的制备工作仍未见报道。
发明内容
本发明的目的是提供一种工艺简单、成品均匀、易规模化的锌纳米线阵列电极的制备方法，首次制备了规则的锌纳米线阵列电极。该方法成本低廉，生长锌纳米线的基底可以灵活更换，生长的面积也可调控便于微纳器件的加工，这些特性对于未来纳米阵列电极的制备以及电化学分析检测、储能、催化、传感等领域的发展都有十分重要的意义。
本发明解决上述问题采用的技术方案，锌纳米线阵列电极制备方法步骤如下：
将含锌化合物与碳材料以质量比为9～5∶1～5球磨混合0.15～2小时得到初料粉体1；将初料粉体1置于刚玉坩埚中并放入双温区管式炉的第一温区2；然后将一块铜、镍、铁、钛、铂、石墨、金、银、石英、刚玉或硅材质的基片置于双温区管式炉的第二温区3；在惰性气体保护下，初料粉体1在双温区管式炉的第一温区2中以500～1100℃煅烧0.5～3小时，升温速率为1～60℃/min，放有基片的双温区管式炉的第二温区3温度设置为15～50℃；待反应完成自然冷却之后，即在基片上获得直径为0.005～1μm的锌纳米线阵列电极4；
所述含锌化合物为氧化锌、氢氧化锌、碳酸锌、乙酸锌中的一种以上；
所述碳材料为活性炭、碳纤维、碳纳米管、生物质炭、石墨中的一种以上；
所述研磨的转速为200～1000转/分，粉体粒径小于100目；
所述基片的尺寸为长10～500毫米，宽10～500毫米，厚0.01～5毫米；
所述基片在放入双温区管式炉的第二温区3之前用去离子水、乙醇反复清洗干净，光面朝上；所述惰性气体为氮气、氩气中的一种以上，流速为1～1000mL/min。
由上述锌纳米线阵列电极制备方法制得锌纳米线阵列电极，所述锌纳米线的直径为0.005～1μm。
本发明提出的锌纳米线阵列电极的制备方法的原理是：首先通过球磨将将锌的化合物与碳材料混合均匀；而后利用惰性气体将管式炉高温区的锌蒸气带到低温区的铜、镍、铁、钛、铂、石墨、金、银、石英、刚玉或硅材质的基底上，即可形成规则致密的锌纳米线阵列电极。
本发明的有益效果：无需精密仪器控制，电极制备方法简单，电极尺寸灵活可控，可以制备面积较大的锌纳米线阵列电极再可切割成预定的尺寸使用，易于批量化生产；所用原料均是常规的试剂，成本低；制备的阵列电极致密均匀，锌纳米线的长度与直径可通过反应时间控制；无需在基底上种植种子以供阵列生长，技术难度低。因此，该方法具有工艺简单、产品均匀致密规则可控、易规模化等优点，适合用于分析检测、柔性储能器件、太阳能电池和传感器等领域。
附图说明
图1锌纳米线阵列电极的制备示意图
图中：1.初料粉体，2.双温区管式炉的第一温区，3.双温区管式炉的第二温区，4.锌纳米线阵列电极。
图2锌纳米线阵列电极的X射线粉末衍射图谱
图中：纵坐标为X射线衍射峰的强度，单位为任意强度；横纵坐标为X射线衍射角度的2倍。
图3锌纳米线阵列电极的扫描电子显微镜照片
具体实施方式
实施例1
首先分别称取氧化锌8克、活性炭2克，置于球磨罐中，球磨机转速为300转/分，球磨15分钟；得到粉体置于刚玉坩埚中；然后将装有原料粉体的坩埚置于管式炉的中部位置，将清洗干净的硅片置于管式炉出气口的尾端，光面朝上，封闭管式炉，通入氩气的保护气冲洗30分钟。然后就开始加热并保持惰性气氛保护(100毫升每分钟)，用1小时将管式炉升温至700摄氏度并保温1小时；反应完成之后待自然冷却，在硅片上即获得锌纳米线的阵列电极。采用扫描电镜测试发现锌纳米线均匀的分布在硅基底上，平均直径为300纳米，锌纳米线的X射线粉末衍射如图2所示，微观结构的扫描电子显微镜图如图3所示。
实施例2
首先分别称取氧化锌8克、生物质碳2克，置于球磨罐中，球磨机转速为300转/分，球磨15分钟；得到粉体置于刚玉坩埚中；然后将装有原料粉体的坩埚置于管式炉的中部位置，将清洗干净的石英片置于管式炉出气口的尾端，光面朝上，封闭管式炉，通入氩气的保护气冲洗30分钟。然后就开始加热并保持惰性气氛保护(100毫升每分钟)，用1小时将管式炉升温至700摄氏度并保温4小时；反应完成之后待自然冷却，在硅片上即获得锌纳米线的阵列电极。采用扫描电镜测试发现锌纳米线均匀的分布在石英基底上，平均直径为500纳米。
实施例3
首先分别称取氧化锌8克、石墨2克，置于球磨罐中，球磨机转速为300转/分，球磨15分钟；得到粉体置于刚玉坩埚中；然后将装有原料粉体的坩埚置于管式炉的中部位置，将清洗干净的铜片置于管式炉出气口的尾端，光面朝上，封闭管式炉，通入氮气的保护气冲洗30分钟。然后就开始加热并保持惰性气氛保护(100毫升每分钟)，用1小时将管式炉升温至700摄氏度并保温2小时；反应完成之后待自然冷却，在铜片上即获得锌纳米线的阵列电极。采用扫描电镜测试发现锌纳米线均匀的分布在铜基底上，平均直径为250纳米。
实施例4
首先分别称取氧化锌8克、活性炭2克，置于球磨罐中，球磨机转速为300转/分，球磨15分钟；得到粉体置于刚玉坩埚中；然后将装有原料粉体的坩埚置于管式炉的中部位置，将清洗干净的硅片置于管式炉出气口的尾端，光面朝上，封闭管式炉，通入氩气的保护气冲洗30分钟。然后就开始加热并保持惰性气氛保护(100毫升每分钟)，用1小时将管式炉升温至450摄氏度并保温1小时；反应完成之后待自然冷却，采用扫描电镜测试发现，由于煅烧温度不够在硅基片上未发现锌纳米线阵列。
以上实例1、2、3中的锌纳米线阵列排列均匀、致密，制备方法简单，并实现了在不同的基底上生长，优于其他文献和研究报道。
Claims (1)
1.一种锌纳米线阵列电极制备方法，其特征在于锌纳米线阵列电极(4)制备方法步骤如下：
将含锌化合物与碳材料以质量比为9～5∶1～5球磨混合0.15～2小时得到初料粉体(1)；将初料粉体(1)置于刚玉坩埚中并放入双温区管式炉的第一温区(2)；然后将一块铜、镍、铁、钛、铂、石墨、金、银、石英、刚玉或硅材质的基片置于双温区管式炉的第二温区(3)；在惰性气体保护下，初料粉体(1)在双温区管式炉的第一温区(2)中以500～1100℃煅烧0.5～3小时，升温速率为1～60℃/min，放有基片的双温区管式炉的第二温区(3)温度设置为15～50℃；待反应完成自然冷却之后，即在基片上获得直径为0.005～1μm的锌纳米线阵列电极(4)；
所述含锌化合物为氧化锌、氢氧化锌、碳酸锌、乙酸锌中的一种以上；
所述碳材料为活性炭、碳纤维、碳纳米管、生物质炭、石墨中的一种以上；
所述研磨的转速为200～1000转/分，粉体粒径小于100目；
所述基片的尺寸为长10～500毫米，宽10～500毫米，厚0.01～5毫米；
所述基片在放入双温区管式炉的第二温区(3)之前用去离子水、乙醇反复清洗干净，光面朝上；
所述惰性气体为氮气、氩气中的一种以上，流速为1～1000mL/min。
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