CN108914188A - 纳米管阵列/纳米丝复合结构、制备方法、量子点敏化复合结构及应用 - Google Patents
纳米管阵列/纳米丝复合结构、制备方法、量子点敏化复合结构及应用 Download PDFInfo
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Abstract
本发明涉及纳米材料领域，具体涉及纳米管阵列/纳米丝复合结构、制备方法、量子点敏化复合结构及应用。该方法制备的TiO2纳米管阵列/纳米丝复合结构的光电流密度比单一的TiO2纳米管提高了8倍；量子点敏化后的CdSe/CdS/TiO2 NWs/NTs（CdSe/CdS量子点共敏化的TiO2纳米管阵列/纳米丝复合结构）的光电流密度比TiO2 NWs/NTs提高了15倍，比普通的TiO2 NTs提高了27倍；此外，该样品在120 min内光降解亚甲基蓝的降解率达99.77%，5次重复使用后的降解率仍保持97.84%。因此，在太阳能电池与光催化降解有机污染物等领域具有巨大的应用前景。
Description
技术领域
本发明涉及纳米材料领域，具体涉及纳米管阵列/纳米丝复合结构、制备方法、量子点 敏化复合结构及应用。
背景技术
TiO2纳米材料因其良好的光稳定性、低毒性、以及相对较低的价格被大量地应用于光电 领域以及环境保护领域，使其成为光电、光催化领域的研究热点。
目前，TiO2的形貌结构主要包括了TiO2纳米颗粒、纳米管、纳米球、纳米棒及纳米线等结构。其中，通过阳极氧化法制备的TiO2纳米管(NTs)表现出高度有序排列的阵列结构，具有较高的电子传输效率，而且TiO2NTs容易制成大面积的二维薄膜材料以满足光电/光催化领域对材料大尺寸及回收利用的需求，因此被认为是最有前途的TiO2结构之一。
近三十年来，相关报道层出不穷。然而，纳米管阵列仍有诸多不足，主要是因为：一方 面是纳米管结构有效比表面积较小，因而对光的吸收面积较小；另一方面，单一TiO2NTs因其自身禁带宽度(3.2eV，anatase)较宽，只能吸收波长较短的紫外光，仅有不到5％的 太阳光可以被其利用，这大大限制了其在光电化学方面的应用。解决的办法，通常是在TiO2NTs表面沉积窄禁带宽度的量子点来提高其对光的响应范围。例如专利CN101956222A公开了硫化镉纳米颗粒敏化的二氧化钛纳米管阵列的制备方法，具体步骤为：将基底材料表 面进行预处理；以含0.25～1.0wt％NH4F的丙三醇和水的混合溶液为电解液，铂金属为对电 极，控制电压为10～30V，对基底进行电化学阳极氧化，在基底表面构筑一层TiO2纳米管 阵列膜；将膜层热处理，得到锐钛矿TiO2纳米管阵列膜；将所得的锐钛矿TiO2纳米管阵列膜在S浓度为0.01～0.05M、Cd/S浓度比为1∶(1～4)的DMSO电解液中沉积，取出样品干 燥，即得到硫化镉纳米颗粒敏化的二氧化钛纳米管阵列。
采用此方法时，在沉积量子点时，TiO2NTs管口容易发生堆积堵塞孔隙，不利于光的吸 收与电子的传输利用；此外，负载了量子点之后，与基底不易形成稳定的异质结构，容易脱 落。
发明内容
为解决上述问题本发明提供一种纳米管阵列/纳米丝复合结构的制备方法，该方法制备 的纳米管阵列/纳米丝复合结构具有更大的光吸收面积及量子点有效负载面积、可改善量子 点负载质量、提高光电转化效率。
纳米管阵列/纳米丝复合结构的制备方法，包括以下步骤：
(1)预处理：将Ti基底材料进行表面预处理；
(2)阳极氧化：以含0.1～0.8wt％的氟化氨的乙二醇/水体系为电解液，铂为阴极，Ti 基底材料为阳极，控制电压为40～70V，对基底材料进行4～7h的阳极氧化处理。
(3)热处理：对经过电化学阳极氧化处理后的基底材料进行热处理，即得到纳米管阵 列/纳米丝复合结构。
本发明通过对电解液浓度配比、电解电压和电解时间的调节，使得在纳米管阵列的表面 撕裂形成螺旋状且规则排列于管口的纳米结构，进而形成纳米管阵列/纳米丝复合结构。
优选的，所述电解液中乙二醇和水的体积比为90～98:2～10。
优选的，所述电解液中氟化铵的含量为0.3～0.5wt％。
优选的，所述电压为50～70V，对基底材料进行阳极氧化的时间为4～6h。
优选的，所述电解液中氟化铵的含量为0.3％，乙二醇和水的体积比为98:2。
优选的，所述表面预处理是对基体材料表面进行打磨、清洗和抛光，所述抛光是指将经 过打磨和清洗的Ti基底材料置于抛光液中抛光处理，所述抛光液是氟化氢、硝酸和水按体 积比1:4:10混合配制而成的。
优选的，步骤(3)中的热处理是指将经过阳极氧化处理后的基底材料于大气气氛下高 温处理，温度为500℃，升温速率为5℃min-1，保温3h。
优选的，所述步骤(2)和步骤(3)之间还经清洗步骤，清洗步骤是指将经过阳极氧化 处理的基体材料依次采用乙醇和去离子水清洗。
由上述制备方法制备的纳米管阵列/纳米丝复合结构也属于本发明保护范围。
上述的纳米管阵列/纳米丝复合结构在通过非金属元素掺杂、有机染料或过渡金属硫族 化合物进行敏化、沉积贵金属颗粒等方法制备表面修饰的纳米管阵列/纳米丝复合结构中的 应用也属于本发明的保护范围。
本发明制备的纳米管阵列/纳米丝复合结构适合于非金属元素掺杂、有机染料或过渡金 属硫族化合物进行敏化、沉积贵金属颗粒等方法对其进行表面改性。
本发明还提供一种量子点敏化复合结构，其特征在于，所述量子点敏化复合结构是量子 点敏化的纳米管阵列/纳米丝复合结构。
优选的，所述量子点敏化的纳米管阵列/纳米丝复合结构是以纳米管阵列/纳米丝复合结 构为基底，沉积法制备的量子点敏化的纳米管阵列/纳米丝复合结构。
上述沉积法是电化学沉积法、化学浴沉积法和/或连续离子层吸附法。
优选的，所述量子点是CdSe量子点、CdS量子点和Cu2O量子点中的一种或多种。
上述制备方法、由上述制备方法制备的纳米管阵列/纳米丝复合结构和/或上述量子点敏 化复合结构在太阳能电池与光催化降解有机污染物等领域的应用也属于本发明的保护范围。
本发明利用阳极氧化法在Ti片表面制得结构高度有序的TiO2纳米管阵列膜层，通过控 制反应条件等措施，使表层TiO2纳米管发生撕裂，形成螺旋状规则排列于管口的纳米丝复 合结构；与单一的TiO2纳米管阵列相比，本发明的TiO2纳米管/丝复合结构具有更大的比表 面积，为稳定负载量子点提供了更大的位置空间，量子点沉积于管内，可提高光在管内的折 射率，从而提高光的利用效率；纳米丝与下端垂直规则排列的TiO2纳米管生长在一起，有 利于电子的传输转移；该样品易于实现大面积的制备，容易满足光催化/光电应用对大尺寸、 重复利用的要求。所制备的TiO2纳米丝/纳米管阵列薄膜的光电流密度比单一的TiO2纳米管 提高了8倍；量子点敏化后的CdSe/CdS/TiO2NWs/NTs(CdSe/CdS量子点共敏化的TiO2纳 米丝/纳米管阵列薄膜)的光电流密度比CdSe/TiO2NTs(TiO2纳米丝/纳米管阵列薄膜)提 高了15倍，比普通的TiO2NTs提高了27倍。
与现有技术相比，本发明具有如下优点：本发明构筑了TiO2纳米管阵列/纳米丝复合结 构具有巨大的比表面积，能够保证充分的量子点负载量；本结构中TiO2丝是由纳米管裂解 而成，丝/管相连，保证了光电子在复合结构中的传输效率，减少了电子空穴复合率；量子 点沉积于管内及丝的表面，提高了光的散射能力，可以有效增强光阳极薄膜的光捕获能力。 该制备工艺绿色环保、简单方便、过程可控，所制备的CdSe/CdS/TiO2NWs/NTs样品量子点 有均匀负载，具有良好的光电效应和光催化效果，并且可以大面积成膜，具有市场发展前景。
附图说明
图1为实施例1、实施例2、实施例4所得样品的X射线衍射(XRD)图；
图2为对比例1制备的TiO2纳米管阵列的场发射扫描电镜图(FESEM)；
图3为实施例1制得的TiO2NWs/NTs的场发射扫描电镜图(FESEM)；
图4为实施例1制得的TiO2NWs/NTs高倍扫描电镜形貌图；
图5为实施例4制得的先后沉积CdS、CdSe量子点于TiO2NWs/NTs后所得样品的FESEM图；
图6为实施例4制得的CdSe/CdS/TiO2NWs/NTs样品量子点沉积管内断面的形貌图；
图7为实施例1、实施例2、实施例4、对比例1所得样品的光电转换测试电流-时间(current–time)响应图；
图8为实施例1、实施例2、实施例4、对比例1所得样品的光催化降解亚甲基蓝效率图；
图9为实施例4所得样品光催化降解亚甲基蓝的重复降解效率图。
具体实施方式
以下结合附图和实施例对本发明进行进一步的说明。
本发明所述的TiO2NWs/NTs是指TiO2二氧化钛纳米管阵列/纳米丝复合结构，本发明 中所用试剂和材料无特殊说明均可通过商业途径购买获得。
对比例1
一种制备TiO2NTs阵列结构的方法，其特征在于，包括如下步骤：
(1)将Ti片裁剪成3cm×3cm×0.01cm，分别用丙酮、乙醇、去离子水对裁剪好的Ti片超声清洗10min，在干燥箱内烘干。将清洗后Ti片置于酸性抛光液(HF:HNO3:H2O＝1:4:10)中进行抛光处理40s，然后将Ti片置于乙醇和去离子水中分别超声清洗10min，再烘干待用，随后利用直流稳压电源对Ti片进行阳极氧化处理，以Ti片作为工作电极(阳极)， Pt片电极作为阴极，选择含体积分数为1.3v/v％HF的水溶液作为电解液，整个阳极氧化过 程在电压20V下持续20min。电解结束后取出样品，分别用乙醇和去离子水冲洗数次后烘 干，随即置于管式炉内，以5℃/min升温速率加热至500℃，保温过程持续1h，得到形貌排 列均匀的锐钛矿晶型的TiO2纳米管阵列。
实施例1
一种原位制备TiO2NWs/NTs复合结构的方法，其特征在于，包括如下步骤：
(1)制备TiO2NWs/NTs。将裁剪好的Ti片(3cm×3cm×0.01cm)分别在丙酮、乙醇、去离子水中超声清洗10min后烘干。将洗净Ti片置于抛光液(HF:HNO3:H2O＝1:4:10)中抛 光处理40s，分别在乙醇和去离子水超声10min，随后利用直流稳压电源对Ti片进行阳极 氧化处理，以Ti片作为工作电极(阳极)，Pt片电极作为阴极，电解液为含0.3wt％NH4F +2vol％H2O的120mL乙二醇溶液，整个阳极氧化过程在电压55V下持续5h。电解结束 后，样品分别用乙醇和去离子水冲洗数次后烘干，之后置于管式炉中，以5℃/min升温速率 加热至500℃，保温过程持续3h，得到形貌优良的TiO2NWs/NTs。
实施例2
CdS量子点敏化的TiO2NWs/NTs(CdS/TiO2NWs/NTs)结构的制备方法，其特征在于，包括如下步骤：
(1)TiO2NWs/NTs的制备方法同实施例1步骤(1)相同。
(2)采用连续离子层吸附与反应(SILAR)化学浴沉淀法，将步骤(1)所得的TiO2NWs/NTs样品正面沉浸于含有0.1mol·L-1CdCl2的乙醇溶液中，沉浸时间为5min，随后取 出样品用乙醇冲洗5次后烘干；随后将样品在0.1mol·L-1Na2S的甲醇溶液中，沉浸5min， 取出样品并甲醇冲洗5次后烘干；最后将样品置于真空环境中在350℃保温1h，制得经过一 个沉积过程的样品CdS(1cycle)/TiO2NWs/NTs。沉积过程还可以重复循环多次，通常做3～5 次沉积循环。
实施例3
CdSe量子点敏化TiO2NWs/NTs(CdSe/TiO2NWs/NTs)结构的制备方法，其特征在于，包括如下步骤：
(1)TiO2NWs/NTs的制备步骤同实施例1步骤(1)相同。
(2)将步骤(1)所得样品TiO2NWs/NTs为工作电极，在CHI 760E电化学工作站进 行电化学沉积，电解液由(10mmol CdCl2+0.2mmol SeO2+2mmol Na2SO4)溶于120mL 去离子水中组成，Pt片为对电极，甘汞电极为参比电极，施加电压-0.7V，沉积时间10-40 min。沉积完成后，将样品分别用去离子水和酒精冲洗5次，60℃烘干后，置于真空环境中 进行高温处理，温度为350℃，保温时间1h，随炉冷却即得样品CdSe/TiO2NWs/NTs。
实施例4
CdSe、CdS共敏化TiO2NWs/NTs(CdSe/CdS/TiO2NWs/NTs)结构的制备，其特征在 于，包括如下步骤：
(1)TiO2NWs/NTs的制备步骤同实施例1步骤(1)相同。
(2)以步骤(1)所得样品TiO2NWs/NTs为基底，制备CdS量子点敏化的TiO2 NWs/NTs的复合结构CdS/TiO2NWs/NTs，制备方法同实施例2中步骤(2)；
(3)将步骤(2)所得样品为工作电极，采用实施例(3)步骤(2)相同处理方法，制 得共敏化的样品CdSe/CdS/TiO2NWs/NTs。
实施例5
Cu2O量子点敏化TiO2NWs/NTs(Cu2O/TiO2NWs/NTs)结构的制备，其特征在于，包 括如下步骤：
(1)TiO2NWs/NTs的制备步骤同实施例1步骤(1)相同。
(2)将步骤(1)所得样品为工作电极，在CHI 760E电化学工作站进行电化学沉积，电解液是120ml的乳酸铜络合物溶液(由0.4mol·L-1CuSO4和3mol·L-1C3H6O3组成，并用mol·L-1NaOH调节溶液pH值为10)，Pt为对电极，饱和甘汞电极作参比电极，在-0.4V的 电压下，恒温60℃的水浴中电化学沉积，沉积时间10-40min，结束后分别用乙醇和去离子 水冲洗3次，在空气中自然晾干。制得样品Cu2O/TiO2NWs/NTs。
实施例6
(1)对对比例1、实施例1、实施例2和实施例3样品进行物相和形貌测试
通过X衍射测试对比例1、实施例1、实施例4中制备样品，结果如图1所示，由图可知除了典型的锐钛矿TiO2和Ti基底的衍射峰外，在25.3°,29.3°处的衍射峰分别对应于为CdSe闪锌矿六方相，及在43.9°处的衍射峰对应CdS的(220)晶面，表面已成功制备 CdSe/CdS/TiO2NWs/NTs样品。通过场发射扫面电镜测试实施例1、实施例2、实施例3、实 施例5样品，结果如图2-6所示。图2为采用常用方法制备的普通TiO2纳米管阵列，管内径 约50～70nm、管壁厚10～20nm；图3为本发明提供的TiO2纳米/纳米管阵列复合结构，表 面包含了大量的纳米丝(NWs)，NWs的长度平均为15μm，直径为10nm，在NWs下面则为 规则排列的NTs，NTs直径约为80nm，管内壁厚度约为10nm，同时在管的内壁还有许多 小孔，这也为量子点的负载提供了更多的场所(如图4所示)。图5为实施例5中样品量子 点沉积于TiO2NWs/NTs表面的形貌图，可见细小均匀的量子点附着于纳米丝的表面，增大 了量子点的负载量。图6为实施例4中样品量子点沉积于纳米管内的断面图，可见纳米管排 列垂直均匀，这有利于光生电子沿管的内壁快速转移；同时，量子点均匀的附着纳米管的内 壁，并没有在管内形成堵塞，这有利于进入管内的太阳光通过内壁的量子点形成折射，提高 光的利用率。
(2)对实施例1、实施例2、实施例4、对比例1样品进行光电响应测试
将所述实施例中所得样品进行光电流测试，以0.5mol·L-1的硫酸钠溶液为测试溶液，用 300W的氙灯作为光源，每20s打开/屏蔽光源一次，测试样品随时间变化的光电流变化(i-t 数据)，结果如图7所示。由图可见，所制备的TiO2NWs/NTs复合结构的光电流密度比单 一的TiO2NTs提高了8倍；CdSe、CdS量子点共敏化后的CdSe/CdS/TiO2NWs/NTs的光电 流密度比NWs/NTs复合结构提高了15倍，比普通的TiO2NTs提高了27倍，表明本发明的TiO2NWs/NTs复合结构具有很好的量子点负载效果及较高的光电转化效率。
(3)对实施例1、实施例2、实施例4、对比例1样品进行光催化测试
将所述实施例中所得样品进行，测试条件为以10mg·L-1的甲基橙溶液为模拟污染物， 在模拟可见光照射下，每20min取样一次，通过测试UV-vis光谱(λMB＝663nm)的强度反映 在不同光照时间后溶液中残留甲基橙的浓度，以反映样品的光催化降解能力。图8为几个样 品进行光催化降解亚甲基蓝实验效果对比，在经过120min模拟太阳光照射后，纯的TiO2 NTs的降解率不足20％，而TiO2NWs/NTs降解率可达51.80％，通过CdS QDs单独敏化的CdS/TiO2NWs/NTs光催化降解率达到96.50％，而CdSe QDs与CdS QDs共敏化的TiO2 NWs/NTs的光催化降解率可达到99.77％，几乎完全降解亚甲基蓝。左下角插图为 CdSe/CdS/TiO2NWs/NTs光降解亚甲基蓝时剩余污染物浓度的UV-vis光谱图。从该图可以 看出，亚甲基蓝的光吸收强度随随着时间的推移在不断降低，并且在120min处吸收峰接近 0，这表明污染物几乎被催化完全。
样品的重复降解率是衡量其光催化应用的重要标志。参见图9可见，CdSe/CdS/TiO2 NWs/NTs样品在光降解亚甲基蓝重复5次后，其降解效果依旧能达到97.84％，保持较高的 重复降解效率，表面本发明所得样品具有很强的实际应用价值。
Claims (10)
1.纳米管阵列/纳米丝复合结构的制备方法，包括以下步骤：
(1)预处理：将Ti基底材料进行表面预处理；
(2)阳极氧化：以含0.1～0.8wt％的氟化氨的乙二醇/水体系为电解液，铂为阴极，Ti基底材料为阳极，控制电压为40～70V，对基底材料进行4～7h的阳极氧化处理。
(3)热处理：对经过电化学阳极氧化处理后的基底材料进行热处理，即得到纳米管阵列/纳米丝复合结构。
2.如权利要求1所述的制备方法，其特征在于，所述电解液中乙二醇和水的体积比为90～98:2～10。
3.如权利要求2所述的制备方法，其特征在于，所述电解液中氟化铵的含量为0.3～0.5wt％。
4.如权利要求1所述的制备方法，其特征在于，所述电压为50～70V，对基底材料进行阳极氧化的时间为4～7h。
5.如权利要求1所述的制备方法，其特征在于，所述表面预处理是对基体材料表面进行打磨、清洗和抛光，所述抛光是指将经过打磨和清洗的Ti基底材料置于抛光液中抛光处理，所述抛光液是氟化氢、硝酸和水按体积比1:4:10混合配制而成的。
6.如权利要求1～5任一项所述的制备方法，其特征在于，步骤(3)中的热处理是指将经过阳极氧化处理后的基底材料于大气气氛下高温处理，温度为500℃，升温速率为5℃min-1，保温3h。优选的，如权利要求1～5任一项所述的制备方法，其特征在于，所述步骤(2)和步骤(3)之间还经清洗步骤，清洗步骤是指将经过阳极氧化处理的基体材料依次采用乙醇和去离子水清洗。
7.权利要求1～6任一项所述的制备方法制备的纳米管阵列/纳米丝复合结构。
8.权利要求7所述的纳米管阵列/纳米丝复合结构在通过非金属元素掺杂、有机染料或过渡金属硫族化合物进行敏化、沉积贵金属颗粒等方法制备表面修饰的纳米管阵列/纳米丝复合结构中的应用。
9.一种量子点敏化复合结构，其特征在于，所述量子点敏化复合结构是量子点敏化的纳米管阵列/纳米丝复合结构。优选的，所述量子点敏化的纳米管阵列/纳米丝复合结构是以纳米管阵列/纳米丝复合结构为基底，沉积法制备的量子点敏化的纳米管阵列/纳米丝复合结构。优选的，所述量子点是CdSe量子点、CdS量子点和Cu2O量子点中的一种或多种。
10.权利要求1～6任一项所述的制备方法、权利要求7所述的纳米管阵列/纳米丝复合结构和/或权利要求8或9所述的量子点敏化复合结构在太阳能电池与光催化降解有机污染物方面的应用。
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