CN108622866B - 一种化学湿法减薄黑磷的方法及其应用 - Google Patents
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Abstract
本发明提供一种化学湿法减薄黑磷的方法及其应用，包括以下步骤将片状黑磷浸入减薄溶液中于室温20‑25℃浸泡，所述减薄溶液的溶质为摩尔比为(1‑50)：(1‑50)的2,2,6,6‑四甲基哌啶氧化物和三苯基四氟硼酸碳，溶剂为二氯甲烷溶液，浸泡5min‑7h后，取出样品、洗涤干燥。本发明的有益效果是：使黑磷材料减薄，得到干净、完整的晶体表面，还可以起到平整黑磷材料的作用，操作步骤简单，无苛刻条件，可实现产业化。
Description
技术领域
本发明属于光电技术领域，尤其是涉及一种化学湿法减薄黑磷的方法及其应用。
背景技术
二维材料，例如石墨烯，黑磷，过渡金属硫化物，由于其特殊性质和在纳米电子中的潜在应用受到极大的关注。其中，石墨烯，二硫化钼，黑磷作为代表性的二维材料已经在柔性电子，光电探测器，电催化，气体传感等应用领域被广泛研究。二维材料的性质与应用起到了很大程度上取决于二维材料的厚度。
例如随着黑磷的减薄，其带隙从0.3eV增大到2.0eV。其载流子迁移率也和厚度有关。目前可以用等离子体或者原子力显微镜减薄，但是需要价格昂贵的大型仪器，成本很高，减薄速率不易控制，操作复杂，尤其是不能用于溶液中大规模减薄黑磷，原子力显微镜减薄速率就更低了，不适用于产业化。尽管二维材料领域发展迅速，但是制备高效、高质量、厚度可控的二维材料仍然是一个重大挑战。因此，在已知黑磷具有广阔应用前景的基础下，亟待开发一种大规模减薄黑磷来制备薄层甚至单层黑磷的方法
发明内容
为了克服以上减薄黑磷方法的弊端，本发明的目的在于：提供一种操作简单、应用广泛的通过化学湿法刻蚀来制备薄层或单层黑磷的方法。
本发明的技术方案是：本发明的一种化学湿法减薄黑磷的方法，包括以下步骤：
将片状黑磷浸入减薄溶液中于室温20-25℃浸泡，所述减薄溶液的溶质为摩尔比为(1-50)：(1-50)的2,2,6,6-四甲基哌啶氧化物和三苯基四氟硼酸碳，溶剂为二氯甲烷溶液，浸泡5min-7h后，取出样品、洗涤干燥。
优选的，所述片状黑磷由块状黑磷通过机械剥离或超声、机械搅拌的方式分解而成。
优选的，所述浸泡时间为30-100min。
优选的，所述洗涤溶剂为二氯甲烷或异丙醇。
优选的，所述干燥作业采用氮气枪吹扫完成。
优选的，所述减薄溶液为等摩尔比的2,2,6,6-四甲基哌啶氧化物和三苯基四氟硼酸碳的二氯甲烷溶液。
优选的，所述减薄溶液的溶质为10mmol的2,2,6,6-四甲基哌啶氧化物和10mmol的三苯基四氟硼酸碳，所述减薄溶液的溶剂为2mL二氯甲烷。
本发明的另一方面，还包括化学湿法减薄黑磷的方法在制备晶体管上的应用，所述晶体管的开关比为106，亚阈值摆幅为450mV/decade，源漏电压差在-40mV-40mV范围内，源漏电流随源漏电压成线性变化，且高度对称。
本发明的另一方面，还包括一种减薄溶液在减薄黑磷上的应用，所述减薄溶液的溶质为摩尔比为(1-50)：(1-50)的2,2,6,6-四甲基哌啶氧化物和三苯基四氟硼酸碳，溶剂为二氯甲烷溶液。
优选的，减薄溶液的溶质为等摩尔比的2,2,6,6-四甲基哌啶氧化物和三苯基四氟硼酸碳。
优选的，所述减薄溶液的溶质为10mmol的2,2,6,6-四甲基哌啶氧化物和10mmol的三苯基四氟硼酸碳，所述减薄溶液的溶剂为2mL二氯甲烷。
本发明具有的优点和积极效果是：
1、本发明除了使黑磷材料减薄，得到干净、完整的晶体表面，还可以起到平整黑磷材料的作用，从而可能实现产业化。
2、该方法操作流程简单，工艺成本低廉，无需价格昂贵的大型仪器，无需在无水无氧条件下操作，无需专业人员即可完成流程。
3、可以在很短时间内对大批量黑磷同时减薄。
附图说明
图1是实施例1黑磷的光学显微镜图(光学显微镜采用高分辨透射电子显微镜Tecnai G2 F20(FEI,USA))，其中图1a是通过机械剥离方法将片状黑磷转移到了Si/SiO2基底上，减薄前的光学显微镜图。图1b是化学湿法减薄2h后得到的黑磷的光学显微镜图。
图2是实施例2化学湿法减薄过程中得到的黑磷的原子力显微镜图(原子力显微镜采用Dimension Icon(Bruker,German))。其中图2a是机械剥离制得的片状黑磷材料的原子力显微镜图，图2b是化学湿法减薄5min后的原子力显微镜图。图2c是化学湿法减薄10min后的原子力显微镜图。其厚度变化为0min，5.78nm(2a)；5min，4.75nm(2b)；10min，2.22nm(2c)。
图3是实施例1化学湿法减薄后得到的黑磷的透射电子显微镜图。
图4是实施例1化学湿法减薄后得到的黑磷的选取电子衍射图。
图5是实施例1化学湿法减薄过程中减薄不同时间得到的黑磷的拉曼光谱图。
图6是实施例2黑磷浸泡前(a)和浸泡30分钟后(b)的原子力显微镜扫描图。
图7是场效应晶体管测试示意图。
图例如下：
1-漏电极Cr/Pd，2-源电极Cr/Pd，3-用四甲基哌啶氮氧化物和三苯基碳四氟硼酸盐溶液减薄的薄层黑磷，4-热氧化的二氧化硅，5-硅衬底，6-半导体分析仪(B1500)
图8是晶体管的输运曲线。
图9是晶体管的输出特性曲线。栅极电压分别设置为-7V(a)、-8V(b)、-9V(c)、-10V(d)。
具体实施方式
下面结合附图对本发明做详细说明。
2,2,6,6-四甲基哌啶氧化物购买于天津希恩思生化科技有限公司，三苯基四氟硼酸碳购买于梯希爱(上海)化成工业发展有限公司。
作为一个实施例，以化学湿法减薄黑磷为例加以说明：
实施例1
(1)将少量块状黑磷置于蓝光胶带上，折叠胶带若干次，通过聚二甲基硅氧烷，将片状黑磷转移到Si/SiO2基底上，光学显微镜图如图1a所示，原子力显微镜图如图2a所示。
(2)在棕色瓶中加入2,2,6,6-四甲基哌啶氧化物(3.1mg,2mmol),三苯基四氟硼酸碳(6.6mg,2mmol)和2mL二氯甲烷，震荡使其溶解。将上述方法得到的片状黑磷浸入溶剂瓶中，于室温浸泡。
(3)用镊子夹出基底，经二氯甲烷、异丙醇洗涤、氮气枪吹干得到尺寸在几个纳米到几百微米，厚度在1nm-30nm的薄层黑磷材料。
当步骤(2)中的室温浸泡时间(减薄时间)为5min，测其原子力显微镜图，如图2b所示，片状黑磷的厚度为4.75nm；
当步骤(2)中的室温浸泡时间(减薄时间)为10min，测其原子力显微镜图，如图2c所示，片状黑磷的厚度为2.22nm。
当步骤(2)室温浸泡时间(减薄时间)为2h时，得到的黑磷的光学显微镜图如图1b所示。
实施例1中得到的黑磷的透射电子显微镜图如图3所示，可见晶格完整，得到的黑磷的选取电子衍射图如图4所示，由此可见黑磷的结构并未发生变化。
对实施例1中减薄时间分别为0min、10min、20min、30min、40min、50min、60min、70min、80min、90min、100min的样品进行拉曼光谱的检测，得到如图5，由此可见，减薄时间越长，拉曼强度越小，黑磷的厚度越薄。
实施例2
(1)将少量块状黑磷置于蓝光胶带上，折叠胶带若干次，通过聚二甲基硅氧烷，将片状黑磷转移到Si/SiO2基底上。
(2)在棕色瓶中加入2,2,6,6-四甲基哌啶氧化物(15.5mg,10mmol),三苯基四氟硼酸碳(33.0mg,10mmol)和2mL二氯甲烷，震荡使其溶解。将上述方法得到的片状黑磷浸入溶剂瓶中，于室温浸泡30分钟。
(3)用镊子夹出基底，经二氯甲烷、异丙醇洗涤、氮气枪吹干得到厚度为2.7nm的薄层黑磷材料。
黑磷浸泡前的原子力显微镜扫描图如图6a所示，厚度为10.8nm，浸泡30分钟后样品的原子力显微镜扫描图如图6b所示，厚度为2.7nm。
实施例3
由实施例1或实施例2减薄的黑磷，制备晶体管，制得的晶体管的结构如图7所示，包括设置在最底层的硅衬底5，硅衬底5的顶端设有热氧化的二氧化硅4，热氧化的二氧化硅4的顶端设有用上述湿法减薄方法减薄的薄层黑磷3，所述薄层黑磷3的左右两侧分别设有漏电极1Cr/Pd(5nm/50nm)和源电极2Cr/Pd(5nm/50nm)。
将上述晶体管半导体放在分析仪载物台进行测试，将源电压Vd设为20mV，漏电压Vs设为0mV，源漏电压差Vds为20mV，栅极电压Vg设置为从-10V到10V，测试得到图8所示的源漏电流随栅极电压变化曲线，开关比(最大源漏电流除以最小源漏电流)为106，亚阈值摆幅(电流每下降一个数量级，电压的变化)为450mV/decade，由图可知栅极电压从-10V到-8V，在小范围内就可实现本装置的场效应晶体管可迅速开关，灵敏度高。
图9为源漏电流随源漏电压变化曲线，将栅极电压Vg分别设置为-7V、-8V、-9V、-10V，由图可看出源漏电压差Vds在-40mV-40mV范围内，源漏电流随源漏电压成线性变化，且高度对称，说明在负电压条件下为欧姆接触。
以上对本发明的一个实施例进行了详细说明，但所述内容仅为本发明的较佳实施例，不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等，均应仍归属于本发明的专利涵盖范围之内。
Claims (10)
1.化学湿法减薄黑磷的方法，其特征在于：包括以下步骤：将片状黑磷浸入减薄溶液中于室温20-25℃浸泡，所述减薄溶液的溶质为摩尔比为(1-50)：(1-50)的2,2,6,6-四甲基哌啶氧化物和三苯基四氟硼酸碳，溶剂为二氯甲烷溶液，浸泡5min-7h后，取出样品、洗涤干燥。
2.根据权利要求1所述的化学湿法减薄黑磷的方法，其特征在于：所述片状黑磷由块状黑磷通过机械剥离或超声、机械搅拌的方式分解而成。
3.根据权利要求1所述的化学湿法减薄黑磷的方法，其特征在于：所述浸泡时间为30-100min。
4.根据权利要求1所述的化学湿法减薄黑磷的方法，其特征在于：所述洗涤溶剂为二氯甲烷或异丙醇。
5.根据权利要求1所述的化学湿法减薄黑磷的方法，其特征在于：所述干燥作业采用氮气枪吹扫完成。
6.根据权利要求1所述的化学湿法减薄黑磷的方法，其特征在于：所述减薄溶液为等摩尔比的2,2,6,6-四甲基哌啶氧化物和三苯基四氟硼酸碳的二氯甲烷溶液。
7.根据权利要求1所述的化学湿法减薄黑磷的方法，其特征在于：所述减薄溶液的溶质为10mmol的2,2,6,6-四甲基哌啶氧化物和10mmol的三苯基四氟硼酸碳，所述减薄溶液的溶剂为2mL二氯甲烷。
8.如权利要求1-7中任一项的减薄黑磷的方法在制备晶体管上的应用，其特征在于：制得的晶体管的开关比为106，亚阈值摆幅为450mV/decade，源漏电压差在-40mV-40mV范围内，源漏电流随源漏电压成线性变化，且高度对称。
9.一种减薄溶液在减薄黑磷上的应用，其特征在于：所述减薄溶液的溶质为摩尔比为(1-50)：(1-50)的2,2,6,6-四甲基哌啶氧化物和三苯基四氟硼酸碳，溶剂为二氯甲烷溶液。
10.根据权利要求9所述的一种减薄溶液在减薄黑磷上的应用，其特征在于：减薄溶液的溶质为等摩尔比的2,2,6,6-四甲基哌啶氧化物和三苯基四氟硼酸碳。
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