CN115011923A - 一种高密度氮原子掺杂的二维单层共价网格结构及其制备方法 - Google Patents
一种高密度氮原子掺杂的二维单层共价网格结构及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种高密度氮原子掺杂的二维单层共价网格结构及其制备方法。在该方法中，通过在超高真空环境下利用“自下而上”的合成策略，将高纯度的前驱体分子蒸发沉积到干净的银单晶基底上，然后将样品退火处理，之后在样品表面获得了高密度氮原子掺杂的二维单层共价网格结构。此外，通过增加前驱体分子沉积的时间，可以获得不同覆盖度的高密度氮原子掺杂的二维单层共价网格。该方法为制备单层二维单层共价网格结构提供了新的思路，具有较高的科研价值和广泛的应用潜力。
Description
技术领域
本发明涉及纳米材料技术领域，具体地涉及一种在基底上预先沉积前驱体分子来合成的氮原子掺杂的二维单层共价网格结构。
背景技术
共价有机框架是一类由轻质元素（C原子）通过共价键连接的有机多孔晶态材料，是继金属有机框架材料之后又一重要的三维有序材料。共价有机框架具有其他传统多孔材料如分子筛、多孔聚合物、金属有机框架材料等无法比拟的优点，诸如低密度，高比表面积，易于修饰改性和功能化等，因此目前共价有机框架材料在气体的储存与分离、非均相催化、储能材料、光电、传感以及药物递送等领域已经有了广泛的研究并展现出优异的应用前景。共价有机框架的合成通常在溶剂热体系中进行，采用单一或混合溶剂以溶解部分单体，通过高温及低压条件下长时间反应获得共价有机框架的微晶聚集体，其间贯穿了包括聚合、结晶、组装等多个过程，因此很难获得均一可调的共价有机框架的材料。
异质原子掺杂是在原子水平上调控纳米结构光学和电子性能的有力手段。通过精确设计含有不同杂原子的前驱体，可以单独或联合地将杂原子掺杂到共价有机框架中。在众多的异质原子当中，氮原子由于其电子受体的特性极大的引起人们的研究兴趣。将氮原子引入共价有机框架中可以有效调控共价有机框架的电学性质，光电性质等。但是由于在溶液中合成的不可控性，很难得到高密度氮掺杂的共价有机框架。
表面合成已被证明是一种高效有效的方法来构建前所未有的纳米结构，包括共价有机框架的合成。利用金属衬底的催化活性，将特定的前驱体分子沉积在衬底表面可以合成清洁无污染的共价有机框架结构。通过优化前驱体分子的设计，可以将氮原子精确的引入共价有机框架当中，形成周期性的结构，对优化共价有机框架结构的电学，光学等性质起到非常关键的作用。
发明内容
本发明的目的是提供一种高密度氮原子掺杂的二维单层共价网格的制备方法。具体地，利用“自下而上”的合成策略，将含氮的前驱体分子沉积到衬底表面，在衬底上获得含有前驱体分子自组装结构的样品；将所述样品升温到特定生长温度后对所述样品进行退火处理，以获得高密度纳米尺寸的氮原子掺杂的二维单层共价网格样品。
本发明通过以下技术方案来实现的：在超高真空环境下，将含氮的前驱体分子蒸发25~30℃的干净的衬底表面，沉积时间为3~5分钟，从而在衬底表面制备得到原子级精确的高密度氮原子掺杂的共价有机框架结构。
优选地，本发明制备的具有原子级精确的高密度氮原子掺杂的共价有机框架结构还包括以下步骤：在前驱体分子沉积结束后，将衬底和沉积到衬底表面上的前驱体分子升温到生长温度，并保持一段时间，然后再将衬底和沉积到衬底表面上的前驱体分子降温至25~30℃的步骤。
优选地，所述生长温度为250~350℃，升温到生长温度后保持的时间为10~30分钟。该步骤在本发明中也被称为“退火处理”步骤。通过进行该步骤，可以使沉积的前驱体分子在衬底的催化作用下充分扩散形成二维规则有序的膜状结构，从而得到更高质量的具有高密度氮原子掺杂的共价有机框架结构。例如，可以将生长温度选择为300℃，从而能够获得较好甚至最优的制备效果。
优选地，所述“自下而上”合成策略是将一种小的前驱体分子经过基底催化作用发生化学反应生成大面积的单层二维结构。
优选地，所述将前驱体分子蒸发并沉积到衬底的步骤是通过热阻式加热使前驱体分子蒸发并沉积到所述衬底上。
优选地，所述增加沉积前驱体分子的时间从0分钟~5分钟可以有效增加的高密度氮原子掺杂的二维单层共价网格结构的面积。
在本发明的某些实施方案中，在190℃～200℃的蒸发温度下使所述前驱体分子蒸发。例如，在将蒸发温度选择为195℃的情况下，可以获得较好的沉积效果。
在本发明的某些实施方案中，所述衬底是通过包括以下步骤的方法制备的：a. 在超高真空腔内，对银单晶进行氩离子溅射处理以清洁衬底；b. 将所述衬底加热并保持在500℃，维持10-30分钟。
优选地，可以在超高真空腔内对衬底进行多次（例如，十几次）氩离子溅射处理，从而得到所述干净的衬底表面。
附图说明
以下，结合附图来详细说明本发明的实施方案，其中：
图1示出了根据本发明实施例的制备方法过程和效果的示意图；
图2示出了根据本发明实施例的具有的高密度氮原子掺杂的二维单层共价网格结构的扫描隧道显微镜图像；
图3示出了根据本发明实施例制备的前驱体分子自组织结构的扫描隧道显微镜图像；
图4示出了根据本发明实施例制备的有机金属配位的共价网络结构的扫描隧道显微镜图像；
图5示出了根据本发明实施例制备高密度氮原子掺杂的二维单层共价网格结构的扫描隧道显微镜图像和原子力显微镜图像；
具体实施方式
下面结合具体实施方式对本发明进行进一步详细的描述，给出的实施例仅为阐明本发明，而不是为了限制本发明的范围。
试验仪器和设备：
低温扫描隧道显微镜：购自德国Omicron公司。
K-cell分子蒸发源：购自德国Omicron公司。
氩离子枪：购自德国Omicron公司。
原料：
前驱体分子：四溴二苯并吡咯并吲哚并咔唑（化学法合成），纯度99.99%。
银单晶衬底：购自MaTecK，纯度99.999%。
实施例
银单晶衬底的制备：在超高真空腔内用氩离子枪对银单晶衬底进行氩离子溅射处理得到银衬底，并将银衬底加热并保持在500℃，维持20 分钟，获得干净平整的银单晶衬底。
具有高密度氮原子掺杂的二维单层共价网格结构的制备与调控：在制备完成银单晶化学法合成后，在超高真空环境下，利用热阻式K-cell分子蒸发源，在195℃的蒸发温度下，将前驱体分子四溴二苯并吡咯并吲哚并咔唑（缩写为：DipICz）蒸发到30℃的银单晶衬底的表面。前驱体分子的沉积时间为4分钟，在沉积过程中，将银单晶衬底和基底上的前驱体保持在30℃的生长温度，制备得到规律的前驱体分子的自组装岛。将银单晶衬底和衬底上的前驱体保持在130℃的生长温度，得到高密度氮原子掺杂的二维单层有机金属网格结构；随后将银单晶衬底和基底上的前驱体保持在200℃的生长温度，得到高密度氮原子掺杂的二维单层共价网格结构。
图1示出了根据本发明的实施例的制备方法，图2对应本发明的实施例的制备方法制备的具有高密度氮原子掺杂的二维单层共价网格结构可以通过扫描隧道显微镜来观察。
通过本发明的实施例的制备方法制备的前驱体分子在银衬底表面的自组装岛，高密度氮原子掺杂的有机金属配位的共价网络及高密度氮原子掺杂的共价有机网络结构的连贯结构。图3示出通过扫描隧道显微镜对前驱体分子沉积在银衬底表面的自组装图像，图像表明前驱体分子不同程度的脱溴原子；图4示出通过扫描隧道显微镜对高密度氮原子掺杂的有机金属配位的共价网络的观察结果，分子间通过银原子衔接，从图中可以测量出分子与分子之间的间距约为1.45± 0.05nm；图5示出通过扫描隧道显微镜（原子力显微镜）对高密度氮原子掺杂的共价有机网络结构的观察结果，连接分子的银原子消失并通过共价键连接，分子与分子之间的间距约为1.35± 0.05nm，成功合成了高密度氮原子掺杂的二维单层共价网格结构。
Claims (5)
1.一种高密度氮原子掺杂的二维单层共价网格结构的制备方法，其特征在于：利用“自下而上”的合成策略，将含氮的前驱体分子沉积到衬底表面，在衬底上获得含有前驱体分子自组装结构的样品；将所述样品升温到特定生长温度后对所述样品进行退火处理，以获得高密度的氮原子掺杂的二维单层共价网格样品。
2.根据权利要求1所述的高密度氮原子掺杂的二维单层共价网格结构的制备方法，其特征在于：所述前驱体分子的沉积温度为190℃~200℃。
3.根据权利要求1所述的高密度氮原子掺杂的二维单层共价网格结构的制备方法，其特征在于：所述前驱体分子的沉积时间为3分钟~5分钟。
4.根据权利要求1所述的高密度氮原子掺杂的二维单层共价网格结构的制备方法，其特征在于：所述的样品的生长温度为250~350℃。
5.根据权利要求1所述的高密度氮原子掺杂的二维单层共价网格结构的制备方法，其特征在于：所述的衬底为金衬底、银衬底和铜衬底。
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