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    宁波材料所在MAX相单原子层元素精准调控方面取得进展

    2019-09-30 宁波材料技术与工程研究所
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      MAX相,一类具有六方晶格结构的纳米层状过渡金属化合物,分子式为Mn+1AXn,(其中M为前过渡族金属,A主要为ⅢA和ⅣA族元素,X为碳或/和氮,n=1-3)。MAX相材料的晶体呈六方对称性,空间群为P63/mmc,由Mn+1Xn单元与A原子层交替堆垛而成,目前已报道的MAX相约有150余种。MAX相材料兼具金属和陶瓷的性质,如良好的导电导热性、优异的抗热震性和损伤容限、良好的抗氧化性和耐腐蚀性以及易加工等特性,在高温电极、摩擦磨损等领域作为高安全结构材料有着广阔的应用前景。因此,目前对于结构与功能一体化的新型MAX相材料创制已经成为国际上该领域的前沿问题。近期,中国科学院宁波材料技术与工程研究所先进能源材料工程实验室通过A位元素置换策略,合成了一系列A位为Zn的MAX相(J. Am. Chem. Soc. 2019, 141, 4730-4737),揭示了后过渡族金属在MAX相单原子A层存在的可行性。Cu元素与Zn等后过渡金属元素一样,最外层d轨道电子尚未填满,可以预测Cu的引入可以使传统MAX相结构材料具有更多d电子相关的功能性,如催化、生物标记、传感等。然而迄今为止还没有有效的合成方法实现Cu原子在MAX相材料A位单原子层间的精确控制。

      宁波材料所先进能源材料工程实验室利用“A-Site-Replacement Reaction”策略,研究发现Cu原子在Ti3AlC2 MAX相A位单原子二维平面内显示出一定程度的有序排列,并通过Cu-Al二元相图对其形成机制进行了讨论。理论分析表明Cu原子在A位层间与Ti3C2亚层结合较弱,但被高电导的Ti3C2亚层有效隔离,因此可望在单原子催化中发挥作用。实验表明,这种Cu原子占位的MAX相可通过催化双氧水分解氧化3,3',5,5'-四甲基联苯胺(TMB)形成蓝色溶液,体现出优异的类酶催化活性,且在高温下仍然保持催化活性和催化稳定性。实验室和宁波大学等团队合作将该类酶催化特性的新型MAX相材料组装为电化学生物传感器。相比传统的Cu、Au、Pt、Ag等纳米颗粒,该MAX相传感器在检测H2O2上具有线性范围宽、检测极限低(0.06μM)和灵敏度高的优点,在食品安全、肿瘤治疗等领域有很好的应用前景。

      相比于上述Ti3(AlxCu1-x)C2 MAX相A位Cu的部分置换,如何制备得到A位为纯Cu的新型MAX相材料则是一个更为严峻的挑战,世界上迄今为止还没有合成出这类MAX相材料。从Cu-Al平衡相图来预测,MAX相中的Al原子应该无法完全被Cu原子置换,然而考虑到A位单原子实际上还受到MX层的二维空间限域作用影响,元素置换反应还有丰富的可调谐性。先进能源材料工程实验室通过选取Ti2AlN作为MAX相前驱体实现了高比率Cu置换的新型MAX相Ti2(Al0.1Cu0.9)N,在其后使用Nb2AlC作为MAX相先驱体材料最终成功制备出A位完全Cu置换的MAX相Nb2CuC。以上工作不仅显示出A位元素置换策略在MAX相新材料创制上的有效性,并且体现了MAX相丰富的结构可能性和功能拓展性。

      以上工作发表在国际材料期刊ACS Nano(2019, 13, 9198-9205)和Materials Research Letters(DOI:10.1080/21663831.2019.1672822)上,申请中国发明专利1项(CN201810751944.0)。该项研究得到国家自然科学基金(21671195, 21805295, 21875271)的资助。

    图1 扫描透射电子显微技术结构和成分分析揭示出高原子序数Cu原子进入Ti3AlC2相Al原子层中并体现出一定的结构有序性

    图2 晶格原子结构示意图显示Cu原子在MAX相中被MX层天然隔离并体现出良好的类酶催化活性

    图3 具有原子分辨的扫描透射电子显微镜技术证实成功合成出首个A位为Cu原子的MAX相材料Nb2CuC

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