刘慧娟, 白帆, 王恩会, 杨涛, 陈俊红, 周国治, 侯新梅. 层状氮化硼纳米片的制备及表征[J]. 工程科学学报, 2019, 41(12): 1543-1549. DOI: 10.13374/j.issn2095-9389.2019.07.04.032
引用本文: 刘慧娟, 白帆, 王恩会, 杨涛, 陈俊红, 周国治, 侯新梅. 层状氮化硼纳米片的制备及表征[J]. 工程科学学报, 2019, 41(12): 1543-1549. DOI: 10.13374/j.issn2095-9389.2019.07.04.032
LIU Hui-juan, BAI Fan, WANG En-hui, YANG Tao, CHEN Jun-hong, CHOU Kuo-Chih, HOU Xin-mei. Preparation and characterization of layered boron nitride nanosheets[J]. Chinese Journal of Engineering, 2019, 41(12): 1543-1549. DOI: 10.13374/j.issn2095-9389.2019.07.04.032
Citation: LIU Hui-juan, BAI Fan, WANG En-hui, YANG Tao, CHEN Jun-hong, CHOU Kuo-Chih, HOU Xin-mei. Preparation and characterization of layered boron nitride nanosheets[J]. Chinese Journal of Engineering, 2019, 41(12): 1543-1549. DOI: 10.13374/j.issn2095-9389.2019.07.04.032

层状氮化硼纳米片的制备及表征

Preparation and characterization of layered boron nitride nanosheets

  • 摘要: 基于前驱体合成与氨气氮化两步法,通过对前驱体合成关键参数B源/N源比、分散剂种类、前驱体干燥方式进行调控,实现了大比表面积、少层氮化硼纳米片材料的制备。其优化条件为以硼酸为硼源,尿素为氮源,硼酸与尿素摩尔比为1∶30,甲醇和去离子水作为分散剂,利用真空冷冻干燥方式合成前驱体。将前驱体在氨气气氛下900 ℃保温3 h合成了氮化硼纳米片。利用X射线衍射测试、X射线光电子能谱测试、拉曼光谱测试、热重分析测试等对合成产物进行了物相和结构表征,利用扫描电子显微镜、原子力显微镜、透射电子显微镜、氮气吸脱附曲线等对合成产物进行了形貌及比表面积表征。结果表明:合成的氮化硼为六方氮化硼纳米片(h-BNNSs),纯度高,形貌类石墨烯,层数为2~4层,厚度平均为1 nm,比表面积为871.8 m2·g−1,单次产物质量平均可达240 mg,合成产物平均产率可达96.7%。该方法简单易操作,实现了大比表面积少层氮化硼的制备,有助于氮化硼在各应用领域的研究,如氮化硼/石墨烯复合材料、纳米电子器件、污染物的吸附、储氢等。

     

    Abstract: Hexagonal boron nitride nanosheets (h-BNNSs) are two-dimensional nanomaterials whose structure, similar to graphene, is called white graphene. They have excellent physical and chemical properties. Few-layered and monolayer h-BNNSs have more extensive applications compared to block BNs due to their wider band gap and stronger insulation. However, the existing preparation methods have the disadvantages of uncontrollable product size, low yield, high cost, and pollution. Researchers are striving to develop an efficient and cheap method, and some have tried to prepared h-BNNSs through evaporation and recrystallization. However, it is difficult to control morphology in this method and prepared products are usually thick with uneven size distribution. Meanwhile, vacuum freeze-drying has been widely used in functional porous ceramics due its simple operation, controllability, and environmental friendliness. In this study, based on the two-step process of precursor synthesis and ammonia nitriding, few-layered h-BNNSs with large surface areas were successfully synthesized on a large scale by controlling key factors of precursor synthesis, such as ratio of atoms B to N in the raw material, dispersant, and drying method. The optimum preparation was using boric acid and urea with a molar ratio of 1∶30 as the source of B and N, and using methanol/deionized water as dispersant to obtain the precursors by vacuum freeze drying. Precursors were then transformed from ammonia vapor to nitride for 3 h at 900 ℃. The product was characterized by X-Ray diffraction, X-ray photoelectron spectroscopy, Raman spectra, thermogravimetric analysis, and differential thermal analysis for phase and molecular structure, and scanning electron microscope, atomic force microscope, transmission electron microscope, and N2 adsorption-desorption isotherms for microstructure and specific surface area. Results indicate that the products are h-BNNSs with high purity, two to four atomic layers, 1 nm thickness, and with a high specific surface area of 871.8 m2·g−1, similar to the microstructure of graphene. Single product mass averages 240 mg and average yield is steadily 96.7%. This method is economical, simple, and easy to operate. It could achieve macro-synthesis of few-layered h-BNNSs with a large area, conducive to research on boron nitride in various field applications, such as boron nitride/graphene composite materials, nano-electronic devices, pollutant adsorption, hydrogen storage, etc.

     

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