球磨增强液相剥离法制备h-BN纳米片的工艺研究  

Preparation Process of h-BN Nanosheets by Ball Milling Enhanced Liquid Phase Exfoliation Methods

作　　者：武黎明 武杨 张振忠[1] 赵芳霞[1] WU Li-ming;WU Yang;ZHANG Zhen-zhong;ZHAO Fang-xia(College of Materials Science&Engineering,Nanjing Tech University,Nanjing 210009,China)

机构地区：[1]南京工业大学材料科学与工程学院,南京210009

出　　处：《人工晶体学报》2018年第11期2248-2254,共7页Journal of Synthetic Crystals

基　　金：江苏高校优势学科建设工程项目(苏证办发2011-6)

摘　　要：针对异丙醇溶液中高质量、高产率六方氮化硼(h-BN)纳米片的制备工艺开发问题,本文在研究h-BN粉在异丙醇(IPA)溶液中分散工艺及其悬浮稳定性的基础上,采用球磨与超声相结合的方法研究其剥离工艺,系统研究超声时间、功率、h-BN浓度及球磨时间对h-BN剥离效果的影响。采用XRD、扫描电镜(SEM)、透射电镜(TEM)、原子力显微镜(AFM)等对h-BN球磨粉体和所制备的h-BN纳米片进行了表征,并用吸光度表征了h-BN剥离产率。研究结果表明:在异丙醇溶液中加入5wt%的油酸(OA)可以提升h-BN粉的悬浮稳定性,从而提升剥离效果和效率;在液相超声剥离时,提高粉体浓度,纳米片层数提高;提高超声功率,可获得少层h-BN纳米片,但纳米片均匀性下降且制备效率较低。将h-BN粉与异丙醇溶液在300 r/min转速下球磨10 h后,以0. 25 mg/m L的BN/IPA溶液在350 W功率下超声20 h,剥离出的h-BN纳米片为10层以下,层间距为0. 33 nm,同时使剥离产率提高6. 4倍。Aiming at the development of high-quality,high-yield hexagonal boron nitride(h-BN)nanosheets in isopropanol solution,based on the dispersion process of h-BN powder in IPA solution and its suspension stability,the exfoliation process was studied by the combination of ball milling and ultrasonic in this paper,the ultrasonic time,power,h-BN concentration and ball milling time was systematically investigated.The h-BN nanosheet and the ball milled h-BN powder were characterized by XRD,SEM,TEM and AFM,and the absorbance was used to characterize the h-BN stripping yield.The results showed that adding 5wt%oleic acid(OA)into IPA solution can improve the suspension stability of h-BN powder,and also the exfoliation effect,the layers of h-BN nanosheets were increased when increased the concentration of BN/IPA solution,by increasing the ultrasonic power,the h-BN nano-sheet with fewer layers could be obtained,but the homogeneity of the nanosheet was decreased and the preparation efficiency was low.The h-BN powder and the IPA solution were ball milled at 300 r/min for 10 h firstly,then ultrasonic at 350 W power for 20 h,and the concentration of BN/IPA solution was 0.25 mg/mL,h-BN nanosheets were obtained under 10 layers,the layer space is 0.33 nm,and the yield increased by 6.4 times.

关 键 词：h-BN纳米片 液相剥离 异丙醇介质 球磨 分散 

分 类 号：O484[理学—固体物理]