Ni纳米孔洞模板的制备  

Preparation of Nickel Template with Nanoholes

作　　者：于冬亮[1] 杨绍光[1] 朱浩[1] 韩毓旺[1] 都有为[1] 

机构地区：[1]南京大学物理系

出　　处：《南京大学学报（自然科学版）》2001年第4期493-496,共4页Journal of Nanjing University（Natural Science）

基　　金：国家重点基础研究发展规划项目 (G19990 6 45 0 8) ;江苏自然科学基金 (BK992 0 7)

摘　　要：使用纯度为 99.5 %的铝片 ,在空气中 5 0 0℃退火 5h ,利用电化学阳极氧化手段将铝片制备成具有纳米级孔洞的氧化铝模板 .用氧化铝模板作母板 ,在高真空下把甲基丙烯酸甲酯(MMA)注入到模板的柱形微孔内进行热聚合 ,制得聚甲基内烯酸甲酯 (PMMA)纳米线阵列复合膜 .把PMMA纳米线陈列复合膜浸入 10 0 g/L的NaOH溶液中 ,去掉氧化铝模板 ,得到PM MA纳米线陈列膜 ,利用化学自动催化方法将Ni沉积到PMMA纳米线阵列上 ,得到Ni纳米孔洞复合膜 ,最后用丙酮将PMMA溶解掉 ,得到具有纳米孔洞阵列的金属Ni模板 .利用透射电子显微镜 (TEM ) ,电子衍射等测试手段对所制备模板进行了研究 .TEM结果显示Ni模板的孔径约为 4 5nm ,孔心距为 6 3nm左右 ,电子衍射结果显示模板是多晶材料 .Nickel template with nanoholes is prepared by two-step replication. Porous alumina membranes with different pore diameters are prepared electrochemically. In the experiments, aluminum foil (99.5% purity) is used as the starting material. After annealed at 500 ℃ for 5 hours in the air, the aluminum foil is chemically polished in 1.0 mol/L NaOH solution for 10 min. The membrane is oxidized at a constant voltage of 20 V in 0.3 mol/L sulphuric acid (H 2SO 4) for 4 hours. The reaction temperature was maintained at 0 ℃ by dipping the cell in a mixture of ice and water. A solution of 5 wt% phosphoric acid is used in the etching treatment step to get different pore diameters by changing etching time at 30 ℃. Porous anodic alumina membrane is thus fabricated and used as the model in the following process. Methyl methacrylate monomer containing 1 % (by weight) benzoyl peroxide, which acted as an initiator for polymerization, was injected into the holes under vacuum conditions and was polymerized by ultraviolet iradiation. After removal of the alumina layer with 10 % (by weight) NaOH, a replicated negative type of polymethyl methacrylate (PMMA) with a cylindrical structure was obtained. The negative type of PMMA had been dipped into the electroless plating solution and the cavity around the PMMA cylindrical was gradually filled up with NiP alloy. The nickel hole array was obtained by dissolving the PMMA with acetone. The metallic template was investigated by transmission electron microscopy (TEM) and Electron diffraction. It was shown that the template has holes about 45 nm in diameter with a center space of 63nm. The distribution of the pores is narrow and the pores are locally ordered. Electron diffraction study revealed that the nickel template is polycrystalline.

关 键 词：纳米孔洞模板 透射电镜 电子衍射 镍 电化学阳极氧化法 氧化铝模板 

分 类 号：TB383[一般工业技术—材料科学与工程]