多孔不锈钢板上制备氮化硼纳米管阵列

发布时间：2018-02-24 13:00

  本文关键词： BNNTs BNNAs 电化学腐蚀 多孔不锈钢板 球磨退火法　出处：《哈尔滨工业大学》2015年硕士论文　论文类型：学位论文

【摘要】：随着纳米材料研究的不断深入,氮化硼纳米管(Boron Nitride Nanotubes,BNNTs)以其独特的性质而受到国内外研究人员的广泛关注。BNNTs作为一种宽禁带半导体,具有不受原子结构影响的稳定电学性质,此外,BNNTs还具有稳定的化学性质、抗氧化性、热稳定性、高热导率、良好的机械强度等,BNNTs的这些优良特性,使其在微纳器件、复合材料、气体存储等方面展露出广阔的应用前景。但目前BNNTs的制备方法大都存在着条件苛刻、设备要求度高、产物产量低、纯度低等问题,而且制备出的纳米管往往分布杂乱、取向不一,这极大程度上阻碍了纳米管的性质研究和应用探索。因此,本文前期探索BNNTs的有效制备,再以此为依据,探索取向一致的纳米管阵列的有效制备方法。本论文对目前国内外关于BNNTs和定向取向纳米管组成的BNNAs(Boron Nitride Nanotube Arrays,BNNAs)的研究进展进行了详细的综述,并提出了以多孔不锈钢板为模板辅助球磨退火法制备BNNAs的实验方案。依据实验方案,第一阶段探索球磨退火法制备BNNTs的工艺条件,选用无定形硼粉、九水硝酸铁、氮氢混合气为原料,以314奥氏体不锈钢板为模板退火后,获得大块的白色粉体材料,经表征产物是结晶度较高的竹节状BNNTs,纳米管的管长范围约为2~8μm,管径范围约为75~100 nm。第二阶段,利用电化学腐蚀制备BNNAs生长所需的多孔不锈钢板基板,并分析直流电压大小、电解液浓度、腐蚀时间等实验参数对腐蚀结果的影响。根据实验结果,发现随着直流电压或电解液浓度的增加,不锈钢板表面的孔径逐渐增大,孔洞逐渐加深,但电压过大或浓度过高时,孔洞逐渐被溶解,规则的孔状结构被破坏。同时,随着电化学腐蚀反应时间的延长,孔的深度不断加深,但当腐蚀时间过长时,孔状结构同样发生被溶解的状况。结合前两个阶段实验结论,采用多孔不锈钢板辅助的球磨退火法制备BNNAs,与第一阶段制备BNNTs的原料配比相同,球磨18 h后,加入乙醇制备硼涂料,涂覆于多孔不锈钢板上放在氮氢混合气、1150℃的条件下进行退火反应,最终在多孔不锈钢板上发现有白色薄膜状物质生成。对产物进行表征分析,发现获得的产物是取向一致、分布密度较高的BNNAs,经进一步的表征,观察到构成阵列的纳米管是结晶度较高的竹节状BNNTs。
[Abstract]:With the development of nanomaterials, Boron Nitride NanobesbesBNNTs (Boron Nitride NanobesbesBNNTs) has been widely concerned by researchers at home and abroad for its unique properties. As a wide band gap semiconductor, BNNTs have stable electrical properties which are not affected by atomic structure. In addition, BNNTs also have stable chemical properties, oxidation resistance, thermal stability, high thermal conductivity, good mechanical strength, and so on. However, there are many problems in the preparation of BNNTs, such as harsh conditions, high equipment requirements, low product yield and low purity. Different orientations greatly hinder the study of the properties and application of nanotubes. Therefore, in this paper, the effective preparation of BNNTs is explored, and based on it, In this paper, the research progress of BNNTs and BNNAs(Boron Nitride Nanotube Arrays-BNNAss, which are composed of BNNAs(Boron Nitride Nanotube, are reviewed in detail. The experimental scheme of preparing BNNAs by using porous stainless steel plate as template was put forward. According to the experimental scheme, the technological conditions of preparing BNNTs by ball milling annealing method were explored in the first stage, the amorphous boron powder and ferric nitrate nine water were selected. After annealing with 314 austenitic stainless steel sheet as template, bulk white powder materials were obtained from nitrogen-hydrogen mixture. The product was bamboo-shaped BNNTs with high crystallinity. The length of nanotubes was about 2 ~ 8 渭 m, and the diameter of nanotubes was about 75 ~ 100 nm. The porous stainless steel plate substrate for the growth of BNNAs was prepared by electrochemical etching. The effects of DC voltage, electrolyte concentration and corrosion time on the corrosion results were analyzed. It is found that with the increase of DC voltage or electrolyte concentration, the pore diameter on the surface of stainless steel plate increases and the hole deepens gradually. However, when the voltage is too high or the concentration is too high, the pore is gradually dissolved and the regular pore structure is destroyed. With the prolongation of electrochemical corrosion reaction time, the depth of the pore deepens, but when the corrosion time is too long, the pore structure also dissolves. The boron coating was prepared by ball milling annealing method assisted by porous stainless steel plate, which was the same as the raw material ratio of the first stage preparation of BNNTs. After 18 h ball milling, the boron coating was prepared by adding ethanol. After annealing reaction at 1150 鈩，

本文编号：1530317