不同炭化条件下Ni掺杂酚醛树脂的炭化研究  

Carbonization of Ni-doped phenol resin under various conditions

作　　者：魏国平 朱伯铨[2] 李享成[2] 马铮 

机构地区：[1]浙江自立股份有限公司,浙江上虞312300 [2]武汉科技大学省部共建耐火材料与冶金国家重点实验室,湖北武汉430081

出　　处：《耐火材料》2015年第4期246-250,共5页Refractories

基　　金：国家自然科学基金项目(51174152);国家"973"计划项目(2012CB722702)

摘　　要：为了提高酚醛树脂的残炭率并优化热解炭的结构和性能，将Ni（NO3）2·6H2O按1：100的质量比掺入热固性酚醛树脂中制备Ni掺杂酚醛树脂，经200℃固化后，分别在不同气氛（埋炭和Ar气氛）和不同温度（600、800、1000和l200℃）下保温3h炭化，然后检测其残炭率，并借助差示扫描量热仪、X射线衍射仪、能谱仪、扫描电镜、透射电镜表征其热分解特征及其热解发的抗氧化性、物柏组成和显微结构。结果表明：1）Ni掺杂酚醛树脂在800和1000℃的残炭率均比未掺杂酚醛树脂的提高较多；2）随炭化温度的升高，M掺杂酚醛树脂热解发逐渐向石墨化碳结构方向演化；3）Ni掺杂酚醛树脂经1000℃炭化形成的热解炭中有大量直径50～100nm、长度可达几十微米的多壁碳纳米管；4）在血气氛中炭化更有利于碳纳米管的生成，并且热解发具有更高的残炭率和结晶度；5）1200℃炭化形成的热解炭的抗氧化性显著提高，氧化峰值温度比未掺杂酚醛树脂的提高约84℃。Ni-doped phenol resin was prepared with 1：100 mass ratio of Ni（ NO3）2 · 6H20 to thermosetting phenol resin to optimize the structure and properties of pyrolytic carbon derived from phenol resin and in- crease its carbon yield. The specimens were cured at 200 ℃ and coked under different atmospheres （car- bon-embedded atmosphere and Ar atmosphere） and at different temperatures （600,800,1 000 and 1 200 ℃） for 3 h, respectively. The carbon yield was measured. Thermal decomposition characteristics of Ni- doped phenol resin, and the oxidation resistance, phase composition and microstructure of pyrolytic carbon were characterized by differential scanning calorimetry,X-ray diffraction, energy dispersive spectroscopy, scanning electron microscopy and transmission electron microscopy. The results show that the carbon yield of Ni-doped phenol resin coked at 800 or 1 000 ℃ is increased significantly, compared with that without any dopants. The graphitization degree of pyrolytic carbon structure derived from Ni-doped phenol resin increa- ses with the increase of carbonization temperature. The massive multi-wall carbon nanotubes of 50 - 100 nm in diameter and of micrometre scale in length are generated at 1 000 ℃. Compared with the carbon-em- bedded atmosphere,carbon nanotubes can be more easily generated under Ar atmosphere, resulting in higher carbon yield and degree of crystallinity of the pyrolytic carbon derived from Ni-doped phenol resin. The oxidation resistance of the pyrolytic carbon derived from Ni-doped phenol resin at 1 200 ℃ is improved significantly and its highest oxidation temperature is increased by about 84 ℃,compared with that from Ni free phenol resin.

关 键 词：酚醛树脂 镍掺杂 炭化 热解炭 碳纳米管 抗氧化性能 

分 类 号：TQ175.12[化学工程—硅酸盐工业]